Food and Drug Administration, HHS Pt. 177
(d) Adjuvant substances permitted to tended technical effect or exceed 15 be used in the preparation of slimicides percent by weight of the finished paper. include substances generally recog- (2) Conditions of use. The glassine and nized as safe for use in food, substances greaseproof papers are used for pack- generally recognized as safe for use in aging dry food or as the food-contact paper and paperboard, substances per- surface for dry food. mitted to be used in paper and paper- board by other regulations in this § 176.350 Tamarind seed kernel pow- chapter, and the following: der. Tamarind seed kernel powder may be Acetone. safely used as a component of articles Butlylene oxide. Dibutyl phthalate. intended for use in producing, manu- Didecyl phthalate. facturing, packing, processing, pre- N,N-Dimethylformamide. paring, treating, packaging, trans- Dodecyl phthalate. porting, or holding food, subject to the Ethanolamine. provisions of this section. Ethylene glycol. (a) Tamarind seed kernel powder is Ethylenediamine. the ground kernel of tamarind seed N-methyl-2-pyrrolidone (CAS Reg. No. 872– (Tamarindus indica L.) after removal of 50–4). the seed coat. a,a′-[Methylenebis[4-(1,1,3,3-tetramethyl- butyl)-o-phenylene]] bis[omega-hydroxypoly (b) It is used in the manufacture of (oxyethylene)] having 6–7.5 moles of ethyl- paper and paperboard. ene oxide per hydroxyl group. Monomethyl ethers of mono-, di-, and tri- PART 177—INDIRECT FOOD propylene glycol. ADDITIVES: POLYMERS Nonylphenol reaction product with 9 to 12 molecules of ethylene oxide. Octylphenol reaction product with 25 mol- Subpart A [Reserved] ecules of propylene oxide and 40 molecules of ethylene oxide. Subpart B—Substances for Use as Basic Components of Single and Repeated [42 FR 14554, Mar. 15, 1977, as amended at 42 Use Food Contact Surfaces FR 41854, Aug. 19, 1977; 44 FR 75627, Dec. 21, 1979; 46 FR 36129, July 14, 1981; 49 FR 5748, Sec. Feb. 15, 1984; 51 FR 19059, May 27, 1986; 51 FR 177.1010 Acrylic and modified acrylic plas- 43734, Dec. 4, 1986; 54 FR 18103, Apr. 27, 1989; tics, semirigid and rigid. 55 FR 31825, Aug. 6, 1990; 64 FR 46130, Aug. 24, 177.1020 Acrylonitrile/butadiene/styrene co– 1999; 64 FR 69900, Dec. 15, 1999; 65 FR 40497, polymer. June 30, 2000; 65 FR 70790, Nov. 28, 2000] 177.1030 Acrylonitrile/butadiene/styrene/ methyl methacrylate copolymer. § 176.320 Sodium nitrate-urea complex. 177.1040 Acrylonitrile/styrene copolymer. Sodium nitrate-urea complex may be 177.1050 Acrylonitrile/styrene copolymer modified with butadiene/styrene elas- safely used as a component of articles tomer. intended for use in producing, manu- 177.1060 n-Alkylglutarimide/acrylic copoly- facturing, packing, processing, pre- mers. paring, treating, packaging, trans- 177.1200 Cellophane. porting, or holding food, subject to the 177.1210 Closures with sealing gaskets for provisions of this section. food containers. (a) Sodium nitrate-urea complex is a 177.1211 Cross-linked polyacrylate copoly- clathrate of approximately two parts mers. 177.1240 1,4-Cyclohexylene dimethylene urea and one part sodium nitrate. terephthalate and 1,4-cyclohexylene (b) Sodium nitrate-urea complex con- dimethylene isophthalate copolymer. forming to the limitations prescribed 177.1310 Ethylene-acrylic acid copolymers. in paragraph (b)(1) of this section is 177.1312 Ethylene-carbon monoxide copoly- used as provided in paragraph (b)(2) of mers. this section. 177.1315 Ethylene-1,4-cyclohexylene (1) Limitations. (i) It is used as a plas- dimethylene terephthalate copolymers. 177.1320 Ethylene-ethyl acrylate copoly- ticizer in glassine and greaseproof mers. paper. 177.1330 Ionomeric resins. (ii) The amount used does not exceed 177.1340 Ethylene-methyl acrylate copoly- that required to accomplish its in- mer resins.
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177.1345 Ethylene/1,3-phenylene oxyethylene 177.1970 Vinyl chloride-lauryl vinyl ether isophthalate/terephthalate copolymer. copolymers. 177.1350 Ethylene-vinyl acetate copolymers. 177.1980 Vinyl chloride-propylene copoly- 177.1360 Ethylene-vinyl acetate-vinyl alco- mers. hol copolymers. 177.1990 Vinylidene chloride/methyl acry- 177.1380 Fluorocarbon resins. late copolymers. 177.1390 Laminate structures for use at tem- 177.2000 Vinylidene chloride/methyl acry- peratures of 250 °F and above. late/methyl methacrylate polymers. 177.1395 Laminate structures for use at tem- peratures between 120 °F and 250° F. Subpart C—Substances for Use Only as 177.1400 Hydroxyethyl cellulose film, water- Components of Articles Intended for insoluble. Repeated Use 177.1420 Isobutylene polymers. 177.1430 Isobutylene-butene copolymers. 177.2210 Ethylene polymer, 177.1440 4,4′-Isopropylidenediphenol- chlorosulfonated. epichlorohydrin resins minimum molec- 177.2250 Filters, microporous polymeric. ular weight 10,000. 177.2260 Filters, resin-bonded. 177.1460 Melamine-formaldehyde resins in 177.2280 4,4′-Isopropylidenediphenol- molded articles. epichlorohydrin thermosetting epoxy 177.1480 Nitrile rubber modified acrylo- resins. nitrile-methyl acrylate copolymers. 177.2355 Mineral reinforced nylon resins. 177.1500 Nylon resins. 177.2400 Perfluorocarbon cured elastomers. 177.1520 Olefin polymers. 177.2410 Phenolic resins in molded articles. 177.1550 Perfluorocarbon resins. 177.2415 Poly(aryletherketone) resins. 177.1555 Polyarylate resins. 177.2420 Polyester resins, cross-linked. 177.1556 Polyaryletherketone resins. 177.2430 Polyether resins, chlorinated. 177.1560 Polyarylsulfone resins. 177.2440 Polyethersulfone resins. 177.1570 Poly-1-butene resins and butene/ 177.2450 Polyamide-imide resins. ethylene copolymers. 177.2460 Poly(2,6-dimethyl-1,4-phenylene) 177.1580 Polycarbonate resins. oxide resins. 177.1585 Polyestercarbonate resins. 177.2465 Polymethylmethacrylate/poly(tri 177.1590 Polyester elastomers. methoxysilylpropyl) methacrylate co- 177.1595 Polyetherimide resin. polymers. 177.1600 Polyethylene resins, carboxyl modi- 177.2470 Polyoxymethylene copolymer. fied. 177.2480 Polyoxymethylene homopolymer. 177.1610 Polyethylene, chlorinated. 177.2490 Polyphenylene sulfide resins. 177.1615 Polyethylene, fluorinated. 177.2500 Polyphenylene sulfone resins. 177.1620 Polyethylene, oxidized. 177.2510 Polyvinylidene fluoride resins. 177.1630 Polyethylene phthalate polymers. 177.2550 Reverse osmosis membranes. 177.1632 Poly (phenyleneterephthalamide) 177.2600 Rubber articles intended for re- resins. peated use. 177.1635 Poly(p-methylstyrene) and rubber- 177.2710 Styrene-divinylbenzene resins, modified poly(p-methylstyrene). cross-linked. 177.1637 Poly(oxy-1,2- 177.2800 Textiles and textile fibers. ethanediyloxycarbonyl-2,6- 177.2910 Ultra-filtration membranes. naphthalenediylcarbonyl) resins. AUTHORITY: 21 U.S.C. 321, 342, 348, 379e. 177.1640 Polystyrene and rubber-modified polystyrene. SOURCE: 42 FR 14572, Mar. 15, 1977, unless 177.1650 Polysulfide polymer-polyepoxy res- otherwise noted. ins. EDITORIAL NOTE: Nomenclature changes to 177.1655 Polysulfone resins. part 177 appear at 61 FR 14482, Apr. 2, 1996. 177.1660 Poly (tetramethylene terephthalate). 177.1670 Polyvinyl alcohol film. Subpart A [Reserved] 177.1680 Polyurethane resins. 177.1810 Styrene block polymers. Subpart B—Substances for Use as 177.1820 Styrene-maleic anhydride copoly- mers. Basic Components of Single 177.1830 Styrene-methyl methacrylate co- and Repeated Use Food Con- polymers. tact Surfaces 177.1850 Textryls. 177.1900 Urea-formaldehyde resins in molded § 177.1010 Acrylic and modified acrylic articles. plastics, semirigid and rigid. 177.1950 Vinyl chloride-ethylene copoly- mers. Semirigid and rigid acrylic and modi- 177.1960 Vinyl chloride-hexene-1 copoly- fied acrylic plastics may be safely used mers. as articles intended for use in contact
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with food, in accordance with the fol- (i) List of minor monomers: lowing prescribed conditions. The Acrylamide. acrylic and modified acrylic polymers Acrylic acid or plastics described in this section 1,3-Butylene glycol dimethacrylate. also may be safely used as components 1,4-Butylene glycol dimethacrylate. of articles intended for use in contact Diethylene glycol dimethacrylate. with food. Diproplylene glycol dimethacrylate. (a) The optional substances that may Divinylbenzene. be used in the formulation of the Ethylene glycol dimethacrylate. Itaconic acid. semirigid and rigid acrylic and modi- Methacrylic acid. fied acrylic plastics, or in the formula- N-Methylolacrylamide. tion of acrylic and modified acrylic N-Methylolmethacrylamide. components of articles, include sub- 4-Methyl-1,4-pentanediol dimethacrylate. stances generally recognized as safe in Propylene glycol dimethacrylate. food, substances used in accordance Trivinylbenzene. with a prior sanction or approval, sub- (ii) List of minor monomers limited stances permitted for use in such plas- to use only in plastic articles intended tics by regulations in parts 170 through for repeated use in contact with food: 189 of this chapter, and substances identified in this paragraph. At least 50 Allyl methacrylate [Chemical Abstracts Service Registry No. 96–05–9] weight-percent of the polymer content tert-Butyl acrylate. of the acrylic and modified acrylic ma- tert-Butylaminoethyl methacrylate. terials used as finished articles or as sec-Butyl methacrylate. components of articles shall consist of tert-Butyl methacrylate. polymer units derived from one or Cyclohexyl methacrylate. more of the acrylic or methacrylic Dimethylaminoethyl methacrylate. monomers listed in paragraph (a)(1) of 2-Ethylhexyl methacrylate. Hydroxyethyl methacrylate. this section. Hydroxyethyl vinyl sulfide. (1) Homopolymers and copolymers of Hydroxypropyl methacrylate. the following monomers: Isobornyl methacrylate. Isobutyl methacrylate. n-Butyl acrylate. Isopropyl acrylate. n-Butyl methacrylate. Ethyl acrylate. Isopropyl methacrylate. 2-Ethylhexyl acrylate. Methacrylamide. Ethyl methacrylate. Methacrylamidoethylene urea. Methyl acrylate. Methacryloxyacetamidoethylethylene urea. Methyl methacrylate. Methacryloxyacetic acid. n-Propyl methacrylate. (2) Copolymers produced by copolym- 3,5,5-Trimethylcyclohexyl methacrylate. erizing one or more of the monomers (4) Polymers identified in paragraphs listed in paragraph (a)(1) of this section (a)(1), (2), and (3) of this section are with one or more of the following mixed together and/or with the fol- monomers: lowing polymers, provided that no Acrylonitrile. chemical reactions, other than addi- Methacrylonitrile. tion reactions, occur when they are α-Methylstyrene. mixed: Styrene. Vinyl chloride. Butadiene-acrylonitrile copolymers. Vinylidene chloride. Butadiene-acrylonitrile-styrene copolymers. Butadiene-acrylonitrile-styrene-methyl (3) Polymers identified in paragraphs methacrylic copolymers. (a)(1) and (2) of this section containing Butadiene-styrene copolymers. no more than 5 weight-percent of total Butyl rubber. polymer units derived by copolym- Natural rubber. erization with one or more of the Polybutadiene. monomers listed in paragraph (a)(3)(i) Poly (3-chloro-1,3-butadiene). and (ii) of this section. Monomers list- Polyester identified in § 175.300(b)(3)(vii) of this chapter. ed in paragraph (a)(3)(ii) of this section Polyvinyl chloride. are limited to use only in plastic arti- Vinyl chloride copolymers complying with cles intended for repeated use in con- § 177.1980. tact with food. Vinyl chloride-vinyl acetate copolymers.
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(5) Antioxidants and stabilizers iden- (1) Total nonvolatile extractives not tified in § 175.300(b)(3)(xxx) of this chap- to exceed 0.3 milligram per square inch ter and the following: of surface tested. (2) Potassium permanganate oxidiz- Di-tert-butyl-p-cresol. 2-Hydroxy-4-methoxybenzophenone. able distilled water and 8 and 50 per- 2-Hydroxy-4-methoxy-2- cent alcohol extractives not to exceed carboxybenzophenone. an absorbance of 0.15. 3-Hydroxyphenyl benzoate. (3) Ultraviolet-absorbing distilled p-Methoxyphenol. water and 8 and 50 percent alcohol ex- Methyl salicylate. tractives not to exceed an absorbance Octadecyl 3,5-di-tert-butyl-4-hydroxyhydro- of 0.30. cinnamate (CAS Reg. No. 2082–79–3): For (4) Ultraviolet-absorbing n-heptane use only: (1) At levels not exceeding 0.2 extractives not to exceed an absorb- percent by weight in semirigid and rigid ance of 0.10. acrylic and modified acrylic plastics, where the finished articles contact foods (c) Analytical methods—(1) Selection of containing not more than 15 percent alco- extractability conditions. These are to be hol; and (2) at levels not exceeding 0.01 per- chosen as provided in § 176.170(c) of this cent by weight in semirigid and rigid chapter. acrylic and modified acrylic plastics in- (2) Preparation of samples. Sufficient tended for repeated food-contact use where samples to allow duplicates of all ap- the finished article may be used for foods plicable tests shall be cut from the ar- containing more than 15 percent alcohol. ticles or formed from the plastic com- Phenyl salicylate. position under tests, as strips about 2.5 (6) Release agents: Fatty acids de- inches by about 0.85-inch wide by about rived from animal and vegetable fats 0.125-inch thick. The total exposed sur- and oils, and fatty alcohols derived face should be 5 square inches ±0.5- from such acids. square inch. The samples, after prepa- (7) Surface active agent: Sodium ration, shall be washed with a clean dodecylbenzenesulfonate. brush under hot tapwater, rinsed under (8) Miscellaneous materials: running hot tapwater (140 °F min- imum), rinsed with distilled water, and Di(2-ethylhexyl) phthalate, for use only as a flow promoter at a level not to exceed 3 air-dried in a dust-free area or in a des- weight-percent based on the monomers. iccator. Dimethyl phthalate. (3) Preparation of solvents. The water Oxalic acid, for use only as a polymerization used shall be double-distilled water, catalyst aid. prepared in a still using a block tin Tetraethylenepentamine, for use only as a condenser. The 8 and 50 percent (by vol- catalyst activator at a level not to exceed ume) alcohol solvents shall be prepared 0.5 weight-percent based on the monomers. from ethyl alcohol meeting the speci- Toluene. fications of the United States Pharma- Xylene. copeia XX and diluted with double-dis- (b) The semirigid and rigid acrylic tilled water that has been prepared in a and modified acrylic plastics, in the still using a tin block condenser. The finished form in which they are to con- n-heptane shall be spectrophotometric tact food, when extracted with the sol- grade. Adequate precautions must be vent or solvents characterizing the taken to keep all solvents dust-free. type of food and under the conditions (4) Blank values on solvents. (i) Dupli- of time and temperature as determined cate determinations of residual solids from tables 1 and 2 of § 176.170(c) of this shall be run on samples of each solvent chapter, shall yield extractives not to that have been exposed to the tempera- exceed the following, when tested by ture-time conditions of the extraction the methods prescribed in paragraph test without the plastic sample. Sixty (c) of this section. The acrylic and milliliters of exposed solvent is modified acrylic polymers or plastics pipetted into a clean, weighed plat- intended to be used as components of inum dish, evaporated to 2–5 milliliters articles also shall yield extractives not on a nonsparking, low-temperature hot to exceed the following limitations plate and dried in 212 °F oven for 30 when prepared as strips as described in minutes. The residue for each solvent paragraph (c)(2) of this section: shall be determined by weight and the
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average residue weight used as the gion of 544 to 552 mµ should be 1.16 but blank value in the total solids deter- must not be less than 1.05 nor more mination set out in paragraph (c)(6) of than 1.25. The absorbance in the 8 and this section. The residue for an accept- 50 percent alcohol must not be less able solvent sample shall not exceed 0.5 than 0.85 nor more than 1.15. milligram per 60 milliliters. (v) Duplicate permanganate test de- (ii) For acceptability in the ultra- terminations shall be run on samples of violet absorbers test, a sample of each distilled water and 8 and 50 percent al- solvent shall be scanned in an ultra- cohol solvents that have been exposed violet spectrophotometer in 5-centi- to the temperature-time conditions of meter silica spectrophotometric ab- the extraction test without the plastic sorption cells. The absorbance of the sample. The procedure shall be as de- distilled water when measured versus air in the reference cell shall not ex- scribed in paragraph (c)(7)(iv) of this ceed 0.03 at any point in the wave- section, except that the appropriate ex- length region of 245 to 310 mµ. The ab- posed solvent shall be substituted sorbance of the 8 percent alcohol when where the directions call for sample ex- measured versus distilled water in the tract. The average difference in the reference cell shall not exceed 0.01 at absorbances in the region of 544 to 552 any point in the wavelength region of mµ shall be used as a blank correction 245 to 310 mµ. The absorbance of the 50 for the determination of permanganate percent alcohol when measured versus oxidizable extractives according to distilled water in the reference cell paragraph (c)(7)(iv) of this section. shall not exceed 0.05 at any point in the (5) Extraction procedure. For each ex- wavelength region of 245 to 310 mµ. The traction, place a plastic sample in a absorbance of the heptane when meas- clean 25 millimeters × 200 millimeters ured versus distilled water in the ref- hard-glass test tube and add solvent erence cell shall not exceed 0.15 at 245, equal to 10 milliliters of solvent per 0.09 at 260, 0.04 at 270, and 0.02 at any square inch of plastic surface. This point in the wavelength region of 280 to amount will be between 45 milliliters µ 310 m . and 55 milliliters. The solvent must be (iii) Duplicate ultraviolet blank de- preequilibrated to the temperature of terminations shall be run on samples of the extraction test. Close the test tube each solvent that has been exposed to with a ground-glass stopper and expose the temperature-time conditions of the to the specified temperature for the extraction test without the plastic sample. An aliquot of the exposed sol- specified time. Cool the tube and con- vent shall be measured versus the un- tents to room temperature if nec- exposed solvent in the reference cell. essary. The average difference in the (6) Determination of total nonvolatile absorbances at any wavelength in the extractives. Remove the plastic strip region of 245 to 310 mµ shall be used as from the solvent with a pair of clean a blank correction for the ultraviolet forceps and wash the strip with 5 milli- absorbers measured at the same wave- liters of the appropriate solvent, add- length according to paragraph (c)(8)(ii) ing the washings to the contents of the of this section. test tube. Pour the contents of the test (iv) The acceptability of the solvents tube into a clean, weighed platinum for use in the permanganate test shall dish. Wash the tube with 5 milliliters be determined by preparing duplicate of the appropriate solvent and add the permanganate test blanks according to solvent to the platinum dish. Evapo- paragraph (c)(7)(iv) of this section. For rate the solvent to 2–5 milliliters on a this test, the directions referring to nonsparking, low-temperature the sample extract shall be dis- hotplate. Complete the evaporation in regarded. The blanks shall be scanned a 212 °F oven for 30 minutes. Cool the in 5-centimeter silica dish in a desiccator for 30 minutes and spectrophotometric cells in the spec- weigh to the nearest 0.1 milligram. Cal- trophotometer versus the appropriate culate the total nonvolatile extractives solvent as reference. The absorbance in distilled water in the wavelength re- as follows:
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− Erlenmeyer flask. Pipette exactly 3.0 Milligrams extractives = eb milliliters of 154 parts per million per square inch aqueous potassium permanganate solu- s tion into the p-methoxyphenol and ex- Extractives in parts eb actly 3.0 milliliters into the blank, in =×100 that order. Swirl both flasks to mix the per million s contents and then transfer aliquots where: from each flask into matched 5-centi- e=Total increase in weight of the dish, in meter spectrophotometric absorption milligrams. cells. The cells are placed in the spec- b=Blank value of the solvent in milligrams, trophotometer cell compartment with as determined in paragraph (c)(4)(i) of the p-methoxyphenol solution in the this section. reference beam. Spectrophotometric s=Total surface of the plastic sample in measurement is conducted as in para- square inches. graph (c)(7)(iv) of this section. The ab- (7) Determination of potassium per- sorbance reading in the region 544–552 manganate oxidizable extractives. (i) Pi- mµ should be 0.24 but must be not less pette 25 milliliters of distilled water than 0.12 nor more than 0.36. This test into a clean 125-milliliter Erlenmeyer shall be run in duplicate. For the pur- flask that has been rinsed several pose of ascertaining compliance with times with aliquots of distilled water. the limitations in paragraph (b)(2) of This is the blank. Prepare a distilled this section, the absorbance measure- water solution containing 1.0 part per ments obtained on the distilled water million of p-methoxyphenol (melting extracts according to paragraph point 54–56 °C, Eastman grade or equiv- (c)(7)(iv) of this section shall be multi- alent). Pipette 25 milliliters of this p- plied by a correction factor, calculated methoxyphenol solution into a rinsed as follows:
024. = Correction factor for water extracts. Average of duplicate ρ -methoxyphenol absorbance determinations according to this paragraph (c)(7)(i) of this section
(ii) The procedure in paragraph ascertaining compliance with the limi- (c)(7)(i) of this section is repeated ex- tations prescribed in paragraph (b)(2) of cept that, in this instance, the solvent this section, the absorbance measure- shall be 8 percent alcohol. The absorb- ments obtained on the 8 percent alco- ance in the region 544–552 mµ should be hol extracts according to paragraph 0.26 but must be not less than 0.13 nor (c)(7)(iv) of this section shall be multi- more than 0.39. This test shall be run in plied by a correction factor, calculated duplicate. For the purpose of as follows:
026. = Correction factor for aqueous Average of duplicate ρ -methoxyphenol 8 percent alcohol extracts. absorbance determination according to this paragraph (c)(7)(ii) of this section
(iii) The procedure in paragraph ance in the region 544–552 mµ should be (c)(7)(i) of this section is repeated ex- 0.25 but must be not less than 0.12 nor cept that, in this instance, the solvent more than 0.38. This test shall be run in shall be 50 percent alcohol. The absorb- duplicate. For the purpose of
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ascertaining compliance with the limi- hol extracts according to paragraph tations prescribed in paragraph (b)(2) of (c)(7)(iv) of this section shall be multi- this section, the absorbance measure- plied by a correction factor, calculated ments obtained on the 50 percent alco- as follows:
025. = Correction factor for 50 percent Average of duplicate ρ -methoxyphenol aqueous alcohol extracts. absorbance determinations according to paragraph (c)(7)(ii) of this section
(iv) Water and 8 and 50 percent alcohol nate was added to the solutions. The extracts. Pipette 25 milliliters of the ap- height of the absorbance peak shall be propriate solvent into a clean, 125-mil- measured, corrected for the blank as liliter Erlenmeyer flask that has been determined in paragraph (c)(4)(v) of rinsed several times with aliquots of this section, and multiplied by the ap- the same solvent. This is the blank. propriate correction factor determined Into another similarly rinsed flask, pi- according to paragraph (c)(7) (i), (ii), pette 25 milliliters of the sample ex- and (iii) of this section. This test shall tract that has been exposed under the be run in duplicate and the two results conditions specified in paragraph (c)(5) averaged. of this section. Pipette exactly 3.0 mil- (8) Determination of ultraviolet-absorb- liliters of 154 parts per million aqueous ing extractives. (i) A distilled water so- potassium permanganate solution into lution containing 1.0 part per million the sample and exactly 3.0 milliliters of p-methoxyphenol (melting point 54 into the blank, in that order. Before °C–56 °C. Eastman grade or equivalent) use, the potassium permanganate solu- tion shall be checked as in paragraph shall be scanned in the region 360 to 220 µ (c)(7)(i) of this section. Both flasks are m in 5-centimeter silica spectrophoto- swirled to mix the contents, and then metric absorption cells versus a dis- aliquots from each flask are trans- tilled water reference. The absorbance ferred to matched 5-centimeter at the wavelength of maximum absorb- spectrophotometric absorption cells. ance (should be about 285 mµ) is about Both cells are placed in the spectro- 0.11 but must be not less than 0.08 nor photometer cell compartment with the more than 0.14. This test shall be run in sample solution in the reference beam. duplicate. For the purpose of The spectrophotometer is adjusted for ascertaining compliance with the limi- 0 and 100 percent transmittance at 700 tations prescribed in paragraph (b) (3) mµ. The spectrum is scanned on the ab- and (4) of this section, the absorbance sorbance scale from 700 mµ to 500 mµ in obtained on the extracts according to such a way that the region 544 mµ to paragraph (c)(8)(ii) of this section shall 552 mµ is scanned within 5 minutes to be multiplied by a correction factor, 10 minutes of the time that permanga- calculated as follows:
011. = Correction factor for ultraviolet Average of duplicate ρ -methoxyphenol absorbers test. absorbance determinations according to this paragraph (c)(8)(i) of this section
(ii) An aliquot of the extract that has tion is scanned in the wavelength re- been exposed under the conditions gion 360 to 220 mµ versus the appro- specified in paragraph (c)(5) of this sec- priate solvent reference in matched 5-
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centimeter silica spectrophotometric butadiene and 23 to 28 parts by weight absorption cells. The height of any ab- of styrene and (ii) 3 to 8 parts by sorption peak shall be measured, cor- weight of a graft polymer having the rected for the blank as determined in same composition range as the matrix paragraph (c)(4)(iii) of this section, and polymer. multiplied by the correction factor de- (b) Adjuvants. The copolymer identi- termined according to paragraph fied in paragraph (a) of this section (c)(8)(i) of this section. may contain adjuvant substances re- (d) In accordance with current good quired in its production. Such adju- manufacturing practice, finished vants may include substances gen- semirigid and rigid acrylic and modi- erally recognized as safe in food, sub- fied acrylic plastics, and articles con- stances used in accordance with prior taining these polymers, intended for repeated use in contact with food shall sanction, substances permitted in this be thoroughly cleansed prior to their part, and the following: first use in contact with food. Substance Limitations (e) Acrylonitrile copolymers identi- fied in this section shall comply with 2-Mercapto- ethanol ...... The finished copolymer shall the provisions of § 180.22 of this chap- contain not more than 100 ppm 2-mercaptoethanol ac- ter. rylonitrile adduct as deter- (f) The acrylic and modified acrylic mined by a method titled polymers identified in and complying ‘‘Analysis of Cycopac Resin for Residual β-(2- with this section, when used as compo- Hydroxyethylmercapto) pro- nents of the food-contact surface of an pionitrile,’’ which is incor- article that is the subject of a regula- porated by reference. Cop- tion in this part and in parts 174, 175, ies are available from the Bureau of Foods (HFSÐ 176, and 178 of this chapter, shall com- 200), Food and Drug Ad- ply with any specifications and limita- ministration, 200 C St. tions prescribed by such regulation for SW., Washington, DC 20204, or available for in- the article in the finished form in spection at the Office of which it is to contact food. the Federal Register, 800 North Capitol Street, NW., [42 FR 14572, Mar. 15, 1977; 42 FR 56728, Oct. suite 700, Washington, DC 28, 1977, as amended at 43 FR 54927, Nov. 24, 20408. 1978; 45 FR 67320, Oct. 10, 1980; 46 FR 46796, Sept. 22, 1981; 49 FR 10108, Mar. 19, 1984; 49 FR (c) Specifications. (1) Nitrogen content 13139, Apr. 3, 1984; 50 FR 31045, July 24, 1985] of the copolymer is in the range of 16 § 177.1020 Acrylonitrile/butadiene/sty- to 18.5 percent as determined by Micro- rene co-polymer. Kjeldahl analysis. Acrylonitrile/butadiene/styrene co- (2) Residual acrylonitrile monomer polymer identified in this section may content of the finished copolymer arti- be safely used as an article or compo- cles is not more than 11 parts per mil- nent of articles intended for use with lion as determined by a gas all foods, except those containing alco- chromatographic method titled ‘‘De- hol, under conditions of use E, F, and G termination of Residual Acrylonitrile described in table 2 of § 176.170(c) of this and Styrene Monomers-Gas chapter. Chromatographic Internal Standard (a) Identity. For the purpose of this Method,’’ which is incorporated by ref- section, the acrylonitrile/butadiene/ erence. Copies are available from the styrene copolymer consists of: Center for Food Safety and Applied Nu- (1) Eighty-four to eighty-nine parts trition (HFS–200), Food and Drug Ad- by weight of a matrix polymer con- ministration, 200 C St. SW., Wash- taining 73 to 78 parts by weight of acry- ington, DC 20204, or available for in- lonitrile and 22 to 27 parts by weight of spection at the Office of the Federal styrene; and Register, 800 North Capitol Street, (2) Eleven to sixteen parts by weight NW., suite 700, Washington, DC 20408. of a grafted rubber consisting of (i) 8 to (d) Extractive limitations. (1) Total 13 parts of butadiene/styrene elastomer nonvolatile extractives not to exceed containing 72 to 77 parts by weight of
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0.0005 milligram per square inch sur- a grafted rubber consisting of (i) 16 to face area when the finished food con- 20 parts of butadiene/styrene/elastomer tact article is exposed to distilled containing 72 to 77 parts by weight of water, 3 percent acetic acid, or n- butadiene and 23 to 28 parts by weight heptane for 8 days at 120 °F. of styrene and (ii) 5 to 10 parts by (2) The finished food-contact article weight of a graft polymer having the shall yield not more than 0.0015 milli- same composition range as the matrix gram per square inch of acrylonitrile polymer. monomer when exposed to distilled (b) Adjuvants. The copolymer identi- water and 3 percent acetic acid at 150 fied in paragraph (a) of this section °F for 15 days when analyzed by a po- may contain adjuvant substances re- larographic method titled ‘‘Extracted quired in its production. Such adju- Acrylonitrile by Differential Pulse Po- vants may include substances gen- larography,’’ which is incorporated by erally recognized as safe in food, sub- reference. Copies are available from stances used in accordance with prior the Center for Food Safety and Applied sanction, substances permitted under Nutrition (HFS–200), Food and Drug applicable regulations in this part, and Administration, 200 C St. SW., Wash- the following: ington, DC 20204, or available for in- spection at the Office of the Federal Substances Limitations Register, 800 North Capitol Street, 2ÐMercaptoethanol ...... The finished copolymer shall NW., suite 700, Washington, DC 20408. contain not more than 800 (e) Acrylonitrile copolymers identi- ppm 2Ðmercaptoethanol fied in this section shall comply with acrylonitrile adduct as de- termined by a method titled the provisions of § 180.22 of this chap- ‘‘Analysis of Cycopac ter. Resin for Residual βÐ(2Ð (f) Acrylonitrile copolymers identi- Hydroxyethylmercapto) pro- fied in this section are not authorized pionitrile,’’ which is incor- porated by reference. Cop- to be used to fabricate beverage con- ies are available from the tainers. Bureau of Foods (HFSÐ 200), Food and Drug Ad- [42 FR 14572, Mar. 15, 1977, as amended at 42 ministration, 200 C St. FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, SW., Washington, DC 1982; 54 FR 24897, June 12, 1989] 20204, or available for in- spection at the Office of § 177.1030 Acrylonitrile/butadiene/sty- the Federal Register, 800 North Capitol Street, NW., rene/methyl methacrylate copoly- suite 700, Washington, DC mer. 20408. Acrylonitrile/butadiene/styrene/ methyl methacrylate copolymer iden- (c) Specifications. (1) Nitrogen content tified in this section may be safely of the copolymer is in the range of 13.0 used as an article or component of arti- to 16.0 percent as determined by Micro- cles intended for use with food identi- Kjeldahl analysis. fied in table 1 of § 176.170(c) of this (2) Residual acrylonitrile monomer chapter as Type I, II, III, IVA, IVB, V, content of the finished copolymer arti- VIB, (except bottles intended to hold cles is not more than 11 parts per mil- carbonated beverages), VIIA, VIIB, VIII lion as determined by a gas and IX, under conditions of use C, D, E, chromatographic method titled ‘‘De- F, and G described in table 2 of termination of Residual Acrylonitrile § 176.170(c) of this chapter with a high and Styrene Monomers-Gas temperature limitation of 190 °F. Chromatographic Internal Standard (a) Identity. For the purpose of this Method,’’ which is incorporated by ref- section, acrylonitrile/butadiene/sty- erence. Copies are available from the rene/methyl methacrylate copolymer Center for Food Safety and Applied Nu- consists of: (1) 73 to 79 parts by weight trition (HFS–200), Food and Drug Ad- of a matrix polymer containing 64 to 69 ministration, 200 C St. SW., Wash- parts by weight of acrylonitrile, 25 to ington, DC 20204, or available for in- 30 parts by weight of styrene and 4 to spection at the Office of the Federal 6 parts by weight of methyl methacry- Register, 800 North Capitol Street, late; and (2) 21 to 27 parts by weight of NW., suite 700, Washington, DC 20408.
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(d) Extractive limitations. (1) Total § 177.1040 Acrylonitrile/styrene copoly- nonvolatile extractives not to exceed mer. 0.0005 milligram per square inch sur- Acrylonitrile/styrene copolymers face area of the food-contact article identified in this section may be safely when exposed to distilled water, 3 per- used as a component of packaging ma- cent acetic acid, 50 percent ethanol, terials subject to the provisions of this and n-heptane for 10 days at 120 °F. (2) The finished food-contact article section. shall yield not more than 0.0025 milli- (a) Identity. For the purposes of this gram per square inch of acrylonitrile section acrylonitrile/styrene copoly- monomer when exposed to distilled mers are basic copolymers meeting the water, 3 percent acetic acid and n- specifications prescribed in paragraph heptane at 190 °F for 2 hours, cooled to (c) of this section. 120 °F (80 to 90 minutes) and main- (b) Adjuvants. (1) The copolymers tained at 120 °F for 10 days when ana- identified in paragraph (c) of this sec- lyzed by a polarographic method titled tion may contain adjuvant substances ‘‘Extracted Acrylonitrile by Differen- required in their production, with the tial Pulse Polarography,’’ which is in- exception that they shall not contain corporated by reference. Copies are mercaptans or other substances which available from the Center for Food form reversible complexes with acryl- Safety and Applied Nutrition (HFS– onitrile monomer. Permissible adju- 200), Food and Drug Administration, vants may include substances gen- 200 C St. SW., Washington, DC 20204, or erally recognized as safe in food, sub- available for inspection at the Office of stances used in accordance with prior the Federal Register, 800 North Capitol sanction, substances permitted under Street, NW., suite 700, Washington, DC applicable regulations in this part, and 20408. those authorized in paragraph (b)(2) of (e) Acrylonitrile copolymers identi- this section. fied in this section shall comply with (2) The optional adjuvants for the ac- the provisions of § 180.22 of this chap- rylonitrile/styrene copolymer identi- ter. fied in paragraphs (c) (1) and (3) of this (f) Acrylonitrile copolymers identi- section are as follows: fied in this section are not authorized to be used to fabricate beverage con- Substances Limitation tainers. Condensation polymer of toluene 0.15 pct maximum. [42 FR 14572, Mar. 15, 1977, as amended at 42 sulfonamide and formaldehyde. FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, 1982; 54 FR 24898, June 12, 1989] (c) Specifications.
Maximum re- sidual acrylo- nitrile mon- Nitrogen con- Maximum extractable fractions at Conformance with Acrylonitrile/styrene copolymers omer content tent of co- specified temperatures and times certain specifications of finished polymer article
1. Acrylonitrile/styrene copolymer 80 ppm1 ...... 17.4 to 19 Total nonvolatile extractives not to Minimum number av- consisting of the copolymer pro- pct. exceed 0.01 mg/in 2 surface erage molecular duced by polymerization of 66Ð area of the food contact article weight is 30,000.1 72 parts by weight of acrylo- when exposed to distilled water nitrile and 28Ð34 parts by weight and 3 pct acetic acid for 10 d at of styrene; for use with food of 66 °C (150 °F). Type VIÐB identified in table 1 of The extracted copolymer shall not ¤ 176.170(c) of this chapter exceed 0.001 mg/in 2 surface under conditions of use C, D, E, area of the food contact article F, G described in table 2 of when exposed to distilled water ¤ 176.170(c) of this chapter. and 3 pct acetic acid for 10 d at 66 °C (150 °F) 1.
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Maximum re- sidual acrylo- nitrile mon- Nitrogen con- Maximum extractable fractions at Conformance with Acrylonitrile/styrene copolymers omer content tent of co- specified temperatures and times certain specifications of finished polymer article
2. Acrylonitrile/styrene copolymer 50 ppm1 ...... 12.2 to 17.2 Extracted copolymer not to exceed Minimum 10 pct solu- consisting of the copolymer pro- pct. 2.0 ppm in aqueous extract or n- tion viscosity at 25 duced by polymerization of 45Ð heptane extract obtained when °C (77 °F) is 10cP.1 65 parts by weight of acrylo- 100 g sample of the basic co- nitrile and 35Ð55 parts by weigth polymer in the form of particles of styrene; for use with food of of a size that will pass through a Types, I, II, III, IV, V, VI (except U.S. Standard Sieve No. 6 and bottles), VII, VIII, and IX identi- that will be held on a U.S. fied in table 1 of ¤ 176.170(c) of Standard Sieve No. 10 is ex- this chapter under conditions B tracted with 250 mil of deionized (not to exceed 93 °C (200 °F)), water or reagent grade n- C, D, E, F, G described in table heptane at reflux temperature 2 of ¤ 176.170(c) of this chapter. for 2 h.1 3. Acrylonitrile/styrene copolymer 0.10 ppm 17.4 to 19 Total nonvolatile extractives not to Maximum carbon di- consisting of the copolymer pro- (calculated pct. exceed 0.01 mg/in 2 surface oxide permeability duced by polymerization of 66Ð on the area of the food contact article at 23 °C (73 °F) for 72 parts by weight of acrylo- basis of when exposed to distilled water the finished article nitrile and 28Ð34 parts by weight the weight and 3 pct acetic acid for 10 d at is 0.04 barrer.3 of styrene; for use with food of of the ac- 66 °C (150 °F). Types VIÐA and VIÐB identified rylonitrile The extracted copolymer shall not in table 1 of ¤ 176.170(c) of this copolymer exceed 0.001 mg/in 2 surface chapter under conditions of use resin in the area of the food contact article C, D, E, F, G described in table finished ar- when exposed to distilled water 2 of ¤ 176.170(c) of this chapter. ticles).2 and 3 pct acetic acid for 10 d at 66 °C (150 °F).1. 1 Use methods for determination of residual acrylonitrile monomer content, maximum extractable fraction, number average mo- lecular weight, and solution viscosity, titled: ‘‘Determination of Residual Acrylonitrile and Styrene Monomers-Gas Chromatographic Internal Standard Method’’; ‘‘Infrared Spectrophotometric Determination of Polymer Extracted from Barex 210 Resin Pellets’’; ‘‘Procedure for the Determination of Molecular Weights of Acrylonitrile/Styrene Copolymers,’’ and ‘‘Analytical Method for 10% Solution Viscosity of Tyril,’’ which are incorproated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ200), 200 C Street SW., Washington, DC 20204, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408. 2 As determined by the method titled ‘‘Headspace Sampling and Gas-Solid Chromatographic Determination of Residual Acrylo- nitrile in Acrylonitrile Copolyemr Solutions,’’ which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ200), 200 C Street SW., Washington, DC 20204, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408. 3 As determined on appropriately shaped test samples of the article or acrylonitrile copolymer layer in a multilayer construction by ASTM method DÐ1434Ð82, ‘‘Standard Method for Determining Gas Permeability Characteristics of Plastic Film and Sheeting,’’ which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ200), 200 C Street SW., Washington, DC 20204, and the American Society for Testing Materials, 1916 Race Street, Philadelphia, PA 19103, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408.
(d) Interim listing. Acrylonitrile co- safely used as a component of bottles polymers identified in this section intended for use with foods identified shall comply with the provisions of in table I of § 176.170(c) of this chapter § 180.22 of this chapter. as Type VI–B under conditions for use (e) Acrylonitrile copolymer identified E, F, or G described in table 2 of in this section may be used to fabricate § 176.170(c) of this chapter. beverage containers only if they com- (a) Identity. For the purpose of this ply with the specifications of item 3 in section, acrylonitrile/styrene copoly- paragraph (c) of this section. mer modified with butadiene/styrene [42 FR 14572, Mar. 15, 1977, as amended at 42 elastomer consists of a blend of: FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, (1) 82–88 parts by weight of a matrix 1982; 49 FR 36643, Sept. 19, 1984; 52 FR 33803, copolymer produced by polymerization Sept. 8, 1987] of 77–82 parts by weight of acrylonitrile and 18–23 parts of styrene; and § 177.1050 Acrylonitrile/styrene copoly- (2) 12–18 parts by weight of a grafted mer modified with butadiene/sty- rubber consisting of (i) 8–12 parts of bu- rene elastomer. tadiene/styrene elastomer containing Acrylonitrile/styrene copolymer 77–82 parts by weight of butadiene and modified with butadiene/styrene elas- 18–23 parts by weight of styrene and (ii) tomer identified in this section may be
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4–6 parts by weight of a graft copoly- ard Method,’’ which is incorporated by mer consisting of 70–77 parts by weight reference. Copies are available from of acrylonitrile and 23–30 parts by the Center for Food Safety and Applied weight of styrene. Nutrition (HFS–200), Food and Drug (b) Adjuvants. The modified copoly- Administration, 200 C St. SW., Wash- mer identified in paragraph (a) of this ington, DC 20204, or available for in- section may contain adjuvant sub- spection at the Office of the Federal stances required in its production. Register, 800 North Capitol Street, Such adjuvants may include substances NW., suite 700, Washington, DC 20408. generally recognized as safe in food, (d) Extractives limitations. The fol- substances used in accordance with lowing extractives limitations are de- prior sanction, substances permitted termined by an infrared spectrophoto- under applicable regulations in this metric method titled ‘‘Infrared part, and the following: Spectrophotometric Determination of Polymer Extracted from Borex 210 Substances Limitations Resin Pellets,’’ which is incorporated n-Dodecylmercaptan ...... The finished copolymer shall by reference. Copies are available from contain not more than 500 the Center for Food Safety and Applied parts per million (ppm) dodecylmercaptan as Nutrition (HFS–200), Food and Drug dodecylmercapto- Administration, 200 C St. SW., Wash- propionitrile as determined ington, DC 20204, or available for in- by the method titled, ‘‘De- spection at the Office of the Federal termination of β-Dodecyl- mercaptopropionitrile in Register, 800 North Capitol Street, NRÐ16 Polymer,’’ which is NW., suite 700, Washington, DC 20408, incorporated by reference. and are applicable to the modified co- Copies are available from the Center for Food Safety polymers in the form of particles of a and Applied Nutrition size that will pass through a U.S. (HFSÐ200), Food and Drug Standard Sieve No. 6 and that will be Administration, 200 C St., held on a U.S. Standard Sieve No. 10: SW., Washington, DC 20204, or available for in- (1) The extracted copolymer shall not spection at the Office of exceed 2.0 ppm in aqueous extract ob- the Federal Register, 800 tained when a 100-gram sample of co- North Capitol Street, NW., suite 700, Washington, DC polymer is extracted with 250 milli- 20408. liters of freshly distilled water at reflux temperature for 2 hours. (c) Specifications. (1) Nitrogen content (2) The extracted copolymer shall not of the modified copolymer is in the exceed 0.5 ppm in n-heptane when a 100- range of 17.7–19.8 percent. gram sample of the basic copol-ymer is (2) Intrinsic viscosity of the matrix extracted with 250 milliliters spectral copolymer in butyrolactone is not less grade n-heptane at reflux temperature than 0.5 deciliter/gram at 35 °C, as de- for 2 hours. termined by the method titled ‘‘Molec- (e) Accelerated extraction end test. The ular Weight of Matrix Copolymer by modified copolymer shall yield acrylo- Solution Viscosity,’’ which is incor- nitrile monomer not in excess of 0.4 porated by reference. Copies are avail- ppm when tested as follows: able from the Center for Food Safety (1) The modified copolymer shall be and Applied Nutrition (HFS–200), Food in the form of eight strips 1⁄2 inch by 4 and Drug Administration, 200 C St. inches by .03 inch. SW., Washington, DC 20204, or available (2) The modified copolymer strips for inspection at the Office of the Fed- shall be immersed in 225 milliliters of 3 eral Register, 800 North Capitol Street, percent acetic acid in a Pyrex glass NW., suite 700, Washington, DC 20408. pressure bottle. (3) Residual acrylonitrile monomer (3) The pyrex glass pressure bottle is content of the modified copolymer ar- then sealed and heated to 150 °F in ei- ticles is not more than 11 ppm as deter- ther a circulating air oven or a thermo- mined by a gas chromatographic meth- stat controlled bath for a period of 8 od titled ‘‘Determination of Residual days. Acrylonitrile and Styrene Monomers- (4) The Pyrex glass pressure bottle is Gas Chromatographic Internal Stand- then removed from the oven or bath
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and cooled to room temperature. A by micro-Kjeldahl analysis, shall not sample of the extracting solvent is exceed 8 percent. then withdrawn and analyzed for acry- (d) Limitations. (1) The n-alkylglutar- lonitrile monomer by a gas imide/acrylic copolymers in the fin- chromatographic method titled ‘‘Gas- ished form in which they shall contact Solid Chromatographic Procedure for food, when extracted with the solvent Determining Acrylonitrile Monomer in or solvents characterizing the type of Acrylonitrile-Containing Polymers and food and under the conditions of time Food Simulating Solvents,’’ which is and temperature described in tables 1 incorporated by reference. Copies, are and 2 of § 176.170(c) of this chapter, available from the Center for Food shall yield extractives not to exceed Safety and Applied Nutrition (HFS– the limitations of § 177.1010(b) of this 200), Food and Drug Administration, chapter, when prepared as strips, as de- 200 C St. SW., Washington, DC 20204, or scribed in § 177.1010(c)(2) of this chapter. available for inspection at the Office of (2) The n-alkylglutarimide/acrylic co- the Federal Register, 800 North Capitol polymers shall not be used as polymer Street, NW., suite 700, Washington, DC modifiers in vinyl chloride homo- or 20408. copolymers. (e) Conditions of use. The n- (f) Acrylonitrile copolymers identi- alkylglutarimide/acrylic copolymers fied in this section shall comply with are used as articles or components of the provisions of § 180.22 of this chap- articles (other than articles composed ter. of vinyl chloride homo- or copolymers) (g) Acrylonitrile copolymers identi- intended for use in contact with all fied in this section are not authorized foods except beverages containing to be used to fabricate beverage con- more than 8 percent alcohol under con- tainers. ditions of use D, E, F, and G as de- [42 FR 14572, Mar. 15, 1977, as amended at 42 scribed in table 2 of § 176.170(c) of this FR 48544, Sept. 23, 1977; 47 FR 11841, Mar. 19, chapter. 1982; 47 FR 16775, Apr. 20, 1982; 54 FR 24898, [54 FR 20382, May 11, 1989, as amended at 58 June 12, 1989] FR 17098, Apr. 1, 1993]
§ 177.1060 n-Alkylglutarimide/acrylic § 177.1200 Cellophane. copolymers. Cellophane may be safely used for n-Alkylglutarimide/acrylic copoly- packaging food in accordance with the mers identified in this section may be following prescribed conditions: safely used as articles or components (a) Cellophane consists of a base of articles intended for use in contact sheet made from regenerated cellulose with food subject to provisions of this to which have been added certain op- section and part 174 of this chapter. tional substances of a grade of purity (a) Identity. For the purpose of this suitable for use in food packaging as section, n-alkylglutarimide/acrylic co- constituents of the base sheet or as polymers are copolymers obtained by coatings applied to impart desired reaction of substances permitted by technological properties. § 177.1010(a) (1), (2), and (3) with the fol- (b) Subject to any limitations pre- lowing substance: Monomethylamine scribed in this part, the optional sub- (CAS Reg. No. 74–89–5), to form n- stances used in the base sheet and methylglutarimide/acrylic copolymers. coating may include: (b) Adjuvants. The copolymers identi- (1) Substances generally recognized fied in paragraph (a) of this section as safe in food. may contain adjuvant substances re- (2) Substances for which prior ap- quired in their production. The op- proval or sanctions permit their use in tional adjuvant substances required in cellophane, under conditions specified the production of the basic polymer in such sanctions and substances listed may include substances permitted for in § 181.22 of this chapter. such use by applicable regulations, as (3) Substances that by any regulation set forth in part 174 of this chapter. promulgated under section 409 of the (c) Specifications. Maximum nitrogen act may be safely used as components content of the copolymer determined of cellophane.
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(4) Substances named in this section (c) List of substances: and further identified as required.
Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
Acrylonitrile-butadiene copolymer resins ...... As the basic polymer. Acrylonitrile-butadiene-styrene copolymer resins ...... Do. Acrylonitrile-styrene copolymer resins ...... Do. Acrylonitrile-vinyl chloride copolymer resins ...... Do. N-Acyl sarcosines where the acyl group is lauroyl or stearoyl ... For use only as release agents in coatings at levels not to ex- ceed a total of 0.3 percent by weight of the finished pack- aging cellophane. Alkyl ketene dimers identified in ¤ 176.120 of this chapter. Aluminum hydroxide. Aluminum silicate. Ammonium persulfate. Ammonium sulfate. Behenamide. Butadiene-styrene copolymer ...... As the basic polymer. 1,3-Butanediol. n-Butyl acetate ...... 0.1 percent. n-Butyl alcohol ...... Do. Calcium ethyl acetoacetate. Calcium stearoyl-2-lactylate identified in ¤ 172.844 of this chap- Not to exceed 0.5 percent weight of cellophane. ter. Carboxymethyl hydroxyethylcellulose polymer. Castor oil, hydrogenated. Castor oil phthalate with adipic acid and fumaric acid-diethyl- As the basic polymer. ene glycol polyester. Castor oil phthalate, hydrogenated ...... Alone or in combination with other phthalates where total phthalates do not exceed 5 percent. Castor oil, sulfonated, sodium salt. Cellulose acetate butyrate. Cellulose acetate propionate. Cetyl alcohol. Clay, natural. Coconut oil fatty acid (C12ÐC18) diethanolamide, coconut oil For use only as an adjuvant employed during the processing of fatty acid (C12ÐC18) diethanolamine soap, and cellulose pulp used in the manufacture of cellophane base diethanolamine mixture having total alkali (calculated as po- sheet. tassium hydroxide) of 16Ð18% and having an acid number of 25Ð35. Copal resin, heat processed ...... As basic resin. Damar resin. Defoaming agents identified in ¤ 176.200 of this chapter. Dialkyl ketones where the alkyl groups are lauryl or stearyl ...... Not to exceed a total of 0.35 percent. Dibutylphthalate ...... Alone or in combination with other phthalates where total phthalates do not exceed 5 percent. Dicyclohexyl phthalate ...... Do. Diethylene glycol ester of the adduct of terpene and maleic an- hydride. Di(2-ethylhexyl) adipate. Di(2-ethylhexyl) phthalate...... Alone or in combination with other phthalates where total phthalates do not exceed 5 percent. Diisobutyl phthalate ...... Do. Dimethylcyclohexyl phthalate ...... Do. Dimethyldialkyl (C8ÐC18) ammonium chloride ...... 0.005 percent for use only as a flocculant for slip agents. Di-n-ocyltin bis (2-ethylhexyl maleate) ...... For use only as a stabilizer at a level not to exceed 0.55 per- cent by weight of the coating solids in vinylidene chloride co- polymer waterproof coatings prepared from vinylidene chlo- ride copolymers identified in this paragraph, provided that such vinylidene chloride copolymers contain not less than 90 percent by weight of polymer units derived from vinylidene chloride. N,N′-Dioleoyethylenediamine, N,N′-dilinoleoylethylene-diamine 0.5 percent. and N-oleoyl-N′linoleoylethylene-diamine mixture produced when tall oil fatty acids are made to react with ethylene- diamine such that the finished mixture has a melting point of 212°Ð228 °F., as determined by ASTM method D127Ð60 (‘‘Standard Method of Test for Melting Point of Petrolatum and Microcrystalline Wax’’ (Revised 1960), which is incor- porated by reference; copies are available from University Microfilms International, 300 N. Zeeb Rd., Ann Arbor, MI 48106, or available for inspection at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Wash- ington, DC 20408), and an acid value of 10 maximum.
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
N,N′-Dioleoylethylenediamine (N,N′-ethylenebisoleamide). Disodium EDTA. Distearic acid ester of di(hydroxyethyl) diethylenetriamine 0.06 percent. monoacetate. N,N′-Distearoylethylenediamine (N,N′-ethylenebis stearamide). Epoxidized polybutadiene ...... For use only as a primer subcoat to anchor surface coatings to the base sheet. Erucamide. Ethyl acetate. Ethylene-vinyl acetate copolymers complying with ¤ 177.1350. 2-Ethylhexyl alcohol ...... 0.1 percent for use only as lubricant. Fatty acids derived from animal and vegetable fats and oils, and the following salts of such acids, single or mixed: Alu- minum, ammonium, calcium, magnesium, potassium, sodium. Ferrous ammonium sulfate. Fumaric acid. Glycerin-maleic anhydride ...... As the basic polymer. Glycerol diacetate. Glycerol monoacetate. Hydroxyethyl cellulose, water-insoluble. Hydroxypropyl cellulose identified in ¤ 172.870 of this chapter. Isopropyl acetate ...... Residue limit 0.1 percent Isopropyl alcohol ...... Do. Itaconic acid. Lanolin. Lauryl alcohol. Lauryl sulfate salts: ammonium, magnesium, potassium, so- dium. Maleic acid ...... 1 percent. Maleic acid adduct of butadienestyrene copolymer. Melamine formaldehyde ...... As the basic polymer. Melamine-formaldehyde modified with one or more of the fol- As the basic polymer, and used as a resin to anchor coatings lowing: Butyl alcohol, diaminopropane, diethylenetriamine, to substrate. ethyl alcohol, guanidine, imino-bis-butylamine, imino-bis-eth- ylamine, imino-bis-propylamine, methyl alcohol, polyamines made by reacting ethylenediamine or trimethylenediamine with dichloroethane or dichloropropane, sulfanilic acid, tetraethylenepentamine, triethanolamine, triethylenetetra- mine. Methyl ethyl ketone ...... Residue limit 0.1 percent Methyl hydrogen siloxane ...... 0.1 percent as the basic polymer. α-Methylstyrene-vinyltoluene copolymer resins (molar ratio 1 α- methylstyrene to 3 vinyltoluene). Mineral oil, white. Mono- and bis-(octadecyldiethylene oxide) phosphates (CAS For use only as a release agent at a level not to exceed 0.6 Reg. No. 62362Ð49Ð6). percent by weight of coatings for cellophane. Naphthalenesulfonic acid-formaldehyde condensate, sodium 0.1 percent, for use only as an emulsifier. salt. Nitrocellulose, 10.9 percentÐ12.2 percent nitrogen. Nylon resins complying with ¤ 177.1500. n-Octyl alcohol ...... For use only as a defoaming agent in the manufacture of cello- phane base sheet. Olefin copolymers complying with ¤ 177.1520. Oleic acid reacted with N-alkyl trimethylenediamine (alkyl C16 to C18). Oleic acid, sulfonated, sodium salt. Oleyl palmitamide. N,N′-Oleoyl-stearylethylenediamine (N-(2-stearoyl- aminoethyl)oleamide). Paraffin, synthetic, complying with ¤ 175.250 of this chapter. Pentaerythritol tetrastearate ...... 0.1 percent. Polyamide resins derived from dimerized vegetable oil acids For use only in cellophane coatings that contact food at tem- (containing not more than 20 percent of monomer acids) and peratures not to exceed room temperature. ethylenediamine as the basic resin. Polyamide resins having a maximum acid value of 5 and a As the basic resin, for use only in coatings that contact food at maximum amine value of 8.5 derived from dimerized vege- temperatures not to exceed room temperature provided that table oil acids (containing not more than 10 percent mon- the concentration of the polyamido resins in the finished omer acids), ethylenediamine, and 4,4-bis(4- food-contact coating does not exceed 5 milligrams per hydroxyphenyl)pentanoic acid (in an amount not to exceed square inch of food-contact surface. 10 percent by weight of said polyamide resins). Polybutadiene resin (molecular weight range 2,000Ð10,200; For use only as an adjuvant in vinylidene chloride copolymer bromine number range 210Ð320). coatings. Polycarbonate resins complying with ¤ 177.1580.
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
Polyester resin formed by the reaction of the methyl ester of rosin, phthalic anhydride, maleic anhydride, and ethylene glycol, such that the polyester resin has an acid number of 4 to 11, a drop-softening point of 70 °CÐ92 °C, and a color of K or paler. Polyethylene. Polyethyleneaminostearamide ethyl sulfate produced when ste- 0.1 percent. aric acid is made to react with equal parts of diethylenetriamine and triethylenetetramine and the reaction product is quaternized with diethyl sulfate. Polyethylene glycol (400) monolaurate. Polyethylene glycol (600) monolaurate. Polyethylene glycol (400) monooleate. Polyethylene glycol (600) monooleate. Polyethylene glycol (400) monostearate. Polyethylene glycol (600) monostearate. Polyethylene, oxidized: complying with the identity prescribed in ¤ 177.1620(a). Polyethylenimine ...... As the basic polymer, for use as a resin to anchor coatings to the substrate and for use as an impregnant in the food-con- tact surface of regenerated cellulose sheet in an amount not to exceed that required to improve heat-sealable bonding between coated and uncoated sides of cellophane. Polyisobutylene complying with ¤ 177.1420. Polyoxypropylene-polyoxyethylene block polymers (molecular For use as an adjuvant employed during the processing of cel- weight 1,900Ð9,000). lulose pulp used in the manufacture of cellophane base sheet. Polypropylene complying with ¤ 177.1520. Polystyrene ...... As the basic polymer. Polyvinyl acetate ...... Do. Polyvinyl alcohol (minimum viscosity of 4 percent aqueous so- lution at 20 °C of 4 centipoises). Polyvinyl chloride ...... As the basic polymer. Polyvinyl stearate ...... Do. n-Propyl acetate ...... Residue limit 0.1 percent. n-Propyl alcohol ...... Do. Rapeseed oil, blown. Rosins and rosin derivatives as provided in ¤ 178.3870 of this chapter. Rubber, natural (natural latex solids). Silica. Silicic acid. Sodium m-bisulfite. Sodium dioctyl sulfosuccinate. Sodium dodecylbenzenesulfonate. Sodium lauroyl sarcosinate ...... 0.35 percent; for use only in vinylidene chloride copolymer coatings. Sodium oleyl sulfate-sodium cetyl sulfate mixture ...... For use only as an emulsifier for coatings; limit 0.005 percent where coating is applied to one side only and 0.01 percent where coating is applied to both sides. Sodium silicate. Sodium stearoyl-2-lactylate identified in ¤ 172.846 of this chap- Not to exceed 0.5 percent weight of cellophane. ter. Sodium sulfate. Sodium sulfite. Spermaceti wax. Stannous oleate. 2-Stearamido-ethyl stearate. Stearyl alcohol. Styrene-maleic anhydride resins ...... As the basic polymer. Terpene resins identified in ¤ 172.615 of this chapter. Tetrahydrofuran ...... Residue limit of 0.1 percent. Titanium dioxide. Toluene ...... Residue limit of 0.1 percent. Toluene sulfonamide formaldehyde ...... 0.6 percent as the basic polymer. Triethylene glycol. Triethylene glycol diacetate, prepared from triethylene glycol containing not more than 0.1 percent of diethylene glycol. 2,2,4-Trimethyl-1,3 pentanediol diisobutyrate ...... For use only in cellophane coatings and limited to use at a level not to exceed 10 percent by weight of the coating sol- ids except when used as provided in ¤ 178.3740 of this chapter Urea (carbamide).
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
Urea formaldehyde ...... As the basic polymer. Urea formaldehyde modified with methanol, ethanol, butanol As the basic polymer, and used as a resin to anchor coatings diethylenetriamine, triethylenetetramine, tetraethylenepenta- to the substrate. mine, guanidine, sodium sulfite, sulfanilic acid, imino-bis-eth- ylamine, imino-bis-propylamine, imino-bis-butylamine, diaminopropane, diaminobutane, aminomethylsulfonic acid, polyamines made by reacting ethylenediamine or trimethylenediamine with dichlorethane or dichloropropane. Vinyl acetate-vinyl chloride copolymer resins ...... As the basic polymer. Vinyl acetate-vinyl chloride-maleic acid copolymer resins ...... Do. Vinylidene chloride copolymerized with one or more of the fol- Do. lowing: Acrylic acid, acrylonitrile, butyl acrylate, butyl meth- acrylate, ethyl acrylate, 2-ethylhexyl acrylate, 2-ethylhexyl methacrylate, ethyl methacrylate, itaconic acid, methacrylic acid, methyl acrylate, methyl methacrylate, propyl acrylate, propyl methacrylate, vinyl chloride. Vinylidene chloride-methacrylate decyloctyl copolymer ...... Do. Wax, petroleum, complying with ¤ 178.3710 of this chapter.
(d) Any optional component listed in stances identified in § 175.300(b) of this this section covered by a specific food chapter, with the exception of para- additive regulation must meet any graph (b)(3) (v), (xxxi), and (xxxii) of specifications in that regulation. that section, and from other optional (e) Acrylonitrile copolymers identi- substances, including the following: fied in this section shall comply with (1) Substances generally recognized the provisions of § 180.22 of this chap- as safe in food. ter. (2) Substances used in accordance [42 FR 14572, Mar. 15, 1977, as amended at 47 with the provisions of a prior sanction FR 11842, Mar. 19, 1982; 64 FR 57978, Oct. 28, or approval within the meaning of sec- 1999] tion 201(s) of the act. (3) Substances that are the subject of § 177.1210 Closures with sealing gas- kets for food containers. regulations in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter and used in Closures with sealing gaskets may be accordance with the conditions pre- safely used on containers intended for scribed. use in producing, manufacturing, pack- ing, processing, preparing, treating, (4) Substances identified in para- packaging, transporting, or holding graph (b)(5) of this section, used in food in accordance with the following amounts not to exceed those required prescribed conditions: to accomplish the intended physical or (a) Closures for food containers are technical effect and in conformance manufactured from substances gen- with any limitation provided; and fur- erally recognized as safe for contact ther provided that any substance em- with food; substances that are subject ployed in the production of closure- to the provisions of prior sanctions; sealing gasket compositions that is the substances authorized by regulations subject of a regulation in parts 174, 175, in parts 174, 175, 176, 177, 178 and § 179.45 176, 177, 178 and § 179.45 of this chapter of this chapter; and closure-sealing conforms with the identity or speci- gaskets, as further prescribed in this fications prescribed. section. (5) Substances that may be employed (b) Closure-sealing gaskets and over- in the manufacture of closure-sealing all discs are formulated from sub- gaskets include:
TABLE 1
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
Arachidy-l-behenyl amide (C20ÐC22fatty acid amides) ...... 5 percent. Azodicarbonamide ...... 1. 2 percent.
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TABLE 1—Continued
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
2. 5 percent; for use only in the manufacture of polyethylene complying with item 2.1 in ¤ 177.1520(c) of this chapter. Balata rubber. Benzyl alcohol ...... 1 percent. Brominated isobutylene-isoprene copolymers, produced when isobutylene-isoprene copolymers complying with ¤ 177.1420(a)(2) are modified by bromination with not more than 2.3 weight-percent of bromine and having a Mooney Viscosity (ML 1+8 (125 °C)) of 27 or higher. The viscosity is determined by the American Society for Testing and Mate- rials (ASTM) method D 1646Ð81, ‘‘Standard Test Method for Rubber—Viscosity and Vulcanization Characteristics (Moon- ey Viscometer),’’ which is incorporated by reference in ac- cordance with 5 U.S.C. 522(a) and 1 CFR part 51. Copies are available from the Association of Official Analytical Chemists International, 481 North Frederick Ave., Suite 500, Gaithersburg, MD 20877-2504 and the Center for Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Ad- ministration, 200 C St. SW., Washington, DC 20204, or available for inspection at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC. 1,3-Butanediol. Calcium tin stearate ...... 2 percent. Calcium zinc stearate ...... Do. Carbon, activated ...... 1 percent. Castor oil, hydrogenated ...... 2 percent. Chlorinated isobutylene-isoprene copolymers complying with ¤ 177.1420. Coco amide (coconut oil fatty acids amides) ...... 2 percent. Cork (cleaned, granulated). Diebenzamide phenyl disulfide ...... 1 percent; for use only in vulcanized natural or synthetic rubber gasket compositions. Di(C7, C9-alkyl) adipate ...... Complying with ¤ 178.3740 of this chapter; except that, there is no limitation on polymer thickness. Di-2-ethylhexyl adipate. Di-2-ethylhexyl sebacate ...... 2 percent. Di-2-ethylhexyl terephthalate (CAS Reg. No. 006422Ð86Ð2). .... For use as a plasticizer at levels not exceeding 75 parts per hundred by weight of permitted vinyl chloride homo- and/or copolymer resins used in contact with food of Types I, II, IVÐ B, VIÐA, VIÐB, VIÐC (up to 15 percent alcohol by volume), VIIÐB, and VIII described in ¤ 176.170(c) of this chapter, table 1, and under conditions of use A through H described in ¤ 176. 170 (c) of this chapter, table 2. Dihexyl ester of sodium sulfosuccinate ...... 1 percent. Diisodecyl phthalate ...... No limitation on amount used but for use only in closure-seal- ing gasket compositions used in contact with non-fatty foods containing no more than 8 percent of alcohol. Di-β-naphthyl-p-phenylenediamine ...... 1 percent. Dipentamethylenethiurametetrasulfide ...... 0.4 percent; for use only in vulcanized natural or synthetic rub- ber gasket compositions. Eicosane (technical grade) (water-white mixture of predomi- nantly straight-chain paraffin hydrocarbons averaging 20 car- bon atoms per molecule). Epoxidized linseed oil. Epoxidized linseed oil modified with trimellitic anhydride. Epoxidized safflower oil. Epoxidized safflower oil modified with trimellitic anhydride. Epoxidized soybean oil modified with trimellitic anhydride. Erucylamide ...... 5 percent. Ethylene-propylene copolymer. Ethylene-propylene modified copolymer elastomers produced when ethylene and propylene are copolymerized with 5- methylene-2-norbornene and/or 5-ethylidine-2-norbornene. The finished copolymer elastomers so produced shall con- tain not more than 5 weight-percent of total polymer units derived from 5-methylene-2-norbornene and/or 5-ethylidine- 2-norbornene, and shall have a minimum viscosity average molecular weight of 120,000 as determined by the method described in ¤ 177.1520(d)(5), and a minimum Mooney vis- cosity of 35 as determined by the method described in ¤ 177.1520(d)(6).
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TABLE 1—Continued
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
Ethylene-vinyl acetate copolymer. Glyceryl mono-12-hydroxystearate (hydrogenated glyceryl 2 percent. ricinoleate). Gutta-percha. Hexamethylenetetramine ...... 1 percent. Hexylene glycol ...... 0.5 percent. Isobutylene-isoprene copolymers complying with ¤ 177.1420. Maleic anhydride-polyethylene copolymer ...... 5 percent. Maleic anhydride-styrene copolymer ...... Do. 2,2′-Methylenebis[6-(1-methylcylcohexyl)-p-cresol] ...... 1 percent. Mixed octylated diphenylamine (CAS Reg. No. 68411Ð46Ð1) ... 0.1 percent in isobutylene-isoprene and chlorinated isobutylene-isoprene copolymers complying with ¤ 177.1420, and brominated isobutylene-isoprene copolymers complying with this section. Napthalene sulfonic acid-formaldehyde condensate, sodium 0.2 percent. salt. Natural rubber (crepe, latex, mechanical dispersions). α-cis-9-Octadecenyl-omega-hydroxypoly (oxyethylene); the 0.5 percent. octadecenyl group is derived from oleyl alcohol and the poly (oxyethylene) content averages 20 moles. Oleyl alcohol ...... 1 percent. 4,4′-Oxybis (benzene sulfonyl hydrazide) ...... 0.5 percent. Paraformaldehyde ...... 1 percent. Polybutadiene. Poly-p-dinitroso benzene (activator for butyl rubber) ...... 1 percent; for use only in vulcanized natural or synthetic rubber gasket compositions. Polyethylene glycol 400 esters of fatty acids derived from ani- 1 percent. mal and vegetable fats and oils. Polyisobutylene complying with ¤ 177.1420. Polyoxypropylene-polyoxyethylene condensate, average mol. 0.05 percent. wt. 2750Ð3000. Polyurethane resins manufactured from diphenylmethane For use only: diisocyanate, 1,4-butanediol, and adipic acid (CAS Reg. No. No limitation on amount used, but for use only in closure 26375Ð23Ð5).. gasket compositions used in contact with food types VIÐA and VIÐC (up to 15 percent alcohol) under conditions of use D, E, F, and G, as described in ¤ 176.170(c) of this chapter, tables 1 and 2, respectively. Potassium benzoate ...... 1 percent. Potassium perchlorate ...... Do. Potassium propionate ...... 2 percent. Potassium and sodium persulfate ...... 1 percent. Resorcinol ...... 0.24 percent; for use only as a reactive adjuvant substance employed in the production of gelatin-bonded cord composi- tions for use in lining crown closures. The gelatin so used shall be technical grade or better. Rosins and rosin derivatives as defined in ¤ 175.300(b)(3)(v) of this chapter for use only in resinous and polymeric coatings on metal substrates; for all other uses as defined in ¤ 178.3870 of this chapter. Sodium cetyl sulfate ...... 1 percent. Sodium decylbenzenesulfonate ...... Do. Sodium decyl sulfate ...... Do. Sodium formaldehyde sulfoxylate ...... 0.05 percent. Sodium lauryl sulfate ...... 1 percent. Sodium lignin sulfonate ...... 0.2 percent. Sodium myristyl sulfate (sodium tetradecyl sulfate) ...... 0.6 percent. Sodium nitrite ...... 0.2 percent; for use only in annular ring gaskets applied in aqueous dispersions to closures for containers having a ca- pacity of not less than 5 gallons. Sodium o-phenylphenate ...... 0.05 percent. Sodium polyacrylate ...... 5 percent. Sodium and potassium pentachlorophenate ...... 0.05 percent. Sodium salt of trisopropyl napthalenesulfonic acid ...... 0.2 percent. Sodium tridecylsulfate ...... 0.6 percent. Stearic acid amide ...... 5 percent. Sulfur ...... For use only as a vulcanizing agent in vulcanized natural or synthetic rubber gasket compositions at a level not to ex- ceed 4 percent by weight of the elastomer content of the rubber gasket composition. Tallow, sulfated ...... 1 percent. Tin-zinc stearate ...... 2 percent.
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TABLE 1—Continued
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
Tri(mixed mono- and dinonylphenyl) phosphite ...... 1 percent. Vinyl chloride-vinyl stearate copolymer. Zinc dibutyldithiocarbamate ...... 0.8 percent; for use only in vulcanized natural or synthetic rub- ber gasket compositions.
TABLE 2—MAXIMUM EXTRACTIVES TOLERANCES cork, or glass that forms a part of the [In parts per million] food-contact surface of the assembly, when extracted on a suitable glass con- Chloro- Chloro- Chloro- tainer with a solvent or solvents char- form form form Type of closure-sealing gas- fraction fraction fraction acterizing the type of foods, and under ket composition of water of of alco- conditions of time and temperature extrac- heptane hol ex- tives extrac- tractives characterizing the conditions of its use tives as determined from tables 3 and 4 shall 1. Plasticized polymers, in- yield net chloroform-soluble extrac- cluding unvulcanized or tives (corrected for zinc as zinc oleate) vulcanized or otherwise not to exceed the tolerances specified cured natural and syn- thetic rubber formed in in table 2, calculated on the basis of place as overall discs or the water capacity of the container on annular rings from a hot which the closure is to be used. Employ melt, solution, plastisol, organisol, mechanical dis- the analytical method described in persion, or latex ...... 50 500 50 § 175.300 of this chapter, adapting the 2. Preformed overall discs procedural details to make the method or annular rings of plasti- cized polymers, including applicable to closures; such as, for ex- unvulcanized natural or ample, placing the closed glass con- synthetic rubber ...... 50 250 50 tainer on its side to assure contact of 3. Preformed overall discs the closure’s food-contacting surface or annular rings of vulcan- ized plasticized polymers, with the solvent. including natural or syn- thetic rubber ...... 50 50 50 TABLE 3—TYPES OF FOOD 4. Preformed overall discs I. Nonacid (pH above 5.0), aqueous products; may contain or annular rings of poly- salt or sugar or both, and including oil-in-water emulsions meric or resinous-coated of low- or high-fat content. paper, paperboard, plas- II. Acidic (pH 5.0 or below), aqueous products; may contain tic, or metal foil substrates 50 250 50 5. Closures with sealing salt or sugar or both, and including oil-in-water emulsions gaskets or sealing com- of low- or high-fat content. positions as described in III. Aqueous, acid or nonacid products containing free oil or 1, 2, 3, and 4, and includ- fat; may contain salt, and including water-in-oil emulsions ing paper, paperboard, of low- or high-fat content. and glassine used for dry IV. Dairy products and modifications: foods only ...... (1 )(1 )(1 ) A. Water-in-oil emulsions, high- or low-fat. B. Oil-in-water emulsions, high- or low-fat. 1 Extractability tests not applicable. V. Low-moisture fats and oils. (c) The closure assembly to include VI. Beverages: the sealing gasket or sealing com- A. Containing alcohol. B. Nonalcoholic. pound, together with any polymeric or VII. Bakery products. resinous coating, film, foil, natural VIII. Dry solids (no end-test required).
TABLE 4—TEST PROCEDURES WITH TIME-TEMPERATURE CONDITIONS FOR DETERMINING AMOUNT OF EXTRACTIVES FROM CLOSURE-SEALING GASKETS, USING SOLVENTS SIMULATING TYPES OF FOODS AND BEVERAGES
Types of food (see Extractant Conditions of use table 3) Water 2 Heptane 12 8 percent alcohol 2
A. High temperature heat-sterilized I, IVÐB ...... 250 °F, 2 hr ...... (e.g., over 212 °F). III, IVÐA, VII ...... do ...... 150 °F, 2 hr. B. Boiling water-sterilized ...... II ...... 212 °F, 30 min ...... III, VII ...... do ...... 120 °F, 30 min.
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TABLE 4—TEST PROCEDURES WITH TIME-TEMPERATURE CONDITIONS FOR DETERMINING AMOUNT OF EXTRACTIVES FROM CLOSURE-SEALING GASKETS, USING SOLVENTS SIMULATING TYPES OF FOODS AND BEVERAGES—Continued
Types of food (see Extractant Conditions of use table 3) Water 2 Heptane 12 8 percent alcohol 2
C. Hot filled or pasteurized above 150 II, IVÐB ...... Fill boiling, cool to . °F. III, IVÐA ...... 100 °F. 120 °F, 15 min. V ...... do ...... do. D. Hot filled or pasteurized below 150 II, IVÐB, VIÐB ...... 150 °F, 2 hr ...... °F. III, IVÐA ...... do ...... 100 °F, 30 min. 150 °F, 2 hr V ...... do ...... VIÐA ...... E. Temperature filled and stored (no II, IVÐB, VIÐB ...... 120 °F, 24 hr ...... thermal treatment in the container). III, IVÐA ...... do ...... 70 °F, 30 min. 120 °F, 24 hr. V ...... do ...... VIÐA ...... F. Refrigerated storage (no thermal I, II, III, IVÐA, IVÐB, 70 °F, 48 hr ...... 70 °F, 30 min ...... treatment). VIÐB, VII. 70 °F, 48 hr. VIÐA ...... G. Frozen storage (no thermal treat- I, II, III, IVÐB, VII ... 70 °F, 24 hr ...... ment in the container). 1 Heptane extractant not applicable to closure-sealing gaskets overcoated with wax. 2 Time and temperature. [42 FR 14572, Mar. 15, 1977; 42 FR 56728, Oct. 28, 1977, as amended at 47 FR 22090, May 21, 1982; 49 FR 5748, Feb. 15, 1984; 55 FR 34555, Aug. 23, 1990; 61 FR 14480, Apr. 2, 1996; 65 FR 26745, May 9, 2000; 65 FR 52908, Aug. 31, 2000]
§ 177.1211 Cross-linked polyacrylate nized as safe in food, and substances copolymers. used in accordance with a prior sanc- Cross-linked polyacrylate copoly- tion or approval. mers identified in paragraph (a) of this (c) Extractives limitations. The copoly- section may be safely used as articles mers identified in paragraph (a) of this or components of articles intended for section, in the finished form in which use in contact with food in accordance they will contact food, must yield low with the following prescribed condi- molecular weight (less than 1,000 Dal- tions: tons) extractives of no more than 0.15 (a) Identity. For the purpose of this percent by weight of the total polymer section, the cross-linked polyacrylate when extracted with 0.2 percent by copolymers consist of: weight of aqueous sodium chloride so- (1) The grafted copolymer of cross- lution at 20 °C for 24 hours. The low linked sodium polyacrylate identified molecular weight extractives shall be as 2-propenoic acid, polymers with N,N- determined using size exclusion chro- di-2-propenyl-2-propen-1-amine and matography or an equivalent method. hydrolyzed polyvinyl acetate, sodium When conducting the extraction test, salts, graft (CAS Reg. No. 166164–74–5); the copolymer, with no other absorp- or tive media, shall be confined either in (2) 2-propenoic acid, polymer with 2- a finished absorbent pad or in any suit- ethyl-2-(((1-oxo-2-pro- able flexible porous article, (such as a penyl)oxy)methyl)-1,3-propanediyl di-2- ‘‘tea bag’’ or infuser), under an applied propenoate and sodium 2-propenoate pressure of 0.15 pounds per square inch (CAS Reg. No. 76774–25–9). (for example, a 4x6 inch square pad is (b) Adjuvants. The copolymers identi- subjected to a 1.6 kilograms applied fied in paragraph (a) of this section mass). The solvent used shall be at may contain optional adjuvant sub- least 60 milliliters aqueous sodium stances required in the production of chloride solution per gram of copoly- such copolymers. The optional adju- mer. vant substances may include sub- (d) Conditions of use. The copolymers stances permitted for such use by regu- identified in paragraph (a)(1) of this lations in parts 170 through 179 of this section are limited to use as a fluid ab- chapter, substances generally recog- sorbent in food-contact materials used
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in the packaging of frozen or refrig- surfaces, subject to the provisions of erated poultry. The copolymers identi- such regulation. fied in paragraph (a)(2) of this section (e) The copolymer conforms with the are limited to use as a fluid absorbent following specifications: in food-contact materials used in the (1) The copolymer, when extracted packaging of frozen or refrigerated with distilled water at reflux tempera- meat and poultry. ture for 2 hours, yields total extrac- tives not to exceed 0.05 percent. [64 FR 28098, May 25, 1999, as amended at 65 (2) The copolymer, when extracted FR 16817, Mar. 30, 2000] with ethyl acetate at reflux tempera- ture for 2 hours, yields total extrac- § 177.1240 1,4-Cyclohexylene dimethylene terephthalate and 1,4- tives not to exceed 0.7 percent. cyclohexylene dimethylene (3) The copolymer, when extracted isophthalate copolymer. with n-hexane at reflux temperature for 2 hours, yields total extractives not Copolymer of 1,4-cyclohexylene to exceed 0.05 percent. dimethylene terephthalate and 1,4- cyclohexylene dimethylene isophtha- [42 FR 14572, Mar. 15, 1977; 49 FR 5748, Feb. 15, late may be safely used as an article or 1984, as amended at 55 FR 34555, Aug. 23, 1990] component of articles used in pro- ducing, manufacturing, packing, proc- § 177.1310 Ethylene-acrylic acid co- polymers. essing, preparing, treating, packaging, transporting, or holding food, subject The ethylene-acrylic acid copolymers to the provisions of this section: identified in paragraph (a) of this sec- (a) The copolymer is a basic poly- tion may be safely used as components ester produced by the catalytic con- of articles intended for use in contact densation of dimethyl terephthalate with food subject to the provisions of and dimethyl isophthalate with 1,4- this section. cyclohexanedimethanol, to which may (a) The ethylene-acrylic acid copoly- have been added certain optional sub- mers consist of basic copolymers pro- stances required in its production or duced by the copolymerization of added to impart desired physical and ethylene and acrylic acid such that the technical properties. finished basic copolymers contain no more than: (b) The quantity of any optional sub- (1) 10 weight-percent of total polymer stance employed in the production of units derived from acrylic acid when the copolymer does not exceed the used in accordance with paragraph (b) amount reasonably required to accom- of this section; and plish the intended physical or technical (2) 25 weight-percent of total polymer effect or any limitation further pro- units derived from acrylic acid when vided. used in accordance with paragraph (c) (c) Any substance employed in the of this section. production of the copolymer that is the (b) The finished food-contact articles subject of a regulation in parts 174, 175, made with no more than 10 percent 176, 177, 178 and § 179.45 of this chapter total polymer units derived from acryl- conforms with any specification in ic acid, when extracted with the sol- such regulation. vent or solvents characterizing the (d) Substances employed in the pro- type of food and under the conditions duction of the copolymer include: of its intended use as determined from (1) Substances generally recognized tables 1 and 2 of § 176.170(c) of this chap- as safe in food. ter, yield net acidified chloroform-solu- (2) Substances subject to prior sanc- ble extractives not to exceed 0.5 milli- tion or approval for use in the copoly- gram per square inch of food-contact mer and used in accordance with such surface when tested by the methods sanction or approval. prescribed in § 177.1330(e)(1), (3)(i) (3) Substances which by regulation in through (iv), (4), (5), and (6), except parts 174, 175, 176, 177, 178 and § 179.45 of that this chapter may be safely used as (1) The total residue method using 3 components of resinous or polymeric percent acetic acid, as prescribed in coatings and film used as food-contact § 177.1330(e)(6)(i)(a), does not apply, and
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(2) The net acidified chloroform-solu- the food-contact or interior core layer ble extractives from paper and paper- of multilaminate food-contact articles. board complying with § 176.170 of this (2) The polymers may be safely used chapter may be corrected for wax, pet- as food-contact materials at tempera- rolatum, and mineral oil as provided in tures not to exceed 121 °C (250 °F). § 176.170(d)(5)(iii)(b) of this chapter. (c) Specifications. (1) Food-contact If the finished food-contact article is layers formed from the basic copoly- itself the subject of a regulation in mer identified in paragraph (a) of this parts 174, 175, 176, 177, 178, and § 179.45 of section shall be limited to a thickness this chapter, it shall also comply with of not more than 0.01 centimeter (0.004 any specifications and limitations pre- inch). scribed for it by that regulation. (2) The copolymers identified in para- (c) The finished food-contact layer graph (a) of this section shall have a made with basic copolymers containing melt index not greater than 500 as de- more than 10 weight-percent but no termined by ASTM method D1238–82, more than 25 weight-percent of total condition E ‘‘Standard Test Method for polymer units derived from acrylic Flow Rates of Thermoplastics by Ex- acid and with a maximum thickness of trusion Plastometer,’’ which is incor- 0.0025 inch (2.5 mils) may be used in porated by reference in accordance contact with food types I, II, IVB, VIA, with 5 U.S.C. 552(a) and 1 CFR part 51. VIB, VIIB, and VIII identified in table Copies may be obtained from the Amer- 1 of § 176.170(c) of the chapter under ican Society for Testing Materials, 1916 conditions of use B through H as de- Race St., Philadelphia, PA 19103, or scribed in table 2 of § 176.170(c) of this may be examined at the Center for chapter, and in contact with food types Food Safety and Applied Nutrition III, IVA, V, VIIA, and IX identified in (HFS–200), Food and Drug Administra- table 1 of § 176.170(c) of this chapter tion, 200 C St. SW., Washington, DC, or under conditions of use E through G as at the Office of the Federal Register, described in table 2 of § 176.170(c) of this 800 North Capitol St. NW., suite 700, chapter. Washington, DC. (d) The provisions of this section are (3) The basic copolymer identified in not applicable to ethylene-acrylic acid paragraph (a) of this section, when ex- copolymers used in food-packaging ad- tracted with the solvent or solvents hesives complying with § 175.105 of this characterizing the type of food and chapter. under the conditions of time and tem- perature characterizing the conditions [42 FR 14572, Mar. 15, 1977, as amended at 51 of its intended use, as determined from FR 19060, May 27, 1986; 53 FR 44009, Nov. 1, 1988] tables 1 and 2 of § 176.170(c) of this chap- ter, yields net chloroform-soluble ex- § 177.1312 Ethylene-carbon monoxide tractives in each extracting solvent copolymers. not to exceed 0.5 milligram per square inch of food-contact surface when test- The ethylene-carbon monoxide co- ed by methods described in § 176.170(d) polymers identified in paragraph (a) of of this chapter. this section may be safely used as com- ponents of articles intended for use in (4) The provisions of this section are contact with food subject to the provi- not applicable to ethylene-carbon mon- sions of this section. oxide copolymers complying with § 175.105 of this chapter. (a) Identity. For the purposes of this section, ethylene-carbon monoxide co- [57 FR 32422, July 22, 1992] polymers (CAS Reg. No. 25052–62–4) con- sist of the basic polymers produced by § 177.1315 Ethylene-1, 4-cyclohexylene the copolymerization of ethylene and dimethylene terephthalate copoly- carbon monoxide such that the copoly- mers. mers contain not more than 30 weight- Ethylene-1, 4-cyclohexylene percent of polymer units derived from dimethylene terephthalate copolymer carbon monoxide. may be safely used as articles or com- (b) Conditions of use. (1) The polymers ponents of articles intended for use in may be safely used as components of contact with food subject to provisions
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of this section and of part 174 of this erized with 1,4-cyclohexanedimethanol chapter. and 1,2-ethanediol) (CAS Reg. No. (a) Identity. For the purposes of this 25038–91–9) are basic copolymers meet- section, ethylene-1,4-cyclohexylene ing the specifications prescribed in dimethylene terephthalate copolymers paragraph (b) of this section, to which (1,4-benzene dicarboxylic acid, di- may have been added certain optional methyl ester, polymerized with 1,4- substances required in their production cyclohexanedimethanol and 1,2- or added to impart desired physical or ethanediol) (CAS Reg. No. 25640–14–6) or technical properties. (1,4-benzenedicarboxylic acid, polym- (b) Specifications:
Maximum extractable fractions of the copolymer in the fin- Ethylene-1,4- ished form at specified tem- cyclohexylene peratures and times (ex- Test for dimethylene Inherent viscosity pressed in micrograms of the orientability Conditions of use terephthalate copolymers terephthaloyl moletles/square centimeter of food-contact sur- face)
1. Non-oriented ethyl- Inherent viscosity (1) 0.23 microgram per square No test required ... In contact with foods, in- ene-1,4-cyclohexylene of a 0.50 per- centimeter (1.5 micrograms cluding foods con- dimethylene cent solution of per square inch) of food-con- taining not more than terephthalate copoly- the copolymer in tact surface when extracted 25 percent (by vol- mer is the reaction phenol-tet with water added at 82.2 °C ume) aqueous alcohol, product of dimethyl rachloroethane (180 °F) and allowed to cool excluding carbonated terephthalate or ter- (60:40 ratio wt/ to 48.9 °C (120 °F) in con- beverages and beer. ephthalic acid with a wt) solvent is tact with the food-contact ar- Conditions of hot fill mixture containing 99 not less than ticle. not to exceed 82.2 °C to 66 mole percent of 0.669 as deter- (180 °F), storage at ethylene glycol and 1 mined by using temperatures not in to 34 mole percent of a Wagner vis- excess of 48.9 °C 1,4-cyclo- cometer (or (120 °F). No thermal hexanedimethanol (70 equivalent) and treatment in the con- percent trans isomer, calculated from tainer. 30 percent cls isomer). the following equation: Inher- ent viscosity = (Natural loga- rithm of (Nr)/(c) where: Nr=Ratio of flow time of the polymer so- lution to that of the solvent, and c=concentration of the test solu- tion expressed in grams per 100 milliliters...... do ...... (2) 0.23 microgram per square ...... do ...... Do. centimeter (1.5 micrograms per square inch) of food-con- tact surface when extracted with 3 percent (by volume) aqueous acetic acid added at 82.2 °C (180 °F) and al- lowed to cool to 48.9 °C (120 °F) in contact with the food-contact article...... do ...... (3) 0.08 microgram per square ...... do ...... Do. centimeter (0.5 microgram per square inch) of food-con- tact surface when extracted for 2 hours with n-heptane at 48.9 °C (120 °F). The heptane extractable results are to be divided by a factor of 5.
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Maximum extractable fractions of the copolymer in the fin- Ethylene-1,4- ished form at specified tem- cyclohexylene peratures and times (ex- Test for dimethylene Inherent viscosity pressed in micrograms of the orientability Conditions of use terephthalate copolymers terephthaloyl moletles/square centimeter of food-contact sur- face)
...... do ...... (4) 0.16 microgram per square ...... do ...... Do. centimeter (1.0 microgram per square inch) of food-con- tact surface when extracted for 24 hours with 25 percent (by volume) aqueous ethanol at 48.9 °C (120 °F). 2. Oriented ethylene-1,4- ...... do ...... (1) 0.23 microgram per square When extracted In contact with non- cyclohexylene centimeter (1.5 micrograms with heptane at alcoholic foods includ- dimethylene per square inch) of food-con- 65.6 °C (150 °F) ing carbonated bev- terephthalate copoly- tact surface of the oriented for 2 hours: erages. Conditions of mer is the reaction copolymer when extracted terephthaloyl hot fill not exceeding product of dimethyl with water added at 87.8 °C moieties do not 87.8 °C (190 °F), stor- terephthalate or ter- (190 °F) and allowed to cool exceed 0.09 age at temperatures ephthalic acid with a to 48.9 °C (120 °F) in con- microgram per not in excess of 48.9 mixture containing 99 tact with the food-contact ar- square centi- °C (120 °F). No ther- to 85 mole percent ticle. meter (0.60 mal treatment in the ethylene glycol and 1 microgram per container. to 15 mole percent of square inch) of 1,4-cyclohexane-di- food-contact methanol (70 percent surface. trans isomer, 30 per- cent cls isomer)...... do ...... (2) 0.23 microgram per square ...... do ...... Do. centimeter (1.5 micrograms per square inch) of food-con- tact surface of oriented co- polymer when extracted with 3 percent (by volume) aque- ous acetic acid added at 87.8 °C (190 °F) and al- lowed to cool to 48.9 °C (120 °F) in contact with the food-contact article...... do ...... (3) 0.08 microgram per square ...... do ...... Do. centimeter (0.5 microgram per square inch) of food-con- tact surface of oriented co- polymer when extracted for 2 hours with n-heptane at 48.9 °C (120 °F). The heptane extractable results are to be divided by a factor of 5...... do ...... (4) 0.23 microgram per square ...... do ...... In contact with foods and centimeter (1.5 micrograms beverages containing per square inch) of food-con- up to 20 percent (by tact surface of oriented co- volume) alcohol. Con- polymer when extracted with ditions of thermal 20 percent (by volume) treatment in the con- aqueous ethanol heated to tainer not exceeding 65.6 °C (150 °F) for 20 min- 65.6 °C (150 °F) for utes and allowed to cool to 20 minutes. Storage at 48.9 °C (120 °F) in contact temperatures not in with the food-contact article. excess of 48.9 °C (120 °F)...... do ...... (5) 0.23 microgram per square ...... do ...... In contact with foods and centimeter (1.5 micrograms beverages containing per square inch) of food-con- up to 50 percent (by tact surface of oriented co- volume) alcohol. Con- polymer when extracted with ditions of fill and stor- 50 percent (by volume) age not exceeding aqueous ethanol at 48.9 °C 48.9 °C (120 °F). No (120 °F) for 24 hours. thermal treatment in the container.
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Maximum extractable fractions of the copolymer in the fin- Ethylene-1,4- ished form at specified tem- cyclohexylene peratures and times (ex- Test for dimethylene Inherent viscosity pressed in micrograms of the orientability Conditions of use terephthalate copolymers terephthaloyl moletles/square centimeter of food-contact sur- face)
3. Ethylene-1,4- No test required ... For each corresponding condi- No test required ... For each corresponding cyclohexylene tion of use, must meet speci- specification, may be dimethylene fications described in used as a base sheet terephthalate copoly- ¤ 177.1630(f), (g), (h), or (j). and base polymer in mer is the reaction accordance with con- product of dimethyl ditions of use de- terephthalate or ter- scribed in ephthalic acid with a ¤ 177.1630(f), (g), (h), mixture containing 99 or (j). to 95 mole percent of ethylene glycol and 1 to 5 mole percent of 1,4- cyclohexanedimethan- ol (70 percent trans isomer, 30 percent cis isomer).
(c) Analytical method for determination with the following prescribed condi- of extractability. The total extracted tions: terephthaloyl moieties can be deter- (a) Ethylene-ethyl acrylate copoly- mined in the extracts, without evapo- mers consist of basic resins produced ration of the solvent, by measuring the by the catalytic copolymerization of ultraviolet (UV) absorbance at 240 ethylene and ethyl acrylate, to which nanometers. The spectrophotometer may have been added certain optional (Varian 635–D, or equivalent) is zeroed substances to impart desired techno- with a sample of the solvent taken logical properties to the resin. Subject from the same lot used in the extrac- to any limitations prescribed in this tion tests. The concentration of the section, the optional substances may total terephthaloyl moieties in water, 3 include: percent acetic acid, and in 8 percent (1) Substances generally recognized aqueous alcohol is calculated as bis(2- as safe in food and food packaging. hydroxyethyl terephthalate) by ref- (2) Substances the use of which is erence to standards prepared in the ap- permitted under applicable regulations propriate solvent. Concentration of the in parts 170 through 189 of this chapter, terephthaloyl moieties in heptane is prior sanction, or approvals. calculated as cyclic trimer (b) The ethyl acrylate content of the copolymer does not exceed 8 percent by (C6H4CO2C2H4CO2)3, by reference to standards prepared in 95:5 percent (v/v) weight unless it is blended with poly- ethylene or with one or more olefin co- heptane: tetrahydrofuran. polymers complying with § 177.1520 or [45 FR 39252, June 10, 1980, as amended at 47 with a mixture of polyethylene and one FR 24288, June 4, 1982; 49 FR 25629, June 22, or more olefin copolymers, in such pro- 1984; 51 FR 22929, June 24, 1986; 60 FR 57926, portions that the ethyl acrylate con- Nov. 24, 1995] tent of the blend does not exceed 8 per- cent by weight, or unless it is used in § 177.1320 Ethylene-ethyl acrylate co- a coating complying with § 175.300 or polymers. § 176.170 of this chapter, in such propor- Ethylene-ethyl acrylate copolymers tions that the ethyl acrylate content may be safely used to produce pack- does not exceed 8 percent by weight of aging materials, containers, and equip- the finished coating. ment intended for use in producing, (c) Ethylene-ethyl acrylate copoly- manufacturing, packing, processing, mers or the blend shall conform to the preparing, treating, packaging, trans- specifications prescribed in paragraph porting, or holding food, in accordance (c)(1) of this section and shall meet the
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ethyl acrylate content limits pre- § 177.1330 Ionomeric resins. scribed in paragraph (b) of this section, Ionomeric resins manufactured from and the extractability limits pre- either ethylene-methacrylic acid co- scribed in paragraph (c)(2) of this sec- polymers (and/or their ammonium, cal- tion, when tested by the methods pre- cium, magnesium, potassium, sodium, scribed for polyethylene in § 177.1520. and/or zinc partial salts), ethylene- (1) Specifications—(i) Infrared identi- methacrylic acid-vinyl acetate copoly- fication. Ethylene-ethyl acrylate co- mers (and/or their ammonium, cal- polymers can be identified by their cium, magnesium, potassium, sodium, characteristic infrared spectra. and/or zinc partial salts,), or meth- (ii) Quantitative determination of ethyl acrylic acid polymers with ethylene acrylate content. The ethyl acrylate can and isobutyl acrylate (and/or their po- be determined by the infrared spectra. tassium, sodium and/or zinc partial Prepare a scan from 10.5 microns to 12.5 salts) may be safely used as articles or microns. Obtain a baseline absorbance components of articles intended for use in contact with food, in accordance at 11.6 microns and divide by the with the following prescribed condi- plaque thickness to obtain absorbance tions: per mil. From a previously prepared (a) For the purpose of this section, calibration curve, obtain the amount of the ethylene-methacrylic acid copoly- ethyl acrylate present. mers consist of basic copolymers pro- (iii) Specific gravity. Ethylene-ethyl duced by the copolymerization of acrylate copolymers have a specific ethylene and methacrylic acid such gravity of not less than 0.920 nor more that the copolymers contain no more than 0.935, as determined by ASTM than 20 weight percent of polymer method D1505–68 (Reapproved 1979), units derived from methacrylic acid, ‘‘Standard Test Method for Density of and the ethylene-methacrylic acid- Plastics by the Density-Gradient Tech- vinyl acetate copolymers consist of nique,’’ which is incorporated by ref- basic copolymers produced by the co- erence. Copies may be obtained from polymerization of ethylene, meth- the American Society for Testing Ma- acrylic acid, and vinyl acetate such terials, 1916 Race St., Philadelphia, PA that the copolymers contain no more than 15 weight percent of polymer 19103, or may be examined at the Office units derived from methacrylic acid. of the Federal Register, 800 North Cap- (b) For the purpose of this section, itol Street, NW., suite 700, Washington, the methacrylic acid copolymers with DC 20408. ethylene and isobutyl acrylate consist (2) Limitations. Ethylene-ethyl acry- of basic copolymers produced by the late copolymers or the blend may be copolymerization of methacrylic acid, used in contact with food except as a ethylene, and isobutyl acrylate such component of articles used for pack- that the copolymers contain no less aging or holding food during cooking than 70 weight percent of polymer provided they meet the following units derived from ethylene, no more extractability limits: than 15 weight percent of polymer (i) Maximum soluble fraction of 11.3 units derived from methacrylic acid, percent in xylene after refluxing and and no more than 20 weight percent of subsequent cooling to 25 °C. polymer units derived from isobutyl (ii) Maximum extractable fraction of acrylate. From 20 percent to 70 percent 5.5 percent when extracted with n- of the carboxylic acid groups may op- hexane at 50 °C. tionally be neutralized to form sodium (d) The provisions of paragraphs (b) or zinc salts. and (c)(2) of this section are not appli- (c) The finished food-contact article described in paragraph (a) of this sec- cable to ethylene-ethyl acrylate co- tion, when extracted with the solvent polymers used in the formulation of ad- or solvents characterizing the type of hesives complying with § 175.105 of this food and under the conditions of time chapter. and temperature characterizing the [42 FR 14572, Mar. 15, 1977, as amended at 49 conditions of its intended use as deter- FR 10108, Mar. 19, 1984] mined from tables 1 and 2 of § 176.170(c)
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of this chapter, yields net acidified square inch 2(0.003 milligram/square chloroform-soluble extractives in each centimeter) of food-contact surface extracting solvent not to exceed 0.5 (water, acetic acid, or ethanol/water milligram per square inch of food-con- extractions) when extracted by the ab- tact surface when tested by the meth- breviated method cited in paragraph ods described in paragraph (e)(1) of this (e)(2)(i) of this section. section, and if the finished food-con- (ii) Alternatively, the net acidified tact article is itself the subject of a chloroform-soluble extractives shall regulation in parts 174, 175, 176, 177, 178 not exceed 0.05 milligram/square inch 3 and § 179.45 of this chapter, it shall also (0.078 mg/square centimeter) of food- comply with any specifications and contact surface (water, acetic acid, or limitations prescribed for it by that ethanol/water extractions) when ex- regulation. tracted by the equilibrium method NOTE: In testing the finished food-contact cited in paragraph (e)(2)(ii) of this sec- article, use a separate test sample for each tion. If when exposed to n-heptane, a required extracting solvent. particular film splits along die lines, (d) The finished food-contact article thus permitting exposure of both sides described in paragraph (b) of this sec- of the film to the extracting solvent, tion, when extracted according to the the results for that film sample are in- methods listed in paragraph (e)(2) of valid and the test must be repeated for this section and referenced in this that sample until no splitting by the paragraph (d), using the solvent or sol- solvent occurs. If the finished food-con- vents characterizing the type of food as tact article is itself the subject of a determined from table I of paragraph regulation in parts 174, 175, 176, 177, 178 (f) of this section, shall yield net acidi- and § 179.45 of this chapter, it shall also fied chloroform-soluble extractives as comply with any specifications and follows: limitations prescribed for it by that (1) For fatty food use. (i) For films of regulation. 2 mil (0.002 inches) thickness or less, NOTE: In testing the finished food-contact extractives shall not exceed 0.70 milli- article, use a separate test sample for each gram/square inch 1 (0.109 milligram/ required extracting solvent. (e) (1) square centimeter) of food-contact sur- Analytical methods— Selection of extractability conditions for ionomeric res- face (n-heptane extractions) when ex- ins. First ascertain the type of food tracted by the abbreviated method (table 1 of § 176.170(c) of this chapter) cited in paragraph (e)(2)(i) of this sec- that is being packed or used in contact tion. with the finished food-contact article (ii) For films of greater than 2 mils described in paragraph (a) of this sec- (0.002 inch) thickness, extractives shall 1 tion, and also ascertain the normal not exceed 0.40 milligram/square inch conditions of thermal treatment used (0.062 milligram/square centimeter) of in packaging or contacting the type of food-contact surface (n-heptane extrac- food involved. Using table 2 of § 176.170 tions) when extracted by the abbre- (c) of this chapter, select the food-sim- viated method cited in paragraph ulating solvent or solvents and the (e)(2)(i) of this section, or time-temperature test conditions that (iii) Alternatively, for films of great- correspond to the intended use of the er than 2 mils thickness, extractives finished food-contact article. Having shall not exceed 0.70 milligram/square selected the appropriate food-simu- 1 inch (0.109 milligram/square centi- lating solvent or solvents and time- meter) of food-contact surface (n- temperature exaggeration over normal heptane extractions) when extracted by use, follow the applicable extraction the equilibrium method cited in para- procedure. graph (e)(2)(ii) of this section. (2) Selection of extractability conditions (2) For aqueous foods. (i) The net for ionomeric resins. Using table I of acidified chloroform-soluble extrac- tives shall not exceed 0.02 milligram/ 2 Average of four separate values, no single value of which differs from the average of 1 Average of four separate values, no single those values by more than ±50 percent. value of which differs from the average of 3See footnote 2 to paragraph (d)(2)(i) of this those values by more then ±10 percent. section.
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paragraph (f) of this section ascertain (ii) n-Heptane. Reagent grade, freshly the type of food that is being packed or redistilled before use, using only mate- used in contact with the finished food- rial boiling at 208 °F (97.8 °C). contact article described in paragraph (iii) Alcohol. 8 or 50 percent (by vol- (b) of this section, and also ascertain ume), prepared from undenatured 95 the food-simulating solvent or solvents percent ethyl alcohol diluted with that correspond to the intended use of demineralized (deionized), distilled the finished food-contact article. water. (i) Abbreviated test. For intended use (iv) Chloroform. Reagent grade, fresh- involving food contact at or below 120 ly redistilled before use, or a grade °F (49 °C), the appropriate food-simu- having an established, consistently low lating solvent is to contact the food- blank. contact film for the time and tempera- (v) Acetic acid. 3 percent (by weight), tures as follows: prepared from glacial acetic acid di- luted with demineralized (deionized), Solvent Time Temperature distilled water. n-Heptane ...... 1 2 120 °F (49 °C). (4) Selection of test method. The fin- Water, 3% acetic acid, or 8%/ 1 48 120 °F (49 °C). ished food-contact articles shall be 50% ethanol. tested either by the extraction cell de- 1 Hours scribed in the Journal of the Association (ii) Equilibrium test. For intended use of Official Agricultural Chemists, Vol. 47, involving food contact at or below 120 No. 1, p. 177–179 (February 1964), also °F (49 °C), the appropriate food-simu- described in ASTM method F34–76 (Re- lating solvent is to contact the food- approved 1980), ‘‘Standard Test Method contact film at a temperature of 120 °F for Liquid Extraction of Flexible Bar- until equilibrium is demonstrated. rier Materials,’’ which are incorporated by reference, or by adapting the in-con- Minimum tainer methods described in § 175.300(e) extraction Solvent times of this chapter. Copies of the material (hours) incorporated by reference are available n-Heptane ...... 8, 10, 12 from the Center for Food Safety and Water, 3% acetic acid, or 8%/50% ethanol ...... 72, 96, Applied Nutrition (HFS–200), Food and 120 Drug Administration, 200 C St. SW., Washington, DC 20204, and the Amer- The results from a series of extraction ican Society for Testing Materials, 1916 times demonstrate equilibrium when Race St., Philadelphia, PA 19103, re- the net chloroform-soluble extractives spectively, or may be examined at the are unchanging within experimental Office of the Federal Register, 800 error appropriate to the method as de- North Capitol Street, NW., suite 700, scribed in paragraphs (d) (1)(i) and (2)(i) Washington, DC 20408. of this section. Should equilibrium not (5) Selection of samples. Quadruplicate be demonstrated over the above time samples should be tested, using for series, extraction times must be ex- each replicate sample the number of tended until three successive unchang- finished articles with a food-contact ing values for extractives are obtained. surface nearest to 100 square inches. In the case where intended uses involve (6) Determination of amount of extrac- temporary food contact above 120 °F, tives—(i) Total residues. At the end of the food-simulating solvent is to be the exposure period, remove the test contacted with the food-contact article container or test cell from the oven, if under conditions of time and tempera- any, and combine the solvent for each ture that duplicate the actual condi- replicate in a clean Pyrex (or equiva- tions in the intended use. Subsequently lent) flask or beaker, being sure to the extraction is to be continued for rinse the test container or cell with a the time period and under the condi- small quantity of clean solvent. Evapo- tions specified in the above table. rate the food-simulating solvents to (3) Reagents—(i) Water. All water used about 100 milliliters in the flask, and in extraction procedures should be transfer to a clean, tared evaporating freshly demineralized (deionized) dis- dish (platinum or Pyrex), washing the tilled water. flask three times with small portions
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of solvent used in the extraction proce- dish, the filter paper, and the sepa- dure, and evaporate to a few milliliters ratory funnel with this second portion on a nonsparking, low-temperature of chloroform. Add this filtrate to the hotplate. The last few milliliters original filtrate and evaporate the should be evaporated in an oven main- total down to a few milliliters on a tained at a temperature of 221 °F (105 low-temperature hotplate. The last few °C). Cool the evaporating dish in a des- milliliters should be evaporated in an iccator for 30 minutes and weigh the oven maintained at 221 °F. Cool the residues to the nearest 0.1 milligram, e. evaporating dish in a desiccator for 30 Calculate the extractives in milligrams minutes and weigh to the nearest 0.1 per square inch of the container or ma- milligram to get the acidified chloro- terial surface. form-soluble extractives residue, e′. (a) Water, 3 percent acetic acid, and 8 This e′ is substituted for e in the equa- percent and 50 percent alcohol. Milli- tions in paragraphs (e)(6)(i) (a) and (b) grams extractives per square inch=e/s. (b) Heptane. Milligrams extractives of this section. per square inch=(e)/(s)(F) (f) The types of food and appropriate solvents are as follows: where: e=Milligrams extractives per sample tested. TABLE 1 s=Surface area tested, in square inches. F=Five, the ratio of the amount of extrac- Types of food Appropriate solvent tives removed by heptane under exagger- ated time-temperature test conditions 1. Nonacid (pH above 5.0), aque- Water, n-heptane. compared to the amount extracted by a ous products; may contain salt or sugar or both, and including fat or oil under exaggerated conditions of oil-in-water emulsions of low- or thermal sterilization and use. high-fat content. e′=Acidified chloroform-soluble extractives 2. Acidic (pH 5.0 or below), aque- n-heptane, water, 3% residue. e′ is substituted for e in the ous products; may contain salt acetic acid. above equations when necessary (See or sugar or both, and including paragraph (e)(6)(ii) of this section for oil-in-water emulsions of low- or method to obtain e′). high-fat content. 3. Aqueous, acid or nonacid prod- Water, n-heptane, 3% If when calculated by the equations in ucts containing free oil or fat; acetic acid. may contain salt, and including paragraphs (e)(6)(i) (a) and (b) of this water-in-oil emulsions of low- or section, the extractives in milligrams high-fat content. per square inch exceed the limitations 4. Dairy products and modifica- prescribed in paragraphs (c) or (d) of tions: Water, n-heptane. this section, proceed to paragraph i. Water-in-oil emulsions, high (e)(6)(ii) of this section (method for de- or low fat. termining the amount of acidified chlo- ii. Oil-in-water emulsions, high roform-soluble extractives residue). or low fat. (ii) Acidified chloroform-soluble extrac- 5. Low moisture fats and oils ...... n-heptane. 6. Beverages: tives residue. Add 3 milliliters of 37 per- i. Containing up to 8% alcohol 8% ethanol/water. cent ACS reagent grade hydrochloric ii. Nonalcoholic ...... 3% acetic acid. acid and 3 milliliters of distilled water iii. Containing more than 8% 50% ethanol/water. to the evaporating dish containing the alcohol. dried and weighed residue, e, obtained 7. Bakery products ...... Water, n-heptane. in paragraph (e)(6)(i) of this section. 8. Dry solids (without free fat or No extraction test re- oil). quired. Mix well so every portion of the residue 9. Dry solids (with free fat or oil) .. n-heptane. is wetted with the hydrochloric acid solution. Then add 50 milliliters of (g) The provisions of paragraphs (c) chloroform. Warm carefully, and filter and (d) of this section are not applica- through Whatman No. 41 filter paper ble to the ionomeric resins that are (or equivalent) in a Pyrex (or equiva- used in food-packaging adhesives com- lent) funnel, collecting the filtrate in a plying with § 175.105 of this chapter. clean separatory funnel. Shake for 1 minute, then draw off the chloroform [45 FR 22916, Apr. 4, 1980, as amended at 49 layer into a clean tared evaporating FR 10108, Mar. 19, 1984; 49 FR 37747, Sept. 26, dish (platinum or Pyrex). Repeat the 1984; 53 FR 44009, Nov. 1, 1988; 54 FR 24898, chloroform extraction, washing the June 12, 1989]
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§ 177.1340 Ethylene-methyl acrylate co- (a) Identity. For the purpose of this polymer resins. section, ethylene/1,3-phenylene oxy- Ethylene-methyl acrylate copolymer ethylene isophthalate/terephthalate copolymer consists of the basic copoly- resins may be safely used as articles or mer produced by the catalytic components of articles intended for use polycondensation of isophthalic acid in contact with food, in accordance and terephthalic acid with ethylene with the following prescribed condi- glycol and 1,3-bis(2- tions: hydroxyethoxy)benzene such that the (a) For the purpose of this section, finished resin contains between 42 and the ethylene-methyl acrylate copoly- 48 mole-percent of isophthalic mer resins consist of basic copolymers moieties, between 2 and 8 mole-percent produced by the copolymerization of of terephthalic moieties, and not more ethylene and methyl acrylate such than 10 mole-percent of 1,3-bis(2- that the copolymers contain no more hydroxyethoxy)benzene moieties. than 25 weight percent of polymer (b) Specifications—(1) Density. Ethyl- units derived from methyl acrylate. ene/1,3-phenylene oxyethylene (b) The finished food-contact article, isophthalate/terephthalate copolymer when extracted with the solvent or sol- identified in paragraph (a) of this sec- vents characterizing the type of food tion has a density of 1.33±0.02 grams per and under the conditions of time and cubic centimeter measured by ASTM temperature characterizing the condi- Method D 1505–85 (Reapproved 1990), tions of its intended use as determined ‘‘Standard Test Method for Density of from tables 1 and 2 of § 176.170(c) of this Plastics by the Density-Gradient Tech- chapter, yields net chloroform-soluble nique,’’ which is incorporated by ref- extractives (corrected for zinc extrac- erence in accordance with 5 U.S.C. tives as zinc oleate) in each extracting 552(a) and 1 CFR part 51. Copies may be solvent not to exceed 0.5 milligram per obtained from the American Society square inch of food-contact surface for Testing and Materials, 1916 Race when tested by the methods described St., Philadelphia, PA 19103, or may be in § 176.170(d) of this chapter. If the fin- examined at the Center for Food Safety ished food-contact article is itself the and Applied Nutrition’s Library, Food subject of a regulation in parts 174, 175, and Drug Administration, 200 C St. 176, 177, 178 and § 179.45 of this chapter, SW., Washington, DC 20204, and the Of- it shall also comply with any specifica- fice of the Federal Register, 800 North tions and limitations prescribed for it Capitol St. NW., suite 700, Washington, by that regulation. DC. NOTE: In testing the finished food-contact (2) Softening point. Ethylene/1,3–phen- article, use a separate test sample for each ylene oxyethylene isophthalate/ required extracting solvent. terephthalate copolymer identified in (c) The provisions of this section are paragraph (a) of this section has a soft- not applicable to ethylene-methyl ac- ening point of 63±5 °C as measured by rylate copolymer resins used in food- ASTM Method D 1525–87, ‘‘Standard packaging adhesives complying with Test Method for VICAT Softening Tem- § 175.105 of this chapter. perature of Plastics,’’ which is incor- porated by reference in accordance § 177.1345 Ethylene/1,3–phenylene oxy- with 5 U.S.C. 552(a) and 1 CFR part 51. ethylene isophthalate/ The availability of this material is pro- terephthalate copolymer. vided in paragraph (b)(1) of this sec- Ethylene/1, 3-phenylene oxyethylene tion. isophthalate/terephthalate copolymer (c) Optional adjuvant substances. (CAS Reg. No. 87365–98–8) identified in Ethylene/1,3–phenylene oxyethylene paragraph (a) of this section may be isophthalate/terephthalate copolymer, safely used, subject to the provisions of identified in paragraph (a) of this sec- this section, as the non-food-contact tion, may contain optional adjuvant layer of laminate structures subject to substances required in their produc- the provisions of § 177.1395, and in tion. The optional adjuvants may in- blends with polyethylene terephthalate clude substances used in accordance polymers complying with § 177.1630. with § 174.5 of this chapter.
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(d) Limitations. Copolymer blends de- (vi) The copolymer of vinylidene flu- scribed above shall not exceed 30 per- oride and hexafluoropropene (CAS Reg. cent by weight of ethylene/1, 3-phen- No. 9011–17–0), containing 65 to 71 per- ylene oxyethylene isophthalate/ cent fluorine and having a Mooney Vis- terephthalate copolymer. The finished cosity of at least 28, for use as a proc- blend may be used in contact with food essing aid at a level not to exceed 0.2 only under conditions of use C through percent by weight of ethylene-vinyl ac- G, as described in table 2 of § 176.170(c) etate copolymers. of this chapter, except that with food (2) Maleic anhydride-grafted ethyl- identified as Type III, IV–A, V, VII–A, ene-vinyl acetate copolymers (CAS and IX in § 176.170(c), table 1, the co- Reg. No. 28064–24–6) consist of basic res- polymer may be used under condition ins produced by the catalytic copolym- of use C at temperatures not to exceed erization of ethylene and vinyl acetate, 160 °F (71 °C). followed by reaction with maleic anhy- [57 FR 43399, Sept. 21, 1992, as amended at 59 dride. Such polymers shall contain not FR 62318, Dec. 5, 1994; 61 FR 14481, Apr. 2, more than 11 percent of polymer units 1996; 62 FR 34628, June 27, 1997] derived from vinyl acetate by weight of total polymer prior to reaction with § 177.1350 Ethylene-vinyl acetate co- maleic anhydride, and not more than 2 polymers. percent of grafted maleic anhydride by Ethylene-vinyl acetate copolymers weight of the finished polymer. Op- may be safely used as articles or com- tional adjuvant substances that may be ponents of articles intended for use in added to the copolymers include sub- producing, manufacturing, packing, stances generally recognized as safe in processing, preparing, treating, pack- food and food packaging, substances aging, transporting, or holding food in the use of which is permitted under ap- accordance with the following pre- plicable regulations in parts 170 scribed conditions: through 189 of this chapter, and sub- (a)(1) Ethylene-vinyl acetate copoly- stances identified in § 175.300(b)(3)(xxv), mers consist of basic resins produced (xxvii), (xxxiii), and (xxx) of this chap- by the catalytic copolymerization of ter and colorants for polymers used in ethylene and vinyl acetate to which accordance with the provisions of may have been added certain optional § 178.3297 of this chapter. substances to impart desired techno- (b)(1) Ethylene-vinyl acetate copoly- logical or physical properties to the mers, with or without the optional sub- resin. Subject to any limitations pre- stances described in paragraph (a) of scribed in this section, the optional this section, when extracted with the substances may include: solvent or solvents characterizing the (i) Substances generally recognized type of food, and under conditions of as safe in food and food packaging. time and temperature characterizing (ii) Substances the use of which is the conditions of their intended use as permitted under applicable regulations determined from tables 1 and 2 of in parts 170 through 189 of this chapter, § 176.170(c) of this chapter, shall yield prior sanction, or approvals. net chloroform-soluble extractives cor- (iii) Substances identified in rected for zinc as zinc oleate not to ex- § 175.300(b)(3) (xxv), (xxvii), (xxx), and ceed 0.5 milligram per square inch of an (xxxiii) of this chapter, and colorants appropriate sample. used in accordance with § 178.3297 of (2) Maleic anhydride grafted ethyl- this chapter. ene-vinyl acetate copolymers shall (iv) Erucamide as identified in have a melt flow index not to exceed 2.1 § 178.3860 of this chapter. grams per 10 minutes as determined by (v) Xanthan gum as identified in ASTM method D 1238–82, ‘‘Standard §172.695 for use as a thickening agent Test Method for Flow Rates of Thermo- at a level not to exceed 1 percent by plastics by Extrusion Plastometer,’’ weight of coating solids in aqueous dis- which is incorporated by reference in persions of ethylene-vinyl acetate co- accordance with 5 U.S.C. 552(a). Copies polymers, where such copolymers are may be obtained from the American used only as coatings or a component Society for Testing Materials, 1916 of coatings. Race St., Philadelphia, PA 19103, or at
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the Division of Petition Control (HFS– growth of microorganisms under the 215), Center for Food Safety and Ap- following conditions: plied Nutrition, Food and Drug Admin- (1) Gamma photons emitted from a istration, 200 C St. SW., Washington, cobalt–60 sealed source in the dose DC 20204, or may be examined at the range of 5–50 kiloGray (0.5–5.0 Center for Food Safety and Applied Nu- megarads). trition’s Library, 200 C St. SW., rm. (2) The irradiated ethylene-vinyl ace- 3321, Washington, DC, or at the Office tate copolymer films, when extracted of the Federal Register, 800 North Cap- with reagent grade n-heptane (freshly itol St. NW., suite 700, Washington, DC. redistilled before use) according to Compliance of the melt flow index methods described under § 176.170(d)(3) specification shall be determined using of this chapter, at 75 °F for 30 minutes conditions and procedures cor- shall yield total extractives not to ex- responding to those described in the ceed 4.5 percent by weight of the film. method as Condition E, Procedure A). The copolymers shall be used in blends [42 FR 14572, Mar. 15, 1977, as amended at 43 with other polymers at levels not to FR 29287, July 7, 1978; 54 FR 35874, Aug. 30, exceed 17 percent by weight of total 1989; 55 FR 18595, May 3, 1990; 56 FR 42932, Aug. 30, 1991; 64 FR 47108, Aug. 30, 1999] polymer, subject to the limitation that when contacting food of types III, IV– § 177.1360 Ethylene-vinyl acetate-vinyl A, V, VI–C, VII–A, and IX, identified in alcohol copolymers. § 176.170(c) of this chapter, Table 1, the polymers shall be used only under con- Ethylene-vinyl acetate-vinyl alcohol ditions of use C, D, E, F, and G, de- copolymers (CAS Reg. No. 26221–27–2) scribed in § 176.170(c) of this chapter, may be safely used as articles or com- Table 2. ponents of articles intended for use in (c) The provisions of paragraph (b) of contact with food, in accordance with this section are not applicable to ethyl- the following prescribed conditions: ene-vinyl acetate copolymers used in (a) Ethylene-vinyl acetate-vinyl alco- food-packaging adhesives complying hol copolymers are produced by the with § 175.105 of this chapter. partial or complete alcoholysis or hy- (d) Ethylene-vinyl acetate copoly- drolysis of those ethylene-vinyl acetate mers may be irradiated under the fol- copolymers complying with § 177.1350. lowing conditions to produce molecular (1) Those copolymers containing a crosslinking of the polymers to impart minimum of 55 percent ethylene and a desired properties such as increased maximum of 30 percent vinyl alcohol strength and increased ability to units by weight may be used in contact shrink when exposed to heat: with foods as described in paragraph (b) (1) Electron beam source of ionizing of this section. radiation at a maximum energy of 3 (2) Those copolymers containing a million electron volts: Maximum ab- minimum of 55 percent ethylene and a sorbed dose not to exceed 150 kiloGray maximum of 15 percent vinyl alcohol (15 megarads). units by weight may be used in contact (2) The finished food-contact film with foods as described in paragraph (c) shall meet the extractives limitations of this section. prescribed in paragraph (e)(2) of this (3) Those copolymers containing 17 to section. 40 percent ethylene and 60 to 83 percent (3) The ethylene-vinyl acetate co- vinyl alcohol units by weight may be polymer films may be further irradi- used in contact with foods as described ated in accordance with the provisions in paragraph (d) of this section. of paragraph (e)(1) of this section: Pro- (b) The finished food-contact article vided, That the total accumulated radi- shall not exceed 0.013 centimeter (0.005 ation dose from both electron beam inch) thickness and shall contact foods and gamma ray radiation does not ex- only of the types identified in table 1 of ceed 150 kiloGray (15 megarads). § 176.170(c) of this chapter in Categories (e) Ethylene-vinyl acetate copolymer I, II, IV–B, VI, VII–B, and VIII under films intended for contact with food conditions of use D through G de- may be irradiated to control the scribed in table 2 of § 176.170(c) of this
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chapter. Film samples of 0.013 centi- table 2 of § 176.170(c) of this chapter. meter (0.005) inch thickness rep- Film samples of 0.018 centimeter (0.007 resenting the finished article shall inch) thickness representing the fin- meet the following extractive limita- ished articles shall meet the following tion when tested by ASTM method extractive limitation when tested by F34–76 (Reapproved 1980), ‘‘Standard ASTM method F34–76 (Reapproved Test Method for Liquid Extraction of 1980), ‘‘Standard Test Methods for Liq- Flexible Barrier Materials,’’ which is uid Extraction of Flexible Barrier Ma- incorporated by reference. Copies may terials,’’ which is incorporated by ref- be obtained from the American Society erence. The availability of this incor- for Testing Materials, 1916 Race St., poration by reference is given in para- Philadelphia, PA 19103, or may be ex- graph (b) of this section. The film when amined at the Office of the Federal extracted with distilled water at 100 °C Register, 800 North Capitol Street, (212 °F) for 30 minutes yields ethylene- NW., suite 700, Washington, DC 20408. vinyl acetate-vinyl alcohol oligomers (1) The film when extracted with dis- not to exceed 0.093 milligram per tilled water at 21 °C (70 °F) for 48 hours square centimeter (0.6 milligram per yields total extractives not to exceed square inch) of food contact surface as 0.0047 milligram per square centimeter determined by a method entitled ‘‘Ana- (0.03 milligram per square inch) of lytical Method of Determining the food-contact surface. Amount of EVOH in the Extractives (2) The film when extracted with 50 Residue of EVOH Film,’’ dated March percent ethyl alcohol at 21 °C (70 °F) for 23, 1987, as developed by the Kuraray 48 hours yields total extractives not to Co., Ltd., which is incorporated by ref- exceed 0.0062 milligram per square cen- erence in accordance with 5 U.S.C. timeter (0.04 milligram per square 552(a) and 1 CFR part 51. Copies may be inch) of food-contact surface. obtained from the Office of Premarket (c) The finished food-contact article Approval (HFS–200), Center for Food shall not exceed 0.0076 centimeter (0.003 Safety and Applied Nutrition, Food and inch) thickness and shall contact foods Drug Administration, 200 C St. SW., only of the types identified in table 1 of Washington, DC 20204, or may be exam- § 176.170(c) of this chapter in Categories ined at the Center for Food Safety and III, IV–A, VII–A, and IX under condi- Applied Nutrition’s Library, 200 C St. tions of use F and G described in table SW., rm. 3321, Washington, DC, or at 2 of § 176.170(c) of this chapter. Film the Office of the Federal Register, 800 samples of 0.0076 centimeter (0.003 inch) North Capitol St. NW., suite 700, Wash- thickness representing the finished ar- ington, DC. ticles shall meet the following extrac- (e) The provisions of this section are tive limitation when tested by ASTM not applicable to ethylene-vinyl ace- method F34–76 (Reapproved 1980), tate-vinyl alcohol copolymers used in ‘‘Standard Test Method for Liquid Ex- the food-packaging adhesives com- traction of Flexible Barrier Materials,’’ plying with § 175.105 of this chapter. which is incorporated by reference. The availability of this incorporation by [47 FR 41531, Sept. 21, 1982, as amended at 49 reference is given in paragraph (b) of FR 10108, Mar. 19, 1984; 65 FR 17135, Mar. 31, this section. The film when extracted 2000] with n-heptane at 38 °C (100 °F) for 30 § 177.1380 Fluorocarbon resins. minutes yields total extractives not to exceed 0.0078 milligram per square cen- Fluorocarbon resins may be safely timeter (0.05 milligram per square used as articles or components of arti- inch) of food-contact surface, after cor- cles intended for use in contact with recting the total extractives by divid- food, in accordance with the following ing by a factor of five. prescribed conditions: (d) The finished food-contact article (a) For the purpose of this section, shall not exceed 0.018 centimeter (0.007 fluorocarbon resins consist of basic res- inch) thickness and may contact all ins produced as follows: foods, except those containing more (1) Chlorotrifluoroethylene resins than 8 percent alcohol, under condi- produced by the homopolymerization tions of use B through H described in of chlorotrifluoroethylene.
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(2) Chlorotrifluoroethylene-1,1- articles or components of articles that difluoroethylene copolymer resins pro- are intended for repeated use in con- duced by copolymerization of tact with food. chlorotrifluoroethylene and 1,1- (3) In accordance with current good difluoroethylene. manufacturing practice, those food- (3) Chlorotrifluoroethylene-1,1- contact articles intended for repeated difluoroethylene-tetrafluoroethylene use shall be thoroughly cleansed prior co-polymer resins produced by co- to their first use in contact with food. polymerization of (c) Extractives limitations are appli- chlorotrifluoroethylene, 1,1- cable to the basic resins in the form of difluoroethylene, and tetrafluoro- pellets that have been ground or cut ethylene. into small particles that will pass (4) Ethylene-chlorotrifluoroethylene through a U.S. Standard Sieve No. 6 copolymer resins produced by copolym- and that will be held on a U.S. Stand- erization of nominally 50 mole percent ard Sieve No. 10. of ethylene and 50 mole percent of (1) A 100-gram sample of the resin chlorotrifluoroethylene. The copoly- pellets, when extracted with 100 milli- mer shall have a melting point of 239 to liters of distilled water at reflux tem- ° 243 C and a melt index of less than or perature for 8 hours, shall yield total equal to 20 as determined by ASTM extractives not to exceed 0.003 percent Method D 3275–89 ‘‘Standard Specifica- by weight of the resins. tion for E–CTFE–Fluoroplastic Mold- (2) A 100-gram sample of the resin ing, Extrusion, and Coating Mate- pellets, when extracted with 100 milli- rials,’’ which is incorporated by ref- liters of 50 percent (by volume) ethyl erence in accordance with 5 U.S.C. alcohol in distilled water at reflux 552(a) and 1 CFR part 51. Copies may be temperature for 8 hours, shall yield obtained from the American Society total extractives not to exceed 0.003 for Testing and Materials, 1916 Race percent by weight of the resins. St., Philadelphia, PA 19013, or may be (3) A 100-gram sample of the resin examined at the Office of the Federal pellets, when extracted with 100 milli- Register, 800 North Capitol Street, liters of n-heptane at reflux tempera- NW., suite 700, Washington, DC. ture for 8 hours, shall yield total ex- (b) Fluorocarbon resins that are iden- tractives not to exceed 0.01 percent by tified in paragraph (a) of this section weight of the resins. and that comply with extractive limi- tations prescribed in paragraph (c) of [42 FR 14572, Mar. 15, 1977, as amended at 57 this section may be used as articles or FR 185, Jan. 3, 1992] components of articles intended for use in contact with food as follows: § 177.1390 Laminate structures for use ≥ (1) Fluorocarbon resins that are iden- at temperatures of 250 F and tified in paragraphs (a)(1), (a)(2), and above. (a)(3) of this section and that comply (a) The high-temperature laminates only with the extractive limitations identified in this section may be safely prescribed in paragraphs (c)(1) and used for food contact at temperatures (c)(2) of this section may be used when not exceeding 135 °C (275 °F) unless oth- such use is limited to articles or com- erwise specified. These articles are lay- ponents of articles that are intended ered constructions that are optionally for repeated use in contact with food or bonded with adhesives. The interior that are intended for one-time use in (food-contact) layer(s) may be sepa- contact with foods only of the types rated from the exterior layer(s) by a identified in § 176.170(c) of this chapter, functional barrier, such as aluminum table 1, under Types I, II, VI, VII–B, foil. Upon review of the physical prop- and VIII. erties of a particular construction, the (2) Fluorocarbon resins that are iden- Food and Drug Administration may tified in paragraph (a)(4) of this section consider other layers to serve as func- and that comply with the extractive tional barriers. This regulation is not limitations prescribed in paragraphs intended to limit these constructions (c)(1) and (c)(2) of this section may be as to shape, degree of flexibility, thick- used only when such use is limited to ness, or number of layers. These layers
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may be laminated, extruded, co- thorized food-contact materials yield extruded, or fused. no more than 0.15 milligrams of epsilon- (b) When containers subject to this caprolactam and 0.04 milligrams of regulation undergo heat sterilization omega-laurolactam per square inch to produce shelf-stable foods, certain when extracted with 95 percent ethanol control measures (in addition to the at 121 °C (250 °F) for 2 hours. food additive requirements in para- (ii) Adjuvants used in these layers graphs (c) and (d) of this section) are must comply with an applicable regu- necessary to ensure proper food steri- lation that permits food type and time/ lization and package integrity. Refer temperature conditions to which the to parts 108, 110, 113, and 114 of this container will be exposed, including chapter for details. sterilization processing. (c) Subject to the provisions of this (2) Adhesives. The use of adhesives in paragraph, food-contact articles pro- these containers is optional. Adhesives duced from high-temperature lami- may be formulated from the following nates may be safely used to package all substances, subject to the prescribed food types except those containing limitations: more than 8 percent ethyl alcohol. (i) Any substance suitable for use in (1) Polymeric films/layers. Films or lay- formulating adhesives that complies ers not separated from food by a func- with an applicable regulation of this tional barrier must meet the following chapter which permits food type and requirements: time/temperature conditions to which (i) Films/layers may consist of the the container will be exposed, includ- following: ing sterilization processing. (a) Polyolefin resins complying with (ii) Substances complying with item 2.2 or 3.2 of the table in § 175.105 of this chapter may be used in § 177.1520(c). these constructions, provided they are (b) Polymeric resin blends formu- separated from the interior (food-con- lated from a base polymer complying tact) layer(s) by a functional barrier as with item 2.2 or 3.2 of the table in discussed under paragraph (a) of this § 177.1520(c) blended with no more than section. 10 percent by weight of a copolymer of (iii) Maleic anhydride adduct of poly- ethylene and vinyl acetate complying propylene complying with § 175.300 of with § 177.1350. this chapter. (c) Polymeric resin blends formulated (iv) Polyester-urethane adhesive for from a base polymer complying with use at temperatures not exceeding 121 item 2.2 or 3.2 of the table in °C (250 °F) and formulated from the fol- § 177.1520(c) blended with no more than lowing: 38 percent by weight of a homopolymer (a) Polyester-urethanediol resin pre- of isobutylene complying with pared by the reaction of a mixture of § 177.1420(a)(1). polybasic acids and polyhydric alcohols (d) Polyethylene phthalate resins listed in § 175.300(b)(3)(vii) of this chap- complying with § 177.1630(e)(4) (i) and ter, 3-isocyanatomethyl-3,5,5- (ii). trimethylcyclohexyl isocyanate (CAS (e) Nylon MXD–6 resins that comply Reg. No. 4098–71–9) and optional with item 10.3 of the table in trimethoxysilane coupling agents con- § 177.1500(b) of this chapter when ex- taining amino, epoxy, ether, and/or tracted with water and heptane under mercapto groups not to exceed 3 per- the conditions of time and temperature cent by weight of the cured adhesive. specified for condition of use A, as set (b) Urethane cross-linking agent forth in Table 2 of § 176.170(c) of this comprising not more than 25 percent chapter. by weight of the cured adhesive and (f) Nylon 6⁄12 resins (CAS Reg. No. formulated from 3-isocyanatomethyl- 25191–04–2) complying with item 13.3 of 3,5,5-trimethylcyclohexyl isocyanate the table in § 177.1500(b), for use as (CAS Reg. No. 4098–71–9) adduct of nonfood-contact layers of laminated trimethylol propane (Cas Reg. No. 77– films and in rigid multilaminate con- 99–6) and/or 1,3-bis(isocyanatomethyl) structions with polypropylene outer benzene (CAS Reg. No. 25854–16–4) layers. Laminate structures with au- adduct of trimethylol propane.
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(v) Polyester-epoxy-urethane adhe- scribed in Table I of § 176.170 of this sives formulated from the following: chapter, and formulated from the fol- (a) Polyester resin formed by the re- lowing mixture: action of polybasic acids and (a)(1) Polyesterpolyurethanediol res- polyhydric alcohols listed in ins prepared by the reaction of a mix- § 175.300(b)(3)(vii) of this chapter. Aze- ture of polybasic acids and polyhydric laic acid may also be used as a alcohols listed in § 175.300(b)(3)(vii) of polybasic acid. this chapter and 3-isocyanatomethyl- (b) Epoxy resin listed in 3,5,5-trimethylcyclohexyl isocyanate § 175.300(b)(3)(viii)(a) of this chapter and (CAS Reg. No. 4098–71–9). Additionally, comprising no more than 30 percent by dimethylol propionic acid and 1,6- weight of the cured adhesive. hexanediol may be used alone or in (c) Urethane cross-linking agent com- combination as reactants in lieu of a prising no more than 14 percent weight polybasic acid and a polyhydric alco- of the cured adhesive and formulated hol. from 3-isocyanatomethyl-3,5.5- (2) Acid dianhydride formulated from trimethylcyclohexyl isocyanate 3a,4,5,7a-tetrahydro-7-methyl-5- cyanurate (CAS Reg. No. 53880–05–0). (tetrahydro-2,5-dioxo-3-furanyl)-1,3- (vi) Polyurethane-polyester resin- isobenzofurandione (CAS Reg. No. epoxy adhesives formulated from the 73003–90–4), comprising not more than following mixture: one percent of the cured adhesive. (a)(1) Polyester-polyurethanediol res- (b) Urethane cross-linking agent, ins prepared by the reaction of a mix- comprising not more than twelve per- ture of polybasic acids and polyhydric cent by weight of the cured adhesive, alcohols listed in § 175.300(b)(3)(vii) of and formulated from trimethylol pro- this chapter and 3-isocyanatomethyl- pane (CAS Reg. No. 77–99–6) adducts of 3,5,5-trimethylcyclohexyl isocyanate 3-isocyanatomethyl-3,5,5- (CAS Reg. No. 4098–71–9). trimethylcyclohexyl isocyanate (CAS (2) Polyester resin formed by the re- Reg. No. 4098–71–9) and/or 1,3- action of polybasic acids and bis(isocyanatomethyl)benzene (CAS polyhydric alcohols listed in Reg. No. 363–48–31). § 175.300(b)(3)(vii) of this chapter. Addi- (3) Test specifications. These specifica- tionally, azelaic acid and 1,6- tions apply only to materials on the hexanediol may also be used as food-contact side of a functional bar- reactants in lieu of a polyhydric alco- rier, if present. All tests must be per- hol. formed on containers made under pro- (3) Epoxy resin listed in duction conditions. Laminated struc- § 175.300(b)(3)(viii)(a) of this chapter and tures submitted to extraction proce- comprising not more than 5 percent by dures must maintain complete struc- weight of the cured adhesive. tural integrity (particularly with re- (4) Optional trimethoxy silane curing gard to delamination) throughout the agents, containing amino, epoxy, ether, test. or mercapto groups not in excess of 3 (i) Nonvolatile extractives. (a) For use percent of the cured adhesive. at temperatures not to exceed 121 °C (b) Urethane cross-linking agent, (250 °F): The container interior (food- comprising not more than 20 percent contact side) shall be extracted with by weight of the cured adhesive, and deionized distilled water at 121 °C (250 formulated from trimethylol propane °F) for 2 hours. (CAS Reg. No. 77–99–6) adducts of 3– (1) The chloroform-soluble fraction of isocyanatomethyl–3,5,5– the total nonvolatile extractives for trimethylcyclohexyl isocyanate (CAS containers using adhesives listed in Reg. No. 4098–71–9) or 1,3- paragraphs (c)(2)(i), (c)(2)(ii), (c)(2)(iii), bis(isocyanatomethyl)benzene (CAS (c)(2)(iv), and (c)(2)(vii) of this section Reg. No. 25854–16–4). shall not exceed 0.0016 milligram per (vii) Polyester-polyurethane resin- square centimeter (0.01 milligram per acid dianhydride adhesives for use at square inch) as determined by a meth- temperatures not to exceed 121 °C (250 od entitled ‘‘Determination of Non- °F), in contact only with food Types I, Volatile Chloroform Soluble Residues II, VIA, VIB, VIIB, and VIII as de- in Retort Pouch Water Extracts,’’
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which is incorporated by reference. paragraph (c)(2)(vi) of this section shall Copies are available from the Center not exceed 0.008 milligram per square for Food Safety and Applied Nutrition centimeter (0.05 milligram per square (HFS–200), Food and Drug Administra- inch) as determined by a method enti- tion, 200 C St. SW., Washington, DC tled, ‘‘Determination of Non-volatile 20204, and may be examined at the Cen- Chloroform Soluble Residues in Retort ter for Food Safety and Applied Nutri- Pouch Water Extracts,’’ which is incor- tion’s Library, 200 C St. SW., rm. 3321, porated by reference in paragraph Washington, DC, or at the Office of the (c)(3)(i)(a)(1) of this section. Federal Register, 800 North Capitol St. (ii) Volatiles. Volatile substances em- NW., suite 700, Washington, DC 20408. ployed in the manufacture of high-tem- (2) The chloroform-soluble fraction of perature laminates must be removed to the total nonvolatile extractives for the greatest extent possible in keeping containers using adhesives listed in with good manufacturing practice pre- paragraph (c)(2)(v) of this section shall scribed in § 174.5(a) of this chapter. not exceed 0.016 milligram per square (d) Nylon 12/aluminum foil high-tem- centimeter (0.10 milligram per square perature laminates: Subject to the pro- inch) as determined by a method titled visions of this paragraph, containers ‘‘Determination of Non-volatile Chlo- constructed of nylon 12 laminated to roform Soluble Residues in Retort aluminum foil may be safely used at Pouch Water Extracts,’’ which is incor- temperatures no greater than 250 °F porated by reference in paragraph (121 °C) in contact with all food types (c)(3)(i)(a)(1) of this section. except those containing more than 8 (b) For use at temperatures not to ex- percent alcohol. ceed 135 °C (275 °F): The container inte- (1) The container is constructed of rior (food-contact side) shall be ex- aluminum foil to which nylon 12 film is tracted with deionized distilled water fused. Prior to fusing the nylon 12, the at 135 °C (275 °F) for 1 hour. aluminum foil may be optionally (1) The chloroform-soluble fraction of precoated with a coating complying the total nonvolatile extractives for with § 175.300 of this chapter. containers using no adhesive, or adhe- (2) Nylon 12 resin complying with sives listed in paragraphs (c)(2) (i), (ii), § 177.1500 and having an average thick- and (iii) of this section shall not exceed ness not to exceed 0.0016 inch (41 mi- 0.0020 milligram per square centimeter crons) may be used as the food-contact (0.013 milligram per square inch) as de- surface of the container. termined by a method titled ‘‘Deter- (3) Container test specifications. On mination of Non-volatile Chloroform exposure to distilled water at 250 °F Soluble Residues in Retort Pouch (121 °C) for 2 hours, extractives from Water Extracts,’’ which is incorporated the food-contact side of the nylon 12 by reference. The availability of this multilayered construction shall not ex- incorporation by reference is given in ceed 0.05 milligram per square inch paragraph (c)(3)(i)(a)(1) of this section. (0.0078 milligram per square centi- (2) The chloroform-soluble fraction of meter) as total nonvolatile extractives. the total nonvolatile extractives for containers using adhesives listed in [45 FR 2843, Jan. 15, 1980, as amended at 47 paragraph (c)(2)(v) of this section shall FR 49639, Nov. 2, 1982; 48 FR 236, Jan. 4, 1983; not exceed 0.016 milligram per square 48 FR 15242, Apr. 8, 1983; 48 FR 17347, Apr. 22, 1983; 49 FR 7558, Mar. 1, 1984; 52 FR 33575, centimeter (0.10 milligram per square Sept. 4, 1987; 53 FR 39084, Oct. 5, 1988; 54 FR inch) as determined by a method titled 24898, June 12, 1989; 61 FR 14481, Apr. 2, 1996; ‘‘Determination of Non-volatile Chlo- 63 FR 55943, Oct. 20, 1998; 64 FR 4785, Feb. 1, roform Soluble Residues in Retort 1999; 64 FR 46272, Aug. 25, 1999] Pouch Water Extracts,’’ which is incor- porated by reference. The availability § 177.1395 Laminate structures for use of this incorporation by reference is at temperatures between 120 ≥F and ≥ given in paragraph (c)(3)(i)(a)(1) of this 250 F. section. (a) The laminates identified in this (3) The chloroform-soluble fraction of section may be safely used at the speci- the total nonvolatile extractives for fied temperatures. These articles are containers using adhesives listed in layered structures that are optionally
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bonded with adhesives. In these arti- Substances Limitations cles, the food-contact layer does not Nylon 6/66 resins complying For use only with: function as a barrier to migration of with ¤ 177.1500(b), item 4.2 1. Nonalcoholic foods at components from non-food-contact lay- of this chapter (CAS Reg. temperatures not to ex- ers. The layers may be laminated, ex- 24993Ð04Ð2). ceed 82.2 cC (180 cF). Laminate structures with truded, coextruded, or fused. authorized food-contact (b) Laminate structures may be man- materials yield no more ufactured from: than 0.15 milligram of ep- silon-caprolactam per (1) Polymers and adjuvants com- square inch when ex- plying with § 177.1390 of this chapter. tracted with water at 82.2 cC (180 cF) for 5 hours. (2) Any polymeric resin listed in 2. Nonalcoholic foods at these regulations so long as the use of temperatures not to ex- the resin in the structure complies ceed 100 cC (212 cF). Laminate films with au- with the conditions of use (food type thorized food-contact ma- and time/temperature) specified in the terials yield no more than regulation for that resin. 0.15 milligram of epsilon- caprolactam per square (3) Optional adjuvant substances used inch when extracted with in accordance with § 174.5 of this chap- water at 100 cC (212 cF) ter. for 5 hours. Nylon 6/69 resins complying For use with nonalcoholic (4) The following substances in non- with ¤ 177.1500(b), item 14, foods under conditions of food-contact layers only: of this chapter (CAS Reg. use B, C, D, E, F, G, and No. 51995Ð62Ð1). H described in table 2 of Substances Limitations ¤ 176.170 of this chapter. Laminate structures with Ethylene/1,3Ðphenylene oxy- For use only with poly- authorized food-contact ethylene isophthalate/ ethylene terephthalate as materials may contain terephthalate copolymer the food-contact layer, nylon 6/69 resins pro- (CAS Reg. No. 87365Ð98Ð8) complying with vided that the nitrogen complying with ¤ 177.1345. ¤ 177.1630 under condi- content of aqueous ex- tions of use C through G tracts of a representative laminate (obtained at 100 described in table 2 of ° ° ¤ 176.170(c) of this chap- C (212 F) for 8 hours) ter. Laminate structures, does not exceed 15 when extracted with 8 micrograms per square percent ethanol at 150 °F centimeter (100 for 2 hours shall not yield micrograms per square m-pheny lenedioxy-O,O′- inch). diethyl isophthalate or cy- clic bis(ethylene [52 FR 33575, Sept. 4, 1987, as amended at 53 isophthalate) in excess of 7.8 micrograms/square FR 19772, May 31, 1988; 57 FR 43399, Sept. 21, decimeter (0.5 1992; 58 FR 32610, June 11, 1993; 62 FR 53957, microgram/square inch) of Oct. 17, 1997] food-contact surface. Nylon 6/12 resins complying For use with nonalcoholic § 177.1400 Hydroxyethyl cellulose film, with ¤ 177.1500(b), item foods at temperatures not water-insoluble. 13.2, of this chapter (CAS to exceed 100 °C (212 Reg. No. 25191Ð04Ð2). °F). Laminate structures Water-insoluble hydroxyethyl cel- with authorized food-con- lulose film may be safely used for tact materials yield no packaging food in accordance with the more than 0.15 milligram of epsilon-caprolactam following prescribed conditions: and 0.04 milligram of (a) Water-insoluble hydroxyethyl cel- omega-laurolactam per lulose film consists of a base sheet square inch when ex- manufactured by the ethoxylation of tracted with water at 100 °C (212 °F) for 5 hours. cellulose under controlled conditions, to which may be added certain optional substances of a grade of purity suitable for use in food packaging as constitu- ents of the base sheet or as coatings applied to impart desired technological properties. (b) Subject to any limitations pre- scribed in parts 170 through 189 of this chapter, the optional substances used
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in the base sheet and coating may in- molar percent of isoprene such that the clude: finished polymers have a molecular (1) Substances generally recognized weight of 300,000 (Flory) or higher. as safe in food. (3) Chlorinated isobutylene-isoprene (2) Substances permitted to be used copolymers produced when in water-insoluble hydroxyethyl cel- isobutylene-isoprene copolymers (mo- lulose film by prior sanction or ap- lecular weight 300,000 (Flory) or higher) proval and under conditions specified are modified by chlorination with not in such sanctions or approval, and sub- more than 1.3 weight-percent of chlo- stances listed in part 181, subpart B of rine. this chapter. (b) The polymers identified in para- (3) Substances that by any regulation graph (a) of this section may contain promulgated under section 409 of the optional adjuvant substances required act may be safely used as components in the production of the polymers. The of water-insoluble hydroxyethyl cel- optional adjuvant substances required lulose film. in the production of the polymers may (4) Substances identified in and used include substances generally recog- in compliance with § 177.1200(c). nized as safe in food, substances used in (c) Any substance employed in the accordance with a prior sanction or ap- production of the water-insoluble hy- proval, and aluminum chloride. droxyethyl cellulose film described in (c) The provisions of this section are this section that is the subject of a reg- not applicable to polyisobutylene used ulation in parts 174, 175, 176, 177, 178 in food-packaging adhesives complying and § 179.45 of this chapter conforms with § 175.105 of this chapter. with any specification in such regula- tion. § 177.1430 Isobutylene-butene copoly- mers. § 177.1420 Isobutylene polymers. Isobutylene-butene copolymers iden- Isobutylene polymers may be safely tified in paragraph (a) of this section used as components of articles in- may be safely used as components of tended for use in producing, manufac- articles intended for use in contact turing, packing, processing, preparing, with food, subject to the provisions of treating, packaging, transporting, or this section. holding food, in accordance with the (a) For the purpose of this section, following prescribed conditions: isobutylene-butene copolymers consist (a) For the purpose of this section, of basic copolymers produced by the isobutylene polymers are those pro- copolymerization of isobutylene with duced as follows: mixtures of n-butenes such that the (1) Polyisobutylene produced by the finished basic copolymers contain not homopolymerization of isobutylene less than 45 weight percent of polymer such that the finished polymers have a units derived from isobutylene and molecular weight of 750,000 (Flory) or meet the specifications prescribed in higher. paragraph (b) of this section when test- (2) Isobutylene-isoprene copolymers ed by the methods described in para- produced by the copolymerization of graph (c) of this section. isobutylene with not more than 3 (b) Specifications:
Maximum Isobutylene-butene copolymers Molecular Viscosity (range) bromine weight (range) value
1. Used as release agents in petroleum wax complying with 300 to 5,000 ... 40 to 20,000 seconds 40 ¤ 178.3710 of this chapter. Saybolt at 200 °F. 2. Used as plasticizers in polyethylene or polypropylene complying 300 to 5,000 ... 40 to 20,000 seconds 40 with ¤ 177.1520, and in polystyrene complying with ¤ 177.1640. Saybolt at 200 °F. 3. Used as components of nonfood articles complying with 300 to 5,000 ... 40 to 20,000 seconds 40 ¤¤ 175.300, 176.170, 176.210, 177.2260(d)(2), 177.2800, and Saybolt at 200 °F. 178.3570 (provided that addition to food does not exceed 10 parts per million), or ¤ 176.180 of this chapter. 4. Used as production aids in the manufacture of expanded 150 to 5,000 ... Less than 20,000 seconds 90. (foamed) polystyrene articles complying with ¤ 177.1640 of this Saybolt at 200 °F. chapter.
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Maximum Isobutylene-butene copolymers Molecular Viscosity (range) bromine weight (range) value
5. Used in release coatings on backings or linings for pressure-sen- 150 to 5,000 ... Less than 20,000 seconds 90 sitive adhesive labels complying with ¤ 175.125 of this chapter. Saybolt at 200 °F.
(c) The analytical methods for deter- preparing, treating, packaging, trans- mining whether isobutylene-butene co- porting, or holding food in accordance polymers conform to the specifications with the following prescribed condi- in paragraph (b) are as follows: tions: (1) Molecular weight. Molecular (a) 4,4′-Isopropylidenediphenol-ep- weight shall be determined by Amer- ichlorohydrin resins consist of basic ican Society for Testing and Materials resins produced by the condensation of (ASTM) method D2503–82, ‘‘Standard equimolar amounts of 4,4′- Test Method for Molecular Weight isopropylidenediphenol and (Relative Molecular Mass) of Hydro- epichlorohydrin terminated with phe- carbons by Thermoelectric Measure- nol, to which may have been added cer- ment of Vapor Pressure,’’ which is in- tain optional adjuvant substances re- corporated by reference. Copies may be quired in the production of the resins. obtained from the American Society (b) The optional adjuvant substances for Testing Materials, 1916 Race St., required in the production of the resins Philadelphia, PA 19103, or may be ex- may include substances generally rec- amined at the Office of the Federal ognized as safe in food, substances used Register, 800 North Capitol Street, in accordance with a prior sanction or NW., suite 700, Washington, DC 20408. approval, and the following: (2) Viscosity. Viscosity shall be deter- mined by ASTM method D445–74, ‘‘Test List of substances Limitations for Kinematic Viscosity of Transparent Butyl alcohol ...... Not to exceed 300 p.p.m. as re- and Opaque Liquids,’’ which is incor- sidual solvent in finished resin. porated by reference. The availability Ethyl alcohol. of this incorporation by reference is Toluene ...... Not to exceed 1,000 p.p.m. as re- given in paragraph (c)(1) of this sec- sidual solvent in finished resin. tion. (3) Maximum bromine value. Maximum (c) 4,4′-Isopropylidenediphenol-ep- bromine value shall be determined by ichlorohydrin resins shall meet the fol- ASTM method D1492–78, ‘‘Standard lowing nonvolatile extractives limita- Test Method for Bromine Index of Aro- tions: matic Hydrocarbons by Coulometric (1) Maximum extractable nonvolatile Titration,’’ which is incorporated by fraction of 2 parts per million when ex- reference. The availability of this in- tracted with distilled water at 70 °C for corporation by reference is given in 2 hours, using a volume-to-surface paragraph (c)(1) of this section. ratio of 2 milliliters per square inch. (d) The provisions of this section are (2) Maximum extractable nonvolatile not applicable to isobutylene-butene fraction of 3 parts per million when ex- copolymers used as provided under tracted with n-heptane at 70 °C for 2 § 175.105 of this chapter. hours, using a volume-to-surface ratio of 2 milliliters per square inch. [52 FR 11641, Apr. 10, 1987, as amended at 63 FR 36175, July 2, 1998] (3) Maximum extractable nonvolatile fraction of 6 parts per million when ex- § 177.1440 4,4′-Isopropylidenediphenol- tracted with 10 percent (by volume) epichlorohydrin resins minimum ethyl alcohol in distilled water at 70 °C molecular weight 10,000. for 2 hours, using a volume-to-surface 4,4′-Isopropylidenediphenol-epichlo- ratio of 2 milliliters per square inch. rohydrin resins having a minimum mo- (d) The provisions of this section are lecular weight of 10,000 may be safely not applicable to 4,4′-isopropylidene- used as articles or components of arti- diphenol-epichlorohydrin resins listed cles intended for use in producing, in other sections of subchapter B of manufacturing, packing, processing, this chapter.
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§ 177.1460 Melamine-formaldehyde res- basic copolymers produced by the graft ins in molded articles. copolymerization of 73–77 parts by Melamine-formaldehyde resins may weight of acrylonitrile and 23–27 parts be safely used as the food-contact sur- by weight of methyl acrylate in the face of molded articles intended for use presence of 8–10 parts by weight of bu- in producing, manufacturing, packing, tadiene-acrylonitrile copolymers con- processing, preparing, treating, pack- taining approximately 70 percent by aging, transporting, or holding food in weight of polymer units derived from accordance with the following pre- butadiene. scribed conditions: (b) The nitrile rubber modified acry- (a) For the purpose of this section, lonitrile-methyl acrylate basic copoly- melamine-formaldehyde resins are mers meet the following specifications those produced when 1 mole of mel- and extractives limitations: amine is made to react with not more (1) Specifications. (i) Nitrogen content than 3 moles of formaldehyde in water is in the range 16.5–19 percent as deter- solution. mined by Kjeldahl analysis. (b) The resins may be mixed with re- (ii) Intrinsic viscosity in acetonitrile fined woodpulp and the mixture may at 25 °C is not less than 0.29 deciliter contain other optional adjuvant sub- per gram as determined by ASTM stances which may include the fol- method D1243–79, ‘‘Standard Test Meth- lowing: od for Dilute Solution Viscosity of Vinyl Chloride Polymers,’’ which is in- List of substances Limitations corporated by reference. Copies may be Colorants used in accord- obtained from the American Society ance with ¤ 178.3297 for Testing Materials, 1916 Race St., of this chapter. Dioctyl phthalate ...... For use as lubricant. Philadelphia, PA 19103, or may be ex- Hexamethylenetetramine For use only as polymerization amined at the Office of the Federal reaction control agent. Register, 800 North Capitol Street, Phthalic acid anhydride .. Do. Zinc stearate ...... For use as lubricant. NW., suite 700, Washington, DC 20408. (iii) Residual acrylonitrile monomer (c) The molded melamine-formalde- content is not more than 11 parts per hyde articles in the finished form in million as determined by gas chroma- which they are to contact food, when tography. extracted with the solvent or solvents (iv) Acetonitrile-soluble fraction characterizing the type of food and after refluxing the base polymer in ace- under the conditions of time and tem- tonitrile for 1 hour is not greater than perature as determined from tables 1 95 percent by weight of the basic co- and 2 of § 175.300(d) of this chapter, polymers. shall yield net chloroform-soluble ex- (2) Extractives limitations. The fol- tractives not to exceed 0.5 milligram lowing extractive limitations are de- per square inch of food-contact surface. termined by an infrared [42 FR 14572, Mar. 15, 1977, as amended at 56 spectrophotometric method titled, ‘‘In- FR 42933, Aug. 30, 1991] frared Spectrophotometric Determina- tion of Polymer Extracted from Borex § 177.1480 Nitrile rubber modified ac- 210 Resin Pellets,’’ which is incor- rylonitrile-methyl acrylate copoly- porated by reference. Copies are avail- mers. able from the Center for Food Safety Nitrile rubber modified acrylonitrile- and Applied Nutrition (HFS–200), Food methyl acrylate copolymers identified and Drug Administration, 200 C St. in this section may be safely used as SW., Washington, DC 20204, or available components of articles intended for for inspection at the Office of the Fed- food-contact use under conditions of eral Register, 800 North Capitol Street, use D, E, F, or G described in table 2 of NW., suite 700, Washington, DC 20408, § 176.170(c) of this chapter, subject to and are applicable to the basic copoly- the provisions of this section. mers in the form of particles of a size (a) For the purpose of this section, that will pass through a U.S. standard nitrile rubber modified acrylonitrile- sieve No. 6 and that will be held on a methyl acrylate copolymers consist of U.S. standard sieve No. 10:
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(i) Extracted copolymer not to ex- (6) Nylon 6 resins are manufactured ceed 2.0 parts per million in aqueous by the polymerization of epsilon- extract obtained when a 100-gram sam- caprolactam. ple of the basic copolymers is extracted (7) Nylon 66T resins are manufac- with 250 milliliters of demineralized tured by the condensation of (deionized) water at reflux temperature hexamethyl-enediamine, adipic acid, for 2 hours. and terephthalic acid such that com- (ii) Extracted copolymer not to ex- position in terms of ingredients is ceed 0.5 part per million in n-heptane 43.1±0.2 weight percent hexamethyl- extract obtained when a 100-gram sam- enediamine, 35.3±1.2 weight percent ple of the basic copolymers is extracted adipic acid, and 21.6±1.2 weight percent with 250 milliliters of reagent grade n- terephthalic acid. heptane at reflux temperature for 2 (8) Nylon 612 resins are manufactured hours. by the condensation of hexamethylenediamine and (c) Acrylonitrile copolymers identi- dodecanedioic acid. fied in this section shall comply with (9) Nylon 12 resins are manufactured the provisions of § 180.22 of this chap- by the condensation of omega- ter. laurolactam. (d) Acrylonitrile copolymers identi- (10)(i) Impact modified Nylon MXD–6 fied in this section are not authorized resins (CAS Reg. No. 59655–05–9) manu- to be used to fabricate beverage con- factured by the condensation of adipic tainers. acid, 1,3-benzenedimethanamine, and [42 FR 14572, Mar. 15, 1977, as amended at 42 T3alpha-(3-aminopropyl)-omega-(3- FR 48544, Sept. 23, 1977; 47 FR 11843, Mar. 19, amino-propoxy)poly- oxyethylene 1982; 47 FR 16775, Apr. 20, 1982; 49 FR 10109, under such conditions that the alpha- Mar. 19, 1984; 54 FR 24898, June 12, 1989; 61 FR (3-amino-propyl)-omega-(3- 14481, Apr. 2, 1996] aminopropoxy) polyoxyethylene mon- omer content does not exceed 7 percent § 177.1500 Nylon resins. by weight of the finished resin. The nylon resins listed in paragraph (ii) Nylon MXD–6 resins (CAS Reg. (a) of this section may be safely used to No. 25718–70–1) manufactured by the produce articles intended for use in condensation of adipic acid and 1,3- processing, handling, and packaging benzenedimethanamine. food, subject to the provisions of this (11) Nylon 12T resins are manufac- section: tured by the condensation of omega- (a) The nylon resins are manufac- laurolactam (CAS Reg. No. 0947–04–6), tured as described in this paragraph so isophthalic acid (CAS Reg. No. 0121–91– as to meet the specifications prescribed 5), and bis(4-amino-3-methylcycl- in paragraph (b) of this section when ohexyl)methane (CAS Reg. No. 6864–37– 5) such that the composition in terms tested by the methods described in ± paragraph (c) of this section. of ingredients is 34.4 1.5 weight percent omega-laurolactam, 26.8±0.4 weight per- (1) Nylon 66 resins are manufactured cent isophthalic acid, and 38.8±0.5 by the condensation of hexamethylene- weight percent bis(4-amino-3- diamine and adipic acid. methylcyclohexyl)-methane. (2) Nylon 610 resins are manufactured (12) Nylon 6I/6T resins (CAS Reg. No. by the condensation of hexamethylene- 25750–23–6) are manufactured by the diamine and sebacic acid. condensation of (3) Nylon 66/610 resins are manufac- hexamethylenediamine, terephthalic tured by the condensation of equal- acid, and isophthalic acid such that 65 weight mixtures of nylon 66 salts and to 80 percent of the polymer units are nylon 610 salts. derived from hexamethylene (4) Nylon 6/66 resins manufactured by isophthalamide. the condensation and polymerization of (13)(i) Nylon 6/12 resins (CAS Reg. No. Nylon 66 salts and epsilon-caprolactam. 25191–04–2) are manufactured by the co- (5) Nylon 11 resins are manufactured polymerization of a 1 to 1 ratio by by the condensation of 11- weight of epsilon-caprolactam and aminoundecanoic acid. omega-laurolactam.
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(ii) Nylon 6/12 resins (CAS Reg. No. (15) Nylon 46 resins (CAS Reg. No. 25191–04–2) are manufactured by the co- 50327–77–0) are manufactured by the polymerization of a ratio of at least 80 condensation of 1,4-butanediamine and weight percent of epsilon-caprolactam adipic acid. and no more than 20 weight percent of (16) Nylon resins PA 6–3–T (CAS Reg- omega-laurolactam. istry No. 26246–77–5) are manufactured (14) Nylon 6/69 resins (CAS Reg. No. by the condensation of 50 mol percent 51995–62–1) are manufactured by the 1,4-benzenedicarboxylic acid, dimethyl condensation of 49.5+0.5 weight percent ester and 50 mol percent of an equimolar mixture of 2,2,4-trimethyl- epsilon-caprolactam, 19.4+0.2 weight 1,6-hexanediamine and 2,4,4-trimethyl- percent hexamethylenediamine and 1,6-hexanediamine. 31.2+0.3 weight percent azelaic acid. (b) Specifications:
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(c) Nylon modifier—(1) Identity. Co- of Nylon modifiers listed in paragraph polyester-graft-acrylate copolymer is (c)(1) of this section may include: the substance 1,4-benzenedicarboxylic (A) Substances generally recognized acid, polymer with 1,4-butanediol, (E)- as safe for use in food and food pack- 2-butenedioic acid, 1,2-ethanediol, aging; ethyl 2-propenoate, hexanedioic acid (B) Substances subject to prior sanc- and 2-propenoic acid, graft (CAS Reg. tion or approval for use in Nylon resins No. 175419–23–5), and is derived from and used in accordance with such sanc- grafting of 25 weight percent of acrylic tions or approval; and polymer with 75 weight percent of co- (C) Optional substances required in polyester. The copolyester is polym- the production of the additive identi- erized terephthalic acid (55 mol%), fied in this paragraph and other op- adipic acid (40 mol%), and fumaric acid tional substances that may be required (5 mol%) with ethylene glycol (40 to accomplish the intended physical or mol%) and 1,4-butanediol (60 mol%). technical effect. The acrylic polymer is made from (d) Analytical methods—(1) Specific acrylic acid (70 mol%) and ethyl acry- gravity. Specific gravity shall be deter- late (30 mol%). mined by weighing a 1-gram to 5-gram (2) Specifications. The finished copoly- sample first in air and then in freshly ester-graft-acrylate copolymer shall boiled distilled water at 23 °C±2 °C. meet the following specifications: (2) Melting point. The melting point (i) Weight average molecular weight shall be determined as follows: Use a 15,000–35,000, hot-stage apparatus. The use of crossed nicol prisms with a microscope hot (ii) pH 7.2 to 8.2, and stage and reading of the thermometer (iii) Glass transition temperature –15 when the birefringence disappears in- c to –25 C. creases the accuracy. If the crossed (3) Conditions of use. (i) Copolyester- nicol apparatus is not available, use graft acrylate copolymer described in the lowest temperature at which the paragraph (c)(1) of this section is in- sample becomes transparent or the tended to improve the adhesive quali- sharp edges or corners of the sample ties of film. It is limited for use as a become rounded as the melting point. modifier of Nylon 6 and Nylon 6 modi- In case of doubt as to the onset of fied with Nylon MXD–6 at a level not melting, the sample is prodded with a to exceed 0.17 weight percent of the ad- sharp instrument. If it sticks to the ditive in the finished film. heating block, it is considered to have (ii) The finished film is used for pack- melted. If the melting point is low, dry aging, transporting, or holding all the sample in an oven at 85 °C for 24 types of foods under conditions of use B hours in a nitrogen atmosphere then through H, described in table 2 of repeat the test. § 176.170(c) of this chapter, except that (3) Solubility in boiling 4.2N HCl. The in the case of Nylon 6 films modified test shall be run on a sample approxi- with Nylon MXD–6 (complying with mately the size of a 1⁄8-inch cube in at § 177.1500, item 10.2), the use complies least 25 milliliters of 4.2 normal hydro- with the conditions of use specified in chloric acid. table 2. (4) Maximum extractable fraction in se- (iii) Extractives. Food contact films lected solvents. The procedure for deter- described in paragraphs (c)(1) of this mining the maximum extractable frac- section, when extracted with solvent or tion of the nylon resins in selected sol- solvents prescribed for the type of food vents is as follows: and under conditions of time and tem- (i) Film should be cut with ordinary perature specified for the intended use, scissors into pieces of a convenient size shall yield total extractives not to ex- such as 1⁄4-inch squares, for the extrac- ceed 0.5 milligram per inch squared of tion tests described in this section. The food-contact surface when tested by granules of nylon molding powders are the methods described in § 176.170(d) of in the proper form for the extraction this chapter. tests. Samples of fabricated articles (iv) Optional adjuvant substances. The such as pipe, fittings, and other similar substances employed in the production articles must be cut to approximately
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the size of the molding powder. This Copies are available from the Center can be done conveniently by using a for Food Safety and Applied Nutrition small-scale commercial plastics (HFS–200), Food and Drug Administra- granulator and cutting the sample tion, 200 C St. SW., Washington, DC through a screen having 1⁄4-inch mesh. 20204, or available for inspection at the Fine particles should be separated from Office of the Federal Register, 800 the cut resin by screening through a 20- North Capitol Street, NW., suite 700, mesh screen. The material retained on Washington, DC 20408. the screen is suitable for the extraction (ii) The viscosity number (VN) for tests. Nylon 6/69 and Nylon PA–6–3–T resins (ii) The organic solvents must be of in a 99 percent cresol solution (5 milli- American Chemical Society analytical grams resin per milliliter) shall be de- reagent grade; distilled water is used. termined at 25 °C (77 °F) by method ISO Approximately 30 grams of the pre- 307–1984(E), ‘‘Plastics-Polyamides-De- pared sample is weighed to the nearest termination of Viscosity Number,’’ milligram. The weighed resin is trans- which is incorporated by reference. The ferred to a 500-milliliter round-bottom availability of this incorporation by flask equipped with a reflux condenser. reference is given in paragraph (d)(5)(i) Approximately 300-milliliters of sol- of this section. vent is added to the flask and the con- tents refluxed gently for 8 hours with a [42 FR 14572, Mar. 15, 1977] heating mantle. The solvent is then fil- EDITORIAL NOTE: ForFEDERAL REGISTER ci- tered off immediately while still hot, tations affecting § 177.1500, see the List of using a Buchner funnel approximately CFR Sections Affected, which appears in the 5 inches in diameter, a suction flask, Finding Aids section of the printed volume and on GPO Access. and a hardened filter paper (Whatman No. 50 or equivalent). The paper is wet § 177.1520 Olefin polymers. with the solvent and a slight suction applied just before starting the filtra- The olefin polymers listed in para- tion. The resin is washed twice with graph (a) of this section may be safely approximately 100-milliliter portions of used as articles or components of arti- solvent and the combined filtrate and cles intended for use in contact with washings are reduced to approximately food, subject to the provisions of this 25 milliliters by evaporation at reduced section. pressure (50 millimeters to 100 millime- (a) For the purpose of this section, ters of mercury, absolute), heating as olefin polymers are basic polymers necessary. The contents of the flask manufactured as described in this para- are transferred to an evaporation dish graph, so as to meet the specifications (which has been held in a vacuum des- prescribed in paragraph (c) of this sec- iccator over anhydrous calcium sulfate tion, when tested by the methods de- until constant weight has been at- scribed in paragraph (d) of this section. tained) and carefully evaporated to (1)(i) Polypropylene consists of basic dryness. The weight of the solid residue polymers manufactured by the cata- is determined by difference after hold- lytic polymerization of propylene. ing in a vacuum desiccator over anhy- (ii) Propylene homopolymer consists drous calcium sulfate until constant of basic polymers manufactured by the weight has been attained. The percent catalytic polymerization of propylene of solids extracted is calculated by di- with a metallocene catalyst. viding the weight of the solid residue (2)(i) Polyethylene consists of basic by the weight of the sample and multi- polymers manufactured by the cata- plying by 100. lytic polymerization of ethylene. (5) Viscosity number (VN). (i) The vis- (ii) Fumaric acid-grafted poly- cosity number (VN) for Nylon 6/12 resin ethylene (CAS Reg. No. 26877–81–6) con- in a 96 percent sulfuric acid solution (5 sists of basic polymers manufactured milligrams resin per milliliter) shall be by the catalytic polymerization of determined at 25 °C (77 °F) by method ethylene followed by reaction with fu- ISO 307–1984(E), ‘‘Plastics-Polyamides- maric acid in the absence of free rad- Determination of Viscosity Number,’’ ical initiators. Such polymers shall which is incorporated by reference. contain grafted fumaric acid at levels
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not to exceed 2 percent by weight of propylene or butene-1, shall contain the finished polymer. not less than 85 weight percent poly- (3) Olefin basic copolymers consist of mer units derived from ethylene. basic copolymers manufactured by the (e) Olefin basic copolymers manufac- catalytic copolymerization of: tured by the catalytic polymerization (i) Two or more of the 1-alkenes hav- of ethylene and octene-1, or ethylene, ing 2 to 8 carbon atoms. Such olefin octene-1, and either hexene-1, butene-1, basic copolymers contain not less than propylene, or 4-methylpentene-1 shall 96 weight-percent of polymer units de- contain not less than 80 weight percent rived from ethylene and/or propylene, of polymer units derived from ethyl- except that: ene. (a)(1) Olefin basic copolymers manu- (ii) 4-Methylpentene-1 and 1-alkenes factured by the catalytic copolym- having from 6 to 18 carbon atoms. Such erization of ethylene and hexene-1 or olefin basic copolymers shall contain ethylene and octene-1 shall contain not not less than 95 molar percent of poly- less than 90 weight-percent of polymer mer units derived from 4- units derived from ethylene; methylpentene-1, except that copoly- (2) Olefin basic copolymers manufac- mers manufactured with 1-alkenes hav- tured by the catalytic copolymeriza- ing from 12 to 18 carbon atoms shall tion of ethylene and hexene-1 shall con- contain not less than 97 molar percent tain not less than 80 but not more than of polymer units derived from 4- 90 weight percent of polymer units de- methylpentene-1; or rived from ethylene. (iii) Ethylene and propylene that (3) Olefin basic copolymers manufac- may contain as modifiers not more tured by the catalytic copolymeriza- than 5 weight-percent of total polymer tion of ethylene and pentene-1 shall units derived by copolymerization with contain not less than 90 weight-percent one or more of the following mono- of polymer units derived from ethyl- mers: ene. (4) Olefin basic copolymers manufac- 5-Ethylidine-2-norbornene. tured by the catalytic polymerization 5-Methylene-2-norbornene. of ethylene and octene-1 shall contain not less than 50 weight-percent of poly- (iv) Ethylene and propylene that may mer units derived from ethylene. contain as a modifier not more than 4.5 (b) Olefin basic copolymers manufac- weight percent of total polymer units tured by the catalytic copolymeriza- derived by copolymerization with 1,4- tion of ethylene and 4-methylpentene-1 hexadiene. shall contain not less than 89 weight- (v) Ethylene and butene-1 copolymers percent of polymer units derived from (CAS Reg. No. 25087–34–7) that shall ethylene; contain not less than 80 weight percent (c)(1) Olefin basic copolymers manu- of polymer units derived from ethyl- factured by the catalytic copolym- ene. erization of two or more of the mono- (vi) Olefin basic copolymers (CAS mers ethylene, propylene, butene-1, 2- Reg. No. 61615–63–2) manufactured by methylpropene-1, and 2,4,4- the catalytic copolymerization of trimethylpentene-1 shall contain not ethylene and propylene with 1,4- less than 85 weight-percent of polymer hexadiene, followed by reaction with units derived from ethylene and/or pro- fumaric acid in the absence of free rad- pylene; ical initiators. Such polymers shall (2) Olefin basic copolymers manufac- contain not more than 4.5 percent of tured by the catalytic copolymeriza- polymer units deriving from 1,4- tion of propylene and butene-1 shall hexadiene by weight of total polymer contain greater than 15 but not greater prior to reaction with fumaric acid and than 35 weight percent of polymer not more than 2.2 percent of grafted fu- units derived from butene-1 with the maric acid by weight of the finished remainder being propylene. polymer. (d) Olefin basic terpolymers manufac- (vii) Ethylene and 2-norbornene (CAS tured by the catalytic copolymeriza- Reg. No. 26007–43–2) copolymers that tion of ethylene, hexene-1, and either shall contain not less than 30 and not
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more than 70 mole percent of polymer weight of copolymer units derived from units derived from 2-norbornene. maleic anhydride. (4) Poly(methylpentene) consists of (b) The basic olefin polymers identi- basic polymers manufactured by the fied in paragraph (a) of this section catalytic polymerization of 4- may contain optional adjuvant sub- methylpentene-1. stances required in the production of (5) Polyethylene graft copolymers such basic olefin polymers. The op- consist of polyethylene complying with tional adjuvant substances required in item 2.2 of paragraph (c) of this section the production of the basic olefin poly- which subsequently has 3a,4,7,7a- tetrahydromethyl-4,7- mers or finished food-contact articles methanoisobenzofuran-1,3-dione graft- may include substances permitted for ed onto it at a level not to exceed 1.7 such use by applicable regulations in percent by weight of the finished co- parts 170 through 189 of this chapter, polymer. substances generally recognized as safe (6) Ethylene-maleic anhydride co- in food and food packaging, substances polymers (CAS Reg. No. 9006–26–2) con- used in accordance with a prior sanc- taining no more than 2 percent by tion or approval, and the following:
Substance Limitations
Aromatic petroleum hydrocarbon resin, hydrogenated (CAS For use only as an adjuvant at levels not to exceed 25 percent Reg. No. 88526Ð47Ð0), produced by the catalytic polym- by weight in blends with polypropylene complying with para- erization of aromatic-substituted olefins from distillates of graph (c), item 1.1 of this section. The finished polymer may cracked petroleum stocks with a boiling point no greater than be used in contact with food Types I, II, IVÐB, VIÐA through 220 °C (428 °F), and the subsequent catalytic hydrogenation VIÐC, VIIÐB, and VIII identified in table 1 of ¤ 176.170(c) of of the resulting aromatic petroleum hydrocarbon resin, hav- this chapter and under conditions of use B through H de- ing a minimum softening point of 110 °C (230 °F), as deter- scribed in table 2 of ¤ 176.170(c) of this chapter; and with mined by ASTM Method E 28Ð67 (Reapproved 1982), food Types III, IVÐA, V, VIIÐA, and IX identified in table 1 of ‘‘Standard Test Method for Softening Point by Ring-and-Ball ¤ 176.170(c) of this chapter and under conditions of use D Apparatus,’’ and a minimum aniline point of 107 °C (225 °F), through G described in table 2 of ¤ 176.170(c) of this chap- as determined by ASTM Method D 611Ð82, ‘‘Standard Test ter. Methods for Aniline Point and Mixed Aniline Point of Petro- leum Products and Hydrocarbon Solvents,’’ both of which are incorporated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies are available from the American Society for Testing and Materials, 1916 Race St., Philadelphia, PA 19103, or from the Center for Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Administra- tion, 200 C St. SW., Washington, DC 20204, or may be ex- amined at the Office of the Federal Register, 800 North Cap- itol St. NW., suite 700, Washington, DC. Colorants used in accordance with ¤ 178.3297 of this chapter. 2,5-Dimethyl-2,5-di(tert-butylperoxy)hexane (CAS Reg. No. 78Ð For use as an initiator in the production of propylene 63Ð7). homopolymer complying with ¤ 177.1520(c), item 1.1 and olefin copolymers complying with ¤ 177.1520(c), items 3.1 and 3.2 and containing not less than 75 weight percent of polymer units derived from propylene, provided that the max- imum concentration of tert-butyl alcohol in the polymer does not exceed 100 parts per million, as determined by a method titled ‘‘Determination of tert-Butyl Alcohol in Polypropylene,’’ which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ 200), Food and Drug Administration, 200 C St. SW., Wash- ington, DC 20204, or available for inspection at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408.
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Substance Limitations
Methyl methacrylate/butyl acrylate-grafted polypropylene co- For use only at levels not to exceed 6 percent by weight of polymer containing methyl methacrylate/butyl acrylate-grafted olefin polymers complying with paragraph (c) of this section, polypropylene (CAS Reg. No. 121510Ð09Ð6), methyl meth- items 1.1, 3.1a, 3.2a, and 3.2b, where the copolymers com- acrylate/butyl acrylate copolymer (CAS Reg. No. 25852Ð37Ð plying with items 3.1a, 3.2a, and 3.2b contain not less than 3), methyl methacrylate homopolymer (CAS Reg. No. 9011Ð 85 weight-percent of polymer units derived from propylene. 14Ð7), and polypropylene (CAS Reg. No. 9003Ð07Ð0), re- sulting from the reaction of a mixture of methyl methacrylate and butyl acrylate with polypropylene. The finished product contains no more than 55 percent by weight of polymer units derived from methyl methacrylate and butyl acrylate as de- termined by a method entitled, ‘‘Determination of the Total Acrylic in PPÐMMA/BA Polymers,’’ which is incorporated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies are available from the Office of Premarket Approval, Center for Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or may be examined at the Center for Food Safety and Applied Nutrition’s Library, 200 C. St. SW., rm. 3321, Washington, DC, or at the Office of the Fed- eral Register, 800 North Capitol St. NW., suite 700, Wash- ington, DC. Petroleum hydrocarbon resins (cyclopentadiene-type), hydro- For use only as an adjuvant at levels not to exceed 30 percent genated (CAS Reg. No. 68132Ð00Ð3) produced by the ther- by weight in blends with: (1) Polypropylene complying with mal polymerization of dicyclopentadiene and cyclodiene paragraph (c), item 1.1 of this section, or (2) a copolymer of codimers (consisting of a mixture of cyclopentadiene, methyl propylene and ethylene containing not less than 94 weight cyclopentadiene, and C4ÐC5 acyclic dienes), followed by hy- percent propylene and complying with paragraph (c), item drogenation and having a ring-and-ball softening point of 119 3.2 of this section. The average thickness of the food-con- °C minimum as determined by ASTM Method E 28Ð67 (Re- tact film is not to exceed 0.1 millimeter (0.004 inch). The fin- approved 1982), ‘‘Standard Test Method for Softening Point ished polymer may be used in contact with (1) Food types I, by Ring-and-Ball Apparatus,’’ and a minimum viscosity of II, IVÐB, VIÐA, VIÐB, VIIÐB, and VIII identified in table 1 of 3,000 centipoise, measured at 160 °C, as determined by ¤ 176.170(c) of this chapter and under conditions of use C ASTM Method D 3236Ð88, ‘‘Standard Test Method for Ap- through G described in table 2 of ¤ 176.170(c) of this chap- parent Viscosity of Hot Melt Adhesives and Coating Mate- ter; and (2) food types III, IVÐA, V, VIÐC, VIIÐA, and IX iden- rials,’’ both of which are incorporated by reference in accord- tified in table 1 of ¤ 176.170(c) of this chapter and under ance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies are conditions of use D through G described in table 2 of available from the American Society for Testing and Mate- ¤ 176.170(c) of this chapter. rials, 1916 Race St., Philadelphia, PA 19103, or from the Center For Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or may be examined at the Office of the Federal Register, 800 North Capitol St. NW., suite 700, Washington, DC. Polymethylsilsesquioxane (CAS Reg. No. 68554Ð70Ð1) ...... For use only as a surface lubricant or anti-blocking agent in films. Poly(vinylidene fluoride) homopolymer (CAS Reg. No. 24937Ð For use only as a processing aid in the production of olefin 79Ð9), having a melt viscosity of 6 to 37 kilopoise at a shear polymers complying with paragraph (c) of this section at lev- rate of 100¥1 seconds at 232 °C as determined by ASTM els not to exceed 1.0 percent by weight of the polymer. The Method D 3835Ð79 (Reapproved 1983), ‘‘Standard Test finished polymers may be used only under the conditions de- Method for Rheological Properties of Thermoplastics with a scribed in ¤ 176.170(c) of this chapter, table 2, under condi- Capillary Rheometer’’ using a capillary of 15:1 L/D, which is tions of use B though H. incorporated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Wash- ington, DC. Polyoxyethylene-grafted polydimethylsiloxane (CAS Reg. No. For use as an extrusion aid in the production of extruded olefin 68937Ð54Ð2). polymers that comply with ¤ 177.1520(c) at levels not to ex- ceed 0.3 percent by weight of the polymer. The finished polymer is used in contact with foods under conditions of use B through H described in table 2 of ¤ 176.170 of this chapter.
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Substance Limitations
Triisopropanolamine (CAS Reg. No. 122Ð20Ð3) ...... For use as a Zeigler-Natta-type catalyst deactivator and anti- oxidant in the production of olefin polymers complying with ¤ 177.1520(c), items 2.1, 2.2, and 2.3, and having a min- imum density of 0.94 grams per cubic centimeter, and co- polymers complying with ¤ 177.1520(c), items 3.1 and 3.2, for use in contact with all foods under the following condi- tions of use: (a) films with a maximum thickness of 0.102 millimeter (0.004 inch) may be used under conditions A through H defined in table 2 of ¤ 176.170(c) of this chapter; and (b) articles with thickness greater than 0.102 millimeter (0.004 inch) may be used under conditions C through G de- fined in table 2 of ¤ 176.170(c) of this chapter. Trimethylpyridine and dimethylpyridine mixture having percent For use only as an adjuvant substance in the production of by weight composition as follows: 2,4,6-trimethylpyridine propylene homopolymers complying with items 1.1, 1.2, and (CAS Reg. No. 108Ð75Ð8), not less than 60 percent; 2,3,6- 1.3, and propylene copolymers complying with items 3.1, trimethylpyridine (CAS Reg. No. 1462Ð84Ð6), not more than and 3.2 of paragraph (c) of this section provided that the ad- 27 percent; 3,5-dimethylpyridine (CAS Reg. No. 591Ð22Ð0), juvant is used at a level not to exceed 20 parts per million not more than 12 percent; and other dimethylpyridines, not by weight of the olefin polymers. more than 6 percent. Vinylidene fluoride-hexafluoropropene copolymer (CAS Reg. For use only as an extrusion aid in the production of extruded No. 9011Ð17Ð0) having a fluorine content of 65 to 71 per- olefin polymers at levels not to exceed 0.2 percent by weight cent and a Mooney viscosity of at least 28, as determined by of the polymer. The finished polymers may be used only a method entitled ‘‘Mooney Viscosity,’’ which is incorporated under the conditions described in ¤ 176.170(c) of this chap- by reference in accordance with 5 U.S.C. 552(a). Copies are ter, table 2, under conditions of use B through H. available from the Center for Food Safety and Applied Nutri- tion (HFSÐ200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or may be examined at the Of- fice of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC. Vinylidene fluoride-hexafluoropropene copolymer (CAS Reg. For use only as a processing aid in the production of olefin No. 9011Ð17Ð0), having a vinylidene fluoride content of not polymers complying with paragraph (c) of this section at lev- less than 87 percent but less than 100 percent by weight els not to exceed 1.0 percent by weight of the polymer. The and a melt viscosity of 12 to 27 kilopoise at a shear rate of finished polymers may be used only under the conditions de- 100¥1 seconds at 232 °C as determined by ASTM Method D scribed in ¤ 176.170(c) of this chapter, table 2, under condi- 3835Ð79 (Reapproved 1983), ‘‘Standard Test Method for tions of use B though H. Rheological Properties of Thermoplastics with a Capillary Rheometer’’ using a capillary of 15:1 L/D, which is incor- porated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Copies are available from the Center for Food Safety and Applied Nutrition (HFSÐ200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or may be examined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408.
(c) Specifications:
Maximum extract- Maximum soluble Melting Point able fraction (ex- fraction (ex- (MP) or softening pressed as per- pressed as per- Olefin polymers Density point (SP) (De- cent by weight of cent by weight of grees Centi- the polymer) in N- polymer) in xy- grade)Ð hexane at speci- lene at specified fied temperatures temperatures
1.1a. Polypropylene described in paragraph 0.880Ð0.913 MP: 160°Ð180 °C 6.4 pct at reflux 9.8 pct at 25 °C (a)(1)(i) of this section temperature 1.1b. Propylene homopolymer described in 0.880Ð0.913Ð MP: 150°Ð180 °C 6.4 pct at reflux 9.8 pct at 25 °C paragraph (a)(1)(ii) of this section temperature 1.2. Polypropylene, noncrystalline; for use 0.80Ð0.88 only to plasticize polyethylene described under items 2.1 and 2.2 of this table, pro- vided that such plasticized polymers meet the maximum extractable fraction and max- imum soluble fraction specifications pre- scribed for such basic polyethylene
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Maximum extract- Maximum soluble Melting Point able fraction (ex- fraction (ex- (MP) or softening pressed as per- pressed as per- Olefin polymers Density point (SP) (De- cent by weight of cent by weight of grees Centi- the polymer) in N- polymer) in xy- grade)Ð hexane at speci- lene at specified fied temperatures temperatures
1.3. Polypropylene, noncrystalline, for use 0.80Ð0.88 SP:115°Ð138 °C. only: To plasticize polypropylene described by item 1.1 of this table, provided that such plasticized polymers meet the maximum ex- tractable fraction and maximum soluble fraction specifications prescribed for such basic polypropylene, and further provided that such plasticized polypropylene contacts food only of the types identified in ¤ 176.170(c) of this chapter, table 1, under Types I, II, IVÐB, VIÐB, VIIÐB, and VIII; and for use at levels not to exceed 50 pct by weight of any mixture employed as a food- contact coating provided such coatings con- tact food only of the types identified in ¤ 176.170(c) of this chapter, table 1, under Types I, II, IVÐB, VIÐB, VIIÐB, and VIII 2.1. Polyethylene for use in articles that con- 0.85Ð1.00 ...... 5.5 pct at 50 °C 11.3 pct at 25 °C tact food except for articles used for pack- ing or holding food during cooking 2.2. Polyethylene for use in articles used for 0.85Ð1.00 ...... 2.6 pct at 50 °C Do. packing or holding food during cooking 2.3. Polyethylene for use only as component 0.85Ð1.00 ...... 53 pct at 50 °C 75 pct at 25 °C of food-contact coatings at levels up to and including 50 percent by weight of any mix- ture employed as a food-contact coating 2.4. Olefin polymers described in paragraph (a)(2)(ii) of this section, having a melt flow index not to exceed 17 grams/per 10 min- utes as determined by the method de- scribed in paragraph (d)(7) of this section, for use in blends with other polymers at lev- els not to exceed 20 percent by weight of total polymer, subject to the limitation that when contacting food of types III, IVÐA, V, VIÐC, VIIÐA, and IX identified in ¤ 176.170(c) of this chapter, Table 1, the polymers shall be used only under condi- tions of use C, D, E, F, and G, described in ¤ 176.170(c) of this chapter, Table 2. 3.1a. Olefin copolymers described in para- 0.85Ð1.00 ...... 5.5 pct at 50 °C 30 pct at 25 °C graph (a)(3)(i) of this section for use in arti- cles that contact food except for articles used for packing or holding food during cooking; except olefin copolymers described in paragraph (a)(3)(i)(a)(3) of this section and listed in item 3.1c of this table and olefin copolymers described in paragraph (a)(3)(i)(e) of this section and listed in item 3.1b of this table 3.1b. Olefin copolymers described in para- 0.9Ð1.00 ...... Do Do. graph (a)(3)(i)(e) of this section for use in contact with food only under conditions of use D, E, F, G, and H described in ¤ 176.170(c) of this chapter, table 2 3.1c. Olefin copolymers described in para- Not less than 0.92 graph (a)(3)(i)(a)(3) of this section for use in contact with food only under conditions of use B, C, D, E, F, G, and H described in ¤ 176.170(c) of this chapter, table 2; except that such copolymers when used in contact with food of the types identified in ¤ 176.170(c), table 1, under types III, IVA, V, VIIA, and IX, shall be used only under conditions of use D, E, F, and G described in ¤ 176.170(c) of this chapter, table 2
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Maximum extract- Maximum soluble Melting Point able fraction (ex- fraction (ex- (MP) or softening pressed as per- pressed as per- Olefin polymers Density point (SP) (De- cent by weight of cent by weight of grees Centi- the polymer) in N- polymer) in xy- grade)Ð hexane at speci- lene at specified fied temperatures temperatures
3.2a. Olefin copolymers described in para- 0.85Ð1.00 ...... 2.6 pct at 50 °C Do. graph (a)(3)(i) of this section for use in arti- cles used for packing or holding food during cooking; except olefin copolymers described in paragraph (a)(3)(i)(c)(2) of this section and listed in item 3.2b of this table; except that olefin copolymers containing 89 to 95 percent ethylene with the remainder being 4-methyl-pentene-1 contacting food Types III, IVA, V, VIIA, and IX identified in ¤ 176.170(c) of this chapter, table 1, shall not exceed 0.051 millimeter (mm) (0.002 inch (in)) in thickness when used under conditions of use A and shall not exceed 0.102 mm (0.004 in) in thickness when used under conditions of use B, C, D, E, and H described in ¤ 176.170(c) of this chapter, table 2. Additionally, olefin copoly- mers described in (a)(3)(i)(a)(2) of this sec- tion may be used only under conditions of use B, C, D, E, F, G, and H described in ¤ 176.170(c) of this chapter, table 2, in con- tact with all food types identified in ¤ 176.170(c) of this chapter, table 1 3.2b. Olefin copolymers described in para- Do. graph (a)(3)(i)(c)(2) of this section have a melt flow index no greater than 10 grams per 10 minutes as determined by the meth- od described in paragraph (d)(7) of this sec- tion, and the thickness of the finished poly- mer contacting food shall not exceed 0.025 mm (0.001 in). Additionally, optional adju- vants permitted for use in olefin copolymers complying with item 3.2a of this table may be used in the production of this copolymer 3.2c. Olefin copolymers described in para- 0.85Ð0.92 ...... graph (a)(3)(i)(a)(4) of this section have a melt flow index no greater than 50 grams per 10 minutes as determined by the meth- od described in paragraph (d)(7) of this sec- tion. Articles manufactured using these polymers may be used with all types of food under conditions of use C through H as de- scribed in table 2 of ¤ 176.170(c) of this chapter 3.3a. Olefin copolymers described in para- ...... graph (a)(3)(ii) of this section and manufac- tured with 1-alkenes having from 6 to 10 carbon atoms 3.3b. Olefin copolymers described in para- graph (a)(3)(ii) of this section, provided that such olefin polymers have a melt tempera- ture of 220 °C to 250 °C (428 °F to 482 °F) as determined by the method described in paragraph (d)(8) of this section and min- imum intrinsic viscosity of 1.0 as determined in paragraph (d)(9) of this section.
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Maximum extract- Maximum soluble Melting Point able fraction (ex- fraction (ex- (MP) or softening pressed as per- pressed as per- Olefin polymers Density point (SP) (De- cent by weight of cent by weight of grees Centi- the polymer) in N- polymer) in xy- grade)Ð hexane at speci- lene at specified fied temperatures temperatures
3.4. Olefin copolymers, primarily non-crys- 0.85Ð0.90 talline, described in par. (a)(3) (iii) of this section provided that such olefin polymers have a minimum viscosity average molec- ular weight of 120,000 as determined by the method described in par. (d)(5) of this sec- tion and a minimum Mooney viscosity of 35 as determined by the method described in par. (d)(6) of this section, and further pro- vided that such olefin copolymers contact food only of the types identified in ¤ 176.170(c) of this chapter, table 1, under Types I, II, III, IV-B, VI, VII, VIII, and IX 3.5. Olefin copolymers, primarily non-crys- 0.85Ð0.90 talline, described in paragraph (a)(3)(iv) of this section, provided that such olefin poly- mers have a minimum viscosity average molecular weight of 95,600 as determined by the method described in paragraph (d)(5) of this section, and further provided that such olefin polymers are used only in blends with olefin polymers described under items 1.1, 2.1, and 2.2 of this table at a maximum level of 25 pct by weight, and provided that such olefin copolymers con- tact food only of the types identified in ¤ 176.170 (c) of this chapter, table 1, under Types I, II, IV-B, VI, VII-B, and VIII at tem- peratures not exceeding 190 °F 3.6. Olefin copolymers described in para- Not less than 0.88 graph (a)(3)(v) of this section for use in blends with olefin polymer resins have a melt flow index no greater than 5 grams/10 minutes as determined by the method de- scribed in paragraph (d)(7) of this section and the thickness of the finished blends shall not exceed 0.1 millimeter (0.004 inch). The ethylene/butene-1 copolymer may be used subject to the following conditions: (1) For use at a level not to exceed 20 weight percent in polypropylene as described under item 1.1 of this table. (2) For use at a level not to exceed 40 weight percent in polyethylene as described under items 2.1 and 2.2 of this table. (3) For use at a level not to exceed 40 weight percent in olefin copolymers as described under items 3.1 and 3.2 of this table
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Maximum extract- Maximum soluble Melting Point able fraction (ex- fraction (ex- (MP) or softening pressed as per- pressed as per- Olefin polymers Density point (SP) (De- cent by weight of cent by weight of grees Centi- the polymer) in N- polymer) in xy- grade)Ð hexane at speci- lene at specified fied temperatures temperatures
3.7. Ethylene/propylene copolymers, meeting Not less than 0.86 the identity described in paragraph (a)(3)(i) of this section, containing not less than 80 mole-percent of polymer units derived from ethylene and having a minimum viscosity average molecular weight of 95,000 as de- termined by the method described in para- graph (d)(5) of this section, and a minimum Mooney viscosity of 13 as determined by the method described in paragraph (d)(6) of this section. Ethylene/propylene copolymers described in this item 3.7 are to be used only in blends with other olefin polymers complying with this section, at levels not to exceed 30 percent by weight of the total polymer blend, and in contact with food only of types identified in ¤ 176.170(c) of this chapter, Table 1, under Types I, II, III, IVÐB, VI, VII, VIII, and IX. Additionally, optional adjuvants permitted for use in olefin copoly- mers complying with item 3.4 of this table may be used in the production of this copolymer 3.8. Olefin polymers described in paragraph (a)(3)(vi) of this section, having a melt flow index not to exceed 9.2 grams per 10 min- utes as determined by the method de- scribed in paragraph (d)(7) of this section, for use in blends with other polymers at lev- els not to exceed 8 percent by weight of total polymer, subject to the limitation that when contacting food of types III, IVÐA, V, VIÐC, VIIÐA, and IX, identified in ¤ 176.170(c) of this chapter, Table 1, the polymers shall be used only under condi- tions of use C, D, E, F, and G, described in ¤ 176.170(c) of this chapter, Table 2. 3.9. Olefin copolymers described in paragraph Not less than 1.0 ...... (a)(3)(vii) of this section may only be used in contact with dry foods, Type VIII, as iden- tified in ¤ 176.170(c) of this chapter, Table 1 4. Poly(methylpentene) 0.82Ð0.85 MP: 235°Ð250 °C 6.6 pct at reflux 7.5 pct at 25 °C temperature 5. Polyethylene copolymer described in para- Not less than 0.94 ...... 0.45 pct at 15 °C 1.8 pct at 25 °C graph (a)(5) of this section and having a melt index not to exceed 2, for use, either alone or in blends with other olefin poly- mers, subject to the limitation that when contacting foods of types III, IV-A, V, VI-C, VII-A, VIII, and IX identified in ¤ 176.170(c) of this chapter, table 1, the thickness of the film (in mils) containing the polyethylene graft copolymer times the concentration of the polyethylene graft copolymer shall not exceed a value of 2 6. Ethylene-maleic anhydride copolymers de- 0.92 or greater ...... 1.36 pct at 50 °C 2.28 pct at 25 °C scribed in paragraph (a)(6) of this section for use as the adhesive component in multi- laminate structures, or as the sealant layer in flexible packaging, in contact with food at temperatures not exceeding 49 °C (120 °F)
(d) The analytical methods for deter- this section are as follows, and are ap- mining whether olefin polymers con- plicable to the basic polymer in film form to the specifications prescribed in form not exceeding 4 mils in thickness.
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The film to be tested shall be cut into 2 hours and filtered at the boiling approximately 1-inch squares by any point. The filtrate is evaporated and convenient method that avoids con- the total residue weighed as a measure tamination by dust, dirt, or grease of the solvent extractable fraction. (NOTE: Do not touch samples with bare (a) Apparatus. (1) Erlenmeyer flasks, fingers—use forceps to hold or transfer 250-milliliter, with ground joint. samples). (2) Condensers, Allihn, 400-millimeter (1) Density. Density shall be deter- jacket, with ground joint. mined by ASTM method D1505–68 (Re- (3) Funnels, ribbed 75-millimeter di- approved 1979), ‘‘Standard Test Method ameter, stem cut to 40 millimeters. for Density of Plastics by the Density- (4) Funnels, Buchner type, with Gradient Technique,’’ which is incor- coarse-porosity fritted disc, 60-milli- porated by reference. Copies may be meter diameter. obtained from the American Society (5) Bell jar for vacuum filtration into for Testing Materials, 1916 Race St., beaker. Philadelphia, PA 19103, or may be ex- (b) Reagent. n-Hexane, commercial amined at the Office of the Federal grade, specific gravity 0.663–0.667 (20 °C/ Register, 800 North Capitol Street, 20 °C), boiling range 66 °C-69 °C, or NW., suite 700, Washington, DC 20408. equivalent. (2) Melting point or softening point—(i) (c) Procedure. Weigh 1 gram of sample Melting point. The melting point shall accurately and place in a 250-milliliter be determined by ASTM method D2117– Erlenmeyer flask containing two or 82, ‘‘Standard Test Method for Melting three boiling stones. Add 100 milliliters Point of Semicrystalline Polymers by of solvent, attach the flask to the con- the Hot Stage Microscopy Method,’’ denser (use no grease), and reflux the which is incorporated by reference. The mixture for 2 hours. Remove the flask availability of this incorporation by from the heat, disconnect the con- reference is given in paragraph (d)(1) of denser, and filter rapidly, while still this section. hot, through a small wad of glass wool (ii) Softening point. The softening packed in a short-stem funnel into a point shall be determined by ASTM tared 150-millimeter beaker. Rinse the method E28–67 (Reapproved 1982), flask and filter with two 10-milliliter ‘‘Standard Test Method for Softening portions of the hot solvent, and add the Point by Ring-and-Ball Apparatus,’’ rinsings to the filtrate. Evaporate the which is incorporated by reference. The filtrate on a stream bath with the aid availability of this incorporation by of a stream of nitrogen. Dry the res- reference is given in paragraph (d)(1) of idue in a vacuum oven at 110 °C for 2 this section. hours, cool in a desiccator, and weigh (3) Maximum extractable fraction in n- to the nearest 0.0001 gram. Determine hexane—(i) Olefin copolymers described the blank on 120 milliliters of solvent in paragraph (a)(3)(ii) of this section, evaporated in a tared 150-milliliter polypropylene, and poly(methylpentene). beaker. Correct the sample residue for A sample is refluxed in the solvent for this blank if significant. Calculation:
Grams of residue = Percent extractable with n-hexane. Grams of sample ×100
(ii) Olefin copolymers described in para- the extraction period to give a measure graph (a)(3)(i) of this section and poly- of the solvent extractable fraction. The ethylene. A preweighed sample is ex- maximum n-hexane-extractable frac- tracted at 50 °C for 2 hours and filtered. tion may be determined by the meth- The filtrate is evaporated and the total ods set forth in paragraphs (d)(3)(ii)(a) residue weighed as a measure of the through (d)(3)(ii)(i) of this section. solvent extractable fraction. Alter- (a) Extraction apparatus. Two-liter, natively, the sample is reweighed after straight-walled, Pyrex (or equivalent)
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resin kettles, fitted with three-hole the filtrate in a tared, glass-stoppered ground-glass covers are most conven- Erlenmeyer flask of 1-liter capacity. ient for this purpose. The cover is Determine the weight of the filtrate re- fitted with a thermometer, a gas-tight covered to the nearest gram. Recovery stirrer driven by an air motor or explo- should be at least 90 percent of the sion-proof electric motor, and a reflux original solvent. Losses due to evapo- condenser. The kettle is fitted with an ration during heating and filtering electric heating mantle of appropriate have been found not to exceed 10 per- size and shape, which is controlled by a cent. Transfer about half of the solvent variable-voltage transformer. filtrate to a 1-liter beaker placed on an (b) Evaporating apparatus. Rapid opening in the steam bath and imme- evaporation of large volumes of solvent diately cover with the special ‘‘gas’’ requires special precautions to prevent cover, the inlet tube of which has been contamination by dust. This is facili- attached with flexible tetrafluoro- tated by a special ‘‘gas’’ cover con- ethylene tubing to a source of high-pu- sisting of an inverted flat Pyrex crys- rity nitrogen in series with a stainless tallizing dish of an appropriate size (190 steel heating coil immersed directly in millimeters × 100 millimeters) to fit a the body of the steam bath. Maintain a 1-liter beaker. Through the center of positive flow of warm nitrogen gas the dish are sealed an inlet tube for throughout the evaporation of the sol- preheated, oxygen-free nitrogen, and vent, adding the remainder of the fil- an outlet tube located 1 inch off center. trate from the Erlenmeyer flask as the Nitrogen is fed from the supply source evaporation proceeds. When the volume through a coil of 1⁄4-inch stainless steel of the solvent has been reduced to tubing immersed in the same steam about 50 milliliters, transfer the con- bath used to supply heat for solvent centrated liquid to a previously tared evaporation. All connections are made weighing dish of suitable size. Wash the with flexible tetrafluoroethylene tub- beaker twice with 20–30 milliliter por- ing. tions of warm solvent, adding the (c) Reagents—(1) n-Hexane. Spectro- washings to the weighing dish while grade n-hexane. continuing to evaporate the remainder (2) Nitrogen. High-purity dry nitrogen of the solvent under the gas cover with containing less than 10 parts per mil- its flow of warm nitrogen directed to- lion of oxygen. ward the center of the dish. In the (d) Procedure. Transfer 2.5 grams (ac- event that an insoluble residue that curately weighed to nearest 0.001 gram) cannot be removed with warm solvent of the polymer to the resin kettle. Add remains in the beaker, it may be nec- 1 liter of solvent and clamp top in posi- essary to heat with a small amount of tion. Start water flowing through jack- a higher boiling solvent such as ben- et of the reflux condenser and apply air zene or toluene, transferring these pressure to the stirring motor to washings to the weighing dish before produce vigorous agitation. Turn on final evaporation to dryness. Transfer heating jacket with transformer set at the weighing dish with its residue to a a predetermined voltage to bring the vacuum desiccator, and allow it to re- temperature of the contents to 50 °C main overnight (at least 12 hours), within 20–25 minutes. As the thermom- after which the net weight of the dry eter reading approaches 45 °C–47 °C, re- residue is determined to the nearest duce the voltage to the predetermined 0.0001 gram. Correct the result for any setting that will just maintain the solvent blank equivalent to the non- temperature at 50 °C. Do not overshoot volatile matter determined to be con- the prescribed temperature. Should tained in the amount of solvents used this occur discard the test and start in the test. afresh. Exactly 2 hours after the sol- (e) Extraction apparatus for alternate vent temperature has reached 50 °C, method. Two-liter extraction vessel, disconnect the heater, remove the resin such as a resin kettle or round bottom kettle from the heating jacket, and de- flask, fitted with an Allihn condenser cant the solvent, while still warm, (size C), a 45/50 male joint with a Teflon through a coarse filter paper placed on sleeve, and a Teflon coated stir bar. top of a fritted-glass funnel, collecting Water bath maintained at 49.5 °C ±0.5
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°C containing a submersible magnetic inch squares using clean sharp scissors. stirrer motor with power supply. Other Proceed with Option 1 or 2. suitable means of maintaining tem- Option 1. Using tweezers and noting perature control, such as electric heat- the number of film pieces, transfer 2.5 ing mantles, may be used provided that grams (accurately weighed to 0.1 milli- the temperature range can be strictly gram) of polymer to the extraction ves- maintained. sel. Extract the film sample for 2 (f) Sample basket (Optional). A per- hours. Allow the vessel to cool and fil- forated stainless steel cylindrical bas- ter the contents through a fritted por- ket that is approximately 1.5 inches in celain funnel. Wash the film pieces diameter, 1.6 inches high, and has per- with fresh n-hexane, aspirate to dry- forations of 0.125 inches in diameter for ness, and transfer, using tweezers, to a 33 holes/in2, or 40 percent open area. beaker. Recount the film pieces to The basket should pass freely through verify that none were lost during the the 45/50 female joint of the extraction transfer. Place the beaker in the vacu- flask. A No. 6–32 stainless steel eye- um oven for 2 hours at 80 °C ±5 °C. After bolt is attached to the lid for posi- 2 hours, remove and place in a desic- tioning the basket in the extraction cator to cool to room temperature vessel. The positioning rod, approxi- (about 1 hour). After cooling, reweigh mately 18 inches long and made from 1/ the film pieces to the nearest 0.1 milli- 16 inch outside diameter 316 stainless gram. Calculate the percent hexane- steel welding rod or equivalent and extractables content from the weight hooked at both ends, is used to position loss of the original sample. Multiply the basket in the extraction apparatus. the result by 0.935 and compare with extraction limits in paragraph (c) of (g) Vacuum oven. Capable of main- this section. Repeat the above proce- taining 80 °C ±5 °C and a minimum of dure for successive samples. 635 millimeters of mercury pressure. Option 2. Transfer 2.5±0.05 grams of (h) Reagents. n-Hexane, reagent or the prepared 1-inch film sections into a spectrograde, aromatic free (less than 1 tared sample basket and accurately milligram per liter), minimum 85 per- weigh to the nearest 0.1 milligram. cent n-hexane. This reagent may be re- Carefully raise the condenser until the used until it contains a maximum of 1.5 hook on the positioning rod is above grams polyolefin extractables or has the neck of the 2-liter extraction ves- been used for 12 determinations. sel. The basket should be totally below (i) Procedure. Assemble the extraction the level of n-hexane solvent. Extract vessel, condenser, and magnetic stir the sample resin film for 2 hours and bar. Add n-hexane (1 liter) to the ex- then raise the basket above the solvent traction vessel and clamp the assembly level to drain momentarily. Remove into a water bath set at 49.5 °C ±0.5 °C. the basket and rinse the contents by Start the water flowing through the immersing several times in fresh n- jacket of the reflux condenser. Adjust hexane. Allow the basket to dry be- the air flow through the stirring motor tween rinsings. Remove the excess sol- to give a smooth and uniform stir rate. vent by briefly blowing the basket with Allow the n-hexane to preheat for 1 a stream of nitrogen or dry air. Place hour to bring the temperature to 49.5 the basket in the vacuum oven for 2 °C±0.5 °C. Temperature is a critical fac- hours at 80 °C ±5 °C. After 2 hours, re- tor in this analysis and it must not move and place in a desiccator to cool vary more than 1 °C. If the temperature to room temperature (about 1 hour). exceeds these limits, the test must be After cooling, reweigh the basket to discontinued and restarted. Blown, the nearest 0.1 milligram. Calculate compression molded, or extrusion cast the percent hexane extractables con- films can be tested. Ideally, the film tent from the weight loss of the origi- should be prepared by the same process nal sample. Multiply the result by 0.935 as will be used with the production and compare with extraction limits in resin. Using gloves and metal tweezers paragraph (c) of this section. Repeat to avoid sample contamination, cut the above procedure for successive about 2.7 grams of the prepared film (4 samples. The same solvent charge mils or less in thickness) into about 1- should remain clear and can be used for
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at least 12 determinations. Applica- (c) Procedure. Weigh 1 to 2 grams of tions of solvent reuse should be con- sample to the nearest 0.001 gram and firmed for each resin type before use. place in a 125-milliliter Pyrex reagent (4) Maximum soluble fraction in xy- bottle containing a 1-inch long tetra- lene—(i) Olefin copolymers described in fluoroethylene-resin-coated stirring paragraph (a)(3)(ii) of this section, poly- bar. Add 100 milliliters of solvent, set propylene, and poly(methylpen-tene). A the stopper in lightly, and place the sample is dissolved completely in xy- bottle in the heating mantle or alu- lene by heating and stirring in a bottle minum block maintained at a tempera- with little free space. The solution is ture of 120 °C, and stir with a magnetic allowed to cool without stirring, stirrer until the sample is completely whereupon the insoluble portion pre- dissolved. Remove the bottle from the cipitates and is filtered off; the total heat and allow it to cool 1 hour in the solids content of the filtrate is then de- air, without stirring. Then place the termined as a measure of the soluble bottle in a water bath maintained at 25 fraction. °C ±0.5 °C, and allow to stand 1 hour (a) Apparatus. (1) Pyrex (or equiva- without stirring. Next, remove the bot- lent) reagent bottle, 125-milliliter, tle from the water bath, shake, and glass-stoppered. pour part of the contents into the (2) Heating mantle of size for 150-mil- coarse-porosity fritted-glass funnel. liliter beaker (or suitable aluminum Apply suction, and draw 30–40 milli- block to fit the 125-milliter bottle de- liters of filtrate through, adding more scribed in paragraph (d)(4)(i)(a)(1) of slurry to the funnel, and catching the this section. filtrate in a large test tube. (If the (3) Magnetic stirrer for use under the slurry is hard to filter, add 10 grams of heating mantle (combination magnetic diatomaceous earth filter aid to the stirrer and hotplate may be used if alu- bottle and shake vigorously just prior minum block is used in place of heat- to the filtration.) Pipet a suitable ali- ing mantle). quot (preferably 20 milliliters) of the (4) Variable-voltage transformer, 7.5 filtrate into a tared aluminum dispos- amperes. able dish. Place the dish on a steam (5) Tetrafluoroethylene-resin-coated bath covered with a fresh sheet of alu- stirring bar, 1-inch long. minum foil and invert a short-stemmed (6) Constant temperature water bath 4-inch funnel over the dish. Pass nitro- maintained at 25 °C±0.5 °C. gen (heated if desired) down through (7) Aluminum dishes, 18 millimeters × the funnel at a rate sufficient to just 60 millimeters, disposable. ripple the surface of the solvent. When (8) Funnel, Buchner type, with the liquid has evaporated, place the coarse-porosity fritted disc, 30–60 milli- dish in a vacuum oven at 140 °C and meter diameter. less than 50 millimeters mercury pres- (b) Reagent. Xylene with antioxidant. sure for 2 hours. Cool in a desiccator Dissolve 0.020 gram of phenyl-β- naph- and weigh. (Note: If the residue value thylamine in 1 liter of industrial grade seems high, redry in the vacuum oven xylene having specific gravity 0.856– for one-half hour to ensure complete 0.867 (20 °C/20 °C) and boiling range 123 removal of all xylene solvent.) Calcula- °C–160 °C. tion:
Grams of residue 100 milliters ××=100 Percent soluble in xylene Grams of sample volume of aliquot in milliliters
(ii) Olefin copolymers described in para- and the total residue weighed as a graph (a)(3)(i) of this section and poly- measure of soluble fraction. ethylene. A sample is extracted in xy- (a) Apparatus—(1) Extraction appa- lene at reflux temperature for 2 hours ratus. Two-liter, straight-walled Pyrex and filtered. The filtrate is evaporated (or equivalent) resin kettles, fitted
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with ground-glass covers, are most con- idly cooled to 25 °C–30 °C by immersing venient for this purpose. The cover is in a cold water bath. Transfer the ket- equipped with a thermometer and an tle to a constant temperature bath set efficient reflux condenser. The kettle is to maintain 25 °C ±0.1 °C, and allow to fitted with an electric heating mantle equilibrate for a least 1 hour (may be of appropriate size and shape which is left overnight if convenient). Break up controlled by a variable-voltage trans- any precipitated polymers that may former. have formed, and decant the xylene so- (2) Constant temperature water bath. It lution successively through a fast filter must be large enough to permit immer- paper and then through a fritted-glass sion of the extraction kettle and set to filter into a tared 1-liter Erlenmeyer maintain 25 °C ±0.1 °C. flask, collecting only the first 450 mil- (3) Evaporating apparatus. Gas cover liliters—500 milliliters of filtrate (any consisting of a flat Pyrex crystallizing attempt to collect more of the xylene dish (190 millimeters × 100 millimeters) solution usually results in clogging the inverted to fit over a 1-liter beaker filter and risking losses). Reweigh the with 8-millimeter gas inlet tube sealed Erlenmeyer flask and calculate the through center and an outlet tube 1 weight of the filtrate obtained to the inch off center. The beaker with gas nearest 0.1 gram. Transfer the filtrate, cover is inserted in an electric heating quantitatively, from the Erlenmeyer mantle equipped with a variable-volt- flask to the 1-liter beaker, insert the age transformer. The outlet tube is at- beaker in its heating mantle, add a tached to an efficient condenser glass-coated magnetic stirring bar, and mounted on a receiving flask for sol- mount the gas cover in place, con- vent recovery and having an outlet for necting the inlet tube to the nitrogen connection to an aspirator pump. The source and the outlet to the condenser heating mantle (with the beaker) is of the receiving flask. Start a flow of mounted on a magnetic stirring device. nitrogen (2 to 3 liters per minute) into An infrared heat lamp is mounted the gas cover and connect an aspirator vertically 3–4 inches above the gas to the receiver using a free-flow rate cover to prevent condensation of the equivalent to 6–7 liters of air per solvent inside the cover. Make all con- minute. With the infrared lamp on, ad- nections with flexible tetrafluoro- just the voltage to the heating mantle ethylene tubing. to give a distillation rate of 12–13 milli- (b) Reagents—(1) Xylene. American liters per minute when the magnetic Chemical Society reagent grade that stirrer is revolving just fast enough to has been redistilled through a promote good boiling. When the vol- fractionating column to reduce the ume of solvent in the beaker has been nonvolatile residue. reduced to 30–50 milliliters, transfer (2) Nitrogen. High-purity dry nitrogen the concentrated extractive to a suit- containing less than 104 parts per mil- able weighing dish that has been pre- lion oxygen. viously tared (dry). Rinse the beaker (c) Procedure. Transfer 5 grams ±0.001 twice with 10–20 milliliter portions of gram of sample to the resin kettle, add fresh xylene, adding the rinsings to the 1,000 milliliters (840 grams) of xylene, weighing dish. Evaporate the remain- and clamp top in position after insert- der of the xylene on an electric ing a piece of glass rod to prevent hotplate set at low heat under the gas bumping during reflux. Start water cover with a stream of nitrogen di- flowing through the jacket of the rected toward the center of the dish. reflux condenser and apply full voltage Avoid any charring of the residue. (115 volts) to the heating mantle. When Transfer the weighing dish to a vacu- the xylene starts to boil, reduce the um desiccator at room temperature voltage to a level just sufficient to and allow to remain under reduced maintain reflux. After refluxing for at pressure for at least 12 hours (over- least 2 hours, disconnect the power night), after which determine the net source to the mantle, remove the ket- weight of the residue to the nearest tle, and allow to cool in air until the 0.0001 gram. Correct the result for non- temperature of the contents drops to 50 volatile solvent blank obtained by °C, after which the kettle may be rap- evaporating the equivalent amount of
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xylene under identical conditions. Cal- test conditions and procedures are as culate the weight of residue originally follows: present in the total weight of solvent (840 grams), using the appropriate fac- List of polymers Conditions/procedures tor based on the weight of filtrate Olefin copolymers described in para- Condition L, proce- evaporated. graph (a)(3)(i)(c)(2) of this section. dure A. (5) Viscosity average molecular weight Olefin copolymers described in para- Condition E, proce- olefin copolymers described in paragraphs graph (a)(3)(v) of this section. dure A. Olefin polymers described in para- Condition E, proce- (a)(3) (iii) and (iv) of this section. The graph (a)(2)(ii) of this section. dure A. viscosity average molecular weight Olefin polymers described in para- Condition E, proce- shall be determined from the kine- graph (a)(3)(vi) of this section. dure A. matic viscosity (using ASTM method D445–74, ‘‘Test for Kinematic Viscosity (8) Melting peak temperature. The melt of Transparent and Opaque Liquids’’ temperature of the olefin polymers de- (Revised 1974), which is incorporated by scribed in paragraph (a)(3)(ii) of this reference; copies are available from section shall be determined by ASTM American Society for Testing and Ma- method D 3418–82, ‘‘Standard Test terials (ASTM), 1916 Race Street, Method for Transition Temperatures of Philadelphia, PA 19103, or available for Polymers by Thermal Analysis,’’ which inspection at the Office of the Federal is incorporated by reference in accord- Register, 800 North Capitol Street, ance with 5 U.S.C. 552(a). The avail- NW., suite 700, Washington, DC 20408) of ability of this incorporation by ref- solutions of the copolymers in solvents erence is given in paragraph (d)(1) of and at temperatures as follows: this section. (i) Olefin polymers described in para- (9) Intrinsic viscosity. The intrinsic graph (a)(3)(iii) of this section in viscosity of the olefin polymers de- ° decahydronaphthalene at 135 C. scribed in paragraph (a)(3)(ii) of this (ii) Olefin polymers described in section shall be determined by ASTM paragraph (a)(3)(iv) of this section in method D 1601–78, ‘‘Standard Test ° tetrachloroethylene at 30 C. Method for Dilute Solution Viscosity (6) Mooney viscosity—olefin copolymers of Ethylene Polymers,’’ which is incor- described in paragraph (a)(3)(iii) of this porated by reference in accordance section. Mooney viscosity is determined with 5 U.S.C. 552(a). The availability of by ASTM method D1646–81, ‘‘Standard this incorporation by reference is given Test Method for Rubber—Viscosity and in paragraph (d)(1) of this section. Vulcanization Characteristics (Mooney Viscometer),’’ which is incorporated by (e) Olefin copolymers described in reference (the availability of this in- paragraph (a)(3) (i) of this section and corporation by reference is given in polyethylene, alone or in combination, paragraph (d)(1) of this section), using may be subjected to irradiation bom- the large rotor at a temperature of 100 bardment from a source not to exceed °C, except that a temperature of 127 °C 2.3 million volts intensity to cause mo- shall be used for those copolymers lecular crosslinking of the polymers to whose Mooney viscosity cannot be de- impart desired properties, such as in- termined at 100 °C. The apparatus con- creased strength and increased ability taining the sample is warmed for 1 to shrink when exposed to heat. minute, run for 8 minutes, and vis- (f) The olefin polymers identified in cosity measurements are then made. and complying with this section, when (7) Melt flow index. The melt flow used as components of the food-contact index of olefin polymers described surface of any article that is the sub- below shall be determined by ASTM ject of a regulation in parts 174, 175, method D–1238–82, ‘‘Standard Test 176, 177, 178, and § 179.45 of this chapter, Method for Flow Rates of Thermo- shall comply with any specifications plastics by Extrusion Plastometer,’’ and limitations prescribed by such reg- which is incorporated by reference in ulation for the article in the finished accordance with 5 U.S.C. 552(a). The form in which it is to contact food. availability of this incorporation by (g) The provisions of this section are reference is given in paragraph (d)(1) of not applicable to olefin polymers iden- this section. The olefin polymers and tified in § 175.105(c) (5) of this chapter
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and used in food-packaging adhesives List of substances Limitations complying with § 175.105 of this chapter. Lithium polysilicate containing For use only as a compo- [42 FR 14572, Mar. 15, 1977] not more than 20 weight per- nent of repeated-use cent silica, not more than 2.1 coatings not exceeding EDITORIAL NOTE: For FEDERAL REGISTER ci- percent lithium oxide and 0.030 millimeter (0.0012 tations affecting § 177.1520, see the List of having a maximum mole inch) in thickness where CFR Sections Affected, which appears in the ratio of Si02/Li20 of 8.5 to 1. the coatings are thermally cured at minimum sinter- Finding Aids section of the printed volume ing temperatures of 371 and on GPO Access. °C (700 °F). Lithium ex- tractives shall not exceed § 177.1550 Perfluorocarbon resins. 1.55 milligrams per square decimeter (0.1 Perfluorocarbon resins identified in milligram per square inch) this section may be safely used as arti- of coating surface when tested in accordance with cles or components of articles intended paragraph (e)(2) of this to contact food, subject to the provi- section. sions of this section: Naphthalene sulfonic acid For use only: formaldehyde condensate, 1. As a component of re- (a) Identity. For the purpose of this sodium salt. peated-use coatings, section, perfluorocarbon resins are based on the those produced by: (1) The perfluorocarbon resin identified in paragraph homopolymerization and/or copolym- (a)(1) of this section, not erization of hexafluoropropylene and to exceed 0.030 milli- tetrafluoroethylene, and (2) the co- meter (0.0012 inch) in thickness, and at a level polymerization of not to exceed 0.4 weight perfluoropropylvinylether and tetra- percent of the coating. fluoroethylene (CAS Reg. No. 26655–00– 2. As a component of re- peated-use coatings, 5). The resins shall meet the extrac- based on the tives limitations in paragraph (d) of perfluorocarbon resin identified in paragraph this section. (a)(2) of this section, not (b) Optional components. The to exceed 0.10 millimeter perfluorocarbon resins identified in (0.004 inch) in thickness, and at a level not to ex- paragraph (a) of this section as well as ceed 0.4 weight percent articles or coating made from these of the coating. resins may include the following op- tional components except that the (c) Optional processing. Poly- tetra- resin identified in paragraph (a)(2) of fluoroethylene resins may be irradi- this section may not be used with the ated by either a cobalt-60 sealed optional component, lithium source, at a maximum dose of gamma polysilicate, mentioned in paragraph radiation not to exceed 7.5 megarads, (b)(4) of this section. or an electron beam at energy levels (1) Substances generally recognized not to exceed 2.5 million electron volts with a maximum dosage of 7.5 as safe (GRAS) in food or food pack- megarads, to produce lubricant pow- aging subject to any limitations cited ders having a particle diameter of not on their use. more than 20 microns for use only as (2) Substances used in accordance components of articles intended for re- with a prior sanction or approval, sub- peated use in contact with food. ject to any limitations cited in the (d) Specifications—(1) Infrared identi- prior sanction or approval. fication. Perfluorocarbon resins can be (3) Substances authorized under ap- identified by their characteristic infra- plicable regulations in this part and in red spectra. parts 175 and 178 of this chapter and (2) Melt-viscosity. (i) The perfluoro- subject to any limitations prescribed carbon resins identified in paragraph therein. (a)(1) of this section shall have a melt (4) The following substances, subject viscosity of not less than 104 poises at to any limitations prescribed: 380 °C (716 °F) as determined by ASTM
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method D1238–82, ‘‘Standard Test Meth- of 6.45 square decimeters (100 square od for Flow Rates of Thermoplastics by inches) or more and at least 1.27 milli- Extrusion Plastometer,’’ which is in- meters (0.05 inch) thick shall be ex- corporated by reference. Copies may be tracted at reflux temperatures for 2 obtained from the American Society hours separately with distilled water, for Testing Materials, 1916 Race St., 50 percent ethanol, n-heptane, and Philadelphia, PA 19103, or may be ex- ethyl acetate. amined at the Office of the Federal (2) Perfluorocarbon resins identified Register, 800 North Capitol Street, in paragraphs (a)(1) and (2) of this sec- NW., suite 700, Washington, DC 20408. tion and intended for use as coatings or The melt viscosity of the perfluorocarbon resins identified in components of coatings shall meet paragraph (a)(1) of this section shall extractability limits prescribed in not vary more than 50 percent within paragraph (e)(3) of this section when one-half hour at 380 °C (716 °F). the resins in the form of coatings de- (ii) Perfluorocarbon resins identified scribed in paragraphs (e)(2) (i) and (ii) in paragraph (a)(2) of this section shall of this section are extracted at reflux have a melt viscosity of not less than temperatures for 2 hours separately 104 poises at 372 °C (702 °F) as deter- with distilled water, 8 percent ethanol, mined by a more detailed method ti- and n-heptane: tled ‘‘Determination of Melt Viscosity, (i) Perfluorocarbon resin coatings Molecular Weight Distribution Index based on resins identified in paragraph and Viscosity Stability,’’ which is in- (a)(1) of this section shall be applied to corporated by reference. Copies are both sides of a 0.025-millimeter (0.001 available from the Center for Food inch) thick aluminum foil to a thick- Safety and Applied Nutrition (HFS– ness of 0.025 millimeter (0.001 inch) 200), Food and Drug Administration, after thermal curing at 399 °C (750 °F) 200 C St. SW., Washington, DC 20204, or available for inspection at the Office of for 10 minutes. If a primer is used, the the Federal Register, 800 North Capitol total thickness of the primer plus top- Street, NW., suite 700, Washington, DC coat shall equal 0.025 millimeter (0.001 20408. inch) after heat curing. (3) Thermal instability index. The ther- (ii) Perfluorocarbon resin coatings mal instability index of the tetra- based on resins identified in paragraph fluoroethylene homopolymer shall not (a)(2) of this section shall be applied to exceed 50 as determined by ASTM both sides of a 0.025-millimeter (0.001 method D1457–56T, ‘‘Test for Thermal inch) thick aluminum foil to a thick- Instablility index of Tetrafluoro- ness of 0.10 millimeter (0.004 inch) after ethylene Homopolymer’’ (Revised 1956), thermal curing at 427 °C (800 °F) for 10 which is incorporated by reference. minutes. If a primer is used, the total Copies are available from University thickness of the primer plus topcoat Microfilms International, 300 N. Zeeb shall equal 0.10 millimeter (0.004 inch) Rd., Ann Arbor, MI 48106, or available after heat curing. for inspection at the Office of the Fed- (3) The extracted surfaces shall meet eral Register, 800 North Capitol Street, the following extractability limits: NW., suite 700, Washington, DC 20408. (i) Total extractives not to exceed 3.1 The requirements of this paragraph do not apply to polytetrafluoroethylene milligrams per square decimeter (0.2 resin lubricant powders described in milligram per square inch). paragraph (c) of this section. (ii) Fluoride extractives calculated as (e) Limitations. 1 (1) Perfluorocarbon- fluorine not to exceed 0.46 milligram molded articles having a surface area per square decimeter (0.03 milligram per square inch). 1 A more detailed procedure of extraction (f) Conditions of use. Perfluorocarbon conditions is entitled, ‘‘Preparation of Ex- resins identified in paragraph (a)(2) of tracts,’’ which is incorporated by reference. Copies are available from the Center for Food Safety and Applied Nutrition (HFS– inspection at the Office of the Federal Reg- 200), Food and Drug Administration, 200 C St. ister, 800 North Capitol Street, NW., suite SW., Washington, DC 20204, or available for 700, Washington, DC 20408.
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this section are limited to use as coat- phenylenecarbonyl-1,4-phenylene) res- ings or components of coatings for arti- ins (CAS Reg. No. 55088–54–5 and CAS cles intended for repeated food-contact Reg. No. 60015–05–6 and commonly re- use. ferred to as polyaryletherketone res- [43 FR 44834, Sept. 29, 1978, as amended at 47 ins) identified in paragraph (a) of this FR 11843, Mar. 19, 1982; 47 FR 14699, Apr. 6, section may be safely used as articles 1982; 49 FR 10109, Mar. 19, 1984; 50 FR 1502, or components of articles intended for Jan. 11, 1985; 54 FR 24898, June 12, 1989; 61 FR repeated use in contact with food, sub- 14481, Apr. 2, 1996] ject to the provisions of this section. (a) Identity. Polyaryletherketone res- § 177.1555 Polyarylate resins. ins consist of basic resins produced by Polyarylate resins (CAS Reg. No. reacting 4,4′-diphenoxy benzophenone 51706–10–6) may be safely used as arti- and terephthaloyl dichloride in such a cles or components of articles intended way that the finished resins have a for use in contact with food in accord- minimum weight average molecular ance with the following prescribed con- weight of 20,000 grams per mole, as de- ditions: termined by light scattering measure- (a) Identity. Polyarylate resins (1, 3- ments in sulfuric acid at room tem- benzenedicarboxylic acid, diphenyl perature. ester, polymer with diphenyl 1,4- (b) Optional adjuvant substances. The benzenedicarboxylate and 4-4′-(1- basic polyaryletherketone resins iden- methylethylidine) bis(phenol)) are tified in paragraph (a) of this section formed by melt polycondensation of may contain optional adjuvant sub- bisphenol-A with diphenylisophthalate stances required in the production of and diphenylterephthalate. such basic resins. These adjuvants may (b) Specifications. (1) The finished co- include substances used in accordance polymers shall contain from 70 to 80 with § 174.5 of this chapter and the fol- weight percent of polymer units de- lowing: rived from diphenylisophthalate and 20 (1) Benzoyl chloride, poly(tetrafluoro to 30 weight percent of polymer units ethylene). derived from diphenylterephthalate. (2) [Reserved] (2) Polyarylate resins shall have a minimum weight average molecular (c) Extractive limitations. The finished weight of 20,000. food-contact article yields net total ex- (3) Polyarylate resins may be identi- tractives in each extracting solvent fied by their characteristic infrared not to exceed 0.052 milligram per spectra. square inch (corresponding to 0.008 mil- (c) Extractive limitations. The finished ligram per square centimeter) of food- polyarylate resins in sheet form at contact surface, when extracted at least 0.5 millimeter (0.020 inch) thick, reflux temperature for 2 hours with the when extracted with water at 121 °C following solvents: Distilled water, 50 (250 °F) for 2 hours, shall yield total percent (by volume) ethyl alcohol in nonvolatile extractives not to exceed distilled water, 3 percent acetic acid 2.33 micrograms per square centimeter (by weight) in distilled water, and n- (15 micrograms per square inch) of the heptane. exposed resin surface. (d) In testing the finished food-con- (d) Limitations. Polyarylate resin ar- tact article made of ticles may be used in contact with all polyaryletherketone resin, use a sepa- foods except beverages containing rate test sample for each required ex- more than 8 volume percent ethanol tracting solvent. under conditions of use A through H, [61 FR 42381, Aug. 15, 1996] described in table 2 of § 176.170(c) of this chapter. § 177.1560 Polyarylsulfone resins. [52 FR 35540, Sept. 22, 1987] Polyarylsulfone resins (CAS Reg. No. 79293–56–4) may be safely used as arti- § 177.1556 Polyaryletherketone resins. cles or components of articles intended The poly(oxy-1,4-phenylenecarbonyl- for use in contact with food, at tem- 1,4-phenyleneoxy-1,4- peratures up to and including normal phenylenecarbonyl-1,4- baking temperatures, in accordance
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with the following prescribed condi- NOTE: In testing the finished polyaryl- tions: sulfone resin use a separate test sample for (a) Identity. Polyarylsulfone resins each required extracting solvent. are copolymers containing not more [50 FR 31046, July 24, 1985] than 25 percent of oxy-p-phenylene- oxy-p-phenylenesulfonyl-p-phenylene § 177.1570 Poly-1-butene resins and polymer units and not less than 75 per- butene/ethylene copolymers. cent of oxy-p-phenylenesulfonyl-p- The poly-1-butene resins and butene/ phenylene-oxy-p-phenylenesulfonyl-p- ethylene copolymers identified in this phenylene polymer units. The copoly- section may be safely used as articles mers have a minimum reduced vis- or components of articles intended for cosity of 0.40 deciliter per gram in 1- use in contact with food subject to the methyl-2-pyrrolidinone in accordance provisions of this section. with ASTM method D2857–70 (Re- (a) Identity. Poly-1-butene resins are approved 1977), ‘‘Standard Test Method produced by the catalytic polymeriza- for Dilute Solution Viscosity of Poly- tion of 1-butene liquid monomer. mers,’’ which is incorporated by ref- Butene/ethylene copolymers are pro- erence. Copies may be obtained from duced by the catalytic polymerization the American Society for Testing and of 1-butene liquid monomer in the pres- Materials, 1916 Race St., Philadelphia, ence of small amounts of ethylene PA 19103, or may be examined at the monomer so as to yield no higher than Office of the Federal Register, 800 a 6-weight percent concentration of North Capitol Street, NW., suite 700, polymer units derived from ethylene in Washington, DC 20408. the copolymer. (b) Poly- (b) Optional adjuvant substances. The Specifications and limitations. 1-butene resins and butene/ethylene co- basic polyarylsulfone resins identified polymers shall conform to the speci- in paragraph (a) of this section may fications prescribed in paragraph (b)(1) contain optional adjuvant substances of this section, and shall meet the required in the production of such extractability limits prescribed in basic copolymers. These optional adju- paragraph (b)(2) of this section. vant substances may include sub- (1) Specifications—(i) Infrared identi- stances permitted for such use by regu- fication. Poly-1-butene resins and lations in parts 170 through 179 of this butene/ethylene copolymers can be chapter, substances generally recog- identified by their characteristic infra- nized as safe in food, substances used in red spectra. accordance with a prior sanction of ap- (ii) Viscosity. Poly-1-butene resins and proval, and substances named in this the butene/ethylene copolymers have paragraph and further identified as re- an intrinsic viscosity 1.0 to 3.2 as deter- quired: mined by ASTM method D1601–78, Substances Limitations ‘‘Standard Test Method for Dilute So- lution Viscosity of Ethylene Poly- Sulfolane ..... Not to exceed 0.15 percent as residual sol- mers,’’ which is incorporated by ref- vent in the finished basic resin. erence. Copies may be obtained from the American Society for Testing Ma- (c) Extractive limitations. The finished terials, 1916 Race St., Philadelphia, PA polyarylsulfone resin when extracted 19103, or may be examined at the Office for 2 hours with the following solvents of the Federal Register, 800 North Cap- at the specified temperatures yields itol Street, NW., suite 700, Washington, total extractives in each extracting DC 20408. solvent not to exceed 0.008 milligram (iii) Density. Poly-1-butene resins per square centimeter of food-contact have a density of 0.904 to 0.920 gms/cm3, surface: distilled water at 121 °C (250 and butene/ethylene copolymers have a °F), 50 percent (by volume) ethyl alco- density of 0.890 to 0.916 gms/cm3 as de- hol in distilled water at 71.1 °C (160 °F), termined by ASTM method D1505–68 3 percent acetic acid in distilled water (Reapproved 1979), ‘‘Standard Test at 100 °C (212 °F), and n-heptane at 65.6 Method for Density of Plastics by the °C (150 °F). Density-Gradient Technique,’’ which is
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incorporated by reference. The avail- § 177.1580 Polycarbonate resins. ability of this incorporation by ref- Polycarbonate resins may be safely erence is given in paragraph (b)(1)(ii) of used as articles or components of arti- this section. cles intended for use in producing, (iv) Melt index. Poly-1-butene resins manufacturing, packing, processing, have a melt index of 0.1 to 24 and the preparing, treating, packaging, trans- butene/ethylene copolymers have a porting, or holding food, in accordance melt index of 0.1 to 20 as determined by with the following prescribed condi- ASTM method D1238–82, condition E, tions: ‘‘Standard Test Method for Flow Rates (a) Polycarbonate resins are poly- of Thermoplastics by Extrusion Plas- esters produced by: tometer,’’ which is incorporated by ref- (1) The condensation of 4,4′-iso- erence. The availability of this incor- propylidenediphenol and carbonyl chlo- poration by reference is given in para- ride to which may have been added cer- graph (b)(1)(ii) of this section. tain optional adjuvant substances re- (2) Limitations. Poly-1-butene resins quired in the production of the resins; and butene/ethylene copolymers for use or by in articles that contact food, and for (2) The reaction of molten 4,4′-iso- articles used for packing or holding propylidenediphenol with molten di- food during cooking shall yield no phenyl carbonate in the presence of the more than the following extractables: ′ (i) Poly-1-butene resins may be used disodium salt of 4,4 -isopro- as articles or components of articles pylidenediphenol. (3) The condensation of 4,4′-isopro- intended for use in contact with food, pylidenediphenol, carbonyl chloride, provided that the maximum and 0.5 percent weight maximum of extractables do not exceed 2.5 percent a2,a6-bis (6-hydroxy-m-tolyl) mesitol to by weight of the polymer when film or which may have been added certain op- molded samples are tested for 2 hours tional adjuvant substances required in at 50 °C (122 °F) in n-heptane. (ii) Butene/ethylene copolymers con- the production of branched taining no more than 6 percent by polycarbonate resins. weight of polymer units derived from (b) The optional adjuvant substances ethylene may be used as articles or required in the production of resins components of articles intended for produced by the methods described in contact with food under conditions of paragraph (a)(1) and (3) of this section use B, C, D, E, F, G, or H described in may include substances generally rec- table 2 of § 176.170(c) of this chapter, ognized as safe in food, substances used subject to the provisions of this section in accordance with a prior sanction or and provided that the maximum approval, and the following: extractables from test films 0.1 to 0.2 List of substances Limitations millimeter (0.004 to 0.008 inch) in thick- ness do not exceed 0.80 percent by p-tert-Butylphenol ...... Chloroform ...... weight of the polymer when extracted p-Cumylphenol (CAS Reg. For use only as a chain ter- in a soxhlet extractor for 6 hours with No. 599Ð64Ð4). minator at a level not to ex- refluxing 95 percent ethanol. ceed 5 percent by weight of the resin. (iii) Poly-1-butene resins may be used Ethylene dichloride. as articles or components of articles Heptane. intended for packaging or holding food Methylene chloride. during cooking, provided that the Monochlorobenzene ...... Not to exceed 500 p.p.m. as residual solvent in finished thickness of such polymers in the form resin. in which they contact food shall not Pentaerythritol tetrastearate For use only as a mold re- exceed 0.1 millimeter (0.004 inch) and (CAS Reg. No. 115Ð83Ð3). lease agent, at a level not to exceed 0.5 percent by yield maximum extractables of not weight of the finished resin. more than 2.5 percent by weight of the Phenol (CAS Reg. No. 108Ð polymer when films are extracted for 2 95Ð2). hours at 50 °C (122 °F) in n-heptane. Pyridine. Toluene: (CAS Reg. No. Not to exceed 800 parts per [42 FR 14572, Mar. 15, 1977, as amended at 49 108Ð88Ð3). million as residual solvent FR 10109, Mar. 19, 1984; 50 FR 31349, Aug. 2, in finished resin. Triethylamine. 1985]
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(c) Polycarbonate resins shall con- by CAS Reg. No. 114096–64–9 when pro- form to the specification prescribed in duced with the use of greater than 2 paragraph (c)(1) of this section and but not greater than 5 weight percent shall meet the extractives limitations p-cumylphenol (CAS Reg. No. 599–64–4), prescribed in paragraph (c)(2) of this as an optional adjuvant substance in section. accordance with paragraph (b)(2) of (1) Specification. Polycarbonate resins this section. can be identified by their char- (b) Optional adjuvants. The optional acteristic infrared spectrum. adjuvant substances required in the (2) Extractives limitations. The production of resins identified in para- polycarbonate resins to be tested shall graph (a) of this section may include: be ground or cut into small particles (1) Substances used in accordance that will pass through a U.S. standard with § 174.5 of this chapter. sieve No. 6 and that will be held on a (2) Substances identified in U.S. standard sieve No. 10. § 177.1580(b). (i) Polycarbonate resins, when ex- (3) Substances regulated in tracted with distilled water at reflux § 178.2010(b) of this chapter for use in temperature for 6 hours, shall yield polycarbonate resins complying with total extractives not to exceed 0.15 per- § 177.1580: cent by weight of the resins. Provided, That the substances are used (ii) Polycarbonate resins, when ex- in accordance with any limitation on tracted with 50 percent (by volume) concentration, conditions of use, and ethyl alcohol in distilled water at food types specified in § 178.2010(b) of reflux temperature for 6 hours, shall this chapter. yield total extractives not to exceed (c) Polyestercarbonate resins shall 0.15 percent by weight of the resins. conform to the specifications pre- (iii) Polycarbonate resins, when ex- scribed in paragraph (c)(1) of this sec- tracted with n-heptane at reflux tem- tion and shall meet the extractive lim- perature for 6 hours, shall yield total itations prescribed in paragraph (c)(2) extractives not to exceed 0.15 percent of this section. by weight of the resins. (1) Specifications. Polyestercarbonate [42 FR 14572, Mar. 15, 1977, as amended at 46 resins identified in paragraph (a) of FR 23227, Apr. 24, 1981; 49 FR 4372, Feb. 6, this section can be identified by their 1984; 50 FR 14096, Apr. 10, 1985; 53 FR 29656, characteristic infrared spectrum. The Aug. 8, 1988; 59 FR 43731, Aug. 25, 1994] resins shall comply with either or both of the following specifications: § 177.1585 Polyestercarbonate resins. (i) The solution intrinsic viscosity of Polyestercarbonate resins may be the polyestercarbonate resins shall be safely used as articles or components a minimum of 0.44 deciliter per gram, of articles intended for use in pro- as determined by a method entitled ducing, manufacturing, packing, proc- ‘‘Intrinsic Viscosity (IV) of Lexan essing, preparing, treating, packaging, Polyestercarbonate Resin by a Single or holding food, in accordance with the Point Method Using Dichloromethane following prescribed conditions: as the Solvent,’’ developed by the Gen- (a) Polyestercarbonate resins (CAS eral Electric Co., September 20, 1985, Reg. No. 71519–80–7) are produced by the which is incorporated by reference in condensation of 4,4′- accordance with 5 U.S.C. 552(a) and 1 isopropylidenediphenol, carbonyl chlo- CFR part 51. Copies are available from ride, terephthaloyl chloride, and the Office of Premarket Approval, Cen- isophthaloyl chloride such that the fin- ter for Food Safety and Applied Nutri- ished resins are composed of 45 to 85 tion (HFS–215), Food and Drug Admin- molepercent ester, of which up to 55 istration, 200 C St. SW., Washington, mole-percent is the terephthaloyl iso- DC 20204, or may be examined at the mer. The resins are manufactured Center for Food Safety and Applied Nu- using a phthaloyl chloride/carbonyl trition’s Library, Food and Drug Ad- chloride mole ratio of 0.81 to 5.7/1 and ministration, 200 C St. SW., rm. 3321, isophthaloyl chloride/terephthaloyl Washington, DC, or at the Office of the chloride mole ratio of 0.81/1 or greater. Federal Register, 800 North Capitol St. The resins are also properly identified NW., suite 700, Washington, DC; or
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(ii) A minimum weight-average mo- chapter, table 1, under Type VIII, in ac- lecular weight of 27,000, as determined cordance with the following prescribed by gel permeation chromatography conditions: using polystyrene standards. (a) For the purpose of this section, (2) Extractives limitations. The polyester elastomers are those pro- polyestercarbonate resins to be tested duced by the ester exchange reaction shall be ground or cut into small par- when one or more of the following ticles that will pass through a U.S. phthalates—dimethyl terephthalate, standard sieve No. 6 and that will be dimethyl orthophthalate, and dimethyl held on U.S. standard sieve No. 10. isophthalate—is made to react with (i) Polyestercarbonate resins, when alpha-hydroomega-hydroxypoly extracted with distilled water at reflux (oxytetramethylene) and/or 1,4- temperature for 6 hours, shall yield butanediol such that the finished elas- total nonvolatile extractives not to ex- tomer has a number average molecular ceed 0.005 percent by weight of the res- weight between 20,000 and 30,000. ins. (b) Optional adjuvant substances em- (ii) Polyestercarbonate resins, when ployed in the production of the poly- extracted with 50 percent (by volume) ester elastomers or added thereto to ethyl alcohol in distilled water at impart desired technical or physical reflux temperature for 6 hours, shall properties may include the following yield total nonvolatile extractives not substances: to exceed 0.005 percent by weight of the resins. List of substances Limitations (iii) Polyestercarbonate resins, when 4,4′ - Bis (alpha, alpha-di- For use only as an anti- extracted with n-heptane at reflux methyl-benzyl) oxidant. temperature for 6 hours, shall yield diphenylamine. total nonvolatile extractives not to ex- Tetrabutyl titanate ...... For use only as a catalyst. ceed 0.002 percent by weight of the res- ins. (c) An appropriate sample of the fin- (3) Residual methylene chloride levels in ished polyester elastomer in the form polyestercarbonate resins. Polyester- in which it contacts food when sub- carbonate resin articles in the finished jected to ASTM method D968–81, form shall not contain residual meth- ‘‘Standard Test Methods for Abrasion ylene chloride in excess of 5 parts per Resistance of Organic Coatings by the million as determined by a method ti- Falling Abrasive Tester,’’ which is in- tled ‘‘Analytical Method for Deter- corporated by reference (copies may be mination of Residual Methylene Chlo- obtained from the American Society ride in Polyestercarbonate Resin,’’ de- for Testing Materials, 1916 Race St., veloped by the General Electric Co., Philadelphia, PA 19103, or may be ex- July 23, 1991, which is incorporated by amined at the Office of the Federal reference in accordance with 5 U.S.C. Register, 800 North Capitol Street, 552(a) and 1 CFR part 51. Copies are NW., suite 700, Washington, DC 20408), available from the Center for Food using No. 50 emery abrasive in lieu of Safety and Applied Nutrition (HFS– Ottawa sand, shall exhibit an abrasion 200), Food and Drug Administration, coefficient of not less than 100 liters 200 C St. SW., Washington, DC 20204, or per mil of thickness. may be examined at the Office of the [42 FR 14572, Mar. 15, 1977, as amended at 49 Federal Register, 800 North Capitol FR 10109, Mar. 19, 1984] Street, NW., suite 700, Washington, DC. § 177.1595 Polyetherimide resin. [57 FR 3940, Feb. 3, 1992, as amended at 64 FR 27178, May 19, 1999] The polyetherimide resin identified in this section may be safely used as an § 177.1590 Polyester elastomers. article or component of an article in- The polyester elastomers identified tended for use in contact with food, in paragraph (a) of this section may be subject to the provisions of this sec- safely used as the food-contact surface tion. of articles intended for use in contact (a) Identity. For the purpose of this with bulk quantities of dry food of the section, the polyetherimide resin is 1,3- type identified in § 176.170(c) of this isobenzofurandione, 5,5′[(1-methyl-
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ethylidene)bis(4,1-phenyleneoxy)] bis- copolymers, containing no more than polymer with 1,3-benzenediamine (CAS 25 weight percent of polymer units de- Reg. No. 61128–46–9), and is derived from rived from methyl acrylate, are made the condensation reaction of m- to react in an aqueous medium with phenylenediamine and bisphenol A- one or more of the following sub- dianhydride. stances: (b) Optional adjuvants. The basic Ammonium hydroxide. polymer identified in paragraph (a) of Calcium carbonate. this section may contain optional adju- Potassium hydroxide. vant substances required in the produc- Sodium hydroxide. tion of basic resins or finished food- (b) The finished food-contact article, contact articles. The optional adjuvant when extracted with the solvent or sol- substances required in the production vents characterizing the type of food of the basic polymer may include sub- and under the conditions of time and stances permitted for such use by ap- temperature characterizing the condi- plicable regulations as set forth in part tions of its intended use as determined 174 of this chapter. from tables 1 and 2 of § 176.170(c) of this (c) Specifications and extractives limi- chapter, yields total extractives in tations—(1) Specifications. each extracting solvent not to exceed Polyetherimide resin identified in 0.5 milligram per square inch of food- paragraph (a) of this section shall have contact surface as determined by the an intrinsic viscosity in chloroform at methods described in § 176.170(d) of this 25 °C (77 °F) of not less than 0.35 deci- chapter; and if the finished food-con- liter per gram as determined by a tact article is itself the subject of a method titled ‘‘Intrinsic Viscosity of regulation in parts 174, 175, 176, 177, 178, ULTEM Polyetherimide Using Chloro- and § 179.45 of this chapter, it shall also form as the Solvent,’’ which is incor- comply with any specifications and porated by reference. Copies are avail- limitations prescribed for it by that able from the Center for Food Safety regulation. In testing the finished food- and Applied Nutrition (HFS–200), Food contact articles, a separate test sample and Drug Administration, 200 C St. is to be used for each required extract- SW., Washington, DC 20204, or available ing solvent. for inspection at the Office of the Fed- (c) The provisions of paragraph (b) of eral Register, 800 North Capitol Street, this section are not applicable to NW., suite 700, Washington, DC 20408. carboxyl-modified polyethylene resins (2) Extractive limitations. Extractive used in food-packaging adhesives com- limitations are applicable to the basic plying with § 175.105 of this chapter. polyetherimide resin in the form of molded discs of thickness 0.16 centi- § 177.1610 Polyethylene, chlorinated. meter (0.063 inch). The resin discs when Chlorinated polyethylene identified ° extracted with distilled water at 121 C in this section may be safely used as ° (250 F) for 2 hours yield total nonvola- articles or components of articles that tile extractives of not more than 12.3 contact food, except for articles used micrograms per square centimeter. for packing or holding food during [50 FR 31351, Aug. 2, 1985; 50 FR 35535, Sept. cooking, subject to the provisions of 3, 1985] this section. (a) For the purpose of this section, § 177.1600 Polyethylene resins, chlorinated polyethylene consists of carboxyl modified. basic polymers produced by the direct Carboxyl-modified polyethylene res- chlorination of polyethylene con- ins may be safely used as the food-con- forming to the density, maximum n- tact surface of articles intended for use hexane extractable fraction, and max- in contact with food in accordance imum xylene soluble fraction specifica- with the following prescribed condi- tions prescribed under item 2.1 of the tions: table in § 177.1520(c). Such chlorinated (a) For the purpose of this section, polyethylene contains a maximum of 60 carboxyl-modified polyethylene resins percent by weight of total chlorine, as consist of basic polymers produced determined by ASTM 1method D1303–55 when ethylene-methyl acrylate basic (Reapproved 1979), ‘‘Standard Test
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Method for Total Chlorine in Vinyl tables 1 and 2 of § 176.170(c) of this chap- Chloride Polymers and Copolymers,’’ ter, yields fluoride ion not to exceed 5 which is incorporated by reference parts per million calculated on the (copies may be obtained from the basis of the volume of food held by the American Society for Testing Mate- food-contact article. rials, 1916 Race St., Philadelphia, PA [48 FR 39057, Aug. 29, 1983] 19103, or may be examined at the Office of the Federal Register, 800 North Cap- § 177.1620 Polyethylene, oxidized. itol Street, NW., suite 700, Washington, Oxidized polyethylene identified in DC 20408), and has a 7.0 percent max- paragraph (a) of this section may be imum extractable fraction in n-hexane safely used as a component of food-con- at 50 °C, as determined by the method tact articles, in accordance with the described in § 177.1520(d)(3)(ii). (b) Chlorinated polyethylene may be following prescribed conditions: (a) Oxidized polyethylene is the basic used in contact with all types of food, resin produced by the mild air oxida- except that when used in contact with tion of polyethylene conforming to the fatty food of Types III, IV–A, V, VII–A, density, maximum n-hexane extract- and IX described in table 1 of § 176.170(c) able fraction, and maximum xylene of this chapter, chlorinated poly- soluble fraction specifications pre- ethylene is limited to use only as a scribed under item 2.3 of the table in modifier admixed at levels not exceed- § 177.1520(c). Such oxidized polyethylene ing 15 weight percent in plastic articles has a minimum number average molec- prepared from polyvinyl chloride and/ ular weight of 1,200, as determined by or from vinyl chloride copolymers com- high temperature vapor pressure os- plying with § 177.1980. mometry, contains a maximum of 5 [42 FR 14572, Mar. 15, 1977, as amended at 49 percent by weight of total oxygen, and FR 10109, Mar. 19, 1984; 59 FR 14550, Mar. 29, has an acid value of 9 to 19. 1994] (b) The finished food-contact article, when extracted with the solvent or sol- § 177.1615 Polyethylene, fluorinated. vents characterizing the type of food Fluorinated polyethylene, identified and under the conditions of time and in paragraph (a) of this section, may be temperature characterizing the condi- safely used as food-contact articles in tions of its intended use as determined accordance with the following pre- from tables 1 and 2 of § 176.170(c) of this scribed conditions: chapter, yields net acidified chloro- (a) Fluorinated polyethylene food- form-soluble extractives not to exceed contact articles are produced by modi- 0.5 milligram per square inch of food- fying the surface of polyethylene arti- contact surface when tested by the cles through action of fluorine gas in methods described in § 177.1330(c), ex- combination with gaseous nitrogen as cept that net acidified chloroform-solu- an inert diluent. Such modification af- ble extractives from paper and paper- fects only the surface of the polymer, board complying with § 176.170 of this leaving the interior unchanged. chapter may be corrected for wax, pet- Fluorinated polyethylene articles are rolatum, and mineral oil as provided in manufactured from basic resins con- § 176.170(d) (5)(iii)(b) of this chapter. If taining not less than 85 weight-percent the finished food-contact article is of polymer units derived from ethylene itself the subject of a regulation in and identified in § 177.1520 (a)(2) and parts 174, 175, 176, 177, 178 and § 179.45 of (3)(i). this chapter, it shall also comply with (b) Fluorinated polyethylene articles any specifications and limitations pre- conform to the specifications and use scribed for it by such regulations. limitations of § 177.1520(c), items 2.1 and (NOTE: In testing the finished food-con- 3.1. tact article, use a separate test sample (c) The finished food-contact article, for each extracting solvent.) when extracted with the solvent or sol- (c) The provisions of this section are vents characterizing the type of food not applicable to oxidized polyethylene and under conditions of time and tem- used as provided in §§ 175.105 and 176.210 perature characterizing the conditions of this chapter, and § 177.2800. The pro- of its intended use as determined from visions of paragraph (b) of this section
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are not applicable to oxidized poly- physical or technical effect or any lim- ethylene used as provided in §§ 175.125 itations further provided. Any sub- and 176.170(a)(5) of this chapter and stance employed in the production of § 177.1200. polyethylene phthalate plastics that is the subject of a regulation in parts 174, § 177.1630 Polyethylene phthalate 175, 176, 177, 178 and 179 of this chapter polymers. conforms with any specification in Polyethylene phthalate polymers such regulation. identified in this section may be safely (e) Substances employed in the pro- used as, or components of plastics duction of polyethylene phthalate plas- (films, articles, or fabric) intended for tics include: use in contact with food in accordance (1) Substances generally recognized with the following prescribed condi- as safe in food. tions: (2) Substances subject to prior sanc- (a) Polyethylene phthalate films con- tion or approval for use in poly- sist of a base sheet of ethylene ethylene phthalate plastics and used in terephthalate polymer, ethylene accordance with such sanction or ap- terephthalate-isophthalate copolymer, proval. or ethylene-1,4-cyclohexylene (3) Substances which by regulation in dimethylene terephthalate copoly- parts 174, 175, 176, 177, 178 and § 179.45 of esters described in § 177.1315(b)(3), to this chapter may be safely used as which have been added optional sub- components of resinous or polymeric stances, either as constituents of the food-contact surfaces subject to the base sheet or as constituents of coat- provisions of such regulation. ings applied to the base sheet. (4) Substances identified in this para- (b) Polyethylene phthalate articles graph (e)(4) subject to the limitations consist of a base polymer of ethylene prescribed: terephthalate polymer, or ethylene-1,4- LIST OF SUBSTANCES AND LIMITATIONS cyclohexylene dimethylene terephthalate copolyesters described in (i) Base sheet: § 177.1315(b)(3), to which have been Ethylene terephthalate copolymers: Pre- added optional substances, either as pared by the condensation of dimethyl constituents of the base polymer or as terephthalate or terephthalic acid with constituents of coatings applied to the ethylene glycol, modified with one or more of the following: Azelaic acid, dimethyl base polymer. azelate, dimethyl sebacate, sebacic acid. (c)(1) Polyethylene phthalate Ethylene terephthalate copolymers: Pre- spunbonded nonwoven fabric consist of pared by the condensation of dimethyl continuous filaments of ethylene terephthalate or terephthalic acid with terephthalate polymer and ethylene ethylene glycol, modified with one or more terephthalate-isophthalate copolymer of the following: Azelaic acid, dimethyl to which may have been added optional azelate, dimethyl sebacate, sebacic acid, adjuvant substances required in their pyromellitic dianhydride. The level of pyromellitic dianhydride shall not exceed preparation and finishing. 0.5 percent by weight of the finished co- (2) The ethylene terephthalate- polymer which may be used under condi- isophthalate copolymer component of tions of use E through H as described in the fabric shall not exceed 25 percent table 2 of § 176.170(c) of this chapter. by weight. The filaments may be blend- Ethylene terephthalate-isophthalate copoly- ed with other fibers regulated for the mers: Prepared by the condensation of di- specific use and the spunbonded fabric methyl terephthalate or terephthalic acid may be further bonded by application and dimethyl isophthalate or isophthalic acid with ethylene glycol. The finished co- of heat and/or pressure. polymers contain either: (3) The fabric shall be used only in (a) 77 to 83 weight percent or accordance with paragraph (i) of this (b) At least 97 weight percent of polymer section. units derived from ethylene (d) The quantity of any optional sub- terephthalate. stance employed in the production of (ii) Base sheet and base polymer: polyethylene phthalate plastics does Ethylene-1,4-cyclohexylene dimethylene not exceed the amount reasonably re- terephthalate copolyesters described in quired to accomplish the intended § 177.1315(b)(3).
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Ethylene terephthalate polymer: Prepared plying with paragraph (a) of this section, by the condensation of dimethyl at levels not to exceed 0.025 gram per terephthalate and ethylene glycol. square meter (0.016 milligram per square Ethylene terephthalate polymer: Prepared inch) of the film, in contact with food of by the condensation of terephthalic acid types VIII and IX in table 1 of § 176.170(c) of and ethylene glycol. this chapter, under use conditions E, F, and G in table 2 of § 176.170(c) of this chap- (iii) Coatings: ter. Acrylic copolymers (CAS Reg. No. 30394–86– 6): Prepared by reaction of ethyl acrylate (iv) Emulsifiers: (CAS Reg. No. 140–88–5), methyl methacry- Sodium dodecylbenzenesulfonate: As an ad- late (CAS Reg. No. 80–62–6), and juvant in the application of coatings to the methacrylamide (CAS Reg. No. 79–39–0) base sheet or base polymer. blended with melamine-formaldehyde resin Sodium lauryl sulfate: As an adjuvant in the (CAS Reg. No. 68002–20–0). For use in coat- application of coatings to the base sheet or ings for polyethylene phthalate films com- base polymer. plying with paragraph (a) of this section.– 2-Sulfoethyl methacrylate, sodium salt (CAS Ethylene azelate-terephthalate copolymer: Reg. No. 1804–87–1). For use only in copoly- The copolymer, dissolved in 1,1,2-trichloro- mer coatings on polyethylene phthalate ethane and/or methylene chloride, may be film under conditions of use E, F, and G de- used as a heat-activated sealant on poly- scribed in table 2 of § 175.300(d) of this chap- ethylene terephthalate film intended for ter, and limited to use at a level not to ex- sealing polyethylene terephthalate pouch- ceed 2.0 percent by weight of the dry co- es that are used as containers of either polymer coating. nonalcoholic beverages or alcoholic bev- erages containing not more than 15 percent (v) Modifier: ethyl alcohol. The copolymer has a 1,4-Benzenedicarboxylic acid, dimethyl ester, terephthalate/azelate molecular ratio of polymer with 1,4-butanediol and α-hydro- 1.25/1.00 and a relative viscosity of not less omega-hydroxypoly(oxy-1,4-butanediyl) than 1.5 as determined by a method title CAS Reg. No. 9078–71–1) meeting the fol- ‘‘General Procedure of Determining the lowing specifications: Relative Viscosity of Resin Polymers,’’ Melting point: 200° to 215 °C as determined which is incorporated by reference. Copies by ASTM method D2117–82, ‘‘Standard are available from the Center for Food Test Method for Melting Point of Safety and Applied Nutrition (HFS–200), Semicrystalline Polymers by the Hot Food and Drug Administration, 200 C St. Stage Microscopy Method,’’ which is in- SW., Washington, DC 20204, or available for corporated by reference. Copies may be inspection, at the Office of the Federal obtained from the American Society for Register, 800 North Capitol Street, NW., Testing Materials, 1916 Race St., Phila- suite 700, Washington, DC 20408. Total re- delphia, PA 19103, or may be examined at sidual copolymer solvent (1,1,2-trichloro- the Office of the Federal Register, 800 ethane and/or methylene chloride) shall North Capitol Street, NW., suite 700, not exceed 0.13 milligram per square inch Washington, DC 20408. of film, and food contact of the film shall Density: 1.15 to 1.20 as determined by ASTM be limited to not more than 1 square inch method D1505–68 (Reapproved 1979), per 250 grams of beverage. ‘‘Standard Test Method for Density of 2-Ethylhexyl acrylate copolymerized with Plastics by the Density-Gradient Tech- one or more of the following: nique,’’ which is incorporated by ref- Acrylonitrile. erence. Copies may be obtained from the Methacrylonitrile. American Society for Testing Materials, Methyl acrylate. 1916 Race St., Philadelphia, PA 19103, or Methyl methacrylate. may be examined at the Office of the Itaconic acid. Federal Register, 800 North Capitol Vinylidene chloride copolymerized with one Street, NW., suite 700, Washington, DC or more of the following: 20408. Methacrylic acid and its methyl, ethyl, The modifier is used at a level not to ex- propyl, butyl, or octyl esters. ceed 5 percent by weight of polyethylene Acrylic acid and its methyl, ethyl, propyl, terephthalate film. The average thick- butyl, or octyl esters. ness of the finished film shall not exceed Acrylonitrile. 0.016 millimeter (0.0006 inch). Methacrylonitrile. Hexanedioic acid polymer with 1,3- Vinyl chloride. benzenedimethanamine (CAS Reg. No. Itaconic acid. 25718–70–1) meeting the specifications in Styrene-maleic anhydride resin, partial 2- § 177.1500(b), item 10, when tested by the butoxyethyl ester, ammonium salt (CAS methods given in § 177.1500(c). The modi- Reg. No. 68890–80–2). For use only as a coat- fier is used in polyethylene terephthalate ing for polyethylene phthalate films com- at a level not to exceed 30 percent by
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weight of the polyethylene from substances identified in para- terephthalate. graphs (e)(4)(i) and (ii) of this section Chloroform-soluble extractives shall not and conforming with the specifications exceed 0.08 milligram/centimeter 2 (0.5 milligram/inch 2) of food-contact surface prescribed in paragraph (h)(1) of this of the modified polyethylene section are used as provided in para- terephthalate article when exposed to graph (h)(2) of this section: the following solvents at temperatures (1) Specifications. (i) The food contact and times indicated: surface, when exposed to distilled (a) Distilled water at 49 °C (120 °F) for 24 hours; water at 250 °F for 2 hours yields chlo- (b) n-Heptane at 49 °C (120 °F) for 24 hours; roform-soluble extractives not to ex- (c) 8 percent ethyl alcohol at 49 °C (120 °F) ceed 0.02 milligram/inch 2 of food con- for 24 hours. tact surface exposed to the solvent; and For use in contact with all types of foods except (a) those containing more than 8 (ii) The food contact surface, when percent alcohol, or (b) those at tempera- exposed to n-heptane at 150 °F for 2 tures over 49 °C (120 °F). hours, yields chloroform-soluble ex- (f) Polyethylene phthalate plastics tractives not to exceed 0.02 milligram/ 2 conforming with the specifications pre- inch of food contact surface exposed scribed in paragraph (f)(1) of this sec- to the solvent. tion are used as provided in paragraph (2) Conditions of use. The plastics are (f)(2) of this section: used to contain foods during oven bak- (1) Specifications. (i) The food contact ing or oven cooking at temperatures surface, when exposed to distilled above 250 °F. water at 250 °F for 2 hours, yields chlo- (i) Polyethylene phthalate fabric, roform-soluble extractives not to ex- identified in paragraph (c) of this sec- ceed 0.5 mg/in 2 of food contact surface tion and conforming with the specifica- exposed to the solvent; and tions prescribed in paragraph (i)(1) of (ii) The food contact surface, when this section, is used only as provided in exposed to n-heptane at 150 °F for 2 paragraph (i)(2) of this section. hours, yields chloroform-soluble ex- (1) Specifications. Chloroform-soluble 2 tractives not to exceed 0.5 mg/in of extractives shall not exceed 0.2 milli- food contact surface exposed to the sol- gram/inch 2 of food-contact surface vent. when exposed to the following solvents (2) Conditions of use. The plastics are at temperatures and times indicated: used for packaging, transporting, or ° holding food, excluding alcoholic bev- (i) Distilled water at 212 F for 2 erages, at temperatures not to exceed hours. 250 °F. (ii) n-Heptane at 150 °F for 2 hours. (g) Polyethylene phthalate plastics (iii) 50 percent ethyl alcohol at 120 °F conforming with the specifications pre- for 24 hours. scribed in paragraph (g)(1) of this sec- (2) Conditions of use. The plastics are tion are used as provided in paragraph intended for: (g)(2) of this section. (i) Dry food contact. (1) Specifications. (i) The food contact (ii) Bulk food (excluding alcoholic surface meets the specifications in beverages) repeated use applications, paragraph (f)(1) of this section; and including filtration, at temperatures (ii) The food contact surface when ex- not exceeding 212 °F. posed to 50 percent ethyl alcohol at 120 (iii) Filtration of bulk alcoholic bev- °F for 24 hours, yields chloroform-solu- erages, not exceeding 50 percent alco- ble extractives not to exceed 0.5 mg/in 2 of food contact surface exposed to the hol by volume, at temperatures not ex- ° solvent. ceeding 120 F. (2) Conditions of use. The plastics are (j) Polyethylene phthalate plastics, used for packaging, transporting, or composed of ethylene terephthalate- holding alcoholic beverages that do not isophthalate containing a minimum of exceed 50 percent alcohol by volume. 98 weight percent of polymer units de- (h) Uncoated polyethylene phthalate rived from ethylene terephthalate, or plastics consisting of a base sheet or ethylene-1,4-cyclohexylene base polymer prepared as prescribed
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dimethylene terephthalate copoly- (1) Optional adjuvant substances au- esters described in § 177.1315(b)(3), con- thorized for this use in accordance with forming with the specifications pre- § 174.5 of this chapter. scribed in paragraph (j)(1) of this sec- (2) Optional finish components, total tion, are used as provided in paragraph weight not to exceed 1 percent by (j)(2) of this section. weight of the base polymer, as follows: (1) Specifications. (i) The food contact surface meets the specifications in List of substances Limitations paragraph (f)(1) of this section and Diundecylphthalate (CAS (ii)(a) Containers with greater than 500 Reg. No. 3648Ð20Ð2). Mono- and dipotassium salts mL capacity. The food-contact surface of lauryl phosphate (CAS when exposed to 95 percent ethanol at Reg. No. 39322Ð78Ð6). 120 °F for 24 hours should not yield o-Phenylphenol (CAS Reg. For use as a fungicide for fin- No. 90Ð43Ð7). ish coating materials. Not chloroform-soluble extractives in ex- to exceed 0.01 percent by cess of 0.005 mg/in 2. weight of the base poly- (b) Containers with less than or equal to mer. 500 mL capacity. The food contact sur- Poly(oxyethylene/ oxypropylen- face when exposed to 95 percent eth- e)monobutylether (CAS anol at 120 °F for 24 hours should not Reg. No. 9038Ð95Ð3). yield chloroform-soluble extractives in Poly(oxyethylene) 2 mono(nonylphenyl)ether excess of 0.05 mg/in . (CAS Reg. No. 9019Ð45Ð (2) Conditions of use. The plastics are 9). used for packaging, transporting, or Polyvinyl methylether (CAS Reg. No. 9003Ð09Ð2). holding alcoholic foods that do not ex- Poly(oxyethylene) sorbitol ceed 95 percent alcohol by volume. monolaurate tetraoleate (CAS Reg. No. 71243Ð28Ð [42 FR 14572, Mar. 15, 1977, as amended at 42 2). FR 18611, Apr. 8, 1977; 44 FR 40886, July 13, Poly(oxyethylene) sorbitol 1979; 45 FR 6541, Jan. 29, 1980; 47 FR 11844, hexaoleate (CAS Reg. No. Mar. 19, 1982; 47 FR 53346, Nov. 26, 1982; 48 FR 57171Ð56Ð9). ′ 30361, July 1, 1983; 49 FR 10110, Mar. 19, 1984; 4,4 -Butylidenebis (6-tert- For use only as an oxidation butyl-m-cresol) (CAS Reg. inhibitor for finish coating 50 FR 31047, July 24, 1985; 51 FR 3772, Jan. 30, No. 85Ð60Ð9). materials. Not to exceed 1986; 52 FR 32917, Sept. 1, 1987; 54 FR 15750, 0.01 percent by weight of Apr. 19, 1989; 54 FR 24898, June 12, 1989; 60 FR the base polymer. 57927, Nov. 24, 1995; 60 FR 61654, Dec. 1, 1995; 61 FR 46718, Sept. 5, 1996] (c) Specifications. (1) Poly(phenyleneterephthalamide) resins § 177.1632 Poly (phenyleneterephthala- in the form of continuous filament mide) resins. yarns or fibers that have been scoured Poly(phenyleneterephthalamide) res- in accordance with paragraph (d)(1) of ins identified in paragraph (a) of this this section, when refluxed in a 50 per- section may be safely used as articles cent ethanol/water mixture for 24 or components of articles intended for hours, yields total extractables not ex- repeated contact with food. ceeding 0.5 percent by weight of the (a) Identity. For the purpose of this sample. section, the poly(phenylene- (2) Poly(phenyleneterephthalamide) terephthalamide) resins (CAS Reg. No. resins in the form of pulp, when 26125–61–1) are produced by the polym- refluxed in a 50 percent ethanol/water erization of terephthalolyl chloride mixture for 24 hours, yields total with p-phenylenediamine. The extractables not exceeding 0.65 percent poly(phenyleneterephthalamide) resin by weight of the sample. fibers and yarns may contain optional (d) Conditions of use. (1) adjuvant substances required in their Poly(phenyleneterephthalamide) resins preparation and finishing. in the form of continuous filament (b) Optional adjuvant substances. The yarns and fibers may be used as compo- poly(phenyleneterephthalamide) resins nents of articles intended for repeated identified in paragraph (a) of this sec- use in contact with food at tempera- tion may contain the following op- tures not to exceed 260 °C (500 °F). All tional adjuvant substances, subject to items are scoured prior to use by agita- any limitation on their use: tion in a water bath containing 0.5
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gram/liter of tetrasodium shall contain not more than 1 weight pyrophosphate and 0.5 percent deter- percent of total residual p- gent. The items are agitated at 80 °C methystyrene monomer, as determined (180 °F) for 20 minutes, and then sub- by a gas chromatographic method ti- jected to a cold water rinse. tled, ‘‘Gas Chromatographic Deter- (2) Poly(phenyleneterephthalamide) mination of PMS and PET in PPMS resins in the form of pulp may be used Basic Polymers,’’ which is incorporated as gaskets and packing for food proc- by reference. Copies are available from essing equipment at temperatures not the Center for Food Safety and Applied to exceed 260 °C (500 °F). Nutrition (HFS–200), Food and Drug [57 FR 3125, Jan. 28, 1992] Administration, 200 C St. SW., Wash- ington, DC 20204, or available for in- § 177.1635 Poly(p-methylstyrene) and spection at the Office of the Federal rubber-modified poly(p-methyl- Register, 800 North Capitol Street, styrene). NW., suite 700, Washington, DC 20408. Poly(p-methylstyrene) and rubber- (2) Rubber-modified poly(p- modified poly(p-methylstyrene) identi- methylstyrene) basic polymers identi- fied in this section may be safely used fied in paragraph (a)(2) of this section as components of articles intended for shall contain not more than 0.5 weight use in contact with food, subject to the percent of total residual p- provisions of this section: methylstyrene monomer, as deter- (a) Identity. For the purposes of this mined by the method identified in section, poly(p-methylstyrene) and paragraph (c)(1) of this section rubber-modified poly(p-methylstyrene) (d) Other specifications and limitations. are basic polymers, manufactured as The poly(p-methylstyrene) and rubber- described in this paragraph, meeting modified poly(p-methylstyrene) identi- the specifications prescribed in para- fied in and complying with this sec- graph (c) of this section. tion, when used as components of the (1) Poly(p-methylstyrene) (CAS Reg. food-contact surface of any article that No. 24936–41–2) polymer produced by the is the subject of a regulation in parts polymerization of p-methylstyrene. 175, 176, 177, 178 and § 179.45 of this chap- (2) Rubber-modified poly(p- ter, shall comply with any specifica- methylstyrene) (CAS Reg. No. 33520–88– tions and limitations prescribed by 6) polymer produced by combining sty- such regulation for the article in the rene-butadiene copolymer and/or finished form in which it is to contact polybutadiene with poly(p- food. methylstyrene), either during or after (e) Conditions of use. Poly(p- polymerization of the poly(p- methylstyrene) basic polymers and methylstyrene), such that the finished rubber-modified poly(p-methylstyrene) polymers contain not less than 75 basic polymers identified in paragraphs weight percent of total polymer units (a)(1) and (a)(2), respectively, of this derived from p-methylstyrene) mon- section shall be used in contact with omer. food only under conditions of use B (b) Optional adjuvants. The basic through H set forth in table 2 of polymers identified in paragraph (a) of § 176.170(c) of this chapter. this section may contain optional adju- [48 FR 31384, July 8, 1983, as amended at 54 vant substances required in the produc- FR 24898, June 12, 1989; 55 FR 52989, Dec. 26, tion of such basic polymers. Such op- 1990] tional adjuvant substances may in- clude substances permitted for such § 177.1637 Poly(oxy-1,2- use by applicable regulations in this ethanediyloxycarbonyl-2,6- chapter, substances generally recog- naphthalenediylcarbonyl) resins. nized as safe in food, substances gen- Poly(oxy-1,2-ethanediyloxycarbonyl- erally recognized as safe in indirect ad- 2,6-naphthalenediylcarbonyl) resins ditives, and substances used in accord- identified in paragraph (a) of this sec- ance with prior sanction or approval. tion may be safely used as articles or (c) Specifications. (1) Poly(p- components of articles intended for use methylstyrene) basic polymers identi- in contact with food in accordance fied in paragraph (a)(1) of this section with the following conditions:
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(a) Identity. For the purpose of this table 2 of § 176.170(c) of this chapter; section, poly(oxy-1,2- and ethanediyloxycarbonyl-2,6- (2) Identified in a manner that will naphthalenediylcarbonyl) resins (CAS differentiate the article from articles Reg. No. 24968–11–4) are polymers made of other polymeric resins to fa- formed by catalytic transesterification cilitate collection and sorting. of 2,6-dimethylnaphthalene [61 FR 14965, Apr. 4, 1996] dicarboxylate with ethylene glycol fol- lowed by catalytic polycondensation. § 177.1640 Polystyrene and rubber- (b) Specifications—(1) Density. The modified polystyrene. density of poly(oxy-1,2- Polystyrene and rubber-modified pol- ethanediyloxycarbonyl-2,6- ystyrene identified in this section may naphthalenediylcarbonyl) resins shall be safely used as components of arti- be between 1.33 and 1.40 grams per cles intended for use in contact with cubic centimeter. food, subject to the provisions of this (2) Inherent viscosity. The finished section. food-contact article shall have a min- (a) Identity. For the purposes of this imum inherent viscosity of 0.55 deci- section, polystyrene and rubber-modi- liter per gram in a solution of 0.1 gram fied polystyrene are basic polymers of polymer in 100 milliliters of a 25/40/ manufactured as described in this para- 35 (weight/weight/weight) solution of p- graph so as to meet the specifications chlorophenol/tetrachloroethane/phenol. prescribed in paragraph (c) of this sec- The viscosity is determined by East- tion when tested by the method de- man Chemical Co.’s method ECD-A-AC- scribed in paragraph (d) of this section. G-V-1-5, ‘‘Determination of Dilute So- (1) Polystyrene consists of basic poly- lution Viscosity of Polyesters,’’ dated mers produced by the polymerization May 31, 1988, which is incorporated by of styrene. reference in accordance with 5 U.S.C. (2) Rubber-modified polystyrene con- 552(a) and 1 CFR part 51. Copies are sists of basic polymers produced by available from the Office of Premarket combining styrene-butadiene copoly- Approval, Center for Food Safety and mers and/or polybutadiene with poly- Applied Nutrition (HFS–215), Food and styrene, either during or after polym- Drug Administration, 200 C St. SW., erization of the polystyrene, such that Washington, DC 20204, or may be exam- the finished basic polymers contain not ined at the Center for Food Safety and less than 75 weight percent of total Applied Nutrition’s Library, Food and polymer units derived from styrene Drug Administration, 200 C St. SW., monomer. rm. 3321, Washington, DC, or at the Of- (b) Optional adjuvants. The basic fice of the Federal Register, 800 North polymers identified in paragraph (a) of Capitol St. NW., Washington, DC. this section may contain optional adju- (c) Extraction limitations. A 0.5 milli- vant substances required in the produc- meter (0.02 inch) thick sheet of resin tion of such basic polymers. Such op- when extracted with water at 121 °C tional adjuvant substances may in- (250 °F) for 2 hours shall yield total clude substances permitted for such nonvolatile extractives not exceeding use by regulations in parts 170 through 2.0 micrograms per square inch of ex- 189 of this chapter, substances gen- posed resin surface. erally recognized as safe in food, and (d) Conditions of use. The finished substances used in accordance with a food contact article shall be: prior sanction or approval. (1) Used in contact only with food of (c) Specifications. (1) Polystyrene Types I, II, IVB, VIA, VIB, VIIB, and basic polymers identified in paragraph VIII identified in table 1 of § 176.170(c) (a)(1) of this section shall contain not of this chapter, under conditions of use more than 1 weight percent of total re- A through H described in table 2 of sidual styrene monomer, as determined § 176.170(c) of this chapter; and with by the method described in paragraph food of Types III, IVA, V, VIC, VIIA, (d) of this section, except that when and IX identified in table 1 of used in contact with fatty foods of § 176.170(c) of this chapter, under condi- Types III, IV-A, V, VII-A, and IX de- tions of use C through H described in scribed in table 1 of § 176.170(c) of this
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chapter, such polystyrene basic poly- (ii) By means of a microliter syringe, mers shall contain not more than 0.5 inject 1 microliter of the standard solu- weight percent of total residual sty- tion into the gas chromatograph. Meas- rene monomer. ure the area of the styrene monomer (2) Rubber-modified polystyrene peak which emerges after approxi- basic polymers identified in paragraph mately 12 minutes. (a)(2) of this section shall contain not (7) Procedure. (i) Transfer 1 gram of more than 0.5 weight percent of total sample (accurately weighed to the residual styrene monomer, as deter- nearest 0.001 gram to a 2-ounce bottle mined by the method described in para- and add several glass beads. Pipette graph (d) of this section. 25.0 milliliters of methylene chloride (d) Analytical method for determination into the bottle. Cap the bottle tightly of total residual styrene monomer con- and place on a mechanical shaker. tent—(1) Scope. This method is suitable Shake until the polymer is completely for the determination of residual sty- dissolved. If any insoluble residue re- rene monomer in all types of styrene mains, allow the bottle to stand (or polymers. centrifuge at a low speed) until a clear supernatant layer appears. (2) Principle. The sample is dissolved (ii) By means of a microliter syringe, in methylene chloride. An aliquot of inject 3 microliters of the clear super- the solution is injected into a gas chro- natant liquid into the gas chro- matograph. The amount of styrene matograph. monomer present is determined from (iii) Measure the area of the resulting the area of the resulting peak. styrene monomer peak. Compare the (3) Apparatus—(i) Gas chromatograph. sample peak area with the area pro- Beckman GC-2A gas chromatograph duced by the standard styrene mon- with hydrogen flame detector or appa- omer solution. Calculation: ratus of equivalent sensitivity. (ii) Chromatograph column. One-quar- Percent residual styrene monomer=Milligrams monomer in stand- ter inch outside diameter stainless ard×peak area of sample/Peak area of mon- steel tubing (0.028 inch wall thickness), omer standard×sample weight in grams×30 4 feet in length, packed with 20 percent polyethylene glycol (20,000 molecular (e) Other specifications and limitations. weight) on alkaline treated 60–80 mesh The polystyrene and rubber-modified firebrick. polystyrene identified in and com- (iii) Recorder. Millivolt range of 0–1, plying with this section, when used as components of the food-contact surface chart speed of 30 inches per hour. of any article that is the subject of a (4) Reagents. Compressed air, purified; regulation in parts 174, 175, 176, 177, 178 helium gas; hydrogen gas; methylene and § 179.45 of this chapter, shall com- chloride, redistilled; and styrene mon- ply with any specifications and limita- omer, redistilled. tions prescribed by such regulation for (5) Operating conditions for the gas the article in the finished form in chromatograph. (i) The column is oper- which it is to contact food. ° ated at a temperature of 100 C with a (f) Nonapplicability. The provisions of helium flow rate of 82 milliliters per this section are not applicable to poly- minute. styrene and rubber-modified poly- (ii) The hydrogen burner is operated styrene used in food-packaging adhe- with 15 pounds per square inch of air sives complying with § 175.105 of this pressure and 7 pounds per square inch chapter. of hydrogen pressure. (iii) The attenuation of the hydrogen § 177.1650 Polysulfide polymer- flame detector is set at 2×102. polyepoxy resins. (6) Standardization. (i) Prepare a Polysulfide polymer-polyepoxy res- standard solution by weighing accu- ins may be safely used as the food-con- rately 15 to 20 milligrams of styrene tact surface of articles intended for monomer into a 2-ounce bottle con- packaging, transporting, holding, or taining 25.0 milliliters of methylene otherwise contacting dry food, in ac- chloride. Cap the bottle tightly and cordance with the following prescribed shake to thoroughly mix the solution. conditions:
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(a) Polysulfide polymer-polyepoxy itol Street, NW., suite 700, Washington, resins are the reaction products of liq- DC 20408), using No. 50 Emery abrasive uid polysulfide polymers and in lieu of Ottawa sand, shall exhibit polyfunctional epoxide resins, cured and abrasion coefficient of not less with the aid of than 20 liters per mil of film thickness. tri(dimethylaminomethyl) phenol, to which have been added certain optional [42 FR 14572, Mar. 15, 1977, as amended at 49 substances to impart desired techno- FR 10110, Mar. 19, 1984] logical properties to the resins. Subject to any limitations prescribed in this § 177.1655 Polysulfone resins. section, the optional substances may Polysulfone resins identified in para- include: graph (a) of this section may be safely (1) Substances generally recognized used as articles or components of arti- as safe in food and food packaging. cles intended for use in contact with (2) Substances the use of which is food, in accordance with the following permitted under applicable regulations prescribed conditions: in this part, prior sanctions, or approv- (a) For the purpose of this section, als. polysulfone resins are: (3) Substances named in this subpara- (1) Poly(oxy-p-phenylenesulfonyl-p- graph and further identified as re- phenyleneoxy-p- quired: phenyleneisopropylidene-p-phenylene) List of substances Limitations resins (CAS Reg. No. 25154–01–2) con- sisting of basic resins produced when Bis(2-chloroethyl) formal. Bis(dichloropropyl) formal ...... Cross-linking agent. the disodium salt of 4,4′- Butyl alcohol ...... Solvent. isopropylidenediphenol is made to Carbon black (channel process). react with 4,4′-dichlorodiphenyl sulfone Chlorinated paraffins ...... Cross-linking agent. Epoxidized linseed oil. in such a way that the finished resins Epoxidized soybean oil. have a minimum number average mo- Epoxy resins (as listed in ¤ 175.300(b)(3)(viii)(a) of this chap- lecular weight of 15,000, as determined ter).. by osmotic pressure in Ethylene glycol monobutyl ether ...... Solvent. monochlorobenzene; or Magnesium chloride. ′ Methyl isobutyl ketone ...... Solvent. (2) 1,1 -Sulfonylbis[4-chlorobenzene] Naphthalene sulfonic acid-formalde- polymer with 4,4′-(1- hyde condensate, sodium salt. methylethylidene)bis[phenol] (min- Sodium dibutyl naphthalene Wetting agent. sulfonate. imum 92 percent) and 4,4′- Sodium hydrosulfide. sulfonylbis[phenol] (maximum 8 per- Sodium polysulfide. cent) (CAS Reg. No. 88285–91–0) pro- β,β′,γ,γ′-Tetrachloro normal propyl Cross-linking agent. ether. duced when a mixture of 4,4′- Titanium dioxide. isopropylidenediphenol (minimum 92 Toluene ...... Solvent. percent) and 4,4′-sulfonylbis[phenol] Trichloroethane ...... Cross-linking agent. 1,2,3-Trichloropropane ...... Do. (maximum 8 percent) is made to react Urea-formaldehyde resins. with 4,4′-dichlorodiphenyl sulfone in Xylene ...... Solvent. such a way that the finished resin has (b) The resins are used as the food- a minimum number average molecular contact surface for dry food. weight of 26,000, as determined by os- (c) An appropriate sample of the fin- motic pressure in dimethylformamide. ished resin in the form in which it con- (b) The basic polysulfone resins iden- tacts food, when subjected to ASTM tified in paragraph (a) of this section method D968–81, ‘‘Standard Test Meth- may contain optional adjuvant sub- ods for Abrasion Resistance of Organic stances required in the production of Coatings by the Falling Abrasive Test- such basic resins. The optional adju- er,’’ which is incorporated by reference vant substances required in the produc- (copies may be obtained from the tion of the basic polysulfone resins American Society for Testing Mate- may include substances described in rials, 1916 Race St., Philadelphia, PA § 174.5(d) of this chapter and the fol- 19103, or may be examined at the Office lowing: of the Federal Register, 800 North Cap-
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List of substances Limitations tion may contain optional adjuvant substances. The quantity of any op- Dimethyl sulfoxide ..... Not to exceed 50 parts per million as residual solvent in finished basic tional adjuvant substance employed in resin in paragraph (a)(1) of this the production of the polymer does not section. exceed the amount reasonably required Monochlorobenzene .. Not to exceed 500 parts per million to accomplish the intended technical as residual solvent in finished basic resin in paragraph (a)(1) of or physical effect. Such adjuvants may this section. include substances generally recog- N-methyl-2- Not to exceed 0.01 percent (100 nized as safe in food, substances used in pyrrolidone. parts per million) as residual sol- vent in finished basic resin in para- accordance with prior sanction, and graph (a)(2) of this section. substances permitted under applicable regulations in this part. (c) Polysulfone resins, when ex- (c) Specifications. (1) Inherent vis- tracted at reflux temperatures for 6 cosity of a 0.50 percent solution of the hours with the solvents—distilled polymer in phenol/tetrachloroethane water, 50 percent (by volume) ethyl al- (60/40 weight ratio) solvent is not less cohol in distilled water, 3 percent ace- than 0.6 as determined using a Wagner tic acid in distilled water, and n- viscometer (or equivalent) and cal- heptane, yield total extractives in each culated from the following equation: extracting solvent not to exceed 0.0078 milligram per square centimeter (0.05 (natural log arithm of N ) Inherent = r milligram per square inch) of resin sur- viscos ity face. Note: In testing the finished (c) polysulfone resins, use a separate resin where: test sample for each required extract- Nr=Ratio of flow time of the polymer solu- ing solvent. tion to that of the solvent and c=polymer (d) Polysulfone resins intended for re- concentration of the test solution in peated use in contact with food may be grams per 100 milliliters. used under conditions of use A through (2) Poly(tetramethylene H in table 2 of § 176.170(c) of this chap- terephthalate) in the finished form in ter. The resins intended for single-serv- which it is to contact food shall yield ice food-contact use may be used only total extractives as follows: under condition of use H described in (i) Not to exceed 0.08 milligram per table 2 of § 176.170(c) of this chapter. square inch of food contact surface when extracted for 2 hours at 250 °F [51 FR 882, Jan. 9, 1986; 51 FR 4165, Feb. 3, 1986; 61 FR 29475, June 11, 1996] with distilled water. (ii) Not to exceed 0.02 milligram per § 177.1660 Poly (tetramethylene square inch of food contact surface terephthalate). when extracted for 2 hours at 150 °F Poly(tetramethylene terephthalate) with n-heptane. (poly (oxytetramethyleneoxyter- (iii) Not to exceed 0.04 milligram per ephthaloyl)) [Chemical Abstracts Serv- square inch of food contact surface ° ice Registry No. 24968–12–5] identified when extracted for 2 hours at 212 F in this section may be safely used as with 3 percent aqueous acetic acid. articles or components of articles in- (iv) Not to exceed 0.02 milligram per tended to contact food, in accordance square inch of food contact surface ° with the following prescribed condi- when extracted for 2 hours at 65.6 C ° tions: (150 F) with 50 percent ethanol. (a) Identity. For the purpose of this [42 FR 14572, Mar. 15, 1977, as amended at 50 section, poly (tetramethylene FR 20748, May 20, 1985; 52 FR 20069, May 29, terephthalate) is the reaction product 1987] of dimethyl terephthalate with 1,4- butanediol to which may have been § 177.1670 Polyvinyl alcohol film. added certain optional substances to Polyvinyl alcohol film may be safely impart desired technological properties used in contact with food of the types to the polymer. identified in § 176.170(c) of this chapter, (b) Optional adjuvant substances. table 1, under Types V, VIII, and IX, in Poly(tetramethylene terephthalate) accordance with the following pre- identified in paragraph (a) of this sec- scribed conditions:
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(a) The polyvinyl alcohol film is pro- 4,4′-Diisocyanato-3,3′-dimethylbiphenyl (bi- duced from polyvinyl alcohol having a tolylene diisocyanate). minimum viscosity of 4 centipoises Diphenylmethane diisocyanate. when a 4-percent aqueous solution is Hexamethylene diisocyanate. ° 3-Isocyanatomethyl - 3,5,5 - trimethylcyclo- tested at 20 C. hexyl isocyanate. (b) The finished food-contact film for 4,4-Methylenebis(cyclohexyl isocyanate). use in contact with Food Types V or Toluene diisocyanate. IX, when extracted with the solvent (2) List of substances: characterizing the type of food and under the conditions of time and tem- Adipic acid. perature characterizing its intended 1,4-Butanediol. use as determined from tables 1 and 2 1,3-Butylene glycol. of § 176.170(c) of this chapter, yields 1,4–Cyclohexane dimethanol (CAS Reg. No. 105–08–8). total extractives not to exceed 0.078 2,2-Dimethyl-1,3-propanediol. milligram per square centimeter (0.5 Ethylene glycol. milligram per square inch) of food-con- 1,6–Hexanediol (CAS Reg. No. 629–11–8).α– tact surface when tested by ASTM Hydro–οµεγα–hydroxypoly(oxy–1,4– method F34–76 (Reapproved 1980), butanediyl) (CAS Reg. No. 25190–06–1). ‘‘Standard Test Method for Liquid Ex- α-Hydro-omega-hydroxypoly (oxytetra- traction of Flexible Barrier Materials,’’ methylene). α α′ which is incorporated by reference. , -(Isopropylidenedi-p-phenylene)bis[omega- hydroxypoly (oxypropylene)(3–4 moles)], Copies may be obtained from the Amer- average molecular weight 675. ican Society for Testing Materials, 1916 Maleic anhydride. Race St., Philadelphia, PA 19103, or Methyl oxirane polymer with oxirane (CAS may be examined at the Office of the Reg. No. 9003–11–6). Federal Register, 800 North Capitol Methyl oxirane polymer with oxirane, ether Street, NW., suite 700, Washington, DC with 1,2,3–propanetriol (CAS Reg. No. 9082– 20408. 00–2). α,α′α″,α′″-Neopentanetetrayltetrakis [omega- (c) The finished food-contact film hydroxypoly (oxypropylene) (1–2 moles)], shall not be used as a component of average molecular weight 400. food containers intended for use in con- Pentaerythritol-linseed oil alcoholysis prod- tact with water. uct. Phthalic anhydride. [42 FR 14572, Mar. 15, 1977, as amended at 49 Polybutylene glycol. FR 10110, Mar. 19, 1984] Polyethyleneadipate modified with ethanol- amine with the molar ratio of the amine to § 177.1680 Polyurethane resins. the adipic acid less than 0.1 to 1. The polyurethane resins identified in Poly(oxycarbonylpentamethylene). ′ paragraph (a) of this section may be Polyoxypropylene ethers of 4.4 -isopropyl- idenediphenol (containing an average of 2– safely used as the food-contact surface 4 moles of propylene oxide). of articles intended for use in contact Polypropylene glycol. with bulk quantities of dry food of the α,α′,α″-1,2,3-Propanetriyltris [omega- type identified in § 176.170(c) of this hydroxypoly (oxypropylene) (15–18 moles)], chapter, table 1, under Type VIII, in ac- average molecular weight 3,000. cordance with the following prescribed Propylene glycol. conditions: α,α′,α″-[Propylidynetris (methylene)] tris (a) For the purpose of this section, [omega-hydroxypoly (oxypropylene) (min- imum 1.5 moles)], minimum molecular polyurethane resins are those produced weight 400. when one or more of the isocyanates α-[ρ(1,1,3,3-Tetramethylbutyl) - phenyl]- listed in paragraph (a)(1) of this section omega-hydroxypoly(oxyethylene) (5 moles), is made to react with one or more of average molecular weight 425. the substances listed in paragraph Trimethylol propane. (a)(2) of this section: (b) Optional adjuvant substances em- (1) Isocyanates: ployed in the production of the poly- Bis(isocyanatomethyl) benzene (CAS Reg. urethane resins or added thereto to im- No. 25854–16–4). part desired technical or physical prop- Bis(isocyanatomethyl) cyclohexane (CAS erties may include the following sub- Reg. No. 38661–72–2). stances:
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List of substances Limitations
1-[(2-Aminoethyl)amino]2-propanol ...... As a curing agent. 1-(3-Chloroallyl)-3,5,7-triaza-1-azoniaadamantane chloride ...... As a preservative. Colorants used in accordance with ¤ 178.3297 of this chapter.. Dibutyltin diacetate ...... As a catalyst. Dibutyltin dichloride ...... Do. Dibutyltin dilaurate ...... Do. N,N-Dimethyldodecylamine ...... Do. N-Dodecylmorpholine ...... Do. a,a′-[Isopropylidenebis[p-phenyleneoxy(2-hydroxytrimethylene) As a stabilizer. ]]bis[omega-hydroxypoly-(oxyethylene) (136Ð170 moles)], av- erage molecular weight 15,000. 4,4′-Methylenedianiline ...... As a curing agent. 1,1′,1″-Nitrilotri-2-propanol ...... Do. 2,2′-(p-Phenylenedioxy) diethanol ...... Do. Polyvinyl isobutyl ether. Polyvinyl methyl ether. Soyaalkyd resin ...... Conforming in composition with ¤ 175.300 of this chapter and containing litharge not to exceed that residual from its use as the reaction catalyst and creosol not to exceed that re- quired as an antioxidant. Tetrakis [methyleneÐ(2,5Ðdi-tert-butyl-4-hydroxyhydrocinna- Stabilizer. mate)]methane (CAS Reg. No. 6683Ð19Ð8). N,N,N′N′-Tetrakis (2-hydroxypropyl)ethylenediamine ...... As a curing agent. Triethanolamine ...... Do. Trimethyleneglycol di (p-aminobenzoate) (CAS Reg. No. As a curing agent. 57609Ð64Ð0).
(c) An appropriate sample of the fin- components of articles intended for use ished resin in the form in which it con- in contact with food, subject to provi- tacts food, when subjected to ASTM sions of this section. method D968–81, ‘‘Standard Test Meth- (a) For the purpose of this section, ods for Abrasion Resistance of Organic styrene block polymers are basic poly- Coatings by the Falling Abrasive Test- mers manufactured as described in this er,’’ which is incorporated by reference paragraph, so that the finished poly- (copies may be obtained from the mers meet the specifications prescribed American Society for Testing Mate- in paragraph (b) of this section, when rials, 1916 Race St., Philadelphia, PA tested by the methods described in 19103, or may be examined at the Office paragraph (c) of this section. of the Federal Register, 800 North Cap- (1) Styrene block polymers with 1,3- itol Street, NW., suite 700, Washington, butadiene are those produced by the DC 20408), using No. 50 Emery abrasive catalytic solution polymerization of in lieu of Ottawa sand, shall exhibit an styrene and 1,3-butadiene. abrasion coefficient of not less than 20 (2) Styrene block polymers with 2- liters per mil of film thickness. methyl-1,3-butadiene are those pro- [42 FR 14572, Mar. 15, 1977, as amended at 46 duced by the catalytic solution polym- FR 57033, Nov. 20, 1981; 49 FR 10110, Mar. 19, erization of styrene and 2-methyl-1,3- 1984; 50 FR 51847, Dec. 20, 1985; 56 FR 15278, butadiene. Apr. 16, 1991; 56 FR 42933, Aug. 30, 1991] (3) Styrene block polymers with 1,3- butadiene, hydrogenated are those pro- § 177.1810 Styrene block polymers. duced by the catalytic solution polym- The styrene block polymers identi- erization of styrene and 1,3-butadiene, fied in paragraph (a) of this section and subsequently hydrogenated. may be safely used as articles or as (b) Specifications:
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Maximum extract- Maximum extract- able fraction in dis- able fraction in 50 Molecular Glass transi- tilled water at spec- percent ethanol at Styrene block polymers weight Solubility tion points ified temperatures, specified tempera- (minimum) times, and tures, times, and thicknesses thicknesses
1. (i) Styrene block polymers with 1,3- 29,000 Completely ¥98 °C 0.0039 mg/cm2 0.002 mg/cm2 (0.01 butadiene; for use as articles or as soluble in (¥144 °F) (0.025 mg/in2) of mg/in2) of sur- components of articles that contact toluene. to ¥71 °C surface at reflux face at 66 °C food of Types I, II, IVÐB, VI, VIIÐB, (¥96 °F) temperature for (150 °F) for 2 hr and VIII identified in table 1 in and 86 °C 30 min on a 0.19 on a 0.19 cm ¤ 176.170(c) of this chapter under (187 °F) to cm (0.075 in) (0.075 in) thick conditions of use D, E, F, and G de- 122 °C thick sample. sample. scribed in table 2 in ¤ 176.170(c) of (252 °F). this chapter. (ii) Styrene block polymers with 1,3-bu- 29,000 ...... do ...... do ...... do ...... Do. tadiene; for use as components of pressure-sensitive adhesives that contact food of Types I, II, IVÐB, VI, VIIÐB, and VIII identified in table 1 in ¤ 176.170(c) of this chapter under conditions of use C, D, E, F and G described in table 2 in ¤ 176.170(c) of this chapter, provided the pressure- sensitive adhesives be applied only to closure tapes for sealing con- tainers having a capacity of not less than 160 cc (5.5 fluid ounces) and that the area of the adhesive ex- posed to food shall not exceed 4.03 cm2 (0.625 in2). The pressure-sen- sitive adhesive may contain terpene resins as identified in ¤ 175.125(b)(2) of this chapter. 2. Styrene block polymers with 2-meth- 29,000 ...... do ...... ¥65 °C (¥85 0.002 mg/cm2 (0.01 0.002 mg/cm2 (0.01 yl-1,3-butadiene; for use as articles °F) to ¥47 mg/in2) of sur- mg/in2) of sur- or as components of articles that °C (¥53 face at reflux face at 66 °C contact food of Types I, II, IVÐB, VI, °F) and 86 temperature for 2 (150 °F) for 2 hr VIIÐB, and VIII identified in table 1 in °C (187 hr on a 0.071 cm on a 0.071 cm ¤ 176.170(c) of this chapter. °F) to 122 (0.028 in) thick (0.028 in) thick °C (252 sample. (Option- sample. (Option- °F). ally, maximum ally, maximum net residue solu- net residue solu- ble in chloroform ble in chloroform shall not exceed shall not exceed 0.00020 mg/cm2 0.00040 mg/cm2 (0.0013 mg/in2) (0.0025 mg/in2) of surface.). of surface.) 3. (i) Styrene block polymers with 1,3- 16,000 ...... do ...... -50 °C (-58 0.002 mg/cm2 (0.01 0.002 mg/cm2 (0.01 butadiene, hydrogenated (CAS Reg. °F) to -30 mg/in2) of sur- mg/in2) of sur- No. 66070Ð58Ð4): for use as articles °C (-22 °F) face at reflux face at 66 °C or as components of articles that and 92 °C temperature for 2 (150 °F) for 2 hr contact food of Types I, II, IVÐB, VI, (198 °F) to hr on a 0.071 cm on a 0.071 cm VIIÐB, and VIII identified in table 1 in 98 °C (208 (0.028 in) thick (0.028 in) thick ¤ 176.170(c) of this chapter. °F). sample. sample. (ii) Styrene block polymers with 1,3-bu- 16,000 ...... do ...... do ...... do ...... Do. tadiene, hydrogenated (CAS Reg. No. 66070Ð58Ð4): for use at levels not to exceed 42.4 percent by weight as a component of closures with sealing gaskets that would contact food of Types III, IVÐA, V, VIIÐA, VIII, and IX identified in table 1 in ¤ 176.170(c) of this chapter, and in condition of use D as described under table 2 in ¤ 176.170(c) of this chapter.
(c) The analytical methods for deter- and are applicable to the finished poly- mining whether styrene block poly- mer. mers conform to the specifications pre- scribed in this section are as follows
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(1) Molecular weight. Molecular cured for 30 minutes at 153 °C to accen- weight shall be determined by intrinsic tuate the upper transition point. viscosity (or other suitable method). (3) Maximum extractable fractions in (2) Glass transition points. The glass distilled water and 50 percent ethanol and transition points shall be determined the maximum net residue solubles in chlo- by either of the following methods: roform. The maximum extractable frac- (i) ASTM method D2236–70 (‘‘Stand- tions in distilled water and 50 percent ard Method of Test for Dynamic Me- ethanol, and the maximum net residue chanical Properties of Plastics by solubles in chloroform, shall be deter- Means of Torsional Pendulum,’’ which mined in accordance with § 176.170(d)(3) is incorporated by reference; copies are of this chapter using a sandwich form available from American Society for of the finished copolymer of the speci- Testing and Materials (ASTM), 1916 fied thickness and for the time and Race Street, Philadelphia, PA 19103, or temperature specified in paragraph (b) available for inspection at the Office of of this section. the Federal Register, 800 North Capitol (d) The provisions of this section are Street, NW., suite 700, Washington, DC not applicable to butadiene-styrene co- 20408) modified by using a forced reso- polymers listed in other sections of nant vibration instead of a fixed vibra- this subpart. tion and by using frequencies of 25 to 40 (e) The provisions of this section are cycles per second instead of 0.1 to 10 not applicable to styrene block poly- cycles per second. mers with 1,3-butadiene listed in (ii) Direct reading viscoelastometric § 175.105 of this chapter. method titled ‘‘Direct Reading Viscoelastrometric Method for Deter- [42 FR 14572, Mar. 15, 1977, as amended at 42 mining Glass Transition Points of Sty- FR 43621, Aug. 30, 1977; 47 FR 11844, Mar. 19, rene Block Polymers’’ (which is incor- 1982; 51 FR 16828, May 7, 1986; 54 FR 24898, porated by reference; copies are avail- June 12, 1989; 58 FR 65546, Dec. 15, 1993] able from the Center for Food Safety and Applied Nutrition (HFS–200), Food § 177.1820 Styrene-maleic anhydride copolymers. and Drug Administration, 200 C St. SW., Washington, DC 20204, or available Styrene-maleic anhydride copoly- for inspection at the Office of the Fed- mers identified in paragraph (a) of this eral Register, 800 North Capitol Street, section may be safely used as articles NW., suite 700, Washington, DC 20408), or components of articles intended for by which the glass transition points use in contact with food, subject to are determined in the tensile mode of provisions of this section. deformation at a frequency of 35 hertz (a) For the purpose of this section, using a Rheovibron Model DDV–II (or styrene-maleic anhydride copolymers equivalent) Direct Reading are those produced by the polymeriza- Viscoelastometer. Take maxima in the tion of styrene and maleic anhydride so out-of-phase component of the complex that the finished polymers meet the modulus as the glass transition points. specifications prescribed in paragraph For block polymers of low styrene con- (b) of this section, when tested by the tent or for simple block polymers, the methods described in paragraph (c) of polymer may be treated with 0.3 part this section. per hundred dicumyl peroxide and (b) Specifications:
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Maximum extract- Maximum extract- Molecular Residual able fraction in dis- able fraction in n- weight Residual sty- maleic anhy- tilled water at spec- heptane at speci- Styrene-maleic copolymers (minimum rene mon- dride mon- ified temperatures, fied temperatures, number omer omer times, and particle times, and particle average) size size
1. Styrene-maleic anhydride copoly- 70,000 0.3 weight 0.1 weight 0.006 weight per- 0.02 weight percent mers containing not more than 15 pct percent. percent. cent at reflux at 73 °F for 2 hr maleic anhydride units by weight; for temperature for 1 utilizing particles use as articles or as components of hr utilizing par- of a size that will articles that contact food of Types I, ticles of a size pass through a II, III, IVÐA, IVÐB, V, VIÐB (except that will pass U.S. standard carbonated beverages), VIIÐA, VIIÐB, through a U.S. sieve No. 10 and VIII, and IX identified in table 1 in standard sieve will be held on a ¤ 176.170(c) of this chapter under No. 10 and will U.S. standard conditions of use B, C, D, E, F, G, be held on a sieve No. 20. and H described in table 2 in U.S. standard ¤ 176.170(c) of this chapter. sieve No. 20. 2. Styrene-maleic anhydride copolymer ...... 0.3 ...... 0.1 ...... 0.015 weight per- 1.0 weight percent modified with butadiene, (CAS Reg. cent at reflux at 23 °C (73 °F) No. 27288Ð99Ð9) containing not temperature for 1 for 2 hours uti- more than 15 percent maleic anhy- hour utilizing par- lizing particles of dride units by weight and not more ticles of a size a size that will than 20 percent styrene-butadiene that will pass pass through a and/or butadiene rubber units by through a U.S. U.S. standard weight; for use (except carbonated standard sieve sieve No. 10 and beverage bottles) as articles or as No. 10 and will will be held on a components of articles that contact be held on a U.S. standard food of Types I, II, III, IVÐA, IVÐB, V, U.S. standard sieve No. 20. VI, VIIÐA, VIIÐB, VIII, and IX identi- sieve No. 20. fied in table I in ¤ 176.170(c) of this chapter under conditions of use B, C, D, E, F, G, and H described in table 2 in ¤ 176.170(c) of this chapter.
(c) The analytical methods for deter- dride copolymers listed in other sec- mining conformance with specifica- tions of this subpart. tions for styrene-maleic anhydride co- [42 FR 14572, Mar. 15, 1977, as amended at 47 polymers prescribed in this section are FR 11844, Mar. 19, 1982; 47 FR 14698, Apr. 6, as follows: 1982; 54 FR 24898, June 12, 1989] (1) Molecular weight. Molecular weight shall be determined by mem- § 177.1830 Styrene-methyl methacry- brane osmometry. late copolymers. (2) Residual styrene monomer content. Styrene-methyl methacrylate co- Residual styrene monomer content polymers identified in this section may shall be determined by the method de- be safely used as components of plastic scribed in § 177.1640(d). articles intended for use in contact (3) Residual maleic anhydride monomer with food, subject to the provisions of content. Residual maleic anhydride this section. monomer content shall be determined (a) For the purpose of this section, by a gas chromatographic method ti- styrene-methyl methacrylate copoly- tled ‘‘Determination of Residual Ma- mers consist of basic copolymers pro- leic Anhydride in Polymers by Gas duced by the copolymerization of sty- Chromatography,’’ which is incor- rene and methyl methacrylate such porated by reference. Copies are avail- that the finished basic copolymers con- able from the Center for Food Safety tain more than 50 weight percent of and Applied Nutrition (HFS–200), Food polymer units derived from styrene. and Drug Administration, 200 C St. (b) The finished plastic food-contact SW., Washington, DC 20204, or available article, when extracted with the sol- for inspection at the Office of the Fed- vent or solvents characterizing the eral Register, 800 North Capitol Street, type of food and under the conditions NW., suite 700, Washington, DC 20408. of time and temperature characterizing (d) The provisions of this section are the conditions of intended use as deter- not applicable to styrene-maleic anhy- mined from tables 1 and 2 of § 176.170(c)
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of this chapter, yields extractives not this section are used as prescribed in to exceed the following when tested by paragraph (d)(2) of this section. the methods prescribed in § 177.1010(c); (1) Conditions of test. Textryls, when (1) Total nonvolatile extractives not extracted with distilled water at reflux to exceed 0.3 milligram per square inch temperature for 1 hour, yield total ex- of surface tested. tractives not to exceed 1 percent. (2) Potassium permanganate oxidiz- (2) Uses. Textryls are used for pack- able distilled water and 8 and 50 per- aging or holding food at ordinary tem- cent alcohol extractives not to exceed peratures and in the brewing of hot an absorbance of 0.15. beverages. (3) Ultraviolet-absorbing distilled water and 8 and 50 percent alcohol ex- § 177.1900 Urea-formaldehyde resins in tractives not to exceed an absorbance molded articles. of 0.30. Urea-formaldehyde resins may be (4) Ultraviolet-absorbing n-heptane safely used as the food-contact surface extractives not to exceed an absorb- of molded articles intended for use in ance of 0.40. contact with food, in accordance with the following prescribed conditions: § 177.1850 Textryls. (a) For the purpose of this section, Textryls identified in this section urea-formaldehyde resins are those may be safely used as articles or com- produced when 1 mole of urea is made ponents of articles, intended for use in to react with not more than 2 moles of producing, manufacturing, packing, formaldehyde in water solution. processing, preparing, treating, pack- (b) The resins may be mixed with re- aging, transporting or holding food, fined wood pulp and the mixture may subject to the provisions of this sec- contain other optional adjuvant sub- tion. stances which may include the fol- (a) Textryls are nonwoven sheets pre- lowing: pared from natural or synthetic fibers, bonded with fibryl (Fibryl consists of a List of substances Limitations polymeric resin in fibrous form com- Hexamethylenetetramine ...... For use only as polymeriza- mingled with fiber to facilitate sheet tion-control agent. formation and subsequently heat cured Tetrachlorophthalic acid an- Do. to fuse the fibryl and effect bonding). hydride. (b) Textryls are prepared from the fi- Zinc stearate ...... For use as lubricant. bers, fibryls, and adjuvants identified (c) The finished food-contact article, in paragraph (c) of this section, and when extracted with the solvent or sol- subject to limitations prescribed in vents characterizing the type of food that paragraph, provided that any sub- and under the conditions of time and stance that is the subject of a regula- temperature characterizing the condi- tion in parts 174, 175, 176, 177, 178 and tions of its intended use as determined § 179.45 of this chapter conforms with from tables 1 and 2 of § 175.300(d) of this any specifications in such regulation chapter, yields total extractives in for that substance as a component of each extracting solvent not to exceed polymeric resins used as food contact 0.5 milligram per square inch of food- surfaces. contact surface as determined by the (c) The fibers, fibryls, and adjuvants methods described in § 175.300(e) of this permitted are as follows: chapter. Substances Limitations NOTE: In testing the finished food-contact article, use a separate test sample for each (1) Fibers prepared from pol- Conforming with ¤ 177.1630. required extracting solvent. yethylene terephthalate resins. (2) Fibryls prepared from As the basic polymer. § 177.1950 Vinyl chloride-ethylene co- vinyl chloride-vinyl acetate polymers. copolymer. (3) Adjuvant substance, As a solvent in the prepara- The vinyl chloride-ethylene copoly- dimethylformamide. tion of fibryl. mers identified in paragraph (a) of this section may be safely used as compo- (d) Textryls meeting the conditions nents of articles intended for contact of test prescribed in paragraph (d)(1) of with food, under conditions of use D, E,
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F, or G described in table 2 of § 176.170 (iii) Total extractives obtained by ex- (c) of this chapter, subject to the provi- tracting with water at 150 °F for 2 sions of this section. hours contain no more than 0.5 milli- (a) For the purpose of this section, gram of vinyl chloride-ethylene copol- vinyl chloride-ethylene copolymers ymer per 100 grams of sample tested as consist of basic copolymers produced determined from the organic chlorine by the copolymerization of vinyl chlo- content. The organic chlorine content ride and ethylene such that the fin- is determined as described in paragraph ished basic copolymers meet the speci- (d)(3) of this section. fications and extractives limitations (d) Analytical methods: The analyt- prescribed in paragraph (c) of this sec- ical methods for determining whether tion, when tested by the methods de- vinyl chloride-ethylene basic copoly- scribed in paragraph (d) of this section. mers conform to the extractives limi- (b) The basic vinyl chloride-ethylene tations prescribed in paragraph (c) of copolymers identified in paragraph (a) this section are as follows and are ap- of this section may contain optional plicable to the basic copolymers in adjuvant substances required in the powder form having a particle size such production of such basic copolymers. that 100 percent will pass through a The optional adjuvant substances re- U.S. Standard Sieve No. 40 and 80 per- quired in the production of the basic cent will pass through a U.S. Standard vinyl chloride-ethylene copolymers Sieve No. 80: may include substances permitted for (1) Reagents—(i) Water. All water used such use by regulations in parts 170 in these procedures shall be through 189 of this chapter, substances demineralized (deionized), freshly dis- generally recognized as safe in food, tilled water. and substances used in accordance with a prior sanction or approval. (ii) n-Heptane. Reagent grade, freshly (c) The vinyl chloride-ethylene basic distilled n-heptane shall be used. copolymers meet the following speci- (2) Determination of total amount of ex- fications and extractives limitations: tractives. All determinations shall be (1) Specifications. (i) Total chlorine done in duplicate using duplicate content is in the range of 53 to 56 per- blanks. Approximately 400 grams of cent as determined by any suitable an- sample (accurately weighed) shall be alytical procedure of generally accept- placed in a 2-liter Erlenmeyer flask. ed applicability. Add 1,200 milliliters of solvent and (ii) Intrinsic viscosity in cover the flask with aluminum foil. cyclohexanone at 30 °C is not less than The covered flask and contents are sus- 0.50 deciliter per gram as determined pended in a thermostated bath and are by ASTM method D1243–79, ‘‘Standard kept, with continual shaking at 150 °F Test Method for Dilute Solution Vis- for 2 hours. The solution is then fil- cosity of Vinyl Chloride Polymers,’’ tered through a No. 42 Whatman filter which is incorporated by reference. paper, and the filtrate is collected in a Copies may be obtained from the Amer- graduated cylinder. The total amount ican Society for Testing Materials, 1916 of filtrate (without washing) is meas- Race St., Philadelphia, PA 19103, or ured and called A milliliters. The fil- may be examined at the Office of the trate is transferred to a Pyrex (or Federal Register, 800 North Capitol equivalent) beaker and evaporated on a Street, NW., suite 700, Washington, DC steam bath under a stream of nitrogen 20408. to a small volume (approximately 50–60 (2) Extractives limitations. The fol- milliliters). The concentrated filtrate lowing extractives limitations are de- is then quantitatively transferred to a termined by the methods described in tared 100-milliliter Pyrex beaker using paragraph (d) of this section: small, fresh portions of solvent and a (i) Total extractives do not exceed rubber policeman to effect the transfer. 0.10 weight-percent when extracted The concentrated filtrate is evaporated with n-heptane at 150 °F for 2 hours. almost to dryness on a hotplate under (ii) Total extractives do not exceed nitrogen, and is then transferred to a 0.03 weight-percent when extracted drying oven at 230 °F in the case of the with water at 150 °F for 2 hours. aqueous extract or to a vacuum oven at
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150 °F in the case of the heptane ex- tract, it is overnight under vacuum at tract. In the case of the aqueous ex- 150 °F. The residue is weighed and cor- tract, the evaporation to constant rected for the solvent blank. Calcula- weight is completed in 15 minutes at tion: 230 °F; and in the case of heptane ex-
Gramsof corrected residue 1, 200 milliliters Total extractives expressed as ××=100 Grams of sample Volume of filtrate percent by weight of sample. A in milliliters
(3) Vinyl chloride-ethylene copolymer evaporated carefully on a steam plate content of aqueous extract—(i) Principle. to a volume of approximately 50 milli- The vinyl chloride-ethylene copolymer liters and then transferred quan- content of the aqueous extract can be titatively, a little at a time, to a clean determined by determining the organic 22-milliliter Parr cup, also on the chlorine content and calculating the steam plate. The solution is evaporated amount of copolymer equivalent to the to dryness. Next 0.25 gram of sucrose organic chlorine content. and 0.5 gram of benzoic acid are added (ii) Total organic chlorine content. A to the cup. One scoop (approximately weighed sample of approximately 400 15 grams) of sodium peroxide is then grams is extracted with 1,200 milliliters added to the cup. The bomb is assem- of water at 150 °F for 2 hours, filtered, bled and ignition is conducted in the and the volume of filtrate is measured usual fashion. (A milliliters) as described in para- (d) After the bomb has cooled, it is graph (d)(2) of this section. rinsed thoroughly with distilled water (a) A slurry of Amberlite IRA–400, or and disassembled. The top of the bomb equivalent, is made with distilled is rinsed into a 250-milliliter beaker water in a 150-milliliter beaker. The with distilled water. The beaker is slurry is added to a chromatographic placed on the steam plate. The bomb column until it is filled to about half cup is placed in the beaker and care- its length. This should give a volume of resin of 15–25 milliliters. The liquid fully tipped over to allow the water to must not be allowed to drain below the leach out the combustion mixture. top of the packed column. After the bubbling has stopped, the cup (b) The column is regenerated to the is removed from the beaker and rinsed basic (OH) form by slowly passing thoroughly. The solution is cooled to through it (10–15 milliliters per minute) room temperature and cautiously neu- 10 grams of sodium hydroxide dissolved tralized with concentrated nitric acid in 200 milliliters of water. The column by slowly pouring the acid down a stir- is washed with distilled water until the ring rod until the bubbling ceases. The effluent is neutral to phenolphthalein. solution is cooled and an equal volume One drop of methyl red indicator is of acetone is added. added to the A milliliters of filtered (e) The solution is titrated with 0.005 aqueous extract and, if on the basic N silver nitrate using standard poten- side (yellow), nitric acid is added drop tiometric titration techniques with a by drop until the solution turns pink. silver electrode as indicator and a po- (c) The extract is deionized by pass- tassium nitrate modified calomel elec- ing it through the exchange column at trode as a reference electrode. An ex- a rate of 10–15 milliliters per minute. panded scale recording titrimeter. The column is washed with 200 milli- Metrohm Potentiograph 2336 or equiva- liters of distilled water. The deionized lent, should be used; a complete blank extract and washings are collected in a must be run in duplicate. 1,500-milliliter beaker. The solution is (iii) Calculations.
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Milligrams of aqueous extracted TF××64.3 = ×100 copolymer per 100-gram sample Weight of sample in grams
where: (1) Specifications. (i) Total chlorine T=Milliliters of silver nitrate (sample minus content is 53 to 56 percent as deter- blank)×normality of silver nitrate. mined by any suitable analytical pro- F=1,200/A (as defined above) cedure of generally accepted applica- (e) The vinyl chloride-ethylene co- bility. polymers identified in and complying (ii) Inherent viscosity in ° with this section, when used as compo- cyclohexanone at 30 C is not less than nents of the food-contact surface of 0.59 deciliters per gram as determined any article that is the subject of a reg- by ASTM method D1243–79, ‘‘Standard ulation in parts 174, 175, 176, 177, 178 Test Method for Dilute Solution Vis- and § 179.45 of this chapter, shall com- cosity of Vinyl Chloride Polymers,’’ ply with any specifications and limita- which is incorporated by reference. tions prescribed by such regulation for Copies may be obtained from the Amer- the article in the finished form in ican Society for Testing Materials, 1916 which it is to contact food. Race St., Philadelphia, PA 19103, or (f) The provisions of this section are may be examined at the Office of the not applicable to vinyl chloride-ethyl- Federal Register, 800 North Capitol ene copolymers used as provided in Street, NW., suite 700, Washington, DC §§ 175.105 and 176.180 of this chapter. 20408. (2) Extractives limitations. The fol- [42 FR 14572, Mar. 15, 1977, as amended at 49 lowing extractives limitations are de- FR 10110, Mar. 19, 1984] termined by the methods prescribed in § 177.1970(d). § 177.1960 Vinyl chloride-hexene-1 co- polymers. (i) Total extractives do not exceed 0.01 weight percent when extracted The vinyl chloride-hexene-1 copoly- with water at 150 °F for 2 hours. mers identified in paragraph (a) of this (ii) Total extractives do not exceed section or as components of articles in- 0.30 weight percent when extracted tended for use in contact with food, with n-heptane at 150 °F for 2 hours. under conditions of use D, E, F, or G (c) Other specifications and limitations. described in table 2 of § 176.170(c) of this The vinyl chloride-hexene-1 copoly- chapter, subject to the provisions of mers identified in and complying with this section. this section, when used as components (a) Identity. For the purposes of this of the food-contact surface of any arti- section vinyl chloride-hexene-1 copoly- cle that is subject to a regulation in mers consist of basic copolymers pro- parts 174, 175, 176, 177, 178 and § 179.45 of duced by the copolymerization of vinyl this chapter, shall comply with any chloride and hexene-1 such that the fin- specifications and limitations pre- ished copolymers contain not more scribed by such regulation for the arti- than 3 mole-percent of polymer units cle in the finished form in which it is derived from hexene-1 and meet the to contact food. specifications and extractives limita- tions prescribed in paragraph (b) of this [42 FR 14572, Mar. 15, 1977, as amended at 49 section. The copolymers may option- FR 10110, Mar. 19, 1984] ally contain hydroxypropyl methyl- cellulose and trichloroethylene used as § 177.1970 Vinyl chloride-lauryl vinyl a suspending agent and chain transfer ether copolymers. agent, respectively, in their produc- The vinyl chloride-lauryl vinyl ether tion. copolymers identified in paragraph (a) (b) Specifications and limitations. The of this section may be used as an arti- vinyl chloride-hexene-1 basic copoly- cle or as a component of an article in- mers meet the following specifications tended for use in contact with food sub- and extractives limitations: ject to the provisions of this section.
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(a) Identity. For the purposes of this (d) Analytical methods. The analytical section vinyl chloride-lauryl vinyl methods for determining total extrac- ether copolymers consist of basic co- tives are applicable to the basic co- polymers produced by the copolym- polymers in powder form having a par- erization of vinyl chloride and lauryl ticle size such that 100 percent will vinyl ether such that the finished co- pass through a U.S. Standard Sieve No. polymers contain not more than 3 40 and such that not more than 10 per- weight-percent of polymer units de- cent will pass through a U.S. Standard rived from lauryl vinyl ether and meet Sieve No. 200. the specifications and extractives limi- (1) Reagents—(i) Water. All water used tations prescribed in paragraph (c) of in these procedures shall be this section. demineralized (deionized), freshly dis- (b) Optional adjuvant substances. The tilled water. basic vinyl chloride-lauryl vinyl ether (ii) n-Heptane. Reagent grade, freshly copolymers identified in paragraph (a) distilled n-heptane shall be used. of this section may contain optional (2) Determination of total amount of ex- adjuvant substances required in the tractives. Place an accurately weighed production of such basic copolymers. sample of suitable size in a clean These optional adjuvant substances borosilicate flask, and for each gram of may include substances permitted for sample add 3 milliliters of solvent pre- such use by regulations in parts 170 viously heated to 150 °F. Maintain the through 189 of this chapter, substances temperature of the contents of the generally recognized as safe in food, flask at 150 °F for 2 hours using a hot and substances used in accordance with plate while also maintaining gentle a prior sanction or approval. mechanical agitation. Filter the con- (c) Specifications and limitations. The tents of the flask rapidly through No. vinyl chloride-lauryl vinyl ether basic 42 Whatman filter paper with the aid of copolymers meet the following speci- suction. Transfer the filtrate to flat fications and extractives limitations: glass dishes that are warmed on a hot (1) Specifications. (i) Total chlorine plate and evaporate the solvent with content is 53 to 56 percent as deter- the aid of a stream of filtered air. When mined by any suitable analytical pro- the volume of the filtrate has been re- cedure of generally accepted applica- duced to 10 to 15 milliliters, transfer bility. the filtrate to tared 50-milliliter (ii) Inherent viscosity in borosilicate glass beakers and com- ° cylcoHhexanone at 30 C is not less plete evaporation to a constant weight than 0.60 deciliter per gram as deter- in a 140 °F vacuum oven. Carry out a mined by ASTM method D1243–79, corresponding blank determination ‘‘Standard Test Method for Dilute So- with each solvent. Determine the lution Viscosity of Vinyl Chloride weight of the residue corrected for the Polymers,’’ which is incorporated by solvent blank and calculate the result reference. Copies may be obtained from as percent of the initial weight of the the American Society for Testing Ma- resin sample taken for analysis. terials, 1916 Race St., Philadelphia, PA 19103, or may be examined at the Office (e) Other specifications and limitations. of the Federal Register, 800 North Cap- The vinyl chloride-lauryl vinyl ether itol Street, NW., suite 700, Washington, copolymers identified in and complying DC 20408. with this section, when used as compo- (2) Extractives limitations. The fol- nents of the food-contact surface of lowing extractives limitations are de- any article that is subject to a regula- termined by the method described in tion in parts 174, 175, 176, 177, 178 and paragraph (d) of this section: § 179.45 of this chapter, shall comply (i) Total extractives do not exceed with any specifications and limitations 0.03 weight-percent when extracted prescribed by such regulation for the with water at 150 °F for 2 hours. article in the finished form in which it is to contact food. (ii) Total extractives do not exceed 0.60 weight-percent when extracted [42 FR 14572, Mar. 15, 1977, as amended at 49 with n-heptane at 150 °F for 2 hours. FR 10110, Mar. 19, 1984]
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§ 177.1980 Vinyl chloride-propylene co- (i) Total extractives do not exceed polymers. 0.10 weight-percent when extracted The vinyl chloride-propylene copoly- with n-heptane at 150 °F for 2 hours. mers identified in paragraph (a) of this (ii) Total extractives do not exceed section may be safely used as compo- 0.03 weight-percent when extracted nents of articles intended for contact with water at 150 °F for 2 hours. with food, subject to the provisions of (iii) Total extractives obtained by ex- this section. tracting with water at 150 °F for 2 (a) For the purpose of this section, hours contain no more than 0.17 milli- vinyl chloride-propylene copolymers gram of vinyl chloride-propylene co- consist of basic copolymers produced polymer per 100 grams of sample tested by the copolymezation of vinyl chlo- as determined from the organic chlo- ride and propylene such that the fin- rine content. For the purpose of this ished basic copolymers meet the speci- section, the organic chlorine content is fications and extractives limitations the difference between the total chlo- prescribed in paragraph (c) of this sec- rine and ionic chlorine contents deter- tion, when tested by the methods de- mined as described in paragraph (d) of scribed in paragraph (d) of this section. this section. (b) The basic vinyl chloride-pro- (d) Analytical methods: The analyt- pylene copolymers identified in para- ical methods for determining whether graph (a) of this section may contain vinyl chloride-propylene basic copoly- optional adjuvant substances required mers conform to the extractives limi- in the production of such basic copoly- tations prescribed in paragraph (c) of mers. The optional adjuvant sub- this section are as follows and are ap- stances required in the production of plicable to the basic copolymers in the basic vinyl chloride-propylene co- powder form having a particle size such polymers may include substances per- that 100 percent will pass through a mitted for such use by regulations in U.S. Standard Sieve No. 40 and 80 per- parts 170 through 189 of this chapter, cent will pass through a U.S. Standard substances generally recognized as safe Sieve No. 80: in food, and substances used in accord- (1) Reagents—(i) Water. All water used ance with a prior sanction or approval. in these procedures shall be (c) The vinyl chloride-propylene demineralized (deionized), freshly dis- basic copolymers meet the following tilled water. specifications and extractives limita- (ii) n-Heptane. Reagent grade, freshly tions: distilled n-heptane shall be used. (1) Specifications. (i) Total chlorine (2) Determination of total amount of ex- content is in the range of 53 to 56 per- tractives. All determinations shall be cent as determined by any suitable an- done in duplicate using duplicate alytical procedure of generally accept- blanks. Approximately 400 grams of ed applicability. sample (accurately weighed) shall be (ii) Intrinsic viscosity in cyclo- placed in a 2-liter Erlenmeyer flask. hexanone at 30 °C is not less than 0.50 Add 1,200 milliliters of solvent and deciliter per gram as determined by cover the flask with aluminum foil. ASTM method D1243–79, ‘‘Standard The covered flask and contents are sus- Test Method for Dilute Solution Vis- pended in a thermostated bath and are cosity of Vinyl Chloride Polymers,’’ kept, with continual shaking, at 150 °F which is incorporated by reference. for 2 hours. The solution is then fil- Copies may be obtained from the Amer- tered through a No. 42 Whatman filter ican Society for Testing Materials, 1916 paper, and the filtrate is collected in a Race St., Philadelphia, PA 19103, or graduated cylinder. The total amount may be examined at the Office of the of filtrate (without washing) is meas- Federal Register, 800 North Capitol ured and called A milliliters. The fil- Street, NW., suite 700, Washington, DC trate is transferred to a Pyrex (or 20408. equivalent) beaker and evaporated on a (2) Extractives limitations. The fol- steam bath under a stream of nitrogen lowing extractives limitations are de- to a small volume (approximately 50–60 termined by the methods described in milliliters). The concentrated filtrate paragraph (d) of this section: is then quantitatively transferred to a
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tared 100-milliliter Pyrex beaker using tract. In the case of the aqueous ex- small, fresh portions of solvent and a tract the evaporation to constant rubber policeman to effect the transfer. weight is completed in 15 minutes at The concentrated filtrate is evaporated 230 °F; and in the case of heptane ex- almost to dryness on a hotplate under tract, it is overnight under vacuum at nitrogen, and is then transferred to a 150 °F. The residue is weighed and cor- drying oven at 230 °F in the case of the rected for the solvent blank. Calcula- aqueous extract or to a vacuum oven at tion: 150 °F in the case of the heptane ex-
Gramsof corrected residue 1, 200 milliliters Total extractives expressed as ××=100 Grams of sample Volume of filtrate percent by weight of sample. A in milliliters
(3) Vinyl chloride-propylene copolymer ducted in the usual fashion using a content of aqueous extract—(i) Principle. Meeker burner. The heating is contin- The vinyl chloride-propylene copoly- ued for 1 minute after the water at the mer content of the aqueous extract can top has evaporated. The bomb is be determined by determining the or- quenched in water, rinsed with distilled ganic chlorine content and calculating water, and placed in a 400-milliliter the amount of copolymer equivalent to beaker. The bomb cover is rinsed with the organic chlorine content. The or- water, catching the washings in the ganic chlorine content is the difference same 400-milliliter beaker. The bomb is between the total chlorine content and covered with distilled water and a the ionic chlorine content. watch glass and heated until the melt (ii) Total chlorine content. A weighed has dissolved. The bomb is removed, sample is extracted with water at 150 rinsed, catching the rinsings in the °F for 2 hours, filtered, and the volume beaker, and the solution is acidified of filtrate is measured (A milliliters) as with concentrated nitric acid using described in paragraph (d)(2) of this section. Two drops of 50 percent by methyl purple as an indicator. The weight sodium hydroxide solution are beaker is covered with a watch glass, added to prevent loss of chloride from and the contents are boiled gently for ammonium chloride, if present, and the 10–15 minutes. After cooling to room solution is evaporated to approxi- temperature the solution is made mately 15 milliliters. The concentrated slightly alkaline with 50 percent by filtrate is quantitatively transferred to weight sodium hydroxide solution, a 22-milliliter Parr bomb fusion cup then acidified with dilute (1:5) nitric and gently evaporated to dryness. To acid. Then 1.5 milliliters of 2 N nitric the contents of the cup are added 3.5 acid per 100 milliliters of solution is grams of granular sodium peroxide, 0.1 added and the solution is titrated with gram of powdered starch, and 0.02 gram 0.005 N silver nitrate to the equivalence potassium nitrate; and the contents potential end point using an expanded are mixed thoroughly. The bomb is as- scale pH meter (Beckman Model 76, or sembled, water is added to the recess at equivalent). A complete blank must be the top of the bomb and ignition is con- run in duplicate. Calculation:
Grams of sample 1,200 milliliters Milliequivalents of total chlorine in ××=100 (B− C) Volume of filtrate aqueous extract of 100 grams of sample A in milliliters
where: A=volume of filtrate obtained in extraction.
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B=milliliters of silver nitrate solution used mately 150 milliliters. The solution is in sample titration×normality of silver quantitatively transferred to a 250-mil- nitrate solution. liliter beaker, methyl purple indicator C=milliliters of silver nitrate solution used in blank titration×normality of silver ni- is added, and the solution is neutral- trate solution. ized with 0.1 N nitric acid. For each 100 milliliters of solution is added 1.5 mil- (iii) Ionic chlorine content. A weighed sample is extracted with water at 150 liliters of 2 N nitric acid. The solution °F for 2 hours, filtered, and the volume is titrated with 0.005 N silver nitrate to of filtrate is measured (A milliliters) as the equivalence potential end point, in paragraph (d)(2) of this section. Two using the expanded scale pH meter de- drops of 50 percent by weight sodium scribed in paragraph (d)(3)(ii) of this hydroxide solution are added and the section. A complete blank must be run solution is evaporated to approxi- in duplicate. Calculation:
DE− 1, 200 milliliters Milliequivalents of ionic chlorine in ××=100 Grams of sample Volume of filtrate aqueousextract of100 gramsof sample. A in milliliters
where: (e) The vinyl chloride-propylene co- A=volume of filtrate obtained in extraction. polymers identified in and complying D=milliliters of silver nitrate solution used with this section, when used as compo- in sample titration×normality of silver nents of the food-contact surface of nitrate solution. any article that is the subject of a reg- E=milliliters of silver nitrate solution used ulation in parts 174, 175, 176, 177, 178 in blank titration×normality of silver ni- and § 179.45 of this chapter, shall com- trate solution. ply with any specifications and limita- (iv) Organic chlorine content and vinyl tions prescribed by such regulation for chloride-propylene copolymer content of the article in the finished form in which it is to contact food. aqueous extract. The organic chlorine (f) The provisions of this section are content and the vinyl chloride pro- not applicable to vinyl chloride-pro- pylene copolymer content of the aque- pylene copolymers used in food-pack- ous extract is calculated as follows: aging adhesives complying with (a) Organic chlorine content. Milli- § 175.105 of this chapter. equivalents of organic chlorine in aqueous extract of 100 grams of sample [42 FR 14572, Mar. 15, 1977, as amended at 49 FR 10111, Mar. 19, 1984] equal milliequivalents of total chlorine in aqueous extract of 100 grams of sam- § 177.1990 Vinylidene chloride/methyl ple (as calculated in paragraph (d)(3)(ii) acrylate copolymers. of this section) minus milliequivalents The vinylidene chloride/methyl acry- of ionic chlorine in aqueous extract of late copolymers (CAS Reg. No. 25038– 100 grams of sample (as calculated in 72–6) identified in paragraph (a) of this paragraph (d)(3)(iii) of this section). section may be safely used as an article (b) Vinyl chloride-propylene copolymer or as a component of an article in- content. Milligrams of vinyl chloride- tended for use in contact with food sub- propylene copolymer in aqueous ex- ject to the provisions of this section. tract of 100 grams of sample equal (a) Identity. For the purposes of this milliequivalents of organic chlorine in section vinylidene chloride/methyl ac- aqueous extract of 100 grams of sample rylate copolymers consist of basic co- (as calculated in paragraph (d)(3)(iv) (a) polymers produced by the copolym- of this section) multiplied by 84.5. erization of vinylidene chloride and NOTE: The conversion factor, 84.5, is de- methyl acrylate such that the copoly- rived from the equivalent weight of chlorine mers contain not more than 15 weight- divided by the chlorine content of the percent of polymer units derived from heptane extractable fraction.) methyl acrylate.
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(b) Optional adjuvant substances. The termination of Residual Vinylidene basic vinylidene chloride/methyl acry- Chloride and Methyl Acrylate in Vinyl- late copolymers identified in paragraph idene Chloride/Methyl Acrylate Co- (a) of this section may contain optional polymer Resins and Films,’’ or, alter- adjuvant substances required in the natively, ‘‘Residual Methyl Acrylate production of such basic copolymers. and Vinylidene Chloride Monomers in These optional adjuvant substances Saran MA/VDC Resins and Pellets by may include substances permitted for Headspace Gas Chromatography,’’ such use by regulations in parts 170 dated March 3, 1986, which are incor- through 179 of this chapter, substances porated by reference in accordance generally recognized as safe in food, with 5 U.S.C. 552(a). Copies are avail- and substances used in accordance with able from the Center for Food Safety a prior sanction or approval. and Applied Nutrition (HFS–200), Food (c) Specifications. (1) The methyl acry- and Drug Administration, 200 C St. late content is determined by an infra- SW., Washington, DC 20204, or available red spectrophotometric method titled for inspection at the Office of the Fed- ‘‘Determination of Copolymer Ratio in Vinylidene Chloride/Methyl Acrylate eral Register, 800 North Capitol Street, Copolymers,’’ which is incorporated by NW., suite 700, Washington, DC 20408. reference. Copies are available from (d) Extractives limitations. The basic the Center for Food Safety and Applied copolymer resin in the form of granules Nutrition (HFS–200), Food and Drug that will pass through a U.S. Standard Administration, 200 C St. SW., Wash- Sieve No. 45 (350 microns) shall meet ington, DC 20204, or available for in- the following extractives limitations: spection at the Office of the Federal (1) 10-gram samples of the resin, Register, 800 North Capitol Street, when extracted separately with 100 NW., suite 700, Washington, DC 20408. milliliters of distilled water at 121 °C (2) The weight average molecular (250 °F) for 2 hours, and 100 milliliters weight of the copolymer is not less of n-heptane at 66 °C (150 °F) for 2 than 50,000 when determined by gel per- hours, shall yield total nonvolatile ex- meation chromatography using tetra- tractives not to exceed 0.5 percent by hydrofuran as the solvent. The gel per- weight of the resin. meation chromatograph is calibrated (2) The basic copolymer in the form with polystyrene standards. The basic of film when extracted separately with gel permeation chromatographic meth- distilled water at 121 °C (250 °F) for 2 od is described in ANSI/ASTM D3536–76, hours shall yield total nonvolatile ex- ‘‘Standard Test Method for Molecular tractives not to exceed 0.047 milligram Weight Averages and Molecular Weight per square centimeter (0.3 milligram Distribution of Polystyrene by Liquid per square inch). Exclusion Chromatography (Gel Per- (e) Conditions of use. The copolymers meation Chromatography-GPC),’’ may be safely used as articles or com- which is incorporated by reference. ponents of articles intended for use in Copies are available from University Microfilms International, 300 North producing, manufacturing, processing, Zeeb Rd., Ann Arbor, MI 48106, or avail- preparing, treating, packaging, trans- able for inspection at the Office of the porting, or holding food, including Federal Register, 800 North Capitol processing of packaged food at tem- Street, NW., suite 700, Washington, DC peratures not to exceed 135 °C (275 °F). 20408. (f) Other specifications and limitations. (3) Residual vinylidene chloride and The vinylidene chloride-methyl acry- residual methyl acrylate in the copoly- late copolymers identified in and com- mer in the form in which it will con- plying with this section, when used as tact food (unsupported film, barrier components of the food contact surface layer, or as a copolymer for blending) of any article that is subject to a regu- will not exceed 10 parts per million and lation in parts 174 through 178 and 5 parts per million, respectively, as de- § 179.45 of this chapter, shall comply termined by either a gas with any specifications and limitations chromatographic method titled ‘‘De- prescribed by such regulation for the
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article in the finished form in which it rived from methyl acrylate monomer is to contact food. and not more than 6 weight percent of polymer units derived from methyl [48 FR 38605, Aug. 25, 1983; 48 FR 50077, Oct. 31, 1983, as amended at 53 FR 47185, Nov. 22, methacrylate monomer. 1988; 54 FR 24898, June 12, 1989] (ii) The basic polymers are limited to a thickness of not more than 0.005 cen- § 177.2000 Vinylidene chloride/methyl timeter (0.002 inches). acrylate/methyl methacrylate poly- (2) The weight average molecular mers. weight of the basic polymer is not less The vinylidene chloride/methyl acry- than 100,000 when determined by gel late/methyl methacrylate polymers permeation chromatography using tet- (CAS Reg. No. 34364–83–5) identified in rahydrofuran as the solvent. The gel paragraph (a) of this section may be permeation chromatography is cali- safely used as articles or as a compo- brated with polystyrene standards. The nent of articles intended for use in con- basic gel permeation chromatographic tact with food subject to the provisions method is described in ANSI/ASTM of this section. D3536–76, which is incorporated by ref- (a) Identity. For the purpose of this erence. Copies are available from the section, vinylidene chloride/methyl ac- American Society for Testing Mate- rylate/methyl methacrylate polymers rials, 1916 Race St., Philadelphia, PA consist of basic polymers produced by 19103, or available for inspection at the the copolymerization of vinylidene Office of the Federal Register, 800 chloride/methyl acrylate/methyl meth- North Capitol Street, NW., suite 700, acrylate such that the basic polymers Washington, DC 20408. or the finished food-contact articles (3) The basic polymer or food-contact meet the specifications prescribed in article described in paragraph (a) of paragraph (d) of this section. this section, when extracted with the (b) Optional adjuvant substances. The solvent or solvents characterizing the basic vinylidene chloride/methyl acry- type of food and under the conditions late/methyl methacrylate polymers of time and temperature characterizing identified in paragraph (a) of this sec- the conditions of its intended use as de- tion may contain optional adjuvant termined from tables 1 and 2 of substances required in the production § 176.170(c) of this chapter, yields net of such basic polymers. These optional chloroform-soluble extractives in each adjuvant substances may include sub- extracting solvent not to exceed .08 stances permitted for such use by regu- milligram per square centimeter (0.5 lations in parts 170 through 179 of this milligram per square inch) of food-con- chapter, substances generally recog- tact surface when tested by the meth- nized as safe in food, and substances ods described in § 176.170(d). If the fin- used in accordance with a prior sanc- ished food-contact article is itself the tion of approval. subject of a regulation in parts 174 (c) Conditions of use. The polymers through 178 and § 179.45 of this chapter, may be safely used as articles or as it shall also comply with any specifica- components of articles intended for use tions and limitations prescribed for it in producing, manufacturing, proc- by the regulation. essing, preparing, treating, packaging, [49 FR 29578, July 23, 1984] transporting, or holding food, including processing of packaged food at tem- peratures up to 121 °C (250 °F). Subpart C—Substances for Use (d) Specifications and limitations. The Only as Components of Arti- vinylidene chloride/methyl acrylate/ cles Intended for Repeated methyl methacrylate basic polymers Use and/or finished food-contact articles meet the following specifications and § 177.2210 Ethylene polymer, chloro- limitations: sulfonated. (1)(i) The basic vinylidene chloride/ Ethylene polymer, chlorosulfonated methyl acrylate/methyl methacrylate as identified in this section may be polymers contain not more than 2 safely used as an article or component weight percent of polymer units de- of articles intended for use in contact
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with food, subject to the provisions of may be safely used, subject to the pro- this section. visions of this section, to remove par- (a) Ethylene polymer, chloro- ticles of insoluble matter in producing, sulfonated is produced by chloro- manufacturing, processing, and pre- sulfonation of a carbon tetrachloride paring bulk quantities of liquid food. solution of polyethylene with chlorine (a) Microporous polymeric filters and sulfuryl chloride. consist of a suitably permeable, contin- (b) Ethylene polymer, chloro- uous, polymeric matrix of polyvinyl sulfonated shall meet the following chloride, vinyl chloride-propylene, or specifications: vinyl chloride-vinyl acetate, in which (1) Chlorine not to exceed 25 percent finely divided silicon dioxide is embed- by weight. ded. Cyclohexanone may be used as a (2) Sulfur not to exceed 1.15 percent solvent in the production of the filters. by weight. (b) Any substance employed in the (3) Molecular weight is in the range production of microporous polymeric of 95,000 to 125,000. filters that is the subject of a regula- Methods for the specifications in this tion in parts 170 through 189 of this paragraph (b), titled ‘‘Chlorine and chapter must conform with any speci- Bromine—Coulometric Titration Meth- fication in such regulation. od by Aminco Chloridometer,’’ (c) Cyclohexanone when used as a sol- ‘‘Hypolon Synthetic Rubber—Deter- vent in the production of the filters mination of Sulfur by Parr Bomb,’’ and shall not exceed 0.35 percent by weight ASTM method D2857–70 (Reapproved of the microporous polymeric filters. 1977), ‘‘Standard Test Method for Di- (d) The microporous polymeric filters lute Solution Viscosity of Polymers,’’ may be colored with colorants used in are incorporated by reference. Copies accordance with § 178.3297 of this chap- of the ASTM method may be obtained ter. from the American Society for Testing (e) The temperature of food being Materials, 1916 Race St., Philadelphia, processed through the microporous pol- ° PA 19103. Copies of the other two meth- ymeric filters shall not exceed 180 F. ods are available from the Center for (f) The microporous polymeric filters Food Safety and Applied Nutrition shall be maintained in a sanitary man- (HFS–200), Food and Drug Administra- ner in accordance with good manufac- tion, 200 C St. SW., Washington, DC turing practice so as to prevent poten- 20204. Copies of all three methods may tial microbial adulteration of the food. be examined at the Office of the Fed- (g) To assure safe use of the micro- eral Register, 800 North Capitol Street, porous polymeric filters, the label or NW., suite 700, Washington, DC 20408. labeling shall include adequate direc- (c) The additive is used as the article, tions for a pre-use treatment, con- or a component of articles, intended for sisting of washing with a minimum of use as liners and covers for reservoirs 2 gallons of potable water at a tem- intended for the storage of water for perature of 180 °F for each square foot drinking purposes. of filter, prior to the filter’s first use in (d) Substances permitted by § 177.2600 contact with food. may be employed in the preparation of [42 FR 14572, Mar. 15, 1977, as amended at 56 ethylene polymers, chlorosulfonated, FR 42933, Aug. 30, 1991] subject to any limitations prescribed therein. § 177.2260 Filters, resin-bonded. (e) The finished ethylene copolymers, Resin-bonded filters may be safely chlorosulfonated shall conform to used in producing, manufacturing, § 177.2600(e) and (g). processing, and preparing food, subject [42 FR 14572, Mar. 15, 1977, as amended at 49 to the provisions of this section. FR 10111, Mar. 19, 1984; 54 FR 24898, June 12, (a) Resin-bonded filters are prepared 1989] from natural or synthetic fibers to which have been added substances re- § 177.2250 Filters, microporous poly- quired in their preparation and fin- meric. ishing, and which are bonded with res- Microporous polymeric filters identi- ins prepared by condensation or polym- fied in paragraph (a) of this section erization of resin-forming materials,
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together with adjuvant substances re- Fatty acid (C10-C18) mono- and diesters of quired in their preparation, applica- polyoxyethylene glycol (molecular weight tion, and curing. 400–3,000). (b) The quantity of any substance Methyl esters of fatty acids (C10-C18). Mineral oil. employed in the production of the Polybutene, hydrogenated; complying with resin-bonded filter does not exceed the the identity prescribed under § 178.3740 (b) amount reasonably required to accom- of this chapter. plish the intended physical or technical Polyoxyethylene (4 mols) ethylenediamine effect or any limitation further pro- monolauramide for use only in lubricant vided. formulations for rayon fiber finishing and (c) Any substance employed in the at a usage level not to exceed 10 percent by production of resin-bonded filters that weight of the lubricant formulations. is the subject of a regulation in parts Ricebran oil. Titanium dioxide. 174, 175, 176, 177, 178 and § 179.45 of this chapter conforms with any specifica- (3) Resins: tion in such regulation. Acrylic polymers produced by polymerizing (d) Substances employed in the pro- ethyl acrylate alone or with one or more of duction of resin-bonded filters include the monomers: Acrylic acid, acrylonitrile, the following, subject to any limita- N-methylolacrylamide, and styrene. The tions provided: finished copolymers shall contain at least 70 weight percent of polymer units derived LIST OF SUBSTANCES AND LIMITATIONS from ethyl acrylate, no more than 2 weight percent of total polymer units derived (1) Fibers: from acrylic acid, no more than 10 weight Cellulose pulp. percent of total polymer units derived Cotton. from acrylonitrile, no more than 2 weight Nylon. (From nylon resins complying with percent of total polymer units derived the provisions of applicable regulations in from N-methylolacrylamide, and no more subchapter B of this chapter. than 25 weight percent of total polymer Polyethylene terephthalate complying in units derived from styrene. For use only as composition with the provisions of provided in paragraph (m) of this section. § 177.1630; for use in inline filtration only as Melamine-formaldehyde. provided for in paragraphs (e) and (f) of Melamine-formaldehyde chemically modified this section. with one or more of the amine catalysts Rayon (viscose). identified in § 175.300(b)(3)(xiii) of this chap- ter. (2) Substances employed in fiber fin- Melamine-formaldehyde chemically modified ishing: with methyl alcohol. Melamine-formaldehyde chemically modified BHT. with urea; for use only as provided for in Butyl (or isobutyl) palmitate or stearate. paragraphs (e), (f), (g), (h), and (i) of this 2,5-Di-tert-butyl hydroquinone for use only in section. lubricant formulations for rayon fiber fin- Phenol-formaldehyde resins. ishing and at a usage level not to exceed Polyvinyl alcohol. 0.1 percent by weight of the lubricant for- Polyvinyl alcohol with the copolymer of mulations. acrylic acid-allyl sucrose. Dimethylpolysiloxane. Polyvinyl alcohol with melamine formalde- 4-Ethyl-4-hexadecyl morpholinium ethyl sul- hyde. fate for use only as a lubricant in the man- Polyvinyl acetate with melamine formalde- ufacture of polyethylene terephthalate fi- hyde. bers specified in paragraph (d)(1) of this p--Toluenesulfonamide-formaldehyde chemi- section at a level not to exceed 0.03 percent cally modified with one or more of the by weight of the finished fibers. amine catalysts identified in § 175.300 Fatty acid (C -C ) diethanolamide conden- 10 18 (b)(3)(xiii) of this chapter. sates. Fatty acids derived from animal or vegetable (4) Adjuvant substances: fats and oils, and salts of such acids, sin- gle or mixed, as follows: Dimethyl polysiloxane with methylcellulose Aluminum. and sorbic acid (as an antifoaming agent). Ammonium. Phosphoric acid. Calcium. Magnesium. (5) Colorants: Colorants used in ac- Potassium. cordance with § 178.3297 of this chapter. Sodium. (e) Resin-bonded filters conforming Triethanolamine. with the specifications of paragraph (e)
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(1) of this section are used as provided nonalcoholic, aqueous foods having a in paragraph (e)(2) of this section: pH above 5.0. (1) Total extractives. The finished fil- (j) Resin-bonded filters conforming ter, when exposed to distilled water at with the specifications of paragraph (j) 100 °F for 2 hours, yields total extrac- (1) of this section are used as provided tives not to exceed 2.8 percent by in paragraph (j)(2) of this section: weight of the filter. (1) Total extractives. The finished fil- (2) Conditions of use. It is used to fil- ter, when exposed to 5 percent (by ter milk or potable water at operating weight) acetic acid for 2 hours at a temperatures not to exceed 100 °F. temperature equivalent to, or higher (f) Resin-bonded filters conforming than, the filtration temperature of the with the specifications of paragraph (f) aqueous food, yields total extractives (1) of this section are used as provided not to exceed 4 percent, by weight, of in paragraph (e)(2) of this section: the filter. (1) Total extractives. The finished fil- (2) Conditions of use. It is used in com- ter, when exposed to distilled water at mercial filtration of bulk quantities of 145 °F for 2 hours, yields total extrac- nonalcoholic, aqueous foods having a tives not to exceed 4 percent by weight pH of 5.0 or below. of the filter. (k) Resin-bonded filters conforming (2) Conditions of use. It is used to fil- with the specifications of paragraph (k) ter milk or potable water at operating (1) of this section are used as provided temperatures not to exceed 145 °F. in paragraph (k)(2) of this section: (1) Total extractives. The finished fil- (g) Resin-bonded filters conforming ter, when exposed to 8 percent (by vol- with the specifications of paragraph (g) ume) ethyl alcohol in distilled water (1) of this section are used as provided for 2 hours at a temperature equivalent in paragraph (g)(2) of this section: to, or higher than, the filtration tem- (1) Total extractives. The finished fil- perature of the alcoholic beverage, ter, when exposed to n-hexane at reflux yields total extractives not to exceed 4 temperature for 2 hours, yields total percent, by weight, of the filter. extractives not to exceed 0.5 percent by (2) Conditions of use. It is used in com- weight of the filter. mercial filtration of bulk quantities of (2) Conditions of use. It is used to fil- alcoholic beverages containing not ter edible oils. more than 8 percent alcohol. (h) Resin-bonded filters conforming (l) Resin-bonded filters conforming with the specifications of paragraph (h) with the specifications of paragraph (l) (1) of this section are used as provided (1) of this section are used as provided in paragraph (h)(2) of this section: in paragraph (l)(2) of this section: (1) Total extractives. The finished fil- (1) Total extractives. The finished fil- ter, when exposed to distilled water at ter, when exposed to 50 percent (by vol- 212 °F for 2 hours, yields total extrac- ume) ethyl alcohol in distilled water tives not to exceed 4 percent by weight for 2 hours at a temperature equivalent of the filter. to, or higher than, the filtration tem- (2) Conditions of use. It is used to fil- perature of the alcoholic beverage, ter milk, coffee, tea, and potable water yields total extractives not to exceed 4 at temperatures not to exceed 212 °F. percent, by weight, of the filter. (i) Resin-bonded filters conforming (2) Conditions of use. It is used in com- with the specifications of paragraph (i) mercial filtration of bulk quantities of (1) of this section are used as provided alcoholic beverages containing more in paragraph (i)(2) of this section: than 8 percent alcohol. (1) Total extractives. The finished fil- (m) Resin-bonded filters fabricated ter, when exposed to distilled water for from acrylic polymers as provided in 2 hours at a temperature equivalent to, paragraph (d)(3) of this section to- or higher than, the filtration tempera- gether with other substances as pro- ture of the aqueous food, yields total vided in paragraph (d), (1), (2), and (4) extractives not to exceed 4 percent, by of this section may be used as follows: weight, of the filter. (1) The finished filter may be used to (2) Conditions of use. It is used in com- filter milk or potable water at oper- mercial filtration of bulk quantities of ating temperatures not to exceed 100
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°F, provided that the finished filter cleansed prior to their first use in con- when exposed to distilled water at 100 tact with food. °F for 2 hours yields total extractives (d) The provisions of this section are not to exceed 1 percent by weight of not applicable to 4,4′-isopropylidenedi- the filter. phenol-epichlorohydrin resins listed in (2) The finished filter may be used to other sections of parts 174, 175, 176, 177, filter milk or potable water at oper- 178 and 179 of this chapter. ating temperatures not to exceed 145 °F, provided that the finished filter [42 FR 14572, Mar. 15, 1977; 49 FR 5748, Feb. 15, when exposed to distilled water at 145 1984] °F for 2 hours yields total extractives not to exceed 1.2 percent by weight of § 177.2355 Mineral reinforced nylon the filter. resins. (n) Acrylonitrile copolymers identi- Mineral reinforced nylon resins iden- fied in this section shall comply with tified in paragraph (a) of this section the provisions of § 180.22 of this chap- may be safely used as articles or com- ter. ponents of articles intended for re- [42 FR 14572, Mar. 15, 1977, as amended at 56 peated use in contact with nonacidic FR 42933, Aug. 30, 1991] food (pH above 5.0) and at use tempera- tures not exceeding 212 °F. in accord- § 177.2280 4,4′-Isopropylidenediphenol- ance with the following prescribed con- epichlorohydrin thermosetting ditions: epoxy resins. (a) For the purpose of this section 4,4′-Isopropylidenediphenol-epichlo- the mineral reinforced nylon resins rohydrin thermosetting epoxy resins consist of nylon 66, as identified in and may be safely used as articles or com- complying with the specifications of ponents of articles intended for re- § 177.1500, reinforced with up to 40 peated use in producing, manufac- weight percent of calcium silicate and turing, packing, processing, preparing, up to 0.5 weight percent 3- treating, packaging, transporting, or (triethoxysilyl) propylamine (Chemical holding food, in accordance with the Abstracts Service Registry No. following prescribed conditions: 000919302) based on the weight of the (a) The basic thermosetting epoxy calcium silicate. resin is made by reacting 4,4′- (b) The mineral reinforced nylon res- isopropylidenediphenol with epichloro- ins may contain up to 0.2 percent by hydrin. (b) The resin may contain one or weight of titanium dioxide as an op- more of the following optional sub- tional adjuvant substance. stances provided the quantity used (c) The mineral reinforced nylon res- does not exceed that reasonably re- ins with or without the optional sub- quired to accomplish the intended ef- stance described in paragraph (b) of fect: this section, and in the form of 1⁄8-inch molded test bars, when extracted with Allyl glycidyl ether ...... As curing system additive. the solvents, i.e., distilled water and 50 Di- and tri-glycidyl ester mix- As modifier at levels not to percent (by volume) ethyl alcohol in ture resulting from the re- exceed equal parts by action of epichlorohydrin weight of the 4,4′- distilled water, at reflux temperature with mixed dimers and isopropylidenediphenol- for 24 hours using a volume-to-surface trimers of unsaturated C18 epichlorohydrin basic resin ratio of 2 milliliters of solvent per monobasic fatty acids de- and limited to use in con- rived from animal and veg- tact with alcoholic bev- square inch of surface tested, shall etable fats and oils. erages containing not more meet the following extractives limita- than 8 percent of alcohol. tions: 1,2-Epoxy-3-phenoxypropane As curing system additive. Glyoxal ...... Do. (1) Total extractives not to exceed 5.0 4,4′-Isopropylidenediphenol ... Do. milligrams per square inch of food-con- 4,4′-Methylenedianiline ...... Do. tact surface tested for each solvent. m-Phenylenediamine ...... Do. Tetrahydrophthalic anhydride Do. (2) The ash after ignition of the ex- tractives described in paragraph (c)(1) (c) In accordance with good manufac- of this section, not to exceed 0.5 milli- turing practice, finished articles con- gram per square inch of food-contact taining the resins shall be thoroughly surface tested.
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(d) In accordance with good manufac- (1) Substances generally recognized turing practice, finished articles con- as safe (GRAS) in food or food pack- taining the mineral reinforced nylon aging. resins shall be thoroughly cleansed (2) Substances used in accordance prior to their first use in contact with with a prior sanction. food. (3) Substances authorized under ap- plicable regulations in this part and in [42 FR 54533, Oct. 7, 1977, as amended at 42 FR parts 175 and 178 of this chapter and 61594, Dec. 6, 1977] subject to any limitations prescribed § 177.2400 Perfluorocarbon cured therein. elastomers. (4) Substances identified in this para- graph (b)(4) subject to such limitations Perfluorocarbon cured elastomers as are provided: identified in paragraph (a) of this sec- tion may be safely used as articles or Substances Limitations components of articles intended for re- Carbon black (channel proc- Not to exceed 15 parts per peated use in contact with nonacid ess of furnace combustion 100 parts of the food (pH above 5.0), subject to the pro- process) (CAS Reg. No. terpolymer. visions of this section. 1333Ð86Ð4). Magnesium oxide (CAS Reg. Not to exceed 5 parts per (a) Identity. (1) For the purpose of No. 1309Ð48Ð4). 100 parts of the this section, perfluorocarbon cured terpolymer. elastomers are produced by terpolymerizing tetrafluorethylene (c) Specifications—(1) Infrared identi- (CAS Reg. No. 116–14–3), fication. Perfluorocarbon cured perfluoromethyl vinyl ether (CAS Reg. elastomers may be identified by the No. 1187–93–5), and perfluoro-2- characteristic infrared spectra of the phenoxypropyl vinyl ether (CAS Reg. pyrolysate breakdown product that is No. 24520–19–2) and subsequent curing of obtained by heating and decomposing the terpolymer (CAS Reg. No. 26658–70– the elastomer using the method enti- 8) using the crosslinking agent, phenol, tled ‘‘Qualitative Identification of 4,4′-[2,2,2-trifluoro-1-(trifluoromethyl) Kalrez by Infrared Examination of ethylidene] bis-,dipotassium salt (CAS Pyrolysate.’’ This method is incor- Reg. No. 25088–69–1) and accelerator, porated by reference. Copies of the 1,4,7,10,13,16-hexaoxacyclooctadecane method are available from the Center (CAS Reg. No. 17455–13–9). for Food Safety and Applied Nutrition (2) The perfluorocarbon base polymer (HFS–200), Food and Drug Administra- shall contain no less than 40 weight- tion, 200 C St. SW., Washington, DC percent of polymer units derived from 20204, or available for inspection at the tetrafluoroethylene, no less than 40 Office of the Federal Register, 800 weight-percent of polymer units de- North Capitol Street, NW., suite 700, rived from perfluoromethyl vinyl ether Washington, DC 20408. and no more than 5 weight-percent (2) Thermogravimetry. Perfluorocarbon polymer units derived from perfluoro-2- cured elastomers have a major decom- ° ± ° phenoxy-propyl vinyl ether. position peak occurring at 490 15 C ° (3) The composition limitations of (914 F). Less than 1.5 percent of the ° the cured elastomer, calculated as elastomers will volatilize below 400 C ° parts per 100 parts of terpolymer, are (752 F) when run under nitrogen at a 10 ° ° as follows: C or 18 F per minute heating rate using a Du Pont Thermal Analyzer Phenol, 4,4′-[2,2,2-trifluoro-1- Model 1099 with Model 951 TGA unit or (trifluoromethyl)-ethylidene] bis- the equivalent. ,dipotassium salt—not to exceed 5 parts. (d) Extractive limitations. Articles fab- 1,4,7,10,13,16-Hexaoxacyclo-octadecane—not ricated from perfluorocarbon cured to exceed 5 parts. elastomers having a thickness of at (b) Optional adjuvant substances. The least 1.0 millimeter (0.039 inch) when perfluorocarbon cured elastomer iden- extracted at reflux temperatures for 2 tified in paragraph (a) of this section hours separately with distilled water, may contain the following optional ad- 50 percent ethanol, and n-heptane, juvant substances, subject to any limi- shall meet the following extractability tations cited on their use: limits:
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(1) Total extractives not to exceed 3.1 Glass fiber. milligrams per square decimeter (0.2 Hexamethylenetetramine ...... For use as curing agent. milligrams per square inch). Mica. Oxalic acid ...... For use as catalyst. (2) Fluoride extractives calculated as Zinc stearate ...... For use as lubricant. fluorine not to exceed 0.47 milligram per square decimeter (0.03 milligram (c) The finished food-contact article, per square inch). when extracted with distilled water at (e) Conditions of use. In accordance reflux temperature for 2 hours, using a with current good manufacturing prac- volume-to-surface ratio of 2 milliliters tice, finished food contact articles con- of distilled water per square inch of taining the perfluorocarbon cured surface tested, shall meet the following elastomers shall be thoroughly cleaned extractives limitations: prior to their first use in contact with (1) Total extractives not to exceed food. 0.15 milligram per square inch of food- [49 FR 43050, Oct. 26, 1984] contact surface. (2) Extracted phenol not to exceed § 177.2410 Phenolic resins in molded 0.005 milligram per square inch of food- articles. contact surface. Phenolic resins identified in this sec- (3) No extracted aniline when tested tion may be safely used as the food- by a spectrophotometric method sen- contact surface of molded articles in- sitive to 0.006 milligram of aniline per- tended for repeated use in contact with square inch of food-contact surface. nonacid food (pH above 5.0), in accord- (d) In accordance with good manufac- ance with the following prescribed con- turing practice, finished molded arti- ditions: cles containing the phenolic resins (a) For the purpose of this section, shall be thoroughly cleansed prior to the phenolic resins are those produced their first use in contact with food. when one or more of the phenols listed in paragraph (a)(1) of this section are § 177.2415 Poly(aryletherketone) res- made to react with one or more of the ins. aldehydes listed in paragraph (a)(2) of this section, with or without aniline Poly(aryletherketone) resins identi- and/or anhydro-formaldehyde aniline fied in paragraph (a) of this section (hexahydro-1, 3,5-triphenyl-s-triazine): may be safely used as articles or com- (1) Phenols: ponents of articles intended for re- peated use in contact with food subject p-tert-Amylphenol. to the provisions of this section. p-tert-Butylphenol. o-, m-, and p-Cresol. (a) Identity. For the purposes of this p-Octylphenol. section, poly(aryletherketone) resins Phenol. are poly(p-oxyphenylene p- o- and p-Phenylethylphenol mixture pro- oxyphenylene p-carboxyphenylene) res- duced when phenol is made to react with ins (CAS Reg. No. 29658–26–2) produced styrene in the presence of sulfuric acid cat- by the polymerization of hydroquinone alyst. and 4,4′-difluorobenzophenone, and (2) Aldehydes: have a minimum weight-average mo- lecular weight of 12,000, as determined Acetaldehyde. Formaldehyde. by gel permeation chromatography in Paraldehyde. comparison with polystyrene stand- ards, and a minimum mid-point glass (b) Optional adjuvant substances em- transition temperature of 142 °C, as de- ployed in the production of the phe- termined by differential scanning nolic resins or added thereto to impart calorimetry. desired technical or physical properties (b) Optional adjuvant substances. The include the following: basic resins identified in paragraph (a) Asbestos fiber. may contain optional adjuvant sub- Barium hydroxide ...... For use as catalyst. stances used in their production. These Calcium stearate ...... For use as lubricant. adjuvants may include substances de- Carbon black (channel proc- ess). scribed in § 174.5(d) of this chapter and Diatomaceous earth. the following:
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Methacrylic. Orthophthalic. Substance Limitations Sebacic. Terephthalic. Diphenyl sulfone ...... Not to exceed 0.2 percent by weight as a residual Trimellitic. solvent in the finished (2) Polyols and polyepoxides: basic resin. Butylene glycol. (c) Extractive limitations. The finished Diethylene glycol. food contact article, when extracted at 2,2-Dimethyl-1,3-propanediol. reflux temperatures for 2 hours with Dipropylene glycol. the following four solvents, yields in Ethylene glycol. each extracting solvent net chloroform Glycerol. 4,4′-Isopropylidenediphenol-epichlorohydrin. soluble extractives not to exceed 0.05 Mannitol. milligrams per square inch of food con- a-Methyl glucoside. tact surface: Distilled water, 50 percent Pentaerythritol. (by volume) ethanol in distilled water, Polyoxypropylene ethers of 4,4′-isopropylide- 3 percent acetic acid in distilled water, nediphenol (containing an average of 2–7.5 and n-heptane. In testing the final food moles of propylene oxide). contact article, a separate test sample Propylene glycol. shall be used for each extracting sol- Sorbitol. Trimethylol ethane. vent. Trimethylol propane. [63 FR 20315, Apr. 24, 1998] 2,2,4-Trimethyl-1,3-pentanediol. (3) Cross-linking agents: § 177.2420 Polyester resins, cross- linked. Butyl acrylate. Cross-linked polyester resins may be Butyl methacrylate. safely used as articles or components Ethyl acrylate. Ethylhexyl acrylate. of articles intended for repeated use in Methyl acrylate. contact with food, in accordance with Methyl methacrylate. the following prescribed conditions: Styrene. (a) The cross-linked polyester resins Triglycidyl isocyanurate (CAS Reg. No. 2451– are produced by the condensation of 62–9), for use only in coatings contacting one or more of the acids listed in para- bulk quantities of dry food of the type graph (a)(1) of this section with one or identified in § 176.170(c) of this chapter, more of the alcohols or epoxides listed table 1, under type VIII. Vinyl toluene. in paragraph (a)(2) of this section, fol- lowed by copolymerization with one or (b) Optional adjuvant substances em- more of the cross-linking agents listed ployed to facilitate the production of in paragraph (a)(3) of this section: the resins or added thereto to impart (1) Acids: desired technical or physical properties include the following, provided that Adipic. the quantity used does not exceed that Fatty acids, and dimers thereof, from nat- ural sources. reasonably required to accomplish the Fumaric. intended physical or technical effect Isophthalic. and does not exceed any limitations Maleic. prescribed in this section:
Limitations (limits of addition expressed as percent by weight List of substances of finished resin)
1. Inhibitors: Total not to exceed 0.08 percent. Benzoquinone ...... 0.01 percent. tert-Butyl catechol. TBHQ. Di-tert-butyl hydroquinone. Hydroquinone. 2. Accelerators: Total not to exceed 1.5 percent. Benzyl trimethyl ammonium chloride ...... 0.05 percent. Calcium naphthenate. Cobalt naphthenate. Copper naphthenate. N, N-Diethylaniline ...... 0.4 percent.
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Limitations (limits of addition expressed as percent by weight List of substances of finished resin)
N, N-Dimethylaniline ...... Do. Ethylene guanidine hydrochloride ...... 0.05 percent. 3. Catalysts: Total not to exceed 1.5 percent, except that methyl ethyl ke- tone peroxide may be used as the sole catalyst at levels not to exceed 2 percent. Azo-bis-isobutyronitrile. Benzoyl peroxide. tert-Butyl perbenzoate. Chlorbenzoyl peroxide. Cumene hydroperoxide. Dibutyltin oxide (CAS Reg. No. 818Ð08Ð6) ...... For use in the polycondensation reaction at levels not to ex- ceed 0.2 percent of the polyester resin. Dicumyl peroxide. Hydroxybutyltin oxide (CAS Reg. No. 2273Ð43Ð0) ...... For use in the polycondensation reaction at levels not to ex- ceed 0.2 percent of the polyester resin. Lauroyl peroxide. p-Menthane hydroperoxide. Methyl ethyl ketone peroxide. Monobutyltin tris(2-ethylhexoate) (CAS Reg. No. 23850Ð For use in the polycondensation reaction at levels not to ex- 94Ð4). ceed 0.2 percent of the polyester resin. 4. Solvents for inhibitors, accelerators, and catalysts: Butyl benzyl phthalate (containing not more than 1.0 per- cent by weight of dibenzyl phthalate). Dibutyl phthalate. Diethylene glycol ...... As a solvent for benzyl trimethyl ammonium chloride or ethyl- ene guanidine hydrochloride only. Dimethyl phthalate. Methyl alcohol. Styrene. Triphenyl phosphate. 5. Reinforcements: Asbestos. Glass fiber. Polyester fiber produced by the condensation of one or more of the acids listed in paragraph (a)(1) of this sec- tion with one or more of the alcohols listed in paragraph (a)(2) of this section. 6. Miscellaneous materials: Castor oil, hydrogenated. α-Methylstyrene. Polyethylene glycol 6000. Silicon dioxide. Wax, petroleum ...... Complying with ¤ 178.3710 of this chapter.
(c) The cross-linked polyester resins, of food-contact surface tested when the with or without the optional sub- prescribed food-simulating solvent is stances described in paragraph (b) of heptane. this section, and in the finished form in (d) In accordance with good manufac- which they are to contact food, when turing practice, finished articles con- extracted with the solvent or solvents taining the cross-linked polyester res- characterizing the type of food and ins shall be thoroughly cleansed prior under the conditions of time and tem- to their first use in contact with food. perature characterizing the conditions of their intended use, as determined [42 FR 14572, Mar. 15, 1977, as amended at 48 from tables 1 and 2 of § 176.170(c) of this FR 37618, Aug. 19, 1983; 54 FR 48858, Nov. 28, chapter, shall meet the following ex- 1989] tractives limitations: (1) Net chloroform-soluble extrac- § 177.2430 Polyether resins, chlorinated. tives not to exceed 0.1 milligram per square inch of food-contact surface Chlorinated polyether resins may be tested when the prescribed food-simu- safely used as articles or components lating solvent is water or 8 or 50 per- of articles intended for repeated use in cent alcohol. producing, manufacturing, packing, (2) Total nonvolatile extractives not processing, preparing, treating, pack- to exceed 0.1 milligram per square inch aging, transporting, or holding food, in
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accordance with the following pre- List of substances Limitations scribed conditions: Diphenylsulfone ...... Not to exceed 0.2 percent as re- (a) The chlorinated polyether resins sidual solvent in the finished are produced by the catalytic polym- basic resin described in para- erization of 3,3-bis(chloromethyl)- graph (a)(1) of this section. Dimethyl sulfoxide ...... Not to exceed 0.01 percent as oxetane, and shall contain not more residual solvent in the finished than 2 percent residual monomer. basic resin described in para- (b) In accordance with good manufac- graph (a)(1) of this section. turing practice, finished articles con- N-methyl-2-pyrrolidone ..... Not to exceed 0.01 percent as residual solvent in the finished taining the chlorinated polyether res- basic resin described in para- ins shall be thoroughly cleansed prior graph (a)(2) of this section. to their first use in contact with food. (c) The finished food-contact article, § 177.2440 Polyethersulfone resins. when extracted at reflux temperatures for 2 hours with the following four sol- Polyethersulfone resins identified in vents, yields net chloroform-soluble ex- paragraph (a) of this section may be tractives in each extracting solvent safely used as articles or components not to exceed 0.02 milligram per square of articles intended for repeated use in inch of food-contact surface: distilled contact with food in accordance with water, 50 percent (by volume) ethyl al- the following prescribed conditions: cohol in distilled water, 3 percent ace- (a) For the purpose of this section, tic acid in distilled water, and n- polyethersulfone resins are: heptane. (Note: In testing the finished (1) Poly(oxy-p-phenylenesulfonyl-p- food-contact article, use a separate phenylene) resins (CAS Reg. No. 25667– test sample for each required extract- 42–9), which have a minimum number ing solvent.) average molecular weight of 16,000. (d) In accordance with good manufac- (2) 1,1′-sulfonylbis[4-chlorobenzene] turing practice, finished food-contact polymer with 4,4′-(1-methylethyl- articles containing the idene)bis[phenol] (maximum 8 percent) polyethersulfone resins shall be thor- and 4,4′-sulfonylbis[phenol] (minimum oughly cleansed before their first use 92 percent) (CAS Reg. No. 88285–91–0), in contact with food. which have a minimum number aver- age molecular weight of 26,000. [44 FR 34493, June 15, 1979, as amended at 47 FR 38885, Sept. 3, 1982; 49 FR 10111, Mar. 19, (3) In paragraphs (a)(1) and (a)(2) of 1984; 50 FR 47211, Nov. 15, 1985; 60 FR 48648, this section, the minimum number av- Sept. 20, 1995] erage molecular weight is determined by reduced viscosity in dimethyl form- § 177.2450 Polyamide-imide resins. amide in accordance with ASTM meth- Polyamide-imide resins identified in od D2857–70 (Reapproved 1977), ‘‘Stand- paragraph (a) of this section may be ard Test Method for Dilute Solution safely used as components of articles Viscosity of Polymers,’’ which is incor- intended for repeated use in contact porated by reference. Copies may be with food, in accordance with the fol- obtained from the American Society lowing prescribed conditions: for Testing Materials, 1916 Race St., (a) Identity. (1) For the purpose of Philadelphia, PA 19103, or may be ex- this section the polyamide-imide resins amined at the Division of Petition Con- are derived from the condensation re- trol (HFS–215), Center for Food Safety action of substantially equimolar parts and Applied Nutrition, 1110 Vermont of trimellitic anhydride and p,p′- Ave. NW., suite 1200, Washington, DC, diphenylmethane diisocyanate. or at the Office of the Federal Register, (2) The polyamide-imide resins (CAS 800 North Capitol St. NW., suite 700, Reg. No. 31957–38–7) derived from the Washington, DC. condensation reaction of equimolar (b) The basic resins identified in parts of benzoyl chloride-3,4- paragraphs (a)(1) and (a)(2) of this sec- dicarboxylic anhydride and 4,4′- tion may contain optional adjuvant diphenylmethanediamine. substances described in § 174.5(d) of this (b) Specifications. (1) Polyamide-imide chapter and the following: resins identified in paragraph (a)(1) of
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this section shall have a nitrogen con- 200), Food and Drug Administration, tent of not less than 7.8 weight percent 200 C St. SW., Washington, DC 20204, or and not more than 8.2 weight percent. available for inspection at the Office of Polyamide-imide resins identified in the Federal Register, 800 North Capitol paragraph (a)(2) of this section shall Street, NW., suite 700, Washington, have a nitrogen content of not less DC). than 7.5 weight percent and not more (c) Extractive limitations are appli- than 7.8 weight percent. Nitrogen con- cable to the polyamide-imide resins tent is determined by the Dumas Nitro- identified in paragraphs (a) (1) and (2) gen Determination as set forth in the of this section in the form of films of 1 ‘‘Official Methods of Analysis of the mil uniform thickness after coating Association of Official Analytical and heat curing at 600 °F for 15 minutes Chemists,’’ 13th Ed. (1980), sections on stainless steel plates, each having 7.016–7.020, which is incorporated by such resin-coated surface area of 100 reference in accordance with 5 U.S.C. square inches. The cured-resin film 552(a). Copies may be obtained from the coatings shall be extracted in accord- Association of Official Analytical ance with the method described in Chemists International, 481 North § 176.170(d)(3) of this chapter, using a Frederick Ave., suite 500, Gaithersburg, plurality of spaced, coated stainless MD 20877–2504, or may be examined at steel plates, exposed to the respective the Office of the FEDERAL REGISTER, 800 North Capitol Street, NW., suite food simulating solvents. The resin 700, Washington, DC. shall meet the following extractive (2) Polyamide-imide resins identified limitations under the corresponding in paragraph (a)(1) of this section shall extraction conditions: have a solution viscosity of not less (1) Distilled water at 250 °F for 2 than 1.200. Polyamide-imide resins hours: Not to exceed 0.01 milligram per identified in paragraph (a)(2) of this square inch. section shall have a solution viscosity (2) Three percent acetic acid at 212 °F of not less than 1.190. Solution vis- for 2 hours: Not to exceed 0.05 milli- cosity shall be determined by a method gram per square inch. titled ‘‘Solution Viscosity’’ which is in- (3) Fifty percent ethyl alcohol at 160 corporated by reference in accordance °F for 2 hours: Not to exceed 0.03 milli- with 5 U.S.C. 552(a). Copies are avail- gram per square inch. able from the Center for Food Safety (4) n-Heptane at 150 °F for 2 hours: and Applied Nutrition (HFS–200), Food Not to exceed 0.05 milligram per square and Drug Administration, 200 C St. inch. SW., Washington, DC 20204, or available (d) In accordance with good manufac- for inspection at the Office of the FED- turing practice, those food contact ar- ERAL REGISTER, 800 North Capitol ticles, having as components the poly- Street, NW., suite 700, Washington, DC. amide-imide resins identified in para- (3) The polyamide-imide resins iden- graph (a) of this section and intended tified in paragraph (a)(1) of this section for repeated use shall be thoroughly ° are heat cured at 600 F for 15 minutes cleansed prior to their first use in con- when prepared for extraction tests and tact with food. the residual monomers: p,p- diphenylmethane diisocyanate should [42 FR 14572, Mar. 15, 1977, as amended at 47 not be present at greater than 100 parts FR 11845, Mar. 19, 1982; 49 FR 10111, Mar. 19, per million and trimellitic anhydride 1984; 54 FR 24898, June 12, 1989; 54 FR 43170, should not be present at greater than Oct. 23, 1989; 61 FR 14481, Apr. 2, 1996] 500 parts per million. Residual mono- mers are determined by gas chroma- § 177.2460 Poly(2,6-dimethyl-1,4-phen- ylene) oxide resins. tography (the gas chromatography method titled ‘‘Amide-Imide Polymer The poly(2,6-dimethyl-1,4-phenylene) Analysis—Analysis of Monomer Con- oxide resins identified in paragraph (a) tent,’’ is incorporated by reference in of this section may be used as an arti- accordance with 5 U.S.C. 552(a). Copies cle or as a component of an article in- are available from the Center for Food tended for use in contact with food sub- Safety and Applied Nutrition (HFS– ject to the provisions of this section.
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(a) Identity. For the purposes of this (iii) Viscometer: Cannno-Ubbelohde se- section, poly(2,6-dimethyl-1,4-phen- ries 25 dilution viscometer (or equiva- ylene) oxide resins consist of basic res- lent). ins produced by the oxidative coupling (iv) Calculation: The calculation of 2,6-xylenol such that the finished method used is that described in appen- basic resins meet the specifications dix X.1.3 (ASTM method D1243–79, cited and extractives limitations prescribed and incorporated by reference in para- in paragraph (c) of this section. graph (c)(1) of this section) with the re- (b) Optional adjuvant substances. The duced viscosity determined for three basic poly(2,6-dimethyl-1,4-phenylene) concentration levels (0.4, 0.2, and 0.1 oxide resins identified in paragraph (a) gram per deciliter) and extrapolated to of this section may contain optional zero concentration for intrinisic vis- adjuvant substances required in the cosity. The following formula is used production of such basic resins. The op- for determining reduced viscosity: tional adjuvant substances required in − the production of the basic poly(2,6-di- Reduced viscosity in terms = tto methyl-1,4-phenylene) oxide resins may of deciliters per gram tc× include substances permitted for such o use by regulations in parts 170 through where: 189 of this chapter, substances gen- t=Solution efflux time. erally recognized as safe in food, sub- to=Solvent efflux time. stances used in accordance with a prior c=Concentration of solution in terms of sanction or approval, and the fol- grams per deciliter. lowing: (2) Extractives limitations. Total resin extracted not to exceed 0.02 weight-per- Limitations (expressed as List of substances percent by weight of finished cent when extracted with n-heptane at basic resin) 160 °F for 2 hours as determined using 200 milliliters of reagent grade n- Diethylamine ...... Not to exceed 0.16 percent as residual catalyst. heptane which has been freshly dis- Methyl alcohol ...... Not to exceed 0.02 percent tilled before use and 25 grams of poly as residual solvent. (2,-6-dimethyl-1,4-phenylene) oxide Toluene ...... Not to exceed 0.2 percent as resin. The resin as tested is in pellet residual solvent. form having a particle size such that (c) Specifications and extractives limita- 100 percent of the pellets will pass tions. The poly(2,6-dimethyl-1,4-phen- through a U.S. Standard Sieve No. 6 and 100 percent of the pellets will be ylene) oxide basic resins meet the fol- held on a U.S. Standard Sieve No. 10. lowing: (d) Other limitations. The poly(2,6-di- (1) Specifications. Intrinsic viscosity methyl-1,4-phenylene) oxide resins is not less than 0.30 deciliter per gram identified in and complying with this as determined by ASTM method D1243– section, when used as components of 79, ‘‘Standard Test Method for Dilute the food-contact surface of any article Solution Viscosity of Vinyl Chloride that is the subject of a regulation in Polymers,’’ which is incorporated by parts 174, 175, 176, 177, 178 and § 179.45 of reference, modified as follows. Copies this chapter, shall comply with any of the incorporation by reference may specifications and limitations pre- be obtained from the American Society scribed by such regulation for the arti- for Testing Materials, 1916 Race St., cle in the finished form in which it is Philadelphia, PA 19103, or may be ex- to contact food. amined at the Office of the Federal (e) Uses. The poly(2,6-dimethyl-1,4- Register, 800 North Capitol Street, phenylene) oxide resins identified in NW., suite 700, Washington, DC 20408. and complying with the limitations in (i) Solvent: Chloroform, reagent grade this section may be used as articles or containing 0.01 percent tert- components of articles intended for re- butylcatechol. peated food-contact use or as articles (ii) Resin sample: Powdered resin ob- or components of articles intended for tained from production prior to mold- single-service food-contact use only ing or extrusion. under the conditions described in
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§ 176.170(c) of this chapter, table 2, con- part desired technological properties to ditions of use H. the copolymer. (b) Optional adjuvant substances. The [42 FR 14572, Mar. 15, 1977, as amended at 49 FR 10111, Mar. 19, 1984; 63 FR 8852, Feb. 23, polyoxymethylene copolymer identi- 1998] fied in paragraph (a) of this section may contain optional adjuvant sub- § 177.2465 Polymethylmethacrylate/ stances required in its production. The poly(trimethoxysilylpropyl)meth- quantity of any optional adjuvant sub- acrylate copolymers. stance employed in the production of Polymethylmethacrylate/ the copolymer does not exceed the poly(trimethoxysilylpropyl) methacry- amount reasonably required to accom- late copolymers (CAS Reg. No. 26936– plish the intended technical or physical 30–1) may be safely used as components effect. Such adjuvants may include of surface primers used in conjunction substances generally recognized as safe with silicone polymers intended for re- in food, substances used in accordance peated use and complying with § 175.300 with prior sanction, substances per- of this chapter and § 177.2600, in accord- mitted under applicable regulations in ance with the following prescribed con- parts 170 through 189 of this chapter, ditions. and the following: (a) Identity. For the purpose of this (1) Stabilizers (total amount of stabi- section, polymethylmethacrylate/ lizers not to exceed 2.0 percent and poly(trimethoxysilylpropyl)methacry- amount of any one stabilizer not to ex- late copolymers are produced by the ceed 1.0 percent of polymer by weight) polymerization of methylmethacrylate Calcium ricinoleate. and Cyanoguanidine. trimethoxysilylpropylmethacrylate. Hexamethylene bis(3,5-di-tert-butyl-4- (b) Conditions of use. (1) The hydroxyhydrocinnamate) (CAS Reg. No. polymethylmethacrylate/ 35074–77–2). poly(trimethoxysilylpropyl)meth- Melamine-formaldehyde resin. ′ acrylate copolymers are used at levels 2,2 -Methylenebis(4-methyl-6-tert-butyl- phenol). not to exceed 6.0 percent by weight of Nylon 6/66, weight ratio 2/3. the primer formulation. Tetrakis [methylene (3,5-di-tert-butyl-4- (2) The copolymers may be used in hydroxyhydrocinnamate)] methane. food contact applications with all food ′ types under conditions of use B (2) Lubricant: N,N Distearoylethyl- through H as described in table 2 of enediamine. § 176.170(c) of this chapter. (c) Specifications. (1) Polyoxymeth- ylene copolymer can be identified by [59 FR 5948, Feb. 9, 1994] its characteristic infrared spectrum. (2) Minimum number average molec- § 177.2470 Polyoxymethylene copoly- ular weight of the copolymer is 15,000 mer. as determined by a method titled Polyoxymethylene copolymer identi- ‘‘Number Average Molecular Weight,’’ fied in this section may be safely used which is incorporated by reference. as an article or component of articles Copies are available from the Center intended for food-contact use in ac- for Food Safety and Applied Nutrition cordance with the following prescribed (HFS–200), Food and Drug Administra- conditions: tion, 200 C St. SW., Washington, DC (a) Identity. For the purpose of this 20204, or available for inspection at the section, polyoxymethylene copolymers Office of the Federal Register, 800 are identified as the following: The re- North Capitol Street, NW., suite 700, action product of trioxane (cyclic Washington, DC 20408. trimer of formaldehyde) and ethylene (d) Extractive limitations. (1) Polyoxy- oxide (CAS Reg. No. 24969–25–3) or the methylene copolymer in the finished reaction product of trioxane (cyclic form in which it is to contact food, trimer of formaldehyde) and a max- when extracted with the solvent or sol- imum of 5 percent by weight of vents characterizing the type of food butanediol formal (CAS Reg. No. 25214 and under conditions of time and tem- 85–1). Both copolymers may have cer- perature as determined from tables 1 tain optional substances added to im- and 2 of § 175.300(d) of this chapter,
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shall yield net chloroform-soluble ex- of any optional adjuvant substance em- tractives not to exceed 0.5 milligram ployed in the production of the per square inch of food-contact surface. homopolymer does not exceed the (2) Polyoxymethylene copolymer amount reasonably required to accom- with or without the optional sub- plish the intended effect. Such adju- stances described in paragraph (b) of vants may include substances gen- this section, when ground or cut into erally recognized as safe in food, sub- particles that pass through a U.S.A. stances used in accordance with prior Standard Sieve No. 6 and that are re- sanction, substances permitted under tained on a U.S.A. Standard Sieve No. applicable regulations in this part, and 10, shall yield total extractives as fol- the following: lows: (1) Stabilizers. The homopolymer may (i) Not to exceed 0.20 percent by contain one or more of the following weight of the copolymer when ex- stabilizers. The total amount of stabi- tracted for 6 hours with distilled water lizers shall not exceed 1.9 percent of at reflux temperature. homopolymer by weight, and the quan- (ii) Not to exceed 0.15 percent by tity of individual stabilizer used shall weight of the copolymer when ex- not exceed the limitations set forth tracted for 6 hours with n-heptane at below: reflux temperature. (e) Conditions of use. (1) The Substances Limitations polyoxymethylene copolymer is for use Hexamethylenebis(3,5-di-tert- At a maximum level of 1 per- as articles or components of articles butyl-4-hydroxy-hydro- cent by weight of homo- intended for repeated use. cinnamate) (CAS Reg. No. polymer. The finished arti- 35074Ð77Ð2). cles shall not be used for (2) Use temperature shall not exceed foods containing more than 250 °F. 8 percent alcohol. (3) In accordance with good manufac- 2,2′-Methylenebis(4-methyl-6- At a maximum level of 0.5 tert-butylphenol). percent by weight of turing practice, finished articles con- homopolymer. taining polyoxymethylene copolymer Nylon 66/610/6 terpolymer, At a maximum level of 1.5 shall be thoroughly cleansed before respective proportions of percent by weight of their first use in contact with food. nylon polymers by weight homopolymer. are: 3/2/4. [42 FR 14572, Mar. 15, 1977, as amended at 48 Nylon 612/6 copolymer (CAS Do. FR 56204, Dec. 20, 1983; 49 FR 5748, Feb. 15, Reg. No. 51733-10-9), weight ratio 6/1. 1984; 50 FR 1842, Jan. 14, 1985; 50 FR 20560, Tetrakis[methylene(3,5-di-tert- At a maximum level of 0.5 May 17, 1985; 52 FR 4493, Feb. 12, 1987, 54 FR butyl-4-hydroxy-hydro- percent by weight of 24898, June 12, 1989] cinnamate)] methane. homopolymer.
§ 177.2480 Polyoxymethylene (2) Lubricant. N,N′-Distearoylethyl- homopolymer. enediamine. Polyoxymethylene homopolymer (3) Molding assistant. Polyethylene identified in this section may be safely glycol 6,000. used as articles or components of arti- (c) Specifications. (1) cles intended for food-contact use in Polyoxymethylene homopolymer can accordance with the following pre- be identified by its characteristic in- scribed conditions: frared spectrum. (a) Identity. For the purpose of this (2) Minimum number average molec- section, polyoxymethylene homopoly- ular weight of the homopolymer is mer is polymerized formaldehyde 25,000. [Chemical Abstracts Service Registry (3) Density of the homopolymer is be- No. 9002–81–7]. Certain optional adju- tween 1.39 and 1.44 as determined by vant substances, described in para- ASTM method D1505–68 (Reapproved graph (b) of this section, may be added 1979), ‘‘Standard Test Method for Den- to impart desired technological prop- sity of Plastics by the Density-Gra- erties to the homopolymer. dient Technique,’’ which is incor- (b) Optional adjuvant substances. The porated by reference. Copies may be polyoxymethylene homopolymer iden- obtained from the American Society tified in paragraph (a) of this section for Testing Materials, 1916 Race St., may contain optional adjuvant sub- Philadelphia, PA 19103, or may be ex- stances in its production. The quantity amined at the Office of the Federal
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Register, 800 North Capitol Street, articles or components of articles in- NW., suite 700, Washington, DC 20408. tended for repeated use. (4) Melting point is between 172 °C (2) Use temperature shall not exceed and 184 °C as determined by ASTM 250 °F. method D2133–66, ‘‘Specifications for (3) In accordance with good manufac- Acetal Resin Injection Molding and Ex- turing practice, finished articles con- trusion Materials’’ (Revised 1966), taining polyoxymethylene which is incorporated by reference. homopolymer shall be thoroughly Copies are available from American So- cleansed prior to first use in contact ciety for Testing and Materials with food. (ASTM), 1916 Race Street, Philadel- [42 FR 14572, Mar. 15, 1977, as amended at 43 phia, PA 19103, or available for inspec- FR 44835, Sept. 29, 1978; 47 FR 11846, Mar. 19, tion at the Office of the Federal Reg- 1982; 47 FR 51562, Nov. 16, 1982; 49 FR 10111, ister, 800 North Capitol Street, NW., Mar. 19, 1984; 54 FR 24898, June 12, 1989] suite 700, Washington, DC 20408. (d) Extractive limitations. (1) § 177.2490 Polyphenylene sulfide res- Polyoxymethylene homopolymer, in ins. the finished form which is to contact Polyphenylene sulfide resins food, when extracted with the solvent (poly(1,4-phenylene sulfide) resins) may or solvents characterizing the type of be safely used as coatings or compo- food and under conditions of time and nents of coatings of articles intended temperature characterizing the condi- for repeated use in contact with food, tions of intended use under paragraphs in accordance with the following pre- (c)(3) and (d) of § 175.300 of this chapter scribed conditions. and as limited by paragraph (e) of this (a) Polyphenylene sulfide resins con- section, shall yield net chloroform- sist of basic resins produced by the re- soluble extractives not to exceed 0.5 action of equimolar parts of p- milligram per square inch of food-con- dichlorobenzene and sodium sulfide, tact surface. such that the finished resins meet the (2) Polyoxymethylene homopolymer, following specifications as determined with or without the optional adjuvant by methods titled ‘‘Oxygen Flask Com- substances described in paragraph (b) bustion-Gravimetric Method for Deter- of this section, when ground or cut into mination of Sulfur in Organic Com- particles that pass through a U.S.A. pounds,’’ ‘‘Determination of the Inher- Standard Sieve No. 6 and that are re- ent Viscosity of Polyphenylene Sul- tained on a U.S.A. Standard Sieve No. fide,’’ and ‘‘Analysis for 10, shall yield extractives as follows: Dichlorobenzene in Ryton (i) Formaldehyde not to exceed 0.0050 Polyphenylene Sulfide,’’ which are in- percent by weight of homopolymer as corporated by reference. Copies are determined by a method titled ‘‘Form- available from the Center for Food aldehyde Release and Formaldehyde Safety and Applied Nutrition (HFS– Analysis,’’ which is incorporated by 200), Food and Drug Administration, reference. Copies are available from 200 C St. SW., Washington, DC 20204, or Center for Food Safety and Applied Nu- available for inspection at the Office of trition (HFS–200) Food and Drug Ad- the Federal Register, 800 North Capitol ministration, 200 C St. SW., Wash- Street, NW., suite 700, Washington, DC ington, DC 20204, or available for in- 20408. spection at the Office of the Federal (1) Sulfur content: 28.2–29.1 percent Register, 800 North Capitol Street, by weight of finished resin. NW., suite 700, Washington, DC 20408. (2) Minimum inherent viscosity: 0.13 (ii) Total extractives not to exceed deciliters per gram. 0.20 percent by weight of homopolymer (3) Maximum residual p- when extracted for 6 hours with dis- dichlorobenzene: 0.8 ppm. tilled water at reflux temperature and (b) Subject to any limitations pre- 0.15 percent by weight of homopolymer scribed in parts 170 through 189 of this when extracted for 6 hours with n- chapter, the following optional sub- heptane at reflux temperature. stances may be added to the (e) Conditions of use. (1) Polyoxy- polyphenylene sulfide basic resins in an methylene homopolymer is for use as amount not to exceed that reasonably
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required to accomplish the intended (a) Identity. For the purpose of this physical or technical effect. section, polyphenylene sulfone resins (1) Substances generally recognized consist of basic resin produced by re- as safe in food. acting polyphenylene sulfide with per- (2) Substances used in accordance acetic acid such that the finished res- with prior sanction or approval. ins meet the specifications set forth in (3) Substances the use of which is paragraph (c) of this section. The permitted in coatings under regula- polyphenylene sulfide used to manufac- tions in parts 170 through 189 of this ture polyphenylene sulfone is prepared chapter. by the reaction of sodium sulfide and p- (c) The finished coatings are ther- dichlorobenzene, and has a minimum mally cured at temperatures of 700 °F weight average molecular weight of and above. 5,000 Daltons. (d) Polyphenylene sulfide resin coat- (b) Optional adjuvant substances. The ings may be used in contact with food basic polyphenylene sulfone resins at temperatures not to exceed the boil- identified in paragraph (a) of this sec- ing point of water; provided that the tion may contain optional adjuvant finished cured coating, when extracted substances required in the production at reflux temperatures for 8 hours sepa- of such basic resins. These optional ad- rately with distilled water, 50 percent juvant substances may include sub- ethanol in water, and 3 percent acetic stances permitted for such use by regu- acid, yields total extractives in each lations in parts 170 through 189 of this extracting solvent not to exceed 0.02 chapter, substances generally recog- milligram per square inch of surface nized as safe in food, or substances and when extracted at reflux tempera- used in accordance with a prior sanc- ture for 8 hours with heptane yields tion or approval. total extractives not to exceed 0.1 mil- (c) Specifications. The glass transition ligram per square inch of surface. temperature of the polymer is 360±5 °C (e) Polyphenylene sulfide resin coat- as determined by the use of differential ings containing perfluorocarbon resins scanning calorimetry. complying with § 177.1550 may be used in contact with food at temperatures [65 FR 15058, Mar. 21, 2000] up to and including normal baking and frying temperatures; provided that the § 177.2510 Polyvinylidene fluoride res- finished cured coating, when extracted ins. at reflux temperatures for 2 hours sepa- Polyvinylidene fluoride resins may rately with distilled water, 50 percent be safely used as articles or compo- ethanol in water, 3 percent acetic acid nents of articles intended for repeated and heptane, yields total extractives in use in contact with food, in accordance each extracting solvent not to exceed with the following prescribed condi- 0.2 milligram per square inch of surface tions: and when extracted at reflux tempera- (a) For the purpose of this section, ture for 1 hour with diphenyl ether the polyvinylidene fluoride resins con- yields total extractives not to exceed sist of basic resins produced by the po- 4.5 milligrams per square inch of sur- lymerization of vinylidene fluoride. face. (b) The finished food-contact article, [42 FR 14572, Mar. 15, 1977, as amended at 47 when extracted at reflux temperatures FR 11846, Mar. 19, 1982; 54 FR 24898, June 12, for 2 hours with the solvents distilled 1989] water, 50 percent (by volume) ethyl al- cohol in distilled water, and n-heptane, § 177.2500 Polyphenylene sulfone res- yields total extractives in each ex- ins. tracting solvent not to exceed 0.01 mil- The polyphenylene sulfone resins ligram per square inch of food-contact (CAS Reg. No. 31833–61–1) identified in surface tested; and if the finished food- paragraph (a) of this section may be contact article is itself the subject of a safely used as articles or components regulation in parts 174, 175, 176, 177, 178 of articles intended for repeated use in and § 179.45 of this chapter, it shall also contact with food, subject to the provi- comply with any specifications and sions of this section. limitations prescribed for it by that
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regulation. (NOTE: In testing the fin- diaminobenzenesulfonic acid, calcium ished food-contact article, use a sepa- salt (2:1) polymer with 1,3- rate test sample for each required ex- benzenediamine, 1,3-benzenedicarbonyl tracting solvent.) dichloride, and 1,4-benzenedicarbonyl (c) In accordance with good manufac- dichloride (CAS Reg. No. 39443–76–0). turing practice, finished food-contact The membrane is the food contact sur- articles containing the polyvinylidene face and may be applied as a film on a fluoride resins shall be thoroughly suitable support. Its maximum weight cleansed prior to their first use in con- is 512 milligrams per square decimeter tact with food. (33 milligrams per square inch). (4) A cross-linked high molecular § 177.2550 Reverse osmosis mem- weight polyamide reaction product of branes. poly(N-vinyl-N-methylamine) (CAS Substances identified in paragraph Reg. No. 31245–56–4), N,N′-bis(3- (a) of this section may be safely used as aminopropyl)ethylenediamine (CAS reverse osmosis membranes intended Reg. No. 10563–26–5), 1,3- for use in processing bulk quantities of benzenedicarbonyl dichloride (CAS liquid food to separate permeate from Reg. No. 99–63–8) and 1,3,5- food concentrate or in purifying water benzenetricarbonyl trichloride (CAS for food manufacturing under the fol- Reg. No. 4422–95–1). The membrane is lowing prescribed conditions: the food-contact surface. Its maximum (a) Identity. For the purpose of this weight is 20 milligrams per square deci- section, reverse osmosis membranes meter (1.3 milligrams per square inch) may consist of either of the following as a thin film composite on a suitable formulations: support. (1) A cross-linked high molecular (5) A polyamide reaction product of weight polyamide reaction product of 1,3,5-benzenetricarbonyl trichloride 1,3,5-benzenetricarbonyl trichloride polymer (CAS Reg. No. 4422–95–1) with with 1,3-benzenediamine (CAS Reg. No. piperazine (CAS Reg. No. 110–85–0) and 83044–99–9) or piperazine (CAS Reg. No. 1,2-diaminoethane (CAS Reg. No. 107– 110–85–0). The membrane is on the food- 15–3). The membrane is the food-con- contact surface, and its maximum tact layer and may be applied as a film weight is 62 milligrams per square deci- on a suitable support. Its maximum meter (4 milligrams per square inch) as weight is 15 milligrams per square deci- a thin film composite on a suitable meter (1 milligram per square inch). support. (b) Optional adjuvant substances. The (2) A cross-linked polyetheramine basic polymer identified in paragraph (CAS Reg. No. 101747–84–6), identified as (a) of this section may contain optional the copolymer of epichlorohydrin, 1,2- adjuvant substances required in the ethanediamine and 1,2-dichloroethane, production of such basic polymer. whose surface is the reaction product These optional adjuvant substances of this copolymer with 2,4- may include substances permitted for toluenediisocyanate (CAS Reg. No. of such use by regulations in parts 170 the final polymer is 99811–80–0) for use through 186 of this chapter, substances as the food-contact surface of reverse generally recognized as safe in food, osmosis membranes used in processing and substances used in accordance with liquid food. The composite membrane a prior sanction or approval. is on the food-contact surface and its (c) Supports. Suitable supports for re- maximum weight is 4.7 milligrams per verse osmosis membranes are mate- square decimeter (0.3 milligrams per rials permitted for such use by regula- square inch) as a thin film composite tions in parts 170 through 186 of this on a suitable support. The maximum chapter, substances generally recog- weight of the 2,4-toluenediisocyanate nized as safe in food, and substances component of the thin film composite used in accordance with a prior sanc- is 0.47 milligrams per square decimeter tion or approval. (0.03 milligrams per square inch). (d) Conditions of use. (1) Reverse os- (3) For the purpose of this section, mosis membranes described in para- the reverse osmosis membrane consists graphs (a)(1), (a)(2), (a)(3), and (a)(5) of of a polyaramide identified as 2,4- this section may be used in contact
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with all types of liquid food at tem- (4) Substances identified in this para- peratures up to 80 °C (176 °F). graph (c)(4), provided that any sub- (2) Reverse osmosis membranes de- stance that is the subject of a regula- scribed in paragraph (a)(4) of this sec- tion in parts 174, 175, 176, 177, 178 and tion may be used in contact with all § 179.45 of this chapter conforms with types of liquid food, except food con- any specification in such regulation. taining more than 8 percent alcohol, at (i) Elastomers. ° ° temperatures up to 80 C (176 F). Acrylonitrile-butadiene copolymer. (3) Reverse osmosis membranes shall Brominated isobutylene-isoprene copolymers be maintained in a sanitary manner in complying with § 177.1210. accordance with current good manufac- Butadiene-acrylonitrile-ethylene glycol turing practice so as to prevent micro- dimethacrylate copolymers containing not bial adulteration of food. more than 5 weight percent of polymer units derived from ethylene glycol (4) To assure their safe use, reverse dimethacrylate. osmosis membranes and their supports Butadiene-acrylonitrile-methacrylic acid co- shall be thoroughly cleaned prior to polymer. their first use in accordance with cur- Butadiene-styrene-methacrylic acid copoly- rent good manufacturing practice. mer. Chloroprene polymers. [49 FR 49448, Dec. 20, 1984, as amended at 52 Chlorotrifluoroethylene-vinylidene fluoride FR 29668, Aug. 11, 1987; 53 FR 31835, Aug. 22, copolymer. 1988; 53 FR 32215, Aug. 24, 1988; 55 FR 8139, Ethylene-propylene copolymer elastomers Mar. 7, 1990; 59 FR 9925, Mar. 2, 1994] which may contain not more than 5 weight-percent of total polymer units de- § 177.2600 Rubber articles intended for rived from 5-methylene-2-norbornene and/ repeated use. or 5-ethylidine-2-norbornene. Rubber articles intended for repeated Ethylene-propylene-dicyclopentadiene co- polymer. use may be safely used in producing, Ethylene-propylene-1,4-hexadiene copoly- manufacturing, packing, processing, mers containing no more than 8 weight preparing, treating, packaging, trans- percent of total polymer units derived porting, or holding food, subject to the from 1,4-hexadiene. provisions of this section. Hydrogenated butadiene/acrylonitrile co- (a) The rubber articles are prepared polymers (CAS Reg. No. 88254–10–8) pro- from natural and/or synthetic polymers duced when acrylonitrile/butadiene copoly- mers are modified by hydrogenation of the and adjuvant substances as described olefinic unsaturation to leave either: (1) in paragraph (c) of this section. Not more than 10 percent trans olefinic (b) The quantity of any substance unsaturation and no α, β-olefinic employed in the production of rubber unsaturation as determined by a method articles intended for repeated use shall entitled ‘‘Determination of Residual α, β- not exceed the amount reasonably re- Olefinic and Trans Olefinic Unsaturation quired to accomplish the intended ef- Levels in HNBR,’’ developed October 1, 1991, by Polysar Rubber Corp., 1256 South fect in the rubber article and shall not Vidal St., Sarnia, Ontario, Canada N7T be intended to accomplish any effect in 7MI; or (2) 0.4 percent to 20 percent olefinic food. unsaturation and Mooney viscosities great- (c) Substances employed in the prep- er than 45 (ML 1 + 4 @ 100 °C), as deter- aration of rubber articles include the mined by ASTM Standard Method D1646– following, subject to any limitations 92, ‘‘Standard Test Method for Rubber— prescribed: Viscosity and Vulcanization Characteris- tics (Mooney Viscometer),’’ which are both (1) Substances generally recognized incorporated by reference in accordance as safe for use in food or food pack- with 5 U.S.C. 552(a) and 1 CFR part 51. Cop- aging. ies of these methods may be obtained from (2) Substances used in accordance the Division of Petition Control (HFS–215), with the provisions of a prior sanction Center for Food Safety and Applied Nutri- or approval. tion, Food and Drug Administration, 200 C (3) Substances that by regulation in St. SW., Washington, DC 20204, or may be examined at the Center for Food Safety parts 170 through 189 of this chapter and Applied Nutrition’s Library, 200 C St. may be safely used in rubber articles, SW., rm. 3321, Washington, DC, or at the subject to the provisions of such regu- Office of the Federal Register, 800 North lation. Capitol St. NW., suite 700, Washington, DC.
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A copy of ASTM Standard Method D1646–92 Vinylidene fluoride-hexafluoropropylene co- may also be obtained from the American polymers (minimum number average mo- Society for Testing and Materials, 100 Barr lecular weight 70,000 as determined by os- Harbor Dr., West Conshohocken, PA 19428– motic pressure in methyl ethyl ketone). 2959. Vinylidene fluoride-hexafluoropropylene- Isobutylene-isoprene copolymer. tetrafluoroethylene copolymers (minimum Polyamide/polyether block copolymers (CAS number average molecular weight 100,000 Reg. No. 77402–38–1 prepared by reacting a as determined by osmotic pressure in copolymer of omega-laurolactam and adipic methyl ethyl ketone). acid with poly(tetramethylene ether gly- col). The polyamide and polyether compo- (ii) Vulcanization materials—(a) Vul- nents are reacted in ratios such that the canizing agents. polyamide component constitutes a min- 4,4′-Bis(aminocyclohexyl)methane carbamate imum of 30 weight-percent of total polymer for use only as cross-linking agent in the units. The copolymers may be used in con- vulcanization of vinylidene tact with foods of Types I, II, III, IV, V, VI, fluoridehexafluoropropylene copolymer VII, VIII, and IX identified in table 1 of and vinylidene fluoride- § 176.170(c) of this chapter at temperatures hexafluoropropylene-tetrafluoroethylene ° not to exceed 150 F except that those co- copolymer elastomers identified under polymers prepared with less than 50 paragraph (c)(4)(i) of this section and lim- weight-percent of polyamide are limited to ited to use at levels not to exceed 2.4 per- use in contact with such foods at tempera- cent by weight of such copolymers. tures not to exceed 100 °F. Diisopropyl xanthogen polysulfide (a 1:2:1 Polybutadiene. mixture of O,O-di(1-methylethyl)trithio- Polyester elastomers derived from the reac- bis-thioformate, O,O-di(1- tion of dimethyl terephthalate, 1,4- methylethyl)tetrathio-bis-thioformate, α butanediol, and -hydro-omega- and O,O-di(1-methylethyl)pentathio-bis- hydroxypoly (oxytetramethylene). Addi- thioformate) for use as a cross linking tionally, trimethyl trimellitate may be agent in the vulcanization of natural rub- used as a reactant. The polyester ber, styrene-butadiene copolymer, acrylo- elastomers may be used only in contact nitrile-butadiene copolymer, and ethylene- with foods containing not more than 8 per- propylene terpolymers identified under cent alcohol and limited to use in contact paragraph (c)(4)(i) of this section and lim- with food at temperatures not exceeding ited to use at levels not to exceed 2.4 per- ° 150 F. cent by weight of such copolymers. Polyisoprene. Hexamethylenediamine carbamate for use Polyurethane resins (CAS Reg. Nos. 37383–28– only as cross-linking agent in the vul- 1 or 9018–04–6) derived from the reaction of canization of vinylidene fluoride- diphenylmethane diisocyanate with 1,4- hexafluoropropylene copolymer and vinyli- butanediol and polytetramethylene ether dene fluoride-hexafluoropropylene-tetra- glycol. fluoroethylene copolymer elastomers iden- Polyurethane resins derived from reactions tified under paragraph (c)(4)(i) of this sec- of diphenylmethane diisocyanate with tion and limited to use at levels not to ex- adipic acid and 1,4-butanediol. ceed 1.5 percent by weight of such copoly- Rubber, natural. mers. Silicone basic polymer as described in ASTM Sulfur, ground. method D1418–81, ‘‘Standard Practice for Rubber and Rubber Latices—Nomen- (b) Accelerators (total not to exceed 1.5 clature,’’ which is incorporated by ref- percent by weight of rubber product). erence. Copies may be obtained from the American Society for Testing Materials, 2-Benzothiazyl-N,N-diethylthiocarbamyl-sul- 1916 Race St., Philadelphia, PA 19103, or fide. may be examined at the Office of the Fed- Benzoyl peroxide. eral Register, 800 North Capitol Street, 1,3-Bis(2-benzothiazolylmercaptomethyl) NW., suite 700, Washington, DC 20408. urea. N-tert-Butyl-2-benzothiazole sulfenamide. Silicone (Si) elastomers containing methyl Butyraldehyde-aniline resin (iodine number groups. 670–705). Silicone (Psi) elastomers containing meth- Carbon disulfide-1,1′-methylenedipiperidine yl and phenyl groups. reaction product. Silicone (Vsi) elastomers containing meth- Copper dimethyldithiocarbamate. yl and vinyl groups. N-Cyclohexyl-2-benzothiazole sulfenamide. Silicone (Fsi) elastomers containing meth- Dibenzoyl-p-quinone dioxime. yl and fluorine groups. Dibenzylamine. Silicone (PVsi) elastomers containing Diisopropyl xanthogen polysulfide (a 1:2:1 phenyl, methyl, and vinyl groups. mixture of O,O-di(1-methylethyl)trithio- Styrene-butadiene copolymer. bis-thioformate, O,O-di(1-
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methylethyl)tetrathio-bis-thioformate, Phthalic anhydride. and O,O-di(1-methylethyl)pentathio-bis- Salicylic acid. thioformate). Di(4-methylbenzoyl) peroxide (CAS Reg. No. (d) Activators (total not to exceed 5 per- 895–85–2) for use only as a crosslinking cent by weight of rubber product except agent in silicone polymers and elastomers magnesium oxide may be used at higher identified under paragraph (c)(4)(i) of this levels). section at levels not to exceed 1 percent by Diethylamine. weight of such polymers and elastomers Fatty acid amines, mixed. where the total of all accelerators does not Fatty acids. exceed 1.5 percent by weight of rubber Magnesium carbonate. product. Magnesium oxide, light and heavy. Di-tert-butyl peroxide. Oleic acid, dibutylamine salt Dibutyl xanthogen disulfide. (dibutylammonium oleate). 2,4-Dichlorobenzoyl peroxide. Stannous chloride. Dicumyl peroxide. Tall oil fatty acids. N,N-Dimethylcyclohexylamine salt of Tetrachloro-p-benzoquinone. dibutyldithiocarbamic acid. Triethanolamine. 2,6-Dimethylmorpholine thiobenzothiazol. Zinc salts of fatty acids. Dipentamethylenethiuram hexasulfide (CAS Reg. No. 971–15–3). (iii) Antioxidants and antiozonants Diphenylguanidine. (total not to exceed 5 percent by weight of Diphenylguanidine phthalate. rubber product). 1,3-Diphenyl-2-thiourea. 2,2′-Dithiobis[benzothiazole]. Aldol-a-naphthylamine. 4,4′-Dithiodimorpholine. Alkylated (C4 and/or C8) phenols. N,N′-Di-o-tolylguanidine. BHT (butylated hydroxytoluene). Di-o-tolylguanidine salt of 4-[[4,6-bis(octylthio)-s-triazin-2-yl]amino]- pyrocatecholborate. 2,6-di-tert-butylphenol (CAS Reg. No. 991– Ethylenediamine carbamate. 84–4) for use only as a stabilizer at levels Heptaldehyde-aniline resin (iodine number not to exceed 0.5 percent by weight of the 430–445). finished rubber product. Hexamethylenetetramine. Butylated reaction product of p-cresol and 2-Mercaptobenzothiazole. dicyclopentadiene as identified in 2-Mercaptothiazoline. § 178.2010(b) of this chapter. N-Oxydiethylene-benzothiazole-2- Butylated, styrenated cresols identified in sulfenamide. § 178.2010(b) of this chapter. ′ Piperidinium pentamethylenedithiocarba- 4,4 -Butylidinebis(6-tert-butyl-m-cresol). ′ mate. N-Cyclohexyl-N -phenylphenylenediamine. ′ Potassium pentamethylenedithiocarbamate. p,p -Diaminodiphenylmethane. p-Quinone dioxime. 2,5-Di-tert-amylhydroquinone. Sodium dibutyldithiocarbamate. Diaryl-p-phenylenediamine, where the aryl Sodium dimethyldithiocarbamate. group may be phenyl, tolyl, or xylyl. Stannous oleate for use only as an accel- 2,6-Di-tert-butyl-p-phenylphenol. erator for silicone elastomers. 1,2-Dihydro-2,2,4-trimethyl-6- Tetrabutylthiuram monosulfide. dodecylquinoline. Tetraethylthiuram disulfide. 1,2-Dihydro-2,2,4-trimethyl-6- (1,1,4,4-Tetramethyltetramethylene)bis [tert- ethoxyquinoline. 1,2-Dihydro-2,2,4-trimethyl-6- butyl peroxide]. phenylquinoline. Tetramethylthiuram monosulfide. 4,4′-Dimethoxydiphenylamine. Thiram (tetramethylthiuram disulfide). 4,6-Dinonyl-o-cresol. Triallyl cyanurate. N,N′-Dioctyl-p-phenylenediamine. Triethylenetetramine. Diphenylamine-acetone resin. 1,3,5-Triethyl-hexahydro-s-triazine Diphenylamine-acetone-formaldehyde resin. (triethyltrimethylenetriamine). N,N′-Diphenylethylenediamine. Triphenylguanidine. N,N′-Disalicylalpropylenediamine. Zinc butyl xanathate. N,N′-Di-o-tolylethylenediamine. Zinc dibenzyl dithiocarbamate. Hydroquinone monobenzyl ether. Zinc dibutyldithiocarbamate. Isopropoxydiphenylamine. Zinc diethyldithiocarbamate. N-Isopropyl-N′-phenyl-p-phenylenediamine. Zinc 2-mercaptobenzothiazole. 2,2′-Methylenebis(6-tert-butyl-4-ethylphenol). Ziram (zinc dimethyldithiocarbamate). 2,2′-Methylenebis(4-methyl-6-tert-butyl- (c) Retarders (total not to exceed 10 per- phenol). cent of weight of rubber product). 2,2′-Methylenebis(4-methyl-6-nonylphenol). 2,2′-Methylenebis(4-methyl-6-tert- Cyanoguanidine. octylphenol).
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Monooctyl- and dioctyldiphenylamine. Diphenyl ketone. N,N′-Di-β-naphthyl-p-phenylenediamine. Fatty acids. Phenyl-a-naphthylamine. Fatty acids, hydrogenated. Phenyl-β-naphthylamine. Isooctyl ester of tall oil fatty acids. Phenyl-β-naphthylamine-acetone aromatic Lanolin. amine resin (average molecular weight 600; a-Methylstyrene-vinyltoluene copolymer nitrogen content 5.3 percent). resins (molar ratio 1 a-methylstyrene to 3 o- and p-Phenylphenol. vinyltoluene). Polybutylated (mixture) 4,4′- Mineral oil; (1) In rubber articles complying isopropylidenediphenol. with this section, not to exceed 30 percent Sodium pentachlorophenate. by weight; (2) Alone or in combination Styrenated cresols produced when 2 moles of with waxes, petroleum, total not to exceed styrene are made to react with 1 mole of a 45 percent by weight of rubber articles that mixture of phenol and o-, m-, and p-cresols contain at least 20 percent by weight of so that the final product has a Brookfield ethylene-propylene copolymer elastomer viscosity at 25 °C of 1400 to 1700 centipoises. complying with paragraph (c)(4)(i) of this Styrenated phenol. section, in contact with foods of Types I, 4,4′-Thiobis (6-tert-butyl-m-cresol). II, III, IV, VI, VII, VIII, and IX idenified in Toluene-2,4-diamine. table 1 of § 176.170(c) of this chapter. N-o-Tolyl-N′-phenyl-p-phenylenediamine. Montan wax. p(p-Tolylsufanilamide) diphenylamine. n-Octyl n-decyl adipate. Tri(mixed mono- and dinonylphenyl) n-Octyl n-decyl phthalate. phosphite. Petrolatum. Tri(nonylphenyl) phosphite-formaldehyde Petroleum hydrocarbon resin resins produced when 1 mole of (cyclopentadiene type), hydrogenated. tri(nonylphenyl) phosphite is made to Petroleum hydrocarbon resin (produced by react with 1.4 moles of formaldehyde or the homo- and copolymerization of dienes produced when 1 mole of nonylphenol is and olefins of the aliphatic, alicyclic, and made to react with 0.36 mole of formalde- monobenzenoid arylalkene types from dis- hyde and the reaction product is then fur- tillates of cracked petroleum stocks). ther reacted with 0.33 mole of phosphorus Petroleum hydrocarbon resin (produced by trichloride. The finished resins have a min- the catalytic polymerization and subse- imum viscosity of 20,000 centipoises at 25 quent hydrogenation of styrene, °C, as determined by LV–series Brookfield vinyltoluene, and indene types from dis- viscometer (or equivalent) using a No. 4 tillates of cracked petroleum stocks). spindle at 12 r.p.m., and have an organic Petroleum oil, sulfonated. phosphorus content of 4.05 to 4.15 percent Phenol-formaldehyde resin. by weight. Pine tar. (iv) Plasticizers (total not to exceed 30 Polybutene. percent by weight of rubber product un- Polystyrene. Propylene glycol. less otherwise specified). n-Propyl ester of tall oil fatty acids. n-Amyl n-decyl phthalate. Rapeseed oil vulcanized with rubber maker’s Butylacetyl ricinoleate. sulfur. n-Butyl ester of tall oil fatty acids. Rosins and rosin derivatives identified in Butyl laurate. § 175.105(c)(5) of this chapter. Butyl oleate. Soybean oil vulcanized with rubber maker’s Butyl stearate. sulfur. Calcium stearate. Styrene-acrylonitrile copolymer. Castor oil. Terpene resins. Coumarone-indene resins. Triethylene glycol dicaprate. 2,2′-Dibenzamidodiphenyl disulfide. Triethylene glycol dicaprylate. Dibenzyl adipate. Waxes, petroleum. Dibutoxyethoxyethyl adipate. Xylene (or toluene) alkylated with Dibutyl phthalate. dicyclopentadiene. Dibutyl sebacate. Zinc 2-benzamidothiophenate. Didecyl adipate. (v) Fillers. Didecyl phthalate. Diisodecyl adipate. Aluminum hydroxide. Diisodecyl phthalate. Aluminum silicate. Diisooctyl adipate. Asbestos fiber, chrysotile or crocidolite. Diisooctyl sebacate. Barium sulfate. Dioctyl adipate. Carbon black (channel process or furnace Dioctyl phthalate. combustion process; total carbon black not Dioctyl sebacate. to exceed 50 percent by weight of rubber Dipentene resin. product; furnace combustion black content
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not to exceed 10 percent by weight of rub- a-(p-Nonylphenyl)-omega-hydroxypoly (oxy- ber products intended for use in contact ethylene) mixture of dihydrogen phosphate with milk or edible oils). and monohydrogen phosphate esters, bar- Cork. ium salt; the nonyl group is a propylene Cotton (floc, fibers, fabric). trimer isomer and the poly (oxyethylene) Mica. content averages 9 moles; for use only as Nylon (floc, fibers, fabric). residual polymerization emulsifier at lev- Silica. els not to exceed 0.7 percent by weight of Titanium dioxide. ethylene-propylene-1,4-hexadiene copoly- Zinc carbonate. mers identified under paragraph (c)(4)(i) of Zinc sulfide. this section. ′ (vi) Colorants. Colorants used in ac- 4,4 -Oxybis (benzenesulfonhydrazide) as chemical blowing agent. cordance with § 178.3297 of this chapter. Phenothiazine. (vii) Lubricants (total not to exceed 2 Potassium persulfate. percent by weight of rubber product). Sodium formaldehyde sulfoxylate. Sodium polysulfide. Polyethylene. Sodium nitrite. Sodium stearate. Sodium salt of ethylenediamine tetraacetic (viii) Emulsifiers. acid and glycine. Sodium sulfide. Fatty acid salts, sodium or potassium. Styrene monomer. Naphthalene sulfonic acid-formaldehyde con- Tall oil. densate, sodium salt. Thioxylenois as peptizing agents. Rosins and rosin-derivatives identified in Tridecyl mercaptan. § 175.105(c)(5) of this chapter. Zinc 4-tert-butylthiophenate as peptizing Sodium decylbenzenesulfonate agent. Sodium dodecylbenzenesulfonate Sodium lauryl sulfate. (d) Rubber articles intended for use Tall oil mixed soap (calcium, potassium, and with dry food are so formulated and sodium). cured under conditions of good manu- (ix) Miscellaneous (total not to exceed 5 facturing practice as to be suitable for percent by weight of rubber product). repeated use. (e) Rubber articles intended for re- Animal glue as described in § 178.3120 of this peated use in contact with aqueous chapter. food shall meet the following specifica- Azodicarbonamide as chemical blowing tions: The food-contact surface of the agent. 2-Anthraquinone sulfonic acid sodium salt rubber article in the finished form in for use only as polymerization inhibitor in which it is to contact food, when ex- chloroprene polymers and not to exceed tracted with distilled water at reflux 0.03 percent by weight of the chloroprene temperature, shall yield total extrac- polymers. tives not to exceed 20 milligrams per 1,2-Benzisothiazolin-3-one (CAS Reg. No. square inch during the first 7 hours of 2634–33–5) for use as a biocide in uncured extraction, nor to exceed 1 milligram liquid rubber latex not to exceed 0.02 per- cent by weight of the latex solids, where per square inch during the succeeding 2 the total of all items listed in paragraph hours of extraction. (c)(4)(ix) of this section does not exceed 5 (f) Rubber articles intended for re- percent of the rubber product. peated use in contact with fatty foods n-Butyllithium for use only as polymeriza- shall meet the following specifications: tion catalyst for polybutadiene. The food-contact surface of the rubber 4-tert-Butyl-o-thiocresol as peptizing agent. article in the finished form in which it tert-Butyl peracetate. is to contact food, when extracted with p-tert-Butylpyrocatechol. ¥ n-hexane at reflux temperature, shall Dialkyl (C8 C18 Di- and triethanolamine. yield total extractives not to exceed Diethyl xanthogen disulfide. 175 milligrams per square inch during 4-(Diiodomethylsulfonyl) toluene, Chemical the first 7 hours of extraction, nor to Abstracts Service Registry No. 20018–09–01, exceed 4 milligrams per square inch for use as an antifungal preservative at during the succeeding 2 hours of ex- levels not to exceed 0.3 percent by weight traction. of the sealants and caulking materials. Dodecyl mercaptan isomers, single or mixed. (g) In accordance with good manufac- 2-Ethoxyethanol. turing practice finished rubber articles Iodoform. intended for repeated use in contact p-Menthane hydroperoxide. with food shall be thoroughly cleansed
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prior to their first use in contact with § 177.2800 Textiles and textile fibers. food. Textiles and textile fibers may safely (h) The provisions of this section are be used as articles or components of ar- not applicable to rubber nursing-bottle ticles intended for use in producing, nipples. manufacturing, packing, processing, (i) Acrylonitrile copolymers identi- preparing, treating, packaging, trans- fied in this section shall comply with porting, or holding food, subject to the the provisions of § 180.22 of this chap- provisions of this section. ter. (a) The textiles and textile fibers are [42 FR 14572, Mar. 15, 1977] prepared from one or more of the fibers EDITORIAL NOTE: For FEDERAL REGISTER ci- identified in paragraph (d) of this sec- tations affecting § 177.2600, see the List of tion and from certain other adjuvant CFR Sections Affected, which appears in the substances required in the production Finding Aids section of the printed volume of the textiles or textile fibers or added and on GPO Access. to impart desired properties. § 177.2710 Styrene-divinylbenzene res- (b) The quantity of any adjuvant sub- ins, cross-linked. stance employed in the production of textiles or textile fibers does not ex- Styrene-divinylbenzene cross-linked ceed the amount reasonably required copolymer resins may be safely used as to accomplish the intended physical or articles or components of articles in- technical effect or any limitation fur- tended for repeated use in producing, ther provided. manufacturing, packing, processing, (c) Any substance employed in the preparing, treating, packaging, trans- production of textiles or textile fibers porting, or holding food, in accordance that is the subject of a regulation in with the following prescribed condi- parts 174, 175, 176, 177, 178 and § 179.45 of tions: this chapter conforms with any speci- (a) The resins are produced by the co- fication in such regulation. polymerization of styrene with divinylbenzene. (d) Substances employed in the pro- (b) The resins meet the extractives duction of or added to textiles and tex- limitations prescribed in this para- tile fibers may include: graph: (1) Substances generally recognized (1) The resins to be tested are ground as safe in food. or cut into small particles that will (2) Substances subject to prior sanc- pass through a U.S. standard sieve No. tion or approval for use in textiles and 3 and that will be held on a U.S. stand- textile fibers and used in accordance ard sieve No. 20. with such sanction or approval. (2) A 100-gram sample of the resins, (3) Substances generally recognized when extracted with 100 milliliters of as safe for use in cotton and cotton fab- ethyl acetate at reflux temperature for rics used in dry-food packaging. 1 hour, yields total extractives not to (4) Substances that by regulation in exceed 1 percent by weight of the res- this part may safely be used in the pro- ins. duction of or as a component of tex- (c) In accordance with good manufac- tiles or textile fibers and subject to turing practice, finished articles con- provisions of such regulation. taining the resins shall be thoroughly (5) Substances identified in this para- cleansed prior to their first use in con- graph (d)(5), subject to such limitations tact with food. as are provided:
List of substances Limitations
(i) Fibers: Cotton. Polyethylene terephthalate complying in composition with For use only in the manufacture of items for repeated use. the provisions of ¤ 177.1630(e)(4)(ii). Rayon. (ii) Adjuvant substances: Aluminum stearate. Borax ...... For use as preservative only. Butyl-acetyl ricinoleate.
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List of substances Limitations
Colorants used in accordance with ¤ 178.3297 of this chapter.. Di-tert-butyl hydroquinone. Dimethylpolysiloxane. Ethylenediaminetetraacetic acid, sodium salt. 4-Ethyl-4-hexadecyl morpholinium ethyl sulfate ...... For use only as a lubricant in the manufacture of polyethylene terephthalate fibers specified in paragraph (d)(5)(i) of this section at a level not to exceed 0.03 percent by weight of the finished fibers. Eugenol. Fats, oils, fatty acids, and fatty alcohols derived from castor, coconut, cottonseed, fish, mustardseed, palm, peanut, rapeseed, ricebran, soybean, sperm, and tall oils and tallow. Fats, oils, fatty acids, and fatty alcohols described in the pre- ceding item reacted with one or more of the following sub- stances: n-Butyl and isobutyl alcohol. Diethylene glycol. Diethanolamine. Glycerol. Hexylene glycol (2-methyl-2,4-pentanediol). Hydrogen. Isopropyl alcohol. Methyl alcohol. Oxygen. Polyethylene glycol (molecular weight 400Ð3,000). Potassium hydroxide. Propylene glycol. Sodium hydroxide. Sulfuric acid. Formaldehyde ...... For use as preservative only. Glyceryl mono-12-hydroxystearate. 2-(9-Heptadecenyl)-1-[2-(10-octadecenamido)ethyl-2- imidazolinium ethyl sulfate. Hexylene glycol (2-methyl,-2,4-pentanediol). Isobutyl alcohol. Isopropyl alcohol. Kerosene. Methyl ester of sulfated ricebran oil. Mineral oil ...... For use only at a level not to exceed 0.15 percent by weight of finished fibers. Mono- and diisopropylated m- and p-cresols (isothymol deriva- tive). N-Oleyl, N′-acetyl, N′-β-hydroxy-ethylenediamine. Petrolatum. Petroleum sulfonate. Pine oil. Polybutene, hydrogenated; complying with the identity pre- scribed under 21 CFR 178.3740(b) of this chapter. Polyethylene, oxidized (air blown). Polyvinyl acetate. Polyvinyl alcohol. Potassium soap of a saponified sulfated castor oil. Sodium bis(2,6-dimethylheptyl-4) sulfosuccinate. Sodium dioctyl sulfosuccinate. Sodium dodecyl benzenesulfonate. Sodium fluoride ...... For use as preservative only. Sodium hydrosulfite. Sodium hypochlorite. Sodium lauryl sulfate. Sodium 2-mercaptobenzothiazole ...... Do. Sodium pentachlorophenate ...... Do. Styrene-butadiene copolymer. Sulfated butyl, isobutyl and propyl oleate. Tallow. Tallow, sulfonated. Titanium dioxide. Triethanolamine. Ultramarine blue. Waxes, petroleum. Zinc hydrosulfite.
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(e) Textile and textile fibers are used practice so as to prevent potential mi- as articles or components of articles crobial adulteration of the food. that contact dry food only. (e) Ultrafiltration membranes identi- (f) The provisions of this section are fied in paragraph (a)(4) may be used to not applicable to jute fibers used as filter aqueous or acidic foods con- prescribed by § 178.3620(d)(2) of this taining up to 13 percent of alcohol at chapter. temperatures not to exceed 21 °C (70 °F). [42 FR 14572, Mar. 15, 1977, as amended at 46 (f) To assure safe use of the ultra-fil- FR 37042, July 17, 1981; 49 FR 4372, Feb. 6, tration membranes, the label or label- 1984; 49 FR 5748, Feb. 15, 1984; 56 FR 42933, Aug. 30, 1991] ing shall include adequate directions for a pre-use treatment, consisting of § 177.2910 Ultra-filtration membranes. conditioning and washing with a min- imum of 8 gallons of potable water Ultra-filtration membranes identi- prior to their first use in contact with fied in paragraphs (a)(1), (a)(2), (a)(3), food. and (a)(4) of this section may be safely (g) Acrylonitrile copolymers identi- used in the processing of food, under fied in this section shall comply with the following prescribed conditions; the provisions of § 180.22 of this chap- (a)(1) Ultra-filtration membranes ter. that consist of paper impregnated with cured phenol-formaldehyde resin, [42 FR 14572, Mar. 15, 1977, as amended at 53 which is used as a support and is coat- FR 17925, May 19, 1988; 58 FR 48599, Sept. 17, ed with a vinyl chloride-acrylonitrile 1993; 60 FR 54426, Oct. 24, 1995] copolymer. (2) Ultra-filtration membranes that PART 178—INDIRECT FOOD ADDI- consist of a sintered carbon support TIVES: ADJUVANTS, PRODUCTION that is coated with zirconium oxide AIDS, AND SANITIZERS (CAS Reg. No. 1314–23–4) containing up to 12 percent yttrium oxide (CAS Reg. Subpart A [Reserved] No. 1314–36–9). (3) Ultra-filtration membranes that Subpart B—Substances Utilized To Control consist of an aluminum oxide support the Growth of Microorganisms that is coated with zirconium oxide Sec. (CAS Reg. No. 1314–23–4) containing up 178.1005 Hydrogen peroxide solution. to 5 percent yttrium oxide (CAS Reg. 178.1010 Sanitizing solutions. No. 1314–36–9). Subpart C—Antioxidants and Stabilizers (4) Ultrafiltration membranes that consist of a microporous 178.2010 Antioxidants and/or stabilizers for poly(vinylidene fluoride) membrane polymers. with a hydrophilic surface modifier 178.2550 4-Hydroxymethyl-2,6-di-tert-butyl- consisting of hydroxypropyl acrylate/ phenol. tetraethylene glycol diacrylate copoly- 178.2650 Organotin stabilizers in vinyl chlo- ride plastics. mer. (b) Any substance employed in the Subpart D—Certain Adjuvants and production of ultra-filtration mem- Production Aids branes that is the subject of a regula- tion in parts 174, 175, 176, 177, 178 and 178.3010 Adjuvant substances used in the § 179.45 of this chapter conforms with manufacture of foamed plastics. 178.3120 Animal glue. the specifications of such regulation. 178.3125 Anticorrosive agents. (c) Ultra-filtration membranes are 178.3130 Antistatic and/or antifogging used in the physical separation of dis- agents in food-packaging materials. solved or colloidally suspended varying 178.3280 Castor oil, hydrogenated. molecular size components of liquids 178.3290 Chromic chloride complexes. during the commercial processing of 178.3295 Clarifying agents for polymers. bulk quantities of food. 178.3297 Colorants for polymers. 178.3300 Corrosion inhibitors used for steel (d) Ultra-filtration membranes shall or tinplate. be maintained in a sanitary manner in 178.3400 Emulsifiers and/or surface-active accordance with good manufacturing agents.
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