Pt. 177 21 CFR Ch. I (4–1–99 Edition)
PART 177—INDIRECT FOOD 177.1570 Poly-1-butene resins and butene/ ethylene copolymers. ADDITIVES: POLYMERS 177.1580 Polycarbonate resins. 177.1585 Polyestercarbonate resins. Subpart A [Reserved] 177.1590 Polyester elastomers. 177.1595 Polyetherimide resin. Subpart B—Substances for Use as Basic 177.1600 Polyethylene resins, carboxyl modi- Components of Single and Repeated fied. Use Food Contact Surfaces 177.1610 Polyethylene, chlorinated. 177.1615 Polyethylene, fluorinated. Sec. 177.1620 Polyethylene, oxidized. 177.1010 Acrylic and modified acrylic plas- 177.1630 Polyethylene phthalate polymers. tics, semirigid and rigid. 177.1632 Poly (phenyleneterephthalamide) 177.1020 Acrylonitrile/butadiene/styrene co– resins. polymer. 177.1635 Poly(p-methylstyrene) and rubber- 177.1030 Acrylonitrile/butadiene/styrene/ modified poly(p-methylstyrene). methyl methacrylate copolymer. 177.1637 Poly(oxy-1,2- 177.1040 Acrylonitrile/styrene copolymer. ethanediyloxycarbonyl-2,6- 177.1050 Acrylonitrile/styrene copolymer naphthalenediylcarbonyl) resins. modified with butadiene/styrene elas- 177.1640 Polystyrene and rubber-modified tomer. polystyrene. 177.1060 n-Alkylglutarimide/acrylic copoly- 177.1650 Polysulfide polymer-polyepoxy res- mers. ins. 177.1200 Cellophane. 177.1655 Polysulfone resins. 177.1210 Closures with sealing gaskets for 177.1660 Poly (tetramethylene food containers. terephthalate). 177.1240 1,4-Cyclohexylene dimethylene 177.1670 Polyvinyl alcohol film. terephthalate and 1,4-cyclohexylene 177.1680 Polyurethane resins. dimethylene isophthalate copolymer. 177.1810 Styrene block polymers. 177.1820 Styrene-maleic anhydride copoly- 177.1310 Ethylene-acrylic acid copolymers. mers. 177.1312 Ethylene-carbon monoxide copoly- 177.1830 Styrene-methyl methacrylate co- mers. polymers. 177.1315 Ethylene-1,4-cyclohexylene 177.1850 Textryls. dimethylene terephthalate copolymers. 177.1900 Urea-formaldehyde resins in molded 177.1320 Ethylene-ethyl acrylate copoly- articles. mers. 177.1950 Vinyl chloride-ethylene copoly- 177.1330 Ionomeric resins. mers. 177.1340 Ethylene-methyl acrylate copoly- 177.1960 Vinyl chloride-hexene-1 copoly- mer resins. mers. 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. 177.1420 Isobutylene polymers. Repeated Use 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.
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177.2450 Polyamide-imide resins. more of the acrylic or methacrylic 177.2460 Poly(2,6-dimethyl-1,4-phenylene) monomers listed in paragraph (a)(1) of oxide resins. this section. 177.2465 Polymethylmethacrylate/poly(tri methoxysilylpropyl) methacrylate co- (1) Homopolymers and copolymers of polymers. the following monomers: 177.2470 Polyoxymethylene copolymer. n-Butyl acrylate. 177.2480 Polyoxymethylene homopolymer. n-Butyl methacrylate. 177.2490 Polyphenylene sulfide resins. Ethyl acrylate. 177.2510 Polyvinylidene fluoride resins. 2-Ethylhexyl acrylate. 177.2550 Reverse osmosis membranes. Ethyl methacrylate. 177.2600 Rubber articles intended for re- Methyl acrylate. peated use. Methyl methacrylate. 177.2710 Styrene-divinylbenzene resins, cross-linked. (2) Copolymers produced by copolym- 177.2800 Textiles and textile fibers. erizing one or more of the monomers 177.2910 Ultra-filtration membranes. listed in paragraph (a)(1) of this section AUTHORITY: 21 U.S.C. 321, 342, 348, 379e. with one or more of the following monomers: SOURCE: 42 FR 14572, Mar. 15, 1977, unless otherwise noted. Acrylonitrile. EDITORIAL NOTE: Nomenclature changes to Methacrylonitrile. α part 177 appear at 61 FR 14482, Apr. 2, 1996. -Methylstyrene. Styrene. Vinyl chloride. Subpart A [Reserved] Vinylidene chloride. (3) Polymers identified in paragraphs Subpart B—Substances for Use as (a)(1) and (2) of this section containing Basic Components of Single no more than 5 weight-percent of total and Repeated Use Food Con- polymer units derived by copolym- tact Surfaces erization with one or more of the monomers listed in paragraph (a)(3)(i) § 177.1010 Acrylic and modified acrylic and (ii) of this section. Monomers list- plastics, semirigid and rigid. ed in paragraph (a)(3)(ii) of this section Semirigid and rigid acrylic and modi- are limited to use only in plastic arti- fied acrylic plastics may be safely used cles intended for repeated use in con- as articles intended for use in contact tact with food. 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. semirigid and rigid acrylic and modi- Itaconic acid. 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 weight-percent of the polymer content Service Registry No. 96–05–9] 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.
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Dimethylaminoethyl methacrylate. and oils, and fatty alcohols derived 2-Ethylhexyl methacrylate. from such acids. Hydroxyethyl methacrylate. (7) Surface active agent: Sodium Hydroxyethyl vinyl sulfide. Hydroxypropyl methacrylate. dodecylbenzenesulfonate. Isobornyl methacrylate. (8) Miscellaneous materials: Isobutyl methacrylate. Di(2-ethylhexyl) phthalate, for use only as a Isopropyl acrylate. flow promoter at a level not to exceed 3 Isopropyl methacrylate. weight-percent based on the monomers. Methacrylamide. Dimethyl phthalate. Methacrylamidoethylene urea. Oxalic acid, for use only as a polymerization Methacryloxyacetamidoethylethylene urea. catalyst aid. Methacryloxyacetic acid. Tetraethylenepentamine, for use only as a n-Propyl methacrylate. catalyst activator at a level not to exceed 3,5,5-Trimethylcyclohexyl methacrylate. 0.5 weight-percent based on the monomers. (4) Polymers identified in paragraphs Toluene. (a)(1), (2), and (3) of this section are Xylene. mixed together and/or with the fol- (b) The semirigid and rigid acrylic lowing polymers, provided that no and modified acrylic plastics, in the chemical reactions, other than addi- finished form in which they are to con- tion reactions, occur when they are tact food, when extracted with the sol- mixed: vent or solvents characterizing the type of food and under the conditions Butadiene-acrylonitrile copolymers. Butadiene-acrylonitrile-styrene copolymers. of time and temperature as determined Butadiene-acrylonitrile-styrene-methyl from tables 1 and 2 of § 176.170(c) of this methacrylic copolymers. chapter, shall yield extractives not to Butadiene-styrene copolymers. exceed the following, when tested by Butyl rubber. the methods prescribed in paragraph Natural rubber. (c) of this section. The acrylic and Polybutadiene. modified acrylic polymers or plastics Poly (3-chloro-1,3-butadiene). Polyester identified in § 175.300(b)(3)(vii) of intended to be used as components of this chapter. articles also shall yield extractives not Polyvinyl chloride. to exceed the following limitations Vinyl chloride copolymers complying with when prepared as strips as described in § 177.1980. paragraph (c)(2) of this section: Vinyl chloride-vinyl acetate copolymers. (1) Total nonvolatile extractives not (5) Antioxidants and stabilizers iden- to exceed 0.3 milligram per square inch tified in § 175.300(b)(3)(xxx) of this chap- of surface tested. ter and the following: (2) Potassium permanganate oxidiz- able distilled water and 8 and 50 per- Di-tert-butyl-p-cresol. cent alcohol extractives not to exceed 2-Hydroxy-4-methoxybenzophenone. an absorbance of 0.15. 2-Hydroxy-4-methoxy-2- carboxybenzophenone. (3) Ultraviolet-absorbing distilled 3-Hydroxyphenyl benzoate. water and 8 and 50 percent alcohol ex- p-Methoxyphenol. tractives not to exceed an absorbance Methyl salicylate. of 0.30. Octadecyl 3,5-di-tert-butyl-4-hydroxyhydro- (4) Ultraviolet-absorbing n-heptane cinnamate (CAS Reg. No. 2082–79–3): For extractives not to exceed an absorb- use only: (1) At levels not exceeding 0.2 ance of 0.10. percent by weight in semirigid and rigid (c) Analytical methods—(1) Selection of acrylic and modified acrylic plastics, where the finished articles contact foods extractability conditions. These are to be containing not more than 15 percent alco- chosen as provided in § 176.170(c) of this hol; and (2) at levels not exceeding 0.01 per- chapter. cent by weight in semirigid and rigid (2) Preparation of samples. Sufficient acrylic and modified acrylic plastics in- samples to allow duplicates of all ap- tended for repeated food-contact use where plicable tests shall be cut from the ar- the finished article may be used for foods ticles or formed from the plastic com- containing more than 15 percent alcohol. position under tests, as strips about 2.5 Phenyl salicylate. inches by about 0.85-inch wide by about (6) Release agents: Fatty acids de- 0.125-inch thick. The total exposed sur- rived from animal and vegetable fats face should be 5 square inches ±0.5-
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square inch. The samples, after prepa- ured versus distilled water in the ref- ration, shall be washed with a clean erence cell shall not exceed 0.15 at 245, brush under hot tapwater, rinsed under 0.09 at 260, 0.04 at 270, and 0.02 at any running hot tapwater (140 °F min- point in the wavelength region of 280 to imum), rinsed with distilled water, and 310 mµ. air-dried in a dust-free area or in a des- (iii) Duplicate ultraviolet blank de- iccator. terminations shall be run on samples of (3) Preparation of solvents. The water each solvent that has been exposed to used shall be double-distilled water, the temperature-time conditions of the prepared in a still using a block tin extraction test without the plastic condenser. The 8 and 50 percent (by vol- sample. An aliquot of the exposed sol- ume) alcohol solvents shall be prepared vent shall be measured versus the un- from ethyl alcohol meeting the speci- exposed solvent in the reference cell. fications of the United States Pharma- The average difference in the copeia XX and diluted with double-dis- absorbances at any wavelength in the tilled water that has been prepared in a region of 245 to 310 mµ shall be used as still using a tin block condenser. The a blank correction for the ultraviolet n-heptane shall be spectrophotometric absorbers measured at the same wave- grade. Adequate precautions must be length according to paragraph (c)(8)(ii) taken to keep all solvents dust-free. of this section. (4) Blank values on solvents. (i) Dupli- (iv) The acceptability of the solvents cate determinations of residual solids for use in the permanganate test shall shall be run on samples of each solvent be determined by preparing duplicate that have been exposed to the tempera- permanganate test blanks according to ture-time conditions of the extraction paragraph (c)(7)(iv) of this section. For test without the plastic sample. Sixty this test, the directions referring to milliliters of exposed solvent is the sample extract shall be dis- pipetted into a clean, weighed plat- regarded. The blanks shall be scanned inum dish, evaporated to 2–5 milliliters in 5-centimeter silica on a nonsparking, low-temperature hot spectrophotometric cells in the spec- plate and dried in 212 °F oven for 30 trophotometer versus the appropriate minutes. The residue for each solvent solvent as reference. The absorbance in shall be determined by weight and the distilled water in the wavelength re- 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 scribed in paragraph (c)(7)(iv) of this air in the reference cell shall not ex- section, except that the appropriate ex- ceed 0.03 at any point in the wave- posed solvent shall be substituted length region of 245 to 310 mµ. The ab- where the directions call for sample ex- sorbance of the 8 percent alcohol when tract. The average difference in the measured versus distilled water in the absorbances in the region of 544 to 552 reference cell shall not exceed 0.01 at mµ shall be used as a blank correction any point in the wavelength region of for the determination of permanganate 245 to 310 mµ. The absorbance of the 50 oxidizable extractives according to percent alcohol when measured versus paragraph (c)(7)(iv) of this section. distilled water in the reference cell (5) Extraction procedure. For each ex- shall not exceed 0.05 at any point in the traction, place a plastic sample in a wavelength region of 245 to 310 mµ. The clean 25 millimeters × 200 millimeters absorbance of the heptane when meas- hard-glass test tube and add solvent
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equal to 10 milliliters of solvent per s=Total surface of the plastic sample in square inch of plastic surface. This square inches. amount will be between 45 milliliters (7) Determination of potassium per- and 55 milliliters. The solvent must be manganate oxidizable extractives. (i) Pi- preequilibrated to the temperature of pette 25 milliliters of distilled water the extraction test. Close the test tube with a ground-glass stopper and expose into a clean 125-milliliter Erlenmeyer to the specified temperature for the flask that has been rinsed several specified time. Cool the tube and con- times with aliquots of distilled water. tents to room temperature if nec- This is the blank. Prepare a distilled essary. water solution containing 1.0 part per (6) Determination of total nonvolatile million of p-methoxyphenol (melting extractives. Remove the plastic strip point 54–56 °C, Eastman grade or equiv- from the solvent with a pair of clean alent). Pipette 25 milliliters of this p- forceps and wash the strip with 5 milli- methoxyphenol solution into a rinsed liters of the appropriate solvent, add- Erlenmeyer flask. Pipette exactly 3.0 ing the washings to the contents of the milliliters of 154 parts per million test tube. Pour the contents of the test aqueous potassium permanganate solu- tube into a clean, weighed platinum tion into the p-methoxyphenol and ex- dish. Wash the tube with 5 milliliters actly 3.0 milliliters into the blank, in of the appropriate solvent and add the that order. Swirl both flasks to mix the solvent to the platinum dish. Evapo- contents and then transfer aliquots rate the solvent to 2–5 milliliters on a from each flask into matched 5-centi- nonsparking, low-temperature meter spectrophotometric absorption hotplate. Complete the evaporation in cells. The cells are placed in the spec- a 212 °F oven for 30 minutes. Cool the trophotometer cell compartment with dish in a desiccator for 30 minutes and the p-methoxyphenol solution in the weigh to the nearest 0.1 milligram. Cal- culate the total nonvolatile extractives reference beam. Spectrophotometric as follows: measurement is conducted as in para- graph (c)(7)(iv) of this section. The ab- e− b sorbance reading in the region 544–552 Milligrams extractives = µ per square inch m should be 0.24 but must be not less s than 0.12 nor more than 0.36. This test shall be run in duplicate. For the pur- Extractives in parts eb = ×100 pose of ascertaining compliance with per million the limitations in paragraph (b)(2) of s this section, the absorbance measure- where: ments obtained on the distilled water e=Total increase in weight of the dish, in extracts according to paragraph milligrams. b=Blank value of the solvent in milligrams, (c)(7)(iv) of this section shall be multi- as determined in paragraph (c)(4)(i) of plied by a correction factor, calculated this section. as follows:
0. 24 = 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 more than 0.39. This test shall be run in (c)(7)(i) of this section is repeated ex- duplicate. For the purpose of cept that, in this instance, the solvent ascertaining compliance with the limi- shall be 8 percent alcohol. The absorb- tations prescribed in paragraph (b)(2) of ance in the region 544–552 mµ should be 0.26 but must be not less than 0.13 nor
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this section, the absorbance measure- (c)(7)(iv) of this section shall be multi- ments obtained on the 8 percent alco- plied by a correction factor, calculated hol extracts according to paragraph as follows:
0. 26 = 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 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 50 percent alcohol. The absorb- ments obtained on the 50 percent alco- ance in the region 544–552 mµ should be hol extracts according to paragraph 0.25 but must be not less than 0.12 nor (c)(7)(iv) of this section shall be multi- more than 0.38. This test shall be run in plied by a correction factor, calculated duplicate. For the purpose of as follows:
0. 25 = 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 sorbance scale from 700 mµ to 500 mµ in extracts. Pipette 25 milliliters of the ap- such a way that the region 544 mµ to propriate solvent into a clean, 125-mil- 552 mµ is scanned within 5 minutes to liliter Erlenmeyer flask that has been 10 minutes of the time that permanga- rinsed several times with aliquots of nate was added to the solutions. The the same solvent. This is the blank. height of the absorbance peak shall be Into another similarly rinsed flask, pi- measured, corrected for the blank as pette 25 milliliters of the sample ex- determined in paragraph (c)(4)(v) of tract that has been exposed under the this section, and multiplied by the ap- conditions specified in paragraph (c)(5) propriate correction factor determined of this section. Pipette exactly 3.0 mil- according to paragraph (c)(7) (i), (ii), liliters of 154 parts per million aqueous and (iii) of this section. This test shall potassium permanganate solution into be run in duplicate and the two results the sample and exactly 3.0 milliliters averaged. into the blank, in that order. Before (8) Determination of ultraviolet-absorb- use, the potassium permanganate solu- ing extractives. (i) A distilled water so- tion shall be checked as in paragraph lution containing 1.0 part per million (c)(7)(i) of this section. Both flasks are of p-methoxyphenol (melting point 54 swirled to mix the contents, and then °C–56 °C. Eastman grade or equivalent) aliquots from each flask are trans- shall be scanned in the region 360 to 220 ferred to matched 5-centimeter mµ in 5-centimeter silica spectrophoto- spectrophotometric absorption cells. metric absorption cells versus a dis- Both cells are placed in the spectro- tilled water reference. The absorbance photometer cell compartment with the at the wavelength of maximum absorb- sample solution in the reference beam. ance (should be about 285 mµ) is about The spectrophotometer is adjusted for 0.11 but must be not less than 0.08 nor 0 and 100 percent transmittance at 700 more than 0.14. This test shall be run in mµ. The spectrum is scanned on the ab- duplicate. For the purpose of
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ascertaining compliance with the limi- paragraph (c)(8)(ii) of this section shall tations prescribed in paragraph (b) (3) be multiplied by a correction factor, and (4) of this section, the absorbance calculated as follows: obtained on the extracts according to
0. 11 = 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 the article in the finished form in been exposed under the conditions which it is to contact food. specified in paragraph (c)(5) of this sec- [42 FR 14572, Mar. 15, 1977; 42 FR 56728, Oct. tion is scanned in the wavelength re- 28, 1977, as amended at 43 FR 54927, Nov. 24, gion 360 to 220 mµ versus the appro- 1978; 45 FR 67320, Oct. 10, 1980; 46 FR 46796, priate solvent reference in matched 5- Sept. 22, 1981; 49 FR 10108, Mar. 19, 1984; 49 FR centimeter silica spectrophotometric 13139, Apr. 3, 1984; 50 FR 31045, July 24, 1985] absorption cells. The height of any ab- § 177.1020 Acrylonitrile/butadiene/sty- sorption peak shall be measured, cor- rene co-polymer. rected for the blank as determined in paragraph (c)(4)(iii) of this section, and Acrylonitrile/butadiene/styrene co- multiplied by the correction factor de- polymer identified in this section may be safely used as an article or compo- termined according to paragraph nent of articles intended for use with (c)(8)(i) of this section. all foods, except those containing alco- (d) In accordance with current good hol, under conditions of use E, F, and G manufacturing practice, finished described in table 2 of § 176.170(c) of this semirigid and rigid acrylic and modi- chapter. fied acrylic plastics, and articles con- (a) Identity. For the purpose of this taining these polymers, intended for section, the acrylonitrile/butadiene/ repeated use in contact with food shall styrene copolymer consists of: be thoroughly cleansed prior to their (1) Eighty-four to eighty-nine parts first use in contact with food. by weight of a matrix polymer con- (e) Acrylonitrile copolymers identi- taining 73 to 78 parts by weight of acry- fied in this section shall comply with lonitrile and 22 to 27 parts by weight of the provisions of § 180.22 of this chap- styrene; and ter. (2) Eleven to sixteen parts by weight (f) The acrylic and modified acrylic of a grafted rubber consisting of (i) 8 to polymers identified in and complying 13 parts of butadiene/styrene elastomer with this section, when used as compo- containing 72 to 77 parts by weight of nents of the food-contact surface of an butadiene and 23 to 28 parts by weight article that is the subject of a regula- of styrene and (ii) 3 to 8 parts by tion in this part and in parts 174, 175, weight of a graft polymer having the same composition range as the matrix 176, and 178 of this chapter, shall com- polymer. ply with any specifications and limita- (b) Adjuvants. The copolymer identi- tions prescribed by such regulation for fied in paragraph (a) of this section
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may contain adjuvant substances re- water and 3 percent acetic acid at 150 quired in its production. Such adju- °F for 15 days when analyzed by a po- vants may include substances gen- larographic method titled ‘‘Extracted erally recognized as safe in food, sub- Acrylonitrile by Differential Pulse Po- stances used in accordance with prior larography,’’ which is incorporated by sanction, substances permitted in this reference. Copies are available from part, and the following: the Center for Food Safety and Applied Nutrition (HFS–200), Food and Drug Substance Limitations Administration, 200 C St. SW., Wash- 2-Mercapto- ethanol ...... The finished copolymer shall ington, DC 20204, or available for in- contain not more than 100 spection at the Office of the Federal ppm 2-mercaptoethanol ac- Register, 800 North Capitol Street, rylonitrile adduct as deter- mined by a method titled NW., suite 700, Washington, DC 20408. ``Analysis of Cycopac (e) Acrylonitrile copolymers identi- Resin for Residual β-(2- fied in this section shall comply with Hydroxyethylmercapto) pro- pionitrile,'' which is incor- the provisions of § 180.22 of this chap- porated by reference. Cop- ter. ies are available from the (f) Acrylonitrile copolymers identi- Bureau of Foods (HFS± 200), Food and Drug Ad- fied in this section are not authorized ministration, 200 C St. to be used to fabricate beverage con- SW., Washington, DC tainers. 20204, or available for in- spection at the Office of [42 FR 14572, Mar. 15, 1977, as amended at 42 the Federal Register, 800 FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, North Capitol Street, NW., suite 700, Washington, DC 1982; 54 FR 24897, June 12, 1989] 20408. § 177.1030 Acrylonitrile/butadiene/sty- (c) Specifications. (1) Nitrogen content rene/methyl methacrylate copoly- of the copolymer is in the range of 16 mer. to 18.5 percent as determined by Micro- Acrylonitrile/butadiene/styrene/ Kjeldahl analysis. methyl methacrylate copolymer iden- (2) Residual acrylonitrile monomer tified in this section may be safely content of the finished copolymer arti- used as an article or component of arti- cles is not more than 11 parts per mil- cles intended for use with food identi- lion as determined by a gas fied in table 1 of § 176.170(c) of this chromatographic method titled ‘‘De- chapter as Type I, II, III, IVA, IVB, V, termination of Residual Acrylonitrile VIB, (except bottles intended to hold and Styrene Monomers-Gas carbonated beverages), VIIA, VIIB, VIII Chromatographic Internal Standard and IX, under conditions of use C, D, E, Method,’’ which is incorporated by ref- F, and G described in table 2 of erence. Copies are available from the § 176.170(c) of this chapter with a high Center for Food Safety and Applied Nu- temperature limitation of 190 °F. trition (HFS–200), Food and Drug Ad- (a) Identity. For the purpose of this ministration, 200 C St. SW., Wash- section, acrylonitrile/butadiene/sty- ington, DC 20204, or available for in- rene/methyl methacrylate copolymer spection at the Office of the Federal consists of: (1) 73 to 79 parts by weight Register, 800 North Capitol Street, of a matrix polymer containing 64 to 69 NW., suite 700, Washington, DC 20408. parts by weight of acrylonitrile, 25 to (d) Extractive limitations. (1) Total 30 parts by weight of styrene and 4 to nonvolatile extractives not to exceed 6 parts by weight of methyl methacry- 0.0005 milligram per square inch sur- late; and (2) 21 to 27 parts by weight of face area when the finished food con- a grafted rubber consisting of (i) 16 to tact article is exposed to distilled 20 parts of butadiene/styrene/elastomer water, 3 percent acetic acid, or n- containing 72 to 77 parts by weight of heptane for 8 days at 120 °F. butadiene and 23 to 28 parts by weight (2) The finished food-contact article of styrene and (ii) 5 to 10 parts by shall yield not more than 0.0015 milli- weight of a graft polymer having the gram per square inch of acrylonitrile same composition range as the matrix monomer when exposed to distilled polymer.
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(b) Adjuvants. The copolymer identi- (2) The finished food-contact article fied in paragraph (a) of this section shall yield not more than 0.0025 milli- may contain adjuvant substances re- gram per square inch of acrylonitrile quired in its production. Such adju- monomer when exposed to distilled vants may include substances gen- water, 3 percent acetic acid and n- erally recognized as safe in food, sub- heptane at 190 °F for 2 hours, cooled to stances used in accordance with prior 120 °F (80 to 90 minutes) and main- sanction, substances permitted under tained at 120 °F for 10 days when ana- applicable regulations in this part, and lyzed by a polarographic method titled the following: ‘‘Extracted Acrylonitrile by Differen- tial Pulse Polarography,’’ which is in- Substances Limitations corporated by reference. Copies are available from the Center for Food 2±Mercaptoethanol ...... The finished copolymer shall Safety and Applied Nutrition (HFS– contain not more than 800 ppm 2±mercaptoethanol 200), Food and Drug Administration, acrylonitrile adduct as de- 200 C St. SW., Washington, DC 20204, or termined by a method titled available for inspection at the Office of ``Analysis of Cycopac Resin for Residual β±(2± the Federal Register, 800 North Capitol Hydroxyethylmercapto) pro- Street, NW., suite 700, Washington, DC pionitrile,'' which is incor- 20408. porated by reference. Cop- (e) Acrylonitrile copolymers identi- ies are available from the Bureau of Foods (HFS± fied in this section shall comply with 200), Food and Drug Ad- the provisions of § 180.22 of this chap- ministration, 200 C St. ter. SW., Washington, DC 20204, or available for in- (f) Acrylonitrile copolymers identi- spection at the Office of fied in this section are not authorized the Federal Register, 800 to be used to fabricate beverage con- North Capitol Street, NW., tainers. suite 700, Washington, DC 20408. [42 FR 14572, Mar. 15, 1977, as amended at 42 FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, (c) Specifications. (1) Nitrogen content 1982; 54 FR 24898, June 12, 1989] of the copolymer is in the range of 13.0 to 16.0 percent as determined by Micro- § 177.1040 Acrylonitrile/styrene copoly- Kjeldahl analysis. mer. (2) Residual acrylonitrile monomer Acrylonitrile/styrene copolymers content of the finished copolymer arti- identified in this section may be safely cles is not more than 11 parts per mil- used as a component of packaging ma- lion as determined by a gas terials subject to the provisions of this chromatographic method titled ‘‘De- section. termination of Residual Acrylonitrile (a) Identity. For the purposes of this section acrylonitrile/styrene copoly- and Styrene Monomers-Gas mers are basic copolymers meeting the Chromatographic Internal Standard specifications prescribed in paragraph Method,’’ which is incorporated by ref- (c) of this section. erence. Copies are available from the (b) Adjuvants. (1) The copolymers Center for Food Safety and Applied Nu- identified in paragraph (c) of this sec- trition (HFS–200), Food and Drug Ad- tion may contain adjuvant substances ministration, 200 C St. SW., Wash- required in their production, with the ington, DC 20204, or available for in- exception that they shall not contain spection at the Office of the Federal mercaptans or other substances which Register, 800 North Capitol Street, form reversible complexes with acryl- NW., suite 700, Washington, DC 20408. onitrile monomer. Permissible adju- (d) Extractive limitations. (1) Total vants may include substances gen- nonvolatile extractives not to exceed erally recognized as safe in food, sub- 0.0005 milligram per square inch sur- stances used in accordance with prior face area of the food-contact article sanction, substances permitted under when exposed to distilled water, 3 per- applicable regulations in this part, and cent acetic acid, 50 percent ethanol, those authorized in paragraph (b)(2) of and n-heptane for 10 days at 120 °F. this section.
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(2) The optional adjuvants for the ac- Substances Limitation rylonitrile/styrene copolymer identi- Condensation polymer of toluene 0.15 pct maximum. fied in paragraphs (c) (1) and (3) of this sulfonamide and formaldehyde. section are as follows: (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 66± area of the food contact article weight is 30,000.1 72 parts by weight of acrylo- when exposed to distilled water nitrile and 28±34 parts by weight and 3 pct acetic acid for 10 d at of styrene; for use with food of 66 °C (150 °F). Type VI±B 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. 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 45± 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 35±55 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 66± 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 28±34 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 VI±A and VI±B 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 (HFS±200), 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 (HFS±200), 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 D±1434±82, ``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 (HFS±200), 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- (e) Acrylonitrile copolymer identified polymers identified in this section in this section may be used to fabricate shall comply with the provisions of § 180.22 of this chapter.
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beverage containers only if they com- Substances Limitations ply with the specifications of item 3 in n-Dodecylmercaptan ...... The finished copolymer shall paragraph (c) of this section. contain not more than 500 parts per million (ppm) [42 FR 14572, Mar. 15, 1977, as amended at 42 dodecylmercaptan as FR 48543, Sept. 23, 1977; 47 FR 11841, Mar. 19, dodecylmercapto- 1982; 49 FR 36643, Sept. 19, 1984; 52 FR 33803, propionitrile as determined Sept. 8, 1987] by the method titled, ``De- termination of β-Dodecyl- mercaptopropionitrile in § 177.1050 Acrylonitrile/styrene copoly- NR±16 Polymer,'' which is mer modified with butadiene/sty- incorporated by reference. rene elastomer. Copies are available from the Center for Food Safety Acrylonitrile/styrene copolymer and Applied Nutrition modified with butadiene/styrene elas- (HFS±200), Food and Drug Administration, 200 C St., tomer identified in this section may be SW., Washington, DC safely used as a component of bottles 20204, or available for in- intended for use with foods identified spection at the Office of the Federal Register, 800 in table I of § 176.170(c) of this chapter North Capitol Street, NW., as Type VI–B under conditions for use suite 700, Washington, DC E, F, or G described in table 2 of 20408. § 176.170(c) of this chapter. (c) Specifications. (1) Nitrogen content (a) For the purpose of this Identity. of the modified copolymer is in the section, acrylonitrile/styrene copoly- range of 17.7–19.8 percent. mer modified with butadiene/styrene (2) Intrinsic viscosity of the matrix elastomer consists of a blend of: copolymer in butyrolactone is not less (1) 82–88 parts by weight of a matrix than 0.5 deciliter/gram at 35 °C, as de- copolymer produced by polymerization termined by the method titled ‘‘Molec- of 77–82 parts by weight of acrylonitrile ular Weight of Matrix Copolymer by and 18–23 parts of styrene; and Solution Viscosity,’’ which is incor- (2) 12–18 parts by weight of a grafted porated by reference. Copies are avail- rubber consisting of (i) 8–12 parts of bu- able from the Center for Food Safety tadiene/styrene elastomer containing and Applied Nutrition (HFS–200), Food 77–82 parts by weight of butadiene and and Drug Administration, 200 C St. 18–23 parts by weight of styrene and (ii) SW., Washington, DC 20204, or available 4–6 parts by weight of a graft copoly- for inspection at the Office of the Fed- mer consisting of 70–77 parts by weight eral Register, 800 North Capitol Street, of acrylonitrile and 23–30 parts by NW., suite 700, Washington, DC 20408. weight of styrene. (3) Residual acrylonitrile monomer content of the modified copolymer ar- (b) Adjuvants. The modified copoly- ticles is not more than 11 ppm as deter- mer identified in paragraph (a) of this mined by a gas chromatographic meth- section may contain adjuvant sub- od titled ‘‘Determination of Residual stances required in its production. Acrylonitrile and Styrene Monomers- Such adjuvants may include substances Gas Chromatographic Internal Stand- generally recognized as safe in food, ard Method,’’ which is incorporated by substances used in accordance with reference. Copies are available from prior sanction, substances permitted the Center for Food Safety and Applied under applicable regulations in this Nutrition (HFS–200), Food and Drug part, and the following: Administration, 200 C St. SW., Wash- ington, DC 20204, or available for in- spection at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408.
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(d) Extractives limitations. The fol- incorporated by reference. Copies, are lowing extractives limitations are de- available from the Center for Food termined by an infrared spectrophoto- Safety and Applied Nutrition (HFS– metric method titled ‘‘Infrared 200), Food and Drug Administration, Spectrophotometric Determination of 200 C St. SW., Washington, DC 20204, or Polymer Extracted from Borex 210 available for inspection at the Office of Resin Pellets,’’ which is incorporated the Federal Register, 800 North Capitol by reference. Copies are available from Street, NW., suite 700, Washington, DC the Center for Food Safety and Applied 20408. Nutrition (HFS–200), Food and Drug (f) Acrylonitrile copolymers identi- Administration, 200 C St. SW., Wash- fied in this section shall comply with ington, DC 20204, or available for in- the provisions of § 180.22 of this chap- spection at the Office of the Federal ter. Register, 800 North Capitol Street, (g) Acrylonitrile copolymers identi- NW., suite 700, Washington, DC 20408, fied in this section are not authorized and are applicable to the modified co- to be used to fabricate beverage con- polymers in the form of particles of a tainers. size that will pass through a U.S. [42 FR 14572, Mar. 15, 1977, as amended at 42 Standard Sieve No. 6 and that will be FR 48544, Sept. 23, 1977; 47 FR 11841, Mar. 19, held on a U.S. Standard Sieve No. 10: 1982; 47 FR 16775, Apr. 20, 1982; 54 FR 24898, (1) The extracted copolymer shall not June 12, 1989] exceed 2.0 ppm in aqueous extract ob- tained when a 100-gram sample of co- § 177.1060 n-Alkylglutarimide/acrylic polymer is extracted with 250 milli- copolymers. liters of freshly distilled water at n-Alkylglutarimide/acrylic copoly- reflux temperature for 2 hours. mers identified in this section may be (2) The extracted copolymer shall not safely used as articles or components exceed 0.5 ppm in n-heptane when a 100- of articles intended for use in contact gram sample of the basic copol-ymer is with food subject to provisions of this extracted with 250 milliliters spectral section and part 174 of this chapter. grade n-heptane at reflux temperature (a) Identity. For the purpose of this for 2 hours. section, n-alkylglutarimide/acrylic co- (e) Accelerated extraction end test. The polymers are copolymers obtained by modified copolymer shall yield acrylo- reaction of substances permitted by nitrile monomer not in excess of 0.4 § 177.1010(a) (1), (2), and (3) with the fol- ppm when tested as follows: lowing substance: Monomethylamine (1) The modified copolymer shall be (CAS Reg. No. 74–89–5), to form n- in the form of eight strips 1⁄2 inch by 4 methylglutarimide/acrylic copolymers. inches by .03 inch. (b) Adjuvants. The copolymers identi- (2) The modified copolymer strips fied in paragraph (a) of this section shall be immersed in 225 milliliters of 3 may contain adjuvant substances re- percent acetic acid in a Pyrex glass quired in their production. The op- pressure bottle. tional adjuvant substances required in (3) The pyrex glass pressure bottle is the production of the basic polymer then sealed and heated to 150 °F in ei- may include substances permitted for ther a circulating air oven or a thermo- such use by applicable regulations, as stat controlled bath for a period of 8 set forth in part 174 of this chapter. days. (c) Specifications. Maximum nitrogen (4) The Pyrex glass pressure bottle is content of the copolymer determined then removed from the oven or bath by micro-Kjeldahl analysis, shall not and cooled to room temperature. A exceed 8 percent. sample of the extracting solvent is (d) Limitations. (1) The n-alkylglutar- then withdrawn and analyzed for acry- imide/acrylic copolymers in the fin- lonitrile monomer by a gas ished form in which they shall contact chromatographic method titled ‘‘Gas- food, when extracted with the solvent Solid Chromatographic Procedure for or solvents characterizing the type of Determining Acrylonitrile Monomer in food and under the conditions of time Acrylonitrile-Containing Polymers and and temperature described in tables 1 Food Simulating Solvents,’’ which is and 2 of § 176.170(c) of this chapter,
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shall yield extractives not to exceed (a) Cellophane consists of a base the limitations of § 177.1010(b) of this sheet made from regenerated cellulose chapter, when prepared as strips, as de- to which have been added certain op- scribed in § 177.1010(c)(2) of this chapter. tional substances of a grade of purity (2) The n-alkylglutarimide/acrylic co- suitable for use in food packaging as polymers shall not be used as polymer constituents of the base sheet or as modifiers in vinyl chloride homo- or coatings applied to impart desired copolymers. technological properties. (e) Conditions of use. The n- (b) Subject to any limitations pre- alkylglutarimide/acrylic copolymers scribed in this part, the optional sub- are used as articles or components of stances used in the base sheet and articles (other than articles composed coating may include: of vinyl chloride homo- or copolymers) (1) Substances generally recognized intended for use in contact with all as safe in food. foods except beverages containing (2) Substances for which prior ap- more than 8 percent alcohol under con- proval or sanctions permit their use in ditions of use D, E, F, and G as de- cellophane, under conditions specified scribed in table 2 of § 176.170(c) of this in such sanctions and substances listed chapter. in § 181.22 of this chapter. [54 FR 20382, May 11, 1989, as amended at 58 (3) Substances that by any regulation FR 17098, Apr. 1, 1993] promulgated under section 409 of the act may be safely used as components § 177.1200 Cellophane. of cellophane. Cellophane may be safely used for (4) Substances named in this section packaging food in accordance with the and further identified as required. following prescribed conditions: (c) List of substances:
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 (C12±C18) diethanolamide, coconut oil For use only as an adjuvant employed during the processing of fatty acid (C12±C18) diethanolamine soap, and cellulose pulp used in the manufacture of cellophane base diethanolamine mixture having total alkali (calculated as po- sheet. tassium hydroxide) of 16±18% and having an acid number of 25±35. Copal resin, heat processed ...... As basic resin. Damar resin. Defoaming agents identified in § 176.200 of this chapter.
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
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 (C8±C18) 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°±228 °F., as determined by ASTM method D127±60 (``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. 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.
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
α-Methylstyrene-vinyltoluene copolymer resins (molar ratio 1 α- methylstyrene to 3 vinyltoluene). Mineral oil, white. Naphthalenesulfonic acid-formaldehyde condensate, sodium 0.1 percent, for use only as an emulsifier. salt. Nitrocellulose, 10.9 percent±12.2 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 2,000±10,200; For use only as an adjuvant in vinylidene chloride copolymer bromine number range 210±320). coatings. Polycarbonate resins complying with § 177.1580. 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 °C±92 °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 1,900±9,000). 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.
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Limitations (residue and limits of addition expressed as percent List of substances by weight of finished packaging cellophane)
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). 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 ing, processing, preparing, treating, this section covered by a specific food packaging, transporting, or holding additive regulation must meet any food in accordance with the following specifications in that regulation. prescribed conditions: (e) Acrylonitrile copolymers identi- (a) Closures for food containers are fied in this section shall comply with manufactured from substances gen- the provisions of § 180.22 of this chap- erally recognized as safe for contact ter. with food; substances that are subject to the provisions of prior sanctions; [42 FR 14572, Mar. 15, 1977, as amended at 47 substances authorized by regulations FR 11842, Mar. 19, 1982] in parts 174, 175, 176, 177, 178 and § 179.45 of this chapter; and closure-sealing § 177.1210 Closures with sealing gas- gaskets, as further prescribed in this kets for food containers. section. Closures with sealing gaskets may be (b) Closure-sealing gaskets and over- safely used on containers intended for all discs are formulated from sub- use in producing, manufacturing, pack- stances identified in § 175.300(b) of this
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chapter, with the exception of para- (4) Substances identified in para- graph (b)(3) (v), (xxxi), and (xxxii) of graph (b)(5) of this section, used in that section, and from other optional amounts not to exceed those required substances, including the following: to accomplish the intended physical or (1) Substances generally recognized technical effect and in conformance as safe in food. with any limitation provided; and fur- (2) Substances used in accordance ther provided that any substance em- with the provisions of a prior sanction ployed in the production of closure- sealing gasket compositions that is the or approval within the meaning of sec- subject of a regulation in parts 174, 175, tion 201(s) of the act. 176, 177, 178 and § 179.45 of this chapter (3) Substances that are the subject of conforms with the identity or speci- regulations in parts 174, 175, 176, 177, 178 fications prescribed. and § 179.45 of this chapter and used in (5) Substances that may be employed accordance with the conditions pre- in the manufacture of closure-sealing scribed. gaskets include:
TABLE 1
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
Arachidy-l-behenyl amide (C20±C22fatty acid amides) ...... 5 percent. Azodicarbonamide ...... 1. 2 percent. 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 1646±81, ``Standard Test Method for RubberÐViscosity 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 (HFS±200), 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. 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.
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TABLE 1ÐContinued
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
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). 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. 68411±46±1) ... 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. 2750±3000. 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.
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TABLE 1ÐContinued
Limitations (expressed as percent by weight of closure-sealing List of substances gasket composition)
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. 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 2ÐMAXIMUM 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- form Chloro- tainer with a solvent or solvents char- form fraction form acterizing the type of foods, and under Type of closure-sealing gas- fraction of fraction ket composition of water heptane of alco- conditions of time and temperature extrac- extrac- hol ex- characterizing the conditions of its use tives tives tractives 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 cured natural and syn- not to exceed the tolerances specified 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 melt, solution, plastisol, which the closure is to be used. Employ 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 or annular rings of plasti- procedural details to make the method 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 or annular rings of vulcan- the closure’s food-contacting surface ized plasticized polymers, with the solvent. including natural or syn- thetic rubber ...... 50 50 50 TABLE 3ÐTYPES OF FOOD 4. Preformed overall discs or annular rings of poly- I. Nonacid (pH above 5.0), aqueous products; may contain meric or resinous-coated salt or sugar or both, and including oil-in-water emulsions paper, paperboard, plas- of low- or high-fat content. tic, or metal foil substrates 50 250 50 II. Acidic (pH 5.0 or below), aqueous products; may contain 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).
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TABLE 4ÐTEST 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 1 2 8 percent alcohol 2
A. High temperature heat-sterilized I, IV±B ...... 250 °F, 2 hr ...... (e.g., over 212 °F). III, IV±A, VII ...... do ...... 150 °F, 2 hr. B. Boiling water-sterilized ...... II ...... 212 °F, 30 min ...... III, VII ...... do ...... 120 °F, 30 min. C. Hot filled or pasteurized above 150 II, IV±B ...... Fill boiling, cool to ...... °F. III, IV±A ...... 100 °F. 120 °F, 15 min. V ...... do ...... do...... D. Hot filled or pasteurized below 150 II, IV±B, VI±B ...... 150 °F, 2 hr ...... °F. III, IV±A ...... do ...... 100 °F, 30 min. V ...... do ...... VI±A ...... 150 °F, 2 hr E. Temperature filled and stored (no II, IV±B, VI±B ...... 120 °F, 24 hr ...... thermal treatment in the container). III, IV±A ...... do ...... 70 °F, 30 min. V ...... do ...... VI±A ...... 120 °F, 24 hr. F. Refrigerated storage (no thermal I, II, III, IV±A, IV±B, 70 °F, 48 hr ...... 70 °F, 30 min ...... treatment). VI±B, VII...... 70 °F, 48 hr. VI±A ...... G. Frozen storage (no thermal treat- I, II, III, IV±B, 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]
§ 177.1240 1,4-Cyclohexylene (c) Any substance employed in the dimethylene terephthalate and 1,4- production of the copolymer that is the cyclohexylene dimethylene subject of a regulation in parts 174, 175, isophthalate copolymer. 176, 177, 178 and § 179.45 of this chapter Copolymer of 1,4-cyclohexylene conforms with any specification in dimethylene terephthalate and 1,4- such regulation. cyclohexylene dimethylene isophtha- (d) Substances employed in the pro- late may be safely used as an article or duction of the copolymer include: component of articles used in pro- (1) Substances generally recognized ducing, manufacturing, packing, proc- as safe in food. essing, preparing, treating, packaging, (2) Substances subject to prior sanc- transporting, or holding food, subject tion or approval for use in the copoly- to the provisions of this section: mer and used in accordance with such (a) The copolymer is a basic poly- sanction or approval. ester produced by the catalytic con- (3) Substances which by regulation in densation of dimethyl terephthalate parts 174, 175, 176, 177, 178 and § 179.45 of and dimethyl isophthalate with 1,4- this chapter may be safely used as cyclohexanedimethanol, to which may components of resinous or polymeric have been added certain optional sub- coatings and film used as food-contact stances required in its production or surfaces, subject to the provisions of added to impart desired physical and such regulation. technical properties. (e) The copolymer conforms with the (b) The quantity of any optional sub- following specifications: stance employed in the production of (1) The copolymer, when extracted the copolymer does not exceed the with distilled water at reflux tempera- amount reasonably required to accom- ture for 2 hours, yields total extrac- plish the intended physical or technical tives not to exceed 0.05 percent. effect or any limitation further pro- vided.
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(2) The copolymer, when extracted parts 174, 175, 176, 177, 178, and § 179.45 of with ethyl acetate at reflux tempera- this chapter, it shall also comply with ture for 2 hours, yields total extrac- any specifications and limitations pre- tives not to exceed 0.7 percent. scribed for it by that regulation. (3) The copolymer, when extracted (c) The finished food-contact layer with n-hexane at reflux temperature made with basic copolymers containing for 2 hours, yields total extractives not more than 10 weight-percent but no to exceed 0.05 percent. more than 25 weight-percent of total [42 FR 14572, Mar. 15, 1977; 49 FR 5748, Feb. 15, polymer units derived from acrylic 1984, as amended at 55 FR 34555, Aug. 23, 1990] acid and with a maximum thickness of 0.0025 inch (2.5 mils) may be used in § 177.1310 Ethylene-acrylic acid co- contact with food types I, II, IVB, VIA, polymers. VIB, VIIB, and VIII identified in table The ethylene-acrylic acid copolymers 1 of § 176.170(c) of the chapter under identified in paragraph (a) of this sec- conditions of use B through H as de- tion may be safely used as components scribed in table 2 of § 176.170(c) of this of articles intended for use in contact chapter, and in contact with food types with food subject to the provisions of III, IVA, V, VIIA, and IX identified in this section. table 1 of § 176.170(c) of this chapter (a) The ethylene-acrylic acid copoly- under conditions of use E through G as mers consist of basic copolymers pro- described in table 2 of § 176.170(c) of this duced by the copolymerization of chapter. ethylene and acrylic acid such that the (d) The provisions of this section are finished basic copolymers contain no not applicable to ethylene-acrylic acid more than: copolymers used in food-packaging ad- (1) 10 weight-percent of total polymer hesives complying with § 175.105 of this units derived from acrylic acid when chapter. used in accordance with paragraph (b) [42 FR 14572, Mar. 15, 1977, as amended at 51 of this section; and FR 19060, May 27, 1986; 53 FR 44009, Nov. 1, (2) 25 weight-percent of total polymer 1988] units derived from acrylic acid when used in accordance with paragraph (c) § 177.1312 Ethylene-carbon monoxide of this section. copolymers. (b) The finished food-contact articles The ethylene-carbon monoxide co- made with no more than 10 percent polymers identified in paragraph (a) of total polymer units derived from acryl- this section may be safely used as com- ic acid, when extracted with the sol- ponents of articles intended for use in vent or solvents characterizing the contact with food subject to the provi- type of food and under the conditions sions of this section. of its intended use as determined from (a) Identity. For the purposes of this tables 1 and 2 of § 176.170(c) of this chap- section, ethylene-carbon monoxide co- ter, yield net acidified chloroform-solu- polymers (CAS Reg. No. 25052–62–4) con- ble extractives not to exceed 0.5 milli- sist of the basic polymers produced by gram per square inch of food-contact the copolymerization of ethylene and surface when tested by the methods carbon monoxide such that the copoly- prescribed in § 177.1330(e)(1), (3)(i) mers contain not more than 30 weight- through (iv), (4), (5), and (6), except percent of polymer units derived from that carbon monoxide. (1) The total residue method using 3 (b) Conditions of use. (1) The polymers percent acetic acid, as prescribed in may be safely used as components of § 177.1330(e)(6)(i)(a), does not apply, and the food-contact or interior core layer (2) The net acidified chloroform-solu- of multilaminate food-contact articles. ble extractives from paper and paper- (2) The polymers may be safely used board complying with § 176.170 of this as food-contact materials at tempera- chapter may be corrected for wax, pet- tures not to exceed 121 °C (250 °F). rolatum, and mineral oil as provided in (c) Specifications. (1) Food-contact § 176.170(d)(5)(iii)(b) of this chapter. layers formed from the basic copoly- If the finished food-contact article is mer identified in paragraph (a) of this itself the subject of a regulation in section shall be limited to a thickness
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of not more than 0.01 centimeter (0.004 (4) The provisions of this section are inch). not applicable to ethylene-carbon mon- (2) The copolymers identified in para- oxide copolymers complying with graph (a) of this section shall have a § 175.105 of this chapter. melt index not greater than 500 as de- termined by ASTM method D1238–82, [57 FR 32422, July 22, 1992] condition E ‘‘Standard Test Method for § 177.1315 Ethylene-1, 4-cyclohexylene Flow Rates of Thermoplastics by Ex- dimethylene terephthalate copoly- trusion Plastometer,’’ which is incor- mers. porated by reference in accordance with 5 U.S.C. 552(a) and 1 CFR part 51. Ethylene-1, 4-cyclohexylene Copies may be obtained from the Amer- dimethylene terephthalate copolymer ican Society for Testing Materials, 1916 may be safely used as articles or com- Race St., Philadelphia, PA 19103, or ponents of articles intended for use in may be examined at the Center for contact with food subject to provisions Food Safety and Applied Nutrition of this section and of part 174 of this (HFS–200), Food and Drug Administra- chapter. tion, 200 C St. SW., Washington, DC, or (a) Identity. For the purposes of this at the Office of the Federal Register, section, ethylene-1,4-cyclohexylene 800 North Capitol St. NW., suite 700, dimethylene terephthalate copolymers Washington, DC. (1,4-benzene dicarboxylic acid, di- (3) The basic copolymer identified in methyl ester, polymerized with 1,4- paragraph (a) of this section, when ex- cyclohexanedimethanol and 1,2- tracted with the solvent or solvents ethanediol) (CAS Reg. No. 25640–14–6) or characterizing the type of food and (1,4-benzenedicarboxylic acid, polym- under the conditions of time and tem- erized with 1,4-cyclohexanedimethanol perature characterizing the conditions and 1,2-ethanediol) (CAS Reg. No. of its intended use, as determined from 25038–91–9) are basic copolymers meet- tables 1 and 2 of § 176.170(c) of this chap- ing the specifications prescribed in ter, yields net chloroform-soluble ex- paragraph (b) of this section, to which tractives in each extracting solvent may have been added certain optional not to exceed 0.5 milligram per square substances required in their production inch of food-contact surface when test- or added to impart desired physical or ed by methods described in § 176.170(d) technical properties. of this chapter. (b) Specifications:
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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)
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...... 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).
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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)
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 19103, or may be examined at the Office than 15 weight percent of polymer 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 resins may be safely used as articles or copolymer consists of the basic copoly- 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- (6) The copolymer of vinylidene fluo- scribed above shall not exceed 30 per- ride 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 (b) Ethylene-vinyl acetate copoly- identified as Type III, IV–A, V, VII–A, mers, with or without the optional sub- and IX in § 176.170(c), table 1, the co- stances described in paragraph (a) of polymer may be used under condition this section, when extracted with the of use C at temperatures not to exceed solvent or solvents characterizing the 160 °F (71 °C). type of food, and under conditions of [57 FR 43399, Sept. 21, 1992, as amended at 59 time and temperature characterizing FR 62318, Dec. 5, 1994; 61 FR 14481, Apr. 2, the conditions of their intended use as 1996; 62 FR 34628, June 27, 1997] determined from tables 1 and 2 of § 176.170(c) of this chapter, shall yield § 177.1350 Ethylene-vinyl acetate co- net chloroform-soluble extractives cor- polymers. rected for zinc as zinc oleate not to ex- Ethylene-vinyl acetate copolymers ceed 0.5 milligram per square inch of an may be safely used as articles or com- appropriate sample. ponents of articles intended for use in (c) The provisions of paragraph (b) of producing, manufacturing, packing, this section are not applicable to ethyl- processing, preparing, treating, pack- ene-vinyl acetate copolymers used in aging, transporting, or holding food in food-packaging adhesives complying accordance with the following pre- with § 175.105 of this chapter. scribed conditions: (d) Ethylene-vinyl acetate copoly- (a) Ethylene-vinyl acetate copoly- mers may be irradiated under the fol- mers consist of basic resins produced lowing conditions to produce molecular by the catalytic copolymerization of crosslinking of the polymers to impart ethylene and vinyl acetate to which desired properties such as increased may have been added certain optional strength and increased ability to substances to impart desired techno- shrink when exposed to heat: logical or physical properties to the (1) Electron beam source of ionizing resin. Subject to any limitations pre- radiation at a maximum energy of 3 scribed in this section, the optional million electron volts: Maximum ab- substances may include: (1) Substances generally recognized sorbed dose not to exceed 150 kiloGray as safe in food and food packaging. (15 megarads). (2) Substances the use of which is (2) The finished food-contact film permitted under applicable regulations shall meet the extractives limitations in parts 170 through 189 of this chapter, prescribed in paragraph (e)(2) of this prior sanction, or approvals. section. (3) Substances identified in (3) The ethylene-vinyl acetate co- § 175.300(b)(3) (xxv), (xxvii), (xxx), and polymer films may be further irradi- (xxxiii) of this chapter, and colorants ated in accordance with the provisions used in accordance with § 178.3297 of of paragraph (e)(1) of this section: Pro- this chapter. vided, That the total accumulated radi- (4) Erucamide as identified in ation dose from both electron beam § 178.3860 of this chapter. and gamma ray radiation does not ex- (5) Xanthan gum as identified in ceed 150 kiloGray (15 megarads). §172.695 for use as a thickening agent (e) Ethylene-vinyl acetate copolymer at a level not to exceed 1 percent by films intended for contact with food weight of coating solids in aqueous dis- may be irradiated to control the persions of ethylene-vinyl acetate co- growth of microorganisms under the polymers, where such copolymers are following conditions: used only as coatings or a component (1) Gamma photons emitted from a of coatings. cobalt–60 sealed source in the dose
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range of 5–50 kiloGray (0.5–5.0 Test Method for Liquid Extraction of megarads). Flexible Barrier Materials,’’ which is (2) The irradiated ethylene-vinyl ace- incorporated by reference. Copies may tate copolymer films, when extracted be obtained from the American Society with reagent grade n-heptane (freshly for Testing Materials, 1916 Race St., redistilled before use) according to Philadelphia, PA 19103, or may be ex- methods described under § 176.170(d)(3) amined at the Office of the Federal of this chapter, at 75 °F for 30 minutes Register, 800 North Capitol Street, shall yield total extractives not to ex- NW., suite 700, Washington, DC 20408. ceed 4.5 percent by weight of the film. (1) The film when extracted with dis- tilled water at 21 °C (70 °F) for 48 hours [42 FR 14572, Mar. 15, 1977, as amended at 43 FR 29287, July 7, 1978; 54 FR 35874, Aug. 30, yields total extractives not to exceed 1989; 55 FR 18595, May 3, 1990; 56 FR 42932, 0.0047 milligram per square centimeter Aug. 30, 1991] (0.03 milligram per square inch) of food-contact surface. § 177.1360 Ethylene-vinyl acetate-vinyl (2) The film when extracted with 50 alcohol copolymers. percent ethyl alcohol at 21 °C (70 °F) for Ethylene-vinyl acetate-vinyl alcohol 48 hours yields total extractives not to copolymers (CAS Reg. No. 26221–27–2) exceed 0.0062 milligram per square cen- may be safely used as articles or com- timeter (0.04 milligram per square ponents of articles intended for use in inch) of food-contact surface. contact with food, in accordance with (c) The finished food-contact article the following prescribed conditions: shall not exceed 0.0076 centimeter (0.003 (a) Ethylene-vinyl acetate-vinyl alco- inch) thickness and shall contact foods hol copolymers are produced by the only of the types identified in table 1 of partial or complete alcoholysis or hy- § 176.170(c) of this chapter in Categories drolysis of those ethylene-vinyl acetate III, IV–A, VII–A, and IX under condi- copolymers complying with § 177.1350. tions of use F and G described in table (1) Those copolymers containing a 2 of § 176.170(c) of this chapter. Film minimum of 55 percent ethylene and a samples of 0.0076 centimeter (0.003 inch) maximum of 30 percent vinyl alcohol thickness representing the finished ar- units by weight may be used in contact ticles shall meet the following extrac- with foods as described in paragraph (b) tive limitation when tested by ASTM of this section. method F34–76 (Reapproved 1980), (2) Those copolymers containing a ‘‘Standard Test Method for Liquid Ex- minimum of 55 percent ethylene and a traction of Flexible Barrier Materials,’’ maximum of 15 percent vinyl alcohol which is incorporated by reference. The units by weight may be used in contact availability of this incorporation by with foods as described in paragraph (c) reference is given in paragraph (b) of of this section. this section. The film when extracted (3) Those copolymers containing 20 to with n-heptane at 38 °C (100 °F) for 30 40 percent ethylene and 60 to 80 percent minutes yields total extractives not to vinyl alcohol units by weight may be exceed 0.0078 milligram per square cen- used in contact with foods as described timeter (0.05 milligram per square in paragraph (d) of this section. inch) of food-contact surface, after cor- (b) The finished food-contact article recting the total extractives by divid- shall not exceed 0.013 centimeter (0.005 ing by a factor of five. inch) thickness and shall contact foods (d) The finished food-contact article only of the types identified in table 1 of shall not exceed 0.018 centimeter (0.007 § 176.170(c) of this chapter in Categories inch) thickness and may contact all I, II, IV–B, VI, VII–B, and VIII under foods except those containing more conditions of use D through G de- than 8 percent alcohol under conditions scribed in table 2 of § 176.170(c) of this of use B through H described in table 2 chapter. Film samples of 0.013 centi- of § 176.170(c) of this chapter. Film sam- meter (0.005) inch thickness rep- ples of 0.018 centimeter (0.007 inch) resenting the finished article shall thickness representing the finished ar- meet the following extractive limita- ticles shall meet the following extrac- tion when tested by ASTM method tive limitation when tested by ASTM F34–76 (Reapproved 1980), ‘‘Standard method F34–76 (Reapproved 1980),
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‘‘Standard Test Method for Liquid Ex- St., Philadelphia, PA 19013, or may be traction of Flexible Barrier Materials,’’ examined at the Office of the Federal which is incorporated by reference. The Register, 800 North Capitol Street, availability of this incorporation by NW., suite 700, Washington, DC. reference is given in paragraph (b) of (b) Fluorocarbon resins that are iden- this section. The film when extracted tified in paragraph (a) of this section with distilled water at 100 °C (212 °F) and that comply with extractive limi- for 30 minutes yields total extractives tations prescribed in paragraph (c) of not to exceed 0.023 milligram per this section may be used as articles or square centimeter (0.15 milligram per components of articles intended for use square inch) of food-contact surface. in contact with food as follows: (e) The provisions of this section are (1) Fluorocarbon resins that are iden- not applicable to ethylene-vinyl ace- tified in paragraphs (a)(1), (a)(2), and tate-vinyl alcohol copolymers used in (a)(3) of this section and that comply the food-packaging adhesives com- only with the extractive limitations plying with § 175.105 of this chapter. prescribed in paragraphs (c)(1) and [47 FR 41531, Sept. 21, 1982, as amended at 49 (c)(2) of this section may be used when FR 10108, Mar. 19, 1984] such use is limited to articles or com- ponents of articles that are intended § 177.1380 Fluorocarbon resins. for repeated use in contact with food or Fluorocarbon resins may be safely that are intended for one-time use in used as articles or components of arti- contact with foods only of the types cles intended for use in contact with identified in § 176.170(c) of this chapter, food, in accordance with the following table 1, under Types I, II, VI, VII–B, prescribed conditions: and VIII. (a) For the purpose of this section, (2) Fluorocarbon resins that are iden- fluorocarbon resins consist of basic res- tified in paragraph (a)(4) of this section ins produced as follows: and that comply with the extractive (1) Chlorotrifluoroethylene resins limitations prescribed in paragraphs produced by the homopolymerization (c)(1) and (c)(2) of this section may be of chlorotrifluoroethylene. used only when such use is limited to (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.
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(3) A 100-gram sample of the resin with item 2.2 or 3.2 of the table in pellets, when extracted with 100 milli- § 177.1520(c) blended with no more than liters of n-heptane at reflux tempera- 10 percent by weight of a copolymer of ture for 8 hours, shall yield total ex- ethylene and vinyl acetate complying tractives not to exceed 0.01 percent by with § 177.1350. weight of the resins. (c) Polymeric resin blends formulated [42 FR 14572, Mar. 15, 1977, as amended at 57 from a base polymer complying with FR 185, Jan. 3, 1992] item 2.2 or 3.2 of the table in § 177.1520(c) blended with no more than § 177.1390 Laminate structures for use 38 percent by weight of a homopolymer at temperatures of 250 ≥F and of isobutylene complying with above. § 177.1420(a)(1). (a) The high-temperature laminates (d) Polyethylene phthalate resins identified in this section may be safely complying with § 177.1630(e)(4) (i) and used for food contact at temperatures (ii). not exceeding 135 °C (275 °F) unless oth- (e) Nylon MXD–6 resins that comply erwise specified. These articles are lay- with item 10.3 of the table in ered constructions that are optionally § 177.1500(b) of this chapter when ex- bonded with adhesives. The interior tracted with water and heptane under (food-contact) layer(s) may be sepa- the conditions of time and temperature rated from the exterior layer(s) by a specified for condition of use A, as set functional barrier, such as aluminum forth in Table 2 of § 176.170(c) of this foil. Upon review of the physical prop- chapter. erties of a particular construction, the (f) Polymeric resins that comply with Food and Drug Administration may an applicable regulation in this chapter consider other layers to serve as func- which permits food type and time/tem- tional barriers. This regulation is not perature conditions to which the con- intended to limit these constructions tainer will be exposed, including steri- as to shape, degree of flexibility, thick- lization processing. ness, or number of layers. These layers (ii) Adjuvants used in these layers may be laminated, extruded, co- must comply with an applicable regu- extruded, or fused. lation that permits food type and time/ (b) When containers subject to this temperature conditions to which the regulation undergo heat sterilization container will be exposed, including to produce shelf-stable foods, certain sterilization processing. control measures (in addition to the (2) Adhesives. The use of adhesives in food additive requirements in para- these containers is optional. Adhesives graphs (c) and (d) of this section) are may be formulated from the following necessary to ensure proper food steri- substances, subject to the prescribed lization and package integrity. Refer limitations: to parts 108, 110, 113, and 114 of this (i) Any substance suitable for use in chapter for details. formulating adhesives that complies (c) Subject to the provisions of this with an applicable regulation of this paragraph, food-contact articles pro- chapter which permits food type and duced from high-temperature lami- time/temperature conditions to which nates may be safely used to package all the container will be exposed, includ- food types except those containing ing sterilization processing. more than 8 percent ethyl alcohol. (ii) Substances complying with (1) Polymeric films/layers. Films or lay- § 175.105 of this chapter may be used in ers not separated from food by a func- these constructions, provided they are tional barrier must meet the following separated from the interior (food-con- requirements: tact) layer(s) by a functional barrier as (i) Films/layers may consist of the discussed under paragraph (a) of this following: section. (a) Polyolefin resins complying with (iii) Maleic anhydride adduct of poly- item 2.2 or 3.2 of the table in propylene complying with § 175.300 of § 177.1520(c). this chapter. (b) Polymeric resin blends formu- (iv) Polyester-urethane adhesive for lated from a base polymer complying use at temperatures not exceeding 121
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°C (250 °F) and formulated from the fol- (3) Epoxy resin listed in lowing: § 175.300(b)(3)(viii)(a) of this chapter and (a) Polyester-urethanediol resin pre- comprising not more than 5 percent by pared by the reaction of a mixture of weight of the cured adhesive. polybasic acids and polyhydric alcohols (4) Optional trimethoxy silane curing listed in § 175.300(b)(3)(vii) of this chap- agents, containing amino, epoxy, ether, ter, 3-isocyanatomethyl-3,5,5- or mercapto groups not in excess of 3 trimethylcyclohexyl isocyanate (CAS percent of the cured adhesive. Reg. No. 4098–71–9) and optional (b) Urethane cross-linking agent, trimethoxysilane coupling agents con- comprising not more than 20 percent taining amino, epoxy, ether, and/or by weight of the cured adhesive, and mercapto groups not to exceed 3 per- cent by weight of the cured adhesive. formulated from trimethylol propane (b) Urethane cross-linking agent (CAS Reg. No. 77–99–6) adducts of 3– comprising not more than 25 percent isocyanatomethyl–3,5,5– by weight of the cured adhesive and trimethylcyclohexyl isocyanate (CAS formulated from 3-isocyanatomethyl- Reg. No. 4098–71–9) or 1,3- 3,5,5-trimethylcyclohexyl isocyanate bis(isocyanatomethyl)benzene (CAS (CAS Reg. No. 4098–71–9) adduct of Reg. No. 25854–16–4). trimethylol propane (Cas Reg. No. 77– (vii) Polyester-polyurethane resin- 99–6) and/or 1,3-bis(isocyanatomethyl) acid dianhydride adhesives for use at benzene (CAS Reg. No. 25854–16–4) temperatures not to exceed 121 °C (250 adduct of trimethylol propane. °F), in contact only with food Types I, (v) Polyester-epoxy-urethane adhe- II, VIA, VIB, VIIB, and VIII as de- sives formulated from the following: scribed in Table I of § 176.170 of this (a) Polyester resin formed by the re- chapter, and formulated from the fol- action of polybasic acids and lowing mixture: polyhydric alcohols listed in (a)(1) Polyesterpolyurethanediol res- § 175.300(b)(3)(vii) of this chapter. Aze- ins prepared by the reaction of a mix- laic acid may also be used as a ture of polybasic acids and polyhydric polybasic acid. alcohols listed in § 175.300(b)(3)(vii) of (b) Epoxy resin listed in this chapter and 3-isocyanatomethyl- § 175.300(b)(3)(viii)(a) of this chapter and 3,5,5-trimethylcyclohexyl isocyanate comprising no more than 30 percent by weight of the cured adhesive. (CAS Reg. No. 4098–71–9). Additionally, (c) Urethane cross-linking agent com- dimethylol propionic acid and 1,6- prising no more than 14 percent weight hexanediol may be used alone or in of the cured adhesive and formulated combination as reactants in lieu of a from 3-isocyanatomethyl-3,5.5- polybasic acid and a polyhydric alco- trimethylcyclohexyl isocyanate hol. cyanurate (CAS Reg. No. 53880–05–0). (2) Acid dianhydride formulated from (vi) Polyurethane-polyester resin- 3a,4,5,7a-tetrahydro-7-methyl-5- epoxy adhesives formulated from the (tetrahydro-2,5-dioxo-3-furanyl)-1,3- following mixture: isobenzofurandione (CAS Reg. No. (a)(1) Polyester-polyurethanediol res- 73003–90–4), comprising not more than ins prepared by the reaction of a mix- one percent of the cured adhesive. ture of polybasic acids and polyhydric (b) Urethane cross-linking agent, alcohols listed in § 175.300(b)(3)(vii) of comprising not more than twelve per- this chapter and 3-isocyanatomethyl- cent by weight of the cured adhesive, 3,5,5-trimethylcyclohexyl isocyanate and formulated from trimethylol pro- (CAS Reg. No. 4098–71–9). pane (CAS Reg. No. 77–99–6) adducts of (2) Polyester resin formed by the re- 3-isocyanatomethyl-3,5,5- action of polybasic acids and trimethylcyclohexyl isocyanate (CAS polyhydric alcohols listed in Reg. No. 4098–71–9) and/or 1,3- § 175.300(b)(3)(vii) of this chapter. Addi- tionally, azelaic acid and 1,6- bis(isocyanatomethyl)benzene (CAS hexanediol may also be used as Reg. No. 363–48–31). reactants in lieu of a polyhydric alco- (3) Test specifications. These specifica- hol. tions apply only to materials on the
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food-contact side of a functional bar- 0.0020 milligram per square centimeter rier, if present. All tests must be per- (0.013 milligram per square inch) as de- formed on containers made under pro- termined by a method titled ‘‘Deter- duction conditions. Laminated struc- mination of Non-volatile Chloroform tures submitted to extraction proce- Soluble Residues in Retort Pouch dures must maintain complete struc- Water Extracts,’’ which is incorporated tural integrity (particularly with re- by reference. The availability of this gard to delamination) throughout the incorporation by reference is given in test. paragraph (c)(3)(i)(a)(1) of this section. (i) ) For use Nonvolatile extractives. (a (2) The chloroform-soluble fraction of at temperatures not to exceed 121 °C the total nonvolatile extractives for (250 °F): The container interior (food- containers using adhesives listed in contact side) shall be extracted with deionized distilled water at 121 °C (250 paragraph (c)(2)(v) of this section shall °F) for 2 hours. not exceed 0.016 milligram per square (1) The chloroform-soluble fraction of centimeter (0.10 milligram per square the total nonvolatile extractives for inch) as determined by a method titled containers using adhesives listed in ‘‘Determination of Non-volatile Chlo- paragraphs (c)(2)(i), (c)(2)(ii), (c)(2)(iii), roform Soluble Residues in Retort (c)(2)(iv), and (c)(2)(vii) of this section Pouch Water Extracts,’’ which is incor- shall not exceed 0.0016 milligram per porated by reference. The availability square centimeter (0.01 milligram per of this incorporation by reference is square inch) as determined by a meth- given in paragraph (c)(3)(i)(a)(1) of this od entitled ‘‘Determination of Non- section. Volatile Chloroform Soluble Residues (3) The chloroform-soluble fraction of in Retort Pouch Water Extracts,’’ the total nonvolatile extractives for which is incorporated by reference. containers using adhesives listed in Copies are available from the Center paragraph (c)(2)(vi) of this section shall for Food Safety and Applied Nutrition not exceed 0.008 milligram per square (HFS–200), Food and Drug Administra- centimeter (0.05 milligram per square tion, 200 C St. SW., Washington, DC inch) as determined by a method enti- 20204, and may be examined at the Cen- tled, ‘‘Determination of Non-volatile ter for Food Safety and Applied Nutri- Chloroform Soluble Residues in Retort tion’s Library, 200 C St. SW., rm. 3321, Pouch Water Extracts,’’ which is incor- Washington, DC, or at the Office of the porated by reference in paragraph Federal Register, 800 North Capitol St. NW., suite 700, Washington, DC 20408. (c)(3)(i)(a)(1) of this section. (2) The chloroform-soluble fraction of (ii) Volatiles. Volatile substances em- the total nonvolatile extractives for ployed in the manufacture of high-tem- containers using adhesives listed in perature laminates must be removed to paragraph (c)(2)(v) of this section shall the greatest extent possible in keeping not exceed 0.016 milligram per square with good manufacturing practice pre- centimeter (0.10 milligram per square scribed in § 174.5(a) of this chapter. inch) as determined by a method titled (d) Nylon 12/aluminum foil high-tem- ‘‘Determination of Non-volatile Chlo- perature laminates: Subject to the pro- roform Soluble Residues in Retort visions of this paragraph, containers Pouch Water Extracts,’’ which is incor- constructed of nylon 12 laminated to porated by reference in paragraph aluminum foil may be safely used at (c)(3)(i)(a)(1) of this section. temperatures no greater than 250 °F (b) For use at temperatures not to ex- (121 °C) in contact with all food types ceed 135 °C (275 °F): The container inte- except those containing more than 8 rior (food-contact side) shall be ex- percent alcohol. tracted with deionized distilled water (1) The container is constructed of at 135 °C (275 °F) for 1 hour. aluminum foil to which nylon 12 film is (1) The chloroform-soluble fraction of fused. Prior to fusing the nylon 12, the the total nonvolatile extractives for containers using no adhesive, or adhe- aluminum foil may be optionally sives listed in paragraphs (c)(2) (i), (ii), precoated with a coating complying and (iii) of this section shall not exceed with § 175.300 of this chapter.
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(2) Nylon 12 resin complying with (4) The following substances in non- § 177.1500 and having an average thick- food-contact layers only: ness not to exceed 0.0016 inch (41 mi- crons) may be used as the food-contact Substances Limitations surface of the container. Ethylene/1,3±phenylene oxy- For use only with poly- (3) Container test specifications. On ethylene isophthalate/ ethylene terephthalate as exposure to distilled water at 250 °F terephthalate copolymer the food-contact layer, ° (CAS Reg. No. 87365±98±8) complying with (121 C) for 2 hours, extractives from complying with § 177.1345. § 177.1630 under condi- the food-contact side of the nylon 12 tions of use C through G multilayered construction shall not ex- described in table 2 of ceed 0.05 milligram per square inch § 176.170(c) of this chap- ter. Laminate structures, (0.0078 milligram per square centi- when extracted with 8 meter) as total nonvolatile extractives. percent ethanol at 150 °F for 2 hours shall not yield [45 FR 2843, Jan. 15, 1980, as amended at 47 m-pheny lenedioxy-O,O′- FR 49639, Nov. 2, 1982; 48 FR 236, Jan. 4, 1983; diethyl isophthalate or cy- 48 FR 15242, Apr. 8, 1983; 48 FR 17347, Apr. 22, clic bis(ethylene 1983; 49 FR 7558, Mar. 1, 1984; 52 FR 33575, isophthalate) in excess of 7.8 micrograms/square Sept. 4, 1987; 53 FR 39084, Oct. 5, 1988; 54 FR decimeter (0.5 24898, June 12, 1989; 61 FR 14481, Apr. 2, 1996; microgram/square inch) of 63 FR 55943, Oct. 20, 1998; 64 FR 4785, Feb. 1, food-contact surface. 1999] Nylon 6/12 resins complying For use with nonalcoholic with § 177.1500(b), item foods at temperatures not 13.2, of this chapter (CAS to exceed 100 °C (212 § 177.1395 Laminate structures for use ° at temperatures between 120 F and Reg. No. 25191±04±2). F). Laminate structures ≥ with authorized food-con- 250 ≥F. tact materials yield no (a) The laminates identified in this more than 0.15 milligram of epsilon-caprolactam section may be safely used at the speci- and 0.04 milligram of fied temperatures. These articles are omega-laurolactam per layered structures that are optionally square inch when ex- tracted with water at 100 bonded with adhesives. In these arti- °C (212 °F) for 5 hours. 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- 24993±04±2).. ceed 82.2 cC (180 cF). ers. The layers may be laminated, ex- Laminate structures with truded, coextruded, or fused. authorized food-contact (b) Laminate structures may be man- materials yield no more than 0.15 milligram of ep- ufactured from: 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 (2) Any polymeric resin listed in cC (180 cF) for 5 hours. 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). with the conditions of use (food type Laminate films with au- thorized food-contact ma- and time/temperature) specified in the terials yield no more than regulation for that resin. 0.15 milligram of epsilon- (3) Optional adjuvant substances used caprolactam per square inch when extracted with in accordance with § 174.5 of this chap- water at 100 cC (212 cF) ter. for 5 hours.
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Substances Limitations (c) Any substance employed in the production of the water-insoluble hy- Nylon 6/69 resins complying For use with nonalcoholic with § 177.1500(b), item 14, foods under conditions of droxyethyl cellulose film described in of this chapter (CAS Reg. use B, C, D, E, F, G, and this section that is the subject of a reg- No. 51995±62±1). H described in table 2 of ulation in parts 174, 175, 176, 177, 178 § 176.170 of this chapter. and § 179.45 of this chapter conforms Laminate structures with authorized food-contact with any specification in such regula- materials may contain tion. nylon 6/69 resins pro- vided that the nitrogen § 177.1420 Isobutylene polymers. content of aqueous ex- tracts of a representative Isobutylene polymers may be safely laminate (obtained at 100 used as components of articles in- °C (212 °F) for 8 hours) does not exceed 15 tended for use in producing, manufac- micrograms per square turing, packing, processing, preparing, centimeter (100 treating, packaging, transporting, or micrograms per square holding food, in accordance with the inch). following prescribed conditions: (a) For the purpose of this section, [52 FR 33575, Sept. 4, 1987, as amended at 53 isobutylene polymers are those pro- FR 19772, May 31, 1988; 57 FR 43399, Sept. 21, 1992; 58 FR 32610, June 11, 1993; 62 FR 53957, duced as follows: Oct. 17, 1997] (1) Polyisobutylene produced by the homopolymerization of isobutylene § 177.1400 Hydroxyethyl cellulose film, such that the finished polymers have a water-insoluble. molecular weight of 750,000 (Flory) or Water-insoluble hydroxyethyl cel- higher. lulose film may be safely used for (2) Isobutylene-isoprene copolymers packaging food in accordance with the produced by the copolymerization of following prescribed conditions: isobutylene with not more than 3 (a) Water-insoluble hydroxyethyl cel- molar percent of isoprene such that the lulose film consists of a base sheet finished polymers have a molecular manufactured by the ethoxylation of weight of 300,000 (Flory) or higher. cellulose under controlled conditions, (3) Chlorinated isobutylene-isoprene to which may be added certain optional copolymers produced when substances of a grade of purity suitable isobutylene-isoprene copolymers (mo- for use in food packaging as constitu- lecular weight 300,000 (Flory) or higher) ents of the base sheet or as coatings are modified by chlorination with not applied to impart desired technological more than 1.3 weight-percent of chlo- properties. rine. (b) Subject to any limitations pre- (b) The polymers identified in para- scribed in parts 170 through 189 of this graph (a) of this section may contain chapter, the optional substances used optional adjuvant substances required in the base sheet and coating may in- in the production of the polymers. The clude: optional adjuvant substances required (1) Substances generally recognized in the production of the polymers may as safe in food. include substances generally recog- (2) Substances permitted to be used nized as safe in food, substances used in in water-insoluble hydroxyethyl cel- accordance with a prior sanction or ap- lulose film by prior sanction or ap- proval, and aluminum chloride. proval and under conditions specified (c) The provisions of this section are in such sanctions or approval, and sub- not applicable to polyisobutylene used stances listed in part 181, subpart B of in food-packaging adhesives complying this chapter. with § 175.105 of this chapter. (3) Substances that by any regulation promulgated under section 409 of the § 177.1430 Isobutylene-butene copoly- act may be safely used as components mers. of water-insoluble hydroxyethyl cel- Isobutylene-butene copolymers iden- lulose film. tified in paragraph (a) of this section (4) Substances identified in and used may be safely used as components of in compliance with § 177.1200(c). articles intended for use in contact
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with food, subject to the provisions of less than 45 weight percent of polymer this section. units derived from isobutylene and (a) For the purpose of this section, meet the specifications prescribed in isobutylene-butene copolymers consist paragraph (b) of this section when test- of basic copolymers produced by the ed by the methods described in para- copolymerization of isobutylene with graph (c) of this section. mixtures of n-butenes such that the (b) Specifications: finished basic copolymers contain not
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. 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- corporation by reference is given in mining whether isobutylene-butene co- paragraph (c)(1) of this section. polymers conform to the specifications (d) The provisions of this section are in paragraph (b) are as follows: not applicable to isobutylene-butene (1) Molecular weight. Molecular copolymers used as provided under weight shall be determined by Amer- § 175.105 of this chapter. ican Society for Testing and Materials [52 FR 11641, Apr. 10, 1987, as amended at 63 (ASTM) method D2503–82, ‘‘Standard FR 36175, July 2, 1998] Test Method for Molecular Weight (Relative Molecular Mass) of Hydro- § 177.1440 4,4′-Isopropylidenediphenol- carbons by Thermoelectric Measure- epichlorohydrin resins minimum molecular weight 10,000. ment of Vapor Pressure,’’ which is in- corporated by reference. Copies may be 4,4′-Isopropylidenediphenol-epichlo- obtained from the American Society rohydrin resins having a minimum mo- for Testing Materials, 1916 Race St., lecular weight of 10,000 may be safely Philadelphia, PA 19103, or may be ex- used as articles or components of arti- amined at the Office of the Federal cles intended for use in producing, manufacturing, packing, processing, Register, 800 North Capitol Street, preparing, treating, packaging, trans- NW., suite 700, Washington, DC 20408. porting, or holding food in accordance (2) Viscosity. Viscosity shall be deter- with the following prescribed condi- mined by ASTM method D445–74, ‘‘Test tions: for Kinematic Viscosity of Transparent (a) 4,4′-Isopropylidenediphenol-ep- and Opaque Liquids,’’ which is incor- ichlorohydrin resins consist of basic porated by reference. The availability resins produced by the condensation of of this incorporation by reference is equimolar amounts of 4,4′- given in paragraph (c)(1) of this sec- isopropylidenediphenol and tion. epichlorohydrin terminated with phe- (3) Maximum bromine value. Maximum nol, to which may have been added cer- bromine value shall be determined by tain optional adjuvant substances re- ASTM method D1492–78, ‘‘Standard quired in the production of the resins. Test Method for Bromine Index of Aro- (b) The optional adjuvant substances matic Hydrocarbons by Coulometric required in the production of the resins Titration,’’ which is incorporated by may include substances generally rec- reference. The availability of this in- ognized as safe in food, substances used
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in accordance with a prior sanction or List of substances Limitations approval, and the following: Colorants used in accord- ance with § 178.3297 List of substances Limitations of this chapter. Butyl alcohol ...... Not to exceed 300 p.p.m. as re- Dioctyl phthalate ...... For use as lubricant. sidual solvent in finished resin. Hexamethylenetetramine For use only as polymerization Ethyl alcohol. reaction control agent. Toluene ...... Not to exceed 1,000 p.p.m. as re- Phthalic acid anhydride .. Do. sidual solvent in finished resin. Zinc stearate ...... For use as lubricant.
(c) 4,4′-Isopropylidenediphenol-ep- (c) The molded melamine-formalde- ichlorohydrin resins shall meet the fol- hyde articles in the finished form in lowing nonvolatile extractives limita- which they are to contact food, when tions: extracted with the solvent or solvents characterizing the type of food and (1) Maximum extractable nonvolatile under the conditions of time and tem- fraction of 2 parts per million when ex- perature as determined from tables 1 ° tracted with distilled water at 70 C for and 2 of § 175.300(d) of this chapter, 2 hours, using a volume-to-surface shall yield net chloroform-soluble ex- ratio of 2 milliliters per square inch. tractives not to exceed 0.5 milligram (2) Maximum extractable nonvolatile per square inch of food-contact surface. fraction of 3 parts per million when ex- tracted with n-heptane at 70 °C for 2 [42 FR 14572, Mar. 15, 1977, as amended at 56 FR 42933, Aug. 30, 1991] hours, using a volume-to-surface ratio of 2 milliliters per square inch. § 177.1480 Nitrile rubber modified ac- (3) Maximum extractable nonvolatile rylonitrile-methyl acrylate copoly- fraction of 6 parts per million when ex- mers. tracted with 10 percent (by volume) Nitrile rubber modified acrylonitrile- ethyl alcohol in distilled water at 70 °C methyl acrylate copolymers identified for 2 hours, using a volume-to-surface in this section may be safely used as ratio of 2 milliliters per square inch. components of articles intended for (d) The provisions of this section are food-contact use under conditions of not applicable to 4,4′-isopropylidene- use D, E, F, or G described in table 2 of diphenol-epichlorohydrin resins listed § 176.170(c) of this chapter, subject to in other sections of subchapter B of the provisions of this section. this chapter. (a) For the purpose of this section, nitrile rubber modified acrylonitrile- § 177.1460 Melamine-formaldehyde res- methyl acrylate copolymers consist of ins in molded articles. basic copolymers produced by the graft Melamine-formaldehyde resins may copolymerization of 73–77 parts by be safely used as the food-contact sur- weight of acrylonitrile and 23–27 parts face of molded articles intended for use by weight of methyl acrylate in the in producing, manufacturing, packing, presence of 8–10 parts by weight of bu- 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
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Vinyl Chloride Polymers,’’ which is in- to be used to fabricate beverage con- corporated by reference. Copies may be tainers. obtained from the American Society [42 FR 14572, Mar. 15, 1977, as amended at 42 for Testing Materials, 1916 Race St., FR 48544, Sept. 23, 1977; 47 FR 11843, Mar. 19, Philadelphia, PA 19103, or may be ex- 1982; 47 FR 16775, Apr. 20, 1982; 49 FR 10109, amined at the Office of the Federal Mar. 19, 1984; 54 FR 24898, June 12, 1989; 61 FR Register, 800 North Capitol Street, 14481, Apr. 2, 1996] NW., suite 700, Washington, DC 20408. § 177.1500 Nylon resins. (iii) Residual acrylonitrile monomer content is not more than 11 parts per The nylon resins listed in paragraph million as determined by gas chroma- (a) of this section may be safely used to tography. produce articles intended for use in (iv) Acetonitrile-soluble fraction processing, handling, and packaging food, subject to the provisions of this after refluxing the base polymer in ace- section: tonitrile for 1 hour is not greater than (a) The nylon resins are manufac- 95 percent by weight of the basic co- tured as described in this paragraph so polymers. as to meet the specifications prescribed (2) Extractives limitations. The fol- in paragraph (b) of this section when lowing extractive limitations are de- tested by the methods described in termined by an infrared paragraph (c) of this section. spectrophotometric method titled, ‘‘In- (1) Nylon 66 resins are manufactured frared Spectrophotometric Determina- by the condensation of hexamethylene- tion of Polymer Extracted from Borex diamine and adipic acid. 210 Resin Pellets,’’ which is incor- (2) Nylon 610 resins are manufactured porated by reference. Copies are avail- by the condensation of hexamethylene- able from the Center for Food Safety diamine and sebacic acid. and Applied Nutrition (HFS–200), Food (3) Nylon 66/610 resins are manufac- and Drug Administration, 200 C St. tured by the condensation of equal- SW., Washington, DC 20204, or available weight mixtures of nylon 66 salts and for inspection at the Office of the Fed- nylon 610 salts. eral Register, 800 North Capitol Street, (4) Nylon 6/66 resins manufactured by NW., suite 700, Washington, DC 20408, the condensation and polymerization of and are applicable to the basic copoly- Nylon 66 salts and epsilon-caprolactam. mers in the form of particles of a size (5) Nylon 11 resins are manufactured that will pass through a U.S. standard by the condensation of 11- sieve No. 6 and that will be held on a aminoundecanoic acid. U.S. standard sieve No. 10: (6) Nylon 6 resins are manufactured (i) Extracted copolymer not to ex- by the polymerization of epsilon- ceed 2.0 parts per million in aqueous caprolactam. extract obtained when a 100-gram sam- (7) Nylon 66T resins are manufac- ple of the basic copolymers is extracted tured by the condensation of hexamethyl-enediamine, adipic acid, with 250 milliliters of demineralized and terephthalic acid such that com- (deionized) water at reflux temperature position in terms of ingredients is for 2 hours. 43.1±0.2 weight percent hexamethyl- (ii) Extracted copolymer not to ex- enediamine, 35.3±1.2 weight percent ceed 0.5 part per million in n-heptane adipic acid, and 21.6±1.2 weight percent extract obtained when a 100-gram sam- terephthalic acid. ple of the basic copolymers is extracted (8) Nylon 612 resins are manufactured with 250 milliliters of reagent grade n- by the condensation of heptane at reflux temperature for 2 hexamethylenediamine and hours. dodecanedioic acid. (c) Acrylonitrile copolymers identi- (9) Nylon 12 resins are manufactured fied in this section shall comply with by the condensation of omega- the provisions of § 180.22 of this chap- laurolactam. ter. (10)(i) Impact modified Nylon MXD–6 (d) Acrylonitrile copolymers identi- resins (CAS Reg. No. 59655–05–9) manu- fied in this section are not authorized factured by the condensation of adipic
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acid, 1,3-benzenedimethanamine, and (13)(i) Nylon 6/12 resins (CAS Reg. No. T3alpha-(3-aminopropyl)-omega-(3- 25191–04–2) are manufactured by the co- amino-propoxy)poly- oxyethylene polymerization of a 1 to 1 ratio by under such conditions that the alpha- weight of epsilon-caprolactam and (3-amino-propyl)-omega-(3- omega-laurolactam. aminopropoxy) polyoxyethylene mon- (ii) Nylon 6/12 resins (CAS Reg. No. omer content does not exceed 7 percent 25191–04–2) are manufactured by the co- by weight of the finished resin. polymerization of a ratio of at least 80 (ii) Nylon MXD–6 resins (CAS Reg. weight percent of epsilon-caprolactam No. 25718–70–1) manufactured by the and no more than 20 weight percent of condensation of adipic acid and 1,3- benzenedimethanamine. omega-laurolactam. (11) Nylon 12T resins are manufac- (14) Nylon 6/69 resins (CAS Reg. No. tured by the condensation of omega- 51995–62–1) are manufactured by the laurolactam (CAS Reg. No. 0947–04–6), condensation of 49.5+0.5 weight percent isophthalic acid (CAS Reg. No. 0121–91– epsilon-caprolactam, 19.4+0.2 weight 5), and bis(4-amino-3-methylcycl- percent hexamethylenediamine and ohexyl)methane (CAS Reg. No. 6864–37– 31.2+0.3 weight percent azelaic acid. 5) such that the composition in terms (15) Nylon 46 resins (CAS Reg. No. of ingredients is 34.4±1.5 weight percent 50327–77–0) are manufactured by the omega-laurolactam, 26.8±0.4 weight per- condensation of 1,4-butanediamine and cent isophthalic acid, and 38.8±0.5 adipic acid. weight percent bis(4-amino-3- (16) Nylon resins PA 6–3–T (CAS Reg- methylcyclohexyl)-methane. istry No. 26246–77–5) are manufactured (12) Nylon 6I/6T resins (CAS Reg. No. by the condensation of 50 mol percent 25750–23–6) are manufactured by the 1,4-benzenedicarboxylic acid, dimethyl condensation of hexamethylenediamine, terephthalic ester and 50 mol percent of an acid, and isophthalic acid such that 65 equimolar mixture of 2,2,4-trimethyl- to 80 percent of the polymer units are 1,6-hexanediamine and 2,4,4-trimethyl- derived from hexamethylene 1,6-hexanediamine. isophthalamide. (b) Specifications:
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N ...... HC1 after 1 h h. after 1 h h. after 1 h h. Solubility in boiling 4.2 ...... do ...... do Insoluble Dissolves in 1 Insoluble Dissolves in 1 Insoluble ...... do Dissolves in 1 ...... do ...... do ...... do 482±518 475±495 405±425 355±375 392±446 392±446 406±420 375±395 355±375 335±355 440±460 380±425 enheit) Melting point (de- grees Fahr- .015 .015 .015 .015 .015 .015 .015 .015 .015 .015 .015 .015 ± ± ± ± ± ± ± ± ± ± ± ± 1.15 1.06 1.10 1.04 1.04 1.01 1.13 1.14 1.16 1.14 1.09 1.15 Specific gravity ......
epsi- . . . F), and B through ° ...... caprolactam monomer . F. ° ......
epsilon- 175.300 of this chapter Nylon resins ...... 176.170(c) of this chapter, except ...... 177.1390(d). . . caprolactam monomer content not to exceed Nylon 6/66 resins, Nylon 6/66 resins with combined caprolactam with food time use in contact with food and which are compliance with § 177.1395 of this chapter (CAS Reg. No. 24993± H of table 2 § content greater than 60 percent and residual time use or repeated in contact with food a. In articles intended for repeated use in contact b. In side-seam cements for articles intended 1- having an average thickness not to exceed 0.001 in having an average thickness not to exceed 0.001 in for repeated use in contact with food at tempera- tures not to exceed 212 not to exceed 0.0016 inch intended for use in con- tact with nonalcoholic food under the conditions of use A (sterilization not to exceed 30 minutes at a temperature not to exceed 250 as provided in § 0.4 percent by weight. For use only as specified in § 04±2) content not to exceed 0.7 percent by weight lon- 1. Nylon 66 resins 2. Nylon 610 resins 3.1 Nylon 66/610 resins 4.1 4.2 5.1 Nylon 11 resins for use in articles intended 1- 5.2 Nylon 11 resins for use only: 6.1 Nylon 6 resins 6.2 Nylon 6 resins for use only in food-contact films 7. Nylon 66T resins for use only in food-contact films 8. Nylon 612 resins for use only in articles intended 9. Nylon 12 resins for use only: a. In food-contact films having an average thickness
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° m . . . 176.170(c) of this chapter . 176.170(c) of this chapter, shall . 176.170(C) of this chapter F) (conditions of use E, F, and G in table 2 ° 176.170(c) of this chapter, except those con- 176.170(c) of this chapter. 176.170(c) of this chapter) 177.1520(c), item 1.1(a) and 1.1(b), of this chap- taining more than 8 percent alcohol, under condi- tions of use B through H described in table 2 § (120 § ter. The finished food-contact laminate, in the form in which it contacts food, when extracted with the food simulating solvent or solvents characterizing the conditions of intended use as determined from Table 2 of § yield not more than 0.5 micrograms of with all food types described in table 1 of § 6 film having an average thickness not to exceed 40 microns (0.0016 inch) for use in processing, handling, and packaging of food types V IX listed in table 1 of § polymer use as modifiers in Nylon 6 resin films complying with paragraph (a)(6) of this sec- tion, at levels not to exceed 13 percent by weight of films whose average thickness will not exceed 15 microns (0.6 mils). The finished film is used for packaging, transporting, or holding food, excluding beverages containing more than 8 percent alcohol (by volume) at temperatures not to exceed 49 contact layers of: (1) Multilayer films and (2) rigid plastic containers composed of polypropylene food- contact and exterior layers, as defined in § of food except those containing more than 8 per- cent alcohol of food except alcoholic beverages containing more than 8 percent alcohol under conditions of use C, D, E, F, G, and H in table 2 of § xylylenediamine-adipic acid cyclic monomer per square inch of food-contact surface, when the food simulating solvent is analyzed by any appropriate, properly validated method b. In coatings intended for repeated use in contact 10.1 Nylon MXD±6 and impact modified MXD± 10.2 Impact modified Nylon MXD±6 resins for use as 10.3 Nylon MXD±6 resins for use only as nonfood- 11. Nylon 12T resins for use in contact with all types 12. Nylon 6I/6T resins for use in contact with all types
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N . . HC1 . . h. hour h. after 1 h. Solubility in boiling 4.2 ...... Dissolves in 1 Dissolves in 1 Dissolves in 1 Insoluble NA 380±400 270±277 260±285 enheit) Melting point (de- 551±09592 grees Fahr- 0.03 0.15 0.02 ± ± ± 0.015 0.015 ± ± 1.12 1.10 1.09 1.06 1.18 Specific gravity -
epsilon . . C. ° . . . 176.170(c) of this chapter -laurolactam not to exceed 0.1 Nylon resins
omega 176.170(c) of this chapter with a hot-fill 177.1395 of this chapter 176.170(c) of this chapter 176.170(c) of this chapter percent by weight. For use only as specified in § films having an average thickness not to exceed 51 microns (0.002 inch). The finished film is intended to contact all foods except those containing more than 8 percent ethanol under conditions of use B, C, D, E, F, G, and H listed in table 2 of § CFR 177.1395 of this chapter brane filters intended for repeated use. The finished membrane filter is intended to contact beverages containing no more than 13 percent alcohol, under conditions of use E, F, and G listed in table 2 § ing bottles) in contact with food of type VIA and VIB described in table 1 of § under conditions of use D through H described in table 2 of § temperature limitation of 40 caprolactam not to exceed 0.5 percent by weight and residual 13.1 Nylon 6/12 resins for use only in food-contact 13.2 Nylon 6/12 resins with residual 14. Nylon 6/69 resins for use only as specified in 21 15. Nylon 46 resins for use only in food-contact mem- 16. Nylon resins PA 6±3±T for repeated-use (exclud-
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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- to –25 cC. 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 in the Finding Aids 5 inches in diameter, a suction flask, section of this volume. and a hardened filter paper (Whatman § 177.1520 Olefin polymers. No. 50 or equivalent). The paper is wet with the solvent and a slight suction The olefin polymers listed in para- applied just before starting the filtra- graph (a) of this section may be safely tion. The resin is washed twice with used as articles or components of arti- approximately 100-milliliter portions of cles intended for use in contact with solvent and the combined filtrate and food, subject to the provisions of this washings are reduced to approximately section. 25 milliliters by evaporation at reduced (a) For the purpose of this section, pressure (50 millimeters to 100 millime- olefin polymers are basic polymers ters of mercury, absolute), heating as manufactured as described in this para- necessary. The contents of the flask graph, so as to meet the specifications are transferred to an evaporation dish prescribed in paragraph (c) of this sec- (which has been held in a vacuum des- tion, when tested by the methods de- iccator over anhydrous calcium sulfate scribed in paragraph (d) of this section. until constant weight has been at- (1)(i) Polypropylene consists of basic tained) and carefully evaporated to polymers manufactured by the cata- dryness. The weight of the solid residue lytic polymerization of propylene. is determined by difference after hold- (ii) Propylene homopolymer consists ing in a vacuum desiccator over anhy- of basic polymers manufactured by the drous calcium sulfate until constant catalytic polymerization of propylene weight has been attained. The percent with a metallocene catalyst. of solids extracted is calculated by di- (2) Polyethylene consists of basic viding the weight of the solid residue polymers manufactured by the cata- by the weight of the sample and multi- lytic polymerization of ethylene. plying by 100. (3) Olefin basic copolymers consist of (5) Viscosity number (VN). (i) The vis- basic copolymers manufactured by the cosity number (VN) for Nylon 6/12 resin catalytic copolymerization of: in a 96 percent sulfuric acid solution (5 (i) Two or more of the 1-alkenes hav- milligrams resin per milliliter) shall be ing 2 to 8 carbon atoms. Such olefin determined at 25 °C (77 °F) by method basic copolymers contain not less than ISO 307–1984(E), ‘‘Plastics-Polyamides- 96 weight-percent of polymer units de- Determination of Viscosity Number,’’ rived from ethylene and/or propylene, which is incorporated by reference. except that:
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(a)(1) Olefin basic copolymers manu- mer units derived from 4- factured by the catalytic copolym- methylpentene-1; or erization of ethylene and hexene-1 or (iii) Ethylene and propylene that ethylene and octene-1 shall contain not may contain as modifiers not more less than 90 weight-percent of polymer than 5 weight-percent of total polymer units derived from ethylene; units derived by copolymerization with (2) Olefin basic copolymers manufac- one or more of the following mono- tured by the catalytic copolymeriza- mers: tion of ethylene and hexene-1 shall con- tain not less than 80 but not more than 5-Ethylidine-2-norbornene. 90 weight percent of polymer units de- 5-Methylene-2-norbornene. rived from ethylene. (iv) Ethylene and propylene that may (3) Olefin basic copolymers manufac- contain as a modifier not more than 4.5 tured by the catalytic copolymeriza- weight percent of total polymer units tion of ethylene and pentene-1 shall derived by copolymerization with 1,4- contain not less than 90 weight-percent hexadiene. of polymer units derived from ethyl- (v) Ethylene and butene-1 copolymers ene. (CAS Reg. No. 25087–34–7) that shall (b) Olefin basic copolymers manufac- contain not less than 80 weight percent tured by the catalytic copolymeriza- of polymer units derived from ethyl- tion of ethylene and 4-methylpentene-1 ene. shall contain not less than 89 weight- (4) Poly(methylpentene) consists of percent of polymer units derived from basic polymers manufactured by the ethylene; catalytic polymerization of 4- (c)(1) Olefin basic copolymers manu- methylpentene-1. factured by the catalytic copolym- (5) Polyethylene graft copolymers erization of two or more of the mono- mers ethylene, propylene, butene-1, 2- consist of polyethylene complying with methylpropene-1, and 2,4,4- item 2.2 of paragraph (c) of this section trimethylpentene-1 shall contain not which subsequently has 3a,4,7,7a- less than 85 weight-percent of polymer tetrahydromethyl-4,7- units derived from ethylene and/or pro- methanoisobenzofuran-1,3-dione graft- pylene; ed onto it at a level not to exceed 1.7 (2) Olefin basic copolymers manufac- percent by weight of the finished co- tured by the catalytic copolymeriza- polymer. tion of propylene and butene-1 shall (6) Ethylene-maleic anhydride co- contain greater than 15 but not greater polymers (CAS Reg. No. 9006–26–2) con- than 35 weight percent of polymer taining no more than 2 percent by units derived from butene-1 with the weight of copolymer units derived from remainder being propylene. maleic anhydride. (d) Olefin basic terpolymers manufac- (b) The basic olefin polymers identi- tured by the catalytic copolymeriza- fied in paragraph (a) of this section tion of ethylene, hexene-1, and either may contain optional adjuvant sub- propylene or butene-1, shall contain stances required in the production of not less than 85 weight percent poly- such basic olefin polymers. The op- mer units derived from ethylene. tional adjuvant substances required in (e) Olefin basic copolymers manufac- the production of the basic olefin poly- tured by the catalytic polymerization mers or finished food-contact articles of ethylene and octene-1, or ethylene, may include substances permitted for octene-1, and either hexene-1, butene-1, such use by applicable regulations in propylene, or 4-methylpentene-1 shall parts 170 through 189 of this chapter, contain not less than 80 weight percent substances generally recognized as safe of polymer units derived from ethyl- in food and food packaging, substances ene. used in accordance with a prior sanc- (ii) 4-Methylpentene-1 and 1-alkenes tion or approval, and the following: having 6 to 10 carbon atoms. Such olefin basic copolymers shall contain not less than 95 molar percent of poly-
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Substance Limitations
Aromatic petroleum hydrocarbon resin, hydrogenated (CAS For use only as an adjuvant at levels not to exceed 25 percent Reg. No. 88526±47±0), 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, IV±B, VI±A through 220 °C (428 °F), and the subsequent catalytic hydrogenation VI±C, VII±B, 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 28±67 (Reapproved 1982), food Types III, IV±A, V, VII±A, 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 611±82, ``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 (HFS±200), 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. 78± For use as an initiator in the production of propylene 63±7). 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 (HFS± 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. 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. 121510±09±6), methyl meth- items 1.1, 3.1a, 3.2a, and 3.2b, where the copolymers com- acrylate/butyl acrylate copolymer (CAS Reg. No. 25852±37± plying with items 3.1a, 3.2a, and 3.2b contain not less than 3), methyl methacrylate homopolymer (CAS Reg. No. 9011± 85 weight-percent of polymer units derived from propylene. 14±7), and polypropylene (CAS Reg. No. 9003±07±0), 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 PP±MMA/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 (HFS±200), 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.
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Substance Limitations
Petroleum hydrocarbon resins (cyclopentadiene-type), hydro- For use only as an adjuvant at levels not to exceed 30 percent genated (CAS Reg. No. 68132±00±3) 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 C4±C5 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 28±67 (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, IV±B, VI±A, VI±B, VII±B, 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 3236±88, ``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, IV±A, V, VI±C, VII±A, 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 (HFS±200), 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. 68554±70±1) ...... For use only as a surface lubricant or anti-blocking agent in films. Poly(vinylidene fluoride) homopolymer (CAS Reg. No. 24937± For use only as a processing aid in the production of olefin 79±9), 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 3835±79 (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 (HFS±200), 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 68937±54±2). 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. Triisopropanolamine (CAS Reg. No. 122±20±3) ...... 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. 108±75±8), not less than 60 percent; 2,3,6- 1.3, and propylene copolymers complying with items 3.1, trimethylpyridine (CAS Reg. No. 1462±84±6), not more than and 3.2 of paragraph (c) of this section provided that the ad- 27 percent; 3,5-dimethylpyridine (CAS Reg. No. 591±22±0), 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. 9011±17±0) 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 (HFS±200), 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.
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Substance Limitations
Vinylidene fluoride-hexafluoropropene copolymer (CAS Reg. For use only as a processing aid in the production of olefin No. 9011±17±0), 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- 3835±79 (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 (HFS±200), 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)± hexane at speci- lene at specified fied temperatures temperatures
1.1a Polypropylene described in paragraph 0.880±0.913 MP: 160°±180 °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 0.880±0.913± MP: 150°±180 °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 only 0.80±0.88 to plasticize polyethylene described under items 2.1 and 2.2 of this table, provided that such plasticized polymers meet the max- imum extractable fraction and maximum soluble fraction specifications prescribed for such basic polyethylene 1.3 Polypropylene, noncrystalline, for use 0.80±0.88 SP:115°±138 °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, IV±B, VI±B, VII±B, 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, IV±B, VI±B, VII±B, and VIII 2.1 Polyethylene for use in articles that con- 0.85±1.00 ...... 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 0.85±1.00 ...... 2.6 pct at 50 °C Do. packing or holding food during cooking 2.3 Polyethylene for use only as component 0.85±1.00 ...... 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
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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)± hexane at speci- lene at specified fied temperatures temperatures
3.1a Olefin copolymers described in para- 0.85±1.00 ...... 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- 0.9±1.00 ...... 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. 3.2a Olefin copolymers described in para- 0.85±1.00 ...... 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 3.3a Olefin polymers described in paragraph 0.82±0.85 MP: 235±250 °C 6.6 pct at reflux 7.5 pct at 25 °C (a)(3)(ii) 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)± hexane at speci- lene at specified fied temperatures temperatures
3.3b Olefin copolymers described in para- 0.82±0.85 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 3.4 Olefin copolymers, primarily non-crys- 0.85±0.90 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- 0.85±0.90 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)± 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, IV±B, 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. 4. Poly(methylpentene) 0.82±0.85 MP: 235°±250 °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±0.94 ...... 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- Gradient Technique,’’ which is incor- mining whether olefin polymers con- porated by reference. Copies may be form to the specifications prescribed in obtained from the American Society this section are as follows, and are ap- for Testing Materials, 1916 Race St., plicable to the basic polymer in film Philadelphia, PA 19103, or may be ex- form not exceeding 4 mils in thickness. amined at the Office of the Federal The film to be tested shall be cut into Register, 800 North Capitol Street, approximately 1-inch squares by any NW., suite 700, Washington, DC 20408. convenient method that avoids con- (2) Melting point or softening point—(i) tamination by dust, dirt, or grease Melting point. The melting point shall (NOTE: Do not touch samples with bare be determined by ASTM method D2117– fingers—use forceps to hold or transfer 82, ‘‘Standard Test Method for Melting samples). Point of Semicrystalline Polymers by (1) Density. Density shall be deter- the Hot Stage Microscopy Method,’’ mined by ASTM method D1505–68 (Re- which is incorporated by reference. The approved 1979), ‘‘Standard Test Method availability of this incorporation by for Density of Plastics by the Density-
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reference is given in paragraph (d)(1) of (5) Bell jar for vacuum filtration into this section. beaker. (ii) Softening point. The softening (b) Reagent. n-Hexane, commercial point shall be determined by ASTM grade, specific gravity 0.663–0.667 (20 °C/ method E28–67 (Reapproved 1982), 20 °C), boiling range 66 °C-69 °C, or ‘‘Standard Test Method for Softening equivalent. Point by Ring-and-Ball Apparatus,’’ (c) Procedure. Weigh 1 gram of sample which is incorporated by reference. The accurately and place in a 250-milliliter availability of this incorporation by Erlenmeyer flask containing two or reference is given in paragraph (d)(1) of three boiling stones. Add 100 milliliters this section. of solvent, attach the flask to the con- (3) Maximum extractable fraction in n- denser (use no grease), and reflux the hexane—(i) Olefin copolymers described mixture for 2 hours. Remove the flask in paragraph (a)(3)(ii) of this section, from the heat, disconnect the con- denser, and filter rapidly, while still polypropylene, and poly(methylpentene). hot, through a small wad of glass wool A sample is refluxed in the solvent for packed in a short-stem funnel into a 2 hours and filtered at the boiling tared 150-millimeter beaker. Rinse the point. The filtrate is evaporated and flask and filter with two 10-milliliter the total residue weighed as a measure portions of the hot solvent, and add the of the solvent extractable fraction. rinsings to the filtrate. Evaporate the (a) Apparatus. (1) Erlenmeyer flasks, filtrate on a stream bath with the aid 250-milliliter, with ground joint. of a stream of nitrogen. Dry the res- (2) Condensers, Allihn, 400-millimeter idue in a vacuum oven at 110 °C for 2 jacket, with ground joint. hours, cool in a desiccator, and weigh (3) Funnels, ribbed 75-millimeter di- to the nearest 0.0001 gram. Determine ameter, stem cut to 40 millimeters. the blank on 120 milliliters of solvent (4) Funnels, Buchner type, with evaporated in a tared 150-milliliter coarse-porosity fritted disc, 60-milli- beaker. Correct the sample residue for meter diameter. this blank if significant. Calculation:
Grams of residue = Percent extractable with n-hexane. Grams of sample ×100
(ii) Olefin copolymers described in para- sion-proof electric motor, and a reflux graph (a)(3)(i) of this section and poly- condenser. The kettle is fitted with an ethylene. A preweighed sample is ex- electric heating mantle of appropriate tracted at 50 °C for 2 hours and filtered. size and shape, which is controlled by a The filtrate is evaporated and the total variable-voltage transformer. residue weighed as a measure of the (b) Evaporating apparatus. Rapid solvent extractable fraction. Alter- evaporation of large volumes of solvent natively, the sample is reweighed after requires special precautions to prevent the extraction period to give a measure contamination by dust. This is facili- of the solvent extractable fraction. The tated by a special ‘‘gas’’ cover con- maximum n-hexane-extractable frac- sisting of an inverted flat Pyrex crys- tion may be determined by the meth- tallizing dish of an appropriate size (190 ods set forth in paragraphs (d)(3)(ii)(a) millimeters × 100 millimeters) to fit a through (d)(3)(ii)(i) of this section. 1-liter beaker. Through the center of (a) Extraction apparatus. Two-liter, the dish are sealed an inlet tube for straight-walled, Pyrex (or equivalent) preheated, oxygen-free nitrogen, and resin kettles, fitted with three-hole an outlet tube located 1 inch off center. ground-glass covers are most conven- Nitrogen is fed from the supply source ient for this purpose. The cover is through a coil of 1⁄4-inch stainless steel fitted with a thermometer, a gas-tight tubing immersed in the same steam stirrer driven by an air motor or explo- bath used to supply heat for solvent
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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 temperature of the contents to 50 °C vacuum desiccator, and allow it to re- within 20–25 minutes. As the thermom- main overnight (at least 12 hours), eter reading approaches 45 °C–47 °C, re- after which the net weight of the dry duce the voltage to the predetermined residue is determined to the nearest setting that will just maintain the 0.0001 gram. Correct the result for any temperature at 50 °C. Do not overshoot solvent blank equivalent to the non- the prescribed temperature. Should volatile matter determined to be con- this occur discard the test and start tained in the amount of solvents used afresh. Exactly 2 hours after the sol- in the test. vent temperature has reached 50 °C, (e) Extraction apparatus for alternate disconnect the heater, remove the resin method. Two-liter extraction vessel, kettle from the heating jacket, and de- such as a resin kettle or round bottom cant the solvent, while still warm, flask, fitted with an Allihn condenser through a coarse filter paper placed on (size C), a 45/50 male joint with a Teflon top of a fritted-glass funnel, collecting sleeve, and a Teflon coated stir bar. the filtrate in a tared, glass-stoppered Water bath maintained at 49.5 °C ±0.5 Erlenmeyer flask of 1-liter capacity. °C containing a submersible magnetic Determine the weight of the filtrate re- stirrer motor with power supply. Other covered to the nearest gram. Recovery suitable means of maintaining tem- should be at least 90 percent of the perature control, such as electric heat- original solvent. Losses due to evapo- ing mantles, may be used provided that ration during heating and filtering the temperature range can be strictly have been found not to exceed 10 per- maintained. cent. Transfer about half of the solvent (f) Sample basket (Optional). A per- filtrate to a 1-liter beaker placed on an forated stainless steel cylindrical bas- opening in the steam bath and imme- ket that is approximately 1.5 inches in diately cover with the special ‘‘gas’’ cover, the inlet tube of which has been diameter, 1.6 inches high, and has per- attached with flexible tetrafluoro- forations of 0.125 inches in diameter for ethylene tubing to a source of high-pu- 33 holes/in2, or 40 percent open area. rity nitrogen in series with a stainless The basket should pass freely through steel heating coil immersed directly in the 45/50 female joint of the extraction the body of the steam bath. Maintain a flask. A No. 6–32 stainless steel eye- positive flow of warm nitrogen gas bolt is attached to the lid for posi- throughout the evaporation of the sol- tioning the basket in the extraction vent, adding the remainder of the fil- vessel. The positioning rod, approxi- trate from the Erlenmeyer flask as the mately 18 inches long and made from 1/ evaporation proceeds. When the volume 16 inch outside diameter 316 stainless of the solvent has been reduced to steel welding rod or equivalent and about 50 milliliters, transfer the con- hooked at both ends, is used to position centrated liquid to a previously tared the basket in the extraction apparatus.
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(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 inch squares using clean sharp scissors. at least 12 determinations. Applica- Proceed with Option 1 or 2. tions of solvent reuse should be con- Option 1. Using tweezers and noting firmed for each resin type before use. the number of film pieces, transfer 2.5 grams (accurately weighed to 0.1 milli- (4) Maximum soluble fraction in xy- gram) of polymer to the extraction ves- lene—(i) Olefin copolymers described in sel. Extract the film sample for 2 paragraph (a)(3)(ii) of this section, poly- hours. Allow the vessel to cool and fil- propylene, and poly(methylpen-tene). A ter the contents through a fritted por- sample is dissolved completely in xy- celain funnel. Wash the film pieces lene by heating and stirring in a bottle with fresh n-hexane, aspirate to dry- with little free space. The solution is ness, and transfer, using tweezers, to a allowed to cool without stirring, beaker. Recount the film pieces to whereupon the insoluble portion pre- verify that none were lost during the cipitates and is filtered off; the total transfer. Place the beaker in the vacu- solids content of the filtrate is then de- um oven for 2 hours at 80 °C ±5 °C. After termined as a measure of the soluble 2 hours, remove and place in a desic- fraction. cator to cool to room temperature (a) Apparatus. (1) Pyrex (or equiva- (about 1 hour). After cooling, reweigh lent) reagent bottle, 125-milliliter, the film pieces to the nearest 0.1 milli- glass-stoppered. gram. Calculate the percent hexane- (2) Heating mantle of size for 150-mil- extractables content from the weight liliter beaker (or suitable aluminum loss of the original sample. Multiply block to fit the 125-milliter bottle de- the result by 0.935 and compare with scribed in paragraph (d)(4)(i)(a)(1) of extraction limits in paragraph (c) of this section.
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(3) Magnetic stirrer for use under the heat and allow it to cool 1 hour in the heating mantle (combination magnetic air, without stirring. Then place the stirrer and hotplate may be used if alu- bottle in a water bath maintained at 25 minum block is used in place of heat- °C ±0.5 °C, and allow to stand 1 hour ing mantle). without stirring. Next, remove the bot- (4) Variable-voltage transformer, 7.5 tle from the water bath, shake, and amperes. pour part of the contents into the (5) Tetrafluoroethylene-resin-coated coarse-porosity fritted-glass funnel. stirring bar, 1-inch long. Apply suction, and draw 30–40 milli- (6) Constant temperature water bath liters of filtrate through, adding more maintained at 25 °C±0.5 °C. slurry to the funnel, and catching the (7) Aluminum dishes, 18 millimeters × filtrate in a large test tube. (If the 60 millimeters, disposable. slurry is hard to filter, add 10 grams of (8) Funnel, Buchner type, with diatomaceous earth filter aid to the coarse-porosity fritted disc, 30–60 milli- bottle and shake vigorously just prior meter diameter. to the filtration.) Pipet a suitable ali- (b) Reagent. Xylene with antioxidant. quot (preferably 20 milliliters) of the Dissolve 0.020 gram of phenyl-β- naph- filtrate into a tared aluminum dispos- thylamine in 1 liter of industrial grade able dish. Place the dish on a steam xylene having specific gravity 0.856– bath covered with a fresh sheet of alu- 0.867 (20 °C/20 °C) and boiling range 123 minum foil and invert a short-stemmed °C–160 °C. 4-inch funnel over the dish. Pass nitro- (c) Procedure. Weigh 1 to 2 grams of gen (heated if desired) down through sample to the nearest 0.001 gram and the funnel at a rate sufficient to just place in a 125-milliliter Pyrex reagent ripple the surface of the solvent. When bottle containing a 1-inch long tetra- the liquid has evaporated, place the fluoroethylene-resin-coated stirring dish in a vacuum oven at 140 °C and bar. Add 100 milliliters of solvent, set less than 50 millimeters mercury pres- the stopper in lightly, and place the sure for 2 hours. Cool in a desiccator bottle in the heating mantle or alu- and weigh. (Note: If the residue value minum block maintained at a tempera- seems high, redry in the vacuum oven ture of 120 °C, and stir with a magnetic for one-half hour to ensure complete stirrer until the sample is completely removal of all xylene solvent.) Calcula- dissolved. Remove the bottle from the 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- controlled by a variable-voltage trans- graph (a)(3)(i) of this section and poly- former. ethylene. A sample is extracted in xy- (2) Constant temperature water bath. It lene at reflux temperature for 2 hours must be large enough to permit immer- and filtered. The filtrate is evaporated sion of the extraction kettle and set to and the total residue weighed as a maintain 25 °C ±0.1 °C. measure of soluble fraction. (3) Evaporating apparatus. Gas cover (a) Apparatus—(1) Extraction appa- consisting of a flat Pyrex crystallizing ratus. Two-liter, straight-walled Pyrex dish (190 millimeters × 100 millimeters) (or equivalent) resin kettles, fitted inverted to fit over a 1-liter beaker with ground-glass covers, are most con- with 8-millimeter gas inlet tube sealed venient for this purpose. The cover is through center and an outlet tube 1 equipped with a thermometer and an inch off center. The beaker with gas efficient reflux condenser. The kettle is cover is inserted in an electric heating fitted with an electric heating mantle mantle equipped with a variable-volt- of appropriate size and shape which is age transformer. The outlet tube is at- tached to an efficient condenser
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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- 4 containing less than 10 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 reflux condenser and apply full voltage rected toward the center of the dish. (115 volts) to the heating mantle. When Avoid any charring of the residue. the xylene starts to boil, reduce the Transfer the weighing dish to a vacu- voltage to a level just sufficient to um desiccator at room temperature maintain reflux. After refluxing for at and allow to remain under reduced least 2 hours, disconnect the power pressure for at least 12 hours (over- source to the mantle, remove the ket- night), after which determine the net tle, and allow to cool in air until the weight of the residue to the nearest temperature of the contents drops to 50 0.0001 gram. Correct the result for non- °C, after which the kettle may be rap- volatile solvent blank obtained by idly cooled to 25 °C–30 °C by immersing evaporating the equivalent amount of in a cold water bath. Transfer the ket- xylene under identical conditions. Cal- tle to a constant temperature bath set culate the weight of residue originally to maintain 25 °C ±0.1 °C, and allow to present in the total weight of solvent equilibrate for a least 1 hour (may be (840 grams), using the appropriate fac- left overnight if convenient). Break up tor based on the weight of filtrate any precipitated polymers that may evaporated. have formed, and decant the xylene so- (5) Viscosity average molecular weight lution successively through a fast filter olefin copolymers described in paragraphs paper and then through a fritted-glass (a)(3) (iii) and (iv) of this section. The filter into a tared 1-liter Erlenmeyer viscosity average molecular weight flask, collecting only the first 450 mil- shall be determined from the kine- liliters—500 milliliters of filtrate (any matic viscosity (using ASTM method attempt to collect more of the xylene D445–74, ‘‘Test for Kinematic Viscosity solution usually results in clogging the of Transparent and Opaque Liquids’’ filter and risking losses). Reweigh the (Revised 1974), which is incorporated by Erlenmeyer flask and calculate the reference; copies are available from weight of the filtrate obtained to the American Society for Testing and Ma- nearest 0.1 gram. Transfer the filtrate, terials (ASTM), 1916 Race Street, quantitatively, from the Erlenmeyer Philadelphia, PA 19103, or available for flask to the 1-liter beaker, insert the inspection at the Office of the Federal beaker in its heating mantle, add a Register, 800 North Capitol Street, glass-coated magnetic stirring bar, and NW., suite 700, Washington, DC 20408) of
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solutions of the copolymers in solvents scribed in paragraph (a)(3)(ii) of this and at temperatures as follows: section shall be determined by ASTM (i) Olefin polymers described in para- method D 1601–78, ‘‘Standard Test graph (a)(3)(iii) of this section in Method for Dilute Solution Viscosity decahydronaphthalene at 135 °C. of Ethylene Polymers,’’ which is incor- (ii) Olefin polymers described in porated by reference in accordance paragraph (a)(3)(iv) of this section in with 5 U.S.C. 552(a). The availability of tetrachloroethylene at 30 °C. this incorporation by reference is given (6) Mooney viscosity—olefin copolymers in paragraph (d)(1) of this section. described in paragraph (a)(3)(iii) of this (e) Olefin copolymers described in section. Mooney viscosity is determined paragraph (a)(3) (i) of this section and by ASTM method D1646–81, ‘‘Standard polyethylene, alone or in combination, Test Method for Rubber—Viscosity and may be subjected to irradiation bom- Vulcanization Characteristics (Mooney bardment from a source not to exceed Viscometer),’’ which is incorporated by 2.3 million volts intensity to cause mo- reference (the availability of this in- lecular crosslinking of the polymers to corporation by reference is given in impart desired properties, such as in- paragraph (d)(1) of this section), using creased strength and increased ability the large rotor at a temperature of 100 to shrink when exposed to heat. ° ° C, except that a temperature of 127 C (f) The olefin polymers identified in shall be used for those copolymers and complying with this section, when whose Mooney viscosity cannot be de- used as components of the food-contact ° termined at 100 C. The apparatus con- surface of any article that is the sub- taining the sample is warmed for 1 ject of a regulation in parts 174, 175, minute, run for 8 minutes, and vis- 176, 177, 178, and § 179.45 of this chapter, cosity measurements are then made. shall comply with any specifications (7) Melt flow index. The melt flow and limitations prescribed by such reg- index of olefin polymers described ulation for the article in the finished below shall be determined by ASTM form in which it is to contact food. method D–1238–82, ‘‘Standard Test (g) The provisions of this section are Method for Flow Rates of Thermo- not applicable to olefin polymers iden- plastics by Extrusion Plastometer,’’ tified in § 175.105(c) (5) of this chapter which is incorporated by reference in and used in food-packaging adhesives accordance with 5 U.S.C. 552(a). The complying with § 175.105 of this chapter. availability of this incorporation by reference is given in paragraph (d)(1) of [42 FR 14572, Mar. 15, 1977] this section. The olefin polymers and EDITORIAL NOTE: For FEDERAL REGISTER ci- test conditions and procedures are as tations affecting § 177.1520, see the List of follows: CFR Sections Affected in the Finding Aids section of this volume. List of polymers Conditions/procedures
Olefin copolymers described in para- Condition L, proce- § 177.1550 Perfluorocarbon resins. graph (a)(3)(i)(c)(2) of this section. dure A. Perfluorocarbon resins identified in Olefin copolymers described in para- Condition E, proce- graph (a)(3)(v) of this section. dure A. this section may be safely used as arti- cles or components of articles intended (8) Melting peak temperature. The melt to contact food, subject to the provi- temperature of the olefin polymers de- sions of this section: scribed in paragraph (a)(3)(ii) of this (a) Identity. For the purpose of this section shall be determined by ASTM section, perfluorocarbon resins are method D 3418–82, ‘‘Standard Test those produced by: (1) The Method for Transition Temperatures of homopolymerization and/or copolym- Polymers by Thermal Analysis,’’ which erization of hexafluoropropylene and is incorporated by reference in accord- tetrafluoroethylene, and (2) the co- ance with 5 U.S.C. 552(a). The avail- polymerization of ability of this incorporation by ref- perfluoropropylvinylether and tetra- erence is given in paragraph (d)(1) of fluoroethylene (CAS Reg. No. 26655–00– this section. 5). The resins shall meet the extrac- (9) Intrinsic viscosity. The intrinsic tives limitations in paragraph (d) of viscosity of the olefin polymers de- this section.
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(b) Optional components. The List of substances Limitations perfluorocarbon resins identified in Naphthalene sulfonic acid For use only: paragraph (a) of this section as well as formaldehyde condensate, 1. As a component of re- articles or coating made from these sodium salt. peated-use coatings, resins may include the following op- based on the perfluorocarbon resin tional components except that the identified in paragraph resin identified in paragraph (a)(2) of (a)(1) of this section, not this section may not be used with the to exceed 0.030 milli- meter (0.0012 inch) in optional component, lithium thickness, and at a level polysilicate, mentioned in paragraph not to exceed 0.4 weight (b)(4) of this section. percent of the coating. 2. As a component of re- (1) Substances generally recognized peated-use coatings, as safe (GRAS) in food or food pack- based on the perfluorocarbon resin aging subject to any limitations cited identified in paragraph on their use. (a)(2) of this section, not (2) Substances used in accordance to exceed 0.10 millimeter (0.004 inch) in thickness, with a prior sanction or approval, sub- and at a level not to ex- ject to any limitations cited in the ceed 0.4 weight percent prior sanction or approval. of the coating. (3) Substances authorized under ap- plicable regulations in this part and in (c) Optional processing. Poly- tetra- parts 175 and 178 of this chapter and fluoroethylene resins may be irradi- subject to any limitations prescribed ated by either a cobalt-60 sealed therein. source, at a maximum dose of gamma radiation not to exceed 7.5 megarads, (4) The following substances, subject or an electron beam at energy levels to any limitations prescribed: not to exceed 2.5 million electron volts List of substances Limitations with a maximum dosage of 7.5 megarads, to produce lubricant pow- Lithium polysilicate containing For use only as a compo- ders having a particle diameter of not not more than 20 weight per- nent of repeated-use cent silica, not more than 2.1 coatings not exceeding more than 20 microns for use only as percent lithium oxide and 0.030 millimeter (0.0012 components of articles intended for re- having a maximum mole inch) in thickness where peated use in contact with food. ratio of Si02/Li20 of 8.5 to 1. the coatings are thermally cured at minimum sinter- (d) Specifications—(1) Infrared identi- ing temperatures of 371 fication. Perfluorocarbon resins can be °C (700 °F). Lithium ex- tractives shall not exceed identified by their characteristic infra- 1.55 milligrams per red spectra. square decimeter (0.1 (2) Melt-viscosity. (i) The perfluoro- milligram per square inch) of coating surface when carbon resins identified in paragraph tested in accordance with (a)(1) of this section shall have a melt paragraph (e)(2) of this viscosity of not less than 104 poises at section. 380 °C (716 °F) as determined by ASTM method D1238–82, ‘‘Standard Test Meth- od for Flow Rates of Thermoplastics by Extrusion Plastometer,’’ which is in- corporated by reference. Copies may be obtained from the American Society for Testing Materials, 1916 Race St., Philadelphia, PA 19103, or may be ex- amined at the Office of the Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC 20408. The melt viscosity of the perfluorocarbon resins identified in paragraph (a)(1) of this section shall not vary more than 50 percent within one-half hour at 380 °C (716 °F).
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(ii) Perfluorocarbon resins identified paragraph (e)(3) of this section when in paragraph (a)(2) of this section shall the resins in the form of coatings de- have a melt viscosity of not less than scribed in paragraphs (e)(2) (i) and (ii) 104 poises at 372 °C (702 °F) as deter- of this section are extracted at reflux mined by a more detailed method ti- temperatures for 2 hours separately tled ‘‘Determination of Melt Viscosity, with distilled water, 8 percent ethanol, Molecular Weight Distribution Index and n-heptane: and Viscosity Stability,’’ which is in- (i) Perfluorocarbon resin coatings corporated by reference. Copies are based on resins identified in paragraph available from the Center for Food (a)(1) of this section shall be applied to Safety and Applied Nutrition (HFS– both sides of a 0.025-millimeter (0.001 200), Food and Drug Administration, inch) thick aluminum foil to a thick- 200 C St. SW., Washington, DC 20204, or ness of 0.025 millimeter (0.001 inch) available for inspection at the Office of after thermal curing at 399 °C (750 °F) the Federal Register, 800 North Capitol for 10 minutes. If a primer is used, the Street, NW., suite 700, Washington, DC total thickness of the primer plus top- 20408. coat shall equal 0.025 millimeter (0.001 (3) Thermal instability index. The ther- inch) after heat curing. mal instability index of the tetra- (ii) Perfluorocarbon resin coatings fluoroethylene homopolymer shall not based on resins identified in paragraph exceed 50 as determined by ASTM (a)(2) of this section shall be applied to method D1457–56T, ‘‘Test for Thermal both sides of a 0.025-millimeter (0.001 Instablility index of Tetrafluoro- inch) thick aluminum foil to a thick- ethylene Homopolymer’’ (Revised 1956), ness of 0.10 millimeter (0.004 inch) after which is incorporated by reference. thermal curing at 427 °C (800 °F) for 10 Copies are available from University minutes. If a primer is used, the total Microfilms International, 300 N. Zeeb thickness of the primer plus topcoat Rd., Ann Arbor, MI 48106, or available shall equal 0.10 millimeter (0.004 inch) for inspection at the Office of the Fed- after heat curing. eral Register, 800 North Capitol Street, (3) The extracted surfaces shall meet NW., suite 700, Washington, DC 20408. the following extractability limits: The requirements of this paragraph do (i) Total extractives not to exceed 3.1 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 of 6.45 square decimeters (100 square per square inch). inches) or more and at least 1.27 milli- (f) Conditions of use. Perfluorocarbon meters (0.05 inch) thick shall be ex- resins identified in paragraph (a)(2) of tracted at reflux temperatures for 2 this section are limited to use as coat- hours separately with distilled water, ings or components of coatings for arti- 50 percent ethanol, n-heptane, and cles intended for repeated food-contact ethyl acetate. use. (2) Perfluorocarbon resins identified in paragraphs (a)(1) and (2) of this sec- [43 FR 44834, Sept. 29, 1978, as amended at 47 FR 11843, Mar. 19, 1982; 47 FR 14699, Apr. 6, tion and intended for use as coatings or 1982; 49 FR 10109, Mar. 19, 1984; 50 FR 1502, components of coatings shall meet Jan. 11, 1985; 54 FR 24898, June 12, 1989; 61 FR extractability limits prescribed in 14481, Apr. 2, 1996]
1 A more detailed procedure of extraction § 177.1555 Polyarylate resins. conditions is entitled, ‘‘Preparation of Ex- Polyarylate resins (CAS Reg. No. tracts,’’ which is incorporated by reference. 51706–10–6) may be safely used as arti- Copies are available from the Center for cles or components of articles intended Food Safety and Applied Nutrition (HFS– for use in contact with food in accord- 200), Food and Drug Administration, 200 C St. SW., Washington, DC 20204, or available for ance with the following prescribed con- inspection at the Office of the Federal Reg- ditions: ister, 800 North Capitol Street, NW., suite (a) Identity. Polyarylate resins (1, 3- 700, Washington, DC 20408. benzenedicarboxylic acid, diphenyl
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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 (c) Extractive limitations. The finished minimum weight average molecular food-contact article yields net total ex- weight of 20,000. tractives in each extracting solvent (3) Polyarylate resins may be identi- not to exceed 0.052 milligram per fied by their characteristic infrared square inch (corresponding to 0.008 mil- spectra. ligram per square centimeter) of food- (c) Extractive limitations. The finished contact surface, when extracted at polyarylate resins in sheet form at reflux temperature for 2 hours with the least 0.5 millimeter (0.020 inch) thick, following solvents: Distilled water, 50 when extracted with water at 121 °C percent (by volume) ethyl alcohol in (250 °F) for 2 hours, shall yield total distilled water, 3 percent acetic acid nonvolatile extractives not to exceed (by weight) in distilled water, and n- 2.33 micrograms per square centimeter heptane. (15 micrograms per square inch) of the (d) In testing the finished food-con- exposed resin surface. tact article made of (d) Limitations. Polyarylate resin ar- polyaryletherketone resin, use a sepa- ticles may be used in contact with all rate test sample for each required ex- foods except beverages containing tracting solvent. more than 8 volume percent ethanol [61 FR 42381, Aug. 15, 1996] under conditions of use A through H, described in table 2 of § 176.170(c) of this § 177.1560 Polyarylsulfone resins. chapter. Polyarylsulfone resins (CAS Reg. No. [52 FR 35540, Sept. 22, 1987] 79293–56–4) may be safely used as arti- cles or components of articles intended § 177.1556 Polyaryletherketone resins. for use in contact with food, at tem- The poly(oxy-1,4-phenylenecarbonyl- peratures up to and including normal 1,4-phenyleneoxy-1,4- baking temperatures, in accordance phenylenecarbonyl-1,4- with the following prescribed condi- phenylenecarbonyl-1,4-phenylene) res- tions: ins (CAS Reg. No. 55088–54–5 and CAS (a) Identity. Polyarylsulfone resins Reg. No. 60015–05–6 and commonly re- are copolymers containing not more ferred to as polyaryletherketone res- than 25 percent of oxy-p-phenylene- ins) identified in paragraph (a) of this oxy-p-phenylenesulfonyl-p-phenylene section may be safely used as articles polymer units and not less than 75 per- or components of articles intended for cent of oxy-p-phenylenesulfonyl-p- repeated use in contact with food, sub- phenylene-oxy-p-phenylenesulfonyl-p- ject to the provisions of this section. phenylene polymer units. The copoly- (a) Identity. Polyaryletherketone res- mers have a minimum reduced vis- ins consist of basic resins produced by cosity of 0.40 deciliter per gram in 1- reacting 4,4′-diphenoxy benzophenone methyl-2-pyrrolidinone in accordance and terephthaloyl dichloride in such a with ASTM method D2857–70 (Re- way that the finished resins have a approved 1977), ‘‘Standard Test Method minimum weight average molecular for Dilute Solution Viscosity of Poly- weight of 20,000 grams per mole, as de- mers,’’ which is incorporated by ref- termined by light scattering measure- erence. Copies may be obtained from ments in sulfuric acid at room tem- the American Society for Testing and perature. Materials, 1916 Race St., Philadelphia,
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PA 19103, or may be examined at the polymer units derived from ethylene in Office of the Federal Register, 800 the copolymer. North Capitol Street, NW., suite 700, (b) Specifications and limitations. Poly- Washington, DC 20408. 1-butene resins and butene/ethylene co- (b) Optional adjuvant substances. The polymers shall conform to the speci- basic polyarylsulfone resins identified fications prescribed in paragraph (b)(1) in paragraph (a) of this section may of this section, and shall meet the contain optional adjuvant substances extractability limits prescribed in required in the production of such paragraph (b)(2) of this section. basic copolymers. These optional adju- (1) Specifications—(i) Infrared identi- vant substances may include sub- fication. Poly-1-butene resins and stances permitted for such use by regu- butene/ethylene copolymers can be lations in parts 170 through 179 of this identified by their characteristic infra- chapter, substances generally recog- red spectra. nized as safe in food, substances used in (ii) Viscosity. Poly-1-butene resins and accordance with a prior sanction of ap- the butene/ethylene copolymers have proval, and substances named in this an intrinsic viscosity 1.0 to 3.2 as deter- paragraph and further identified as re- mined by ASTM method D1601–78, quired: ‘‘Standard Test Method for Dilute So- lution Viscosity of Ethylene Poly- Substances Limitations mers,’’ which is incorporated by ref- Sulfolane ..... Not to exceed 0.15 percent as residual sol- erence. Copies may be obtained from vent in the finished basic resin. the American Society for Testing Ma- terials, 1916 Race St., Philadelphia, PA (c) Extractive limitations. The finished 19103, or may be examined at the Office polyarylsulfone resin when extracted of the Federal Register, 800 North Cap- for 2 hours with the following solvents itol Street, NW., suite 700, Washington, at the specified temperatures yields DC 20408. total extractives in each extracting (iii) Density. Poly-1-butene resins solvent not to exceed 0.008 milligram have a density of 0.904 to 0.920 gms/cm3, per square centimeter of food-contact and butene/ethylene copolymers have a surface: distilled water at 121 °C (250 density of 0.890 to 0.916 gms/cm3 as de- °F), 50 percent (by volume) ethyl alco- termined by ASTM method D1505–68 hol in distilled water at 71.1 °C (160 °F), (Reapproved 1979), ‘‘Standard Test 3 percent acetic acid in distilled water Method for Density of Plastics by the at 100 °C (212 °F), and n-heptane at 65.6 Density-Gradient Technique,’’ which is °C (150 °F). incorporated by reference. The avail- NOTE: In testing the finished polyaryl- ability of this incorporation by ref- sulfone resin use a separate test sample for erence is given in paragraph (b)(1)(ii) of each required extracting solvent. this section. [50 FR 31046, July 24, 1985] (iv) Melt index. Poly-1-butene resins have a melt index of 0.1 to 24 and the § 177.1570 Poly-1-butene resins and butene/ethylene copolymers have a butene/ethylene copolymers. melt index of 0.1 to 20 as determined by The poly-1-butene resins and butene/ ASTM method D1238–82, condition E, ethylene copolymers identified in this ‘‘Standard Test Method for Flow Rates section may be safely used as articles of Thermoplastics by Extrusion Plas- or components of articles intended for tometer,’’ which is incorporated by ref- use in contact with food subject to the erence. The availability of this incor- provisions of this section. poration by reference is given in para- (a) Identity. Poly-1-butene resins are graph (b)(1)(ii) of this section. produced by the catalytic polymeriza- (2) Limitations. Poly-1-butene resins tion of 1-butene liquid monomer. and butene/ethylene copolymers for use Butene/ethylene copolymers are pro- in articles that contact food, and for duced by the catalytic polymerization articles used for packing or holding of 1-butene liquid monomer in the pres- food during cooking shall yield no ence of small amounts of ethylene more than the following extractables: monomer so as to yield no higher than (i) Poly-1-butene resins may be used a 6-weight percent concentration of as articles or components of articles
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intended for use in contact with food, (3) The condensation of 4,4′-isopro- provided that the maximum pylidenediphenol, carbonyl chloride, extractables do not exceed 2.5 percent and 0.5 percent weight maximum of by weight of the polymer when film or a2,a6-bis (6-hydroxy-m-tolyl) mesitol to molded samples are tested for 2 hours which may have been added certain op- at 50 °C (122 °F) in n-heptane. tional adjuvant substances required in (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 millimeter (0.004 to 0.008 inch) in thick- List of substances Limitations ness do not exceed 0.80 percent by p-tert-Butylphenol ...... weight of the polymer when extracted Chloroform ...... in a soxhlet extractor for 6 hours with p-Cumylphenol (CAS Reg. For use only as a chain ter- No. 599±64±4). minator at a level not to ex- refluxing 95 percent ethanol. ceed 5 percent by weight (iii) Poly-1-butene resins may be used of the resin. as articles or components of articles Ethylene dichloride. intended for packaging or holding food Heptane. Methylene chloride. during cooking, provided that the Monochlorobenzene ...... Not to exceed 500 p.p.m. as thickness of such polymers in the form residual solvent in finished in which they contact food shall not resin. Pentaerythritol tetrastearate For use only as a mold re- exceed 0.1 millimeter (0.004 inch) and (CAS Reg. No. 115±83±3). lease agent, at a level not yield maximum extractables of not to exceed 0.5 percent by more than 2.5 percent by weight of the weight of the finished resin. polymer when films are extracted for 2 Phenol (CAS Reg. No. 108± 95±2). 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 49 108±88±3). million as residual solvent FR 10109, Mar. 19, 1984; 50 FR 31349, Aug. 2, in finished resin. 1985] Triethylamine.
§ 177.1580 Polycarbonate resins. (c) Polycarbonate resins shall con- Polycarbonate resins may be safely form to the specification prescribed in used as articles or components of arti- paragraph (c)(1) of this section and cles intended for use in producing, shall meet the extractives limitations manufacturing, packing, processing, prescribed in paragraph (c)(2) of this preparing, treating, packaging, trans- section. porting, or holding food, in accordance (1) Specification. Polycarbonate resins with the following prescribed condi- can be identified by their char- tions: acteristic infrared spectrum. (a) Polycarbonate resins are poly- (2) Extractives limitations. The esters produced by: polycarbonate resins to be tested shall (1) The condensation of 4,4′-iso- be ground or cut into small particles propylidenediphenol and carbonyl chlo- that will pass through a U.S. standard ride to which may have been added cer- sieve No. 6 and that will be held on a tain optional adjuvant substances re- U.S. standard sieve No. 10. quired in the production of the resins; (i) Polycarbonate resins, when ex- or by tracted with distilled water at reflux (2) The reaction of molten 4,4′-iso- temperature for 6 hours, shall yield propylidenediphenol with molten di- total extractives not to exceed 0.15 per- phenyl carbonate in the presence of the cent by weight of the resins. disodium salt of 4,4′-isopro- (ii) Polycarbonate resins, when ex- pylidenediphenol. tracted with 50 percent (by volume)
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ethyl alcohol in distilled water at (1) Specifications. Polyestercarbonate reflux temperature for 6 hours, shall resins identified in paragraph (a) of yield total extractives not to exceed this section can be identified by their 0.15 percent by weight of the resins. characteristic infrared spectrum. The (iii) Polycarbonate resins, when ex- solution intrinsic viscosity of the tracted with n-heptane at reflux tem- polyestercarbonate resins shall have a perature for 6 hours, shall yield total range of 0.50 to 0.58 deciliter per gram extractives not to exceed 0.15 percent as determined by a method titled, ‘‘In- by weight of the resins. trinsic Viscosity (IV) of Lexan [42 FR 14572, Mar. 15, 1977, as amended at 46 Polycarbonate Resin by a Single Point FR 23227, Apr. 24, 1981; 49 FR 4372, Feb. 6, Method Using Dichloromethane as the 1984; 50 FR 14096, Apr. 10, 1985; 53 FR 29656, Solvent,’’ developed by the General Aug. 8, 1988; 59 FR 43731, Aug. 25, 1994] Electric Co., September 20, 1985, which is incorporated by reference in accord- § 177.1585 Polyestercarbonate resins. ance with 5 U.S.C. 552(a) and 1 CFR Polyestercarbonate resins may be part 51. Copies are available from the safely used as articles or components Center for Food Safety and Applied Nu- of articles intended for use in pro- trition (HFS–200), Food and Drug Ad- ducing, manufacturing, packing, proc- ministration, 200 C St. SW., Wash- essing, preparing, treating, packaging, ington, DC 20204, or may be examined or holding food, in accordance with the at the Office of the Federal Register, following prescribed conditions: 800 North Capitol Street, NW., suite (a) Polyestercarbonate resins (CAS 700, Washington, DC. Reg. No. 71519–80–7) are produced by the (2) Extractives limitations. The condensation of 4,4′-isopropyli- polyestercarbonate resins to be tested denediphenol, carbonyl chloride, shall be ground or cut into small par- terephthaloyl chloride, and ticles that will pass through a U.S. isophthaloyl chloride such that the res- standard sieve No. 6 and that will be ins are composed of 70 to 85 percent held on U.S. standard sieve No. 10. ester, of which up to 10 percent is the (i) Polyestercarbonate resins, when terephthaloyl isomer. The resins are extracted with distilled water at reflux manufactured using a phthaloyl chlo- temperature for 6 hours, shall yield ride/carbonyl chloride mole ratio of total nonvolatile extractives not to ex- 2.3–4.0/1 and an isophthaloyl chloride/ ceed 0.005 percent by weight of the res- terephthaloyl chloride mole ratio of ins. 9.0/1 or greater. (ii) Polyestercarbonate resins, when (b) Optional adjuvants. The optional extracted with 50 percent (by volume) adjuvant substances required in the ethyl alcohol in distilled water at production of resins identified in para- reflux temperature for 6 hours, shall graph (a) of this section may include: yield total nonvolatile extractives not (1) Substances used in accordance to exceed 0.005 percent by weight of the with § 174.5 of this chapter. resins. (2) Substances identified in (iii) Polyestercarbonate resins, when § 177.1580(b). extracted with n-heptane at reflux (3) Substances regulated in temperature for 6 hours, shall yield § 178.2010(b) of this chapter for use in total nonvolatile extractives not to ex- polycarbonate resins complying with ceed 0.002 percent by weight of the res- § 177.1580: ins. Provided, That the substances are used (3) Residual methylene chloride levels in in accordance with any limitation on polyestercarbonate resins. Polyester- concentration, conditions of use, and carbonate resin articles in the finished food types specified in § 178.2010(b) of form shall not contain residual meth- this chapter. ylene chloride in excess of 5 parts per (c) Polyestercarbonate resins shall million as determined by a method ti- conform to the specifications pre- tled ‘‘Analytical Method for Deter- scribed in paragraph (c)(1) of this sec- mination of Residual Methylene Chlo- tion and shall meet the extractive lim- ride in Polyestercarbonate Resin,’’ de- itations prescribed in paragraph (c)(2) veloped by the General Electric Co., of this section. July 23, 1991, which is incorporated by
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reference in accordance with 5 U.S.C. NW., suite 700, Washington, DC 20408), 552(a) and 1 CFR part 51. Copies are using No. 50 emery abrasive in lieu of available from the Center for Food Ottawa sand, shall exhibit an abrasion Safety and Applied Nutrition (HFS– coefficient of not less than 100 liters 200), Food and Drug Administration, per mil of thickness. 200 C St. SW., Washington, DC 20204, or [42 FR 14572, Mar. 15, 1977, as amended at 49 may be examined at the Office of the FR 10109, Mar. 19, 1984] Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC. § 177.1595 Polyetherimide resin. [57 FR 3940, Feb. 3, 1992] 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- chapter, table 1, under Type VIII, in ac- ethylidene)bis(4,1-phenyleneoxy)] bis- cordance with the following prescribed polymer with 1,3-benzenediamine (CAS conditions: Reg. No. 61128–46–9), and is derived from (a) For the purpose of this section, the condensation reaction of m- phenylenediamine and bisphenol A- polyester elastomers are those pro- dianhydride. duced by the ester exchange reaction (b) Optional adjuvants. The basic when one or more of the following polymer identified in paragraph (a) of phthalates—dimethyl terephthalate, this section may contain optional adju- dimethyl orthophthalate, and dimethyl vant substances required in the produc- isophthalate—is made to react with tion of basic resins or finished food- alpha-hydroomega-hydroxypoly contact articles. The optional adjuvant (oxytetramethylene) and/or 1,4- substances required in the production butanediol such that the finished elas- of the basic polymer may include sub- tomer has a number average molecular stances permitted for such use by ap- weight between 20,000 and 30,000. plicable regulations as set forth in part (b) Optional adjuvant substances em- 174 of this chapter. ployed in the production of the poly- (c) Specifications and extractives limi- ester elastomers or added thereto to tations—(1) Specifications. impart desired technical or physical Polyetherimide resin identified in properties may include the following paragraph (a) of this section shall have substances: an intrinsic viscosity in chloroform at List of substances Limitations 25 °C (77 °F) of not less than 0.35 deci- liter per gram as determined by a 4,4′ - Bis (alpha, alpha-di- For use only as an anti- method titled ‘‘Intrinsic Viscosity of methyl-benzyl) oxidant. diphenylamine. ULTEM Polyetherimide Using Chloro- Tetrabutyl titanate ...... For use only as a catalyst. form as the Solvent,’’ which is incor- porated by reference. Copies are avail- (c) An appropriate sample of the fin- able from the Center for Food Safety ished polyester elastomer in the form and Applied Nutrition (HFS–200), Food in which it contacts food when sub- and Drug Administration, 200 C St. jected to ASTM method D968–81, SW., Washington, DC 20204, or available ‘‘Standard Test Methods for Abrasion for inspection at the Office of the Fed- Resistance of Organic Coatings by the eral Register, 800 North Capitol Street, Falling Abrasive Tester,’’ which is in- NW., suite 700, Washington, DC 20408. corporated by reference (copies may be (2) Extractive limitations. Extractive obtained from the American Society limitations are applicable to the basic for Testing Materials, 1916 Race St., polyetherimide resin in the form of Philadelphia, PA 19103, or may be ex- molded discs of thickness 0.16 centi- amined at the Office of the Federal meter (0.063 inch). The resin discs when Register, 800 North Capitol Street, extracted with distilled water at 121 °C
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(250 °F) for 2 hours yield total nonvola- § 177.1610 Polyethylene, chlorinated. tile extractives of not more than 12.3 Chlorinated polyethylene identified micrograms per square centimeter. in this section may be safely used as [50 FR 31351, Aug. 2, 1985; 50 FR 35535, Sept. articles or components of articles that 3, 1985] contact food, except for articles used for packing or holding food during § 177.1600 Polyethylene resins, cooking, subject to the provisions of carboxyl modified. this section. Carboxyl-modified polyethylene res- (a) For the purpose of this section, ins may be safely used as the food-con- chlorinated polyethylene consists of tact surface of articles intended for use basic polymers produced by the direct in contact with food in accordance chlorination of polyethylene con- with the following prescribed condi- forming to the density, maximum n- tions: hexane extractable fraction, and max- (a) For the purpose of this section, imum xylene soluble fraction specifica- carboxyl-modified polyethylene resins tions prescribed under item 2.1 of the consist of basic polymers produced table in § 177.1520(c). Such chlorinated when ethylene-methyl acrylate basic polyethylene contains a maximum of 60 copolymers, containing no more than percent by weight of total chlorine, as 25 weight percent of polymer units de- determined by ASTM method D1303–55 rived from methyl acrylate, are made (Reapproved 1979), ‘‘Standard Test to react in an aqueous medium with Method for Total Chlorine in Vinyl one or more of the following sub- Chloride Polymers and Copolymers,’’ stances: which is incorporated by reference (copies may be obtained from the Ammonium hydroxide. American Society for Testing Mate- Calcium carbonate. rials, 1916 Race St., Philadelphia, PA Potassium hydroxide. 19103, or may be examined at the Office Sodium hydroxide. of the Federal Register, 800 North Cap- (b) The finished food-contact article, itol Street, NW., suite 700, Washington, when extracted with the solvent or sol- DC 20408), and has a 7.0 percent max- vents characterizing the type of food imum extractable fraction in n-hexane and under the conditions of time and at 50 °C, as determined by the method temperature characterizing the condi- described in § 177.1520(d)(3)(ii). tions of its intended use as determined (b) Chlorinated polyethylene may be from tables 1 and 2 of § 176.170(c) of this used in contact with all types of food, chapter, yields total extractives in except that when used in contact with each extracting solvent not to exceed fatty food of Types III, IV–A, V, VII–A, 0.5 milligram per square inch of food- and IX described in table 1 of § 176.170(c) contact surface as determined by the of this chapter, chlorinated poly- methods described in § 176.170(d) of this ethylene is limited to use only as a chapter; and if the finished food-con- modifier admixed at levels not exceed- tact article is itself the subject of a ing 15 weight percent in plastic articles regulation in parts 174, 175, 176, 177, 178, prepared from polyvinyl chloride and/ and § 179.45 of this chapter, it shall also or from vinyl chloride copolymers com- comply with any specifications and plying with § 177.1980. limitations prescribed for it by that [42 FR 14572, Mar. 15, 1977, as amended at 49 regulation. In testing the finished food- FR 10109, Mar. 19, 1984; 59 FR 14550, Mar. 29, contact articles, a separate test sample 1994] is to be used for each required extract- ing solvent. § 177.1615 Polyethylene, fluorinated. (c) The provisions of paragraph (b) of Fluorinated polyethylene, identified this section are not applicable to in paragraph (a) of this section, may be carboxyl-modified polyethylene resins safely used as food-contact articles in used in food-packaging adhesives com- accordance with the following pre- plying with § 175.105 of this chapter. scribed conditions:
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(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 tables 1 and 2 of § 176.170(c) of this chap- are not applicable to oxidized poly- ter, yields fluoride ion not to exceed 5 ethylene used as provided in §§ 175.125 parts per million calculated on the and 176.170(a)(5) of this chapter and basis of the volume of food held by the § 177.1200. food-contact article. [48 FR 39057, Aug. 29, 1983] § 177.1630 Polyethylene phthalate polymers. § 177.1620 Polyethylene, oxidized. Polyethylene phthalate polymers Oxidized polyethylene identified in identified in this section may be safely paragraph (a) of this section may be used as, or components of plastics safely used as a component of food-con- (films, articles, or fabric) intended for tact articles, in accordance with the use in contact with food in accordance following prescribed conditions: with the following prescribed condi- (a) Oxidized polyethylene is the basic tions: resin produced by the mild air oxida- (a) Polyethylene phthalate films con- tion of polyethylene conforming to the sist of a base sheet of ethylene density, maximum n-hexane extract- terephthalate polymer, ethylene able fraction, and maximum xylene terephthalate-isophthalate copolymer, soluble fraction specifications pre- or ethylene-1,4-cyclohexylene scribed under item 2.3 of the table in dimethylene terephthalate copoly- § 177.1520(c). Such oxidized polyethylene esters described in § 177.1315(b)(3), to has a minimum number average molec- which have been added optional sub- ular weight of 1,200, as determined by stances, either as constituents of the high temperature vapor pressure os- base sheet or as constituents of coat- mometry, contains a maximum of 5 ings applied to the base sheet. percent by weight of total oxygen, and (b) Polyethylene phthalate articles has an acid value of 9 to 19. consist of a base polymer of ethylene (b) The finished food-contact article, terephthalate polymer, or ethylene-1,4- when extracted with the solvent or sol- cyclohexylene dimethylene vents characterizing the type of food terephthalate copolyesters described in and under the conditions of time and § 177.1315(b)(3), to which have been temperature characterizing the condi- added optional substances, either as tions of its intended use as determined constituents of the base polymer or as from tables 1 and 2 of § 176.170(c) of this constituents of coatings applied to the chapter, yields net acidified chloro- base polymer.
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(c)(1) Polyethylene phthalate of the following: Azelaic acid, dimethyl spunbonded nonwoven fabric consist of azelate, dimethyl sebacate, sebacic acid. continuous filaments of ethylene Ethylene terephthalate copolymers: Pre- terephthalate polymer and ethylene pared by the condensation of dimethyl terephthalate or terephthalic acid with terephthalate-isophthalate copolymer ethylene glycol, modified with one or more to which may have been added optional of the following: Azelaic acid, dimethyl adjuvant substances required in their azelate, dimethyl sebacate, sebacic acid, preparation and finishing. pyromellitic dianhydride. The level of (2) The ethylene terephthalate- pyromellitic dianhydride shall not exceed isophthalate copolymer component of 0.5 percent by weight of the finished co- the fabric shall not exceed 25 percent polymer which may be used under condi- tions of use E through H as described in by weight. The filaments may be blend- table 2 of § 176.170(c) of this chapter. ed with other fibers regulated for the Ethylene terephthalate-isophthalate copoly- specific use and the spunbonded fabric mers: Prepared by the condensation of di- may be further bonded by application methyl terephthalate or terephthalic acid of heat and/or pressure. and dimethyl isophthalate or isophthalic (3) The fabric shall be used only in acid with ethylene glycol. The finished co- accordance with paragraph (i) of this polymers contain either: (a) 77 to 83 weight percent or section. (b) At least 97 weight percent of polymer (d) The quantity of any optional sub- units derived from ethylene stance employed in the production of terephthalate. polyethylene phthalate plastics does (ii) Base sheet and base polymer: not exceed the amount reasonably re- Ethylene-1,4-cyclohexylene dimethylene quired to accomplish the intended terephthalate copolyesters described in physical or technical effect or any lim- § 177.1315(b)(3). itations further provided. Any sub- Ethylene terephthalate polymer: Prepared stance employed in the production of by the condensation of dimethyl polyethylene phthalate plastics that is terephthalate and ethylene glycol. the subject of a regulation in parts 174, Ethylene terephthalate polymer: Prepared 175, 176, 177, 178 and 179 of this chapter by the condensation of terephthalic acid and ethylene glycol. conforms with any specification in such regulation. (iii) Coatings: (e) Substances employed in the pro- Acrylic copolymers (CAS Reg. No. 30394–86– duction of polyethylene phthalate plas- 6): Prepared by reaction of ethyl acrylate tics include: (CAS Reg. No. 140–88–5), methyl methacry- late (CAS Reg. No. 80–62–6), and (1) Substances generally recognized methacrylamide (CAS Reg. No. 79–39–0) as safe in food. blended with melamine-formaldehyde resin (2) Substances subject to prior sanc- (CAS Reg. No. 68002–20–0). For use in coat- tion or approval for use in poly- ings for polyethylene phthalate films com- ethylene phthalate plastics and used in plying with paragraph (a) of this section.– accordance with such sanction or ap- Ethylene azelate-terephthalate copolymer: proval. The copolymer, dissolved in 1,1,2-trichloro- ethane and/or methylene chloride, may be (3) Substances which by regulation in used as a heat-activated sealant on poly- parts 174, 175, 176, 177, 178 and § 179.45 of ethylene terephthalate film intended for this chapter may be safely used as sealing polyethylene terephthalate pouch- components of resinous or polymeric es that are used as containers of either food-contact surfaces subject to the nonalcoholic beverages or alcoholic bev- provisions of such regulation. erages containing not more than 15 percent ethyl alcohol. The copolymer has a (4) Substances identified in this para- terephthalate/azelate molecular ratio of graph (e)(4) subject to the limitations 1.25/1.00 and a relative viscosity of not less prescribed: than 1.5 as determined by a method title ‘‘General Procedure of Determining the LIST OF SUBSTANCES AND LIMITATIONS Relative Viscosity of Resin Polymers,’’ which is incorporated by reference. Copies (i) Base sheet: are available from the Center for Food Ethylene terephthalate copolymers: Pre- Safety and Applied Nutrition (HFS–200), pared by the condensation of dimethyl Food and Drug Administration, 200 C St. terephthalate or terephthalic acid with SW., Washington, DC 20204, or available for ethylene glycol, modified with one or more inspection, at the Office of the Federal
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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 plying with paragraph (a) of this section, weight of the polyethylene at levels not to exceed 0.025 gram per terephthalate. square meter (0.016 milligram per square Chloroform-soluble extractives shall not inch) of the film, in contact with food of exceed 0.08 milligram/centimeter 2 (0.5 types VIII and IX in table 1 of § 176.170(c) of milligram/inch 2) of food-contact surface this chapter, under use conditions E, F, of the modified polyethylene and G in table 2 of § 176.170(c) of this chap- terephthalate article when exposed to ter. the following solvents at temperatures and times indicated: (iv) Emulsifiers: (a) Distilled water at 49 °C (120 °F) for 24 Sodium dodecylbenzenesulfonate: As an ad- hours; juvant in the application of coatings to the (b) n-Heptane at 49 °C (120 °F) for 24 hours; base sheet or base polymer. (c) 8 percent ethyl alcohol at 49 °C (120 °F) Sodium lauryl sulfate: As an adjuvant in the for 24 hours. application of coatings to the base sheet or For use in contact with all types of foods base polymer. except (a) those containing more than 8 2-Sulfoethyl methacrylate, sodium salt (CAS percent alcohol, or (b) those at tempera- Reg. No. 1804–87–1). For use only in copoly- tures over 49 °C (120 °F). mer coatings on polyethylene phthalate film under conditions of use E, F, and G de- (f) Polyethylene phthalate plastics scribed in table 2 of § 175.300(d) of this chap- conforming with the specifications pre- ter, and limited to use at a level not to ex- scribed in paragraph (f)(1) of this sec- ceed 2.0 percent by weight of the dry co- tion are used as provided in paragraph polymer coating. (f)(2) of this section: (v) Modifier: (1) Specifications. (i) The food contact 1,4-Benzenedicarboxylic acid, dimethyl ester, surface, when exposed to distilled polymer with 1,4-butanediol and α-hydro- water at 250 °F for 2 hours, yields chlo- omega-hydroxypoly(oxy-1,4-butanediyl) roform-soluble extractives not to ex- CAS Reg. No. 9078–71–1) meeting the fol- ceed 0.5 mg/in 2 of food contact surface lowing specifications: exposed to the solvent; and Melting point: 200° to 215 °C as determined (ii) The food contact surface, when by ASTM method D2117–82, ‘‘Standard exposed to n-heptane at 150 °F for 2 Test Method for Melting Point of Semicrystalline Polymers by the Hot hours, yields chloroform-soluble ex- Stage Microscopy Method,’’ which is in- tractives not to exceed 0.5 mg/in 2 of corporated by reference. Copies may be food contact surface exposed to the sol- obtained from the American Society for vent.
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(2) Conditions of use. The plastics are (i) Distilled water at 212 °F for 2 used for packaging, transporting, or hours. holding food, excluding alcoholic bev- (ii) n-Heptane at 150 °F for 2 hours. erages, at temperatures not to exceed (iii) 50 percent ethyl alcohol at 120 °F 250 °F. for 24 hours. (g) Polyethylene phthalate plastics (2) Conditions of use. The plastics are conforming with the specifications pre- intended for: scribed in paragraph (g)(1) of this sec- (i) Dry food contact. tion are used as provided in paragraph (g)(2) of this section. (ii) Bulk food (excluding alcoholic (1) Specifications. (i) The food contact beverages) repeated use applications, surface meets the specifications in including filtration, at temperatures ° paragraph (f)(1) of this section; and not exceeding 212 F. (ii) The food contact surface when ex- (iii) Filtration of bulk alcoholic bev- posed to 50 percent ethyl alcohol at 120 erages, not exceeding 50 percent alco- °F for 24 hours, yields chloroform-solu- hol by volume, at temperatures not ex- ble extractives not to exceed 0.5 mg/in 2 ceeding 120 °F. of food contact surface exposed to the (j) Polyethylene phthalate plastics, solvent. composed of ethylene terephthalate- (2) Conditions of use. The plastics are isophthalate containing a minimum of used for packaging, transporting, or 98 weight percent of polymer units de- holding alcoholic beverages that do not rived from ethylene terephthalate, or exceed 50 percent alcohol by volume. ethylene-1,4-cyclohexylene (h) Uncoated polyethylene phthalate dimethylene terephthalate copoly- plastics consisting of a base sheet or esters described in § 177.1315(b)(3), con- base polymer prepared as prescribed forming with the specifications pre- from substances identified in para- scribed in paragraph (j)(1) of this sec- graphs (e)(4)(i) and (ii) of this section tion, are used as provided in paragraph and conforming with the specifications (j)(2) of this section. prescribed in paragraph (h)(1) of this (1) Specifications. (i) The food contact section are used as provided in para- surface meets the specifications in graph (h)(2) of this section: paragraph (f)(1) of this section and (1) Specifications. (i) The food contact (ii)( ) surface, when exposed to distilled a Containers with greater than 500 water at 250 °F for 2 hours yields chlo- mL capacity. The food-contact surface roform-soluble extractives not to ex- when exposed to 95 percent ethanol at ° ceed 0.02 milligram/inch 2 of food con- 120 F for 24 hours should not yield tact surface exposed to the solvent; and chloroform-soluble extractives in ex- (ii) The food contact surface, when cess of 0.005 mg/in 2. exposed to n-heptane at 150 °F for 2 (b) Containers with less than or equal to hours, yields chloroform-soluble ex- 500 mL capacity. The food contact sur- tractives not to exceed 0.02 milligram/ face when exposed to 95 percent eth- inch 2 of food contact surface exposed anol at 120 °F for 24 hours should not to the solvent. yield chloroform-soluble extractives in (2) Conditions of use. The plastics are excess of 0.05 mg/in 2. used to contain foods during oven bak- (2) Conditions of use. The plastics are ing or oven cooking at temperatures used for packaging, transporting, or above 250 °F. holding alcoholic foods that do not ex- (i) Polyethylene phthalate fabric, ceed 95 percent alcohol by volume. identified in paragraph (c) of this sec- tion and conforming with the specifica- [42 FR 14572, Mar. 15, 1977, as amended at 42 tions prescribed in paragraph (i)(1) of FR 18611, Apr. 8, 1977; 44 FR 40886, July 13, this section, is used only as provided in 1979; 45 FR 6541, Jan. 29, 1980; 47 FR 11844, Mar. 19, 1982; 47 FR 53346, Nov. 26, 1982; 48 FR paragraph (i)(2) of this section. 30361, July 1, 1983; 49 FR 10110, Mar. 19, 1984; (1) Specifications. Chloroform-soluble 50 FR 31047, July 24, 1985; 51 FR 3772, Jan. 30, extractives shall not exceed 0.2 milli- 1986; 52 FR 32917, Sept. 1, 1987; 54 FR 15750, gram/inch 2 of food-contact surface Apr. 19, 1989; 54 FR 24898, June 12, 1989; 60 FR when exposed to the following solvents 57927, Nov. 24, 1995; 60 FR 61654, Dec. 1, 1995; at temperatures and times indicated: 61 FR 46718, Sept. 5, 1996]
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§ 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 (1) Optional adjuvant substances au- gram/liter of tetrasodium thorized for this use in accordance with pyrophosphate and 0.5 percent deter- ° § 174.5 of this chapter. gent. The items are agitated at 80 C ° (2) Optional finish components, total (180 F) for 20 minutes, and then sub- weight not to exceed 1 percent by jected to a cold water rinse. weight of the base polymer, as follows: (2) Poly(phenyleneterephthalamide) resins in the form of pulp may be used List of substances Limitations as gaskets and packing for food proc- essing equipment at temperatures not Diundecylphthalate (CAS Reg. No. 3648±20±2). to exceed 260 °C (500 °F). Mono- and dipotassium salts of lauryl phosphate (CAS [57 FR 3125, Jan. 28, 1992] Reg. No. 39322±78±6). o-Phenylphenol (CAS Reg. For use as a fungicide for fin- § 177.1635 Poly(p-methylstyrene) and No. 90±43±7). ish coating materials. Not rubber-modified poly(p-methyl- to exceed 0.01 percent by styrene). weight of the base poly- mer. Poly(p-methylstyrene) and rubber- Poly(oxyethylene/ modified poly(p-methylstyrene) identi- oxypropylen- fied in this section may be safely used e)monobutylether (CAS Reg. No. 9038±95±3). as components of articles intended for Poly(oxyethylene) use in contact with food, subject to the mono(nonylphenyl)ether provisions of this section: (CAS Reg. No. 9019±45± 9). (a) Identity. For the purposes of this Polyvinyl methylether (CAS section, poly(p-methylstyrene) and Reg. No. 9003±09±2). rubber-modified poly(p-methylstyrene) Poly(oxyethylene) sorbitol monolaurate tetraoleate are basic polymers, manufactured as (CAS Reg. No. 71243±28± described in this paragraph, meeting 2). the specifications prescribed in para- Poly(oxyethylene) sorbitol graph (c) of this section. hexaoleate (CAS Reg. No. 57171±56±9). (1) Poly(p-methylstyrene) (CAS Reg. 4,4′-Butylidenebis (6-tert- For use only as an oxidation No. 24936–41–2) polymer produced by the butyl-m-cresol) (CAS Reg. inhibitor for finish coating polymerization of p-methylstyrene. No. 85±60±9). materials. Not to exceed 0.01 percent by weight of (2) Rubber-modified poly(p- the base polymer. methylstyrene) (CAS Reg. No. 33520–88– 6) polymer produced by combining sty- (c) Specifications. (1) rene-butadiene copolymer and/or Poly(phenyleneterephthalamide) resins polybutadiene with poly(p-
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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: shall contain not more than 1 weight (a) Identity. For the purpose of this percent of total residual p- section, poly(oxy-1,2- methystyrene monomer, as determined ethanediyloxycarbonyl-2,6- by a gas chromatographic method ti- naphthalenediylcarbonyl) resins (CAS tled, ‘‘Gas Chromatographic Deter- Reg. No. 24968–11–4) are polymers mination of PMS and PET in PPMS formed by catalytic transesterification Basic Polymers,’’ which is incorporated of 2,6-dimethylnaphthalene by reference. Copies are available from dicarboxylate with ethylene glycol fol- the Center for Food Safety and Applied lowed by catalytic polycondensation. Nutrition (HFS–200), Food and Drug (b) Specifications—(1) Density. The Administration, 200 C St. SW., Wash- density of poly(oxy-1,2- ington, DC 20204, or available for in- ethanediyloxycarbonyl-2,6- spection at the Office of the Federal naphthalenediylcarbonyl) resins shall Register, 800 North Capitol Street, be between 1.33 and 1.40 grams per NW., suite 700, Washington, DC 20408. cubic centimeter. (2) Rubber-modified poly(p- (2) Inherent viscosity. The finished methylstyrene) basic polymers identi- food-contact article shall have a min- fied in paragraph (a)(2) of this section imum inherent viscosity of 0.55 deci- shall contain not more than 0.5 weight liter per gram in a solution of 0.1 gram percent of total residual p- of polymer in 100 milliliters of a 25/40/ methylstyrene monomer, as deter- 35 (weight/weight/weight) solution of p- mined by the method identified in chlorophenol/tetrachloroethane/phenol. paragraph (c)(1) of this section The viscosity is determined by East- (d) Other specifications and limitations. man Chemical Co.’s method ECD-A-AC- The poly(p-methylstyrene) and rubber- G-V-1-5, ‘‘Determination of Dilute So- modified poly(p-methylstyrene) identi- lution Viscosity of Polyesters,’’ dated fied in and complying with this sec- May 31, 1988, which is incorporated by tion, when used as components of the reference in accordance with 5 U.S.C. food-contact surface of any article that 552(a) and 1 CFR part 51. Copies are is the subject of a regulation in parts available from the Office of Premarket 175, 176, 177, 178 and § 179.45 of this chap- Approval, Center for Food Safety and ter, shall comply with any specifica- Applied Nutrition (HFS–215), Food and tions and limitations prescribed by Drug Administration, 200 C St. SW., such regulation for the article in the Washington, DC 20204, or may be exam- finished form in which it is to contact ined at the Center for Food Safety and food. Applied Nutrition’s Library, Food and
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Drug Administration, 200 C St. SW., polymer units derived from styrene rm. 3321, Washington, DC, or at the Of- monomer. fice of the Federal Register, 800 North (b) Optional adjuvants. The basic Capitol St. NW., Washington, DC. polymers identified in paragraph (a) of (c) Extraction limitations. A 0.5 milli- this section may contain optional adju- meter (0.02 inch) thick sheet of resin vant substances required in the produc- when extracted with water at 121 °C tion of such basic polymers. Such op- (250 °F) for 2 hours shall yield total tional adjuvant substances may in- nonvolatile extractives not exceeding clude substances permitted for such 2.0 micrograms per square inch of ex- use by regulations in parts 170 through posed resin surface. 189 of this chapter, substances gen- (d) Conditions of use. The finished erally recognized as safe in food, and food contact article shall be: substances used in accordance with a (1) Used in contact only with food of prior sanction or approval. Types I, II, IVB, VIA, VIB, VIIB, and (c) Specifications. (1) Polystyrene VIII identified in table 1 of § 176.170(c) basic polymers identified in paragraph of this chapter, under conditions of use (a)(1) of this section shall contain not A through H described in table 2 of more than 1 weight percent of total re- § 176.170(c) of this chapter; and with sidual styrene monomer, as determined food of Types III, IVA, V, VIC, VIIA, by the method described in paragraph and IX identified in table 1 of (d) of this section, except that when § 176.170(c) of this chapter, under condi- used in contact with fatty foods of tions of use C through H described in Types III, IV-A, V, VII-A, and IX de- table 2 of § 176.170(c) of this chapter; scribed in table 1 of § 176.170(c) of this and chapter, such polystyrene basic poly- (2) Identified in a manner that will mers shall contain not more than 0.5 differentiate the article from articles weight percent of total residual sty- made of other polymeric resins to fa- rene monomer. cilitate collection and sorting. (2) Rubber-modified polystyrene [61 FR 14965, Apr. 4, 1996] basic polymers identified in paragraph (a)(2) of this section shall contain not § 177.1640 Polystyrene and rubber- more than 0.5 weight percent of total modified polystyrene. residual styrene monomer, as deter- Polystyrene and rubber-modified pol- mined by the method described in para- ystyrene identified in this section may graph (d) of this section. be safely used as components of arti- (d) Analytical method for determination cles intended for use in contact with of total residual styrene monomer con- food, subject to the provisions of this tent—(1) Scope. This method is suitable section. for the determination of residual sty- (a) Identity. For the purposes of this rene monomer in all types of styrene section, polystyrene and rubber-modi- polymers. fied polystyrene are basic polymers (2) Principle. The sample is dissolved manufactured as described in this para- in methylene chloride. An aliquot of graph so as to meet the specifications the solution is injected into a gas chro- prescribed in paragraph (c) of this sec- matograph. The amount of styrene tion when tested by the method de- monomer present is determined from scribed in paragraph (d) of this section. the area of the resulting peak. (1) Polystyrene consists of basic poly- (3) Apparatus—(i) Gas chromatograph. mers produced by the polymerization Beckman GC-2A gas chromatograph of styrene. with hydrogen flame detector or appa- (2) Rubber-modified polystyrene con- ratus of equivalent sensitivity. sists of basic polymers produced by (ii) Chromatograph column. One-quar- combining styrene-butadiene copoly- ter inch outside diameter stainless mers and/or polybutadiene with poly- steel tubing (0.028 inch wall thickness), styrene, either during or after polym- 4 feet in length, packed with 20 percent erization of the polystyrene, such that polyethylene glycol (20,000 molecular the finished basic polymers contain not weight) on alkaline treated 60–80 mesh less than 75 weight percent of total firebrick.
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(iii) Recorder. Millivolt range of 0–1, 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: (ii) By means of a microliter syringe, (a) Polysulfide polymer-polyepoxy inject 1 microliter of the standard solu- resins are the reaction products of liq- tion into the gas chromatograph. Meas- uid polysulfide polymers and ure the area of the styrene monomer polyfunctional epoxide resins, cured peak which emerges after approxi- with the aid of mately 12 minutes. tri(dimethylaminomethyl) phenol, to (7) (i) Transfer 1 gram of Procedure. which have been added certain optional sample (accurately weighed to the substances to impart desired techno- nearest 0.001 gram to a 2-ounce bottle logical properties to the resins. Subject and add several glass beads. Pipette to any limitations prescribed in this 25.0 milliliters of methylene chloride section, the optional substances may into the bottle. Cap the bottle tightly include: and place on a mechanical shaker. (1) Substances generally recognized Shake until the polymer is completely as safe in food and food packaging. dissolved. If any insoluble residue re- (2) Substances the use of which is mains, allow the bottle to stand (or permitted under applicable regulations centrifuge at a low speed) until a clear in this part, prior sanctions, or approv- supernatant layer appears. als. (ii) By means of a microliter syringe, (3) Substances named in this subpara- inject 3 microliters of the clear super- graph and further identified as re- natant liquid into the gas chro- quired: matograph. (iii) Measure the area of the resulting List of substances Limitations styrene monomer peak. Compare the sample peak area with the area pro- Bis(2-chloroethyl) formal. Bis(dichloropropyl) formal ...... Cross-linking agent. duced by the standard styrene mon- Butyl alcohol ...... Solvent. omer solution. Calculation: Carbon black (channel process). Chlorinated paraffins ...... Cross-linking agent. Percent residual styrene mon- Epoxidized linseed oil. omer=Milligrams monomer in stand- Epoxidized soybean oil. ard×peak area of sample/Peak area of mon- Epoxy resins (as listed in omer standard×sample weight in grams×30 § 175.300(b)(3)(viii)(a) of this chap- ter).. (e) Other specifications and limitations. Ethylene glycol monobutyl ether ...... Solvent. The polystyrene and rubber-modified Magnesium chloride. Methyl isobutyl ketone ...... Solvent. polystyrene identified in and com- Naphthalene sulfonic acid-formalde- plying with this section, when used as hyde condensate, sodium salt.
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List of substances Limitations imum 92 percent) and 4,4′- sulfonylbis[phenol] (maximum 8 per- Sodium dibutyl naphthalene Wetting agent. sulfonate. cent) (CAS Reg. No. 88285–91–0) pro- Sodium hydrosulfide. duced when a mixture of 4,4′- Sodium polysulfide. isopropylidenediphenol (minimum 92 β,β′,γ,γ′-Tetrachloro normal propyl Cross-linking agent. ′ ether. percent) and 4,4 -sulfonylbis[phenol] Titanium dioxide. (maximum 8 percent) is made to react Toluene ...... Solvent. with 4,4′-dichlorodiphenyl sulfone in Trichloroethane ...... Cross-linking agent. such a way that the finished resin has 1,2,3-Trichloropropane ...... Do. Urea-formaldehyde resins. a minimum number average molecular Xylene ...... Solvent. weight of 26,000, as determined by os- motic pressure in dimethylformamide. (b) The resins are used as the food- (b) The basic polysulfone resins iden- contact surface for dry food. tified in paragraph (a) of this section (c) An appropriate sample of the fin- may contain optional adjuvant sub- ished resin in the form in which it con- stances required in the production of tacts food, when subjected to ASTM such basic resins. The optional adju- method D968–81, ‘‘Standard Test Meth- vant substances required in the produc- ods for Abrasion Resistance of Organic tion of the basic polysulfone resins Coatings by the Falling Abrasive Test- may include substances described in er,’’ which is incorporated by reference § 174.5(d) of this chapter and the fol- (copies may be obtained from the lowing: American Society for Testing Mate- rials, 1916 Race St., Philadelphia, PA List of substances Limitations 19103, or may be examined at the Office Dimethyl sulfoxide ..... Not to exceed 50 parts per million as of the Federal Register, 800 North Cap- residual solvent in finished basic itol Street, NW., suite 700, Washington, resin in paragraph (a)(1) of this DC 20408), using No. 50 Emery abrasive section. in lieu of Ottawa sand, shall exhibit Monochlorobenzene .. Not to exceed 500 parts per million as residual solvent in finished and abrasion coefficient of not less basic resin in paragraph (a)(1) of than 20 liters per mil of film thickness. this section. N-methyl-2- Not to exceed 0.01 percent (100 [42 FR 14572, Mar. 15, 1977, as amended at 49 pyrrolidone. parts per million) as residual sol- FR 10110, Mar. 19, 1984] vent in finished basic resin in para- graph (a)(2) of this section. § 177.1655 Polysulfone resins. Polysulfone resins identified in para- (c) Polysulfone resins, when ex- graph (a) of this section may be safely tracted at reflux temperatures for 6 used as articles or components of arti- hours with the solvents—distilled cles intended for use in contact with water, 50 percent (by volume) ethyl al- food, in accordance with the following cohol in distilled water, 3 percent ace- prescribed conditions: tic acid in distilled water, and n- (a) For the purpose of this section, heptane, yield total extractives in each polysulfone resins are: extracting solvent not to exceed 0.0078 (1) Poly(oxy-p-phenylenesulfonyl-p- milligram per square centimeter (0.05 phenyleneoxy-p- milligram per square inch) of resin sur- phenyleneisopropylidene-p-phenylene) face. Note: In testing the finished resins (CAS Reg. No. 25154–01–2) con- polysulfone resins, use a separate resin sisting of basic resins produced when test sample for each required extract- the disodium salt of 4,4′- ing solvent. isopropylidenediphenol is made to (d) Polysulfone resins intended for re- react with 4,4′-dichlorodiphenyl sulfone peated use in contact with food may be in such a way that the finished resins used under conditions of use A through have a minimum number average mo- H in table 2 of § 176.170(c) of this chap- lecular weight of 15,000, as determined ter. The resins intended for single-serv- by osmotic pressure in ice food-contact use may be used only monochlorobenzene; or under condition of use H described in (2) 1,1′-Sulfonylbis[4-chlorobenzene] table 2 of § 176.170(c) of this chapter. polymer with 4,4′-(1- [51 FR 882, Jan. 9, 1986; 51 FR 4165, Feb. 3, methylethylidene)bis[phenol] (min- 1986; 61 FR 29475, June 11, 1996]
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§ 177.1660 Poly (tetramethylene (ii) Not to exceed 0.02 milligram per terephthalate). square inch of food contact surface ° Poly(tetramethylene terephthalate) when extracted for 2 hours at 150 F (poly (oxytetramethyleneoxyter- with n-heptane. ephthaloyl)) [Chemical Abstracts Serv- (iii) Not to exceed 0.04 milligram per ice Registry No. 24968–12–5] identified square inch of food contact surface ° in this section may be safely used as when extracted for 2 hours at 212 F articles or components of articles in- with 3 percent aqueous acetic acid. tended to contact food, in accordance (iv) Not to exceed 0.02 milligram per with the following prescribed condi- square inch of food contact surface tions: when extracted for 2 hours at 65.6 °C ° (a) Identity. For the purpose of this (150 F) with 50 percent ethanol. section, poly (tetramethylene [42 FR 14572, Mar. 15, 1977, as amended at 50 terephthalate) is the reaction product FR 20748, May 20, 1985; 52 FR 20069, May 29, of dimethyl terephthalate with 1,4- 1987] butanediol to which may have been added certain optional substances to § 177.1670 Polyvinyl alcohol film. impart desired technological properties Polyvinyl alcohol film may be safely to the polymer. used in contact with food of the types (b) Optional adjuvant substances. identified in § 176.170(c) of this chapter, Poly(tetramethylene terephthalate) table 1, under Types V, VIII, and IX, in identified in paragraph (a) of this sec- accordance with the following pre- tion may contain optional adjuvant scribed conditions: substances. The quantity of any op- (a) The polyvinyl alcohol film is pro- tional adjuvant substance employed in duced from polyvinyl alcohol having a the production of the polymer does not minimum viscosity of 4 centipoises exceed the amount reasonably required when a 4-percent aqueous solution is to accomplish the intended technical tested at 20 °C. or physical effect. Such adjuvants may (b) The finished food-contact film for include substances generally recog- use in contact with Food Types V or nized as safe in food, substances used in IX, when extracted with the solvent accordance with prior sanction, and characterizing the type of food and substances permitted under applicable under the conditions of time and tem- regulations in this part. perature characterizing its intended (c) Specifications. (1) Inherent vis- use as determined from tables 1 and 2 cosity of a 0.50 percent solution of the of § 176.170(c) of this chapter, yields polymer in phenol/tetrachloroethane total extractives not to exceed 0.078 (60/40 weight ratio) solvent is not less milligram per square centimeter (0.5 than 0.6 as determined using a Wagner milligram per square inch) of food-con- viscometer (or equivalent) and cal- tact surface when tested by ASTM culated from the following equation: method F34–76 (Reapproved 1980), (natural log arithm of N ) ‘‘Standard Test Method for Liquid Ex- Inherent = r traction of Flexible Barrier Materials,’’ viscos ity (c) which is incorporated by reference. Copies may be obtained from the Amer- where: ican Society for Testing Materials, 1916 Nr=Ratio of flow time of the polymer solu- Race St., Philadelphia, PA 19103, or tion to that of the solvent and c=polymer may be examined at the Office of the concentration of the test solution in grams per 100 milliliters. Federal Register, 800 North Capitol Street, NW., suite 700, Washington, DC (2) Poly(tetramethylene 20408. terephthalate) in the finished form in which it is to contact food shall yield (c) The finished food-contact film total extractives as follows: shall not be used as a component of (i) Not to exceed 0.08 milligram per food containers intended for use in con- square inch of food contact surface tact with water. when extracted for 2 hours at 250 °F [42 FR 14572, Mar. 15, 1977, as amended at 49 with distilled water. FR 10110, Mar. 19, 1984]
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§ 177.1680 Polyurethane resins. α-Hydro-omega-hydroxypoly (oxytetra- methylene). The polyurethane resins identified in α,α′-(Isopropylidenedi-p-phenylene)bis[omega- paragraph (a) of this section may be hydroxypoly (oxypropylene)(3–4 moles)], safely used as the food-contact surface average molecular weight 675. of articles intended for use in contact Maleic anhydride. with bulk quantities of dry food of the Methyl oxirane polymer with oxirane (CAS type identified in § 176.170(c) of this Reg. No. 9003–11–6). chapter, table 1, under Type VIII, in ac- Methyl oxirane polymer with oxirane, ether with 1,2,3–propanetriol (CAS Reg. No. 9082– cordance with the following prescribed 00–2). conditions: α,α′α″,α′″-Neopentanetetrayltetrakis [omega- (a) For the purpose of this section, hydroxypoly (oxypropylene) (1–2 moles)], polyurethane resins are those produced average molecular weight 400. when one or more of the isocyanates Pentaerythritol-linseed oil alcoholysis prod- listed in paragraph (a)(1) of this section uct. is made to react with one or more of Phthalic anhydride. the substances listed in paragraph Polybutylene glycol. (a)(2) of this section: Polyethyleneadipate modified with ethanol- amine with the molar ratio of the amine to (1) Isocyanates: the adipic acid less than 0.1 to 1. Bis(isocyanatomethyl) benzene (CAS Reg. Poly(oxycarbonylpentamethylene). No. 25854–16–4). Polyoxypropylene ethers of 4.4′-isopropyl- Bis(isocyanatomethyl) cyclohexane (CAS idenediphenol (containing an average of 2– Reg. No. 38661–72–2). 4 moles of propylene oxide). 4,4′-Diisocyanato-3,3′-dimethylbiphenyl (bi- Polypropylene glycol. tolylene diisocyanate). α,α′,α″-1,2,3-Propanetriyltris [omega- Diphenylmethane diisocyanate. hydroxypoly (oxypropylene) (15–18 moles)], Hexamethylene diisocyanate. average molecular weight 3,000. 3-Isocyanatomethyl - 3,5,5 - trimethylcyclo- Propylene glycol. hexyl isocyanate. α,α′,α″-[Propylidynetris (methylene)] tris 4,4-Methylenebis(cyclohexyl isocyanate). [omega-hydroxypoly (oxypropylene) (min- Toluene diisocyanate. imum 1.5 moles)], minimum molecular weight 400. (2) List of substances: α-[ρ(1,1,3,3-Tetramethylbutyl) - phenyl]- Adipic acid. omega-hydroxypoly(oxyethylene) (5 moles), 1,4-Butanediol. average molecular weight 425. 1,3-Butylene glycol. Trimethylol propane. 1,4–Cyclohexane dimethanol (CAS Reg. No. (b) Optional adjuvant substances em- 105–08–8). ployed in the production of the poly- 2,2-Dimethyl-1,3-propanediol. Ethylene glycol. urethane resins or added thereto to im- 1,6–Hexanediol (CAS Reg. No. 629–11–8).α– part desired technical or physical prop- Hydro–οµεγα–hydroxypoly(oxy–1,4– erties may include the following sub- butanediyl) (CAS Reg. No. 25190–06–1). stances:
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) (136±170 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.
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List of substances Limitations
Tetrakis [methylene±(2,5±di-tert-butyl-4-hydroxyhydrocinna- Stabilizer. mate)]methane (CAS Reg. No. 6683±19±8). 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. 57609±64±0).
(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:
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, IV±B, VI, VII±B, (¥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.
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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
(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, IV±B, VI, VII±B, 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, IV±B, VI, °F) and 86 temperature for 2 (150 °F) for 2 hr VII±B, 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. 66070±58±4): 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, IV±B, VI, (198 °F) to hr on a 0.071 cm on a 0.071 cm VII±B, 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. 66070±58±4): 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, IV±A, V, VII±A, 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- (2) Glass transition points. The glass mining whether styrene block poly- transition points shall be determined mers conform to the specifications pre- by either of the following methods: scribed in this section are as follows (i) ASTM method D2236–70 (‘‘Stand- and are applicable to the finished poly- ard Method of Test for Dynamic Me- mer. chanical Properties of Plastics by (1) Molecular weight. Molecular Means of Torsional Pendulum,’’ which weight shall be determined by intrinsic is incorporated by reference; copies are viscosity (or other suitable method). available from American Society for Testing and Materials (ASTM), 1916 Race Street, Philadelphia, PA 19103, or
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available for inspection at the Office of ethanol, and the maximum net residue the Federal Register, 800 North Capitol solubles in chloroform, shall be deter- Street, NW., suite 700, Washington, DC mined in accordance with § 176.170(d)(3) 20408) modified by using a forced reso- of this chapter using a sandwich form nant vibration instead of a fixed vibra- of the finished copolymer of the speci- tion and by using frequencies of 25 to 40 fied thickness and for the time and cycles per second instead of 0.1 to 10 temperature specified in paragraph (b) cycles per second. of this section. (ii) Direct reading viscoelastometric (d) The provisions of this section are method titled ‘‘Direct Reading not applicable to butadiene-styrene co- Viscoelastrometric Method for Deter- polymers listed in other sections of mining Glass Transition Points of Sty- this subpart. rene Block Polymers’’ (which is incor- (e) The provisions of this section are porated by reference; copies are avail- not applicable to styrene block poly- able from the Center for Food Safety mers with 1,3-butadiene listed in and Applied Nutrition (HFS–200), Food § 175.105 of this chapter. and Drug Administration, 200 C St. SW., Washington, DC 20204, or available [42 FR 14572, Mar. 15, 1977, as amended at 42 for inspection at the Office of the Fed- FR 43621, Aug. 30, 1977; 47 FR 11844, Mar. 19, eral Register, 800 North Capitol Street, 1982; 51 FR 16828, May 7, 1986; 54 FR 24898, NW., suite 700, Washington, DC 20408), June 12, 1989; 58 FR 65546, Dec. 15, 1993] by which the glass transition points § 177.1820 Styrene-maleic anhydride are determined in the tensile mode of copolymers. deformation at a frequency of 35 hertz using a Rheovibron Model DDV–II (or Styrene-maleic anhydride copoly- equivalent) Direct Reading mers identified in paragraph (a) of this Viscoelastometer. Take maxima in the section may be safely used as articles out-of-phase component of the complex or components of articles intended for modulus as the glass transition points. use in contact with food, subject to For block polymers of low styrene con- provisions of this section. tent or for simple block polymers, the (a) For the purpose of this section, polymer may be treated with 0.3 part styrene-maleic anhydride copolymers per hundred dicumyl peroxide and are those produced by the polymeriza- cured for 30 minutes at 153 °C to accen- tion of styrene and maleic anhydride so tuate the upper transition point. that the finished polymers meet the (3) Maximum extractable fractions in specifications prescribed in paragraph distilled water and 50 percent ethanol and (b) of this section, when tested by the the maximum net residue solubles in chlo- methods described in paragraph (c) of roform. The maximum extractable frac- this section. tions in distilled water and 50 percent (b) Specifications:
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, IV±A, IV±B, V, VI±B (except that will pass U.S. standard carbonated beverages), VII±A, VII±B, 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.
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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
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. 27288±99±9) 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, IV±A, IV±B, V, U.S. standard sieve No. 20. VI, VII±A, VII±B, 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- § 177.1830 Styrene-methyl methacry- mining conformance with specifica- late copolymers. tions for styrene-maleic anhydride co- Styrene-methyl methacrylate co- polymers prescribed in this section are polymers identified in this section may as follows: be safely used as components of plastic (1) Molecular weight. Molecular articles intended for use in contact weight shall be determined by mem- with food, subject to the provisions of brane osmometry. this section. (2) Residual styrene monomer content. (a) For the purpose of this section, Residual styrene monomer content styrene-methyl methacrylate copoly- shall be determined by the method de- mers consist of basic copolymers pro- scribed in § 177.1640(d). duced by the copolymerization of sty- (3) Residual maleic anhydride monomer rene and methyl methacrylate such content. Residual maleic anhydride that the finished basic copolymers con- monomer content shall be determined tain more than 50 weight percent of by a gas chromatographic method ti- polymer units derived from styrene. tled ‘‘Determination of Residual Ma- (b) The finished plastic food-contact leic Anhydride in Polymers by Gas article, when extracted with the sol- Chromatography,’’ which is incor- vent or solvents characterizing the porated by reference. Copies are avail- type of food and under the conditions able from the Center for Food Safety of time and temperature characterizing and Applied Nutrition (HFS–200), Food the conditions of intended use as deter- and Drug Administration, 200 C St. mined from tables 1 and 2 of § 176.170(c) SW., Washington, DC 20204, or available of this chapter, yields extractives not for inspection at the Office of the Fed- to exceed the following when tested by eral Register, 800 North Capitol Street, the methods prescribed in § 177.1010(c); NW., suite 700, Washington, DC 20408. (1) Total nonvolatile extractives not (d) The provisions of this section are to exceed 0.3 milligram per square inch not applicable to styrene-maleic anhy- of surface tested. dride copolymers listed in other sec- (2) Potassium permanganate oxidiz- tions of this subpart. able distilled water and 8 and 50 per- cent alcohol extractives not to exceed [42 FR 14572, Mar. 15, 1977, as amended at 47 an absorbance of 0.15. FR 11844, Mar. 19, 1982; 47 FR 14698, Apr. 6, 1982; 54 FR 24898, June 12, 1989] (3) Ultraviolet-absorbing distilled water and 8 and 50 percent alcohol ex- tractives not to exceed an absorbance of 0.30.
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(4) Ultraviolet-absorbing n-heptane § 177.1900 Urea-formaldehyde resins in extractives not to exceed an absorb- molded articles. ance of 0.40. Urea-formaldehyde resins may be safely used as the food-contact surface § 177.1850 Textryls. of molded articles intended for use in Textryls identified in this section contact with food, in accordance with may be safely used as articles or com- the following prescribed conditions: ponents of articles, intended for use in (a) For the purpose of this section, producing, manufacturing, packing, urea-formaldehyde resins are those processing, preparing, treating, pack- produced when 1 mole of urea is made aging, transporting or holding food, to react with not more than 2 moles of subject to the provisions of this sec- formaldehyde in water solution. tion. (b) The resins may be mixed with re- (a) Textryls are nonwoven sheets pre- fined wood pulp and the mixture may pared from natural or synthetic fibers, contain other optional adjuvant sub- bonded with fibryl (Fibryl consists of a stances which may include the fol- polymeric resin in fibrous form com- lowing: mingled with fiber to facilitate sheet List of substances Limitations formation and subsequently heat cured to fuse the fibryl and effect bonding). Hexamethylenetetramine ...... For use only as polymeriza- tion-control agent. (b) Textryls are prepared from the fi- Tetrachlorophthalic acid an- Do. bers, fibryls, and adjuvants identified hydride. in paragraph (c) of this section, and Zinc stearate ...... For use as lubricant. subject to limitations prescribed in that paragraph, provided that any sub- (c) The finished food-contact article, stance that is the subject of a regula- when extracted with the solvent or sol- vents characterizing the type of food tion in parts 174, 175, 176, 177, 178 and and under the conditions of time and § 179.45 of this chapter conforms with temperature characterizing the condi- any specifications in such regulation tions of its intended use as determined for that substance as a component of from tables 1 and 2 of § 175.300(d) of this polymeric resins used as food contact chapter, yields total extractives in surfaces. each extracting solvent not to exceed (c) The fibers, fibryls, and adjuvants 0.5 milligram per square inch of food- permitted are as follows: contact surface as determined by the methods described in § 175.300(e) of this Substances Limitations chapter. (1) Fibers prepared from pol- Conforming with § 177.1630. NOTE: In testing the finished food-contact yethylene terephthalate article, use a separate test sample for each resins. required extracting solvent. (2) Fibryls prepared from As the basic polymer. vinyl chloride-vinyl acetate copolymer. § 177.1950 Vinyl chloride-ethylene co- (3) Adjuvant substance, As a solvent in the prepara- polymers. dimethylformamide. tion of fibryl. The vinyl chloride-ethylene copoly- mers identified in paragraph (a) of this (d) Textryls meeting the conditions section may be safely used as compo- of test prescribed in paragraph (d)(1) of nents of articles intended for contact this section are used as prescribed in with food, under conditions of use D, E, paragraph (d)(2) of this section. F, or G described in table 2 of § 176.170 (1) Conditions of test. Textryls, when (c) of this chapter, subject to the provi- extracted with distilled water at reflux sions of this section. temperature for 1 hour, yield total ex- (a) For the purpose of this section, tractives not to exceed 1 percent. vinyl chloride-ethylene copolymers (2) Uses. Textryls are used for pack- consist of basic copolymers produced aging or holding food at ordinary tem- by the copolymerization of vinyl chlo- peratures and in the brewing of hot ride and ethylene such that the fin- beverages. ished basic copolymers meet the speci- fications and extractives limitations
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prescribed in paragraph (c) of this sec- (d) Analytical methods: The analyt- tion, when tested by the methods de- ical methods for determining whether scribed in paragraph (d) of this section. vinyl chloride-ethylene basic copoly- (b) The basic vinyl chloride-ethylene mers conform to the extractives limi- copolymers identified in paragraph (a) tations prescribed in paragraph (c) of of this section may contain optional this section are as follows and are ap- adjuvant substances required in the plicable to the basic copolymers in production of such basic copolymers. powder form having a particle size such The optional adjuvant substances re- that 100 percent will pass through a quired in the production of the basic U.S. Standard Sieve No. 40 and 80 per- vinyl chloride-ethylene copolymers cent will pass through a U.S. Standard may include substances permitted for Sieve No. 80: such use by regulations in parts 170 (1) Reagents—(i) Water. All water used through 189 of this chapter, substances in these procedures shall be generally recognized as safe in food, demineralized (deionized), freshly dis- and substances used in accordance with tilled water. 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 (iii) Total extractives obtained by ex- 150 °F in the case of the heptane ex- tracting with water at 150 °F for 2 tract. In the case of the aqueous ex- hours contain no more than 0.5 milli- tract, the evaporation to constant gram of vinyl chloride-ethylene copol- weight is completed in 15 minutes at ymer per 100 grams of sample tested as 230 °F; and in the case of heptane ex- determined from the organic chlorine tract, it is overnight under vacuum at content. The organic chlorine content 150 °F. The residue is weighed and cor- is determined as described in paragraph rected for the solvent blank. Calcula- (d)(3) of this section. tion:
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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.
Milligrams of aqueous extracted TF× × 64.3 = ×100 copolymer per 100-gram sample Weight of sample in grams
where: T=Milliliters of silver nitrate (sample minus blank)×normality of silver nitrate.
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F=1,200/A (as defined above) cosity of Vinyl Chloride Polymers,’’ (e) The vinyl chloride-ethylene co- which is incorporated by reference. polymers identified in and complying Copies may be obtained from the Amer- with this section, when used as compo- ican Society for Testing Materials, 1916 nents of the food-contact surface of Race St., Philadelphia, PA 19103, or any article that is the subject of a reg- may be examined at the Office of the ulation in parts 174, 175, 176, 177, 178 Federal Register, 800 North Capitol and § 179.45 of this chapter, shall com- Street, NW., suite 700, Washington, DC ply with any specifications and limita- 20408. tions prescribed by such regulation for (2) Extractives limitations. The fol- the article in the finished form in lowing extractives limitations are de- which it is to contact food. termined by the methods prescribed in (f) The provisions of this section are § 177.1970(d). not applicable to vinyl chloride-ethyl- (i) Total extractives do not exceed ene copolymers used as provided in 0.01 weight percent when extracted ° §§ 175.105 and 176.180 of this chapter. with water at 150 F for 2 hours. (ii) Total extractives do not exceed [42 FR 14572, Mar. 15, 1977, as amended at 49 0.30 weight percent when extracted FR 10110, Mar. 19, 1984] with n-heptane at 150 °F for 2 hours. (c) Other specifications and limitations. § 177.1960 Vinyl chloride-hexene-1 co- polymers. The vinyl chloride-hexene-1 copoly- mers identified in and complying with The vinyl chloride-hexene-1 copoly- this section, when used as components mers identified in paragraph (a) of this of the food-contact surface of any arti- section or as components of articles in- cle that is subject to a regulation in tended for use in contact with food, parts 174, 175, 176, 177, 178 and § 179.45 of under conditions of use D, E, F, or G this chapter, shall comply with any described in table 2 of § 176.170(c) of this specifications and limitations pre- chapter, subject to the provisions of scribed by such regulation for the arti- this section. cle in the finished form in which it is (a) Identity. For the purposes of this to contact food. section vinyl chloride-hexene-1 copoly- mers consist of basic copolymers pro- [42 FR 14572, Mar. 15, 1977, as amended at 49 duced by the copolymerization of vinyl FR 10110, Mar. 19, 1984] chloride and hexene-1 such that the fin- ished copolymers contain not more § 177.1970 Vinyl chloride-lauryl vinyl than 3 mole-percent of polymer units ether copolymers. derived from hexene-1 and meet the The vinyl chloride-lauryl vinyl ether specifications and extractives limita- copolymers identified in paragraph (a) tions prescribed in paragraph (b) of this of this section may be used as an arti- section. The copolymers may option- cle or as a component of an article in- ally contain hydroxypropyl methyl- tended for use in contact with food sub- cellulose and trichloroethylene used as ject to the provisions of this section. a suspending agent and chain transfer (a) Identity. For the purposes of this agent, respectively, in their produc- section vinyl chloride-lauryl vinyl tion. ether copolymers consist of basic co- (b) Specifications and limitations. The polymers produced by the copolym- vinyl chloride-hexene-1 basic copoly- erization of vinyl chloride and lauryl mers meet the following specifications vinyl ether such that the finished co- and extractives limitations: polymers contain not more than 3 (1) Specifications. (i) Total chlorine weight-percent of polymer units de- content is 53 to 56 percent as deter- rived from lauryl vinyl ether and meet mined by any suitable analytical pro- the specifications and extractives limi- cedure of generally accepted applica- tations prescribed in paragraph (c) of bility. this section. (ii) Inherent viscosity in (b) Optional adjuvant substances. The cyclohexanone at 30 °C is not less than basic vinyl chloride-lauryl vinyl ether 0.59 deciliters per gram as determined copolymers identified in paragraph (a) by ASTM method D1243–79, ‘‘Standard of this section may contain optional Test Method for Dilute Solution Vis- adjuvant substances required in the
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production of such basic copolymers. borosilicate flask, and for each gram of These optional adjuvant substances sample add 3 milliliters of solvent pre- may include substances permitted for viously heated to 150 °F. Maintain the such use by regulations in parts 170 temperature of the contents of the through 189 of this chapter, substances flask at 150 °F for 2 hours using a hot generally recognized as safe in food, plate while also maintaining gentle and substances used in accordance with mechanical agitation. Filter the con- a prior sanction or approval. tents of the flask rapidly through No. (c) Specifications and limitations. The 42 Whatman filter paper with the aid of vinyl chloride-lauryl vinyl ether basic suction. Transfer the filtrate to flat copolymers meet the following speci- glass dishes that are warmed on a hot fications and extractives limitations: plate and evaporate the solvent with (1) Specifications. (i) Total chlorine the aid of a stream of filtered air. When content is 53 to 56 percent as deter- the volume of the filtrate has been re- mined by any suitable analytical pro- duced to 10 to 15 milliliters, transfer cedure of generally accepted applica- the filtrate to tared 50-milliliter bility. borosilicate glass beakers and com- (ii) Inherent viscosity in plete evaporation to a constant weight cylcoHhexanone at 30 °C is not less in a 140 °F vacuum oven. Carry out a than 0.60 deciliter per gram as deter- corresponding blank determination mined by ASTM method D1243–79, with each solvent. Determine the ‘‘Standard Test Method for Dilute So- weight of the residue corrected for the lution Viscosity of Vinyl Chloride solvent blank and calculate the result Polymers,’’ which is incorporated by as percent of the initial weight of the reference. Copies may be obtained from resin sample taken for analysis. the American Society for Testing Ma- (e) Other specifications and limitations. terials, 1916 Race St., Philadelphia, PA The vinyl chloride-lauryl vinyl ether 19103, or may be examined at the Office copolymers identified in and complying of the Federal Register, 800 North Cap- with this section, when used as compo- itol Street, NW., suite 700, Washington, nents of the food-contact surface of DC 20408. any article that is subject to a regula- (2) Extractives limitations. The fol- tion in parts 174, 175, 176, 177, 178 and lowing extractives limitations are de- § 179.45 of this chapter, shall comply termined by the method described in with any specifications and limitations paragraph (d) of this section: prescribed by such regulation for the (i) Total extractives do not exceed article in the finished form in which it 0.03 weight-percent when extracted is to contact food. with water at 150 °F for 2 hours. (ii) Total extractives do not exceed [42 FR 14572, Mar. 15, 1977, as amended at 49 0.60 weight-percent when extracted FR 10110, Mar. 19, 1984] with n-heptane at 150 °F for 2 hours. (d) Analytical methods. The analytical § 177.1980 Vinyl chloride-propylene co- polymers. methods for determining total extrac- tives are applicable to the basic co- The vinyl chloride-propylene copoly- polymers in powder form having a par- mers identified in paragraph (a) of this ticle size such that 100 percent will section may be safely used as compo- pass through a U.S. Standard Sieve No. nents of articles intended for contact 40 and such that not more than 10 per- with food, subject to the provisions of cent will pass through a U.S. Standard this section. Sieve No. 200. (a) For the purpose of this section, (1) Reagents—(i) Water. All water used vinyl chloride-propylene copolymers in these procedures shall be consist of basic copolymers produced demineralized (deionized), freshly dis- by the copolymezation of vinyl chlo- tilled water. ride and propylene such that the fin- (ii) n-Heptane. Reagent grade, freshly ished basic copolymers meet the speci- distilled n-heptane shall be used. fications and extractives limitations (2) Determination of total amount of ex- prescribed in paragraph (c) of this sec- tractives. Place an accurately weighed tion, when tested by the methods de- sample of suitable size in a clean scribed in paragraph (d) of this section.
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(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 content is in the range of 53 to 56 per- (2) Determination of total amount of ex- cent as determined by any suitable an- tractives. All determinations shall be alytical procedure of generally accept- done in duplicate using duplicate ed applicability. blanks. Approximately 400 grams of (ii) Intrinsic viscosity in cyclo- sample (accurately weighed) shall be hexanone at 30 °C is not less than 0.50 placed in a 2-liter Erlenmeyer flask. deciliter per gram as determined by Add 1,200 milliliters of solvent and ASTM method D1243–79, ‘‘Standard cover the flask with aluminum foil. Test Method for Dilute Solution Vis- The covered flask and contents are sus- cosity of Vinyl Chloride Polymers,’’ pended in a thermostated bath and are ° which is incorporated by reference. kept, with continual shaking, at 150 F Copies may be obtained from the Amer- for 2 hours. The solution is then fil- ican Society for Testing Materials, 1916 tered through a No. 42 Whatman filter Race St., Philadelphia, PA 19103, or paper, and the filtrate is collected in a may be examined at the Office of the graduated cylinder. The total amount Federal Register, 800 North Capitol of filtrate (without washing) is meas- Street, NW., suite 700, Washington, DC ured and called A milliliters. The fil- 20408. trate is transferred to a Pyrex (or (2) Extractives limitations. The fol- equivalent) beaker and evaporated on a lowing extractives limitations are de- steam bath under a stream of nitrogen termined by the methods described in to a small volume (approximately 50–60 paragraph (d) of this section: milliliters). The concentrated filtrate (i) Total extractives do not exceed is then quantitatively transferred to a 0.10 weight-percent when extracted tared 100-milliliter Pyrex beaker using with n-heptane at 150 °F for 2 hours. small, fresh portions of solvent and a (ii) Total extractives do not exceed rubber policeman to effect the transfer. 0.03 weight-percent when extracted The concentrated filtrate is evaporated with water at 150 °F for 2 hours. almost to dryness on a hotplate under (iii) Total extractives obtained by ex- nitrogen, and is then transferred to a tracting with water at 150 °F for 2 drying oven at 230 °F in the case of the hours contain no more than 0.17 milli- aqueous extract or to a vacuum oven at gram of vinyl chloride-propylene co- 150 °F in the case of the heptane ex- polymer per 100 grams of sample tested tract. In the case of the aqueous ex- as determined from the organic chlo- tract the evaporation to constant rine content. For the purpose of this weight is completed in 15 minutes at section, the organic chlorine content is 230 °F; and in the case of heptane ex- the difference between the total chlo- tract, it is overnight under vacuum at rine and ionic chlorine contents deter- 150 °F. The residue is weighed and cor- mined as described in paragraph (d) of rected for the solvent blank. Calcula- this section. tion:
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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: in paragraph (d)(2) of this section. Two A=volume of filtrate obtained in extraction. drops of 50 percent by weight sodium B=milliliters of silver nitrate solution used hydroxide solution are added and the in sample titration×normality of silver solution is evaporated to approxi- nitrate solution. mately 150 milliliters. The solution is C=milliliters of silver nitrate solution used quantitatively transferred to a 250-mil- × in blank titration normality of silver ni- liliter beaker, methyl purple indicator trate solution. is added, and the solution is neutral- (iii) Ionic chlorine content. A weighed ized with 0.1 N nitric acid. For each 100 sample is extracted with water at 150 milliliters of solution is added 1.5 mil- °F for 2 hours, filtered, and the volume liliters of 2 N nitric acid. The solution of filtrate is measured (A milliliters) as is titrated with 0.005 N silver nitrate to
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the equivalence potential end point, section. A complete blank must be run using the expanded scale pH meter de- in duplicate. Calculation: scribed in paragraph (d)(3)(ii) of this
DE− 1, 200 milliliters Milliequivalents of ionic chlorine in × ×100 = Grams of sample Volume of filtrate aqueousextract of100 gramsof sample. A in milliliters
where: (f) The provisions of this section are A=volume of filtrate obtained in extraction. not applicable to vinyl chloride-pro- D=milliliters of silver nitrate solution used pylene copolymers used in food-pack- in sample titration×normality of silver aging adhesives complying with nitrate solution. § 175.105 of this chapter. E=milliliters of silver nitrate solution used in blank titration×normality of silver ni- [42 FR 14572, Mar. 15, 1977, as amended at 49 trate solution. FR 10111, Mar. 19, 1984] (iv) Organic chlorine content and vinyl § 177.1990 Vinylidene chloride/methyl chloride-propylene copolymer content of acrylate copolymers. aqueous extract. The organic chlorine The vinylidene chloride/methyl acry- content and the vinyl chloride pro- late copolymers (CAS Reg. No. 25038– pylene copolymer content of the aque- 72–6) identified in paragraph (a) of this ous extract is calculated as follows: section may be safely used as an article (a) Organic chlorine content. Milli- or as a component of an article in- equivalents of organic chlorine in tended for use in contact with food sub- aqueous extract of 100 grams of sample ject to the provisions of this section. equal milliequivalents of total chlorine (a) Identity. For the purposes of this in aqueous extract of 100 grams of sam- section vinylidene chloride/methyl ac- ple (as calculated in paragraph (d)(3)(ii) rylate copolymers consist of basic co- of this section) minus milliequivalents polymers produced by the copolym- of ionic chlorine in aqueous extract of erization of vinylidene chloride and 100 grams of sample (as calculated in methyl acrylate such that the copoly- paragraph (d)(3)(iii) of this section). mers contain not more than 15 weight- (b) Vinyl chloride-propylene copolymer percent of polymer units derived from content. Milligrams of vinyl chloride- methyl acrylate. propylene copolymer in aqueous ex- (b) Optional adjuvant substances. The tract of 100 grams of sample equal basic vinylidene chloride/methyl acry- milliequivalents of organic chlorine in late copolymers identified in paragraph aqueous extract of 100 grams of sample (a) of this section may contain optional (as calculated in paragraph (d)(3)(iv) (a) adjuvant substances required in the of this section) multiplied by 84.5. production of such basic copolymers. NOTE: The conversion factor, 84.5, is de- These optional adjuvant substances rived from the equivalent weight of chlorine may include substances permitted for divided by the chlorine content of the such use by regulations in parts 170 heptane extractable fraction.) through 179 of this chapter, substances (e) The vinyl chloride-propylene co- generally recognized as safe in food, polymers identified in and complying and substances used in accordance with with this section, when used as compo- a prior sanction or approval. nents of the food-contact surface of (c) Specifications. (1) The methyl acry- any article that is the subject of a reg- late content is determined by an infra- ulation in parts 174, 175, 176, 177, 178 red spectrophotometric method titled and § 179.45 of this chapter, shall com- ‘‘Determination of Copolymer Ratio in ply with any specifications and limita- Vinylidene Chloride/Methyl Acrylate tions prescribed by such regulation for Copolymers,’’ which is incorporated by the article in the finished form in reference. Copies are available from which it is to contact food. the Center for Food Safety and Applied
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Nutrition (HFS–200), Food and Drug Sieve No. 45 (350 microns) shall meet Administration, 200 C St. SW., Wash- the following extractives limitations: ington, DC 20204, or available for in- (1) 10-gram samples of the resin, spection at the Office of the Federal when extracted separately with 100 Register, 800 North Capitol Street, milliliters of distilled water at 121 °C NW., suite 700, Washington, DC 20408. (250 °F) for 2 hours, and 100 milliliters (2) The weight average molecular of n-heptane at 66 °C (150 °F) for 2 weight of the copolymer is not less hours, shall yield total nonvolatile ex- than 50,000 when determined by gel per- tractives not to exceed 0.5 percent by meation chromatography using tetra- weight of the resin. hydrofuran as the solvent. The gel per- (2) The basic copolymer in the form meation chromatograph is calibrated of film when extracted separately with ° ° with polystyrene standards. The basic distilled water at 121 C (250 F) for 2 gel permeation chromatographic meth- hours shall yield total nonvolatile ex- od is described in ANSI/ASTM D3536–76, tractives not to exceed 0.047 milligram ‘‘Standard Test Method for Molecular per square centimeter (0.3 milligram Weight Averages and Molecular Weight per square inch). (e) Conditions of use. The copolymers Distribution of Polystyrene by Liquid may be safely used as articles or com- Exclusion Chromatography (Gel Per- ponents of articles intended for use in meation Chromatography-GPC),’’ producing, manufacturing, processing, which is incorporated by reference. preparing, treating, packaging, trans- Copies are available from University porting, or holding food, including Microfilms International, 300 North processing of packaged food at tem- Zeeb Rd., Ann Arbor, MI 48106, or avail- peratures not to exceed 135 °C (275 °F). able for inspection at the Office of the (f) Other specifications and limitations. Federal Register, 800 North Capitol The vinylidene chloride-methyl acry- Street, NW., suite 700, Washington, DC late copolymers identified in and com- 20408. plying with this section, when used as (3) Residual vinylidene chloride and components of the food contact surface residual methyl acrylate in the copoly- of any article that is subject to a regu- mer in the form in which it will con- lation in parts 174 through 178 and tact food (unsupported film, barrier § 179.45 of this chapter, shall comply layer, or as a copolymer for blending) with any specifications and limitations will not exceed 10 parts per million and prescribed by such regulation for the 5 parts per million, respectively, as de- article in the finished form in which it termined by either a gas is to contact food. chromatographic method titled ‘‘De- termination of Residual Vinylidene [48 FR 38605, Aug. 25, 1983; 48 FR 50077, Oct. Chloride and Methyl Acrylate in Vinyl- 31, 1983, as amended at 53 FR 47185, Nov. 22, 1988; 54 FR 24898, June 12, 1989] idene Chloride/Methyl Acrylate Co- polymer Resins and Films,’’ or, alter- § 177.2000 Vinylidene chloride/methyl natively, ‘‘Residual Methyl Acrylate acrylate/methyl methacrylate poly- and Vinylidene Chloride Monomers in mers. Saran MA/VDC Resins and Pellets by The vinylidene chloride/methyl acry- Headspace Gas Chromatography,’’ late/methyl methacrylate polymers dated March 3, 1986, which are incor- (CAS Reg. No. 34364–83–5) identified in porated by reference in accordance paragraph (a) of this section may be with 5 U.S.C. 552(a). Copies are avail- safely used as articles or as a compo- able from the Center for Food Safety nent of articles intended for use in con- and Applied Nutrition (HFS–200), Food tact with food subject to the provisions and Drug Administration, 200 C St. of this section. SW., Washington, DC 20204, or available (a) Identity. For the purpose of this for inspection at the Office of the Fed- section, vinylidene chloride/methyl ac- eral Register, 800 North Capitol Street, rylate/methyl methacrylate polymers NW., suite 700, Washington, DC 20408. consist of basic polymers produced by (d) Extractives limitations. The basic the copolymerization of vinylidene copolymer resin in the form of granules chloride/methyl acrylate/methyl meth- that will pass through a U.S. Standard acrylate such that the basic polymers
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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 rived from methyl acrylate monomer with food, subject to the provisions of and not more than 6 weight percent of this section. polymer units derived from methyl (a) Ethylene polymer, chloro- methacrylate monomer. sulfonated is produced by chloro- (ii) The basic polymers are limited to sulfonation of a carbon tetrachloride a thickness of not more than 0.005 cen- solution of polyethylene with chlorine timeter (0.002 inches). and sulfuryl chloride. (2) The weight average molecular (b) Ethylene polymer, chloro- weight of the basic polymer is not less sulfonated shall meet the following than 100,000 when determined by gel specifications: permeation chromatography using tet- (1) Chlorine not to exceed 25 percent rahydrofuran as the solvent. The gel by weight. permeation chromatography is cali- (2) Sulfur not to exceed 1.15 percent brated with polystyrene standards. The by weight. basic gel permeation chromatographic (3) Molecular weight is in the range method is described in ANSI/ASTM of 95,000 to 125,000. D3536–76, which is incorporated by ref- erence. Copies are available from the Methods for the specifications in this American Society for Testing Mate- paragraph (b), titled ‘‘Chlorine and rials, 1916 Race St., Philadelphia, PA Bromine—Coulometric Titration Meth- 19103, or available for inspection at the od by Aminco Chloridometer,’’ Office of the Federal Register, 800 ‘‘Hypolon Synthetic Rubber—Deter- North Capitol Street, NW., suite 700, mination of Sulfur by Parr Bomb,’’ and Washington, DC 20408. ASTM method D2857–70 (Reapproved
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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 be examined at the Office of the Fed- tial microbial adulteration of the food. eral Register, 800 North Capitol Street, (g) To assure safe use of the micro- NW., suite 700, Washington, DC 20408. porous polymeric filters, the label or (c) The additive is used as the article, labeling shall include adequate direc- or a component of articles, intended for tions for a pre-use treatment, con- use as liners and covers for reservoirs sisting of washing with a minimum of intended for the storage of water for 2 gallons of potable water at a tem- drinking purposes. perature of 180 °F for each square foot (d) Substances permitted by § 177.2600 of filter, prior to the filter’s first use in may be employed in the preparation of contact with food. ethylene polymers, chlorosulfonated, subject to any limitations prescribed [42 FR 14572, Mar. 15, 1977, as amended at 56 therein. FR 42933, Aug. 30, 1991] (e) The finished ethylene copolymers, § 177.2260 Filters, resin-bonded. chlorosulfonated shall conform to § 177.2600(e) and (g). Resin-bonded filters may be safely used in producing, manufacturing, [42 FR 14572, Mar. 15, 1977, as amended at 49 FR 10111, Mar. 19, 1984; 54 FR 24898, June 12, processing, and preparing food, subject 1989] to the provisions of this section. (a) Resin-bonded filters are prepared § 177.2250 Filters, microporous poly- from natural or synthetic fibers to meric. which have been added substances re- Microporous polymeric filters identi- quired in their preparation and fin- fied in paragraph (a) of this section ishing, and which are bonded with res- may be safely used, subject to the pro- ins prepared by condensation or polym- visions of this section, to remove par- erization of resin-forming materials, ticles of insoluble matter in producing, together with adjuvant substances re- manufacturing, processing, and pre- quired in their preparation, applica- paring bulk quantities of liquid food. tion, and curing. (a) Microporous polymeric filters (b) The quantity of any substance consist of a suitably permeable, contin- employed in the production of the uous, polymeric matrix of polyvinyl resin-bonded filter does not exceed the chloride, vinyl chloride-propylene, or amount reasonably required to accom- vinyl chloride-vinyl acetate, in which plish the intended physical or technical finely divided silicon dioxide is embed- effect or any limitation further pro- ded. Cyclohexanone may be used as a vided. solvent in the production of the filters. (b) Any substance employed in the (c) Any substance employed in the production of microporous polymeric production of resin-bonded filters that filters that is the subject of a regula- is the subject of a regulation in parts tion in parts 170 through 189 of this 174, 175, 176, 177, 178 and § 179.45 of this chapter must conform with any speci- chapter conforms with any specifica- fication in such regulation. tion in such regulation. (c) Cyclohexanone when used as a sol- (d) Substances employed in the pro- vent in the production of the filters duction of resin-bonded filters include shall not exceed 0.35 percent by weight the following, subject to any limita- of the microporous polymeric filters. tions provided:
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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 percent of total polymer units derived Cellulose pulp. 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. BHT. Melamine-formaldehyde chemically modified Butyl (or isobutyl) palmitate or stearate. with urea; for use only as provided for in 2,5-Di-tert-butyl hydroquinone for use only in paragraphs (e), (f), (g), (h), and (i) of this lubricant formulations for rayon fiber fin- section. ishing and at a usage level not to exceed Phenol-formaldehyde resins. 0.1 percent by weight of the lubricant for- Polyvinyl alcohol. mulations. Polyvinyl alcohol with the copolymer of Dimethylpolysiloxane. acrylic acid-allyl sucrose. 4-Ethyl-4-hexadecyl morpholinium ethyl sul- Polyvinyl alcohol with melamine formalde- fate for use only as a lubricant in the man- hyde. ufacture of polyethylene terephthalate fi- Polyvinyl acetate with melamine formalde- bers specified in paragraph (d)(1) of this hyde. section at a level not to exceed 0.03 percent p--Toluenesulfonamide-formaldehyde chemi- by weight of the finished fibers. cally modified with one or more of the Fatty acid (C10-C18) diethanolamide conden- amine catalysts identified in § 175.300 sates. (b)(3)(xiii) of this chapter. Fatty acids derived from animal or vegetable fats and oils, and salts of such acids, sin- (4) Adjuvant substances: gle or mixed, as follows: Aluminum. Dimethyl polysiloxane with methylcellulose Ammonium. and sorbic acid (as an antifoaming agent). Calcium. Phosphoric acid. Magnesium. Potassium. (5) Colorants: Colorants used in ac- Sodium. cordance with § 178.3297 of this chapter. Triethanolamine. (e) Resin-bonded filters conforming Fatty acid (C10-C18) mono- and diesters of with the specifications of paragraph (e) polyoxyethylene glycol (molecular weight (1) of this section are used as provided 400–3,000). in paragraph (e)(2) of this section: Methyl esters of fatty acids (C10-C18). Mineral oil. (1) Total extractives. The finished fil- Polybutene, hydrogenated; complying with ter, when exposed to distilled water at the identity prescribed under § 178.3740 (b) 100 °F for 2 hours, yields total extrac- of this chapter. tives not to exceed 2.8 percent by Polyoxyethylene (4 mols) ethylenediamine weight of the filter. monolauramide for use only in lubricant formulations for rayon fiber finishing and (2) Conditions of use. It is used to fil- at a usage level not to exceed 10 percent by ter milk or potable water at operating weight of the lubricant formulations. temperatures not to exceed 100 °F. Ricebran oil. (f) Resin-bonded filters conforming Titanium dioxide. with the specifications of paragraph (f) (3) Resins: (1) of this section are used as provided in paragraph (e)(2) of this section: Acrylic polymers produced by polymerizing (1) Total extractives. The finished fil- ethyl acrylate alone or with one or more of the monomers: Acrylic acid, acrylonitrile, ter, when exposed to distilled water at N-methylolacrylamide, and styrene. The 145 °F for 2 hours, yields total extrac- finished copolymers shall contain at least tives not to exceed 4 percent by weight 70 weight percent of polymer units derived of the filter.
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(2) Conditions of use. It is used to fil- (1) of this section are used as provided ter milk or potable water at operating in paragraph (k)(2) of this section: temperatures not to exceed 145 °F. (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 nonalcoholic, aqueous foods having a °F, provided that the finished filter pH above 5.0. when exposed to distilled water at 100 (j) Resin-bonded filters conforming °F for 2 hours yields total extractives with the specifications of paragraph (j) not to exceed 1 percent by weight of (1) of this section are used as provided the filter. in paragraph (j)(2) of this section: (2) The finished filter may be used to (1) Total extractives. The finished fil- filter milk or potable water at oper- ter, when exposed to 5 percent (by ating temperatures not to exceed 145 weight) acetic acid for 2 hours at a °F, provided that the finished filter temperature equivalent to, or higher when exposed to distilled water at 145 than, the filtration temperature of the °F for 2 hours yields total extractives aqueous food, yields total extractives not to exceed 1.2 percent by weight of not to exceed 4 percent, by weight, of the filter. the filter. (2) Conditions of use. It is used in com- (n) Acrylonitrile copolymers identi- mercial filtration of bulk quantities of fied in this section shall comply with nonalcoholic, aqueous foods having a the provisions of § 180.22 of this chap- pH of 5.0 or below. ter. (k) Resin-bonded filters conforming [42 FR 14572, Mar. 15, 1977, as amended at 56 with the specifications of paragraph (k) FR 42933, Aug. 30, 1991]
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§ 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. weight of titanium dioxide as an op- (b) The resin may contain one or tional adjuvant substance. more of the following optional sub- (c) The mineral reinforced nylon res- stances provided the quantity used ins with or without the optional sub- does not exceed that reasonably re- stance described in paragraph (b) of 1 quired to accomplish the intended ef- this section, and in the form of ⁄8-inch fect: molded test bars, when extracted with the solvents, i.e., distilled water and 50 Allyl glycidyl ether ...... As curing system additive. percent (by volume) ethyl alcohol in Di- and tri-glycidyl ester mix- As modifier at levels not to distilled water, at reflux temperature ture resulting from the re- exceed equal parts by for 24 hours using a volume-to-surface action of epichlorohydrin weight of the 4,4′- with mixed dimers and isopropylidenediphenol- ratio of 2 milliliters of solvent per trimers of unsaturated C18 epichlorohydrin basic resin square inch of surface tested, shall monobasic fatty acids de- and limited to use in con- meet the following extractives limita- rived from animal and veg- tact with alcoholic bev- tions: etable fats and oils. erages containing not more than 8 percent of alcohol. (1) Total extractives not to exceed 5.0 1,2-Epoxy-3-phenoxypropane As curing system additive. milligrams per square inch of food-con- Glyoxal ...... Do. tact surface tested for each solvent. ′ 4,4 -Isopropylidenediphenol ... Do. (2) The ash after ignition of the ex- 4,4′-Methylenedianiline ...... Do. m-Phenylenediamine ...... Do. tractives described in paragraph (c)(1) Tetrahydrophthalic anhydride Do. of this section, not to exceed 0.5 milli- gram per square inch of food-contact (c) In accordance with good manufac- surface tested. turing practice, finished articles con- (d) In accordance with good manufac- taining the resins shall be thoroughly turing practice, finished articles con- cleansed prior to their first use in con- taining the mineral reinforced nylon tact with food. resins shall be thoroughly cleansed (d) The provisions of this section are prior to their first use in contact with not applicable to 4,4′-isopropylidenedi- food. phenol-epichlorohydrin resins listed in other sections of parts 174, 175, 176, 177, [42 FR 54533, Oct. 7, 1977, as amended at 42 FR 61594, Dec. 6, 1977] 178 and 179 of this chapter. [42 FR 14572, Mar. 15, 1977; 49 FR 5748, Feb. 15, § 177.2400 Perfluorocarbon cured 1984] elastomers. Perfluorocarbon cured elastomers § 177.2355 Mineral reinforced nylon identified in paragraph (a) of this sec- resins. tion may be safely used as articles or Mineral reinforced nylon resins iden- components of articles intended for re- tified in paragraph (a) of this section peated use in contact with nonacid may be safely used as articles or com- food (pH above 5.0), subject to the pro- ponents of articles intended for re- visions of this section. peated use in contact with nonacidic (a) Identity. (1) For the purpose of food (pH above 5.0) and at use tempera- this section, perfluorocarbon cured tures not exceeding 212 °F. in accord- elastomers are produced by
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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- (trifluoromethyl)-ethylidene] bis- Model 1099 with Model 951 TGA unit or ,dipotassium salt—not to exceed 5 parts. the equivalent. 1,4,7,10,13,16-Hexaoxacyclo-octadecane—not (d) Extractive limitations. Articles fab- to exceed 5 parts. ricated from perfluorocarbon cured 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: (1) Substances generally recognized as safe (GRAS) in food or food pack- (1) Total extractives not to exceed 3.1 aging. milligrams per square decimeter (0.2 (2) Substances used in accordance milligrams per square inch). with a prior sanction. (2) Fluoride extractives calculated as (3) Substances authorized under ap- fluorine not to exceed 0.47 milligram plicable regulations in this part and in per square decimeter (0.03 milligram parts 175 and 178 of this chapter and per square inch). subject to any limitations prescribed (e) Conditions of use. In accordance therein. with current good manufacturing prac- (4) Substances identified in this para- tice, finished food contact articles con- graph (b)(4) subject to such limitations taining the perfluorocarbon cured as are provided: elastomers shall be thoroughly cleaned prior to their first use in contact with Substances Limitations food.
Carbon black (channel proc- Not to exceed 15 parts per [49 FR 43050, Oct. 26, 1984] ess of furnace combustion 100 parts of the process) (CAS Reg. No. terpolymer. § 177.2410 Phenolic resins in molded 1333±86±4). Magnesium oxide (CAS Reg. Not to exceed 5 parts per articles. No. 1309±48±4). 100 parts of the Phenolic resins identified in this sec- terpolymer. tion may be safely used as the food-
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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 Poly(aryletherketone) resins identi- this section, with or without aniline fied in paragraph (a) of this section and/or anhydro-formaldehyde aniline may be safely used as articles or com- (hexahydro-1, 3,5-triphenyl-s-triazine): ponents of articles intended for re- (1) Phenols: peated use in contact with food subject p-tert-Amylphenol. to the provisions of this section. p-tert-Butylphenol. (a) Identity. For the purposes of this o-, m-, and p-Cresol. section, poly(aryletherketone) resins p-Octylphenol. are poly(p-oxyphenylene p- Phenol. 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 have a minimum weight-average mo- (2) Aldehydes: lecular weight of 12,000, as determined Acetaldehyde. by gel permeation chromatography in Formaldehyde. comparison with polystyrene stand- Paraldehyde. 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) may contain optional adjuvant sub- Asbestos fiber. stances used in their production. These Barium hydroxide ...... For use as catalyst. Calcium stearate ...... For use as lubricant. adjuvants may include substances de- Carbon black (channel proc- scribed in § 174.5(d) of this chapter and ess). the following: Diatomaceous earth. Glass fiber. Hexamethylenetetramine ...... For use as curing agent. Mica. Oxalic acid ...... For use as catalyst. Substance Limitations Zinc stearate ...... For use as lubricant. Diphenyl sulfone ...... Not to exceed 0.2 percent by weight as a residual (c) The finished food-contact article, solvent in the finished when extracted with distilled water at basic resin. reflux temperature for 2 hours, using a volume-to-surface ratio of 2 milliliters (c) Extractive limitations. The finished of distilled water per square inch of food contact article, when extracted at surface tested, shall meet the following reflux temperatures for 2 hours with extractives limitations: the following four solvents, yields in (1) Total extractives not to exceed each extracting solvent net chloroform 0.15 milligram per square inch of food- soluble extractives not to exceed 0.05 contact surface. milligrams per square inch of food con- (2) Extracted phenol not to exceed tact surface: Distilled water, 50 percent 0.005 milligram per square inch of food- (by volume) ethanol in distilled water, contact surface. 3 percent acetic acid in distilled water, (3) No extracted aniline when tested and n-heptane. In testing the final food by a spectrophotometric method sen- contact article, a separate test sample
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shall be used for each extracting sol- Ethylene glycol. vent. Glycerol. 4,4′-Isopropylidenediphenol-epichlorohydrin. [63 FR 20315, Apr. 24, 1998] Mannitol. a-Methyl glucoside. § 177.2420 Polyester resins, cross- Pentaerythritol. linked. Polyoxypropylene ethers of 4,4′-isopropylide- Cross-linked polyester resins may be nediphenol (containing an average of 2–7.5 safely used as articles or components moles of propylene oxide). of articles intended for repeated use in Propylene glycol. contact with food, in accordance with Sorbitol. Trimethylol ethane. the following prescribed conditions: Trimethylol propane. (a) The cross-linked polyester resins 2,2,4-Trimethyl-1,3-pentanediol. are produced by the condensation of one or more of the acids listed in para- (3) Cross-linking agents: graph (a)(1) of this section with one or Butyl acrylate. more of the alcohols or epoxides listed Butyl methacrylate. in paragraph (a)(2) of this section, fol- Ethyl acrylate. lowed by copolymerization with one or Ethylhexyl acrylate. more of the cross-linking agents listed Methyl acrylate. in paragraph (a)(3) of this section: Methyl methacrylate. (1) Acids: Styrene. Triglycidyl isocyanurate (CAS Reg. No. 2451– Adipic. 62–9), for use only in coatings contacting Fatty acids, and dimers thereof, from nat- bulk quantities of dry food of the type ural sources. identified in § 176.170(c) of this chapter, Fumaric. table 1, under type VIII. Isophthalic. Vinyl toluene. Maleic. Methacrylic. (b) Optional adjuvant substances em- Orthophthalic. ployed to facilitate the production of Sebacic. the resins or added thereto to impart Terephthalic. desired technical or physical properties Trimellitic. include the following, provided that (2) Polyols and polyepoxides: the quantity used does not exceed that Butylene glycol. reasonably required to accomplish the Diethylene glycol. intended physical or technical effect 2,2-Dimethyl-1,3-propanediol. and does not exceed any limitations Dipropylene glycol. 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. 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. 818±08±6) ...... For use in the polycondensation reaction at levels not to ex- ceed 0.2 percent of the polyester resin. Dicumyl peroxide.
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Limitations (limits of addition expressed as percent by weight List of substances of finished resin)
Hydroxybutyltin oxide (CAS Reg. No. 2273±43±0) ...... 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. 23850± For use in the polycondensation reaction at levels not to ex- 94±4). 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, ins shall be thoroughly cleansed prior with or without the optional sub- to their first use in contact with food. stances described in paragraph (b) of [42 FR 14572, Mar. 15, 1977, as amended at 48 this section, and in the finished form in FR 37618, Aug. 19, 1983; 54 FR 48858, Nov. 28, which they are to contact food, when 1989] extracted with the solvent or solvents characterizing the type of food and § 177.2430 Polyether resins, under the conditions of time and tem- chlorinated. perature characterizing the conditions Chlorinated polyether resins may be of their intended use, as determined safely used as articles or components from tables 1 and 2 of § 176.170(c) of this of articles intended for repeated use in chapter, shall meet the following ex- producing, manufacturing, packing, tractives limitations: processing, preparing, treating, pack- (1) Net chloroform-soluble extrac- aging, transporting, or holding food, in tives not to exceed 0.1 milligram per accordance with the following pre- square inch of food-contact surface scribed conditions: tested when the prescribed food-simu- (a) The chlorinated polyether resins lating solvent is water or 8 or 50 per- are produced by the catalytic polym- cent alcohol. erization of 3,3-bis(chloromethyl)- (2) Total nonvolatile extractives not oxetane, and shall contain not more to exceed 0.1 milligram per square inch than 2 percent residual monomer. of food-contact surface tested when the (b) In accordance with good manufac- prescribed food-simulating solvent is turing practice, finished articles con- taining the chlorinated polyether res- heptane. ins shall be thoroughly cleansed prior (d) In accordance with good manufac- to their first use in contact with food. turing practice, finished articles con- taining the cross-linked polyester res- § 177.2440 Polyethersulfone resins. Polyethersulfone resins identified in paragraph (a) of this section may be
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safely used as articles or components inch of food-contact surface: distilled of articles intended for repeated use in water, 50 percent (by volume) ethyl al- contact with food in accordance with cohol in distilled water, 3 percent ace- the following prescribed conditions: tic acid in distilled water, and n- (a) For the purpose of this section, heptane. (Note: In testing the finished polyethersulfone resins are: food-contact article, use a separate (1) Poly(oxy-p-phenylenesulfonyl-p- test sample for each required extract- phenylene) resins (CAS Reg. No. 25667– ing solvent.) 42–9), which have a minimum number (d) In accordance with good manufac- average molecular weight of 16,000. turing practice, finished food-contact (2) 1,1′-sulfonylbis[4-chlorobenzene] articles containing the polymer with 4,4′-(1-methylethyl- polyethersulfone resins shall be thor- idene)bis[phenol] (maximum 8 percent) oughly cleansed before their first use and 4,4′-sulfonylbis[phenol] (minimum in contact with food. 92 percent) (CAS Reg. No. 88285–91–0), which have a minimum number aver- [44 FR 34493, June 15, 1979, as amended at 47 FR 38885, Sept. 3, 1982; 49 FR 10111, Mar. 19, age molecular weight of 26,000. 1984; 50 FR 47211, Nov. 15, 1985; 60 FR 48648, (3) In paragraphs (a)(1) and (a)(2) of Sept. 20, 1995] this section, the minimum number av- erage molecular weight is determined § 177.2450 Polyamide-imide resins. by reduced viscosity in dimethyl form- Polyamide-imide resins identified in amide in accordance with ASTM meth- paragraph (a) of this section may be od D2857–70 (Reapproved 1977), ‘‘Stand- safely used as components of articles ard Test Method for Dilute Solution intended for repeated use in contact Viscosity of Polymers,’’ which is incor- with food, in accordance with the fol- porated by reference. Copies may be lowing prescribed conditions: obtained from the American Society (a) Identity. (1) For the purpose of for Testing Materials, 1916 Race St., this section the polyamide-imide resins Philadelphia, PA 19103, or may be ex- are derived from the condensation re- amined at the Division of Petition Con- action of substantially equimolar parts trol (HFS–215), Center for Food Safety of trimellitic anhydride and p,p′- and Applied Nutrition, 1110 Vermont diphenylmethane diisocyanate. Ave. NW., suite 1200, Washington, DC, (2) The polyamide-imide resins (CAS or at the Office of the Federal Register, Reg. No. 31957–38–7) derived from the 800 North Capitol St. NW., suite 700, condensation reaction of equimolar Washington, DC. parts of benzoyl chloride-3,4- (b) The basic resins identified in dicarboxylic anhydride and 4,4′- paragraphs (a)(1) and (a)(2) of this sec- diphenylmethanediamine. tion may contain optional adjuvant (b) Specifications. (1) Polyamide-imide substances described in § 174.5(d) of this resins identified in paragraph (a)(1) of chapter and the following: this section shall have a nitrogen con- List of substances Limitations tent of not less than 7.8 weight percent and not more than 8.2 weight percent. Diphenylsulfone ...... Not to exceed 0.2 percent as re- Polyamide-imide resins identified in sidual solvent in the finished basic resin described in para- paragraph (a)(2) of this section shall graph (a)(1) of this section. have a nitrogen content of not less Dimethyl sulfoxide ...... Not to exceed 0.01 percent as than 7.5 weight percent and not more residual solvent in the finished basic resin described in para- than 7.8 weight percent. Nitrogen con- graph (a)(1) of this section. tent is determined by the Dumas Nitro- N-methyl-2-pyrrolidone ..... Not to exceed 0.01 percent as gen Determination as set forth in the residual solvent in the finished basic resin described in para- ‘‘Official Methods of Analysis of the graph (a)(2) of this section. Association of Official Analytical Chemists,’’ 13th Ed. (1980), sections (c) The finished food-contact article, 7.016–7.020, which is incorporated by when extracted at reflux temperatures reference in accordance with 5 U.S.C. for 2 hours with the following four sol- 552(a). Copies may be obtained from the vents, yields net chloroform-soluble ex- Association of Official Analytical tractives in each extracting solvent Chemists International, 481 North not to exceed 0.02 milligram per square Frederick Ave., suite 500, Gaithersburg,
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MD 20877–2504, or may be examined at steel plates, exposed to the respective the Office of the FEDERAL REGISTER, food simulating solvents. The resin 800 North Capitol Street, NW., suite shall meet the following extractive 700, Washington, DC. limitations under the corresponding (2) Polyamide-imide resins identified extraction conditions: in paragraph (a)(1) of this section shall (1) Distilled water at 250 °F for 2 have a solution viscosity of not less hours: Not to exceed 0.01 milligram per than 1.200. Polyamide-imide resins square inch. identified in paragraph (a)(2) of this (2) Three percent acetic acid at 212 °F section shall have a solution viscosity for 2 hours: Not to exceed 0.05 milli- of not less than 1.190. Solution vis- gram per square inch. cosity shall be determined by a method (3) Fifty percent ethyl alcohol at 160 titled ‘‘Solution Viscosity’’ which is in- °F for 2 hours: Not to exceed 0.03 milli- corporated by reference in accordance gram per square inch. with 5 U.S.C. 552(a). Copies are avail- ° 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- [42 FR 14572, Mar. 15, 1977, as amended at 47 diphenylmethane diisocyanate should FR 11845, Mar. 19, 1982; 49 FR 10111, Mar. 19, not be present at greater than 100 parts 1984; 54 FR 24898, June 12, 1989; 54 FR 43170, per million and trimellitic anhydride Oct. 23, 1989; 61 FR 14481, Apr. 2, 1996] should not be present at greater than 500 parts per million. Residual mono- § 177.2460 Poly(2,6-dimethyl-1,4-phen- mers are determined by gas chroma- ylene) oxide resins. tography (the gas chromatography The poly(2,6-dimethyl-1,4-phenylene) method titled ‘‘Amide-Imide Polymer oxide resins identified in paragraph (a) Analysis—Analysis of Monomer Con- of this section may be used as an arti- tent,’’ is incorporated by reference in cle or as a component of an article in- accordance with 5 U.S.C. 552(a). Copies tended for use in contact with food sub- are available from the Center for Food ject to the provisions of this section. Safety and Applied Nutrition (HFS– (a) Identity. For the purposes of this 200), Food and Drug Administration, section, poly(2,6-dimethyl-1,4-phen- 200 C St. SW., Washington, DC 20204, or available for inspection at the Office of ylene) oxide resins consist of basic res- the Federal Register, 800 North Capitol ins produced by the oxidative coupling Street, NW., suite 700, Washington, of 2,6-xylenol such that the finished DC). basic resins meet the specifications (c) Extractive limitations are appli- and extractives limitations prescribed cable to the polyamide-imide resins in paragraph (c) of this section. identified in paragraphs (a) (1) and (2) (b) Optional adjuvant substances. The of this section in the form of films of 1 basic poly(2,6-dimethyl-1,4-phenylene) mil uniform thickness after coating oxide resins identified in paragraph (a) and heat curing at 600 °F for 15 minutes of this section may contain optional on stainless steel plates, each having adjuvant substances required in the such resin-coated surface area of 100 production of such basic resins. The op- square inches. The cured-resin film tional adjuvant substances required in coatings shall be extracted in accord- the production of the basic poly(2,6-di- ance with the method described in methyl-1,4-phenylene) oxide resins may § 176.170(d)(3) of this chapter, using a include substances permitted for such plurality of spaced, coated stainless use by regulations in parts 170 through
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189 of this chapter, substances gen- c=Concentration of solution in terms of erally recognized as safe in food, sub- grams per deciliter. stances used in accordance with a prior (2) Extractives limitations. Total resin sanction or approval, and the fol- extracted not to exceed 0.02 weight-per- lowing: cent when extracted with n-heptane at Limitations (expressed as 160 °F for 2 hours as determined using List of substances percent by weight of finished 200 milliliters of reagent grade n- basic resin) heptane which has been freshly dis- Diethylamine ...... Not to exceed 0.16 percent tilled before use and 25 grams of poly as residual catalyst. (2,-6-dimethyl-1,4-phenylene) oxide Methyl alcohol ...... Not to exceed 0.02 percent as residual solvent. resin. The resin as tested is in pellet Toluene ...... Not to exceed 0.2 percent as form having a particle size such that residual solvent. 100 percent of the pellets will pass through a U.S. Standard Sieve No. 6 (c) Specifications and extractives limita- and 100 percent of the pellets will be tions. The poly(2,6-dimethyl-1,4-phen- held on a U.S. Standard Sieve No. 10. ylene) oxide basic resins meet the fol- (d) Other limitations. The poly(2,6-di- lowing: methyl-1,4-phenylene) oxide resins (1) Specifications. Intrinsic viscosity identified in and complying with this is not less than 0.30 deciliter per gram section, when used as components of as determined by ASTM method D1243– the food-contact surface of any article 79, ‘‘Standard Test Method for Dilute that is the subject of a regulation in Solution Viscosity of Vinyl Chloride parts 174, 175, 176, 177, 178 and § 179.45 of Polymers,’’ which is incorporated by this chapter, shall comply with any reference, modified as follows. Copies specifications and limitations pre- of the incorporation by reference may scribed by such regulation for the arti- be obtained from the American Society cle in the finished form in which it is for Testing Materials, 1916 Race St., to contact food. Philadelphia, PA 19103, or may be ex- (e) Uses. The poly(2,6-dimethyl-1,4- amined at the Office of the Federal phenylene) oxide resins identified in Register, 800 North Capitol Street, and complying with the limitations in NW., suite 700, Washington, DC 20408. this section may be used as articles or (i) Solvent: Chloroform, reagent grade components of articles intended for re- containing 0.01 percent tert- peated food-contact use or as articles butylcatechol. (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 (iii) Viscometer: Cannno-Ubbelohde se- § 176.170(c) of this chapter, table 2, con- ries 25 dilution viscometer (or equiva- ditions of use H. lent). [42 FR 14572, Mar. 15, 1977, as amended at 49 (iv) Calculation: The calculation FR 10111, Mar. 19, 1984; 63 FR 8852, Feb. 23, method used is that described in appen- 1998] dix X.1.3 (ASTM method D1243–79, cited and incorporated by reference in para- § 177.2465 Polymethylmethacrylate/ graph (c)(1) of this section) with the re- poly(trimethoxysilylpropyl)meth- duced viscosity determined for three acrylate copolymers. concentration levels (0.4, 0.2, and 0.1 Polymethylmethacrylate/ gram per deciliter) and extrapolated to poly(trimethoxysilylpropyl) methacry- zero concentration for intrinisic vis- late copolymers (CAS Reg. No. 26936– cosity. The following formula is used 30–1) may be safely used as components for determining reduced viscosity: of surface primers used in conjunction with silicone polymers intended for re- − Reduced viscosity in terms = t to peated use and complying with § 175.300 of deciliters per gram × of this chapter and § 177.2600, in accord- to c ance with the following prescribed con- where: ditions. t=Solution efflux time. (a) Identity. For the purpose of this to=Solvent efflux time. section, polymethylmethacrylate/
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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- not to exceed 6.0 percent by weight of phenol). the primer formulation. Nylon 6/66, weight ratio 2/3. (2) The copolymers may be used in Tetrakis [methylene (3,5-di-tert-butyl-4- food contact applications with all food hydroxyhydrocinnamate)] methane. 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- [59 FR 5948, Feb. 9, 1994] ylene copolymer can be identified by its characteristic infrared spectrum. § 177.2470 Polyoxymethylene copoly- (2) Minimum number average molec- mer. ular weight of the copolymer is 15,000 Polyoxymethylene copolymer identi- as determined by a method titled fied in this section may be safely used ‘‘Number Average Molecular Weight,’’ as an article or component of articles which is incorporated by reference. intended for food-contact use in ac- Copies are available from the Center cordance with the following prescribed for Food Safety and Applied Nutrition conditions: (HFS–200), Food and Drug Administra- (a) Identity. For the purpose of this tion, 200 C St. SW., Washington, DC section, polyoxymethylene copolymers 20204, or available for inspection at the are identified as the following: The re- Office of the Federal Register, 800 action product of trioxane (cyclic North Capitol Street, NW., suite 700, trimer of formaldehyde) and ethylene Washington, DC 20408. oxide (CAS Reg. No. 24969–25–3) or the (d) Extractive limitations. (1) Polyoxy- reaction product of trioxane (cyclic methylene copolymer in the finished trimer of formaldehyde) and a max- form in which it is to contact food, imum of 5 percent by weight of when extracted with the solvent or sol- butanediol formal (CAS Reg. No. 25214 vents characterizing the type of food 85–1). Both copolymers may have cer- and under conditions of time and tem- tain optional substances added to im- perature as determined from tables 1 part desired technological properties to and 2 of § 175.300(d) of this chapter, the copolymer. shall yield net chloroform-soluble ex- (b) Optional adjuvant substances. The tractives not to exceed 0.5 milligram polyoxymethylene copolymer identi- per square inch of food-contact surface. fied in paragraph (a) of this section (2) Polyoxymethylene copolymer may contain optional adjuvant sub- with or without the optional sub- stances required in its production. The stances described in paragraph (b) of quantity of any optional adjuvant sub- this section, when ground or cut into stance employed in the production of particles that pass through a U.S.A. the copolymer does not exceed the Standard Sieve No. 6 and that are re- amount reasonably required to accom- tained on a U.S.A. Standard Sieve No. plish the intended technical or physical 10, shall yield total extractives as fol- effect. Such adjuvants may include lows: substances generally recognized as safe (i) Not to exceed 0.20 percent by in food, substances used in accordance weight of the copolymer when ex- with prior sanction, substances per- tracted for 6 hours with distilled water mitted under applicable regulations in at reflux temperature. parts 170 through 189 of this chapter, (ii) Not to exceed 0.15 percent by and the following: weight of the copolymer when ex- (1) Stabilizers (total amount of stabi- tracted for 6 hours with n-heptane at lizers not to exceed 2.0 percent and reflux temperature.
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(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- (2) Use temperature shall not exceed 35074±77±2). cles shall not be used for ° 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 turing practice, finished articles con- tert-butylphenol). percent by weight of 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 be identified by its characteristic in- accordance with the following pre- frared spectrum. scribed conditions: (2) Minimum number average molec- (a) Identity. For the purpose of this ular weight of the homopolymer is section, polyoxymethylene homopoly- 25,000. mer is polymerized formaldehyde (3) Density of the homopolymer is be- [Chemical Abstracts Service Registry tween 1.39 and 1.44 as determined by No. 9002–81–7]. Certain optional adju- ASTM method D1505–68 (Reapproved vant substances, described in para- 1979), ‘‘Standard Test Method for Den- graph (b) of this section, may be added sity of Plastics by the Density-Gra- to impart desired technological prop- dient Technique,’’ which is incor- erties to the homopolymer. porated by reference. Copies may be (b) Optional adjuvant substances. The obtained from the American Society polyoxymethylene homopolymer iden- for Testing Materials, 1916 Race St., tified in paragraph (a) of this section Philadelphia, PA 19103, or may be ex- may contain optional adjuvant sub- amined at the Office of the Federal stances in its production. The quantity Register, 800 North Capitol Street, of any optional adjuvant substance em- NW., suite 700, Washington, DC 20408. ployed in the production of the (4) Melting point is between 172 °C homopolymer does not exceed the and 184 °C as determined by ASTM amount reasonably required to accom- method D2133–66, ‘‘Specifications for plish the intended effect. Such adju- Acetal Resin Injection Molding and Ex- vants may include substances gen- trusion Materials’’ (Revised 1966), erally recognized as safe in food, sub- which is incorporated by reference. stances used in accordance with prior Copies are available from American So- sanction, substances permitted under ciety for Testing and Materials applicable regulations in this part, and (ASTM), 1916 Race Street, Philadel- the following: phia, PA 19103, or available for inspec- (1) Stabilizers. The homopolymer may tion at the Office of the Federal Reg- contain one or more of the following ister, 800 North Capitol Street, NW., stabilizers. The total amount of stabi- suite 700, Washington, DC 20408. lizers shall not exceed 1.9 percent of (d) Extractive limitations. (1) homopolymer by weight, and the quan- Polyoxymethylene homopolymer, in tity of individual stabilizer used shall the finished form which is to contact not exceed the limitations set forth food, when extracted with the solvent below: or solvents characterizing the type of
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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 articles or components of articles in- required to accomplish the intended tended for repeated use. physical or technical effect. (2) Use temperature shall not exceed (1) Substances generally recognized 250 °F. as safe in food. (3) In accordance with good manufac- (2) Substances used in accordance turing practice, finished articles con- with prior sanction or approval. taining polyoxymethylene (3) Substances the use of which is homopolymer shall be thoroughly permitted in coatings under regula- cleansed prior to first use in contact tions in parts 170 through 189 of this with food. chapter. [42 FR 14572, Mar. 15, 1977, as amended at 43 (c) The finished coatings are ther- FR 44835, Sept. 29, 1978; 47 FR 11846, Mar. 19, mally cured at temperatures of 700 °F 1982; 47 FR 51562, Nov. 16, 1982; 49 FR 10111, and above. Mar. 19, 1984; 54 FR 24898, June 12, 1989] (d) Polyphenylene sulfide resin coat- ings may be used in contact with food § 177.2490 Polyphenylene sulfide res- at temperatures not to exceed the boil- ins. ing point of water; provided that the Polyphenylene sulfide resins finished cured coating, when extracted (poly(1,4-phenylene sulfide) resins) may at reflux temperatures for 8 hours sepa- be safely used as coatings or compo- rately with distilled water, 50 percent
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ethanol in water, and 3 percent acetic rate test sample for each required ex- acid, yields total extractives in each tracting solvent.) extracting solvent not to exceed 0.02 (c) In accordance with good manufac- milligram per square inch of surface turing practice, finished food-contact and when extracted at reflux tempera- articles containing the polyvinylidene ture for 8 hours with heptane yields fluoride resins shall be thoroughly total extractives not to exceed 0.1 mil- cleansed prior to their first use in con- ligram per square inch of surface. tact with food. (e) Polyphenylene sulfide resin coat- ings containing perfluorocarbon resins § 177.2550 Reverse osmosis mem- branes. complying with § 177.1550 may be used in contact with food at temperatures Substances identified in paragraph up to and including normal baking and (a) of this section may be safely used as frying temperatures; provided that the reverse osmosis membranes intended finished cured coating, when extracted for use in processing bulk quantities of at reflux temperatures for 2 hours sepa- liquid food to separate permeate from rately with distilled water, 50 percent food concentrate or in purifying water ethanol in water, 3 percent acetic acid for food manufacturing under the fol- and heptane, yields total extractives in lowing prescribed conditions: each extracting solvent not to exceed (a) Identity. For the purpose of this 0.2 milligram per square inch of surface section, reverse osmosis membranes and when extracted at reflux tempera- may consist of either of the following ture for 1 hour with diphenyl ether formulations: yields total extractives not to exceed (1) A cross-linked high molecular 4.5 milligrams per square inch of sur- weight polyamide reaction product of face. 1,3,5-benzenetricarbonyl trichloride with 1,3-benzenediamine (CAS Reg. No. [42 FR 14572, Mar. 15, 1977, as amended at 47 83044–99–9) or piperazine (CAS Reg. No. FR 11846, Mar. 19, 1982; 54 FR 24898, June 12, 110–85–0). The membrane is on the food- 1989] contact surface, and its maximum weight is 62 milligrams per square deci- § 177.2510 Polyvinylidene fluoride res- meter (4 milligrams per square inch) as ins. a thin film composite on a suitable Polyvinylidene fluoride resins may support. be safely used as articles or compo- (2) A cross-linked polyetheramine nents of articles intended for repeated (CAS Reg. No. 101747–84–6), identified as use in contact with food, in accordance the copolymer of epichlorohydrin, 1,2- with the following prescribed condi- ethanediamine and 1,2-dichloroethane, tions: whose surface is the reaction product (a) For the purpose of this section, of this copolymer with 2,4- the polyvinylidene fluoride resins con- toluenediisocyanate (CAS Reg. No. of sist of basic resins produced by the po- the final polymer is 99811–80–0) for use lymerization of vinylidene fluoride. as the food-contact surface of reverse (b) The finished food-contact article, osmosis membranes used in processing when extracted at reflux temperatures liquid food. The composite membrane for 2 hours with the solvents distilled is on the food-contact surface and its water, 50 percent (by volume) ethyl al- maximum weight is 4.7 milligrams per cohol in distilled water, and n-heptane, square decimeter (0.3 milligrams per yields total extractives in each ex- square inch) as a thin film composite tracting solvent not to exceed 0.01 mil- on a suitable support. The maximum ligram per square inch of food-contact weight of the 2,4-toluenediisocyanate surface tested; and if the finished food- component of the thin film composite contact article is itself the subject of a is 0.47 milligrams per square decimeter regulation in parts 174, 175, 176, 177, 178 (0.03 milligrams per square inch). and § 179.45 of this chapter, it shall also (3) For the purpose of this section, comply with any specifications and the reverse osmosis membrane consists limitations prescribed for it by that of a polyaramide identified as 2,4- regulation. (NOTE: In testing the fin- diaminobenzenesulfonic acid, calcium ished food-contact article, use a sepa- salt (2:1) polymer with 1,3-
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benzenediamine, 1,3-benzenedicarbonyl (2) Reverse osmosis membranes de- dichloride, and 1,4-benzenedicarbonyl scribed in paragraph (a)(4) of this sec- dichloride (CAS Reg. No. 39443–76–0). tion may be used in contact with all The membrane is the food contact sur- types of liquid food, except food con- face and may be applied as a film on a taining more than 8 percent alcohol, at suitable support. Its maximum weight temperatures up to 80 °C (176 °F). is 512 milligrams per square decimeter (3) Reverse osmosis membranes shall (33 milligrams per square inch). be maintained in a sanitary manner in (4) A cross-linked high molecular accordance with current good manufac- weight polyamide reaction product of turing practice so as to prevent micro- poly(N-vinyl-N-methylamine) (CAS bial adulteration of food. Reg. No. 31245–56–4), N,N′-bis(3- aminopropyl)ethylenediamine (CAS (4) To assure their safe use, reverse Reg. No. 10563–26–5), 1,3- osmosis membranes and their supports benzenedicarbonyl dichloride (CAS shall be thoroughly cleaned prior to Reg. No. 99–63–8) and 1,3,5- their first use in accordance with cur- benzenetricarbonyl trichloride (CAS rent good manufacturing practice. Reg. No. 4422–95–1). The membrane is [49 FR 49448, Dec. 20, 1984, as amended at 52 the food-contact surface. Its maximum FR 29668, Aug. 11, 1987; 53 FR 31835, Aug. 22, weight is 20 milligrams per square deci- 1988; 53 FR 32215, Aug. 24, 1988; 55 FR 8139, meter (1.3 milligrams per square inch) Mar. 7, 1990; 59 FR 9925, Mar. 2, 1994] as a thin film composite on a suitable support. § 177.2600 Rubber articles intended for (5) A polyamide reaction product of repeated use. 1,3,5-benzenetricarbonyl trichloride Rubber articles intended for repeated polymer (CAS Reg. No. 4422–95–1) with use may be safely used in producing, piperazine (CAS Reg. No. 110–85–0) and manufacturing, packing, processing, 1,2-diaminoethane (CAS Reg. No. 107– preparing, treating, packaging, trans- 15–3). The membrane is the food-con- porting, or holding food, subject to the tact layer and may be applied as a film provisions of this section. on a suitable support. Its maximum weight is 15 milligrams per square deci- (a) The rubber articles are prepared meter (1 milligram per square inch). from natural and/or synthetic polymers (b) Optional adjuvant substances. The and adjuvant substances as described basic polymer identified in paragraph in paragraph (c) of this section. (a) of this section may contain optional (b) The quantity of any substance adjuvant substances required in the employed in the production of rubber production of such basic polymer. articles intended for repeated use shall These optional adjuvant substances not exceed the amount reasonably re- may include substances permitted for quired to accomplish the intended ef- such use by regulations in parts 170 fect in the rubber article and shall not through 186 of this chapter, substances be intended to accomplish any effect in generally recognized as safe in food, food. and substances used in accordance with (c) Substances employed in the prep- a prior sanction or approval. aration of rubber articles include the (c) Supports. Suitable supports for re- following, subject to any limitations verse osmosis membranes are mate- prescribed: rials permitted for such use by regula- (1) Substances generally recognized tions in parts 170 through 186 of this as safe for use in food or food pack- chapter, substances generally recog- aging. nized as safe in food, and substances used in accordance with a prior sanc- (2) Substances used in accordance tion or approval. with the provisions of a prior sanction (d) Conditions of use. (1) Reverse os- or approval. mosis membranes described in para- (3) Substances that by regulation in graphs (a)(1), (a)(2), (a)(3), and (a)(5) of parts 170 through 189 of this chapter this section may be used in contact may be safely used in rubber articles, with all types of liquid food at tem- subject to the provisions of such regu- peratures up to 80 °C (176 °F). lation.
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(4) Substances identified in this para- tact with foods of Types I, II, III, IV, V, VI, graph (c)(4), provided that any sub- VII, VIII, and IX identified in table 1 of stance that is the subject of a regula- § 176.170(c) of this chapter at temperatures not to exceed 150 °F except that those co- tion in parts 174, 175, 176, 177, 178 and polymers prepared with less than 50 § 179.45 of this chapter conforms with weight-percent of polyamide are limited to any specification in such regulation. use in contact with such foods at tempera- (i) Elastomers. tures not to exceed 100 °F. Polybutadiene. Acrylonitrile-butadiene copolymer. Polyester elastomers derived from the reac- Brominated isobutylene-isoprene copolymers tion of dimethyl terephthalate, 1,4- complying with § 177.1210. butanediol, and α-hydro-omega- Butadiene-acrylonitrile-ethylene glycol hydroxypoly (oxytetramethylene). Addi- dimethacrylate copolymers containing not tionally, trimethyl trimellitate may be more than 5 weight percent of polymer used as a reactant. The polyester units derived from ethylene glycol elastomers may be used only in contact dimethacrylate. with foods containing not more than 8 per- Butadiene-acrylonitrile-methacrylic acid co- cent alcohol and limited to use in contact polymer. with food at temperatures not exceeding Butadiene-styrene-methacrylic acid copoly- 150 °F. mer. Polyisoprene. Chloroprene polymers. Polyurethane resins (CAS Reg. Nos. 37383–28– Chlorotrifluoroethylene-vinylidene fluoride 1 or 9018–04–6) derived from the reaction of copolymer. diphenylmethane diisocyanate with 1,4- Ethylene-propylene copolymer elastomers butanediol and polytetramethylene ether which may contain not more than 5 glycol. weight-percent of total polymer units de- Polyurethane resins derived from reactions rived from 5-methylene-2-norbornene and/ of diphenylmethane diisocyanate with or 5-ethylidine-2-norbornene. adipic acid and 1,4-butanediol. Ethylene-propylene-dicyclopentadiene co- Rubber, natural. polymer. Silicone basic polymer as described in ASTM Ethylene-propylene-1,4-hexadiene copoly- method D1418–81, ‘‘Standard Practice for mers containing no more than 8 weight Rubber and Rubber Latices—Nomen- percent of total polymer units derived clature,’’ which is incorporated by ref- from 1,4-hexadiene. erence. Copies may be obtained from the Hydrogenated butadiene/acrylonitrile co- American Society for Testing Materials, polymers (CAS Reg. No. 88254–10–8) pro- 1916 Race St., Philadelphia, PA 19103, or duced when acrylonitrile/butadiene copoly- may be examined at the Office of the Fed- mers are modified by hydrogenation of the eral Register, 800 North Capitol Street, olefinic unsaturation to leave not more NW., suite 700, Washington, DC 20408. than 10 percent trans olefinic unsaturation and no α,β-olefinic unsaturation as deter- Silicone (Si) elastomers containing methyl mined by a method entitled ‘‘Determina- groups. tion of Residual α,β-Olefinic and Trans Ole- Silicone (Psi) elastomers containing meth- finic Unsaturation Levels in HNBR,’’ de- yl and phenyl groups. Silicone (Vsi) elastomers containing meth- veloped October 1, 1991, by Polysar Rubber yl and vinyl groups. Corp., 1256 South Vidal St., Sarnia, On- Silicone (Fsi) elastomers containing meth- tario, Canada N7T 7MI, which is incor- yl and fluorine groups. porated by reference in accordance with 5 Silicone (PVsi) elastomers containing U.S.C. 552(a) and 1 CFR part 51. Copies may phenyl, methyl, and vinyl groups. be obtained from the Center for Food Safe- ty and Applied Nutrition (HFS–200), Food Styrene-butadiene copolymer. and Drug Administration, 200 C St. SW., Vinylidene fluoride-hexafluoropropylene co- Washington, DC 20204, or may be examined polymers (minimum number average mo- at the Office of the Federal Register, 800 lecular weight 70,000 as determined by os- North Capitol St. NW., suite 700, Wash- motic pressure in methyl ethyl ketone). ington, DC. 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- (ii) Vulcanization materials—(a) Vul- col). The polyamide and polyether compo- canizing agents. nents are reacted in ratios such that the 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
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fluoridehexafluoropropylene copolymer Dicumyl peroxide. and vinylidene fluoride- N,N-Dimethylcyclohexylamine salt of hexafluoropropylene-tetrafluoroethylene dibutyldithiocarbamic acid. copolymer elastomers identified under 2,6-Dimethylmorpholine thiobenzothiazol. paragraph (c)(4)(i) of this section and lim- Dipentamethylenethiuram hexasulfide (CAS ited to use at levels not to exceed 2.4 per- Reg. No. 971–15–3). cent by weight of such copolymers. Diphenylguanidine. Diisopropyl xanthogen polysulfide (a 1:2:1 Diphenylguanidine phthalate. mixture of O,O-di(1-methylethyl)trithio- 1,3-Diphenyl-2-thiourea. bis-thioformate, O,O-di(1- 2,2′-Dithiobis[benzothiazole]. methylethyl)tetrathio-bis-thioformate, 4,4′-Dithiodimorpholine. and O,O-di(1-methylethyl)pentathio-bis- N,N′-Di-o-tolylguanidine. thioformate) for use as a cross linking Di-o-tolylguanidine salt of agent in the vulcanization of natural rub- pyrocatecholborate. ber, styrene-butadiene copolymer, acrylo- Ethylenediamine carbamate. nitrile-butadiene copolymer, and ethylene- Heptaldehyde-aniline resin (iodine number propylene terpolymers identified under 430–445). paragraph (c)(4)(i) of this section and lim- Hexamethylenetetramine. ited to use at levels not to exceed 2.4 per- 2-Mercaptobenzothiazole. cent by weight of such copolymers. 2-Mercaptothiazoline. Hexamethylenediamine carbamate for use N-Oxydiethylene-benzothiazole-2- only as cross-linking agent in the vul- sulfenamide. canization of vinylidene fluoride- Piperidinium pentamethylenedithiocarba- hexafluoropropylene copolymer and vinyli- mate. dene fluoride-hexafluoropropylene-tetra- Potassium pentamethylenedithiocarbamate. fluoroethylene copolymer elastomers iden- p-Quinone dioxime. tified under paragraph (c)(4)(i) of this sec- Sodium dibutyldithiocarbamate. tion and limited to use at levels not to ex- Sodium dimethyldithiocarbamate. ceed 1.5 percent by weight of such copoly- Stannous oleate for use only as an accel- mers. erator for silicone elastomers. Sulfur, ground. Tetrabutylthiuram monosulfide. Tetraethylthiuram disulfide. (b) Accelerators (total not to exceed 1.5 (1,1,4,4-Tetramethyltetramethylene)bis [tert- percent by weight of rubber product). butyl peroxide]. Tetramethylthiuram monosulfide. 2-Benzothiazyl-N,N-diethylthiocarbamyl-sul- Thiram (tetramethylthiuram disulfide). fide. Triallyl cyanurate. Benzoyl peroxide. Triethylenetetramine. 1,3-Bis(2-benzothiazolylmercaptomethyl) 1,3,5-Triethyl-hexahydro-s-triazine urea. (triethyltrimethylenetriamine). N-tert-Butyl-2-benzothiazole sulfenamide. Triphenylguanidine. Butyraldehyde-aniline resin (iodine number Zinc butyl xanathate. 670–705). Zinc dibenzyl dithiocarbamate. Carbon disulfide-1,1′-methylenedipiperidine Zinc dibutyldithiocarbamate. reaction product. Zinc diethyldithiocarbamate. Copper dimethyldithiocarbamate. Zinc 2-mercaptobenzothiazole. N-Cyclohexyl-2-benzothiazole sulfenamide. Ziram (zinc dimethyldithiocarbamate). Dibenzoyl-p-quinone dioxime. Dibenzylamine. (c) Retarders (total not to exceed 10 per- Diisopropyl xanthogen polysulfide (a 1:2:1 cent of weight of rubber product). mixture of O,O-di(1-methylethyl)trithio- Cyanoguanidine. bis-thioformate, O,O-di(1- Phthalic anhydride. methylethyl)tetrathio-bis-thioformate, Salicylic acid. and O,O-di(1-methylethyl)pentathio-bis- thioformate). (d) Activators (total not to exceed 5 per- Di(4-methylbenzoyl) peroxide (CAS Reg. No. cent by weight of rubber product except 895–85–2) for use only as a crosslinking magnesium oxide may be used at higher agent in silicone polymers and elastomers levels). identified under paragraph (c)(4)(i) of this 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.
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Tall oil fatty acids. Styrenated phenol. Tetrachloro-p-benzoquinone. 4,4′-Thiobis (6-tert-butyl-m-cresol). Triethanolamine. Toluene-2,4-diamine. Zinc salts of fatty acids. N-o-Tolyl-N′-phenyl-p-phenylenediamine. p(p-Tolylsufanilamide) diphenylamine. (iii) Antioxidants and antiozonants Tri(mixed mono- and dinonylphenyl) (total not to exceed 5 percent by weight of phosphite. rubber product). Tri(nonylphenyl) phosphite-formaldehyde Aldol-a-naphthylamine. resins produced when 1 mole of tri(nonylphenyl) phosphite is made to Alkylated (C4 and/or C8) phenols. BHT (butylated hydroxytoluene). react with 1.4 moles of formaldehyde or 4-[[4,6-bis(octylthio)-s-triazin-2-yl]amino]- produced when 1 mole of nonylphenol is 2,6-di-tert-butylphenol (CAS Reg. No. 991– made to react with 0.36 mole of formalde- 84–4) for use only as a stabilizer at levels hyde and the reaction product is then fur- not to exceed 0.5 percent by weight of the ther reacted with 0.33 mole of phosphorus finished rubber product. trichloride. The finished resins have a min- Butylated reaction product of p-cresol and imum viscosity of 20,000 centipoises at 25 dicyclopentadiene as identified in °C, as determined by LV–series Brookfield § 178.2010(b) of this chapter. viscometer (or equivalent) using a No. 4 Butylated, styrenated cresols identified in spindle at 12 r.p.m., and have an organic § 178.2010(b) of this chapter. phosphorus content of 4.05 to 4.15 percent 4,4′-Butylidinebis(6-tert-butyl-m-cresol). by weight. N-Cyclohexyl-N′-phenylphenylenediamine. (iv) Plasticizers (total not to exceed 30 p,p′-Diaminodiphenylmethane. 2,5-Di-tert-amylhydroquinone. percent by weight of rubber product un- Diaryl-p-phenylenediamine, where the aryl less otherwise specified). group may be phenyl, tolyl, or xylyl. n-Amyl n-decyl phthalate. 2,6-Di-tert-butyl-p-phenylphenol. Butylacetyl ricinoleate. 1,2-Dihydro-2,2,4-trimethyl-6- n-Butyl ester of tall oil fatty acids. dodecylquinoline. Butyl laurate. 1,2-Dihydro-2,2,4-trimethyl-6- Butyl oleate. ethoxyquinoline. Butyl stearate. 1,2-Dihydro-2,2,4-trimethyl-6- Calcium stearate. phenylquinoline. Castor oil. ′ 4,4 -Dimethoxydiphenylamine. Coumarone-indene resins. 4,6-Dinonyl-o-cresol. 2,2′-Dibenzamidodiphenyl disulfide. N,N′-Dioctyl-p-phenylenediamine. Dibenzyl adipate. Diphenylamine-acetone resin. Dibutoxyethoxyethyl adipate. Diphenylamine-acetone-formaldehyde resin. Dibutyl phthalate. N,N′-Diphenylethylenediamine. N,N′-Disalicylalpropylenediamine. Dibutyl sebacate. N,N′-Di-o-tolylethylenediamine. Didecyl adipate. Hydroquinone monobenzyl ether. Didecyl phthalate. Isopropoxydiphenylamine. Diisodecyl adipate. N-Isopropyl-N′-phenyl-p-phenylenediamine. Diisodecyl phthalate. 2,2′-Methylenebis(6-tert-butyl-4-ethylphenol). Diisooctyl adipate. 2,2′-Methylenebis(4-methyl-6-tert-butyl- Diisooctyl sebacate. phenol). Dioctyl adipate. 2,2′-Methylenebis(4-methyl-6-nonylphenol). Dioctyl phthalate. 2,2′-Methylenebis(4-methyl-6-tert- Dioctyl sebacate. octylphenol). Dipentene resin. 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
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section, in contact with foods of Types I, Polyethylene. II, III, IV, VI, VII, VIII, and IX idenified in Sodium stearate. table 1 of § 176.170(c) of this chapter. Montan wax. (viii) Emulsifiers. n-Octyl n-decyl adipate. Fatty acid salts, sodium or potassium. n-Octyl n-decyl phthalate. Naphthalene sulfonic acid-formaldehyde con- Petrolatum. densate, sodium salt. Petroleum hydrocarbon resin Rosins and rosin-derivatives identified in (cyclopentadiene type), hydrogenated. § 175.105(c)(5) of this chapter. Petroleum hydrocarbon resin (produced by Sodium decylbenzenesulfonate the homo- and copolymerization of dienes Sodium dodecylbenzenesulfonate and olefins of the aliphatic, alicyclic, and Sodium lauryl sulfate. monobenzenoid arylalkene types from dis- Tall oil mixed soap (calcium, potassium, and tillates of cracked petroleum stocks). sodium). Petroleum hydrocarbon resin (produced by the catalytic polymerization and subse- (ix) Miscellaneous (total not to exceed 5 quent hydrogenation of styrene, percent by weight of rubber product). vinyltoluene, and indene types from dis- Animal glue as described in § 178.3120 of this tillates of cracked petroleum stocks). chapter. Petroleum oil, sulfonated. Azodicarbonamide as chemical blowing Phenol-formaldehyde resin. agent. Pine tar. 2-Anthraquinone sulfonic acid sodium salt Polybutene. for use only as polymerization inhibitor in Polystyrene. chloroprene polymers and not to exceed Propylene glycol. 0.03 percent by weight of the chloroprene n-Propyl ester of tall oil fatty acids. polymers. Rapeseed oil vulcanized with rubber maker’s 1,2-Benzisothiazolin-3-one (CAS Reg. No. sulfur. 2634–33–5) for use as a biocide in uncured Rosins and rosin derivatives identified in liquid rubber latex not to exceed 0.02 per- § 175.105(c)(5) of this chapter. cent by weight of the latex solids, where Soybean oil vulcanized with rubber maker’s the total of all items listed in paragraph sulfur. (c)(4)(ix) of this section does not exceed 5 Styrene-acrylonitrile copolymer. percent of the rubber product. Terpene resins. n-Butyllithium for use only as polymeriza- Triethylene glycol dicaprate. tion catalyst for polybutadiene. Triethylene glycol dicaprylate. 4-tert-Butyl-o-thiocresol as peptizing agent. Waxes, petroleum. tert-Butyl peracetate. Xylene (or toluene) alkylated with p-tert-Butylpyrocatechol. dicyclopentadiene. ¥ Dialkyl (C8 C18 Zinc 2-benzamidothiophenate. Di- and triethanolamine. (v) Fillers. Diethyl xanthogen disulfide. 4-(Diiodomethylsulfonyl) toluene, Chemical Aluminum hydroxide. Abstracts Service Registry No. 20018–09–01, Aluminum silicate. for use as an antifungal preservative at Asbestos fiber, chrysotile or crocidolite. levels not to exceed 0.3 percent by weight Barium sulfate. of the sealants and caulking materials. Carbon black (channel process or furnace Dodecyl mercaptan isomers, single or mixed. combustion process; total carbon black not 2-Ethoxyethanol. to exceed 50 percent by weight of rubber Iodoform. product; furnace combustion black content p-Menthane hydroperoxide. 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. 4,4′-Oxybis (benzenesulfonhydrazide) as (vi) Colorants. Colorants used in ac- 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.
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Sodium polysulfide. § 177.2710 Styrene-divinylbenzene res- Sodium nitrite. ins, cross-linked. Sodium salt of ethylenediamine tetraacetic acid and glycine. Styrene-divinylbenzene cross-linked Sodium sulfide. copolymer resins may be safely used as Styrene monomer. articles or components of articles in- Tall oil. tended for repeated use in producing, Thioxylenois as peptizing agents. manufacturing, packing, processing, Tridecyl mercaptan. preparing, treating, packaging, trans- Zinc 4-tert-butylthiophenate as peptizing agent. porting, or holding food, in accordance with the following prescribed condi- (d) Rubber articles intended for use tions: with dry food are so formulated and (a) The resins are produced by the co- cured under conditions of good manu- polymerization of styrene with facturing practice as to be suitable for divinylbenzene. repeated use. (b) The resins meet the extractives (e) Rubber articles intended for re- limitations prescribed in this para- peated use in contact with aqueous graph: food shall meet the following specifica- (1) The resins to be tested are ground tions: The food-contact surface of the or cut into small particles that will rubber article in the finished form in pass through a U.S. standard sieve No. which it is to contact food, when ex- 3 and that will be held on a U.S. stand- tracted with distilled water at reflux ard sieve No. 20. temperature, shall yield total extrac- (2) A 100-gram sample of the resins, tives not to exceed 20 milligrams per when extracted with 100 milliliters of square inch during the first 7 hours of ethyl acetate at reflux temperature for extraction, nor to exceed 1 milligram 1 hour, yields total extractives not to per square inch during the succeeding 2 exceed 1 percent by weight of the res- hours of extraction. ins. (f) Rubber articles intended for re- (c) In accordance with good manufac- peated use in contact with fatty foods turing practice, finished articles con- shall meet the following specifications: taining the resins shall be thoroughly The food-contact surface of the rubber cleansed prior to their first use in con- article in the finished form in which it tact with food. is to contact food, when extracted with n-hexane at reflux temperature, shall § 177.2800 Textiles and textile fibers. yield total extractives not to exceed Textiles and textile fibers may safely 175 milligrams per square inch during be used as articles or components of ar- the first 7 hours of extraction, nor to ticles intended for use in producing, exceed 4 milligrams per square inch manufacturing, packing, processing, during the succeeding 2 hours of ex- preparing, treating, packaging, trans- traction. porting, or holding food, subject to the (g) In accordance with good manufac- provisions of this section. turing practice finished rubber articles (a) The textiles and textile fibers are intended for repeated use in contact prepared from one or more of the fibers with food shall be thoroughly cleansed identified in paragraph (d) of this sec- prior to their first use in contact with tion and from certain other adjuvant food. substances required in the production (h) The provisions of this section are of the textiles or textile fibers or added not applicable to rubber nursing-bottle to impart desired properties. nipples. (b) The quantity of any adjuvant sub- (i) Acrylonitrile copolymers identi- stance employed in the production of fied in this section shall comply with textiles or textile fibers does not ex- the provisions of § 180.22 of this chap- ceed the amount reasonably required ter. to accomplish the intended physical or [42 FR 14572, Mar. 15, 1977] technical effect or any limitation fur- EDITORIAL NOTE: For FEDERAL REGISTER ci- ther provided. tations affecting § 177.2600, see the List of (c) Any substance employed in the CFR Sections Affected in the Finding Aids production of textiles or textile fibers section of this volume. that is the subject of a regulation in
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parts 174, 175, 176, 177, 178 and § 179.45 of (3) Substances generally recognized this chapter conforms with any speci- as safe for use in cotton and cotton fab- fication in such regulation. rics used in dry-food packaging. (d) Substances employed in the pro- (4) Substances that by regulation in duction of or added to textiles and tex- this part may safely be used in the pro- tile fibers may include: duction of or as a component of tex- (1) Substances generally recognized tiles or textile fibers and subject to as safe in food. provisions of such regulation. (2) Substances subject to prior sanc- (5) Substances identified in this para- tion or approval for use in textiles and textile fibers and used in accordance graph (d)(5), subject to such limitations with such sanction or approval. 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. 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 400±3,000). 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).
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List of substances Limitations
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.
(e) Textile and textile fibers are used poly(vinylidene fluoride) membrane as articles or components of articles with a hydrophilic surface modifier that contact dry food only. consisting of hydroxypropyl acrylate/ (f) The provisions of this section are tetraethylene glycol diacrylate copoly- not applicable to jute fibers used as mer. prescribed by § 178.3620(d)(2) of this (b) Any substance employed in the chapter. production of ultra-filtration mem- branes that is the subject of a regula- [42 FR 14572, Mar. 15, 1977, as amended at 46 FR 37042, July 17, 1981; 49 FR 4372, Feb. 6, tion in parts 174, 175, 176, 177, 178 and 1984; 49 FR 5748, Feb. 15, 1984; 56 FR 42933, § 179.45 of this chapter conforms with Aug. 30, 1991] the specifications of such regulation. (c) Ultra-filtration membranes are § 177.2910 Ultra-filtration membranes. used in the physical separation of dis- Ultra-filtration membranes identi- solved or colloidally suspended varying fied in paragraphs (a)(1), (a)(2), (a)(3), molecular size components of liquids and (a)(4) of this section may be safely during the commercial processing of used in the processing of food, under bulk quantities of food. the following prescribed conditions; (d) Ultra-filtration membranes shall (a)(1) Ultra-filtration membranes be maintained in a sanitary manner in that consist of paper impregnated with accordance with good manufacturing cured phenol-formaldehyde resin, practice so as to prevent potential mi- which is used as a support and is coat- crobial adulteration of the food. ed with a vinyl chloride-acrylonitrile (e) Ultrafiltration membranes identi- copolymer. fied in paragraph (a)(4) may be used to (2) Ultra-filtration membranes that filter aqueous or acidic foods con- consist of a sintered carbon support taining up to 13 percent of alcohol at that is coated with zirconium oxide temperatures not to exceed 21 °C (70 (CAS Reg. No. 1314–23–4) containing up °F). to 12 percent yttrium oxide (CAS Reg. (f) To assure safe use of the ultra-fil- No. 1314–36–9). tration membranes, the label or label- (3) Ultra-filtration membranes that ing shall include adequate directions consist of an aluminum oxide support for a pre-use treatment, consisting of that is coated with zirconium oxide conditioning and washing with a min- (CAS Reg. No. 1314–23–4) containing up imum of 8 gallons of potable water to 5 percent yttrium oxide (CAS Reg. prior to their first use in contact with No. 1314–36–9). food. (4) Ultrafiltration membranes that (g) Acrylonitrile copolymers identi- consist of a microporous fied in this section shall comply with
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the provisions of § 180.22 of this chap- 178.3730 Piperonyl butoxide and pyrethrins ter. as components of bags. 178.3740 Plasticizers in polymeric sub- [42 FR 14572, Mar. 15, 1977, as amended at 53 stances. FR 17925, May 19, 1988; 58 FR 48599, Sept. 17, 178.3750 Polyethylene glycol (mean molec- 1993; 60 FR 54426, Oct. 24, 1995] ular weight 200–9,500). 178.3760 Polyethylene glycol (400) PART 178—INDIRECT FOOD ADDI- monolaurate. 178.3770 Polyhydric alcohol esters of TIVES: ADJUVANTS, PRODUCTION oxidatively refined (Gersthofen process) AIDS, AND SANITIZERS montan wax acids. 178.3780 Polyhydric alcohol esters of long Subpart A [Reserved] chain monobasic acids. 178.3790 Polymer modifiers in semirigid and Subpart B—Substances Utilized To Control rigid vinyl chloride plastics. the Growth of Microorganisms 178.3800 Preservatives for wood. 178.3850 Reinforced wax. Sec. 178.3860 Release agents. 178.1005 Hydrogen peroxide solution. 178.3870 Rosins and rosin derivatives. 178.1010 Sanitizing solutions. 178.3900 Sodium pentachlorophenate. 178.3910 Surface lubricants used in the man- Subpart C—Antioxidants and Stabilizers ufacture of metallic articles. 178.2010 Antioxidants and/or stabilizers for 178.3930 Terpene resins. polymers. 178.3940 Tetraethylene glycol di-(2-ethyl- 178.2550 4-Hydroxymethyl-2,6-di-tert-butyl- hexoate). phenol. 178.3950 Tetrahydrofuran. 178.2650 Organotin stabilizers in vinyl chlo- AUTHORITY: 21 U.S.C. 321, 342, 348, 379e. ride plastics. SOURCE: 42 FR 14609, Mar. 15, 1977, unless Subpart D—Certain Adjuvants and otherwise noted. Production Aids EDITORIAL NOTE: Nomenclature changes to part 178 appear at 61 FR 14482, Apr. 2, 1996. 178.3010 Adjuvant substances used in the manufacture of foamed plastics. 178.3120 Animal glue. Subpart A [Reserved] 178.3125 Anticorrosive agents. 178.3130 Antistatic and/or antifogging Subpart B—Substances Utilized To agents in food-packaging materials. 178.3280 Castor oil, hydrogenated. Control the Growth of Micro- 178.3290 Chromic chloride complexes. organisms 178.3295 Clarifying agents for polymers. 178.3297 Colorants for polymers. § 178.1005 Hydrogen peroxide solution. 178.3300 Corrosion inhibitors used for steel Hydrogen peroxide solution identi- or tinplate. 178.3400 Emulsifiers and/or surface-active fied in this section may be safely used agents. to sterilize polymeric food-contact sur- 178.3450 Esters of stearic and palmitic acids. faces identified in paragraph (e)(1) of 178.3480 Fatty alcohols, synthetic. this section. 178.3500 Glycerin, synthetic. (a) Identity. For the purpose of this 178.3505 Glyceryl tri-(12-acetoxystearate). section, hydrogen peroxide solution is 178.3520 Industrial starch-modified. an aqueous solution containing not 178.3530 Isoparaffinic petroleum hydro- more than 35 percent hydrogen per- carbons, synthetic. 178.3570 Lubricants with incidental food oxide (CAS Reg. No. 7722–84–1) by contact. weight, meeting the specifications pre- 178.3600 Methyl glucoside-coconut oil ester. scribed in paragraph (c) of this section. 178.3610 a-Methylstyrene-vinyltoluene res- (b) Optional adjuvant substances. Hy- ins, hydrogenated. drogen peroxide solution identified in 178.3620 Mineral oil. paragraph (a) of this section may con- 178.3650 Odorless light petroleum hydro- tain substances generally recognized as carbons. safe in or on food, substances generally 178.3690 Pentaerythritol adipate–stearate. 178.3700 Petrolatum. recognized for their intended use in 178.3710 Petroleum wax. food packaging, substances used in ac- 178.3720 Petroleum wax, synthetic. cordance with a prior sanction or ap- 178.3725 Pigment dispersants. proval, and substances permitted by
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