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IS 14137 (1994): Cetyl Alcohol for Cosmetic Industry [PCD 19: Cosmetics]

“ान एक न भारत का नमण” Satyanarayan Gangaram Pitroda “Invent a New India Using Knowledge”

“ान एक ऐसा खजाना जो कभी चराया नह जा सकताह ै”ै Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen”

IS 14137:1994

Indian Standard CETYL ALCOHOL FOR COSMETIC INDUSTRY- SPECIFICATION

UDC 665’58 [ 547’288’19 ]

tQ BIS 1994

BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002

Price Group 3 November 1994 Cosmetics Sectional Committee, PCD 19

FOREWORD

This Indian Standard was adopted by the Bureau of Indian Standards, after the draft finalized by the Cosmetics Sectional Committee, had been approved by the Petroleum, Coal and Related Products Division Council.

Cetyl alcohol is a white unctuous mixture of solid alcohols consisting chiefly of n-hexadecanol. It is soluble in ethanol, ether, chloroform and toluene and insoluble in water. It conforms to the formula: CHs ( CH2 ) lKH,OH

Cetyl alcohol is an important ingredient in cosmetic products like creams, lotions, etc. either as such or after ethoxylation. It is obtained by high pressure hydrogenation of palmitic acid. In certain cosmetic products, a mixture of cetyl alcohol and stearyl alcohol gives better properties than pure cetyl alcohol.

Cetearyl alcohol, a mixture of cetyl and stearyl alcohols. is an odourless, white, waxy solid which is soluble in diethyl ether, benzene and chloroform. It is slightly soluble in petroleum ether, ethanol and acetone and is insoluble in water.

This standard provides specifications for pure cetyl alcohol, whereas requirement for cetearyl alcohol ( mixture of cetyl and stearyl alcohols ) are given for information only.

This standard is essentially based on Cosmetic, Toiletries Fragrance Association ( CTFA ) Specification For Cetyl alcohol and Cetearyl alcohol.

For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test, shall be rounded off in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (.revised )‘. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard.

. - . _- “. _ _.. ,_“._. .‘_‘~II

IS 14137: 1994 Indian Standard CETYLALCOHOL FOR COSMETIC INDUSTRY- SPECIFICATION

3.2 The material shall comply with the requirements 1 SCOPE . given in Table 1. This standard prescribes the requirements and methods of sampling and test for cetyl alcohol. The requirements for cetearyl alcohol (mixture of cetyl Table 1 Requirements for Cetyl Alcohol for and stearyl alcohols) are given in Table 2 for guidance Cosmetic Industry only. (Clauses 3.2, 6 and A-10.3.3)

2 REFERENCES SI Characteristic Requirenwt Method of The followinrr Indian Standards are necessary adjuncts NO. TCSl to this standird: (1) (2) (3) (4)

IS No. Title 9 Appearance Solid - 264 : 1976 Nitric acid (second re~isioti) flakes or lumps 265 : 1987 Hydrochloric acid (second re~i.~io~)

286 : 1978 Methods of sampling and tests ii) COIOW As agreed to between A-l for soaps (second revision) the buyer mid the seller

1070 : 1992 Reagent grade water - iii) Iiydroxyl value A-2 Specification (third revision) iv) Acid value, Max A-3 2088 : 1988 Methods for determination of arsenic urst revision) A-4 2362 : 1973 Determination of water by the Karl Fischer’s method Y;rst revision) 3958 : 19s4 Methods of sampling cosmetics vi) Iodine value, Mm (‘lause 7 of (Jrst revision) IS ‘86 : 1978 4707 Classification of cosmetic raw A-5 materials and adjuncts vii) Moisture. percent by mass. Mm (Part 1) : 1988 Dyes, colour and pigments

(J7rst revision) viii) Hydrocarbon, percent A-6 (Part 2) : 1993 List of raw materials generally by mass, MN\. not’ recognized as safe for use in cosmetics (first revision) A-7

Thr above mentioned standards contain provisions which, through reference in this text, constitute provisions of this standard. At the time of publication, the cd&ions indicated were valid. All standards are subject to revision, and parties to agreements based on this standard are rncouragcd to investigate the possibility of applying the most recent editions of the standards indicated above. A-K

3 REQUIREMENTS A-Y 3.1 Ikscription A-10 Cetyl alcohol shall be straight chain even numbered saturated alcohol containing predominantly C,, alcohol or a mixture of C and C alcohols. The material xiii) lieavy meinls, :IS lead A-II shall be solid eithe:in a flake form or in lump form. (Ph). ppm, MNV It shall be free from visible impurities. 1 IS 14137 : 1994 Table 2 Requirements for Cetearyl Alcohol for 4 PACKING AND MARKING Cosmetic Industry 4.1 Packing ( Clause 1 ) The material shall be packed in suitable well closed SI Charscteristic Requirement Method of containers as agreed to between the buyer and the No. Test seller.

(1) (2) (3) (4) 4.2 Marking The containers shall be legibly marked with the - 9 Appearance Solid following information: flakes game of the material; or lumps Indication of the source of manufacture; ii) Colour As agreed lo between A-l Net mass of the material; the buyer and the seller Batch number in code or otherwise, to enable the lot of manufacture to be traced back from iii) Hydroxyl value 200-220 A-2 records; and Any other requirement as required by statutory iv) Acid value, Mar 1.0 A-3 authorities. Saponification value, 3.0 A-4 v) 4.3 BIS Certification Marking MRY The product may also be marked with Standard Mark. vi) Iodine value, Mar 3.0 Clause 17 of 1s 286 : 1978 4.3.1 The use of the Standard Mark is governed by the provisions of Bureau of Indian Standards Act, Moisture, percent by 0.2 A-5 vii) 1986 and the Rules and Regulations made thereunder. mass, Mar The details of conditions under which the licence for viii) Hydrocarbon, percent 1.5 A-6 the use of Standard Mark may be granted to by mass, Mar manufacturers or producers may be obtained from the Bureau of Indian Standards. ix) Assay by GC, percenr by 90 A-7 mass, Mi~z, with following break-up 5 SAMPLING 5.1 Representative samples of the material shall be c,, 0 to 3 : C,, 40 to 60 drawn as prescribed in IS 3958 1984. C,* 40 to 60 5.2 Tests for sll characteristics shall be carried out on composite satnple. X) pH of 10 percent 7 to 9 A-8 suspension 5.3 The material shall be taken to have conformed to the specification if the composite sample passes xi) Melting range, “C 45 to 51 A-9 all the tests. xii) Arsenic (as As) ppm, Mow 2 A-10 6 TEST METHODS xiii) Heavy melals, as leao 20 A-11 Tests shall be conducted as prescribed in co1 (as Pb), ppm, Mnr 4 of Table 1. Reference to relevant standards is give11 in co1 4 of Table 1.

ANNEX A (Clauses 3.2 and 6)

A-l DETERMINATION OF COLOUR ( HAZEN ) the lens and rotate the calorimeter wheel till both . sides of calorimeter show same colour. Note down A-l.1 Apparatus the reading of calorimeter.

A-1.1.1 Any Suitdde Cohrimeter A-2 DETERMINATION OF HYDROXYL VALUE

A-l .1.2 Nessler Cylinders The hydroxyl value is the number of milligrams oT 2 cm internal diameter, 12 cm long with marking at potassium hydroxide equivalent to the hydroxyl content 4.7 cm. of one gram of sample. A-2.1 Reagents A-l.2 Procedure A-2.1.1 Acetylnting Reagents Fill one Nessler cylinder with water and other with fatty alcohol. Put the calorimeter wheel marked with Freshly prepared before use by mixing 25 ml of acelic No. 5, 10, 15, 20, 30, 40,50, 60 and 70. See through anhydride with 75 ml pyridinc. 2 IS 14137 : 1994

A-2.1.2 Methanol A-4 DETERMINATION OF SAPONIFICATION VALUE A-2.1.3 Isopropanol Saponification value is the number of milligrams of A-2.1.4 Alcoholic Potassium Hydroxide - 0.5 N. potassium hydroxide required to saponify 1 g of sample. A-2.2 Procedure A-4.1 Reagents Weigh 0.5 to 0.6 g of the sample into a stoppered conical flask. Add 5 ml of the freshly prepared A-4.1.1 Alcoholic Potassium Hydroxide - 0.1 N. acetylating reagent accurately by a pipette. Attach an air condenser and retlux on a steam bath for 1 hour, A-4.1.2 Hydrochloric Acid - 0.1 N, add 5 ml of distilled water through the air condenser. Reflux for a further 10 minutes. Cool to room A-4.2 Procedure temperature. Rinse the air condenser and the neck of the flask with 25 ml of a neutralized mixture of Accurately weigh about 3 to 5 g of the sample into 2 : 1 methanol : Isopropanol. Titrate against 0.5 N a 250-ml stoppered conical flask. Add accurately 40 alcoholic potassium hydroxide. Conduct a duplicate ml of 0.1 N alcoholic potassium hydroxide to the and two blanks simultaneously. sample from a burette and reflux on a sand bath/ mantle with an air condenser for 30 minutes. Titrate A-2.3 Calculation against 0.1 N hydrochloric acid with phenolphthalein indicator. Conduct a blank estimation simultaneously. (B -- S) x N x 56.1 Hydroxyl value = M A-4.3 Calculation

where (B - S) x N x 56.1 B = volume in ml of potassium Saponification = hydroxide solution required for value M blank, s = volume in ml of potassium where hydroxide solution required for B = ml of 0.1 N hydrochloric acid acetylated sample, required for neutralization of blank, M= mass in g of the sample, and N= normality of potassium hydroxide S = ml of 0.1 N hydrochloric acid solution. solution, N = normality of hydrochloric acid A-3 DETERMINATION OF ACID VALUE solution, and A-3.0 Acid value is the number of milligranls of M = mass in g of the sample. potassium hydroxide required to neutralize free fatty acids in 1 g of sample. A-5 DETERMINATION OF MOISTURE A-3.1 Reagents A-5.1 Outline of the Method A-3.1.1 Alcoholic Sodium Hydroxide - 0.1 N. The method determines the actual water content of A-3.1.2 Methanol the material by titration with Karl Fischer reagent which reacts quantitatively with water. A-3.1.3 Isopropanol A-5.2 Procedure A-3.2 Procedure Take about 20 g of material, weigh accurately and Weigh accurately about 10 g of the sample into a dctemline the moisture content by the procedure given conical flask. Add about 25 ml of a 2 : 1 mixture of methanol : Isopropanol previously neutral&d with in IS 2362 : 1973. 0.1 N sodium hydroxide to a faint pink phenolphthalein A-6 DETERMINATION OF HYDROCARBON colour. Warm to dissolve the sample. Titrate against 0.1 sodium hydroxide to the same faint pink colour. The analysis measures the hydrocarbon content in A-3.3 Calculation fatty alcohols. The principle in the. analysis is the absorption of the fatty alcohols on silica gel, while T x N x 56.1 the hydrocarbons are not absorbed. Acid value =pp M A-6.1 Reagents where T = ml of sodium hydroxide required A-6.1.1 Pentane for neutralization, A-6.2 Procedure N= normality of hydroxide solution, and Weigh accurately about 2 g of sample into a 100- M= mass in g of the sample. ml flask and add 50 ml of pentane to it. If it is an 3 IS 14137 : 1994 alcohol with a high melting point then it has to be guidance only. The percentage of various fatty alcohols melted first in a steam bath and weighed promptly in a given sample is determined by gas chromatography. and, after adding pentane, the mixture has to be heated. A-7.1 Outline of the Method Take a glass tube of 50 cm length and 1.2 cm internal A sample of the material is dissolved in a suitable diameter. Fill the bottom of the tube with some spu11 solvent (for example, hexane, cyclohexane, chloroform glass and press it together with a metal rod. Fill up and petroleum ether) and is injected into the gas with powdered silica gel (800-200 mesh) and gently chromatograph where it is carried by the carrier gas tap the tube against a wooden plate about 30 times from one end of the column to the other. During its until the column is 45 cm full. movement, the constituents of the sample undergo distribution at different rates and ultimately get Place a loo-ml flask underneath the tube. Transfer separated from one another. The separated constituents the sample solution by a small funnel to a round flask emerge from the end of the column one after another with a long and narrow neck. Put the long necked and are detected by suitable means whose response flask upside down into the silica gel tube and allow is related to the amount of a specific component the pentane to drip. When the round flask is empty, leaving the column. the sample flask is washed by SO-ml pentane, which is transferred to the long necked flask and dripped A-7.2 Apparatus through the silica gel tube. This takes about two hours. After this, remove the lOO-ml flask in which A-7.2.1 Any suitable gas chromatograph and column the pentane, with extracts, is collected and put another capable of being operated under conditions suitable 50 ml pentane through the silica gel collect it in a for resolving the individual constituents into distinct separate flask. peaks may be used. The typical chromatogram for cetyl alcohol with the following chromatographic For C,, and other aicohols with a high melting point, conditions is shown in Fig. 1. silica gel tube shall be heated with a heating bulb. The heating bulb is placed at a distance from the Sample size 0.1 to 0.2 microlitres as column sufficient to keep the alcohol in a liquid state. 50 percent solution in Care should be taken that the pentane does not boil. chloroform After the extraction is complete, evaporate the pentane from the loo-ml flask on the steam bath until about Column 5 ml solution is left in the flask. Transfer this solution Material Stainless steel to a dry and weighed (iI4) aluminium bowl. Wash the 2.28 111 flask twice with 5 ml of pentane. Keep the aluminum Length 0.32 cm bowl on the steam bath and gently evaporate the Orifice Stationary phase SE 30 pentane. Watch the pentane evaporation closely, and and solid support Chromosorb WAW when bubbling ceases, remove the bowl immediately. loo- 120 Mesh Keep the bowl in the vacuum desiccator at ambient temperature for 15 minutes. Weigh the aluminium DMCS bowl again (N). The difference in mass (N - M) gives Carrier Gas Nitrogen the hydrocarbon weight. The second extraction with 40 ml/min gas flow 50 ml pentanc is done in the same way and the hydrocarbon determination should not be more than Conditions 1 mg. Temperature A-6.3 Calculution Column temperature Programming programming 1 lO*C Mass of hydrocarbon x 100 (1 to 7”C/minu te) Hydrocarbon, - 220°C hold percent by mass = Mass of sample Injection port 250°C = (N - M) x 100 temperature (1 where Detector N = mass in g of the residue, F.T.D. M = mass in g of the aluminium bowl, TYPC Temperature 300°C and (I = mass in g of the sample. A-7.3 Calculation A-7 GAS CHROMATOGRAI’HIC ANALYSIS A-7.3.1 Calculate from the peak areas ot’ individual OF ACETYI, ALCOHOL FOR COSMETIC constituents shown on the chromatogram of the material, INDUSTRY concentrations of constituents on the basis of peaks area on chromatogram obtained with known amount A-7.0 General of pure constituents using the same apparatus under The chromatographic conditions given here are for identical conditions.

4 IS 14137 : 1994

A-7.3.2 Area Measuremmt (See Note) bath and continue heating with constant stirring at a rate of approximately 3 deg/min until a temperature Since normal peaks approximate a triangle, the area 3°C below the expected melting point is attained. is measured by multiplying the peak height times the Then carefully regulate the rate to about 1 to 2 deg/ width of half height. The normal peak base is not min until the sample is completely melted. taken since large deviations may be observed due to tailing or adsorption. The technique is rapid, simple A-9.2.3 The temperature at which the column sample and fairly accurate when peaks are symmetrical and is observed to collapse definitely against the side of of reasonable width. the tube at any point shall be taken as the beginning of the melting and the temperature at which the sample A-7.3.3 Area Normalization becomes liquid throughout shall be taken as the end of melting. By normalizing, it is meant, calculating the percentage composition by measuring the area of each and dividing A-9.2.4 Both the temperature noted shall fall within the individual areas by total area, for example: the specified melting range. Area of A Percentage of A = x 100 A-10 DETERMINATION OF HEAVY METALS Total area AS LEAD (Pb)

NOTE - Other methods of area measurements, namely. A-10.0 Outline of the Method triangulation, disc inkgrator and electronic digital integrator if Cixcd with G1.C machine, would be of great advantage. The colour produced with hydrogen sulphide solution is matched against that obtained with standard lead A-8 DETERMINATION OF pH OF 10 PERCENT SUSPENSION solution.

A-8.1 Apparatus A-10.1 Apparatus A-10.1.1 ml capacity. APH meter, preferably equipped with glass electrode. Nessker Cylinders - 50

A-8.2 Procedure A-10.2 Reagents

Boil 1 g of the sample in 10 ml of water and determine A-10.2.1 Concentrated Hydrochloric Acid - see the pH of the suspelLGon after cooling using pH IS 265 : 1987. meter. A-10.2.2 Concentrated Nitric Acid - see IS 264 : A-9 DETERMINATION OF MELTING POINT 1976.

A-9.1 Apparatus A-10.2.3 Dilute Acetic Acid - 6 percent acetic acid (60 ml diluted to 1 000 ml with water). A-9.1.1 Oil Bath - consisting of liquid paraffin in A-10.2.4 Hydrogen Sulphide Solution - saturated. a glass container. A-9.1.2 Heat Source - electrical or open flame, A-10.2.5 Standard Lead Solution capable of being controlled to a desired rate of heating. Dissolve 1.600 g of lead nitrate in water and make A-9.1.3 Capillary Tubes - of glass, 10 cm long and up the solution to 1 000 ml. Pipette out 10 ml of the 0.8 to 1.2 mm in internal diameter. solution and dilute again to 1 000 ml with water. One millilitre of this solution contains 0.01 mg of lcad Thermometer -calibrated A-9.1.4 against a certified (as Pb). thermometer.

A-9.2 Procedure A-10.3 Procedure

A-9.2.1 Reduce the sample to a fine powder. Fill in A-10.3.1 Place 2 g of sample accurately weighed a capillary tube, which is sealed at one end, sufficient in a plaGnum dish and incinerate for about 2 hours quantity of dry powder 10 form a rolunm 2.5 to 3.5 at 525 to 550 “C. Cool and add 1 to 2 ml of hydrochloric mm in height when packed down as closely as possible. acid and 0.5 ml nitric acid and evaporate to dryness on the steam bath. Dissolve the residue in 5 ml hot A-9.2.2 Heat the bath until a temperature water, evaporate to dryness and treat it with hydrofluoric approximately 30°C below the expected melting poittt acid. Evaporate again to dryness. Dilute it with water is reached. Attach capillary tube containing the (about 50 ml). Filter the solulion, if necessary, with powdered sample to the thermometer by wetting both suction through a fine frilled glass filter and dilute with a drop of liquid paraffin and adjust its height the filtrate and washing to 100 ml in a graduated so that the material in the capillary is in level with Flask. This solution shall be used for tests given in the thermometer bulb. Return the thermometer to the A-10.3.2 and A-11.2.

IS 14137 : 1994 A-10.3.2 Transfer 50 ml of sample solution prepared with four volumes of water, a11d to this add 10 g of in A-10.3.1 in a Nessler cylinder washi11g it with sodiu1n chloride for each 100 1111of the solution. water and add 1 ml of dilute acetic acid. In the second Nessler cylinder, place 1 ml dilute acetic acid and A-11.1.2 Ferric Ammonium Sulphate Solution 2 ml of standard lead solution. Add to each cylinder 10 ml of hydrogen sulphide solution and make up the Dissolve 84 g of ferric ammo11ium sulphate in water volume with water to 100 ml. Mix, allow to stand containing 10 ml of mixed acid and make up to one for 10 minutes and the11 compare the colour produced litre. in the two Nessler cylinders. A-10.3.3 The limit prescribed in Table 1 shall be A-11.1.3 Concentrated Hydrochloric Acid - take11 as 11ot having bee11 exceeded if the inte11sity See IS 265 : 1987. of colour produced in the test with the material is not greater tha11 that produced in the second Nessler A-11.1.4 Stannous Chloride Solution cyli11der which is a control test. Dissolve 80 g of stannous chloride (SnC12.2H,0) in A-11 DETERMINATION OF ARSENIC 100 ml of water containing 5 ml of coiiccntrated A-11.0 Outline of the Method hydrochloric acid. Arsenic present in a solution of the material is reduced A-II.2 Procedure to arsi11e which is made to react with tnercuric bromide paper. The stain produced is compared with a standard stain. Carry out the test as directed in IS 2088 : 1988, adding into the Gutzeit bottle 2 ml of ferric ammonium A-11.1 Reagents sulphate solution, 0.5 ml of stannous chloride solution h-11.1.1 Mixed Acid and 25 ml of the solution as prepared in A-10.3.1. For comparison, prepare a stain using 0’001 mg of Dilute one volume of concentrated sulphuric acid arsenic trioxide.

AkEA PERCENTAGE c 16 228 SQ mm 94.2 c II 14 SQ mm 5.8

CIS AL’OHOL

FIG. 1 GAS CIIROMATOGKAPIUCANAI.YSIS OF CI:INYI. AKOIIOJ.

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Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote harmonious development of the activities of standardization. marking and quality certification of goods and attending to connected matters in the country.

Indian Standards are reviewed periodically and revised, when necessary and amendments, if any, are issued from time to time. Users of Indian Standards should ascertain that they are in possession of the latest amendments or edition.

This Indian Standard has been developed from Dot : No. PCD 18 ( 1175 )

Amendments Issued Slncs Fublicatloo

Amend No. Date of Issue Text Affected

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