KINGDOM OF SAUDI ARABIA PLES UG eae U ley SASO 492/1987 SAUDI ARABIAN STANDARDKINGDOM OF SAUDI ARABIA. SAUDI ARABIAN STANDARDS ORGANIZATION P.O. BOX 3437, Riyadh 11471 METHODS OF TESTING TOILET SOAP ‘This Saudi mandatory standard is issued in accordance with the rules of the Royal Decree M/10 dated 1392(H)-03-03 Date of SASO-Board of Directors’ Approval : 1408(H)-01-23 (1987-09-16) Date of Publication in the Official Gazette : 1408(H)-03-08 (1987-10-30) Date of Enforcement of this Standard : }408(H).09-08 (1988-04-24) «The Arabic text is the official text having the legal force» Al rights reserved to SASOSAUDI ARABIAN STANDARD SSA 492/1987 METHODS OF TESTING TOILET SOAPS 1- SCOPE AND FI OF APPLICATION ‘This Standard is concerned with the methods of testing toilet soaps in cake form intended for use in personal bathing. It does not apply to soaps containing carbolic acids or speciality soaps such as transparent soap, medicated soap or soap containing synthetic detergents 2 COMPLEMENTARY REFERENCES = Saudi Standard No, 299 «Determination of Moisture and Volatile Matter Content -Oven Method». = Saudi Standard No. 298 «Analysis of Soaps -Determination of Ethanol Insoluble Matter». = Saudi Standard No. 300 «Surface Active Agents -Analysis of Soaps -Determination of Free Caustic Alkali». = Saudi Standard No. 301 «Analysis of Soaps - Determination of Total Free Alkali». = Saudi Standard No. 302 «Analysis of Soaps - Determination of Total Alkali Content and Total Fatty Matter Content», = Saudi Standard No, 303 «Analysis of Soaps - Determination of Unsaponifiable, Unsaponified and Unsaponified Saponifiable Matter» = Saudi Standard No. 304 «Soap - Determination of Chloride Content - Titrimetric Method». ~ Saudi Standard No. 509 «Synthetic Detergents - Part 2 - Methods of Testing Synthetic Powdered Detergents for General Cleaning Purposes». Saudi Standard to be approved by SASO on «Soaps and Synthetic Detergents - Sampling». 3+ REQUIREMENTS The following shall be fulfilled in carrying out the tests: 3.1 The reagents used shall be of an analytical grade. 3.2. The water used shall be distilled PECTION ‘The cakes shall be visually examined to check the following:SAUDI ARABIAN STANDARD ‘SSA 492/1987 41 Marking 4.2 Homogeneity in composition, smoothness to touch and tenacity of the cake. 4.3 The colour of the soap, presence or absence of perfume. 44 Presence or freedom of objectionable odour. 4.5 Not weight of each cake on the condition that weighing shall be carried out on complete unbroken cake. 5- PREPARATION OF THE SAMPLE FOR TESTING The test sample shall be prepared according to Saudi Standard to be approved by SASO on «Soaps and ‘Synthetic Detergents - Sampling». For the preparation of the tests sample the following shall be fulfilled: 5.1 Grind all the cakes of the sample with a suitable food chopper. In case of large sample, it is permissible to grind one half or one quarter from each cake. 5.2 Mix thoroughly all the ground quantities on a clean, dry, non absorbent plane surface, and divide into four equal parts. 5.3 Discard two opposite quarters. Re-mix the remaining two quarters in the same manner until you get a final sample of about I kg. 5.4 Place the final sample directly in a clean, dry, non absorbent air tight container. Label the date of the sampling and the batch number. 6 DETERMINATION OF MOISTURE AND VOLATILE MATTERS The content of moisture and volatile matters shall be determined at (105+2)°C in accordance with the Saudi Standard No. 299 «Soap - Determination of Moisture and Volatile Matter Content - Oven Method. In case of soaps made of fatty materials which are liable to be easily oxidized, the content of moisture and volatile matters shall be determined in accordance with the Saudi Standard No. 309 «Surface Active Agents and Soaps - Determination of Water Content - Azeotro} 7- DETERMINATION OF ETHANOL-INSOLUBLE MATTERS CONTENT ‘The content of ethanol - insoluble matter shall be determined in accordance with the Saudi Standard No, 298 «Analysis of Soaps - Determination of Ethanol - Insoluble Matter. 8- DETERMINATION OF WATER INSOLUBLE MATTERS CONTENT 8.1 Reagents Ethanol, 95% (v/v).SAUDI ARABIAN STANDARD SSA 492/1987 83 8.3.1 83.2 8.3.5 83.8 83.9 8.3.10 84 Apparatus Conical flasks, 500 ml, with conical ground glass joints. Reflux condenser, water-cooled, with a conical ground glass joint. Oven, capable of being controlled at (105 +2)°C. Analytical balance, accurate to 0.001 g. Procedure Weigh, to the nearest 0.01 g, about 5 g of test sample in a 250 ml beaker. Place 200 ml of the ethanol in one of the conical flask, connect the conical flask under the reflux condenser. Heat to gentle boiling, while swirling so as to avoid, as far as possible, the material sticking to the bottom of the conical flask. Dry the filter paper, used for the filteration of the insoluble matter, in the oven controlled at (1052)°C and weigh it; place it in a funnel mounted on a second conical flask. After the dissolution of the soap, decant the supernatant liquid on the filter. Wash the insoluble ‘matters in the same conical flask with the addition of ethanol heated to near its boiling point. Transfer the insoluble matters to the filter paper with the aid of small quantities of warm ethanol. Wash the filter paper and the residue with warm ethanol until it i er ly free from soap. Change the conical flask containing the ethanol-soluble matters by another empty task. ‘Wash the residue on the filter paper five times, each of $0 ml of hot water at a temperature of about 60°C. Dry the filter paper in the oven controlled at (105+ 2)°C. After | hour, remove the filter paper, leave it in the dissicator just long enough to cool completely to ambient temperature and weigh it Repeat the operations of drying in oven, cooling and weighing until the difference in mass between two successive weighings is less than 0.001 g. Record the final weight. Calculation ‘The content of water - insoluble matters, expressed as a percentage by mass, is calculated by using the following formula: Water-insoluble matters, percent = "1 _ x 100 Where: m, = Weight, in grams, of the water-insoluble matters. m = Weight, in grams, of the test sample (on the basis of 12% moisture)SAUDI ARABIAN STANDARD SSA 492/1987 8.5 Report The report shall include the following: 8.5.1 All informations nevessary for the complete identification of the sample. 8.5.2. The results obtained, and the form in which they are expressed. 8.5.3 The method used, and the test conditions. 8.5.4 Any additional details. 9- DETERMINATION OF TOTAL FATTY MATTERS CONTI The content of total fatty matters shall be determined in accordance with the Saudi Standard No. 302 «Analysis of Soaps - Determination of Total Alkali Content and Total Fatty Matter Content», 10. DETERMINATION OF UNSAPONIFIABLE MATTERS’ CONTENT ‘The content of unsaponifiable matters shall be determined in accordance with the Saudi Standard No, 303 «Analysis of Soaps - Determination of Unsaponifiable, Unsaponified and Unsaponified Saponifiable Matter», 11- DETERMINATION OF CHLORIDE CONTENT The content of chloride shall be determined in accordance with the Saudi Standard No, 304 «Soaps ~ Determination of Chloride Content - Titrimetric Method». 12. DETERMINATION OF FREE CAUSTIC ALKALI CONTENT ‘The content of free caustic alkali shall be determined in accordance with the Saudi Standard No. 300 «Surface Active Agents - Analysis of Soaps - Determination of Free Caustic Alkali. 13- DETERMINATION OF TOTAL FREE ALKALI ‘The content of total free alkali shall be determined in accordance with the Saudi Standard No. 301 «Analysis of Soaps - Determination of Total Free Alkali», 14. DETERMINATION OF ACID NUMBER OF FATTY MATTERS 14.1 Separation of the total fatty matters 14.1.1 ReagentsSAUDI ARABIAN STANDARD SSA 492/1987 Madd 14.1.1.2 14.1.2 141.24 14.1.2.2 141.23 14.13 14.3.1 14.1.3.2 14.1.3.3 14134 14.1.3.5 14.136 14.1.3.7 14.1.3.8 14.212 14.213 Sulphuric acid solution, anprosinately 30% (m/v). Add cautiously 1 volume of sulphuric acid, (density 1.84) to 4 vatames of cold water, Methyl orange indicator, 0.04% (m/v) aqueous solution. Apparatus Separating funnel, | litre capacity Electric hot plate. Drying oven. Procedure Weigh 50g to 100g of the test sample in a 800 ml beaker. Dissolve the test portion in about $00 ml hot water. If soaps contain alcohol, the alcohol shall be removed by evaporation. Add 100 ml of sulphuric acid solution, few drops of methyl orange indicator solution, and. check that there shall be an excess of the acid in the solution. Heat the solution tll it boils gently and the fatty matter separates and collects in a clear layer. Draw off the acidic layer (lower), wash the fatty layer with about $00 ml of hot water. Allow to settle and draw off the washing water layer. Repeat the washing of the faity matters with hot water, till the washing is neutral to methyl orange indicator. Note that the washing of the fatty matters shall be done in the least possible time and the separating funnel shall be kept covered during washings to prevent oxidation of the fatty matters. Remove any visible water, while fatty matters are kept in completely melted state, filter the fatty matter through a dry filter paper of coarse porosity. Dry the filter paper in a drying oven controlled at (105 +2)°C for 45-60 minutes, and leave it to cool. Determination of the acid number Reagents Potassium hydroxide solution, 0.5 N acvurately standardized, Ethanol, 95% (V/V) solution, carbon i side tree and shall be neutralized with 0.1N hot potassium hydroxide solution in the presenz2 2° phenolphtahlein indicator, to the appearance of a faint pink colou Phenolphthalein indicator solution 1%, in 95% ethanol.SAUDI ARABIAN STANDARD. ‘SSA 492/1987 14.2.2 14.2.2.1 14.2.2.2 14.2.3 1423.1 14.2.3.2 Procedure Weigh, to the nearest 0.001 g, about 2g of the fatty matters, prepared according to item 14.1, in an Erlenmeyer flask. Add 20-30 ml neutral ethanol and 0.5 ml phenolphthalein indicator solution. Titrate immediately while shaking continuously, with 0 SN potassium hydroxide solution, till the appearance of a faint pink colour that shall last at least for 15 seconds. Expression of Results Caleulation ‘The acid number is expressed as milligrams of potassium hydroxide per gram of fatty matters as in the following formula: Acid number = Y_< N 56.1 Where: M = is the weight, in grams, of the test sample (on the basis of 12% moisture). v is the volume, millilitres, of standard potassium hydroxide used in titration, N = the exact normality of potassium hydroxide solution. ‘The result shall be reported to the nearest 0.1 18- DETERMINATION OF THE TOXIC MINERAL ELEMENTS ‘The content of total toxic mineral elements shall be determined in accordance with the Saudi Standard No, $09 «Synthetic Detergents - Part 2 - Methods of Testing Synthetic Powdered Detergents for General Cleaning Purposes». 16- DETERMINATION OF ROSIN 16.1 16.1.1 16.1.1 16.1.1.2 16.1.2 Test for the presence of rosin (Liebermann-Storch Test) Reagents Acetic anhydride Sulphuric acid, (sp. gr. 1.53). Prepared by adding 34.7 ml of sulphuric acid (sp.gr. 1.84) to 35.7 ml of cold water. Apparatus A white flat porcelain dish. ProcedureSAUDI ARABIAN STANDARD. SSA 492/1987 1613.1 161.82 1614 16.2.1.2 16.2.1.3 16.214 16.2.2.1 16.2.2.2 16.2.3.1 16.2.3.2 16.2.3.3 16.2.3.4 Transfer 1 ml to 2 ml of the fatty acids prepared in accordance with item 14.1 to a test tube, add § to 10 ml acetic anhydride to it and warm gently on a steam bath or a hot plate. Cool the contents, transfer from it 1 to 2 ml into a white porcelain dish and add cautiously several drops of sulphuric acid (sp.et. 1.53), til the two solutions come in contact with each other. Observe the colour of the solution at the interface. The result 4 fugitive violet colour changing to a brownish tinge at the interface, indicates the presence of rosin Devermination of rosin (quantitatively) by MeNicol method Reagents Naphthalene-BSulphonic acid solution: Prepared by dissolving 40 g of Naphthalene- Sulphonic acid in 1000 ml of absolute methanol. Sulphuric acid, dilute solution Potassium hydroxide, 0.2N ethanolic solution: Standerdize against standard sulphuric or hydrochloric acid solution each time when the sotution is used. Phenolphthalein indi (or, 0.5% (m/v) solution in 95% (v/v) ethanol. Apparatus Esteritication flask, round-bottom, capacity 150 ml with a ground glass joint. Suitable glass-water cooled reflux condenser, Procedure Prepare the total fatty acids according to the method specified in item 14.1 Weigh. 10 the nearest 0.001 g, about 2 g of the total fatty acids in the esterification flask. ‘Add 20 ml of naphthalene- B-Sulphonic acid solution and a few glass beads to regulate boiling. Fix the flask to the condenser and heat to boil gently and then leave for 30 minutes. Carry out a blank test at the same time using 20 mi of naphthalene- 8 -Sulphonic acid solution alone. Cool the contents of both flasks and titrate with standard potassium hydroxide solution using, 0.5 ml of phenolphthalein indicator.SAUDI ARABIAN STANDARD 16.2.4 Calculations Percentage of rosin acids by mass of total fatty matter -[ 6.52 (T-1y), ‘| nae yo — Percentage of rosin by mass of total fatty matter = [2] 0 Mi Where: T = volume, in mililitres, of 0.2N potassium hydroxide solution used in titrating the sample. T, = volume, in millitres, of 0.2N potassium hydroxide solution used in the blank M = ‘mass, in grams, of total fatty matter used in the test. 17- DERMATOLOGICAL TESTS. The dermatological tests shall be carried out according to Saudi Standard to be approved by SASO on «Dermatological Tests for Cosmetic Products».SAUDI ARABIAN STANDARDS REFERENCES Main References — American Society for Testing and Materials ASTM D460/1984 «Sampling and Chemical Analysis of Soaps and Soap Products». ~ British Standard BS 1715/1965 «Methods of Analysis of Soaps and Soaps Powders». Other References Indian Standard 1s 286/1978 «Methods of Sampling and Test for Soaps» = Iraqi Standard 108 - 19/1969 «Standard Methods for Chemical Analysis of Soaps», Official and Tentative Methods of the American Oil Chemists Society Vol. 1 11 3rd, Edition, Revision 1973, SSA 492/1987 ew esp eit! lee ASN daabl dele ally VARIES 3 od teh ely GLAS pleat » 6 Splatt Clrsiay Opleall Aglegdt Qa esi — Veie/IVVe hy oA ein abl jaLal doll — Maal dy 2 Oy lall slaty Sly) bef Eb » Aalall LoLal aed — vena 95 GES Sued Stl ll» +4 pall ESA Spall Gla haa «Ad dada yc) let 2 NAVY aly