DKS 2115:2007 DRAFT KENYA STANDARD Soap powder or chips – Specification Public Review Draft March 2007 KENYA BUREAU OF STANDARDS (KEBS) DKS 2115:2007 TECHNICAL COMMITTEE REPRESENTATION The following organizations were represented on the Technical Committee: PZ Cussons EA Unilever Kenya BIDCO (K) Ltd. Mep Chemical Industries K.I.R.D.I Government Chemist University of Nairobi Sanchem Enterprises Ltd. Consumer Information Network Haco Industries Kenya bureau of standards – Secretariat REVISION OF KENYA STANDARDS In order to keep abreast of progress in industry, Kenya Standards shall be regularly reviewed. Suggestions for improvements to published standards, addressed to the Managing Director, Kenya Bureau of Standards, are welcome. © Kenya Bureau of Standards. 2007 Copyright. Users are reminded that by virtue of section 6 of the Copyright Act, Cap. 130 of the Laws of Kenya, copyright subsists in all Kenya Standards and except as provided under section 7 of this Act, no Kenya Standard produced by Kenya Bureau of Standards may be reproduced, stored in a retrieval system in any form or transmitted by any means without prior permission in writing from the Managing Director. ii © KEBS 2007 All rights reserved DKS 2115:2007 DRAFT KENYA STANDARD Soap powder or chips – Specification KENYA BUREAU OF STANDARDS (KEBS) Head Office: P.O. Box 54974 - 00200, Nairobi, Tel.: (+254 020) 605490, 602350, Fax: (+254 020) 604031 E-Mail: info@kebs.org, Web: http://www.kebs.org Coast Region P.O. Box 99376 - 80100, Mombasa Tel.: (+254 041) 2229563, 2230938/40 Fax: (+254 041) 229448 E-mail: kebs_msa@swiftmombasa.com © KEBS 2007 All rights reserved Lake Region P.O. Box 2949 - 40100, Kisumu Tel.: (+254 057) 23549, 22396 Fax: (+254 057) 21814 E-mail: kebs_ksm@swiftkisumu.com North Rift Region P.O. Box 2138 - 20100, Nakuru Tel.: (+254 051) 2210553, 2210555 Fax: (+254 051) 2210076 iii DKS 2115:2007 Foreword This Kenya standard was developed by the Technical Committee on Soaps and Detergents under the guidance of the Chemical Industry Committee, and is in accordance with the procedures of the Bureau. During the preparation of this standard, reference was made to the following document: SABS 245:2000: Specification for Soap powder or chips Acknowledgement is hereby made for assistance derived from this source. iv © KEBS 2007 – All rights reserved KENYA STANDARD DKS 2115: 2007 Soap powder or chips – Specification 1 Scope This Kenya standard specifies requirements and methods of test for four types of soap for use in laundry. 2 Normative references This Kenya Standard incorporates by dated and undated reference, provisions from other publications. These normative references are cited at the appropriate place in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this Kenya Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. KS 45: Methods of analysis for soaps ISO 684:1974: Analysis of soaps - Determination of total free alkali ISO 4323:1977: Soaps - Determination of chlorides content - Potentiometric method ISO 1067:1974: Analysis of soaps - Determination of unsaponifiable, unsaponified and unsaponified saponifiable matter ISO 457:1983: Soaps - Determination of chloride content - Titrimetric method ISO 685:1975: Analysis of soaps - Determination of total alkali content and total fatty matter content ASTM D 502-89: Test method for particle size of soaps and other detergents 3. Definitions For the purpose of this specification the following definitions shall apply: 3.1 Batch Soap manufactured from one boil or, in the case of continuous production processes, the material from a single day’s production. 3.2 Boil Soap from pan or vat. 3.4 Defective Soap or its container that fails in one or more respects to comply with the appropriate requirements of the specification. 3.5 Lot That quantity of soap powder or chips bearing the same batch identification and from one manufacturer, submitted at any one time for inspection and testing. 4. Requirements 4.1 Types The soap shall be of one of the following types Type I High titre soap powder or chips intended for washing at high temperatures with soft water. Type II Low titre soap powder or chips intended for washing at low temperatures with soft water, where the presence of alkaline salts is not desirable. © KEBS 2007 – All rights reserved 1 DKS 2115:2007 Type III High titre, mildly built laundry soap powder intended for general purpose washing with soft water, where the presence of an equal ratio of soap to alkaline salts is desirable. Type IV High titre, fully built laundry soap powder intended for high temperature washing with soft water, where the presence of a high ratio of alkaline salts to soap is desirable. 4.2 General 4.2.1 The soap shall be uniform, free flowing and it shall not contain ingredients in quantities that are toxic to human beings. 4.2.2 It shall possess good lathering properties in water at ambient temperature and having a hardness (expressed as calcium carbonate) of 200 p.p.m. 4.2.3 When stored or transported under normal conditions in its original container, the soap shall not cake into hard lumps. 4.3 Odour The soap, both as received and when dissolved in hot water, shall possess a pleasant, fresh odour and shall not develop an objectionable one during storage at ambient temperature. 4.4 Detailed requirements The soap shall comply with the relevant requirements given in table 1. 2 © KEBS 2007 – All rights reserved DKS 2115:2007 Table 1: Detailed requirements Sl. No. Requirement Property Type I Type II Type III Type IV 0.2 0.2 0.25 0.25 90.0 1.0 90.0 1.0 70.0 1.0 70.0 1.0 82.0 82.0 40.0 22.0 1.0 1.0 1.0 1.0 1.0 1.0 0.5 0.3 - - 15.0 25 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 3.0 3.0 3.0 1.0 38.0 - 27.0 - 38.0 0.5 38.0 0.5 1) Free alkali content* (as NaOH), % (m/m), 2) 3) 4) max Anhydrous matter content+, % (m/m), min Ratio between (the actual anhydrous matter content+ x the average mass of units ‡) and (the specified minimum anhydrous matter content x the marked unit mass), min Fatty matter content+, % (m/m), min 5) Ratio between (the actual fatty matter content+ x the average mass of units ‡) and (the specified minimum fatty matter content x the marked unit mass), min 6) Unsaponified plus unsaponifiable matter content*, % (m/m) max 7) Total alkali content+ (as sodium hydroxide), % (m/m), min 8) Water insoluble matter content*, % (m/m), max 9) Chloride content* (as sodium chloride), % (m/m), max. 10) Rosin content of fatty matter, % (m/m), max 11) Titre of fatty matter, oC, min. Max. 12) Fineness of soap powder: Retained on a 2.80 mm aperture sieve, % (m/m), max. Test Method KS ISO 684 Annex A - KS ISO 685 - KS ISO 1067 KS ISO 685 KS 45 Clause 4 KS ISO 457/4323 KS 45 Clause 9 Annex B ASTM D 502-89 * Corrected to a fatty content of 82 % (m/m) for type I and type II soap powders, 40 % (m/m) for type III soap powder, and 22 % (m/m) for type IV soap powder. + On the soap as received ‡ See 6.1 (b). 2 © KEBS 2007 – All rights reserved DKS 2115:2007 5. Packing and marking 5.1 Packing The soap powder or chips shall be so packed as to prevent excessive drying out, leakage, or contamination of the product. The product shall be packed in containers that are strong enough to withstand normal usage and transportation. These containers may then be packed in bulk packages 5.2 Marking Each container and bulk package shall bear (in prominent, legible, and indelible marking) the following particulars: i) ii) iii) iv) v) vi) vii) viii) ix) Words indicating that the product is a soap powder or soap chips as relevant and the type The name and address of the manufacturer and trade mark if any. The net weight of the contents In the case of bulk packages, the number of containers All ingredients except moisture Batch number or code number Instructions for use Storage instructions Country of origin 6 Sampling and compliance with the specification2) 6.1 Sampling The following sampling procedure shall be applied in determining whether a lot complies with the appropriate requirements of the specification. The samples so drawn shall be deemed to present the lot. a) From the lot take at random 1) 2) if the lot is packed in containers of net mass not exceeding 5 kg: five containers; if the lot is packed in containers of net mass greater than 5 kg: three containers. b) Weigh the contents of each container taken in accordance with (a) above, record these masses, and calculate the average mass. Take enough soap powder from each container to provide a composite sample of total mass at least 1 kg (take approximately equal quantities of soap powder from all containers). Immediately place the sample so drawn in a clean, dry, airtight glass or plastic container clearly marked with the manufacturer’s name or trade mark, the batch identification, and the date of sampling. Note The contents of each container shall be thoroughly mixed before sampling. 6.2 Compliance with the specification The lot shall be deemed to comply with the requirements of the specification if, after inspection and testing of the samples taken in accordance with 6.1, no defective is found. This section applies to the sampling for inspection and testing before acceptance or rejection of single lots (consignments) in cases where no information about the implementation of quality control or testing during manufacture is available to help in assessing the quality of the lot. It is also used as the procedure for adjudicating in cases of dispute. 2) © KEBS 2007 – All rights reserved 3 DKS 2115:2007 7 Inspection Inspect the containers taken in accordance with 6.1 for compliance with the requirements of section 5. 8 Preparation of test samples 8.1 Composite sample Mix the sample, taken in accordance with 6.1(b), thoroughly by hand in the original sample container for at least 2 min 8.1.1 Sample for testing Immediately after mixing the composite sample take at one time all test samples required. Weigh out last the test sample required for the determination of free alkali content and use it immediately. Note Ensure that any loss or pick-up of moisture is reduced to a minimum by carrying out the weighing and the preparation of the sample as rapidly as possible. 4 © KEBS 2007 – All rights reserved DKS 2115:2007 Annex A Determination of anhydrous matter content A.1 Apparatus A.1.1 Flask ― A flask of 500 ml capacity, having a ground-joint neck, and with a round bottom (if a heating mantle is to be used as the means of heating), or with a flat bottom (if a hotplate is to be used as the means of heating). A.1.2 Condenser ― See Fig. 1 A.1.3 Receiver ― A dean and stark type receiver of one of the following sizes, depending on the expected water content of the sample: a) 2 ml capacity graduated in 0.05 ml divisions, for Type I and Type II soap powders (see Fig. 2). b) 7.5 ml capacity graduated in 0.1 ml divisions, for Type III and Type IV soap powders (see Fig. 3). A.1.4 Source of heat ― A heating mantle for 500 ml flasks or a hotplate. Note Before assembling the apparatus, clean the receiver and the inner tube of the condenser thoroughly with chromic-sulphuric acid, then rinse with distilled water followed by acetone, and dry in an oven. A.2 Reagents Note Use only analytical grade reagents and carbon dioxide-free distilled water. 2. A.1 Toluene ― Shake toluene vigorously for approximately 30s with a small quantity of water. Let the water settle, then decant the clear toluene into a distillation flask and distil it. Discard the first, normally turbid fraction of the distillate and use only the following clear fraction for the determination. A.2.2 Anhydrous sodium acetate ― Sodium acetate dried at 105 ± 5oC to constant mass. A.3 Procedure A.3.1 Weigh, to the nearest 0.1 g approximately 20 g of the test sample into the flask. Add to it approximately 10 g of the anhydrous sodium acetate (to prevent violent frothing), 3 - 5 glass beads, and 100 ml of the toluene. Assemble the apparatus and fill the receiver with the toluene by pouring 50 ml of it through the reflux condenser. In order to ensure better control of the distillation, wrap the flask and the tube leading to the receiver in asbestos cloth. A.3.2 Heat the contents of the flask to moderate boiling. At the start the distillation rate should be approximately 100 drops per min, and when the greater part of the water has distilled, the rate should be increased to approximately 200 drops per min. Reflux for at least 2 h. Note Rinse down the reflux condenser during the distillation process with small portions of the toluene in order to collect any water droplets that might adhere to the condenser tube. Any toluene trapped inside the graduated tube of the receiver may be separated from the distilled water by moving a spiral copper wire up and down inside the tube. © KEBS 2007 – All rights reserved 5 DKS 2115:2007 A.3.3 Disconnect the apparatus, allow the receiver to cool to room temperature, and record the volume of the water in the graduated tube. Note When the water volume is read, there shall be no emulsified zone between the solvent and the water layer. A.4 Calculation 4.1 Anhydrous matter content, % (m/m) = 100 A 100 B Where A = volume of water distilled, ml B = mass of the test sample used, g 6 © KEBS 2007 – All rights reserved DKS 2115:2007 Annex B Determination of Titre of fatty matter (Metric units) B.1 Apparatus (see Fig. 1) B.1.1 Water bath ― A two litre low-form beaker B.1.2 Wide-mouth bottle ― An approximately 450 ml bottle that is about 190 mm high, having a neck of inside diameter approximately 40 mm and fitted with a cork that holds the test tube (B.1.3). The bottle contains sufficient lead shot or other dense ballast to hold it steady when placed in the water bath. B.1.3 Test tube ― A test tube of length 100 mm, of inside diameter 25 mm, and marked 57 mm from the bottom to indicate the level to which the sample should be added. It is fitted with a bored cork to support the stirrer and the titre-test thermometer. B.1.4 Stirrer ― A stirrer made from glass or stainless steel of diameter 2-3 mm, and with the lower end formed into a loop 19 mm in diameter. The upper end of the stirrer is shaped as a handle for hand operation. B.1.5 Laboratory thermometer ― A 0 -150oC thermometer B.1.6 Titre-test thermometer ― An ASTM titre-test thermometer, having a range of -2 to +68oC and conforming to the relevant requirements given in ASTM designation E1. B.2 Procedure B.2.1 Heat the fatty matter (retained from the determination of rosin content) to a temperature approximately 10oC above the expected titre and pour sufficient into the test tube to reach the 57 mm mark. Fit the test tube in the wide-mouth bottle and place the assembly in the water bath. The water level should be approximately 10 mm above the 57 mm mark on the test tube. Adjust the temperature of the water bath to 20oC below the expected titre (for titres 35oC and over) or to 15-20oC below expected titre (for titres below 35oC). B.2.2 Ensure that the titre-test thermometer is situated approximately along the axis of the test tube and at such a height that the immersion mark coincides with the top of the sample of fatty matter. B.2.3 When the titre-test thermometer reads 10oC above the expected titre, commence stirring at the rate of about 100 completed up and down strokes per min. (The stirrer should travel through a distance of approximately 40 mm on each stroke.) Read the thermometer every 15s and continue stirring until the temperature remains constant for 30s or just begins to rise. At this point stop stirring, and note the rise in temperature. Record the highest temperature reached. B.2.4 Repeat the procedure given in B.2.1 – B.2.3 B.2.5 The recorded temperatures of the two determinations shall not differ by more than 0.2 oC. (If the difference exceeds 0.2oC, repeat the determination until two readings agree). Report as the titre of the fatty matter, the mean of the tow temperature readings that agree to within 0.2oC. © KEBS 2007 – All rights reserved 7