1、BRITISH STANDARD BS1715-2.11: 1989 ISO673:1981 Analysis of soaps Part 2: Quantitative test methods Section 2.11 Method for determination of ethanol-insoluble matter content ISO title: SoapsDetermination of content of ethanol-insoluble matter UDC 661.18:543BS1715-2.11:1989 This British Standard, havi
2、ng been prepared under the directionof the Chemicals Standards Policy Committee, waspublished under the authorityof the Board of BSI andcomes into effect on 31July1989 BSI 09-1999 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment 88/53272
3、DC ISBN 0 580 17321 6 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Chemicals Standards Policy Committee (CIC/-) to Technical Committee CIC/34, upon which the following bodies were represented: Chemical Industries Association Consumer
4、Policy Committee of BSI Department of the Environment Department of Trade and Industry (Laboratory of the Government Chemist) Ministry of Defence Royal Society of Chemistry Soap and Detergent Industry Association Society of Dyers and Colourists Amendments issued since publication Amd. No. Date of is
5、sue CommentsBS1715-2.11:1989 BSI 09-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope and field of application 1 2 Definition 1 3 Principle 1 4 Reagent 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Test report 2BS1715-2.11:1989 ii BS
6、I 09-1999 National foreword This Section of BS 1715 has been prepared under the direction of the Chemicals Standards Policy Committee. It is identical with ISO673:1981 “Soaps Determination of content of ethanol-insoluble matter” published by the International Organization for Standardization (ISO).
7、This method supersedes the method “Determination of matter insoluble in ethanol” given in BS1715:1963, which is deleted by amendment. Terminology and conventions. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some termin
8、ology and certain conventions are not identical with those used in British Standards; attention is drawn especially to the following. The comma has been used as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. The symbol “ml” ha
9、s been used to denote millilitre. In British Standards it is current practice to use the symbol “mL”. Wherever the words “International Standard” appear, referring to this standard, they should be read as “Section of BS1715”. Additional information. For the purposes of4.1, the ethanol may be replace
10、d by industrial methylated spirits complying with BS 3591 “Specification for industrial methylated spirits” of appropriate strength. It should be noted that the use of industrial methylated spirits is governed by the Methylated Spirits Regulations, 1983 (SI 1983 No.252). It is not permissible to use
11、 duty-free ethanol, received under the provisions of the Alcoholic Liquors Duties Act1972, Section10, for purposes for which industrial methylated spirits is an acceptable alternative. With reference to clause6, information on sampling is included in BS1715 “Analysis of soaps”, Part 1:1989 “General
12、introduction, sampling, and test for presence of synthetic anionic-active surface active agents.” This Section describes a method of test only, and should not be used or quoted as a specification defining limits of purity. Reference to this Section should indicate that the method of test used is in
13、accordance with BS1715-2.11. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of p
14、ages This document comprises a front cover, an inside front cover, pagesi andii, pages1and2 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS1715-2.11:1989 BSI 09-
15、1999 1 1 Scope and field of application This International Standard specifies a method for the determination of the content of ethanol-insoluble matter in commercial soaps, excluding compounded products. 2 Definition For the purpose of this International Standard, the following definition applies. e
16、thanol-insoluble matter the matter not dissolved by the procedure specified in this International Standard NOTE1The ethanol-insoluble matter corresponds to the additives and foreign matter, of low solubility or insoluble in95%(V/V) ethanol, added to soaps, and also to substances in all soap formulat
17、ions, such as alkali carbonates and chlorides, of low solubility in95%(V/V) ethanol. NOTE2The foreign matter may be inorganic (carbonates, borates, perborates, chlorides, sulphates, silicates, phosphates, iron oxides, etc.) or organic (starches, dextrins, caseins, sugars, cellulose derivatives, algi
18、nates, etc.). 3 Principle Dissolution of the soap in ethanol, filtration and weighing of the undissolved residue. 4 Reagent 4.1 Ethanol, 95%(V/V). 5 Apparatus Ordinary laboratory apparatus and 5.1 Conical flasks, of capacity 500ml, having ground glass necks. 5.2 Reflux condenser, water-cooled, with
19、a conical ground glass joint at the bottom to fit the conical flasks (5.1). 5.3 Water bath 5.4 Oven, capable of being controlled at103 2 C. 5.5 Analytical balance, accurate to 0,001 g. 6 Sampling Procedures for the preparation and storage of the laboratory sample will form the subject of a future In
20、ternational Standard. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,01 g, about 5 g of the laboratory sample into a conical flask (5.1). 7.2 Determination Add 200 ml of the ethanol (4.1) to the test portion(7.1) in the conical flask and connect the reflux condenser (5.2). Heat to gentle boili
21、ng, swirling in order to avoid, as far as possible, material adhering to the bottom of the flask. Dry the filter paper to be used for the filtration of the insoluble matter in the oven (5.4), controlled at103 2 C, for1h. Allow it to cool to ambient temperature in a desiccator and weigh it to the nea
22、rest0,001g. Place it in a funnel mounted on a second conical flask (5.1). When dissolution of the soap appears to be complete, decant the supernatant liquid on to the filter paper, wash the insoluble matter in the conical flask by decantation with the ethanol(4.1), previously heated to near its boil
23、ing point, and transfer the insoluble matter to the filter paper with the aid of small quantities of warm ethanol(4.1). Wash the filter paper and the residue with the warm ethanol until entirely free from soap. 1) During this operation, it is advantageous to place the conical flask carrying the funn
24、el on the water bath (5.3) so as to keep the flitrate gently boiling. An independently heated funnel may also be used. At the same time, cover the funnel with a watch glass. By this means, cooling of the wash liquor is avoided and ethanol vapour, which condenses on the watch glass and drops back on
25、the filter paper completes the washing of the latter. Dry the filter paper in air and then place it in the oven (5.4), controlled at103 2 C. After1h, remove the filter paper, leave it in the desiccator just long enough for it to cool completely to ambient temperature and weigh it. Repeat the operati
26、ons of drying in the oven, cooling and weighing until the difference in mass between two successive weighings is less than0,001g. Note the final mass. NOTEWith certain soaps, especially silicated soaps, the insoluble matter cannot be completely detached from the bottom of the conical flask. In this
27、case, after thoroughly washing the residue with ethanol, dissolve it in a little hot distilled water. Transfer this solution to a weighed evaporating dish, evaporate on the boiling water bath and dry in the oven (5.4), controlled at103 2 C. Allow to cool in a desiccator and weigh. Repeat the operati
28、ons of drying (for periods of 1 h), cooling and weighing until the difference in mass between two successive weighings is less than0,001g. Add this mass to that of the residue on the filter paper. 1) The final washings should show no appreciable residue on evaporation.BS1715-2.11:1989 2 BSI 09-1999
29、8 Expression of results 8.1 Calculation The content of ethanol-insoluble matter, expressed as a percentage by mass, is given by the formula 8.2 Reproducibility The difference between the results obtained on the same sample in two different laboratories shall not exceed0,05 % for contents of ethanol-
30、insoluble matter less than or equal to1%, and shall not exceed0,1% for contents of ethanol-insoluble matter higher than1%. 9 Test report The test report shall include the following particulars: a) all information necessary for the complete identification of the sample; b) the reference of the method
31、 used (reference to this International Standard); c) the results, together with the form in which they are expressed; d) the test conditions; e) any operations not specified in this International Standard, or regarded as optional, as well as any incidents likely to have affected the results. where m
32、 0 is the mass, in grams, of the test portion; m is the mass, in grams, of the residue. m m 0 -100 blankBS1715-2.11: 1989 ISO673:1981 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents t
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