1、BRITISH STANDARD CONFIRMED JULY1990 BS3762-3.15: 1985 Analysis of formulated detergents Part3: Quantitative test methods Section3.15 Method for estimation of carboxymethylcellulose content NOTEIt is recommended that this Section be read in conjunction with the information in the “General Introductio
2、n”, published separately as BS3762-0. UDC 661.185:543.42:547.458.8BS3762-3.15:1985 This BritishStandard, having been prepared under the directionof the Chemicals Standards Committee, waspublished under the authorityofthe Board of BSI and comes into effect on 31January1985 BSI12-1999 The committees r
3、esponsible for this BritishStandard are shown inPart0. The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment 84/50245 DC ISBN 0 580 14121 7 Foreword This Section of BS3762 has been prepared under the direction of the Chemicals Standards Commit
4、tee and supersedes method D4 of BS3762:1964. This standard describes a method of test only and should not be referred to as a specification defining limits of purity. Reference to the standard should indicate that the method of test used is in conformity with BS3762-3.12. A British Standard does not
5、 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 pages This document comprises a front cover, an inside fr
6、ont cover, pagesi andii, pages1 and2, an inside back cover 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. Amendments issued since publication Amd. No. Date of iss
7、ue CommentsBS3762-3.15:1985 BSI 12-1999 i Contents Page Foreword Inside front cover 1 Scope 1 2 Principle 1 3 Reagents 1 4 Apparatus 1 5 procedure 1 6 Expression of results 1 7 Test report 1 Publications referred to Inside back coverii blankBS3762-3.15:1985 BSI 12-1999 1 1 Scope This Section of BS37
8、62 describes a method of analysis for the estimation of carboxymethylcellulose content of formulated detergents. NOTEThe titles of the publications referred to in this Section are listed on the inside back cover. 2 Principle Hydrolysis and dehydration of the carboxymethylcellulose to furfural deriva
9、tives, which produce a green colour with a solution of anthrone in60% sulphuric acid. The method is not specific for carboxymethylcellulose as most cellulose derivatives, and also other carbohydrates such as sucrose, react similarly. The intensity of the colour decreases with the increase in the deg
10、ree of substitution of the carboxymethylcellulose and it is essential to prepare a standardization graph from similar material to that in the sample, or to express the result in terms of an arbitrary standard. NOTEThe method is based on that reported by Black, H.C. Analytical Chemistry,1951,23,1792-
11、5. 3 Reagents The reagents shall be of a recognized analytical reagent quality. Water complying with the requirements of BS3978 shall be used throughout. 3.1 Kieselguhr 3.2 Sulphuric acid,60% (V/V) solution. Add60mL of the concentrated sulphuric acid ( =1.84g/mL) slowly to40mL of water, cooling well
12、. Dilute to100mL with water when cold. 3.3 Anthrone solution. Dissolve0.2g of anthrone (C 6 H 4 COC 6 H 4 CH 2 ) in about50m L of concentrated sulphuric acid ( =1.84g/mL), which has been added to5mL of water. Cool and dilute to200mL with the concentrated sulphuric acid. Allow the solution to stand f
13、or4h before use. Do not use a solution that is more than24h old. 4 Apparatus Ordinary laboratory apparatus and the following are required. 4.1 One-mark volumetric flasks of capacity50,100 and200mL, complying with the requirements of BS1792. 4.2 Filter, sintered or fritted glass or silica, porosity g
14、rade no.4, complying with the requirements of BS1752. 4.3 Spectrometer (or photoelectric absorptiometer fitted with filters providing maximum transmission at a wavelength of about625nm) and a cell of optical path length10mm. 5 Procedure 5.1 Test portion Weigh1.00g of the well mixed test sample. 5.2
15、Determination Dissolve the test portion in the sulphuric acid solution(3.2), and, using this acid, dilute to100mL in a one-mark volumetric flask. If per-salts are present, heat the test portion for2h in an oven at150 C and then allow it to cool, before dissolving in the acid. Filter the solution thr
16、ough the filter(4.2), using a little kieselguhr(3.1) to aid filtration. Transfer5mL of the filtered solution to a50mL one-mark volumetric flask. Add80mL of the anthrone solution(3.3) in a slow continuous stream to50mL water while stirring. Add30mL of the resulting warm solution to the50mL flask cont
17、aining the sample solution and to a second flask for a blank. Heat the flasks in a boiling water bath for15min. Cool and dilute each to the mark with the sulphuric acid(3.2). Measure the absorbance of the sample solution in a cell of optical path length10mm at625nm against the blank. Prepare a stand
18、ardizing graph from the figures obtained by treating known amounts of carboxymethylcellulose (see clause2) by the above procedure, to cover a suitable range. 6 Expression of results Record the percentage of carboxymethylcellulose in the sample by reference to the graph. 7 Test report The test report
19、 shall include the following information: a) a reference to this BritishStandard, i.e.BS3762-3.15; b) the results and the method of expression used; c) the test conditions.2 blankBS3762-3.15:1985 BSI 12-1999 Publications referred to BS1752, Laboratory sintered or fritted filters. BS1792, One-mark vo
20、lumetric flasks. BS3978, Water for laboratory use. BS3762-3.15: 1985 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level.
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