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1、BRITISH STANDARD BS 6829-5.1: 1990 ISO 6842:1989 Analysis of surface active agents (raw materials) Part 5: Ethoxylated alcohol and alkylphenol sulphates Section 5.1 Method for determination of total active matter content Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006,
2、 Uncontrolled Copy, (c) BSI BS 6829-5.1:1990 This British Standard, having been prepared under the direction of the Chemicals Standards Policy Committee, was published under the authority of the Board of BSI and comes into effect on 31 January 1990 BSI 12-1999 First published February 1987 Second ed
3、ition January 1990 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft (ref. 89/54245) announced in BSI News, October 1989 ISBN 0 580 18182 2 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the
4、Chemicals Standards Policy Committee (CIC/-) to Technical Committee CIC/34, upon which the following bodies were represented: Chemical Industries Association Consumer Policy Committee of BSI Department of the Environment Department of Trade and Industry (Laboratory of the Government Chemist) Ministr
5、y of Defence Royal Society of Chemistry Soap and Detergent Industry Association Society of Dyers and Colourists Amendments issued since publication Amd. No.Date of issueComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1:199
6、0 BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative reference1 3Principle1 4Reagents1 5Apparatus1 6Sampling1 7Procedure1 8Expression of results2 9Test report2 Publication referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na,
7、 Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1:1990 ii BSI 12-1999 National foreword This Section of BS 6829 has been prepared under the direction of the Chemicals Standards Policy Committee. It is identical with ISO 6842:1989 “Surface active agents Sulfated ethoxylated
8、alcohols and alkylphenols Determination of total active matter content”, published by the International Organization for Standardization (ISO). This Section of BS 6829 supersedes the 1987 edition of BS 6829-5.1, which is withdrawn. The principal difference between this Section of BS 6829 and the 198
9、7 edition is the correction of an error in 8.1, although minor editorial modifications have also been made. Additional information. With reference to clause 4, water complying with grade 3 of BS 3978 “Specification for water for laboratory use” is suitable. This Section describes a method of test on
10、ly 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 accordance with BS 6829-5.1. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Stan
11、dards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-reference International StandardCorresponding British Standard ISO 607:1980BS 3762 Analysis of formulated detergents Part 1:1983 Methods of sample
12、division (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 and 2, 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 amendm
13、ent table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1:1990 BSI 12-19991 1 Scope This International Standard specifies a method for the determination of the total active matter present in ordinary co
14、mmercial neutralized products of sulfation of ethoxylated alcohols or alkylphenols alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates). The total active matter comprises the organic material soluble in ethanol (alkylether s
15、ulfates, alkylphenylether sulfates, polyglycol sulfates and non-ionic fractions). 2 Normative reference The following standard contains provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid.
16、 All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standar
17、ds. ISO 607:1980, Surface active agents and detergents Methods of sample division. 3 Principle Boiling, under reflux, of a test portion with ethanol in the presence of sodium sulfate. Filtration, evaporation of the filtrate and weighing of the residue. Determination of any sodium chloride present, b
18、y dissolution of the residue in aqueous acetone and titration with standard volumetric silver nitrate solution. Correction of the mass of the residue for the sodium chloride content. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of
19、 equivalent purity. 4.1 Ethanol, 99 % (V/V). 4.2 Dichloromethane 4.3 Sodium sulfate, anhydrous. 4.4 Acetone, 50 % (V/V) aqueous solution. 4.5 Silver nitrate, standard volumetric solution, c(AgNO3) = 0,1 mol/l. 4.6 Potassium chromate, 100 g/l indicator solution. 5 Apparatus Ordinary laboratory appara
20、tus and: 5.1 Conical flask, of capacity 250 ml, with a ground glass neck. 5.2 Rotary evaporator, with round-bottomed flasks of capacity 250 ml. 5.3 Condenser, to fit the conical flask (5.1). 6 Sampling The laboratory sample of surface active agent shall be prepared and stored in accordance with the
21、requirements of ISO 607. 7 Procedure 7.1 Test portion From the laboratory sample, rendered homogeneous (if necessary) by the addition of a known, appropriate quantity of water, weigh, to the nearest 1 mg, into the conical flask (5.1) a quantity of homogeneous material containing about 0,5 g to 1,5 g
22、 of total active matter. 7.2 Determination Introduce into the conical flask containing the test portion (7.1) 100 ml of ethanol (4.1) and 100 mg of sodium sulfate (4.3), fit the condenser (5.3), and boil under reflux for 30 min. Disconnect the condenser. Rinse the inner wall of the condenser and the
23、 neck of the flask with ethanol, collecting the washings in the flask. Allow to settle. Filter the contents of the conical flask whilst still hot through a fast filter paper into one of the round-bottomed flasks (5.2), previously dried and tared to the nearest 1 mg. Rinse the conical flask with abou
24、t 50 ml of hot ethanol, filtering the washings into the round-bottomed flask. Evaporate the ethanolic solution by means of the rotary evaporator (5.2) maintained at approximately 40 C. Add 10 ml of dichloromethane (4.2) and evaporate. Repeat this step using a further 10 ml of dichloromethane. Remove
25、 the last traces of water by evaporation and leave the flask for a further 15 min on the rotary evaporator. Remove the flask from the rotary evaporator, allow to stand in a desiccator for 15 min and weigh the flask and contents. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:
26、00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1:1990 2 BSI 12-1999 Place the flask on the rotary evaporator for a further 15 min, then allow it to stand in the desiccator for 15 min and again weigh the flask and contents. Repeat the process of drying and weighing until the difference between two con
27、secutive weighings does not exceed 3 mg. Dissolve the residue in 60 ml to 80 ml of the aqueous acetone (4.4). Add 1 ml of the potassium chromate indicator solution (4.6) and titrate with the silver nitrate solution (4.5) until a permanent brown coloration is obtained. 7.3 Blank test Carry out a blan
28、k test at the same time as the determination, using the same reagents and following the same procedure, but omitting the test portion. 8 Expression of results 8.1 Method of calculation The total active matter content, expressed as a percentage by mass, is given by the formula where m0is the mass, in
29、 grams, of the test portion (7.1);1) m1is the mass, in grams, of the residue obtained; cis the actual concentration, in moles of AgNO3 per litre, of the silver nitrate solution (4.5); V0is the volume, in millilitres, of the silver nitrate solution (4.5) used for the blank test (7.3); V1is the volume
30、, in millilitres, of the silver nitrate solution (4.5) used for the determination (7.2) of any sodium chloride present; 0,058 5is the mass, in grams, of sodium chloride corresponding to 1,00 ml of silver nitrate solution, c(AgNO3) = 1,000 mol/l. 8.2 Precision Comparative analyses, carried out in 15
31、laboratories, have given the following statistical results: mean total active matter, % (m/m): 58,67 repeatability standard deviation, r: 0,33 reproducibility standard deviation, R: 0,94 9 Test report The test report shall include the following information: a) all information necessary for the compl
32、ete identification of the sample; b) the method used (a reference to this International Standard); c) the results obtained and the units in which they have been expressed; d) any operational details not specified in this International Standard or in the International Standard to which reference is m
33、ade, and any operation regarded as optional, as well as any incidents likely to have affected the results. 1) Corrected for dilution in the case of heterogeneous products. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1:1990 BSI
34、12-1999 Publication referred to See national foreword. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.1: 1990 ISO 6842:1989 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national
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43、se details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained. If permission is granted, the terms may include royalty payments or a licensing agreement. Details and advice can be obtained from the Copyright Manager. Tel: 020 8996 7070. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI