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 contentBS6829-5.1:1990 This British Standard, having been prepared under the directiono
2、f the Chemicals Standards Policy Committee, waspublished under the authorityof the Board of BSIandcomes into effect on 31January1990 BSI 12-1999 First published February1987 Second edition January1990 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft
3、(ref. 89/54245) announced in BSI News, October1989 ISBN 0 580 18182 2 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 repres
4、ented: Chemical Industries Association Consumer 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 Amendme
5、nts issued since publication Amd. No. Date of issue CommentsBS6829-5.1:1990 BSI 12-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope 1 2 Normative reference 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Tes
6、t report 2 Publication referred to Inside back coverBS6829-5.1:1990 ii BSI 12-1999 National foreword This Section of BS6829 has been prepared under the direction of the Chemicals Standards Policy Committee. It is identical with ISO6842:1989 “Surface active agents Sulfated ethoxylated alcohols and al
7、kylphenols Determination of total active matter content”, published by the International Organization for Standardization (ISO). This Section of BS6829 supersedes the1987 edition of BS6829-5.1, which is withdrawn. The principal difference between this Section of BS6829 and the1987 edition is the cor
8、rection of an error in8.1, although minor editorial modifications have also been made. Additional information. With reference to clause4, water complying with grade3 of BS3978 “Specification for water for laboratory use” is suitable. This Section describes a method of test only and should not be use
9、d 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 BS6829-5.1. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for
10、 their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-reference International Standard Corresponding British Standard ISO 607:1980 BS 3762 Analysis of formulated detergents Part 1:1983 Methods of sample division (Identical) Su
11、mmary of pages This document comprises a front cover, an inside front 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 fro
12、nt cover.BS6829-5.1:1990 BSI 12-1999 1 1 Scope This International Standard specifies a method for the determination of the total active matter present in ordinary commercial neutralized products of sulfation of ethoxylated alcohols or alkylphenols alkyl oxyethylene sulfates (ethoxylated alcohol sulf
13、ates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates). The total active matter comprises the organic material soluble in ethanol (alkylether sulfates, alkylphenylether sulfates, polyglycol sulfates and non-ionic fractions). 2 Normative reference The following standard contains
14、 provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate th
15、e possibility of applying the most recent edition of the standard indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 607:1980, Surface active agents and detergents Methods of sample division. 3 Principle Boiling, under reflux, of a test portion
16、 with ethanol in the presence of sodium sulfate. Filtration, evaporation of the filtrate and weighing of the residue. Determination of any sodium chloride present, by dissolution of the residue in aqueous acetone and titration with standard volumetric silver nitrate solution. Correction of the mass
17、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 equivalent purity. 4.1 Ethanol, 99% (V/V). 4.2 Dichloromethane 4.3 Sodium sulfate, anhydrous. 4.4 Acetone, 50% (V/V) aqueous solution.
18、 4.5 Silver nitrate, standard volumetric solution,c(AgNO 3 ) = 0,1mol/l. 4.6 Potassium chromate, 100g/l indicator solution. 5 Apparatus Ordinary laboratory apparatus and: 5.1 Conical flask, of capacity250ml, with a ground glass neck. 5.2 Rotary evaporator, with round-bottomed flasks of capacity250ml
19、. 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 requirements of ISO607. 7 Procedure 7.1 Test portion From the laboratory sample, rendered homogeneous (if necessary) by the addition of a know
20、n, appropriate quantity of water, weigh, to the nearest1mg, into the conical flask (5.1) a quantity of homogeneous material containing about0,5g to1,5g of total active matter. 7.2 Determination Introduce into the conical flask containing the test portion (7.1)100ml of ethanol (4.1) and100mg of sodiu
21、m sulfate (4.3), fit the condenser (5.3), and boil under reflux for30min. Disconnect the condenser. Rinse the inner wall of the condenser and the 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
22、 fast filter paper into one of the round-bottomed flasks (5.2), previously dried and tared to the nearest1mg. Rinse the conical flask with about50ml of hot ethanol, filtering the washings into the round-bottomed flask. Evaporate the ethanolic solution by means of the rotary evaporator (5.2) maintain
23、ed at approximately40 C. Add10ml of dichloromethane(4.2) and evaporate. Repeat this step using a further10ml of dichloromethane. Remove the last traces of water by evaporation and leave the flask for a further15min on the rotary evaporator. Remove the flask from the rotary evaporator, allow to stand
24、 in a desiccator for15min and weigh the flask and contents.BS6829-5.1:1990 2 BSI 12-1999 Place the flask on the rotary evaporator for a further15min, then allow it to stand in the desiccator for15min and again weigh the flask and contents. Repeat the process of drying and weighing until the differen
25、ce between two consecutive weighings does not exceed3mg. Dissolve the residue in60ml to80ml of the aqueous acetone (4.4). Add1ml 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
26、out a blank 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 m 0 is
27、the mass, in grams, of the test portion(7.1); 1) m 1 is the mass, in grams, of the residue obtained; c is the actual concentration, in moles of AgNO 3per litre, of the silver nitrate solution(4.5); V 0 is the volume, in millilitres, of the silver nitrate solution (4.5) used for the blank test(7.3);
28、V 1 is the volume, 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 to1,00ml of silver nitrate solution, c(AgNO 3 )=1,000mol/l. 8.2 Precision Comparative analyses, carri
29、ed out in15 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
30、for the complete 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 r
31、eference is made, 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.BS6829-5.1:1990 BSI 12-1999 Publication referred to See national foreword.BS 6829-5.1: 1990 ISO 6842:1989 BSI 389 Ch
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