《BS-6829-1.6-1991 ISO-6839-1982.pdf》由会员分享，可在线阅读，更多相关《BS-6829-1.6-1991 ISO-6839-1982.pdf（10页珍藏版）》请在三一文库上搜索。
1、BRITISH STANDARD BS 6829-1.6: 1991 ISO 6839:1982 Analysis of surface active agents (raw materials) Part 1: General methods Section 1.6 Method for determination of solubility in water Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.
2、6:1991 This British Standard, having been prepared under the direction of the Chemicals Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 31 October 1991 BSI 12-1999 The following BSI references relate to the work on this standard: Committe
3、e reference CIC/34 Draft for comment 91/52314 DC ISBN 0 580 20105 8 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 represen
4、ted: British Association for Chemical Specialities Chemical Industries Association Chemical Industries Association (GOSIP) Department of Trade and Industry (Laboratory of the Government Chemist) Ministry of Defence Royal Society of Chemistry Soap and Detergent Industry Association Amendments issued
5、since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii 0Introduction1 1Scope and field of application1 2
6、Reference1 3Principle1 4Reagent1 5Apparatus1 6Sampling1 7Procedure1 8Expression of results2 9Test report2 Table3 Publication(s) referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 ii BSI 12-1999 Nati
7、onal foreword This Section of BS 6829 has been prepared under the direction of the Chemicals Standards Policy Committee. It is identical with ISO 6839:1982 “Anionic surface active agents Determination of solubility in water”, published by the International Organization for Standardization (ISO). Wit
8、h reference to 5.2, precision thermometers complying with BS 5074:1974 “Specification for short and long solid-stem thermometers for precision use” are technically equivalent to, and may be used in place of, those complying with ISO 653:1980. Additional information. With reference to clause 1, it sh
9、ould be noted that, despite the applicability of the method as stated, in the UK it is considered that the use of the method should be restricted to surface active agent raw materials and not applied to technical products or formulations. With reference to clause 4, water complying with grade 3 of B
10、S 3978:1987 “Specification for water for laboratory use” is suitable. With reference to the Table, the name recommended in the UK for “sodium lauryl sulfate” is “sodium dodecyl sulfate” (see BS 2474:1983 “Recommendations for names for chemicals used in industry”). A British Standard does not purport
11、 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. Cross-references International StandardCorresponding British Standard ISO 60
12、7:1980BS 3762 Analysis of formulated detergents Part 1:1983 Methods of sample division (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, pages 1 to 4, an inside back cover and a back cover. This standard has been updated (see copyright date) a
13、nd may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 BSI 12-19991 0 Introduction The method described in this Inter
14、national Standard is one of the simplest of the methods which can be used for this purpose; it is sufficiently accurate and is suitable for a number of practical uses. 1 Scope and field of application This International Standard specifies a method of establishing the curve representing the solubilit
15、y of an anionic surface active agent in water as a function of temperature, and, consequently, of allowing evaluation of its solubility at a given temperature. The method is applicable both to pure surface active agents and to technical products or formulations of liquid anionic surface active agent
16、s, provided that the solutions of these products are optically clear and are not very strongly coloured. NOTEThe determination of solubility may be carried out without restriction in the temperature range from 0 to 90 C; at temperatures lower than 0 C, the determination is possible provided that the
17、 solution does not freeze. The solubility curve obtained in the case of pure products may possibly allow the Krafft temperature to be determined. 2 Reference ISO 607, Surface active agents and detergents Methods of sample division. 3 Principle Preliminary determination on an aqueous solution of know
18、n anionic surface active agent concentration of the temperatures at which the solution changes, on heating, from being cloudy to clear and, on cooling, from being clear to cloudy. Placing in a bath, controlled at a temperature within the range established in the preliminary determination, of two sol
19、utions of the same concentration, one being colder and cloudy and the other being warmer and clear, and noting the appearance of the two solutions at temperature equilibrium. Repetition of the test, varying the temperature of the bath within the range established by the preliminary determination, un
20、til the clear solution remains clear and the cloudy solution remains cloudy, or the solutions change very slowly from being cloudy to clear or vice versa. From the surface active agent concentrations and the limiting temperatures of solubility, plotting the solubility curve. 4 Reagent During the det
21、ermination, use only distilled water or water of equivalent purity. 5 Apparatus Usual laboratory equipment, and 5.1 Test tubes, made of borosilicate glass, of diameter 20 mm and length 200 mm. 5.2 Precision thermometers, complying with the requirements of ISO 653. 5.3 Thermostatically controlled wat
22、er bath, capable of being controlled at 5 C to + 90 C, to within 0,1 C, with a transparent cell. 6 Sampling The laboratory sample of anionic surface active agent shall be prepared and stored in accordance with the instructions given in ISO 607. 7 Procedure 7.1 Test portion Weigh, to the nearest 0,01
23、 g, the quantity of laboratory sample corresponding to one of the surface active agent concentrations to be studied concentrations usually between 1 and 50 % (m/m) then prepare approximately 100 ml of solution. If the solution contains dispersed impurities, it is advisable to filter it after heating
24、 to a temperature higher than that at which it is cloudy. This procedure shall not involve any alteration of the surface active agent concentration. 7.2 Preliminary determination Transfer approximately 10 ml of the test solution (7.1) to a test tube (5.1) and heat it directly over a flame until the
25、solution becomes clear. Allow to cool slowly in the ambient environment until it becomes cloudy, then slowly raise the temperature again, stirring the solution with a thermometer (5.2), and, as soon as the solution becomes clear, note the temperature (t1). Allow to cool slowly, stirring the solution
26、 with the thermometer, and, as soon as the solution becomes cloudy, note the temperature (t2). The temperature range thus determined is generally of the order of 10 C. 7.3 Determination of the limiting temperature of solubility Set the thermostatically controlled bath (5.3) at a temperature within t
27、he range defined by the preliminary determination (7.2) and keep it constant to within 0,1 C. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 2 BSI 12-1999 Fill two test tubes (5.1) with the solution (7.1), stopper them, adj
28、ust their temperatures so that the solution in one becomes clear and the solution in the other becomes cloudy, and then place them in the thermostatically controlled bath. When the temperatures of the two solutions are equal to that of the water bath, note whether the two solutions are clear or clou
29、dy. If both solutions are clear, lower the temperature of the water bath by a few degrees Celsius if both solutions are cloudy, raise it to a slightly higher temperature and repeat the above test. Carry out a third test, or more if necessary, controlling the bath at a temperature deduced from the pr
30、evious tests, until the change in appearance of the solutions (cloudy to clear or clear to cloudy) occurs very slowly or the clear solution remains clear and the cloudy solution remains cloudy. A maximum observation period of 2 to 3 h may be adopted. Note the temperature at which this occurs to the
31、nearest 0,1 C, as the limiting temperature of solubility. If the appearance of the solutions remains unchanged, take the temperature immediately below that at which the two solutions remained cloudy. NOTEThe speed with which the limpidity and cloudiness are reversed is a function of the temperatures
32、 t1 and t2 determined in 7.2 in relation to that of the bath. 7.4 Plotting the solubility curve Repeat the above procedures (7.1, 7.2 and 7.3), using different quantities of test portion so as to cover the range of concentrations to be studied. Plot the solubility curve as a function of the concentr
33、ations and corresponding limiting temperatures of solubility. This curve makes it possible to deduce the solubility of the surface active agent at a given temperature; determine, if required, the Krafft temperature. 8 Expression of results 8.1 Method of calculation Express the solubility of the anio
34、nic surface active agent in water, for a given temperature, as a percentage by mass. 8.2 Precision Comparative analyses on samples of three different surface active agents, carried out in eight laboratories, have provided the information given in the Table. 9 Test report The test report shall includ
35、e the following information: a) all the information necessary for the complete identification of the sample and details of the treatment of the test portion (and, if required, the temperature to which the solution was heated before filtration); b) the reference of the method used (reference to this
36、International Standard); c) the results obtained and the method of expression used: temperature (t1) at which the solution becomes cloudy for the concentration being studied; temperature (t2) at which the solution becomes clear for the concentration being studied; limiting temperature of solubility
37、for the concentration being studied; d) if necessary, the solubility curve (and the Krafft temperature, if required); e) details of any operations not specified in this International Standard or regarded as optional, together with details of any incidents likely to have affected the results. License
38、d Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 BSI 12-19993 Table Surface active agent Concentration Mean observed limiting temperature of solubility Standard deviation of reproducibility % (m/m)CC Sodium laurate, purity 96,4 % 2,
39、5 5 10 20 30 24 27,7 31,7 38,6 42,7 2 1,7 2 1,6 1,6 Sodium lauryl sulphate, purity 99 % 2,5 5 10 20 30 14 15,3 17 19,8 22,1 1,2 1,6 1,2 1,3 1,4 Sodium alkane sulphonate, purity 98 % 40 41 42 43 45 13,5 17,7 23 34,7 57,5 1,5 1 2,5 3 3,5 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28
40、GMT+00:00 2006, Uncontrolled Copy, (c) BSI 4 blank Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6:1991 BSI 12-1999 Publication(s) referred to See national foreword. Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:36:28
41、 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-1.6: 1991 ISO 6839:1982 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the internati
42、onal level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We wo
43、uld be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: 020 8996 9000. Fax: 020 8996 7400. BSI offers members an individual upd
44、ating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel: 020 8996 9001. Fax: 020 8996 7001. In response to orde
45、rs for international standards, it is BSI policy to supply the BSI implementation of those that have been published as British Standards, unless otherwise requested. Information on standards BSI provides a wide range of information on national, European and international standards through its Librar
46、y and its Technical Help to Exporters Service. Various BSI electronic information services are also available which give details on all its products and services. Contact the Information Centre. Tel: 020 8996 7111. Fax: 020 8996 7048. Subscribing members of BSI are kept up to date with standards dev
47、elopments and receive substantial discounts on the purchase price of standards. For details of these and other benefits contact Membership Administration. Tel: 020 8996 7002. Fax: 020 8996 7001. Copyright Copyright subsists in all BSI publications. BSI also holds the copyright, in the UK, of the pub
48、lications of the international standardization bodies. Except as permitted under the Copyright, Designs and Patents Act 1988 no extract may be reproduced, stored in a retrieval system or transmitted in any form or by any means electronic, photocopying, recording or otherwise without prior written pe
49、rmission from BSI. This does not preclude the free use, in the course of implementing the standard, of necessary details such as symbols, and size, type or grade designations. If these 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 14:36:28