1、BRITISH STANDARD BS 6829-2.1: 1988 Analysis of surface active agents (raw materials) Part 2: Alkane sulphonates Section 2.1 Method for determination of total alkane sulphonates content UDC 661.185.1:543.2 112BS6829-2.1:1988 This British Standard, having been prepared under the directionof the Chemic
2、als Standards Committee, was published under the authority ofthe Board of BSI and comesintoeffect on 30December1988 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment87/53363 DC ISBN 0 580 16797 6 Committees responsible for this
3、 British Standard The preparation of this British Standard was entrusted by the Chemicals Standards Committee (CIC/-) to Technical Committee CIC/34, upon which the following bodies were represented: Chemicals Industries Association Consumer Policy Committee of BSI Department of the Environment Depar
4、tment 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 issue CommentsBS6829-2.1:1988 BSI 12-1999 i Contents Page Com
5、mittees responsible Inside front cover Foreword ii 1 Scope 1 2 Definition 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Precision 2 10 Test report 2 Publications referred to Inside back coverBS6829-2.1:1988 ii BSI 12-1999 Foreword This Section ofBS
6、6829 has been prepared under the direction of the Chemicals Standards Committee. The technique described follows that given in ISO6122:1978 “Surface active agents Technical alkane sulphonates Determination of total alkane sulphonates content”, except that reference is made toBS3762-3.16, which diffe
7、rs from the corresponding International Standard method included inISO894. 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 accordance withBS6829-2.
8、1. 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 pages This document compris
9、es 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 front cover.BS6829-2.1:1988 BSI 12-1999
10、 1 1 Scope This Section ofBS6829 describes a method for the determination of total alkane sulphonates content of technical alkane sulphonates containing small quantities of alkanes. It is applicable to all alkali metal salts of the products of sulphochlorination and sulphoxidation of alkanes. NOTETh
11、e titles of the publications referred to in this Section ofBS6829 are listed on the inside back cover. 2 Definition For the purposes of this Section ofBS6829, the following definition applies. 2.1 alkane sulphonate an alkali metal salt of the sulphonic acids present inthe products of sulphochlorinat
12、ion and sulphoxidation of pure straight-chain alkanes ofwhich the chain consists of between12 and20carbon atoms 3 Principle Dispersion of a test portion of the technical alkane sulphonate in a sodium sulphate solution, and addition of a mixture of butan-1-ol and acetone to precipitate sodium sulphat
13、e decahydrate and part of the sodium chloride. Filtration to obtain a mixture of alkane sulphonates (mono- and di-), which may be contaminated by a little sodium chloride. Evaporation of solvent so that the small quantities of alkanes are eliminated, gravimetric determination of the alkane sulphonat
14、es content, and potentiometric determination of any sodium chloride present. 4 Reagents The reagents shall be of a recognized analytical grade. Water complying with grade3 of BS3978 shall be used throughout. 4.1 Acetone 4.2 Butan-1-ol and acetone mixture. Mix three volumes of butan-1-ol with two vol
15、umes of acetone. 4.3 Sodium sulphate, anhydrous,200 g/L solution. 5 Apparatus Ordinary laboratory apparatus and the following are required. 5.1 Boiling flask or crystallizing dish, glass,250mL. 5.2 Oven, capable of being controlled at120 2 C. 5.3 Magnetic stirrer 6 Sampling The laboratory sample sha
16、ll have been prepared and stored in accordance with BS3762-1. 7 Procedure 7.1 Test portion Weigh to the nearest0.001g, into a250mL conical flask a test portion containing approximately0.5g to1g of total alkane sulphonates. 7.2 Determination Add to the test portion (7.1)15mL of the sodium sulphate so
17、lution (4.3) and heat the mixture to50 C, stirring with the magnetic stirrer (5.3). When the suspension is homogeneous, stop the heating and add, while stirring,150mL of the butan-1-ol and acetone mixture (4.2) in a thin trickle. Stopper the conical flask and cool to room temperature. Decant the cle
18、ar phase through a fast filter paper and collect the filtrate in the boiling flask or the crystallizing dish (5.1), previously weighed to the nearest0.001g. Wash the large-grained precipitate and the sides of the conical flask four times, each time with15mL of the butan-1-ol and acetone mixture. Eva
19、porate the filtrate and the added washing solutions to dryness on a boiling water-bath and under a slow stream of cold dry air or nitrogen. To eliminate the last traces of water and unsulphonated matter, dissolve the residue in10mL of the acetone (4.1) in the boiling flask or the crystallizing dish
20、and evaporate to dryness on a water-bath and under a dry unheated stream of air or nitrogen. Repeat this procedure twice more. Dry the residue in the oven (5.2), regulated at120 2 C, for1h, allow to cool in a desiccator to room temperature and weigh to the nearest0.001g.BS6829-2.1:1988 2 BSI 12-1999
21、 To determine the sodium chloride which may be present, dissolve the residue obtained after weighing in80mL of water and20mL of the acetone and determine the sodium chloride content by the method described in BS3762-3.16. NOTEIn the case of alkane sulphonates containing20 carbon atoms in the alkane
22、chain, the procedure for removing unsulphonated matter is not fully effective. 8 Expression of results The total alkane sulphonates content, expressed as a percentage by mass, is given by the following expression: where 9 Precision Comparative analyses on a sample in the form of a homogeneous aqueou
23、s solution containing about25% (m/m) of total soluble matter comprising alkane mono-, di- and polysulphonates in the form of their sodium salts, sodium sulphate and small quantities of alkanes, carried out in18 laboratories, have given the following statistical results: 10 Test report The test repor
24、t shall include the following information: a) a reference to this British Standard, i.e.BS6829-2.1:1988; b) the results expressed in accordance with clause8; c) a complete identification of the sample. m 0 is the mass of the test portion (in g); m 1 is the mass of the residue obtained (in g); T is t
25、he volume of silver nitrate solution used in the determination in BS3762-3.16 (inmL); c is the actual concentration of the silver nitrate solution used for the determination in BS3762-3.16 (in mol/L). m 1 Tc 0.0585 () m 0 -100 mean (percentage by mass) : 24.10; standard deviation of repeatability (s
26、 r ) :0.45; standard deviation of reproducibility (s R ):0.93.BS6829-2.1:1988 BSI 12-1999 Publications referred to BS 3762, Analysis of formulated detergents. BS 3762-1, Methods of sample division. BS 3762-3.16, Method for determination of chloride content. BS 3978, Specification for water for labor
27、atory use. ISO 894, Surface active agents Technical sodium primary alkylsulphates Methods of analysis 1) . ISO 6122, Surface active agents Technical alkane sulphonates Determination of the total alkane sulphonates content 1) . 1) Referred to in the foreword only.BS 6829-2.1: 1988 BSI 389 Chiswick Hi
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