1、BRITISH STANDARD BS 6829-4.2: 1989 ISO 2268:1972 Analysis of surface active agents (rawmaterials) Part4: Ethylene oxide adducts Section4.2 Method for determination ofpolyethylene glycols and non-ionic active matter contents UDC 661.185.1.014:543.8+661.185.211.2.014:547.222.2:543.832BS6829-4.2:1989 T
2、his British Standard, having been prepared under the directionof the Chemicals Standards Policy Committee, waspublished under the authorityof the Board of BSI andcomes into effect on 31August1989 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/34
3、 Draft for comment88/52457 DC ISBN 0 580 17444 1 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Chemicals Standards Policy Committee (CIC/-) to Technical CommitteeCIC/34, upon which the following bodies were represented: Chemical Indust
4、ries 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 Amendments issued since publi
5、cation Amd. No. Date of issue CommentsBS6829-4.2:1989 BSI 12-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope 1 2 Field of application 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Procedure 1 7 Expression of results 3 8 Test report 3 Annex Maintenance of te
6、mperature during the separations 4 Appendix General diagram of separations 6 Figure Suitable type of separating funnel with jacket 5 Publications referred to Inside back coverBS6829-4.2:1989 ii BSI 12-1999 National foreword This Section ofBS6829 has been prepared under the direction of the Chemicals
7、 Standards Policy Committee. It is identical withISO2268:1972 “Surface active agents (non-ionic) Determination of polyethylene glycols and non-ionic active matter (adducts) Weibull method” published by the International Organization for Standardization (ISO). Additional information. With reference t
8、oclause4, water complying with grade3 ofBS3978 is suitable. Textual error. InA.2, line8, the expression “Figure2” should be read as “theFigure”. 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 shoul
9、d indicate that the method of test used is in accordance withBS6829-4.2. 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 i
10、mmunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, pages1 to6, 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
11、amendment table on the inside front cover.BS6829-4.2:1989 BSI 12-1999 1 1 Scope This International Standard specifies a method for the determination of polyethylene glycols and non-ionic active matter (adducts) in fatty alcohol and alkylphenol polyoxyethylate derivatives. Generally the commercial pr
12、oducts contain polyethylene glycols as a by-product. The Weibull method allows the determination of both the non-ionic active matter (adducts) and the polyethylene glycols impurity. 2 Field of application Alkyl and alkylphenol polyoxyethylates correspond to the formulae(1) and(2) given below: where
13、n is a mean number of oxyethylene (CH 2 CH 2 O) groups per molecule of hydrophobe and R is, in formula(1), a straight or branched chain alkyl group, usually comprising C 10to C 18 , and, in formula(2), a branched chain alkyl group, usually nonyl or tertiary octyl. The method is applicable to all com
14、mercial non-ionic surface active agents containing from2 to80oxyethylene groups per molecule. 3 Principle The method relies on the facts that both non-ionic adducts and polyethylene glycols are soluble in sodium chloride solution, but one is soluble in ethyl acetate whereas the other is not. Separat
15、ion of the polyethylene glycols and the adducts is, therefore, possible by the following method: Dissolution of the sample in ethyl acetate and extraction, at35 1 C, of polyethylene glycols by sodium chloride solution and successive washes of the sodium chloride solution by ethyl acetate, and of the
16、 ethyl acetate by the sodium chloride solution. Extraction of the polyethylene glycols isolated in the sodium chloride solution with chloroform, removal of the solvent and weighing of the residue. Evaporation of the ethyl acetate solution which contains the adducts and weighing of the residue. 4 Rea
17、gents The water used shall be distilled water or water of at least equivalent purity. The reagents used shall have the following properties. 4.1 Ethyl acetate, 20 =0,90g/ml, distilling between75,5 and77,5 C. 4.2 Sodium chloride solution Dissolve300g of sodium chloride in1000ml of distilled water. 4.
18、3 Chloroform, 20 =1,48g/ml, distilling between59,5 and61,2 C. 4.4 Acetone, anhydrous, 20 =0,79g/ml, distilling between55 and57 C. 4.5 Light petroleum, distilling between40 and60 C. 5 Apparatus Ordinary laboratory apparatus and: 5.1 Separating funnels 5.1.1 three separating funnels, capacity250ml, wi
19、th ground glass stoppers, for method1 (seeAnnex). 5.1.2 three separating funnels, capacity250ml, with ground glass stoppers and jackets, according toFigure, for method2 (seeAnnex). 5.2 One separating funnel, capacity500ml, with ground glass stopper. 5.3 Two flasks, capacity250ml, wide-necked, with g
20、round glass stoppers. 5.4 Conical flask, capacity500ml, wide-necked flat-bottomed. 6 Procedure 6.1 Preparation of the sample 6.1.1 Liquid products If the sample is a clear liquid, stir it with a glass rod or spoon to ensure that the sample is homogeneous. If the liquid is cloudy or contains a solid
21、deposit, heat the product slowly to45 C maximum, leaving the cover or the stopper of the container in position until the liquid is clear. Then stir with a glass rod or spoon to obtain a homogeneous sample. 6.1.2 Solid products If the sample is in a solid form, heat it slowly to45 C maximum, as descr
22、ibed above, in a dry oven until the sample has just melted. RO(CH 2 CH 2 O) n H .(1) .(2)BS6829-4.2:1989 2 BSI 12-1999 Remove from the oven and stir until solidification is well advanced and stirring is impossible. Allow the sample to cool to room temperature. 6.2 Test portion Weigh, to the nearest0
23、,01g,5 0,05g of a sample prepared as described in6.1. 6.3 Determination 6.3.1 Separation of the polyethylene glycols and adducts During this separation, all the operations, including the rest phases, shall be carried out at35 1 C, the reagents and glassware having beforehand been raised to this temp
24、erature (seeAnnex). Dissolve the test portion in the ethyl acetate(4.1) and transfer it quantitatively to the250ml separating funnel(5.1) (A), bringing the final volume to75ml. Add50ml of the sodium chloride solution(4.2), shake to mix well, leave standing for about30min or until the two phases are
25、well separated and then run the sodium chloride solution into the second250ml separating funnel(5.1) (B). Again add50ml of the sodium chloride solution(4.2) to the ethyl acetate solution contained in funnel (A) and begin the extraction operation again under the same conditions as before, collecting
26、the sodium chloride solution in funnel (B). Repeat the extraction for a third time, again with50ml of the sodium chloride solution(4.2). Add25ml of the ethyl acetate(4.1) to funnel (B), which now contains the three portions of sodium chloride solution, shake, leave standing for about30min, and then
27、run the sodium chloride solution into the third250ml separating funnel(5.1) (C). Add25ml of the ethyl acetate(4.1) to funnel (C) and start the washing process again, under the same conditions as above, collecting the sodium chloride solution in the500ml separating funnel(5.2) (D). Transfer the ethyl
28、 acetate from funnel (C) to funnel (B). Add25ml of the sodium chloride solution(4.2) to funnel (B), which now contains the two portions of ethyl acetate used for washing the sodium chloride solution. Shake, allow the phases to separate and run the sodium chloride solution into funnel (C). Use this s
29、olution to rinse funnel (C) and transfer this rinse to funnel (D). Rinse funnel (C) with10ml of sodium chloride solution(4.2) and transfer this rinse to funnel (D). Funnel (D) now contains the sodium chloride solution in which the polyethylene glycols are to be found, while the adducts are in soluti
30、on in the ethyl acetate contained in funnels (A) and (B). 6.3.2 Determination of adducts Transfer the ethyl acetate solution in funnel (A) to the250ml wide-neck flask(5.3) and evaporate the solvent. Rinse funnel (A) with the ethyl acetate solution contained in funnel (B), then transfer this solution
31、 to the250ml flask. Pour25ml of the ethyl acetate(4.1) into funnel (B) to rinse it, transfer this rinse to funnel (A) to rinse it also, then run into the250ml flask. Repeat this operation with25ml of the ethyl acetate(4.1) then evaporate if off completely. Dissolve the residue in75ml of the ethyl ac
32、etate(4.1), heat at45 C and filter immediately through filter paper (Whatman No.541,9cm diameter or equivalent) collecting the filtrate in the tared250ml flask(5.3) fitted with a ground glass stopper. Rinse the first flask and the filter paper six times with10ml portions of warm ethyl acetate(4.1),
33、always collecting the filtrate in the tared flask. Completely evaporate the solvent on a steam bath. Dry the residue by adding10ml of the acetone(4.4), evaporate it off, then remove as much solvent vapour as possible by passing a stream of cold dry air through the flask. Repeat these operations with
34、 a further10ml of the acetone(4.4). Then add10ml of the light petroleum(4.5), evaporate off and remove the last traces of solvent vapour with a stream of cold dry air. Stopper the flask, cool in a desiccator and weigh after releasing and immediately replacing the stopper. Heat the flask in an oven a
35、t100 C for10min, blow out with a stream of cold dry air, replace the stopper, allow to cool and weigh again. Repeat these heating and weighing operations until the difference between two consecutive weighings does not exceed0,1% of the mass of active matter. 6.3.3 Determination of polyethylene glyco
36、ls Add100ml of the chloroform(4.3) to separating funnel (D) containing the sodium chloride solution, shake, leave to stand for at least15min and run the chloroform phase into the500ml conical flask(5.4). Repeat this operation twice more, each time with100ml of the chloroform(4.3). Evaporate off the
37、chloroform. Dissolve the residue in50ml of the chloroform(4.3), filter through filter paper (Whatman No.541,9cm diameter or equivalent) and collect the filtrate in a tared, wide-neck flask with a ground glass stopper. Rinse the original flask and filter paper six times with10ml portions of warm chlo
38、roform(4.3) always collecting the filtrate in the tared flask. Evaporate off the solvent on a steam bath.BS6829-4.2:1989 BSI 12-1999 3 Dry the residue twice with30ml of the acetone(4.4) and once with10ml of the light petroleum(4.5) using the same procedure as described in6.3.2. Then weigh as before.
39、 NOTEA general diagram of the separation procedures is given inanAppendix. 7 Expression of results The percentage by mass of polyethylene glycols in the sample is equal to The percentage by mass of non-ionic active matter (adducts) is equal to where m 0 is the mass, in grams, of the test portion; m
40、1 is the mass, in grams, of polyethylene glycols, weighed as described in6.3.3; m 2 is the mass, in grams, of adducts, weighed as described in6.3.2. 8 Test report The test report shall include the following particulars: a) all information necessary for the complete identification of the sample; b) t
41、he method used, reference being made to this International Standard; c) the results obtained; d) the test conditions; e) any operational details not specified in this International Standard, or optional, as well as all incidents likely to have influenced the results. m 1 100 m 0 - m 2 100 m 0 -BS682
42、9-4.2:1989 4 BSI 12-1999 Annex Maintenance of temperature during the separations The two following techniques may be used for maintaining the temperature during the separations. A.1 Method 1 The separations are carried out either in a small room or in a large cupboard, maintained at35 1 C by means o
43、f a thermostat, in which the reagents and apparatus shall be kept permanently. Dissolving the sample and all the separations shall be carried out at this temperature and the separating funnels(5.1.1) used shall not, under any circumstances, be withdrawn from this room until all the separations with
44、ethyl acetate have been completed. (The extraction of polyethylene glycols from the sodium chloride solution with chloroform may be carried out at ambient temperature.) A.2 Method 2 The separations are carried out in separating funnels with ground glass stoppers and jackets(5.1.2). These jackets are
45、 fitted with inlets and outlets, like reflux condensers, which enable water, at a temperature controlled by a thermostat, to circulate continuously between the double walls so that the content of the funnels can be maintained at a suitable temperature. The dimensions and form of such a funnel are gi
46、ven inFigure2.BS6829-4.2:1989 BSI 12-1999 5 Figure Suitable type of separating funnel with jacket(5.1.2)BS6829-4.2:1989 6 BSI 12-1999 Appendix General diagram of separationsBS6829-4.2:1989 BSI 12-1999 Publications referred to Seenational foreword.BS 6829-4.2: 1989 ISO 2268:1972 BSI 389 Chiswick High
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