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1、BRITISH STANDARD BS 6829-5.2: 1989 ISO 6843:1988 Analysis of surface active agents (raw materials) Part 5: Ethoxylated alcohol and alkylphenol sulphates Section 5.2 Method for estimation of mean relative molecular mass ISO title: Surface active agents Sulfated ethoxylated alcohols and alkylphenols E
2、stimation of the mean relative molecular mass UDC 661.185.1:543.2 112 Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 This British Standard, having been prepared under the direction of the Chemicals Standards Committee, was
3、published under the authority of the Board of BSI and comes into effect on 31 March 1989 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CIC/34 Draft for comment 86/50631 DC ISBN 0 580 17137 X Committees responsible for this British Standard The prep
4、aration of this British Standard was entrusted by the Chemicals Standards 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
5、 (Laboratory of the Government Chemist) London Regional Transport 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 issueComments Licensed Copy: sheffieldun sheffieldun, na, Wed D
6、ec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii 1Scope1 2Normative references1 3Principle1 4Reagents and materials1 5Apparatus1 6Sampling2 7Procedure2 8Expression of results3 9Test repo
7、rt4 Annex A (normative) General scheme of analysis5 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 ii BSI 12-1999 National foreword This Section of BS 6829 has been prepared under t
8、he direction of the Chemicals Standards Committee. It is identical with ISO 6843:1988 “Surface active agents Sulfated ethoxylated alcohols and alkylphenols Estimation of the mean relative molecular mass”, published by the International Organization for Standardization (ISO). Terminology and conventi
9、ons. The text of the International Standard has been approved as suitable for publication as a British Standard without deviation. Some terminology and certain conventions are not identical with those used in British Standards; attention is drawn especially to the following. The comma has been used
10、as a decimal marker. In British Standards it is current practice to use a full point on the baseline as the decimal marker. The symbol “l” has been used to denote litre (and in its submultiples). In British Standards it is current practice to use the symbol “L”. In British Standards it is current pr
11、actice to use the spelling “sulphur”, etc., instead of “sulfur”, etc. Wherever the words “International Standard” appear, referring to this Standard, they should be read as “Section of BS 6829”. Additional information. With reference to clause 4, water complying with grade 3 of BS 3978 “Specificatio
12、n for water for laboratory use” is suitable. With reference to 4.5, the concentration of the hydrochloric acid solution required is c (HCl) = 2 mol/L. 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
13、 should indicate that the method of test used is in accordance with BS 6829-5.2. Cross-references International StandardCorresponding British Standard ISO 607:1980BS 3762 Analysis of formulated detergents Part 1:1983 Methods of sample division (Identical) ISO 1042:1983BS 1792:1982 Specification for
14、one-mark volumetric flasks (Identical) ISO 2271:1972BS 3762 Analysis of formulated detergents Part 3: Quantitative test methods Section 3.1:1983 Method for determination of anionic-active matter content (Identical) ISO 4800:1977BS 2021:1980 Specification for separating and dropping funnels for labor
15、atory use (Identical) ISO 6842:1983 BS 6829 Analysis of surface active agents (raw materials) Part 5: Ethoxylated alcohol and alkylphenol sulphates Section 5.1:1987 Method for determination of total active matter content (Identical) ISO 8799:1988Section 5.3:1988 Method for determination of unsulphat
16、ed matter content (Identical) Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 BSI 12-1999iii A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsib
17、le for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages 1 to 6, an inside back cover and a back cover. This standard has been up
18、dated (see copyright date) and 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 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na
19、, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 BSI 12-19991 1 Scope This International Standard specifies a method for the estimation of the mean relative molecular mass of the anionic-active matter present in ordinary commercial neutralized products of sulfation o
20、f ethoxylated alcohols or alkylphenols alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates) containing an average of not more than 20 oxyethylene groups per molecule. It also sets out, in Annex A, a general scheme of analysi
21、s. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on t
22、his International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 607:1980, Surface active agents and detergents Methods of sample divi
23、sion. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 2271:1972, Surface active agents Detergents Determination of anionic-active matter (Direct two-phase titration procedure). ISO 4800:1977, Laboratory glassware Separating funnels and dropping funnels. ISO 6842:1983, Surface act
24、ive agents Polyethoxylated alcohol and alkylphenol sulfates Determination of total active matter. ISO 8799:1988, Sulfated ethoxylated alcohols and alkylphenols Determination of content of unsulfated matter. 3 Principle From a solution of the test portion saturated with sodium chloride, extraction of
25、 alkylether sulfate with an ethyl acetate/butan-1-ol mixture, then evaporation of the aqueous phase containing the polyglycol, the polyglycol sulfate and possibly traces of ether sulfates; then removal of salts from the residue by treatment with methanol and filtration. Evaporation of an aliquot por
26、tion of the filtrate and weighing of the residue, then redissolution in water and determination of the sodium chloride and anionic-active matter contents. Determination of the polyglycol content by passing the remaining fraction of filtrate through an ion-exchange resin. Determination of the polygly
27、col sulfate content by difference between the above determinations. From the content of anionic surface active agent (alkylether sulfate) and the anionic surface active matter content determined by two-phase titration, estimation of the mean relative molecular mass. NOTEThe content of anionic surfac
28、e active agent (alkylether sulfate) is obtained by the difference between the total active matter content and the unsulfated matter and polyglycol sulfate contents. 4 Reagents and materials During the analysis, use only reagents of recognized analytical reagent grade and only distilled water or wate
29、r of equivalent purity. 4.1 Methanol 4.2 Sodium chloride 4.3 Ethyl acetate/butan-1-ol, mixture (9 + 1) by volume. 4.4 Sodium chloride, 59 g/l solution. 4.5 Hydrochloric acid, 73 g/l solution. 4.6 Sodium hydroxide, 80 g/l solution. 4.7 Silver nitrate, standard volumetric solution, c(AgNO3) = 0,100 mo
30、l/l. 4.8 Cation-exchange resin, polystyrene sulfonic acid type, 2 % crosslinked, 150 to 330 4m, hydrogen form. 4.9 Anion-exchange resin, polystyrene quaternary ammonium type, 2 % crosslinked, 150 to 330 4m, chloride form. 5 Apparatus Ordinary laboratory apparatus and 5.1 Separating funnel, of capaci
31、ty 250 ml, in accordance with ISO 4800. 5.2 Separating funnel, jacketed, of capacity 250 ml. 5.3 One-mark volumetric flask, of capacity 100 ml, in accordance with ISO 1042. 5.4 Water bath, capable of being controlled at 50 C. 5.5 Reflux condenser 5.6 Rotary evaporator, with round-bottom flasks of ca
32、pacity 250 ml. 5.7 Ion-exchange column: Glass tube of internal diameter 25 mm and length 200 mm, restricted at the bottom and provided with a glass stopcock. The ion-exchange resin is supported at the bottom by a 10 to 20 mm layer of glass wool or by a sintered glass filter. Licensed Copy: sheffield
33、un sheffieldun, na, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 2 BSI 12-1999 6 Sampling The laboratory sample of surface active agent shall be prepared and stored in accordance with the instructions given in ISO 607. 7 Procedure 7.1 Test portion From the laborato
34、ry sample, if necessary homogenized by introducing a definite and appropriate quantity of water, weigh, to the nearest 0,1 g, into a 100 ml beaker, a quantity corresponding to about 25 mmol of anionic-active matter. 7.2 Preparation of the ion-exchange resins If preferred, the resins may be prepared
35、in smaller amounts than 1 kg with proportionately smaller volumes of reagents. 7.2.1 Anion-exchange resin Take 1 kg of the anion-exchange resin (4.9) and allow to distend in water for 48 h. Transfer the resin to a suitable column and pass 5 litres of the sodium hydroxide solution (4.6) through the c
36、olumn, followed by 2 to 3 litres of water. Then pass 4 litres of the hydrochloric acid solution (4.5) through the column and again wash with 2 to 3 litres of water. The treated resin may be stored in water. 7.2.2 Cation-exchange resin Take 1 kg of the cation-exchange resin (4.8) and allow to distend
37、 in water for 48 h. Transfer the resin to a suitable column and pass 5 litres of the hydrochloric acid solution (4.5) through the column, then wash with water until the washings are neutral. The treated resin may be stored in water. 7.3 Final preparation of resins Take the required amount of anion-e
38、xchange resin, prepared as specified in 7.2.1, namely 25 ml per determination, and transfer to a suitable column. Pass through the column five times its volume of the sodium hydroxide solution (4.6), wash with water until neutral, then wash with 1 to 2 volumes of the methanol (4.1). Take the require
39、d amount (25 ml) of cation-exchange resin, prepared as specified in 7.2.2, and, after introduction into a suitable column, wash with twice its volume of methanol (4.1). 7.4 Arrangement of the mixed-bed exchange column Mix 25 ml of the cation-exchange resin and 25 ml of the anion-exchange resin, prep
40、ared as specified in 7.3, in a beaker. Fill the column (5.7) with the mixed resin in small portions and compress the mixed resin with a glass rod to a volume between 50 and 60 ml, and wash with 500 ml of the methanol (4.1). 7.5 Separation of polyglycol sulfate 7.5.1 Dissolve the test portion (7.1) i
41、n 50 ml of the sodium chloride solution (4.4) and 50 ml of the ethyl acetate/butan-1-ol mixture (4.3). Transfer the solution to a separating funnel (5.1) and rinse the beaker with a few millilitres of the sodium chloride solution (4.4) and of the ethyl acetate/butan-1-ol mixture, then add the rinsin
42、g solution to the separating funnel. Shake the separating funnel vigorously and allow the phases to separate. Draw off the aqueous phase into the jacketed separating funnel (5.2), thermoregulated at 60 C, add 5 g of the sodium chloride (4.2) and shake to complete dissolution. Add 50 ml of the ethyl
43、acetate/butan-1-ol mixture and shake. After separation of the phases, draw off the aqueous phase into a 250 ml round-bottom flask (5.6) and evaporate to dryness by means of the rotary evaporator (5.6) on a water bath (5.4), controlled at 50 C, under vacuum, using a water-jet air pump. Add to the res
44、idue 30 ml of the methanol (4.1) and boil under reflux for 3 min and filter through a medium-speed filter paper, collecting the filtrate in a 250 ml flask (5.6). Repeat these operations three times. Evaporate to dryness using the rotary evaporator. Treat the new residue with 30 ml of the methanol (4
45、.1), boil under reflux for 3 min and filter through a medium-speed filter paper, collecting the filtrate in the 100 ml one-mark volumetric flask (5.3). Repeat these operations three times and dilute to the mark with the methanol. By means of a pipette, transfer 50 ml of the solution to a tared 150 m
46、l beaker, evaporate under a nitrogen current, dry at 105 C to constant mass, and weigh the residue (m1). Licensed Copy: sheffieldun sheffieldun, na, Wed Dec 06 14:27:40 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 6829-5.2:1989 BSI 12-19993 7.5.2 Pass the 50 ml remaining in the volumetric flask thr
47、ough the column prepared as specified in 7.4. Regulate the rate of flow to 5 ml/min and wash the column with 100 ml of the methanol. Transfer the eluate to a tared 250 ml round-bottom flask (5.6) and evaporate with the rotary evaporator on the water bath, controlled at 50 C, under vacuum, using a wa
48、ter-jet air pump. Dry at 105 C to constant mass, and weigh the residue (m2). 7.5.3 Dissolve the dry residue (ml) in 50 ml of water. On 10 ml of this solution, determine the anionic-active matter content (A2) by direct two-phase titration in accordance with ISO 2271. 7.5.4 On another 10 ml of this so
49、lution, determine the chloride content by titration with the silver nitrate solution (4.7). 7.6 Estimation of the mean relative molecular mass The mean relative molecular mass is obtained by calculation (see 8.1.2). 8 Expression of results 8.1 Method of calculation 8.1.1 Polyglycol sulfate content The polyglycol sulfate content PS, expressed as a percentage by mass, is given by the equation PS = R P A where the meaning of the letter symbols is as follows. 8.1.1.1 R is the percentage by mass of residue in the aqueous phase after extracti