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 112BS6829-5.2:1989 This British Standard, having been prepared under the directionof the Chemicals Standards Committee, was published under the authority ofthe Board of BSI and comes intoeffect on 31March1989 BSI 12-1999 The following
3、 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 preparation of this British Standard was entrusted by the Chemicals Standards Committee (CIC/-) to Technical Committee
4、 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 (Laboratory of the Government Chemist) London Regional Transport Ministry of Defence Royal Society of Chemistry S
5、oap and Detergent Industry Association Society of Dyers and Colourists Amendments issued since publication Amd. No. Date of issue CommentsBS6829-5.2:1989 BSI 12-1999 i Contents Page Committees responsible Inside front cover National foreword ii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reag
6、ents and materials 1 5 Apparatus 1 6 Sampling 2 7 Procedure 2 8 Expression of results 3 9 Test report 4 Annex A (normative) General scheme of analysis 5 Publications referred to Inside back coverBS6829-5.2:1989 ii BSI 12-1999 National foreword This Section of BS6829 has been prepared under the direc
7、tion of the Chemicals Standards Committee. It is identical with ISO6843:1988 “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 conventions. The
8、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 as a deci
9、mal 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 practice to
10、 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 BS6829”. Additional information. With reference to clause4, water complying with grade3 of BS3978 “Specification for water f
11、or laboratory use” is suitable. With reference to4.5, the concentration of the hydrochloric acid solution required is c (HCl) = 2mol/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 should indicat
12、e that the method of test used is in accordance with BS6829-5.2. Cross-references International Standard Corresponding British Standard ISO 607:1980 BS 3762 Analysis of formulated detergents Part 1:1983 Methods of sample division (Identical) ISO 1042:1983 BS 1792:1982 Specification for one-mark volu
13、metric flasks (Identical) ISO 2271:1972 BS 3762 Analysis of formulated detergents Part 3: Quantitative test methods Section 3.1:1983 Method for determination of anionic-active matter content (Identical) ISO 4800:1977 BS 2021:1980 Specification for separating and dropping funnels for laboratory use (
14、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 8799:1988 Section 5.3:1988 Method for determination of unsulphated matter
15、content (Identical)BS6829-5.2:1989 BSI 12-1999 iii 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 obl
16、igations. Summary of pages This document comprises a front cover, an inside front cover, pagesi toiv, pages1to6, 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 i
17、nside front cover.iv blankBS6829-5.2:1989 BSI 12-1999 1 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 of ethoxylated alcohols or alkylphenols
18、alkyl oxyethylene sulfates (ethoxylated alcohol sulfates) or alkylphenol oxyethylene sulfates (ethoxylated alkylphenol sulfates) containing an average of not more than20 oxyethylene groups per molecule. It also sets out, inAnnex A, a general scheme of analysis. 2 Normative references The following s
19、tandards 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 this International Standard are encouraged
20、 to investigate the possibility of applying the most recent editions of the standards listed below. Members of IEC and ISOmaintain registers of currently valid International Standards. ISO 607:1980, Surface active agents and detergents Methods of sample division. ISO 1042:1983, Laboratory glassware
21、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 active agents Polyethoxylated alcohol and alk
22、ylphenol 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 alkylether sulfate with an ethyl acetate/
23、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 portion of the filtrate and weighing of the r
24、esidue, 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 polyglycol sulfate content by difference between
25、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 surface active agent (alkylether sulfate) is obt
26、ained 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 water of equivalent purity. 4.1 Methanol 4.2 S
27、odium chloride 4.3 Ethyl acetate/butan-1-ol, mixture (9+1) by volume. 4.4 Sodium chloride, 59g/l solution. 4.5 Hydrochloric acid, 73g/l solution. 4.6 Sodium hydroxide, 80g/l solution. 4.7 Silver nitrate, standard volumetric solution, c(AgNO 3 )=0,100mol/l. 4.8 Cation-exchange resin, polystyrene sulf
28、onic acid type, 2% crosslinked, 150to3304m, hydrogen form. 4.9 Anion-exchange resin, polystyrene quaternary ammonium type, 2% crosslinked, 150to3304m, chloride form. 5 Apparatus Ordinary laboratory apparatus and 5.1 Separating funnel, of capacity250ml, in accordance with ISO4800. 5.2 Separating funn
29、el, jacketed, of capacity250ml. 5.3 One-mark volumetric flask, of capacity100ml, in accordance with ISO1042. 5.4 Water bath, capable of being controlled at50 C. 5.5 Reflux condenser 5.6 Rotary evaporator, with round-bottom flasks of capacity250ml. 5.7 Ion-exchange column: Glass tube of internal diam
30、eter25mm and length200mm, restricted at the bottom and provided with a glass stopcock. The ion-exchange resin is supported at the bottom by a10 to20mm layer of glass wool or by a sintered glass filter.BS6829-5.2:1989 2 BSI 12-1999 6 Sampling The laboratory sample of surface active agent shall be pre
31、pared and stored in accordance with the instructions given in ISO607. 7 Procedure 7.1 Test portion From the laboratory sample, if necessary homogenized by introducing a definite and appropriate quantity of water, weigh, to the nearest0,1g, into a100ml beaker, a quantity corresponding to about25mmol
32、of anionic-active matter. 7.2 Preparation of the ion-exchange resins If preferred, the resins may be prepared in smaller amounts than1kg with proportionately smaller volumes of reagents. 7.2.1 Anion-exchange resin Take1kg of the anion-exchange resin (4.9) and allow to distend in water for48h. Transf
33、er the resin to a suitable column and pass5litres of the sodium hydroxide solution (4.6) through the column, followed by2to3litres of water. Then pass4litres of the hydrochloric acid solution (4.5) through the column and again wash with2 to3litres of water. The treated resin may be stored in water.
34、7.2.2 Cation-exchange resin Take1kg of the cation-exchange resin (4.8) and allow to distend in water for48h. Transfer the resin to a suitable column and pass5litres of the hydrochloric acid solution (4.5) through the column, then wash with water until the washings are neutral. The treated resin may
35、be stored in water. 7.3 Final preparation of resins Take the required amount of anion-exchange resin, prepared as specified in7.2.1, namely25ml 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
36、until neutral, then wash with1to2 volumes of the methanol (4.1). Take the required amount (25ml) of cation-exchange resin, prepared as specified in7.2.2, 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 Mix2
37、5ml of the cation-exchange resin and25ml of the anion-exchange resin, prepared as specified in7.3, 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 between50 and60ml, and wash with500ml of the methanol(4.1). 7.5 Separ
38、ation of polyglycol sulfate 7.5.1 Dissolve the test portion (7.1) in50ml of the sodium chloride solution (4.4) and50ml 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) a
39、nd of the ethyl acetate/butan-1-ol mixture, then add the rinsing 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 at60 C, add5g of the sodium chloride (4.2
40、) and shake to complete dissolution. Add50ml of the ethyl acetate/butan-1-ol mixture and shake. After separation of the phases, draw off the aqueous phase into a250ml round-bottom flask (5.6) and evaporate to dryness by means of the rotary evaporator (5.6) on a water bath (5.4), controlled at50 C, u
41、nder vacuum, using a water-jet air pump. Add to the residue30ml of the methanol (4.1) and boil under reflux for3min and filter through a medium-speed filter paper, collecting the filtrate in a250ml flask (5.6). Repeat these operations three times. Evaporate to dryness using the rotary evaporator. Tr
42、eat the new residue with30ml of the methanol(4.1), boil under reflux for3min and filter through a medium-speed filter paper, collecting the filtrate in the100ml one-mark volumetric flask(5.3). Repeat these operations three times and dilute to the mark with the methanol. By means of a pipette, transf
43、er50ml of the solution to a tared150ml beaker, evaporate under a nitrogen current, dry at105 C to constant mass, and weigh the residue (m 1 ).BS6829-5.2:1989 BSI 12-1999 3 7.5.2 Pass the50ml remaining in the volumetric flask through the column prepared as specified in7.4. Regulate the rate of flow t
44、o5ml/min and wash the column with100ml of the methanol. Transfer the eluate to a tared250ml round-bottom flask (5.6) and evaporate with the rotary evaporator on the water bath, controlled at50 C, under vacuum, using a water-jet air pump. Dry at105 C to constant mass, and weigh the residue (m 2 ). 7.
45、5.3 Dissolve the dry residue (m l ) in50ml of water. On10ml of this solution, determine the anionic-active matter content (A 2 ) by direct two-phase titration in accordance with ISO2271. 7.5.4 On another10ml of this solution, determine the chloride content by titration with the silver nitrate soluti
46、on (4.7). 7.6 Estimation of the mean relative molecular mass The mean relative molecular mass is obtained by calculation (see8.1.2). 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 th
47、e 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 extraction by the ethyl acetate/butan-1-ol mixture, given by the equation where m 0 is the mass, in grams, of the test portion(7.1); m 1 is the mass,
48、 in grams, of the residue from the aqueous phase obtained in7.5.1; V is the volume, in millilitres, of the silver nitrate solution (4.7) used in7.5.4. 8.1.1.2 P is the percentage by mass of polyglycol in the aqueous phase after extraction by the ethyl acetate/butan-1-ol mixture, given by the equatio
49、n where m 0 is the mass, in grams, of the test portion(7.1); m 2 is the mass, in grams, of the residue obtained after passing 50 ml of the methanolic solution prepared in7.5.1 through the ion-exchange column as described in7.5.2. 8.1.1.3 A is the percentage by mass of anionic-active matter in the aqueous phase after extraction by the ethyl acetate/butan-1-ol mixture, given by the equation where A 1 is the anionic-active matter content, expressed in millimoles per gram, determined on the sample by direct two-phase titration in accordance wi
