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1、BRITISH STANDARD BS EN 13273:2001 Surface active agents Determination of the content of non-ionic substances in anionic surface active agents by high performance liquid chromatography (HPLC) The European Standard EN 13273:2001 has the status of a British Standard ICS 71.100.40 NO COPYING WITHOUT BSI
2、 PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13273:2001 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was publis
3、hed under the authority of the Standards Committee and comes into effect on 15 June 2001 BSI 06-2001 ISBN 0 580 37402 5 National foreword This British Standard is the official English language version of EN 13273:2001. The UK participation in its preparation was entrusted to Technical Committee CII/
4、34, Methods of test for surface active agents, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Additional information Some textual errors were discovered when the English language version of EN 13273:2001 was adopted
5、 as the national standard. Some of the chemical names are not consistently presented and do not conform to IUPAC recommendations. These textual errors have been reported to CEN in a proposal to amend the text of the European Standard. Cross-references The British Standards which implement internatio
6、nal or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions o
7、f 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. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretatio
8、n, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 14, an inside back cover and a back cove
9、r. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUR
10、OPISCHE NORM EN 13273 April 2001 ICS 71.100.40 English version Surface active agents Determination of the content of non-ionic substances in anionic surface active agents by high performance liquid chromatography (HPLC) Agents de surface Dtermination de la teneur en substances non-ioniques dans les
11、agents de surfaces anioniques par chromatographie liquide haute performance (CLHP) Grenzflchenaktive Stoffe Bestimmung des Gehaltes von nichtionischen Substanzen in anionischen grenzflchenaktiven Stoffen mittels Hochleistungs- Flssigchromatographie (HPLC) This European Standard was approved by CEN o
12、n 20 January 2001. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards m
13、ay be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Mana
14、gement Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
15、 EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13273:2001 E Licensed
16、Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 2 EN 13273:2001 BSI 06-2001 Contents Page Foreword.3 1Scope .4 2Normative references .4 3Principle.4 4Reagents4 5Apparatus 4 6Calibration .5 7Sampling and preparation of the test sample7 8Procedure
17、 7 9Calculation and expression of results7 10Precision8 11Test report .8 Annex A (informative) Flow diagram for the backflush valve in position 1 and position 29 Annex B (informative) Example chromatograms 10 Annex C (informative) Ring test results.14 Licensed Copy: sheffieldun sheffieldun, na, Mon
18、Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 3 EN 13273:2001 BSI 06-2001 Foreword This European Standard has been prepared by Technical Committee CEN/TC 276, Surface active agents, the Secretariat of which is held by AFNOR. This European Standard shall be given the status of a nat
19、ional standard, either by publication of an identical text or by endorsement, at the latest by October 2001, and conflicting national standards shall be withdrawn at the latest by October 2001. Annexes A, B and C are informative. According to the CEN/CENELEC Internal Regulations, the national standa
20、rds organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Cop
21、y: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 4 EN 13273:2001 BSI 06-2001 1 Scope This European Standard specifies a method for the determination of the contents of non-ionic substances in anionic surface active agents (sulfates, sulfonates and e
22、thoxysulfates) by high performance liquid chromatography (HPLC). 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed he
23、reafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN ISO 369
24、6, Water for analytical laboratory use Specification and test methods (ISO 3696:1987). ISO 607, Surface active agents and detergents Methods of sample division. 3 Principle A specified mass of sample is dissolved and then made up to standard volume with methanol. For sulfonic acids only, the sample
25、is neutralized with aqueous sodium hydroxide solution prior to the dissolution. The solution is then analysed by reverse phase high performance liquid chromatography (RP-HPLC). An octadecylsilane bonded stationary phase, methanol/water mobile phase, differential refractometer detector and external m
26、eans of quantification are employed. A back flush technique is used to “focus” the non-ionic components after all the active matter components and water have eluted from the column. 4 Reagents During the analysis, only use reagents of recognized analytical grade and water complying with grade 3 as d
27、efined in EN ISO 3696. 4.1Methanol, CH4O HPLC grade. 4.2Sodium hydroxide NaOH c(NaOH) = 1 mol/l solution. 4.3Phenolphthalein indicator, ethanolic solution, C20H14O4, w(C20H14O4) = 0,1 g/100 g. 4.4Calibration substances, based on the feedstock from which the surface active agent/sulfonic acid has bee
28、n produced, e.g.: ? parent linear alkyl benzene (LAB) for alkyl benzene sulfonates; ? parent alcohols for alcohol sulfates; ? parent alcohol ethoxylates for alcohol ethoxy sulfates. 5 Apparatus Ordinary laboratory apparatus and the following. 5.1High performance liquid chromatograph, suitable for an
29、alysis according to the conditions given in 6.3. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 5 EN 13273:2001 BSI 06-2001 5.2Data logger/plotter giving the chromatographic peak areas. 5.3Burette, capacity 10 ml with polytetrafluoreth
30、ylene (PTFE) key, never lubricated with stopcock grease. 5.4Syringe, capacity 1 ml with “Luer” fitting. 5.5Needle with “Luer” fitting to suit sample injection valve, or use an automated injector. 5.6Syringe filter or membrane suitable for use with methanol, 0,45 m, with “Luer” fittings. 6 Calibratio
31、n 6.1 General Always wash glassware thoroughly with water and then acetone (propan-2-one). Dry thoroughly. 6.2Determination of the optimum backflush time Prepare and analyse the appropriate calibration substance (4.4) according to clause 7, but keep the backflush valve in position 1 (see Figure A.1)
32、 throughout the complete analysis. The chromatogram of the calibration substance alkyl ether sulfate, type 2, used in the ring test is shown in Figure B.1. Note the elution time just before the first peak of the calibration substance appears. This is the backflush valve switching time. The above val
33、ve switching time needs only be determined if the method is being set up or if it becomes apparent that the retention times have changed during routine use. 6.3Determination of response factors Determine the response factors for each type of the surface active agents as follows. Prepare a calibratio
34、n solution by weighing (0,15 0,02) g of the calibration substance (4.4) to the nearest 0,1 mg into a 100 ml volumetric flask. Dissolve with methanol (4.1) and make up to volume. Load the syringe (5.4) with 1 ml of the calibration solution and mount a new syringe filter fitted with the needle (5.5).
35、Use the following conditions: Column: TypeHPLC column with appropriate fittings. A radial compression type is suitable if used with appropriate conditions. Length ? internal diameterDimensions which enable results similar to the chromatograms in annex B. For a radial compression column, 100 mm ? 8 m
36、m is suitable. For conventional columns, 250 mm ? 4,6 mm is suitable. Stationary phaseOctadecylsilyl bonded micro-particulate silica of mean particle size not more than 5 m. This should be of the completely-end-capped or deactivated type. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:
37、44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 6 EN 13273:2001 BSI 06-2001 Mobile Phase: CompositionA mixture of methanol and water capable of use with the chosen HPLC column so as to give results similar to the examples in annex B. A mixture of methanol : water of 85:15 parts by volume can be s
38、uitable Flow rate1 ml/min to 2 ml/min to the nearest 0,01 ml/min. Detector: TypeDifferential refractometer SensitivityA setting which gives a display of peak sizes such that deviations from normal appearance can be readily seen. Temperatures: Column30,0 C NOTEThermostatting of the column gives impro
39、ved stability, but the method can be used with the column at ambient temperatures. Detector40,0 C Injection system:High pressure syringe-loading injection valve or a suitable automated injector, fitted with an injection loop of appropriate volume, for example 50 l. Backflush valve:A 6 port high pres
40、sure switching valve for HPLC, fitted with a very low volume by-pass loop. Valve positioning:Position 1 at the beginning of the analysis. Switch to position 2 at time A (see Figures A.1 and B.1) Switch to position 1 on completion of the analysis (typical analysis time: 20 min). Run the chromatograph
41、 in accordance with the manufacturers instructions. When injecting the blend ensure the sample loop is completely flushed by dispensing the total syringe volume taking care not to introduce any air bubbles. An example chromatogram is given in Figure B.1. NOTEThe calibration peak elutes at a run time
42、 twice that of the backflush valve switch time. This time can vary depending on the sample type and is derived in 6.2. The response factor, F, is calculated using the equation (1): c c A m F ?(1) where: mc is the mass of the calibration substance used, in grams; Ac is the area of the calibration pea
43、k, in arbitrary units. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 7 EN 13273:2001 BSI 06-2001 7 Sampling and preparation of the test sample Sample the material to be tested in accordance with ISO 607. 8 Procedure 8.1Determine the o
44、ptimum backflush time from the calibration carried out in 6.2. 8.2Weigh (1 0,1) g of the sample to the nearest 0,1 mg into a 25 ml volumetric flask. 8.3For sulfonic acids only, add one drop of phenolphthalein indicator (4.3) and then add 2,00 ml of sodium hydroxide solution (4.2). Swirl to dissolve.
45、 When completely dissolved, titrate dropwise with sodium hydroxide solution (4.2) to the end point characterized by faint pink colour (total titrant addition typically about 3,2 ml). For the other surface active agents, continue to 8.4. Use a burette (5.3). 8.4Dissolve and make up to volume with met
46、hanol (4.1). Allow to stand for a short time such that any precipitate formed settles to the bottom of the flask. 8.5Load the syringe (5.4) with 1 ml of supernatant from the sample solution. Mount a new syringe filter or membrane (5.6). Use this to deliver a filtered sample portion for use in the an
47、alysis. Where possible, this should be done by direct delivery into the injection valve, via the needle (5.5). 8.6Analyse the sample according to the conditions given in 6.3. When injecting the sample ensure the sample loop is completely flushed by dispensing the total syringe volume taking care not
48、 to introduce any air bubbles. NOTE 1An example chromatogram is given in Figure B.2 and Figure B.4. If the valve was not used, a chromatogram as shown in Figure B.3 should result. NOTE 2The operation of the backflush valve should be automated. 9 Calculation and expression of results The content of n
49、on-ionic substances wNIS of the sample expressed in grams per 100 g is calculated using the equation (2): 4 100 ? ? ? s s NIS m FA w(2) where: As is the area of the peak of non-ionic substances, as used for Ac (see 6.3) in arbitrary units; F is the response factor of the calibration solution (6.3); ms is the mass of the sample (8.2) in grams. Report the result to the nearest 0,001 g/100 g. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:13:44 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Page 8 EN 13273:2001 BSI 06-2001 10 Prec