Surface active agents - Determination of the content of non-ionic substances in anionic surface active agents by high performance liquid chromatography (HPLC)

This European Standard specifies a method for the determination of the contents of non-ionic substances in anionic surface active agents (sulfates, sulfonates and ethoxysulfates) by high performance liquid chromatography (HPLC).

Grenzflächenaktive Stoffe - Bestimmung des Gehaltes von nichtionischen Substanzen in anionischen grenzflächenaktiven Stoffen mittels Hochleistungs-Flüssigchromatographie (HPLC)

1 Anwendun sbereic
Diese Europäische Norm legt ein Verfahren zur Bestimmung des Gehaltes an nichtionischen Substanzen in
anionischen  grenzflächenaktiven  Stoffen  (Sulfaten,  Sulfonaten  und  Ethoxysulfaten)  mittels  Hochleistungs-Flüssigchromatographie (
HPLC) fest

Agents de surface - Détermination de la teneur en substances non-ioniques dans les agents de surfaces anioniques par chromatographie liquide a haute performance (CLHP)

Domaine d'application
La présente norme européenne spécifie une méthode de détermination des teneurs en substances non-ioniques contenues dans les agents de surface anioniques (sulfates, sulfonates et éthoxysulfates) par chromatographie liquide a haute performance (CLHP).

Povšinsko aktivne snovi - Določevanje neionskih substanc v anionskih površinsko aktivnih snoveh s tekočinsko kromatografijo (HPLC)

General Information

Status
Published
Publication Date
31-Dec-2001
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jan-2002
Due Date
01-Jan-2002
Completion Date
01-Jan-2002

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EN 13273:2002
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Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Grenzflächenaktive Stoffe - Bestimmung des Gehaltes von nichtionischen Substanzen in anionischen grenzflächenaktiven Stoffen mittels Hochleistungs-Flüssigchromatographie (HPLC)Agents de surface - Détermination de la teneur en substances non-ioniques dans les agents de surfaces anioniques par chromatographie liquide a haute performance (CLHP)Surface active agents - Determination of the content of non-ionic substances in anionic surface active agents by high performance liquid chromatography (HPLC)71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13273:2001SIST EN 13273:2002en01-januar-2002SIST EN 13273:2002SLOVENSKI
STANDARD



SIST EN 13273:2002



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13273April 2001ICS 71.100.40English versionSurface active agents - Determination of the content of non-ionicsubstances in anionic surface active agents by highperformance liquid chromatography (HPLC)Agents de surface - Détermination de la teneur ensubstances non-ioniques dans les agents de surfacesanioniques par chromatographie liquide à hauteperformance (CLHP)Grenzflächenaktive Stoffe - Bestimmung des Gehaltes vonnichtionischen Substanzen in anionischengrenzflächenaktiven Stoffen mittels Hochleistungs-Flüssigchromatographie (HPLC)This European Standard was approved by CEN on 20 January 2001.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.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.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2001 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13273:2001 ESIST EN 13273:2002



Page 2EN 13273:2001ContentsPageForeword.31Scope.42Normative references.43Principle.44Reagents.45Apparatus.46Calibration.57Sampling and preparation of the test sample.68Procedure.69Calculation and expression of results.710Precision.711Test report.8Annex A (informative)
Flow diagram for the backflush valve in position 1 and position 2.9Annex B (informative)
Example chromatograms.10Annex C (informative)
Ring test results.14SIST EN 13273:2002



Page 3EN 13273:2001ForewordThis European Standard has been prepared by Technical Committee CEN/TC 276 "Surface active agents", thesecretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by October 2001, and conflicting national standards shall be withdrawn at the latestby October 2001.Annexes A, B and C are informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries 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.SIST EN 13273:2002



Page 4EN 13273:20011 ScopeThis European Standard specifies a method for the determination of the contents of non-ionic substances inanionic surface active agents (sulfates, sulfonates and ethoxysulfates) by high performance liquid chromatography(HPLC).2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN ISO 3696, Water for analytical laboratory use – Specification and test methods. (ISO 3696:1987)ISO 607, Surface active agents and detergents – Methods of sample division.3 PrincipleA specified mass of sample is dissolved and then made up to standard volume with methanol. For sulfonic acids only,the sample is neutralised with aqueous sodium hydroxide solution prior to the dissolution. The solution is thenanalysed by Reverse Phase High Performance Liquid Chromatography (RP-HPLC). An octadecylsilane bondedstationary phase, methanol/water mobile phase, differential refractometer detector and external means ofquantification are employed. A back flush technique is used to "focus" the non-ionic components after all the activematter components and water have eluted from the column.4 ReagentsDuring the analysis, only use reagents of recognized analytical grade and water complying with grade 3 as definedin 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 beenproduced, eg. : parent linear alkyl benzene (LAB) for alkyl benzene sulfonates ; parent alcohols for alcohol sulfates ; parent alcohol ethoxylates for alcohol ethoxy sulfates.5 ApparatusOrdinary laboratory apparatus and the following.5.1High performance liquid chromatograph, suitable for analysis according to the conditions given in 6.3.5.2Datta logger/plotter giving the chromatographic peak areas.5.3Burette, capacity 10 ml with polytetrafluorethylene (PTFE) key, never lubricated with stopcock grease.SIST EN 13273:2002



Page 5EN 13273:20015.4Syringe, 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 µm, with "Luer" fittings.6 Calibration6.1 GeneralAlways wash glassware thoroughly with water and then acetone (propan-2-one). Dry thoroughly.6.2Determination of the optimum backflush timePrepare and analyse the appropriate calibratio
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