SIST EN 13320:2002
(Main)Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates
Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates
This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acid polyglycol esters.
Grenzflächenaktive Stoffe - Gaschromatographische Spurenbestimmung von freiem Ethylenoxid in Ethoxylaten
Diese Europäische Norm legt ein Verfahren zur Bestimmung von freiem Ethylenoxid im Bereich von 1 mg/kg bis 100 mg/kg in Polyglycolen, Ethoxylaten von Alkoholen und Alkylphenolen und in Fettsäurepolyglycolestern fest.
Agents de surface - Détermination de traces d'oxyde d'éthylene libre dans les éthoxylats par chromatographie en phase gazeuse
La présente Norme européenne spécifie une méthode de détermination de la teneur en oxyde d'éthylene libre comprise entre 1 mg/kg et 100 mg/kg dans les polyglycols, les éthoxylats d'alcools et d'alkylphénols ainsi que dans les esters de polyglycol d'acides gras.
Površinsko aktivne snovi - Določevanje sledov prostega etilen oksida v etoksilatih s plinsko kromatografijo
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Grenzflächenaktive Stoffe - Gaschromatographische Spurenbestimmung von freiem Ethylenoxid in EthoxylatenAgents de surface - Détermination de traces d'oxyde d'éthylene libre dans les éthoxylats par chromatographie en phase gazeuseSurface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13320:2002SIST EN 13320:2002en01-september-2002SIST EN 13320:2002SLOVENSKI
STANDARD
SIST EN 13320:2002
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13320February 2002ICS 71.100.40English versionSurface active agents - Gas chromatographic tracedetermination of free ethylene oxide in ethoxylatesAgents de surface - Détermination de traces d'oxyded'éthylène libre dans les éthoxylats par chromatographie enphase gazeuseGrenzflächenaktive Stoffe - GaschromatographischeSpurenbestimmung von freiem Ethylenoxid in EthoxylatenThis European Standard was approved by CEN on 16 November 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, Malta, 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© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13320:2002 ESIST EN 13320:2002
EN 13320:2002 (E)2ContentspageForeword.31Scope.42Normative references.43Principle.44Reagents.45Apparatus.46Sampling and preparation of the test sample.57Procedure.58Calculation and expression of results.79Precision.710Test report.8Annex A (informative)
Ring test results.9Annex B (informative)
Titration of ethylene oxide stock solution.11SIST EN 13320:2002
EN 13320:2002 (E)3ForewordThis document EN 13320 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 August 2002, and conflicting national standards shall be withdrawn at the latest byAugust 2002.The annexes A and B 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, Malta, Netherlands, Norway, Portugal, Spain,Sweden, Switzerland and the United Kingdom.SIST EN 13320:2002
EN 13320:2002 (E)41 ScopeThis European Standard specifies a test method for the determination of the content of free ethylene oxide in therange from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acidpolyglycol esters.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 – Test methods of sample division.3 PrincipleThe ethoxylates are, after addition of water, analyzed by gas chromatography using a head-space samplingaccessory. The free ethylene oxide content is determined by the standard addition test method.4 ReagentsDuring the analysis, unless otherwise specified, use only reagents of recognized analytical grade and have beenchecked in advance as to not interfere with the analytical results.4.1Water complying with grade 1 as defined in EN ISO 3696.4.2Ethylene oxide, C2H4O, w(C2H4O)
99,5 %.4.3Ethylene oxide, C2H4O, dissolved in dichloromethane, vials containing 50 mg of ethylene oxide dissolvedin 1 ml of dichloromethane.4.4N,N-dimethylformamide, C3H7NO.5 ApparatusOrdinary laboratory apparatus and the following.5.1Capillary gas chromatograph, with flame ionisation detector (FID) and head-space sampling accessory. Theapparatus shall be equipped with a split system. The head-space sampling accessory shall be designed such thateach head-space bottle can be thermostated for a defined time.NOTESince ethylene oxide is easily decomposed by traces of impurities such as acids and transition metals, (catalyseddecomposition), a meticulously clean sampling accessory is necessary.5.2Fused silica capillary column, coating: crosslinked dimethylpolysiloxanes, column length 30 m, internaldiameter 0,25 mm, film thickness 1,0 .5.3Vials, closable by means of a septum, 20 ml, suitable for head-space sampling accessory.5.4Septums and aluminium caps, lined with aluminium or polytetrafluoroethylene (PTFE) for closing the vials.SIST EN 13320:2002
EN 13320:2002 (E)55.5Sealing pliers, for sealing the caps onto the vials.5.6Integrator or computer, with appropriate evaluation programme.5.7Analytical balance, accurate to 0,1 mg.6 Sampling and preparation of the test sample6.1 SamplingThe laboratory samples shall be prepared and stored in accordance with ISO 607.6.2 Test sampleNOTE 1The test samples can be in liquid, paste or solid form.For paste-like products, liquefy and homogenize the laboratory samples by gentle warming.NOTE 2If the test sample is heated above 50 °C, low results will be obtained.Do not melt solid products above 50 °C.7 Procedure7.1 Preparation of calibration solutions7.1.1 Standard solutionsPrepare a stock solution of ethylene oxide (EO) (4.2) either by :a) Difference weighingWeigh a 200 ml volumetric flask containing about 100 ml of water. Pass about 500 mg of ethylene oxide (4.2) intothe water and reweigh. Make up the solution to 200 ml with water. In place of difference weighing, the addition ofethylene oxide (4.2) can be carried out by weighing-in using a cooled syringe, orb) Using a vialDissolve the contents of a vial of ethylene oxide (4.3) in 250 ml of N,N-dimethylformamide (4.4).NOTEA method of titration of the ethylene oxide stock solution is given in annex B.Prepare standard solutions with concentrations of (C2H4O) = 0,1 g/100 ml and (C2H4O) = 0,01 g/100 ml bymultistage dilutions with water from the stock solution.Store the standard solutions in a refrigerator.7.1.2 Calibration solutionsPrepare
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