SIST EN 14207:2003
(Main)Water quality - Determination of epichlorohydrin
Water quality - Determination of epichlorohydrin
This European Standard specifies a method for the determination of epichlorohydrin in drinking water and water used for drinking water processing. According to the given procedure, the limit of determination in routine analysis is about 0,5 µg/l 1) . The limit of determination may be lowered to monitor 0,1 µg/l.
1) This value will be checked in an interlaboratory trial.
Wasserbeschaffenheit - Bestimmung von Epichlorhydrin
Anwendungsbereich
Diese Europäische Norm legt ein Verfahren zur Bestimmung von Epichlorhydrin in Trinkwasser und Rohwasser für die Trinkwasseraufbereitung fest. Nach dem hier beschriebenen Verfahren beträgt die Bestimmungsgrenze etwa 0,5 µg/l ). Die Bestimmungsgrenze kann erniedrigt werden, so dass die Überwachung eines Werts von 0,1 µg/l möglich ist.
Qualité de l'eau - Dosage de l'épichlorhydrine
La présente Norme européenne spécifie une méthode de dosage de l'épichlorhydrine dans l'eau potable et dans les eaux utilisées pour le traitement de l'eau potable. Conformément au mode opératoire indiqué, la limite de détermination est d'environ 0,5 µg/l ) lors des analyses de routine. Cette limite de détermination peut etre abaissée de façon a contrôler 0,1 µg/l.
Kakovost vode – Določevanje epiklorohidrina
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Wasserbeschaffenheit - Bestimmung von EpichlorhydrinQualité de l'eau - Dosage de l'épichlorhydrineWater quality - Determination of epichlorohydrin13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN 14207:2003SIST EN 14207:2003en01-september-2003SIST EN 14207:2003SLOVENSKI
STANDARD
SIST EN 14207:2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14207April 2003ICS 13.060.50English versionWater quality - Determination of epichlorohydrinQualité de l'eau - Dosage de l'épichlorhydrineWasserbeschaffenheit - Bestimmung von EpichlorhydrinThis European Standard was approved by CEN on 17 January 2003.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,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14207:2003 ESIST EN 14207:2003
EN 14207:2003 (E)2ContentspageForeword.3Introduction.31Scope.32Normative references.33Principle.44Interferences / Losses.45Reagents.46Apparatus.67Sampling.78Procedure.79Calibration.810Calculation of the results.1011Expression of results.1012Test report.1013Precision data.11Annex A (informative)
Example of sorbents.12Annex B (informative)
Examples of recommended capillary columns.13Annex C (informative)
Examples of chromatograms and spectra.14SIST EN 14207:2003
EN 14207:2003 (E)3ForewordThis document EN 14207:2003 has been prepared by Technical Committee CEN/TC 230 “Water analysis”, thesecretariat of which is held by DIN.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 2003, and conflicting national standards shall be withdrawn at the latestby October 2003.Annexes A, B and C are informative.WARNING — Persons using this standard should be familiar with normal laboratory practice. This standarddoes not propose to address all of the safety problems, if any, associated with its use. It is theresponsibility of the user to establish appropriate safety and health practices and to ensure compliancewith any national regulatory conditions.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, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.IntroductionIt is highly recommended that the test described in this standard be carried out by suitably qualified staff.It should be investigated whether and to what extent particular problems will require the specification of additionalmarginal conditions.1 ScopeThis European Standard specifies a method for the determination of epichlorohydrin in drinking water and waterused for drinking water processing. According to the given procedure, the limit of determination in routine analysisis about 0,5 µg/l 1). The limit of determination can be lowered to monitor 0,1 µg/l.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 25667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes (ISO 5667-1:1980).EN 25667-2, Water quality — Sampling — Part 2: Guidance on sampling techniques (ISO 5667-2:1991).
1)This value was checked in an interlaboratory trial.SIST EN 14207:2003
EN 14207:2003 (E)4EN ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples(ISO 5667-3:1994).ISO 5667-5, Water quality — Sampling — Part 5: Guidance on sampling of drinking water and water used for foodand beverage processing.ISO 8466-1, Water quality - Calibration and evaluation of analytical methods and estimation of performancecharacteristics - Part 1: Statistical evaluation of the linear calibration function.3 PrincipleSolid phase extraction of epichlorohydrin from the drinking water sample followed by gas chromatography using amass spectrometer (MS) as detector. Alternatively, an electron capture detector (ECD) can be used.4 Interferences / Losses4.1 Interferences during samplingIn order to avoid interferences, withdraw the sample according to clause 7, taking into account the informationgiven in EN 25667-1, EN 25667-2 and EN ISO 5667-3.In order to avoid losses due to the easy decomposition of epichlorohydrin, avoid unnecessary storage and analysethe sample as soon as possible after sampling. If storage is unavoidable, store between 2 °C and 5 °C until samplepretreatment.4.2 Interferences during enrichmentThe commercially available adsorbance materials are often of varying quality. Considerable batch-to-batchdifferences in quality and selectivity of these materials are possible. Perform calibration and analysis with one andthe same batch of material. Make sure to avoid any losses when removing the residual water in the adsorbancematerial (8.1.2).4.3 Interferences in the gas chromatography and mass spectrometrySet the operational conditions in accordance with the manufacturer’s instructions. Check these settings at regularintervals.General interferences, caused by the injection system can be eliminated with the help of special laboratoryexperience and the instruments manuals.The stability of the analytical system should be checked (for example by application of a measuring standard).5 ReagentsUse reagents of the reagent grade “for residual analysis” or equivalent as far as available. Impurities in thereagents and in the water contributing to the blank shall be negligibly low. Check the blank regularly, especiallyprior to the use of a new batch.5.1 WaterUse double-distilled water or water of comparable purity.SIST EN 14207:2003
EN 14207:2003 (E)55.2 Operating gases for the gas chromatography / mass spectrometry / ECD, according to themanufacturer’s instructions. The operating gases shall be of high purity.5.3 Nitrogen, high purity, minimum 99,996 % (v/v), for removal of water in the sorbent packing after sampleextraction.5.4 Solvents5.4.1 Diisopropyl ether, C6H14O.5.4.2 Methanol, CH3OH, as conditioning agent.5.5 Reducing agents, e.g. sodium thiosulfate (Na2S2O3).5.6 Epichlorohydrin stock solutionWeigh 50 mg of epichlorohydrin (C3H5ClO) into a 100-ml volumetric flask containing diisopropyl ether (5.4.1) up tothe neck and fill to mark with diisopropyl ether (5.4.1). Store the solution in a refrigerator between 2 °C and 5 °C.The shelf-life of the solution is limited (about 6 months). Check the concentration prior to analysis in order to makesure that no significant differences arise.5.7 Internal standard stock solutionThe internal standard shall not be present in the sample itself.5.7.1 13C3-epichlorohydrin stock solution for GC-MSThis solution may be purchased as certified solution (e.g. at a concentration of 100 µg/ml in nonane) or prepared from purestandard material according to 5.6. Never add more than 100 µl of a diluted internal standard stock solution in diisopropyl ether(5.4.1) to 100 ml of the water sample, a greater volume may result in poor recovery.NOTEThe peak area of the internal standard should be equivalent to that of 1 µg/l of the analyte. For example, if the con-centration of the stock solution is 100 µg/ml of 13C3-epichlorohydrin in nonane, 100 µl, dissolved in 1 ml diisopropyl ether (5.4.1)is required to produce a 10 µg/ml spiking solution from which a volume of 10 µl can be injected directly into 100 ml of water(5.1).5.7.2 Ethyl 2-chloropropionate (C5H9ClO2) stock solution for GC-ECD (see 5.6)5.8 Epichlorohydrin spiking solutionsUsing stock standard solution (5.6), prepare spiking solutions by appropriate dilution in a 100-ml volumetric flaskcontaining diisopropyl ether (5.4.1). Prepare the spiking solutions at concentrations such that the aqueouscalibration solutions (5.9) will cover the working range of the analytical system. Store spiking solutions in arefrigerator between 2 °C and 5 °C. Let the solutions adjust to room temperature before preparing calibrationsolutions. The storage time shall not exceed one month.5.9 Epichlorohydrin calibration solutions for the multipoint calibrationPrepare aqueous calibration solutions from the spiking solutions (5.8) by injection of an appropriate volume (e.g.10 µl) of the spiking solution directly into 100 ml of water (5.1). However, do not use more than 100 µl of a spikingsolution to produce the calibration solutions. Mix the aqueous calibration solutions thoroughly by inverting the flaskseveral times. Prepare five different concentration levels. Prepare calibration solutions fresh daily.Table 1 gives an example for a dilution scheme.SIST EN 14207:2003
EN 14207:2003 (E)6Table 1 — Dilution schemeMillilitre of 5.6 added to 100 ml5.4.1Analyte concentration in thespiking solution in milligram permillilitreConcentration (in microgram per litre) in thecalibration solution( 10 µl of the spiking solution added to 100 mlwater )0,20,0010,10,60,0030,31,00,0050,51,40,0070,71,80,0090,9If the desired measuring range differs from that of Table 1, different solution ratios should be taken.5.10 Solid phase materialSolid phase material on styrene-divinylbenzene copolymer basis is normally used, e.g. commercially availablecartridges or adequately glass columns filled with a minimum packing of 200 mg of the sorbent (see annex A). Arecovery of 6 Apparatus6.1 General requirementsEquipment or parts of it which may come into contact with the water sample or the extract should be free frominterfering compounds.6.2 Sample bottles, preferably brown glass, 500 ml, with glass stoppers or PTFE-lined (PTFE = polytetrafluoro-ethene) screw caps.6.3 Solid phase extraction cartridges, see 5.10.6.4 Vacuum or pressure assembly, for the extraction step.6.5 Volumetric flasks with inert stopper.6.6 Vials, suitable for automatic or manual injection, preferably brown glass, with PTFE-lined septa.6.7 Capilla
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