Water quality - Determination of selected phenoxyalkanoic herbicides, including bentazones and hydroxybenzonitriles by gas chromatography and mass spectrometry after solid phase extraction and derivatization (ISO 15913:2000)

This standard specifies a method for the determination of phenoxyalkanoic acids in ground and drinking water in mass concentrations > 0,05 µg/l. The single substances are listed in the above mentioned standard. The method includes a solid-liquid extraction,
derivatization and gas chromatography with MS detection.

Wasserbeschaffenheit - Bestimmung ausgewählten Phenoxyalkancarbonsäure-Herbiziden, einschließlich Bentazon und Hydroxybenzonitrilen mittels Gaschromatographie und massenspektrometrischer Detektion nach Fest-Flüssig-Extraktion und Derivatisierung (ISO 15913:2000)

Diese Internationale Norm legt ein Verfahren zur Bestimmung von Phenoxyalkancarbonsäuren in Grund- und Trinkwasser in Massenkonzentrationen = 50 ng/l fest (genauere Information siehe Tabelle A.1 in Anhang A). Beispiele für Phenoxyalkancarbonsäuren, die nach diesem Verfahren bestimmt werden können, siehe Tabelle 1.
Die Anwendbarkeit des Verfahrens auf weitere, in Tabelle 1 nicht genannte Verbindungen ist nicht ausgeschlossen; sie muss jedoch im Einzelfall geprüft werden (siehe Anhang B).

Qualité de l'eau - Dosage de certains herbicides phénoxyalcanoiques, y compris bentazones et hydroxybenzonitriles, par chromatographie en phase gazeuse et spectrométrie de masse apres extraction en phase solide et dérivatisation (ISO 15913:2000)

La présente Norme internationale spécifie une méthode de dosage des herbicides phenoxyalcanoïques présents
dans les eaux souterraines et les eaux destinées à la consommation humaine en concentrations en masse
W 50 ng/l (des informations détaillées sont données dans le Tableau A.1 de l'annexe A). Des exemples d'acides
phénoxyalcanoïques pouvant être déterminés par la présente méthode sont donnés dans le Tableau 1.
La présente méthode peut être appliquée à d'autres composés ne figurant pas dans le Tableau 1 ou à d'autres
types d'eau. Il convient toutefois de contrôler l'applicabilité de la présente méthode à ces cas spéciaux (voir
l'annexe B).
Tableau 1 — Agents de protection des plantes pouvant être déterminés par la présente méthode

Kakovost vode - Določevanje izbranih fenoksialkanojskih herbicidov, vključno bentazonov in hidroksibenzonitrilov, s plinsko kromatografijo in masno spektrometrijo po ekstrakciji na trdni fazi in derivatizaciji (ISO 15913:2000)

General Information

Status
Published
Publication Date
31-Aug-2003
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Sep-2003
Due Date
01-Sep-2003
Completion Date
01-Sep-2003

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PDVQRWasserbeschaffenheit - Bestimmung ausgewählten Phenoxyalkancarbonsäure-Herbiziden, einschließlich Bentazon und Hydroxybenzonitrilen mittels Gaschromatographie und massenspektrometrischer Detektion nach Fest-Flüssig-Extraktion und Derivatisierung (ISO 15913:2000)Qualité de l'eau - Dosage de certains herbicides phénoxyalcanoiques, y compris bentazones et hydroxybenzonitriles, par chromatographie en phase gazeuse et spectrométrie de masse apres extraction en phase solide et dérivatisation (ISO 15913:2000)Water quality - Determination of selected phenoxyalkanoic herbicides, including bentazones and hydroxybenzonitriles by gas chromatography and mass spectrometry after solid phase extraction and derivatization (ISO 15913:2000)13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN ISO 15913:2003SIST EN ISO 15913:2003en01-september-2003SIST EN ISO 15913:2003SLOVENSKI
STANDARD



SIST EN ISO 15913:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 15913March 2003ICS 13.060.50English versionWater quality - Determination of selected phenoxyalkanoicherbicides, including bentazones and hydroxybenzonitriles bygas chromatography and mass spectrometry after solid phaseextraction and derivatization (ISO 15913:2000)Qualité de l'eau - Dosage de certains herbicidesphénoxyalcanoïques, y compris bentazones ethydroxybenzonitriles, par chromatographie en phasegazeuse et spectrométrie de masse après extraction enphase solide et dérivatisation (ISO 15913:2000)Wasserbeschaffenheit - Bestimmung ausgewähltenPhenoxyalkancarbonsäure-Herbiziden, einschließlichBentazon und Hydroxybenzonitrilen mittelsGaschromatographie und massenspektrometrischerDetektion nach Fest-Flüssig-Extraktion und Derivatisierung(ISO 15913:2000)This European Standard was approved by CEN on 9 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, Slovak Republic, Spain, Sweden, Switzerland andUnited Kingdom.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 ISO 15913:2003 ESIST EN ISO 15913:2003



EN ISO 15913:2003 (E)2ForewordThe text of ISO 15913:2000 has been prepared by Technical Committee ISO/TC 147 "Waterquality" of the International Organization for Standardization (ISO) and has been taken over asEN ISO 15913:2003 by Technical Committee CEN/TC 230 "Water analysis", the secretariat ofwhich is held by DIN.This European Standard shall be given the status of a national standard, either by publication ofan identical text or by endorsement, at the latest by September 2003, and conflicting nationalstandards shall be withdrawn at the latest by September 2003.According to the CEN/CENELEC Internal Regulations, the national standards organizations ofthe following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,Luxembourg, Malta, Netherlands, Norway, Portugal, Slovak Republic, Spain, Sweden,Switzerland and the United Kingdom.Endorsement noticeThe text of ISO 15913:2000 has been approved by CEN as EN ISO 15913:2003 without anymodifications.NOTE
Normative references to International Standards are listed in Annex ZA (normative).SIST EN ISO 15913:2003



EN ISO 15913:2003 (E)3Annex ZA(normative)Normative references to international publicationswith their relevant European publicationsThis European Standard incorporates by dated or undated reference, provisions from otherpublications. These normative references are cited at the appropriate places in the text and thepublications are listed hereafter. For dated references, subsequent amendments to or revisions ofany of these publications apply to this European Standard only when incorporated in it byamendment or revision. For undated references the latest edition of the publication referred toapplies (including amendments).NOTE Where an International Publication has been modified by common modifications, indicatedby (mod.), the relevant EN/HD applies.PublicationYearTitleENYearISO 5667-11980Water quality - Sampling - Part 1:Guidance on the design ofsampling programmesEN 25667-11993ISO 5667-21991Water quality - Sampling - Part 2:Guidance on sampling techniquesEN 25667-21993ISO 5667-31994Water quality - Sampling - Part 3:Guidance on the preservation andhandling of samplesEN ISO 5667-31995SIST EN ISO 15913:2003



SIST EN ISO 15913:2003



ReferencenumberISO15913:2000(E)©ISO2000INTERNATIONALSTANDARDISO15913Firstedition2000-04-01Waterquality—Determinationofselectedphenoxyalkanoicherbicides,includingbentazonesandhydroxybenzonitrilesbygaschromatographyandmassspectrometryaftersolidphaseextractionandderivatizationQualitédel'eau—Dosagedecertainsherbicidesphénoxyalcanoïques,ycomprisbentazonesethydroxybenzonitriles,parchromatographieenphasegazeuseetspectrométriedemasseaprèsextractionenphasesolideetdérivatisationSIST EN ISO 15913:2003



ISO15913:2000(E)PDFdisclaimerThisPDFfilemaycontainembeddedtypefaces.InaccordancewithAdobe'slicensingpolicy,thisfilemaybeprintedorviewedbutshallnotbeeditedunlessthetypefaceswhichareembeddedarelicensedtoandinstalledonthecomputerperformingtheediting.Indownloadingthisfile,partiesacceptthereintheresponsibilityofnotinfringingAdobe'slicensingpolicy.TheISOCentralSecretariatacceptsnoliabilityinthisarea.AdobeisatrademarkofAdobeSystemsIncorporated.DetailsofthesoftwareproductsusedtocreatethisPDFfilecanbefoundintheGeneralInforelativetothefile;thePDF-creationparameterswereoptimizedforprinting.EverycarehasbeentakentoensurethatthefileissuitableforusebyISOmemberbodies.Intheunlikelyeventthataproblemrelatingtoitisfound,pleaseinformtheCentralSecretariatattheaddressgivenbelow.©ISO2000Allrightsreserved.Unlessotherwisespecified,nopartofthispublicationmaybereproducedorutilizedinanyformorbyanymeans,electronicormechanical,includingphotocopyingandmicrofilm,withoutpermissioninwritingfromeitherISOattheaddressbeloworISO'smemberbodyinthecountryoftherequester.ISOcopyrightofficeCasepostale56CH-1211Geneva20Tel.+41227490111Fax+41227341079E-mailcopyright@iso.chWebwww.iso.chPrintedinSwitzerlandii©ISO2000–AllrightsreservedSIST EN ISO 15913:2003



ISO15913:2000(E)©ISO2000–AllrightsreservediiiContentsPageForeword.iv1Scope.12Normativereferences.23Term,definition,abbreviationsandsubscripts.24Principle.35Interferences.36Reagents.37Apparatus.68Sampling.79Procedure.710Calculation.1411Precision.1512Testreport.15AnnexA(informative)Resultsofaninterlaboratorytrial.16AnnexB(informative)Furthersubstanceswhichmaybeanalysedbythisprocedure.17AnnexC(informative)Exampleofhydrolysisofphenoxyalkanoiccarbonicesters.18AnnexD(informative)Massspectraforsomephenoxyalkanoicherbicides.19SIST EN ISO 15913:2003



ISO15913:2000(E)iv©ISO2000–AllrightsreservedForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,inliaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3.DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting.PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote.AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectofpatentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.InternationalStandardISO15913waspreparedbyTechnicalCommitteeISO/TC147,Waterquality,SubcommitteeSC2,Physical,chemicalandbiochemicalmethods.AnnexesA,B,CandDofthisInternationalStandardareforinformationonly.SIST EN ISO 15913:2003



INTERNATIONALSTANDARDISO15913:2000(E)©ISO2000–Allrightsreserved1Waterquality—Determinationofselectedphenoxyalkanoicherbicides,includingbentazonesandhydroxybenzonitrilesbygaschromatographyandmassspectrometryaftersolidphaseextractionandderivatizationWARNING—Diazomethaneisexplosive,extremelytoxicandseverelyirritating,causingpulmonaryoedemawheninhaledinhighconcentrations.Long-term,low-levelexposuremayleadtosensibilization,resultinginasthma-likesymptoms.Also,diazomethaneandseveralofitschemicalprecursorshavebeencitedascarcinogens.1ScopeThisInternationalStandardspecifiesamethodforthedeterminationofphenoxyalkanoicacidsingroundanddrinkingwaterinmassconcentrations50ng/l(detailedinformationisgiveninTableA.1ofannexA).ExamplesofphenoxyalkanoicacidswhichcanbedeterminedbythismethodaregiveninTable1.ThismethodmaybeapplicabletocompoundsnotmentionedinTable1ortoothertypesofwater.However,itisnecessarytoverifytheapplicabilityofthismethodforthesespecialcases(seeannexB).Table1—PlanttreatmentagentsdeterminedbythismethodNameMolecularformulaRelativemolecularmassCASregistryNo.(2,4-Dichlorophenoxy)aceticacidC8H6Cl2O3221,094-75-7MecopropC10H11ClO3214,6593-65-2DichlorpropC9H8Cl2O3235,06120-36-5MCPAC9H9ClO3200,694-74-6MCPBC11H13ClO3228,6794-81-5(2,4,5-Trichlorophenoxy)aceticacidC8H5Cl3O3255,593-76-5BentazoneC10H12N2O3S240,325057-89-0BromoxynilC7H3Br2NO276,91689-84-54-(2,4-Dichlorophenoxy)-butanoicacidC10H10Cl2O3249,194-82-6FenopropC9H7Cl3O3269,5193-72-1SIST EN ISO 15913:2003



ISO15913:2000(E)2©ISO2000–Allrightsreserved2NormativereferencesThefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsofthisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthesepublicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedtoinvestigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintainregistersofcurrentlyvalidInternationalStandards.ISO5667-1:1980,Waterquality—Sampling—Part1:Guidanceonthedesignofsamplingprogrammes.ISO5667-2:1991,Waterquality—Sampling—Part2:Guidanceonsamplingtechniques.ISO5667-3:1994,Waterquality—Sampling—Part3:Guidanceonthepreservationandhandlingofsamples.3Term,definition,abbreviationsandsubscripts3.1TermanddefinitionForthepurposesofthisInternationalStandard,thefollowingtermanddefinitionapplies.3.1.1phenoxyalkanoicherbicidesherbicideswhichundergoderivatizationwithdiazomethaneandwhichmaysubsequentlybedeterminedbygaschromatographyEXAMPLETypicalphenoxyalkanoicherbicidesincludealkylhalogenatedphenoxyacids,hydroxybenzonitrilesandbentazone.3.2Abbreviations2,4-D(2,4-dichlorophenoxy)aceticacid2,4-DB4-(2,4-dichlorophenoxy)butanoicacid2,4-DPdichlorpropMCPPmecoprop2,4,5-T(2,4,5-trichlorophenoxy)aceticacid2,4-TPfenoprop3.3SubscriptsccalibrationstepusinganexternalstandardgoverallprocedureiidentityofthesubstanceiisinternalstandardjconsecutivefigurejforpairsofvaluessamsamplesolsolventSIST EN ISO 15913:2003



ISO15913:2000(E)©ISO2000–Allrightsreserved34PrincipleAfteracidification,substancesareenrichedonsolidphaseadsorbentmaterial[forexampleRP1)-C18material],elutedwithsolvent,methylatedwithdiazomethaneandthendeterminedbygaschromatographyusingamassspectrometricdetector.Insomecases,thesubstancesmaybepresentastheiresters,forexampleoctanoicesters.Hydrolysisofthewatersample(seeannexC)mayleadtohigherconcentrationsofthefreeacids.5Interferences5.1OccurrenceInterferencesmayoccurespeciallywhenexaminingothertypesofwater,forexamplesurfacewater.5.2SamplingToavoidinterferencescollectthesampleasdescribedinclause8.5.3EnrichmentThecommerciallyavailableadsorbentmaterialsareoftenofvaryingquality.Considerablebatch-to-batchdifferencesinqualityandselectivityofthismaterialarepossible.Therecoverymayvarywiththeconcentration.Therefore,checkrecoveryregularlyatdifferentconcentrations.Performcalibrationandanalysiswithmaterialtakenonlyfromthesamebatch.Suspendedmatterinthewatersample(suchasironhydroxide,calciumcarbonate)occurringduringsampling,storageandsamplepreparation,oranincreaseintheconcentrationofmicroorganismsmayclogthepacking.Inthiscase,filterthewatersamplethroughaglassfibrefilterpriortoenrichment.5.4GaschromatographyandmassspectrometryUsetheoperationalconditionssetinaccordancewithmanufacturer'sinstructions.Checkthesesettingsatregularintervals.Generalinterferences,causedbytheinjectionsystemorinsufficientseparationcanbeeliminatedwiththehelpofspeciallaboratoryexperienceandtheinstrument'smanuals.6Reagents6.1GeneralUse,asfarasavailable,"forresidualanalysis"reagents.Useonlyreagentsandwaterwithnegligiblylowimpurities,i.e.resultingincleanblanks.6.2Operatinggasesforthegaschromatography/massspectrometry,ofhighpurityandinaccordancewithmanufacturer'sspecifications.6.3Nitrogen,ofhighpurity,i.e.minimum99,996%byvolume,fordryingandeventuallyforconcentrationbyevaporation.6.4Hydrochloricacid,c(HCl)=2mol/l.6.5Diethylether,C4H10O,stabilized.1)RP=reversedphaseSIST EN ISO 15913:2003



ISO15913:2000(E)4©ISO2000–Allrightsreserved6.6Ethanol,C2H5OH.6.7Aceticacid,CH3COOH,10%byvolume,aqueoussolution(usedtodestroydiazomethane).6.8Sodiumhydroxidesolution,c(NaOH)=6mol/l.6.9Solventsfortheelution,forexampleacetoneC3H6O,ormethanol,CH3OH.6.10Methanol,CH3OH,asconditioningagent.6.11Potassiumhydroxidesolution,KOH,volumicmassof60%.6.12Diazald(N-methyl-N-nitroso-4-toluenesulfonamide),C8H10N2O3S.6.13Solidphaseadsorbentmaterial,mostcommonlyRP-C18-material,intheformofcommerciallyavailablecartridgesoradequatelyglasscolumnsfilledaccordingto7.4withaminimumpackingof1,0g.Forselectivityofthematerialsee5.3.6.14Internalstandard,preferablydeuteratedor13C-labelledcompounds.Thestandardsareoftencommerciallyavailableataconcentrationof100µg/ml.Dilutethisstandardwithacetone.Thefinalconcentrationinthewatersampleshallbeforexampleabout100ng/l.6.15Diazomethanesolution.WARNING—Diazaldisanirritantandallskincontactshouldbeavoided.Preparediazomethaneinadistillationapparatus,suchastheoneshowninFigure1.Forsecurityreasons,installtwowashbottles;keepthefirstoneemptyforthepurposeofprotectingthesolutionfrombackflushandfillthesecondwithaceticacid(6.7).Insert8mloftheKOHsolution(6.11)and10mlofethanol(6.6)ina250mlreactionflask.Suspend5,0gofdiazald(6.12)in45mlofdiethylether(6.5)inapressure-equalizingfunnel.Cautiouslywarmthereactionflasktoabout60°C(waterbath)and,within20min,dropwiseaddthediazaldsuspensionfromthefilterfunnel.Collectthediazomethanebeingformedduringthisprocessandthediethyletherinthetrap(cooledwithice/NaCl).Afterthisreaction,addanadditional10mlofdiethyletherthroughthefilterfunnelanddistiltheremainingdiazomethane.Stopperthetrapandstoreitatabout18°C.Checkthestabilityofthediazomethanewhichshouldhaveanintensiveyellowcolour.NOTEExcessdiazomethanemaybedestroyedbyaddingasolutionofaceticacid(6.7).Priortocleaning,rinsealldiazomethaneglasswarewithaceticacid(6.7).SIST EN ISO 15913:2003



ISO15913:2000(E)©ISO2000–Allrightsreserved5Figure1—Exampleofadistillationapparatus6.16Referencesubstances:6.16.1Methylesterreferencesubstances(methylestersoftheacidslistedinTable1)ofdefinedconcentrationsuitableforthepreparationofreferencesolutionsforgaschromatography.6.16.1.1Solutionsofindividualmethylesters.Asanexample,place50,0mgeachofareferencesubstanceintoa100mlvolumetricflask,dissolvewithacetone(6.9)anddilutetovolume.Storethesolutionat18°C,protectedfromlight.Checktheconcentrationregularly.6.16.1.2Methylesterstocksolutions.Asanexample,pipette1mlofeachofthesolutionoftheindividualsubstance(6.16.1.1)intoa100mlvolumetricflaskanddilutetovolumewithacetone(see6.9).Storethesolutionsat18°C,protectedfromlight.Checktheconcentrationofthestocksolutionsregularly.6.16.1.3Methylesterreferencesolutions(workingstandardsolution).Preparethereferencesolutionsbyanadequatedilutionofthestocksolution(6.16.1.2).Storethereferencesolutionintherefrigerator.Referencesolutionsarestableforabout6months.SIST EN ISO 15913:2003



ISO15913:2000(E)6©ISO2000–Allrightsreserved6.16.2Free-acidreferencesubstances:6.16.2.1Solutionsoftheindividualfreeacid.Asanexample,place50,0mgofeachofthereferencesubstanceintoa100mlvolumetricflask,dissolvewithacetone(6.9)anddilutetovolume.Storethesolutionsat18°C,protectedfromlight.Checktheconcentrationofthestocksolutionsregularly.6.16.2.2Free-acidstocksolution(intermediatestandardsolutions).Asanexample,pipette1mlofeachofthesolutionsoftheindividualfreeacid(6.16.2.1)intoa100mlvolumetricflaskanddilutetovolume.Storethesolutionsat18°C,protectedfromlight.Checktheconcentrationofthefree-acidstocksolutionsregularly.6.16.2.3Free-acidreferencesolutions(workingstandardsolutions).Preparethesolutionsbyadequatedilutionofthestocksolution(6.16.2.2).Storethefree-acidreferencesolutionsinarefrigerator.Theirshelf-lifeislimited.7Apparatus7.1GeneralrequirementsEquipmentorpartsofitwhicharelikelytocomeintocontactwiththewatersampleoritsextractshallbefreefromresiduescausinginterferences.Itisrecommendedtousevesselsmadeofglassorstainlesssteel.7.2Flat-bottomedflasks,preferablybrownglass,1000mland2000ml,withglassstoppers.7.3Graduatedcylinders,1000ml.7.4Cartridges,madeofpolypropeneorglass,filledwithsolid-phasematerial,forexampleRP-C18material,(6.13).NOTEThecartridgesarecommerciallyavailable.7.5Vacuumpumporpressureassembly.7.6Vials,suitableforautomaticormanualinjection.7.7Volumetricflasks,10mlor100ml.7.8Capillarygaschromatograph,equippedwithanon-discriminatinginjectionsystemandamass-spectrometricdetector.7.9Capillarycolumns,forgaschromatography;forexamplesseeannexD,FiguresD.5andD.6.7.10Glass-fibrefilters,madeofborosilicateglass,offibrediameterforexamplefrom0,75µmto1,5µm,withinorganicbindingmaterial.SIST EN ISO 15913:2003



ISO15913:2000(E)©ISO2000–Allrightsreserved77.11pHmeter.7.12Injectionsyringes,nominalcapacity5µlandhigher.7.13Apparatusforpreparingdiazomethane,(seeexampleinFigure1),comprisingthefollowing:double-necked,round-bottomedflask,250mlcapacity;pressure-equalizingfunnel,100mlcapacity;distillationcolumn,forexampleVigreuxcolumn;distillationhead;condenser,forexampleLiebigcondenser;flaskforabsorptionofdiazomethane;securityflask;oracomme
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