SIST EN ISO 15913:2003
(Main)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)
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 International Standard specifies a method for the determination of phenoxyalkanoic acids in ground and
drinking water in mass concentrations W 50 ng/l (detailed information is given in Table A.1 of annex A). Examples
of phenoxyalkanoic acids which can be determined by this method are given in Table 1.
This method may be applicable to compounds not mentioned in Table 1 or to other types of water. However, it is
necessary to verify the applicability of this method for these special cases (see annex B).
Table 1 — Plant treatment agents determined by this method
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
- KAV - Water quality
- Current Stage
- 6060 - National Implementation/Publication (Adopted Project)
- Start Date
- 01-Sep-2003
- Due Date
- 01-Sep-2003
- Completion Date
- 01-Sep-2003
Relations
- Effective Date
- 01-Sep-2003
Overview
EN ISO 15913:2003 (ISO 15913:2000 adopted by CEN) defines an analytical method for determining selected phenoxyalkanoic herbicides (and related compounds such as bentazones and hydroxybenzonitriles) in groundwater and drinking water. The procedure combines solid phase extraction (SPE), derivatization (methylation with diazomethane), and analysis by gas chromatography–mass spectrometry (GC–MS). The method is suitable for low-level quantification - mass concentrations on the order of 50 ng/L (see Annex A for details) - and lists example target compounds (e.g., 2,4‑D, MCPP, MCPA, dichlorprop, bentazone, bromoxynil).
Key Topics and Requirements
- Scope and applicability: Validated for phenoxyalkanoic acids in ground and drinking water; applicability to other compounds or water types must be verified (Annex B).
- Sampling guidance: References ISO 5667 series for sampling, preservation and handling to avoid contamination or loss.
- Enrichment (SPE): Acidify sample and enrich analytes on reversed‑phase adsorbent (commonly RP‑C18 cartridges or glass columns). The standard notes batch-to-batch variability of commercial sorbents and recommends performance checks and consistent use of the same batch.
- Derivatization: Convert acids to methyl esters using diazomethane prior to GC–MS. (WARNING: diazomethane is explosive and highly toxic; strict safety precautions required.)
- Instrumental analysis: Separation and detection by GC–MS with internal standards (preferably deuterated or 13C-labelled). Calibration and blank control are mandatory; the standard addresses interferences and instrument maintenance.
- Quality control: Use of reference solutions (methyl ester and free‑acid standards), internal standards, recovery checks at various concentrations, and interlaboratory trial data (Annex A).
- Supporting material: Annex C on hydrolysis of esterified forms; Annex D includes example mass spectra.
Practical Applications and Users
This standard is designed for:
- Environmental and water quality laboratories performing pesticide and herbicide monitoring
- Regulatory and public‑health authorities assessing drinking water compliance
- Contract analytical labs offering trace-level pesticide analysis in groundwater
- Research groups studying environmental fate of phenoxyalkanoic herbicides
Typical uses include routine monitoring, compliance testing, trend analysis, and validation of remediation efforts.
Related Standards
- ISO 5667‑1, ISO 5667‑2, ISO 5667‑3 - guidance on sampling programmes, sampling techniques and sample preservation
- Adopted as EN ISO 15913:2003 by CEN (European adoption)
Keywords: EN ISO 15913:2003, water quality, phenoxyalkanoic herbicides, SPE, derivatization, diazomethane, GC–MS, drinking water, groundwater, analytical method.
Frequently Asked Questions
SIST EN ISO 15913:2003 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "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 covers: This International Standard specifies a method for the determination of phenoxyalkanoic acids in ground and drinking water in mass concentrations W 50 ng/l (detailed information is given in Table A.1 of annex A). Examples of phenoxyalkanoic acids which can be determined by this method are given in Table 1. This method may be applicable to compounds not mentioned in Table 1 or to other types of water. However, it is necessary to verify the applicability of this method for these special cases (see annex B). Table 1 — Plant treatment agents determined by this method
This International Standard specifies a method for the determination of phenoxyalkanoic acids in ground and drinking water in mass concentrations W 50 ng/l (detailed information is given in Table A.1 of annex A). Examples of phenoxyalkanoic acids which can be determined by this method are given in Table 1. This method may be applicable to compounds not mentioned in Table 1 or to other types of water. However, it is necessary to verify the applicability of this method for these special cases (see annex B). Table 1 — Plant treatment agents determined by this method
SIST EN ISO 15913:2003 is classified under the following ICS (International Classification for Standards) categories: 13.060.50 - Examination of water for chemical substances. The ICS classification helps identify the subject area and facilitates finding related standards.
SIST EN ISO 15913:2003 has the following relationships with other standards: It is inter standard links to SIST ISO 15913:2001. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
SIST EN ISO 15913:2003 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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
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
Normative references to International Standards are listed in Annex ZA (normative).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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