1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN ISO 10695:2000 The
2、European Standard EN ISO 10695:2000 has the status of a British Standard ICS 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Water quality Determination of selected organic nitrogen and phosphorus compounds Gas chromatographic methodsThis British Standard, having bee
3、n prepared under the direction of the Health and Environment Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 October 2000 BSI 10-2000 ISBN 0 580 34634 X BS EN ISO 10695:2000 Amendments issued since publication Amd. No. Date Comments National
4、 foreword This British Standard is the official English language version of EN ISO 10695:2000. It is identical with ISO 10695:2000. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical present to the responsible
5、international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this subcommittee can be obtained on reques
6、t to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these international or Eur
7、opean publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the nec
8、essary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title pag
9、e, EN ISO foreword page, ISO title page, pages ii to iv, pages 1 to 23, the annex ZA page, an inside back cover and a back cover. The BSI copyright notice displayed this document indicates when the document was last issued.EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO10695 April2000 ICS13.060
10、 Englishversion WaterqualityDeterminationofselectedorganicnitrogenand phosphoruscompoundsGaschromatographicmethods(ISO 10695:2000) QualitdeleauDosagedecertainscomposs organiquesazotsetphosphorsslectionnsMthodes parchromatographieenphasegazeuse(ISO10695:2000) WasserbeschaffenheitBestimmungausgewhlter
11、 organischerStickstoffundPhosphorverbindungen GaschromatographischeVerfahren(ISO10695:2000) ThisEuropeanStandardwasapprovedbyCENon25February2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwitho
12、utanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofa
13、CENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandand
14、UnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO10695:2000EForeword Corrected2 000 081
15、7 Thetext oft heI nternationalS tandard ISO1 0695:2000 hasb een preparedbyTech nical Committee ISO/TC 147 “Water quality“incolla boration withTech nicalCo mmittee CEN/TC 230“Wateran alysis“, the secretariato f whichis heldby DIN. ThisEurop ean Standardsh all be given thesta tuso f a nationalsta ndar
16、d, eitherby publication ofan identical textorby endorsement,atthe latestbyOct ober2 000, and conflicting national standardssh allb e withdrawna t the latestbyOcto ber2 000. Accordingt o the CEN/CENELEC Internal Regulations,t hen ationalsta ndardsor ganizationsof the followingc ountriesare bound toim
17、ple ment this EuropeanS tandard: Austria,B elgium, CzechRe public,D enmark, Finland,France, Germany,Greece,Ic eland,Ir eland, Italy, Luxembourg,Ne therlands, Norway,Portu gal,S pain, Sweden, Switzerland and the United Kingdom. Endorsementnotice Thetext oft heI nternationalS tandard ISO1 0695:2000 wa
18、sa pprovedby CEN asaEuro pean Standard withoutany modification. NOTE:No rmativerefer encesto International Standardsareliste d in annexZA( normative). EN ISO 10695:2000Referencenumber ISO10695:2000(E) INTERNATIONAL STANDARD ISO 10695 Firstedition 2000-04-01 WaterqualityDeterminationofselected organi
19、cnitrogenandphosphorus compoundsGaschromatographic methods Qualit de leau Dosage de certains composs organiques azots et phosphors slectionns Mthodes par chromatographie en phase gazeuse EN ISO 10695:2000ii EN ISO 10695:2000 iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences2 3 Liquid/liqu
20、idextraction.2 3.1 Principle2 3.2 Reagents.2 3.3 Apparatus.4 3.4 Samplingandsamplepreparation.4 3.5 Procedure.5 4 Liquid/solidextraction6 4.1 Principle6 4.2 Reagents.7 4.3 Apparatus.8 4.4 Sampling.8 4.5 Procedure(forRP-C18material)8 5 Calibration9 5.1 General9 5.2 Calibrationusingexternalstandards9
21、5.3 Calibrationusinganinternalstandard13 6 Identificationandcalculation.14 6.1 Identificationofindividualcompounds.14 6.2 Calculation14 6.3 Summaryofresults.15 7 Expressionofresults16 8 Testreport16 AnnexA(informative)Detectionlimitsofcertainorganicnitrogenandphosphoruscompounds17 AnnexB(informative
22、)Examplesofgaschromatograms.18 AnnexC(informative)Characteristicionsformassspectrometry22 AnnexD(informative)Precisiondataforcertainorganicnitrogenandphosphoruscompounds (liquid/solidextractionmethod).23 EN ISO 10695:2000iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefede
23、rationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,government
24、alandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandard
25、sadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresp
26、onsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO10695waspreparedbyTechnicalCommitteeISO/TC147, Water quality, SubcommitteeSC2, Physical, chemical and biochemical methods. AnnexesA,B,CandDofthisInternationalStandardareforinformationonly. EN ISO 10695:2000 1 WaterqualityDetermin
27、ationofselectedorganicnitrogenand phosphoruscompoundsGaschromatographicmethods WARNINGThisInternationalStandardmakesuseofflammableandtoxicorganicsolventsandsome toxicorganicandphosphoruscompounds.Observethesafetyregulationsineffect. 1 Scope ThisInternationalStandardspecifiestwomethodsforthedetermina
28、tionofcertainorganicnitrogenandphosphorus compoundsinwatersbygaschromatography(seeTable1). Themethodsmaybeextendedtoincludeadditionalsubstances,providedthemethodsarevalidatedforeach individualcase. Clause3describestheliquid/liquidextractionmethod,whichisapplicabletosamplesofdrinkingwaters,ground wat
29、ers,surfacewatersandwastewaterscontainingupto0,05g/lofsuspendedsolids.Inthepresenceoforganic matter,suspendedmatterandcolloids,interferencesaremorenumerousandconsequentlythedetectionlimitsof thismethodcanbehigher. NOTE Becauseoftheverylowconcentrationsnormallypresentinthewaters,theproblemofcontamina
30、tionisextremely important.Thelowerthelevelmeasured,themoreprecautionshavetobeobserved. Clause4describestheliquid/solidextractionmethodwhichisapplicabletosamplesofgroundwater,surfacewater anddrinkingwatercontainingmassconcentrationsofaboutW0,05g/l.Interferencesoccurringwiththe examinationofsometypeso
31、fsurfacewatercanpreventtheapplicationofthismethod. DetectionlimitsaregivenforinformationinannexA. NOTE WhenapplyingthisInternationalStandard,theguideonanalyticalqualitycontrolforwateranalysis(see ISO/TR13530)shouldbefollowed. EN ISO 10695:20002 Table1Organicnitrogenandphosphoruscompoundsanalysedbyth
32、esemethods Name Molecularformula Molarmass CASNo. a Atrazine C 8 H 14 ClN 5 215,7 001912-24-9 Cyanazine C 9 H 13 ClN 6 240,7 021725-46-2 Metazachlor C 14 H 16 ClN 3 O 277,8 067129-08-2 Parathion(ethyl) C 10 H 14 NO 5 PS 291,3 00056-38-2 Parathion(methyl) C 8 H 10 NO 5 PS 263,2 298-00-0 Pendimethalin
33、 C 13 H 19 N 3 O 4 281,3 040487-42-1 Propazine C 9 H 16 ClN 5 229,7 000139-40-2 Sebuthylazine C 9 H 16 ClN 5 229,7 007286-69-3 Simazine C 7 H 12 ClN 5 201,7 000122-34-9 Terbuthylazine C 9 H 16 ClN 5 229,7 005915-41-3 Trifluralin C 13 H 16 F 3 N 3 O 4 335,3 001582-09-8 Vinclozolin C 12 H 9 Cl 2 NO 3
34、286,1 050471-44-8 a ChemicalAbstractsRegistryNumber. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.Howeve
35、r,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInterna
36、tionalStandards. ISO5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. ISO/TR13530:1997, Water quality Guide to analytical quality control for water analysis. 3 Liquid/liquidextrac
37、tion 3.1 Principle Theorganicnitrogenandphosphoruscompoundsinthewatersampleareextractedbyliquid-liquidextractionwith dichloromethane.Afterconcentration,thesampleextractsareanalysedbygaschromatography,usinganitrogen- phosphorusdetector. 3.2 Reagents Allreagents,includingwater,shallbeofsufficientpurit
38、ythattheydonotgiverisetosignificantinterferingpeaksin thegaschromatogramsoftheblanks.Thepurityofreagentsusedintheprocedureshallbeverifiedforeachbatch ofmaterialbyrunningblankdeterminations(3.5.6). Reagentsshallbestoredinglasscontainers. EN ISO 10695:2000 3 NOTE Commercial“pesticidegrade“solventsarea
39、vailable.Theuseoftheseproductsisrecommendedonlyafterverifying theirquality.Thequalityofasolventischeckedbyevaporationofabout200mldownto1mlandanalysisoftheconcentrateto determinethecompoundssubsequentlyanalysed.Thesolventshouldbeconsideredacceptableifitdoesnotgiveany detectableinterferingpeaksinthech
40、romatogramforthesubstanceofinterest. 3.2.1 Water,purifiedusing,forexample,ionexchangeandcarboncolumnadsorption. 3.2.2 Dichloromethane(CH 2 Cl 2 )extractionsolvent. 3.2.3 Solventsfordissolution,e.g.acetoneorethylacetate. 3.2.4 Sodiumsulfate,anhydrous HeatNa 2 SO 4 powderat500 C 20 Cfor4h 30min,coolto
41、about200 Cinamufflefurnaceandthento ambienttemperatureinadesiccatorcontainingmagnesiumperchlorateorequivalentalternative. 3.2.5 Solutionsforneutralization a) Sodiumhydroxide,aqueoussolution,c(NaOH)=1mol/l. b) Hydrochloricacid,aqueoussolution,c(HCl)=1mol/l. 3.2.6 Standardstocksolutions Standardstocks
42、olutionsshallbepreparedbydissolvingpureor,ifavailable,certifiedorganicnitrogenand phosphoruscompoundsinacetone(3.2.3). Unlessmanufacturersinformationorstabilitytrialsindicateotherwise,storethesolutionsataround+4 Cinthe dark(theycanbestoredataround 18 C,butsomeseptaclosuresmayhardenatsuchatemperature
43、with possiblelossesofsolvent). ForcompoundslistedinTable1,thestocksolutionsarestableforaroundsixmonths.Forothercompounds,the laboratoryshallcheckthestabilityofthesolutions. Priortouse,thesolutionsshallbebroughttoambienttemperature. NOTE1 Aconvenientconcentrationofstandardstocksolutionisobtainedbywei
44、ghingaccuratelyapproximately50,0mgof eachdeterminandanddissolvingitin100mlofacetone(3.2.3). NOTE2 Certifiedcommercialstandardsmaybeused. 3.2.7 Intermediatestandardsolutions Prepareintermediatestandardsolutionsbyasuitabledilutionofthestocksolution(3.2.6)withthesolventfor dissolution(3.2.3).Atypicalva
45、lueis1mg/100ml. Unlessmanufacturersinformationorstabilitytrialsindicateotherwise,storethesesolutionsataround+4 Cinthe dark. ForcompoundslistedinTable1,theintermediatestandardsolutionsarestableuptotwomonthsinacetone, exceptforcyanazineandvinclozolin(oneweek).Forothercompounds,thelaboratoryshallcheckt
46、hestabilityof thesolutions. 3.2.8 Workingstandardsolutions Prepareatleastfivedifferentconcentrationsbysuitabledilutionsoftheintermediatestandardsolutions(3.2.7)with thesolventfordissolution(3.2.3).Asuitableconcentrationrangeis1gto100gper100ml. EN ISO 10695:20004 Unlessmanufacturersinformationorstabi
47、litytrialsindicateotherwise,storethesesolutionsataround+4 Cinthe dark. ThelifetimeofthesesolutionsislimitedtooneweekforthecompoundslistedinTable1.Forothercompounds,the laboratoryshallcheckthestabilityofthesolutions. NOTE Attheselowconcentrations,degradationbylightandadsorptionontotheglassbecomemorea
48、pparent. 3.3 Apparatus 3.3.1 Gaschromatograph,fittedwithacapillarycolumn,anitrogen-phosphorusdetectorandadataprocessing system. Atleasttwoglassorfused-silicacapillarycolumnsshallbeused,withaninsidediameteroflessthan0,4mmanda lengthof25mto60m,coatedwithstationaryphasesofdifferentpolarityallowingtheseparationofthecompounds ofinterest. NOTE Ifamassspectrometerisusedforconfirmation,onecapillarycolumnisnormallysufficient. AnnexBprovidesexamplesofgaschr
