EN ISO 17993-2003 en Water quality Determination of 15 polycyclic aromatic hydrocarbons (PAH) in water by HPLC with fluorescence detection after liquid-liquid extraction《水质 用液-液萃取后.pdf

1、BRITISH STANDARD BS EN ISO 17993:2003 BS 6068-2.79:2003 Incorporating Amendment No. 1 to BS ISO 17993:2002 (renumbers the BS ISO as BS EN ISO 17993: 2003) Water quality Determination of 15 polycyclic aromatic hydrocarbons (PAH) in water by HPLC with fluorescence detection after liquid-liquid extract

2、ion The European Standard EN ISO 17993:2003 has the status of a British Standard ICS 13.060.50 BS EN ISO 17993:2003 This British Standard, having been prepared under the direction of the Health and Environment Sector Policy and Strategy Committee, was published under the authority of the Standards P

3、olicy and Strategy Committee on 17 September 2002 BSI 23 January 2004 ISBN 0 580 40357 2 National foreword This British Standard is the official English language version of EN ISO 17993:2003. It is identical with ISO 17993:2002. The UK participation in its preparation was entrusted by Technical Comm

4、ittee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. This is one of a series of standards on water quality, others of which

5、 have been, or will be, published as Sections of BS 6068. The various Sections of BS 6068 are comprised within Parts 1 to 7, which, together with Part 0, are listed below. Part 0 Introduction Part 1 Glossary Part 2 Physical, chemical and biochemical methods Part 3 Radiological methods Part 4 Microbi

6、ological methods Part 5 Biological methods Part 6 Sampling Part 7 Precision and accuracy NOTE The tests described in this British Standard should only be carried out by suitably qualified persons with an appropriate level of chemical expertise. Standard chemical procedures should be followed through

7、out. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of Bri

8、tish Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; prese

9、nt to the responsible 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. Summary of pages This document comprises a front cover, an i

10、nside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pages 1 to 20, the Annex ZA page and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication

11、 Amd. No. Date Comments 14911 23 January 2004 Implementation of the European StandardEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO17993 November2003 ICS13.060.50 Englishversion WaterqualityDeterminationof15polycyclicaromatic hydrocarbons(PAH)inwaterbyHPLCwithfluorescence detectionafterliquidl

12、iquidextraction(ISO17993:2002) QualitdeleauDosagede15hydrocarburesaromatiques polycycliques(HAP)dansleauparHPLCavecdtection parfluorescenceaprsextractionliquideliquide(ISO 17993:2002) WasserbeschaffenheitBestimmungvon15polycyclischen aromatischenKohlenwasserstoffen(PAK)inWasserdurch HPLCmitFluoresze

13、nzdetektionnachFlssigFlssig Extraktion(ISO17993:2002) ThisEuropeanStandardwasapprovedbyCENon3November2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliog

14、raphicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtot

15、heManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUR

16、OPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO17993:2003EINESO71:3992003(E) 2 Foreword ThetextofISO17993

17、:2002hasbeenpreparedbyTechnicalCommitteeISO/TC147“Water quality”oftheInternationalOrganizationforStandardization(ISO)andhasbeentakenoveras ENISO17993:2003byTechnicalCommitteeCEN/TC230“Wateranalysis“,thesecretariatof whichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eithe

18、rbypublicationof anidenticaltextorbyendorsement,atthelatestbyMay2004,andconflictingnationalstandards shallbewithdrawnatthelatestbyMay2004. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Cze

19、ch Republic,Denmark,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,Switzerlandand theUnitedKingdom. Endorsementnotice ThetextofISO17993:2002hasbeenapprovedbyCENasENISO17993:2003withoutany modifications. NOTENormativeref

20、erencestoInternationalStandardsarelistedinAnnexZA(normative). ENISO17993:2003 Reference number ISO 17993:2002(E) OSI 2002INTERNATIONAL STANDARD ISO 17993 First edition 2002-08-15 Water quality Determination of 15 polycyclic aromatic hydrocarbons (PAH) in water by HPLC with fluorescence detection aft

21、er liquid-liquid extraction Qualit de leau Dosage de 15 hydrocarbures aromatiques polycycliques (HAP) dans leau par HPLC avec dtection par fluorescence aprs extraction liquide-liquide ENISO17993:2003IS:39971 O2002(E) DPlcsid Fremia ihTs PDF file mc yatnoaie nmt deddebyfepca.se Icca ncnadrow eitA heb

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26、 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mial coirypthgis.oc h Web ww.wiso.ch ii ISO 2002 Allr ithgsr esedevrENISO17993:2003IS:39971 O2002(E) I SO 2002 All irthgs ersedevr iiiContents Page Foreword iv Introduction. v 1 Scope 1 2 Normative references 1 3 Principle . 1 4 Interferences 3 5 Reagents

27、4 6 Apparatus. 5 7 Sampling 6 8 Procedure. 6 9 Calculation . 11 10 Precision 11 11 Test report 13 Annex A (informative) Examples of chromatographic conditions and columns . 14 Annex B (informative) Examples for the construction of special apparatus 18 ENISO17993:2003IS:39971 O2002(E) iv I SO 2002 Al

28、l irthgs ersedevrForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subj

29、ect for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IE

30、C) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committ

31、ees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO

32、 shall not be held responsible for identifying any or all such patent rights. ISO 17993 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. Annexes A and B of this International Standard are for information only. ENISO17993:20

33、03IS:39971 O2002(E) I SO 2002 All irthgs ersedevr vIntroduction Polycyclic aromatic hydrocarbons (PAH) occur in nearly all types of waters. These compounds are adsorbed on solids (sediments, suspended matter) as well as dissolved in the liquid phase. Some PAH are known or suspected to cause cancer.

34、The Council Directive 98/83/EC on the quality of water intended for human consumption set the maximum acceptable level for benzo(a)pyrene at 0,010 g/l, and for the sum of four specified PAH benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(ghi)perylene, indeno(1,2,3-cd)- pyrene at 0,100 g/l. ENISO17

35、993:2003blank ENISO17993:2003INTENRATIONAL TSANDADR IS:39971 O2002(E)I SO 2002 All irthgs ersedevr 1Water quality Determination of 15 polycyclic aromatic hydrocarbons (PAH) in water by HPLC with fluorescence detection after liquid-liquid extraction WARNING Some compounds being measured are presumed

36、to be carcinogenic. Acetonitrile and hexane are toxic. Persons using this International Standard should be familiar with normal laboratory practice. This International Standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the us

37、er to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies a method using high performance liquid chromatography (HPLC) with fluorescence detection after liquid-liquid extraction for the dete

38、rmination of 15 selected PAH (see Table 1) in drinking and ground water in mass concentrations greater than 0,005 g/l (for each single compound) and surface waters in mass concentrations above 0,01 g/l. This method is, with some modification, also suitable for the analysis of wastewater. This method

39、 may be applicable to other PAH, provided the method is validated for each case. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or

40、 revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the

41、normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 5667-2, Water quality Sampling Part 2: Guidance on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of samples ISO

42、 8466-1, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function 3 Principle The PAH present in the aqueous sample are extracted from the water sample with hexane. The extract is co

43、ncentrated by evaporation and the residue taken up in a solvent appropriate for HPLC analysis. If necessary, extracts of surface water or more contaminated water samples are cleaned by chromatography over silica prior to analysis. PAH are separated by HPLC on a suitable stationary phase using gradie

44、nt elution. Identification and quantification is performed by means of fluorescence detection with wavelength programming for both the excitation and the emission wavelength. NOTE If only a limited number of PAH are to be determined, separation can also be performed under isocratic conditions. ENISO

45、17993:2003IS:39971 O2002(E) 2 I SO 2002 All irthgs ersedevrTable 1 Polycyclic aromatic hydrocarbons determinable by this method Name Chemical formula Molar mass Percentage carbon CAS-number Structure Naphthalene C 10 H 8128,17 g/mol 93,75 % C 091-20-3 Acenaphthene C 12 H 10154,21 g/mol 93,05 % C 083

46、-32-9 Phenanthrene C 14 H 10178,23 g/mol 94,05 % C 085-01-8 Fluoranthene C 16 H 10202,26 g/mol 95,0 % C 206-44-0 Benzo(a)anthracene C 18 H 12228,29 g/mol 94,45 % C 056-55-3 Benzo(b)fluorantheneaC 20 H 12252,32 g/mol 95,2 % C 205-99-2 Benzo(a)pyreneaC 20 H 12252,32 g/mol 95,2 % C 050-32-8 Dibenzo(a,h

47、)anthracene C 22 H 14278,35 g/mol 94,7 % C 053-70-3 Fluorene C 13 H 10166,22 g/mol 93,59 % C 086-73-7 Anthracene C 14 H 10178,23 g/mol 94,05 % C 120-12-7 Pyrene C 16 H 10202,26 g/mol 95,0 % C 129-00-0 ENISO17993:2003IS:39971 O2002(E) I SO 2002 All irthgs ersedevr 3Table 1 (continued) Name Chemical f

48、ormula Molar mass Percentage carbon CAS-number Structure Chrysene C 18 H 12228,29 g/mol 94,45 % C 218-01-9 Benzo(k)fluorantheneaC 20 H 12252,32 g/mol 95,2 % C 207-08-9 Indeno(1,2,3-cd)pyreneaC 22 H 12276,34 g/mol 95,6 % C 193-39-5 Benzo(ghi)peryleneaC 22 H 12276,34 g/mol 95,6 % C 191-24-2 NOTE The 15 PAH selected fo