1、BRITISH STANDARD BS EN ISO 17495:2003 Water quality Determination of selected nitrophenols Method by solid-phase extraction and gas chromatography with mass spectrometric detection The European Standard EN ISO 17495:2003 has the status of a British Standard ICS 13.060.50 BS EN ISO 17495:2003 This Br
2、itish Standard was published under the authority of the Standards Policy and Strategy Committee on 17 March 2003 BSI 17 March 2003 ISBN 0 580 41434 5 National foreword This British Standard is the official English language version of EN ISO 17495:2003. It is identical with ISO 17495:2001. The UK par
3、ticipation in its preparation was entrusted by Technical Committee 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. Cross-ref
4、erences The British Standards which implement international or European 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 Briti
5、sh 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; present
6、 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 ins
7、ide 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 19, the Annex ZA page, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued
8、 since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO17495 March2003 ICS13.060.50 Englishversion WaterqualityDeterminationofselectednitrophenolsMethod bysolidphaseextractionandgaschromatographywithmass spectrometricdetection(ISO17495:2001) QualitdeleauDosagede
9、snitrophnolsslectionns Mthodeparextractionenphasesolideavecdtectionpar chromatographieenphasegazeuseetspectromtriede masse(ISO17495:2001) WasserbeschaffenheitBestimmungausgewhlter NitrophenoleVerfahrenmittelsFestphasenanreicherung undGaschromatographiemitmassenspektrometrischer Detektion(ISO17495:20
10、01) ThisEuropeanStandardwasapprovedbyCENon9January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standards
11、maybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official ve
12、rsions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,SlovakRepublic,Spain,Sweden,Switzerland and UnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPEN
13、DENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO17495:2003EForeword ThetextofISO17495:2001hasbeenpreparedbyTechnicalCommitteeISO/TC147“Water quality“of
14、theInternationalOrganizationforStandardization(ISO)andhasbeentakenoveras ENISO17495:2003byTechnicalCommitteeCEN/TC230“Wateranalysis“,thesecretariatof whichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbySepte
15、mber2003,andconflictingnational standardsshallbewithdrawnatthelatestbySeptember2003. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Hung
16、ary,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,SlovakRepublic,Spain,Sweden, SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextofISO17495:2001hasbeenapprovedbyCENasENISO17495:2003withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinAnnexZ
17、A(normative). ENISO17495:2003Reference number ISO 17495:2001(E) INTERNATIONAL STANDARD ISO 17495 First edition 2001-08-15 Water quality Determination of selected nitrophenols Method by solid-phase extraction and gas chromatography with mass spectrometric detection Qualit de leau Dosage des nitrophno
18、ls slectionns Mthode par extraction en phase solide avec dtection par chromatographie en phase gazeuse et spectromtrie de masse ENISO17495:2003ISO 59471:(1002)E DPF dlcsiremia ihTs PDF file mya ctnoain emdeddeb tyfepcaes. In acccnadroe with Aebods licnesign lopic,y this file may be pirntde ro ivwede
19、 tub slahl ton eb ideted lnuess teh tyfepacse which aer emdeddeb era licnesed to dna intslaled on teh computre freporming teh idetign. In wodlnidaogn this f,eli trapies accept tniereh teh sersnoptilibiy of ton nifrgnigni Asebod licsnegni ilopcy. ehT ISO tneClar Secteraairt accepts no lilibaity ni th
20、is .aera Aebod is a tedarmakr fo Aebod Stsyems Icntaropro.de teDails fo the sfotwera pcudorts sude to crtaee tihs PFD file can be fdnuo in the Glarene Info leratiev to the fil;e the Pc-FDaertion arapmteres were tpoimizde for pirtning. Evyre cera sah neeb taken to enseru taht teh file is suitlbae fro
21、 sue by ISO member idob.se In teh lnuikley etnev ttah a plborem leratign to it is f,dnuo lpsaee ifnrom teh tneClar Sceterairat at the sserdda givne lebwo. ii ENISO17495:2003 iii Contents Page Foreword.iv Introduction.v 1 Scope 1 2 Normative references 1 3 Principle2 4 Interferences 2 5 Reagents.3 6
22、Apparatus .5 7 Sampling.6 8 Procedure .6 9 Calibration 9 10 Calculation12 11 Expression of results 14 12 Test report 14 Annex A (informative) Examples of suitable capillary columns.15 Annex B (informative) Examples of sorbents suitable for solid-phase extraction of nitrophenols .16 Annex C (informat
23、ive) Precision data17 Annex D (informative) Example of typical spectra.18 Bibliography19 ENISO17495:2003iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is no
24、rmally carried out through ISO technical committees. Each member body interested in a subject 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
25、 the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the tech
26、nical committees 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 paten
27、t rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 17495 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. Annexes A to D of this International Standard are
28、for information only. ENISO17495:2003 v Introduction Several methods may be applied to determine nitrophenols in water. This International Standard describes a gas chromatographic/mass spectrometric determination after solid-phase extraction and derivatization with diazomethane. It should be investi
29、gated whether and to what extent particular problems will require the specification of additional marginal conditions. ENISO17495:2003INTENRATIONAL TSANDADR ISO 59471:(1002)E1 Water quality Determination of selected nitrophenols Method by solid-phase extraction and gas chromatography with mass spect
30、rometric detection WARNING Persons using this International Standard should be familar with normal laboratory practice. This International Standard does not purport to address all safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate health a
31、nd safety practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies a method for the determination of selected nitrophenols (see Table 1) in drinking, ground and surface water in mass concentrations 0,5 g/l 1) . Table 1 Nitrophenols to
32、which this method is applicable CAS No. CAS No. 2-Nitrophenol 88-75-5 2,4-Dinitrophenol 51-28-5 3-Nitrophenol 554-84-7 2,5-Dinitrophenol 329-71-5 4-Nitrophenol 100-02-7 2,6-Dinitrophenol 573-56-8 4-Methyl-2-nitrophenol 119-33-5 2,4-Dinitro-6-methylphenol 534-52-1 3-Methyl-4-nitrophenol 2581-34-2 2,6
33、-Dimethyl-4-nitrophenol 2423-71-4 5-Methyl-2-nitrophenol 700-38-9 2,4-Dichloro-6-nitrophenol 609-89-2 3-Methyl-2-nitrophenol 4920-77-8 2,6-Dichloro-4-nitrophenol 618-80-4 CAS Chemical Abstracts Service. 2 Normative references The following normative documents contain provisions which, through refere
34、nce in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or 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 applyi
35、ng the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part 1: Guid
36、ance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques. 1) See the results from the interlaboratory trial given in annex C. ENISO17495:20032 ISO 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation and handling o
37、f samples. ISO 8466-1:1990, Water quality Calibration and evaluation of analytical methods and estimation of performance characteristics Part 1: Statistical evaluation of the linear calibration function. 3P r i n c i p l e Solid-phase extraction of the nitrophenols is carried out from the acidified
38、sample, followed by solvent elution, derivatization with diazomethane and determination by gas chromatography and mass spectrometry. It is absolutely essential that the tests described in this International Standard be carried out by suitably qualified staff. 4 Interferences 4.1 Interferences during
39、 enrichment In order to avoid losses, analyse the sample as soon as possible after sampling. If storage is unavoidable, store at 4 C until sample pretreatment. The commercially available adsorbance materials are often of varying quality. Considerable batch-to-batch variations in quality and selectiv
40、ity of this material are possible. The recovery may vary with the concentration, and shall therefore regularly be checked at different concentrations. Calibration and analysis shall be performed with material from one and the same batch only. Suspended matter in the water sample (such as iron hydrox
41、ide, calcium carbonate) occurring on sampling, storage and sample preparation, as well as increased concentrations of microorganisms, may clog the packing. In this case the water sample may be filtered through a glass-fibre filter prior to the enrichment. A filtration step shall be mentioned in the
42、test report. Possible losses due to heating and volume reduction of the eluate may be reduced by the addition of a keeper (for example iso-octane) 4.2 Interferences in the gas chromatograph The operating conditions shall be set in accordance with the manufacturers instructions. These settings shall
43、be checked at regular intervals. General interferences, caused by the injection system or insufficient separation, can be eliminated with the help of special laboratory experience and the instrument manuals. Excess diazomethane may cause instrument failure or damage, due to its high reactivity. Ther
44、efore care should be taken to remove excess diazomethane as far as possible by reducing the volume of the solution. The use of alcohol as solvent should be avoided because any alcohol may destroy the deactivation layer (poly- siloxane) of the glass liner, leading to column load and an overload of th
45、e detector. In this case, the quantification of the analyte and the reproducibility of the result are no longer possible. The stability of the analyte system should be checked (for example by application of a measuring standard). ENISO17495:2003 3 5 Reagents Reagents “for residual analysis” shall be
46、 used. Impurities of the reagents and of the water contributing to the blank shall be negligibly low. The blank shall be checked before use, especially prior to the use of a new batch. 5.1 Water, double-distilled or of comparable purity. 5.2 Operating gases for the gas chromatograph/mass spectromete
47、r, in accordance with the manufacturers instructions. The operating gases shall be of high purity. 5.3 Nitrogen, high purity, minimum 99,996 % (volume fraction), for drying and eventually for concentration by evaporation. 5.4 Hydrochloric acid, c(HCl) 2mo l /l . 5.5 Diethyl ether,C 4 H 10 O, stabili
48、zed only with ethanol. 5.6 Potassium hydroxide, KOH, aqueous solution, 0,6. 5.7 Ethanol,C 2 H 5 OH. 5.8 N-methyl-N-nitroso-4-toluenesulfonamide, (Diazald) C 8 H 10 N 2 O 3 S. 5.9 Acetic acid,C H 3 COOH , aqueous solution, 10 % volume fraction (used to destroy diazomethane). 5.10 Solvents 5.10.1 Acetone, C 3 H 6 O. 5.10.2 Methanol,CH
