1、BRITISH STANDARD BS EN ISO 15586:2003 BS 6068-2.84:2003 Incorporating Corrigendum No. 1 Water quality Determination of trace elements using atomic absorption spectrometry with graphite furnace The European Standard EN ISO 15586:2003 has the status of a British Standard ICS 13.060.50 BS EN ISO15586:2
2、003 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 October 2003 BSI 23 December 2003 ISBN 0 580 42808 7 National foreword This British Standard is the official English language version of EN ISO 15586:2003. It is identical with ISO 15586:
3、2003. The UK participation 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 secr
4、etary. Cross-references 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 Catal
5、ogue or of British 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 t
6、he text; present 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 fro
7、nt cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the 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 in this document indicates when the document was last issued. Amendments i
8、ssued since publication Amd. No. Date Comments 14923 Corrigendum No. 1 23 December 2003 Correction to EN ISO foreword and incorporation of Annex ZA pageEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO15586 October2003 ICS13.060.50 Englishversion WaterqualityDeterminationoftraceelementsusingatomi
9、c absorptionspectrometrywithgraphitefurnace(ISO15586:2003) QualitdeleauDosagedesoligolmentspar spectromtriedabsorptionatomiqueenfourgraphite(ISO 15586:2003) WasserbeschaffenheitBestimmungvon SpurenelementenmittelsAtomabsorptionsspektrometrie mitdemGraphitrohrVerfahren(ISO15586:2003) ThisEuropeanStan
10、dardwasapprovedbyCENon1September2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapp
11、licationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembers
12、arethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISC
13、HESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO15586:2003ECORRECTED20031203 Foreword Thisdocument(ENISO15586:2003)hasbeenpreparedbyTechnicalCommitteeISO/TC147 “Waterquality“i
14、ncollaborationwithTechnicalCommitteeCEN/TC230“Wateranalysis“,the secretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyApril2004,andconflictingnational standardsshallbewithdrawnatthelatestbyApril2
15、004. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy, Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia
16、,Spain,Sweden,Switzerlandand theUnitedKingdom. Endorsementnotice ThetextofISO15586:2003hasbeenapprovedbyCENasENISO15586:2003withoutany modifications. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO15586:2003 Reference number ISO 15586:2003(E)INTERNATIONAL STANDAR
17、D ISO 15586 First edition 2003-10-01 Water quality Determination of trace elements using atomic absorption spectrometry with graphite furnace Qualit de leau Dosage des lments traces par spectromtrie dabsorption atomique en four graphite ENISO15586:2003IS:68551 O3002(E) DPlcsid Fremia ihTs PDF file m
18、ya ctnoian emdebt dedyfepcaes. In ccacnadrow eitA hebods licnesilop gnic,y tihs file mirp eb yatnde iv roweb detu slahl ton ide ebtlnu deess teh typfecaes wihce era hml era deddebicsnede ti dna onstlalde t noeh comuptfrep reromign tide ehtin.g In wodlnidaot gnihs fil,e trapise atpecc tiereht nser eh
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21、 sswrehise specified, on trap fo this lbupictaion maeb y cudorperro de tuilizi den yna form ro na ybm ynae,s lecetrinoc ro mceinahcla, incliduntohp gcoiypodna gn micrfoilm, wittuoh repmissii now nritign from ietI rehSa Ot tsserdda eh ebolw or ISOs memreb i ydobn the cnuotfo yr ttseuqer ehe.r ISO cir
22、ypothg fofice saCe tsopale 65 eneG 1121-HC 02 av leT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mial coirypthgis.o gro We bwww.is.o groii ENISO15586:2003 iiiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Principle . 2 4 Interferences 3 5 Reagents 3 6 Apparatus. 5 7 Sampling and pr
23、e-treatment 6 8 Chemical modification 8 9 Determination 10 10 Calibration 10 11 Calculation. 11 12 Precision 12 13 Test report 17 Annex A (informative) Preparation of stock solutions, 1 000 mg/l 18 Annex B (normative) Digestion of sediment samples 20 Annex C (informative) Examples of instrumental pa
24、rameter settings 22 Bibliography . 23 ENISO15586:2003iv 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 normally carried out through ISO technical committees
25、. 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 the work. ISO collaborates closely with the Intern
26、ational 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 2. The main task of technical committees is to prepare International Standards. Draft International Sta
27、ndards adopted by the technical 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 document may be the subj
28、ect of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 15586 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical, chemical and biochemical methods. ENISO15586:2003INTENRATIONAL TSANDADR IS:68551 O3002(E)1Water
29、 quality Determination of trace elements using atomic absorption spectrometry with graphite furnace WARNING 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, associ
30、ated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard includes principles and procedures for the determination of trace levels of: Ag, Al, As,
31、Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, Tl, V, and Zn in surface water, ground water, drinking water, wastewater and sediments, using atomic absorption spectrometry with electrothermal atomization in a graphite furnace. The method is applicable to the determination of low concentrations of eleme
32、nts. The detection limit of the method for each element depends on the sample matrix as well as of the instrument, the type of atomizer and the use of chemical modifiers. For water samples with a simple matrix (i.e. low concentration of dissolved solids and particles), the method detection limits wi
33、ll be close to instrument detection limits. The minimum acceptable detection limit values for a 20-l sample volume are given in Table 1. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited appl
34、ies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 5667-1, Water quality Sampling Part 1: Guidance on the design of sampling programmes ISO 5667-2, Water
35、quality Sampling Part 2: Guidance on sampling techniques ISO 5667-3, Water quality Sampling Part 3: Guidance on the preservation and handling of water samples ISO 5667-4, Water quality Sampling Part 4: Guidance on sampling from lakes, natural and man-made ISO 5667-5, Water quality Sampling Part 5: G
36、uidance on sampling of drinking water and water used for food and beverage processing ISO 5667-6, Water quality Sampling Part 6: Guidance on sampling of rivers and streams ISO 5667-10, Water quality Sampling Part 10: Guidance on sampling of waste waters ISO 5667-11, Water quality Sampling Part 11: G
37、uidance on sampling of groundwaters ISO 5667-15, Water quality Sampling Part 15: Guidance on preservation and handling of sludge and sediment samples ISO 15587-1, Water quality Digestion for the determination of elements in water Part 1: Aqua regia digestion ENISO15586:20032 ISO 15587-2, Water quali
38、ty Digestion for the determination of elements in water Part 2: Nitric acid digestion Table 1 Approximate characteristic masses, instrument detection limits and optimum working ranges for water samples using a 20 l sample volume Characteristic mass m 0 aDetection limit bOptimum working range cElemen
39、t pg g/l g/l Ag 1,5 0,2 1 to 10 Al 10 1 6 to 60 As 15 1 10 to 100 Cd 0,7 0,1 0,4 to 4 Co 10 1 6 to 60 Cr 3 0,5 2 to 20 Cu 5 d0,5 3 to 30 Fe 5 1 3 to 30 Mn 2,5 0,5 1,5 to 15 Mo 10 1 6 to 60 Ni 13 1 7 to 70 Pb 15 1 10 to 100 Sb 20 1 10 to 100 Se 25 2 15 to 150 Tl 10 d1 6 to 60 V 35 2 20 to 200 Zn 0,8
40、0,5 0,5 to 5 a The characteristic mass (m 0 ) of an element is the mass in picograms, corresponding to a signal of 0,004 4 s, using the integrated absorbance (peak area) for evaluation. b The detection limits are calculated as three times (3 ) the standard deviation of repeated measurements of a bla
41、nk solution. c The optimum working range is defined as the concentration range that corresponds to integrated absorbance readings between 0,05 s and 0,5 s. d If Zeeman effect background correction is used, the m 0 -value will be higher.3 Principle Water samples are preserved by acid treatment, filte
42、red and preserved by addition of acid, or digested. Sediment samples are digested. A small sub-sample of sample solution is injected into a graphite furnace of an atomic absorption spectrometer. The furnace is electrically heated. By increasing the temperature stepwise, the sample is dried, pyrolize
43、d and atomized. Atomic absorption spectrometry is based on the ability of free atoms to absorb light. A light source emits light specific for a certain element (or elements). When the light beam passes through the atom cloud in the heated graphite furnace, the light is selectively absorbed by atoms
44、of the chosen element(s). The decrease in light intensity is measured with a detector at a specific wavelength. The concentration of an element in a sample is determined by comparing the absorbance of the sample with the absorbance of calibration solutions. If necessary, interferences may be overcom
45、e by adding a matrix modifier to the samples before analysis, or by performing the calibration with the standard addition technique. The results are given as the mass of analyte (micrograms, g, or milligrams, mg) per litre of water, or per kilogram of dried material in sediments. ENISO15586:2003 34
46、Interferences Some sample solutions, especially wastewaters and digestions of sediments, may contain large amounts of substances that may affect the results. High concentrations of chloride may cause low results, because the volatility of many elements is increased and analyte loss may occur during
47、the pyrolysis step. Matrix effects may be overcome, partially or completely, by optimization of the temperature programme, the use of pyrolytically-coated tubes and platforms, the use of chemical modifiers, the standard addition technique and the use of background correction. 5 Reagents For pre-trea
48、tment of samples and preparation of solutions, use only chemicals and solutions of highest possible purity unless stated otherwise. 5.1 Water, Grade 1 as specified in ISO 3696:1987 (u 0,01 mS/m), or better. Use this water to prepare all solutions. Check the quality of the water before use. 5.2 Nitric acid, concentrated, c(HNO 3 ) = 14,4 mol/l, 1,4
