1、BS EN 15309:2007ICS 13.030.10; 13.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCharacterizationof waste and soil Determination ofelemental compositionby X-ray fluorescenceLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrol
2、led Copy, (c) BSIThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 May 2009 BSI 2009ISBN 978 0 580 55631 9Amendments/corrigenda issued since publicationDate CommentsBS EN 15309:2007National forewordThis British Standard is the UK implementation
3、of EN 15309:2007.The UK participation in its preparation was entrusted to TechnicalCommittee B/508/3, Characterization of waste.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof
4、 a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE
5、 NORMEN 15309May 2007ICS 13.030.10; 13.080.10English VersionCharacterization of waste and soil - Determination of elementalcomposition by X-ray fluorescenceCaractrisation des dchets et du sol - Dtermination de lacomposition lmentaire par fluorescence XCharakterisierung von Abfllen und Bden - Bestimm
6、ungder elementaren Zusammensetzung durchRntgenfluoreszenz-AnalyseThis European Standard was approved by CEN on 22 March 2007.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 wit
7、hout any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language
8、made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,Franc
9、e, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORM
10、UNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15309:2007: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 1530
11、9:2007EN 15309:2007 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Safety remarks .7 5 Principle7 6 Apparatus .7 7 Reagents.8 8 Interferences and sources of error 8 9 Sample preparation .9 9.1 General9 9.2 Drying and determination of dry
12、 mass9 9.3 Preparation of pressed pellet .9 9.4 Preparation of fused beads 10 10 Procedure .10 10.1 Analytical measurement conditions 10 10.2 Calibration 11 10.3 Analysis of the samples17 11 Quality control18 11.1 Drift correction procedure 18 11.2 Blank test18 11.3 Reference materials.18 12 Calcula
13、tion of the result18 13 Test report 19 Annex A (informative) Semi-quantitative screening analysis of waste, sludge and soil samples .20 Annex B (informative) Examples for operational steps of the sample preparation for soil and waste samples23 Annex C (informative) Suggested analytical lines, crysta
14、ls and operating conditions.29 Annex D (informative) List of reference materials applicable for XRF-analysis.31 Annex E (informative) Validation .32 Bibliography 40 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 3
15、Foreword This document (EN 15309:2007) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste“, the secretariat of which is held by NEN. This document has been prepared in coordination with ISO/TC 190 “Soil quality”. This European Standard shall be given the status of a natio
16、nal standard, either by publication of an identical text or by endorsement, at the latest by November 2007, and conflicting national standards shall be withdrawn at the latest by November 2007. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following c
17、ountries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia,
18、Spain, Sweden, Switzerland and United Kingdom Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 4 Introduction X-ray fluorescence spectrometry is a fast and reliable method for the quantitative analysis of the total c
19、ontent of certain elements within different matrices. The quality of the results obtained depends very closely on the type of instrument used, e.g. bench top or high performance, energy dispersive or wavelength dispersive instruments. When selecting a specific instrument several factors have to be c
20、onsidered, such as the matrices to be analyzed, elements to be determined, detection limits required and the measuring time. The quality of the results depends on the element to be determined and on the surrounding matrix. Due to the wide range of matrix compositions and the lack of suitable referen
21、ce materials in the case of inhomogeneous matrices like waste, it is generally difficult to set up a calibration with matrix-matched reference materials. Therefore this standard describes two different procedures: a quantitative analytical procedure for homogeneous solid waste, soil and soil-like ma
22、terial in the normative part. The calibration is based on matrix-matched standards; an XRF screening method for solid and liquid material as waste, sludge and soil in the informative Annex A which provides a total element characterisation at a semi-quantitative level. The calibration is based on mat
23、rix-independent calibration curves, previously set up by the manufacturer. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 5 1 Scope This European Standard specifies the procedure for a quantitative determination of
24、 major and trace element concentrations in homogeneous solid waste, soil and soil-like material by energy dispersive X-ray fluorescence (EDXRF) spectrometry or wavelength dispersive X-ray fluorescence (WDXRF) spectrometry using a calibration with matrix-matched standards. This European Standard is a
25、pplicable for the following elements: Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Y, Zr, Nb, Mo, Ag, Cd, Sn, Sb, Te, I, Cs, Ba, Ta, W, Hg, Tl, Pb, Bi, Th and U. Concentration levels between approximately 0,000 1 % and 100 % can be determined depending on t
26、he element and the instrument used. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments)
27、 applies. EN 14346, Characterisation of waste Calculation of dry matter by determination of dry residue or water content EN 15002, Characterisation of waste Preparation of test portions from the laboratory sample EN ISO/IEC 17025, General requirements for the competence of testing and calibration la
28、boratories (ISO/IEC 17025:1999) ISO 11464, Soil quality Pretreatment of samples for physico-chemical analysis ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method 3 Terms and definitions For the purpose of this document, the following terms and def
29、initions apply. NOTE See 13 and 10 for non specified terms. 3.1 absorption edge jump of the mass absorption coefficient at a specific wavelength or energy 3.2 absorption of X-rays loss of intensity of X-rays by an isotropic and homogenous material as described by the Bouger-Lambert law 3.3 analytica
30、l line specific characteristic X-ray spectral line of the atom or ion of the analyte used for determination of the analyte content 3.4 Bremsstrahlung; continuous radiation electromagnetic radiation produced by the acceleration of a charged particle, such as an electron, when deflected by another cha
31、rged particle, such as an atomic nucleus Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 6 3.5 Compton-line spectral line due to incoherent scattering (Compton-effect) occurring when the incident X-ray photon strike
32、 an atom without promoting fluorescence NOTE Energy is lost in the collision and therefore the resulting scattered X-ray photon is of lower energy than the incident X-ray photon. 3.6 drift correction monitors physically stable samples used to correct for instrumental drift 3.7 emitted sample X-rays
33、radiation emitted by sample consisting of X-ray fluorescence radiation and scattered primary X-rays 3.8 fused bead analyte sample prepared by dissolution in a flux 3.9 liquid sample analyte sample submitted as a solution for direct measurement in the sample cup 3.10 mass absorption coefficient const
34、ant describing the fractional decrease in the intensity of a beam of X-radiation as it passes through an absorbing medium, expressed in units of cm2/g. The mass absorption coefficient is a function of the wavelength of the absorbed radiation and the atomic number of the absorbing element 3.11 polari
35、sed excitation X-ray spectrometer energy dispersive X-ray spectrometer where the excitation is performed by polarised radiation and the emitted X-ray fluorescence radiation is detected along the direction of polarisation 3.12 powder sample analyte sample submitted as a powder for direct measurement
36、in the sample cup 3.13 precision closeness of agreement of results obtained by applying the method several times under prescribed conditions ISO 5725-2:1994 3.14 pressed pellet analyte sample prepared by pressing milled material into a disk 3.15 primary X-rays X-rays by which the sample is radiated
37、3.16 quality control sample stable sample with known contents, e.g. certified reference material (CRM) used to monitor instrument and calibration performance Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 7 3.17 X-
38、ray fluorescence radiation emission of characteristic X-rays from a sample that has been bombarded by high-energy X-rays or gamma rays 4 Safety remarks Anyone dealing with waste and sludge analysis has to be aware of the typical risks that this kind of material presents irrespective of the parameter
39、 to be determined. Waste and sludge samples may contain hazardous e.g. toxic, reactive, flammable, infectious substances, which could potentially undergo biological and/or chemical reaction. Consequently it is recommended that these samples should be handled with special care. The gases that may be
40、produced by microbiological or chemical activity are potentially flammable and will pressurise sealed bottles. Bursting bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. The X-ray
41、fluorescence spectrometer shall comply with European and national regulations relevant to radiation protection. The person responsible for managing or supervising the operation of X-ray equipment shall provide evidence of his knowledge of radiation protection according to national regulations. 5 Pri
42、nciple After a suitable preparation, if necessary, the sample is introduced into a XRF-spectrometer and excited by primary X-rays. The intensities of the secondary fluorescent energy lines specific for each element are measured and the elemental composition of the sample is determined by reference t
43、o previously established calibration graphs or equations and applying corrections for inter-element effects. The calibration equations and inter-element corrections are established using pure reagents and/or series of internal or reference materials providing they meet all the requirements of the re
44、levant preparation technique. 6 Apparatus 6.1 X-ray fluorescence spectrometer The X-ray fluorescence spectrometer shall be able to analyse the elements according to the scope of this European Standard. The following types of X-ray fluorescence spectrometers are applicable: energy dispersive X-ray fl
45、uorescence (EDXRF) spectrometer that achieves the dispersion of the emitted X-ray fluorescence radiation by an energy dispersive detector; wavelength dispersive X-ray fluorescence (WDXRF) spectrometer that achieves the dispersion of the emitted X-ray fluorescence radiation by diffraction by a crysta
46、l or a synthetic multilayer. The spectrometer consists of a number of components: primary X-ray source, an X-ray tube with a high voltage generator; a sample holder; detector unit including electronic equipment; source modifiers to modify the shape or intensity of the source spectrum or the beam sha
47、pe (like source filters, secondary targets, polarising targets, collimators, focussing optics etc.). Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 01/09/2009 07:39, Uncontrolled Copy, (c) BSIBS EN 15309:2007EN 15309:2007 (E) 8 The detector unit is different for WDXRF and for EDXRF spectrome
48、ters. WDXRF spectrometers take advantage of the dispersion of the emitted radiation by scattering by a crystal or a synthetic multilayer. The detector does not need to be capable of energy discrimination. EDXRF spectrometers use an energy dispersive detector. Pulses of current from the detector, whi
49、ch are a measure of the energy of the incoming X-rays, are segregated into channels according to energy using a Multi-Channel Analyser (MCA). NOTE 1 The use of a high-energy X-ray tube increases the potential for losses of volatile analytes from samples by heating in the spectrometer during analysis. NOTE 2 The new generation of EDXRF spectrometers takes advantage of the polarising target theory resulting in a significant decrease of the background scattering, and therefore lower limits of detection can be achieved (comparable to WDXRF). 6.2 Mi
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