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1、BS EN 15309:2007 ICS 13.030.10; 13.080.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BRITISH STANDARD Characterization of waste and soil Determination of elemental composition by X-ray fluorescence Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontroll
2、ed Copy, (c) BSI This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 May 2009 BSI 2009 ISBN 978 0 580 55631 9 Amendments/corrigenda issued since publication DateComments BS EN 15309:2007 National foreword This British Standard is the UK implem
3、entation of EN 15309:2007. The UK participation in its preparation was entrusted to Technical Committee B/508/3, Characterization of waste. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessar
4、y provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EUROPEAN STANDARD NORME EUROPEN
5、NE EUROPISCHE NORM EN 15309 May 2007 ICS 13.030.10; 13.080.10 English Version Characterization of waste and soil - Determination of elemental composition by X-ray fluorescence Caractrisation des dchets et du sol - Dtermination de la composition lmentaire par fluorescence X Charakterisierung von Abfl
6、len und Bden - Bestimmung der elementaren Zusammensetzung durch Rntgenfluoreszenz-Analyse This 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 European Standard the status
7、 of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards 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 v
8、ersion in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic,
9、 Denmark, Estonia, Finland, France, 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 STANDARDIZATION COMIT EUROPEN DE NORM
10、ALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15309:2007: E Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncon
11、trolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 2 Contents Page Foreword3 Introduction.4 1 Scope 5 2 Normative references5 3 Terms and definitions .5 4 Safety remarks.7 5 Principle7 6 Apparatus .7 7 Reagents.8 8 Interferences and sources of error8 9 Sample preparation .9 9.1 General9 9.2 Dr
12、ying and determination of dry mass9 9.3 Preparation of pressed pellet.9 9.4 Preparation of fused beads 10 10 Procedure .10 10.1 Analytical measurement conditions10 10.2 Calibration11 10.3 Analysis of the samples17 11 Quality control18 11.1 Drift correction procedure 18 11.2 Blank test18 11.3 Referen
13、ce materials.18 12 Calculation of the result18 13 Test report19 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
14、 analytical lines, crystals and operating conditions.29 Annex D (informative) List of reference materials applicable for XRF-analysis.31 Annex E (informative) Validation.32 Bibliography40 Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 1
15、5309:2007 (E) 3 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 s
16、tatus of a national 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
17、 the following countries 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, Slov
18、akia, Slovenia, Spain, Sweden, Switzerland and United Kingdom Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 4 Introduction X-ray fluorescence spectrometry is a fast and reliable method for the quantitative analysis of th
19、e total content 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 hav
20、e to be considered, 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 suitabl
21、e reference 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 soi
22、l-like material 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 bas
23、ed on matrix-independent calibration curves, previously set up by the manufacturer. Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 5 1 Scope This European Standard specifies the procedure for a quantitative determination
24、of 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
25、 applicable 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
26、 the 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 amendment
27、s) 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
28、laboratories (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 d
29、efinitions 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 analyti
30、cal 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 c
31、harged particle, such as an atomic nucleus Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 6 3.5 Compton-line spectral line due to incoherent scattering (Compton-effect) occurring when the incident X-ray photon strike an a
32、tom 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 radia
33、tion 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 constant d
34、escribing 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 polarised e
35、xcitation 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 in th
36、e 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 3.16
37、quality control sample stable sample with known contents, e.g. certified reference material (CRM) used to monitor instrument and calibration performance Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 7 3.17 X-ray fluoresc
38、ence 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 to be deter
39、mined. 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 produced by
40、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 fluorescence
41、 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 Principle After
42、 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 to previously
43、 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 relevant prepa
44、ration 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 fluorescence (
45、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 crystal or a synth
46、etic 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 shape (like sou
47、rce filters, secondary targets, polarising targets, collimators, focussing optics etc.). Licensed CopyChinese University of Hong Kong, 13/06/2009 05:34, Uncontrolled Copy, (c) BSI BS EN 15309:2007 EN 15309:2007 (E) 8 The detector unit is different for WDXRF and for EDXRF spectrometers. WDXRF spectro
48、meters 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, which are a measure of
49、 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 Mill, preferable