DIN EN 16424-2015 Characterization of waste - Screening methods for the element composition by portable X-ray fluorescence instruments German version EN 16424 2014《废弃物的特性描述 使用便携式X射.pdf

1、March 2015 Translation by DIN-Sprachendienst.English price group 16No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、13.030.01!%A*K“2300740www.din.deDDIN EN 16424Characterization of waste Screening methods for the element composition by portable X-rayfluorescence instruments;English version EN 16424:2014,English translation of DIN EN 16424:2015-03Charakterisierung von Abfllen Screening-Verfahren zur Bestimmung der

3、 elementaren Zusammensetzung mit tragbarenRntgenfluoreszenzspektrometern;Englische Fassung EN 16424:2014,Englische bersetzung von DIN EN 16424:2015-03Caractrisation des dchets Mthode de dpistage pour la dtermination de la composition lmentaire au moyendanalyseurs portables de fluorescence X;Version

4、anglaise EN 16424:2014,Traduction anglaise de DIN EN 16424:2015-03SupersedesDIN EN 16424:2015-01www.beuth.deDocument comprises 35 pagesIn case of doubt, the German-language original shall be considered authoritative.02.15DIN EN 16424:2015-03 2 A comma is used as the decimal marker. National foreword

5、 This document (EN 16424:2014) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee

6、NA 119-01-02-02 UA Chemische und physikalische Verfahren. The European Standards referred to in this document have been published as DIN EN or DIN EN ISO Standards with the same number. The DIN Standard corresponding to the European Standard referred to in this document is as follows: CEN/TR 16176:2

7、011 DIN CEN/TR 16176 (DIN SPEC 19776):2012-03 Amendments This standard differs from DIN EN 16424:2015-01 as follows: a) in Clause 8 “Screening strategy”, Step 1, reference to European and national legislation has been added; b) in Annex D “Validation”, some sample designations have been corrected; c

8、) in Tables D.1, D.3 and D.5, a value has been corrected; d) in the key of Tables D.1, D.2, D.9 and D.10, reference to the limit value has been deleted; e) missing keys in Tables D.5 and D.6 have been supplemented; f) in the key of Tables D.3, D.4, D.7 and D.8, the limit value designation has been c

9、orrected. National Annex NA (informative) Bibliography DIN CEN/TR 16176 (DIN SPEC 19776):2012-03, Characterization of waste Screening methods for elemental composition by X-ray fluorescence spectrometry for on-site verification EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16424 October 2014

10、ICS 13.030.01 English Version Characterization of waste - Screening methods for the element composition by portable X-ray fluorescence instruments Caractrisation des dchets - Mthode de dpistage pour la dtermination de la composition lmentaire au moyen danalyseurs portables de fluorescence X Charakte

11、risierung von Abfllen - Screening-Verfahren zur Bestimmung der elementaren Zusammensetzung mit tragbaren Rntgenfluoreszenzspektrometern This European Standard was approved by CEN on 16 August 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditio

12、ns for giving this European Standard the status 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-CENELEC Management Centre or to any CEN member. This European Standard exists in

13、 three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standard

14、s bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Sloven

15、ia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved w

16、orldwide for CEN national Members. Ref. No. EN 16424:2014 EEN 16424:2014 (E) 2 Contents Page Foreword 4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle 5 5 Safety remarks .6 6 Apparatus and equipment 6 6.1 X-ray fluorescence spectrometer .6 6.2 Direct measurement using a ha

17、nd-held instrumentation in direct contact with the sample .7 6.3 Hand-held instrumentation mounted on a stand using sample cups filled with the sample 7 6.4 Portable bench top XRF instrument 7 6.5 Spoon, stamp and/or hammer 7 6.6 Mortar and pestle .7 6.7 Thin-film support .7 6.8 Sample cups .7 7 Cal

18、ibration 7 7.1 General 7 7.2 Interferences 8 7.3 Calibration procedure .8 7.4 Validation of the calibration 9 8 Screening strategy 10 9 Sample preparation 12 9.1 General . 12 9.2 Sample preparation for direct measurement . 12 9.3 Sample preparation for filling cups 12 9.4 Sample preparation for hete

19、rogeneous samples 12 10 Analysis . 12 10.1 General . 12 10.2 Direct in situ measurement (hand-held method) . 12 10.3 Measurement by using a mounted hand-held XRF instrument or a small portable closed XRF instrument . 13 11 Calculation of the result . 13 12 Assessment of the XRF screening measurement

20、 . 13 12.1 General . 13 12.2 Identification of the presence or absence of the elements under investigation 13 12.3 Indication of the concentration range of the elements under investigation 14 13 Quality control . 14 13.1 Drift correction procedure . 14 13.2 Blank test . 14 13.3 Reference materials 1

21、4 14 Test report . 15 Annex A (informative) Examples of instrumentation 16 Annex B (informative) List of analytical lines and spectral line overlaps 19 DIN EN 16424:2015-03 EN 16424:2014 (E) 3 Annex C (informative) Evaluation of the acceptance criteria . 20 C.1 Uncertainty . 20 C.2 Test of the absen

22、ce of an element . 20 C.3 Test of the documented concentration of an element . 20 C.4 Estimation of uncertainty . 21 Annex D (informative) Validation . 22 Bibliography 33 DIN EN 16424:2015-03 EN 16424:2014 (E) 4 Foreword This document (EN 16424:2014) has been prepared by Technical Committee CEN/TC 2

23、92 “Characterization of waste”, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by April 2015, and conflicting national standards shall be withdrawn at the la

24、test by April 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. X-ray fluorescence spectrometry (XRF) is a fast and reliable metho

25、d for the determination of the total content of certain elements within different matrices. Quantitative analysis using XRF is described in EN 15309 2. For screening purposes, portable instruments are often used, especially when only the absence or presence of elements is under investigation or qual

26、itative results with an indication of the concentration level are requested. This standard is applicable for on-site verification at landfills (see CEN/TR 16130 4) and it is an exemplification of EN 16123 3. According to the CEN-CENELEC Internal Regulations, the national standards organizations of t

27、he following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether

28、lands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16424:2015-03 EN 16424:2014 (E) 5 1 Scope This European Standard is dedicated to field portable X-ray fluorescence (XRF) equipment (hand-held or portable bench top) and spe

29、cifies a screening method for the determination of the elemental composition of waste materials for on-site verification. Portable XRF spectrometers are used for a rapid and exploratory analysis of paste-like or solid materials. The absence or presence of specific elements is displayed qualitatively

30、 with an indication of the concentration level. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition

31、 of the referenced document (including any amendments) applies. EN 15002, Characterization of waste Preparation of test portions from the laboratory sample 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 field portable XRF spectrometer XRF sp

32、ectrometer for analyzing samples in the field, namely hand-held or portable bench top XRF spectrometers 3.2 hand-held XRF spectrometer XRF spectrometer which can be used for in-situ analysis by direct probing or mounted on a stand 3.3 on-site verification third level of inspection according to the L

33、andfill Directive and the Landfill Decision to ensure that the waste accepted at a landfill is the same as described in the accompanying documents and that it is in accordance with the basic characterization and/or compliance testing 3.4 portable bench top spectrometer compact bench top XRF spectrom

34、eter which can easily be carried into the field 3.5 screening application of any analytical method for exploratory analysis 4 Principle The sample can be measured directly or after a suitable sample preparation. In principle two different methods are used for probing the sample, either a pistol-like

35、 instrument is placed directly on the sample or a sufficient test portion is taken and put into a sample cup for measurement with the XRF instrument. The presence of a specific element is verified if a significant intensity for that element is measured. The intensities of the lines can be evaluated

36、to indicate the concentration range. DIN EN 16424:2015-03 EN 16424:2014 (E) 6 5 Safety remarks The X-ray fluorescence spectrometers on the market are generally fully protected apparatus which are subjected to specific official approval and acceptance conditions. This means that the user is not expos

37、ed to radiation when operating the apparatus correctly. Nevertheless while measuring in the field, scattering radiation can be produced when probing directly on the sample. Providing a protective radiation shield around the sample when measuring avoids these risks. The person responsible for managin

38、g or supervising the operation of X-ray equipment shall provide evidence of his knowledge of radiation protection according to national regulations. Proper safety precautions shall be considered when conducting field XRF measurements. The operator should always be aware that X-rays are produced duri

39、ng measurements. The operator should never point the open source at anyone and be aware that X-rays can penetrate through light atomic mass matrices. Proper training regarding handling of XRF instruments is an obligation. Take care when handling samples that may contain sharps or are of a dusty natu

40、re. Handling of samples should be performed with gloves and in the case of dusty materials with respiratory mask and gloves. Take special precautions with samples from potentially hazardous waste. Avoid any contact with the skin and/or inhaling of dust. 6 Apparatus and equipment 6.1 X-ray fluorescen

41、ce spectrometer The X-ray fluorescence spectrometer shall comply with European and national regulations relevant to radiation protection. The X-ray fluorescence spectrometer shall be able to analyse the relevant elements. The following types of X-ray fluorescence spectrometers are applicable: energy

42、 dispersive X-ray fluorescence spectrometer (EDXRF) which gains the dispersion of the emitted X-ray fluorescence radiation by an energy dispersive detector; wavelength dispersive X-ray fluorescence spectrometer (WDXRF) which gains the dispersion of the emitted X-ray fluorescence radiation by diffrac

43、tion by a crystal. For screening analysis generally EDXRF instruments are applied. Portable spectrometers comprise mainly the following components: a primary X-ray source, a miniaturised X-ray tube with a low voltage generator; a detector unit including electronic equipment; a power supply including

44、 rechargeable batteries; a radiation shield according to safety regulations; optional source modifiers to modify the shape or intensity of the source spectrum or the beam shape e.g. primary source filters. Portable spectrometers are mostly hand-held instruments which may be mounted on a stand. Alter

45、natively small bench top systems are available which are equipped with a sample holder. In general, the weight of portable instruments should be below 10 kg and the size should be less than 500 mm wide, 500 mm deep and 200 mm high. DIN EN 16424:2015-03 EN 16424:2014 (E) 7 The detector unit is differ

46、ent for wavelength dispersive (WDXRF) and for energy dispersive (EDXRF) spectrometers. WDXRF spectrometers take advantage of the dispersion of the emitted radiation by scattering by a crystal. EDXRF spectrometers are using an energy dispersive detector. The detector current pulses, a measure for the

47、 energy of the incoming X-rays, are segregated into channels according to energy using a multi-channel analyser (MCA). 6.2 Direct measurement using a hand-held instrumentation in direct contact with the sample When using a pistol-like instrument, direct probing of the sample is possible (see Figure

48、A.1 and Figure A.2). To avoid uncertainties due to different measurement geometry such as distance to sample, angle between sample and incident beam, the measuring window of the instrument should be in close contact to the sample. 6.3 Hand-held instrumentation mounted on a stand using sample cups fi

49、lled with the sample For practical reasons or to improve the accuracy of the results due to different measurement geometries, hand-held instruments may be mounted in a stand to operate with a well-defined geometry. Sample cups containing the material under investigation are placed into the instrument at a fixed position (see Figure A.3 and Figure A.4). 6.4 Portable bench top XRF instrument Portable bench top XRF systems equipped with a sample holder for positioning sample cups may show improved repeatability of the results compared