BS ISO 18227-2014 Soil quality Determination of elemental composition by X-ray fluorescence《土质 采用X射线荧光对元素组成的测定》.pdf

1、BSI Standards PublicationBS ISO 18227:2014Soil quality Determinationof elemental composition by X-ray fluorescenceBS ISO 18227:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 18227:2014.The UK participation in its preparation was entrusted to TechnicalComm

2、ittee EH/4, Soil quality.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014.

3、Published by BSI StandardsLimited 2014ISBN 978 0 580 80816 6ICS 13.080.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2014.Amendments issued since pub

4、licationDate Text affectedBS ISO 18227:2014 ISO 2014Soil quality Determination of elemental composition by X-ray fluorescenceQualit du sol Dtermination de la composition lmentaire par fluorescence XINTERNATIONAL STANDARDISO18227First edition2014-03-01Reference numberISO 18227:2014(E)BS ISO 18227:201

5、4ISO 18227:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the

6、internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb w

7、ww.iso.orgPublished in SwitzerlandBS ISO 18227:2014ISO 18227:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Safety remarks 35 Principle 36 Apparatus . 37 Reagents 48 Interferences and sources of error 59 S

8、ample preparation . 59.1 General . 59.2 Drying and determination of dry mass 69.3 Preparation of pressed pellet . 69.4 Preparation of fused beads . 610 Procedure. 710.1 Analytical measurement conditions . 710.2 Calibration 811 Quality control .1311.1 Drift correction procedure . 1311.2 Blank test 14

9、11.3 Reference materials . 1412 Calculation of the result .1413 Test report 14Annex A (informative) Semi-quantitative screening analysis of waste, sludge, and soil samples .15Annex B (informative) Examples for operational steps of the sample preparation for soil and waste samples 18Annex C (informat

10、ive) Suggested analytical lines, crystals, and operating conditions 23Annex D (informative) List of reference materials applicable for XRF analysis 26Annex E (informative) Validation 28Bibliography .37BS ISO 18227:2014ISO 18227:2014(E)ForewordISO (the International Organization for Standardization)

11、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. Each member body interested in a subject for which a technical committee has been established has the right to be repres

12、ented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develo

13、p this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/I

14、EC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during th

15、e development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning

16、of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 190, Soi

17、l quality, Subcommittee SC 3, Chemical methods and soil characteristics.iv ISO 2014 All rights reservedBS ISO 18227:2014ISO 18227:2014(E)IntroductionX-ray fluorescence spectrometry is a fast and reliable method for the quantitative analysis of the total content of certain elements within different m

18、atrices.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 considered, such as the matrices to be analyse

19、d, the elements to be determined, the detection limits required, and the measuring times. 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 reference materials in the case of inhomoge

20、neous matrices such as waste, it is generally difficult to set up a calibration with matrix-matched reference materials.Therefore, this International Standard describes two different procedures: a quantitative analytical procedure for homogeneous solid waste, soil, and soil-like material in the norm

21、ative part. The calibration is based on matrix-matched standards; an XRF screening method for solid and liquid materials as waste, sludge, and soil in Annex A which provides a total element characterization at a semi-quantitative level. The calibration is based on matrix-independent calibration curv

22、es, previously set up by the manufacturer.The technical content of this International Standard is identical with the European Standard EN 15309:2007. ISO 2014 All rights reserved vBS ISO 18227:2014BS ISO 18227:2014Soil quality Determination of elemental composition by X-ray fluorescence1 ScopeThis I

23、nternational Standard specifies the procedure for a quantitative determination 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) spectrome

24、try using a calibration with matrix-matched standards.This International Standard is 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. Concentr

25、ation levels between approximately 0,000 1 % and 100 % can be determined depending on the element and the instrument used.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, o

26、nly the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 11464, Soil quality Pretreatment of samples for physico-chemical analysisISO 11465, Soil quality Determination of dry matter and water content on a mass basis G

27、ravimetric methodISO/IEC 17025, General requirements for the competence of testing and calibration laboratoriesEN 14346:2006, Characterization of waste Calculation of dry matter by determination of dry residue or water contentEN 15002:2006, Characterization of waste Preparation of test portions from

28、 the laboratory sample3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.NOTE See References 11 and 14 for non-specified terms.3.1absorption edgejump of the mass absorption coefficient at a specific wavelength or energy3.2absorption of X-raysloss of i

29、ntensity of X-rays by an isotropic and homogenous material as described by the Bouger-Lambert law3.3analytical linespecific characteristic X-ray spectral line of the atom or ion of the analyte used for the determination of the analyte contentINTERNATIONAL STANDARD ISO 18227:2014(E) ISO 2014 All righ

30、ts reserved 1BS ISO 18227:2014ISO 18227:2014(E)3.4continuous radiationelectromagnetic radiation produced by the acceleration of a charged particle, such as an electron, when deflected by another charged particle, such as an atomic nucleus3.5Compton-linespectral line due to incoherent scattering (Com

31、pton-effect) occurring when the incident X-ray photon strike an atom without promoting fluorescenceNote 1 to entry: Energy is lost in the collision and therefore the resulting scattered X-ray photon is of lower energy than the incident X-ray photon.3.6drift correction monitorphysically stable sample

32、 used to correct for instrumental drift3.7emitted sample X-rayradiation emitted by a sample consisting of X-ray fluorescence radiation and scattered primary X-rays3.8fused beadanalyte sample prepared by dissolution in a flux3.9liquid sampleanalyte sample submitted as a solution for direct measuremen

33、t in the sample cup3.10mass absorption coefficientconstant describing the fractional decrease in the intensity of a beam of X-radiation as it passes through an absorbing mediumNote 1 to entry: This is expressed in cm2/g.Note 2 to entry: The mass absorption coefficient is a function of the wavelength

34、 of the absorbed radiation and the atomic number of the absorbing element.3.11polarized excitation X-ray spectrometerenergy dispersive X-ray spectrometer where the excitation is performed by polarized radiation and the emitted X-ray fluorescence radiation is detected along the direction of polarizat

35、ion3.12powder sampleanalyte sample submitted as a powder for direct measurement in the sample cup3.13precisioncloseness of agreement of results obtained by applying the method several times under prescribed conditionsSOURCE: ISO 5725-2:19943.14pressed pelletanalyte sample prepared by pressing milled

36、 material into a disk3.15primary X-rayX-ray by which the sample is radiated2 ISO 2014 All rights reservedBS ISO 18227:2014ISO 18227:2014(E)3.16quality control samplestable sample with known contents, e.g. certified reference material (CRM), used to monitor instrument and calibration performance3.17X

37、-ray fluorescence radiationemission of characteristic X-rays from a sample that has been bombarded by high-energy X-rays or gamma rays4 Safety remarksAnyone dealing with waste and sludge analysis has to be aware of the typical risks that this kind of material presents irrespective of the parameter t

38、o be determined. Waste and sludge samples can contain hazardous e.g. toxic, reactive, flammable, and 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 can

39、be produced by microbiological or chemical activity are potentially flammable and pressurize 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 fl

40、uorescence spectrometer shall comply with international 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 Pr

41、incipleAfter a suitable preparation, if necessary, the sample is introduced into an 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

42、to 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 r

43、elevant preparation technique.6 Apparatus6.1 X-ray fluorescence spectrometer, shall be able to analyse the elements according to the scope of this International Standard.The following types of X-ray fluorescence spectrometers are applicable: energy dispersive X-ray fluorescence (EDXRF) spectrometer

44、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 synthetic multilayer.The

45、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; ISO 2014 All rights reserved 3BS ISO 18227:2014ISO 18227:2014(E) source modifiers to modify the shape or intensity of the

46、 source spectrum or the beam shape (such as source filters, secondary targets, polarizing targets, collimators, focusing optics, etc.).The detector unit is different for WDXRF and for EDXRF spectrometers. WDXRF spectrometers take advantage of the dispersion of the emitted radiation by scattering by

47、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 the energy of the incoming X-rays, are segregated into channels according to ener

48、gy 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 polarizing target theory resu

49、lting in a significant decrease of the background scattering, and therefore lower limits of detection can be achieved (comparable to WDXRF).6.2 Mill, preferable with walls made of agate, corundum, or zircon.6.3 Pellet preparation equipment, manual or automatic pellet press, capable of providing a pressure of at least 100 kN.6.4 Aluminium cup, supporting backing cup for pressed pellets.6.5 Fusion apparatus, electric, gas, or high-frequency induction furnace that can be heated up to a fixed temperature of between 1 050 C and 1