1、BSI Standards PublicationBS EN ISO 13196:2015Soil quality Screening soils for selected elements by energy-dispersive X-ray fluorescence spectrometry using a handheld or portable instrumentBS EN ISO 13196:2015 BRITISH STANDARDNational forewordThe UK participation in its preparation was entrusted to T
2、 e c h n i c a l Committee EH/4, Soil quality.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 necessary provisions of a contract. Users are responsible for its correct application. The British Stan
3、dards Institution 2015. Published by BSI Standards Limited 2015.ISBN 978 0 580 88558 7 ICS 13.080.10 Compliance with a British Standard cannot confer immunityfrom legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2013
4、.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dThis British Standard is the UK implementation of EN ISO 13196:2015. It is identical to ISO 13196:2013. It supersedes BS ISO 13196:2013 which is withdrawn.31 July 2015 This corrigendum renumbers BS ISO 13196:2013as BS EN ISO
5、13196:2015EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13196 July 2015 ICS 13.080.10 English Version Soil quality - Screening soils for selected elements by energy-dispersive X-ray fluorescence spectrometry using a handheld or portable instrument (ISO 13196:2013) Qualit du sol - Analyse
6、rapide dune slection dlments dans les sols laide dun spectromtre de fluorescence X dispersion dnergie portable ou portatif (ISO 13196:2013)Bodenbeschaffenheit - Screening ausgewhlter Elemente inBden mit handhaltbaren oder tragbaren Rntgenfluoreszenzspektrometern (ISO 13196:2013) This European Standa
7、rd was approved by CEN on 16 July 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such
8、 national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in 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
9、language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Gr
10、eece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUN
11、G CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13196:2015 EEuropean foreword The text of ISO 13196:2013 has been prepared by Technical Committee ISO/TC 19
12、0 “Soil quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 13196:2015 by Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, ei
13、ther by publication of an identical text or by endorsement, at the latest by January 2016, and conflicting national standards shall be withdrawn at the latest by January 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN an
14、d/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Cze
15、ch 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, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdo
16、m. Endorsement notice The text of ISO 13196:2013 has been approved by CEN as EN ISO 13196:2015 without any modification. EN ISO 13196:2015 (E) iiBS EN ISO 13196:2015ISO 13196:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and
17、definitions . 14 Principle 25 Apparatus . 25.1 X-ray fluorescence spectrometer (XRF) 25.2 Container for sampling and preparation 25.3 Spoon . 25.4 Sieve (optional) 25.5 Sample cup for portable XRF 25.6 Sample container for handheld XRF . 25.7 Drying device (optional) . 26 Procedure. 36.1 General . 3
18、6.2 Performance check of instrument 36.3 Calibration 36.4 In situ measurement . 36.5 Analysis of soil with sampling . 47 Quality control 47.1 Performance test by standard reference material 47.2 Energy calibration 58 Test report . 5Annex A (informative) Precision data . 6Bibliography .12BS EN ISO 13
19、196:2015ISO 13196:2013(E)ForewordISO (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. Each member body interested in
20、 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 International Electrotechnical Commiss
21、ion (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 Standards adopted by the technical co
22、mmittees 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 subject of patent rights. ISO shall not
23、 be held responsible for identifying any or all such patent rights.ISO 13196 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics.iv ISO 2013 All rights reservedBS EN ISO 13196:2015ISO 13196:2013(E)IntroductionX-ray fluorescence s
24、pectrometry (XRF) is a quick method for determination of total elemental compositions of soil samples. Unlike analyses by atomic absorption spectroscopy and inductively coupled plasma spectroscopy, XRF needs no digestion step to prepare a test solution to be analysed. Factory pre-set calibrations ca
25、n be used. Consequently XRF is suitable for the rapid on-site determination of selected elements, mainly heavy metals in screening processes. Typical elements that can be analysed are Cr, As, Se, Cd, Hg and Pb, depending on the instrument. For in situ or abbreviated preparation analyses at a site, a
26、 battery-powered handheld or portable XRF equipment is required.When performing analyses at a site, it might be important to have information on the presence of an element and also obtain semiquantitative results. It is often impracticable to carry out calibration using reference materials at the si
27、te to be investigated. In these situations, factory pre-set calibrations should be used.This International Standard describes rapid methods for the on-site analysis of selected elements, including heavy metals, using battery-powered handheld or portable energy-dispersive XRF (EDXRF). ISO 2013 All ri
28、ghts reserved vBS EN ISO 13196:2015BS EN ISO 13196:2015Soil quality Screening soils for selected elements by energy-dispersive X-ray fluorescence spectrometry using a handheld or portable instrumentWARNING Soil samples may contain toxic contaminants. Avoid direct contact of soil samples with exposed
29、 parts of the body. Appropriate measures shall be taken to avoid ingestion and inhalation.Exposure to X-rays may give rise to dermal and haematological diseases. X-ray fluorescence spectrometers shall comply with national regulations relevant to radiation protection. At least one person involved in
30、X-ray fluorescence analysis shall qualify for managing or supervising the operation of X-ray apparatus according to national regulations.1 ScopeThis International Standard specifies the procedure for screening soils and soil-like materials for selected elements when handheld or portable energy-dispe
31、rsive XRF spectrometers are used. This quick method is assumed to be applied on-site to obtain qualitative or semiquantitative data that assists decisions on further sampling strategy for assessing soil quality. The higher the efforts for pretreatment used on soil samples, the better the analytical
32、results can be expected (see e.g. Reference4).This International Standard does not explicitly specify elements for which it is applicable, since the applicability depends on the performance of the apparatus and the objective of the screening. The elements which can be determined are limited by the p
33、erformance of the instruments used, the concentration of the element present in the soil, and the requirements of the investigation (e.g. guideline value).For Hg, Cd, Co, Mo, V and Sb, a majority of instruments are not sensitive enough to reach sufficiently low limits of quantification (LOQ) to meet
34、 the requirements (limit or threshold values) set in the ordinances of different countries. In this case, other methods need to be employed to measure these low concentrations. Usually, wet chemical methods are used, based on aqua regia extracts, in combination with optical or mass spectrometric (MS
35、) methods like atomic absorption spectrometry (AAS), inductively coupled plasmaoptical emission spectrometry (ICPOES) or ICPMS.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For un
36、dated references, the latest edition of the referenced document (including any amendments) applies.ISO 12404, Soil quality Guidance on the selection and application of screening methodsEN 15309, Characterization of waste and soil Determination of elemental composition by X-ray fluorescence3 Terms an
37、d definitionsFor the purposes of this document, the following terms and definitions apply.3.1fundamental parameter approachmethod to obtain element composition through successive approximation of the theoretical X-ray fluorescence intensities to the measured X-ray fluorescence intensitiesNote 1 to e
38、ntry: The calculation of the theoretical X-ray fluorescence intensities is carried out based on assumed element composition, theoretical parameters and pre-determined sensitivity coefficients of the X-ray fluorescence spectrometer.INTERNATIONAL STANDARD ISO 13196:2013(E) ISO 2013 All rights reserved
39、 1BS EN ISO 13196:2015ISO 13196:2013(E)3.2handheld XRF spectrometerXRF spectrometer which can be used for in-situ analysis by handheld operation3.3portable XRF spectrometerXRF spectrometer for samples taken out of a site, which can be carried to the site by hand4 PrincipleThe concentration of select
40、ed elements in soil is determined using a handheld or portable XRF in the field. Element concentrations are measured after sampling and limited pretreatment or directly in situ.5 Apparatus5.1 X-ray fluorescence spectrometer (XRF)Appropriate battery-powered handheld or portable energy-dispersive X-ra
41、y fluorescence spectrometer (EDXRF).5.2 Container for sampling and preparationA plastic cup or tray that can accommodate a sufficient amount of soil sample. The plastic material shall be strong enough to hold aggregates while crushing them by pressing.5.3 SpoonA non-metal spoon (e.g. plastic, cerami
42、c) to take soil samples from sites and to disaggregate the sample.5.4 Sieve (optional)A sieve of size 2 mm.5.5 Sample cup for portable XRFA plastic cup, which is suitable for the XRF-equipment to be used, having a window at its bottom made of polypropylene or polyethylene terephthalate. Alternativel
43、y, for heavy metals a plastic bag may be used. The concentration of target elements in the cup or plastic bag material shall be negligible.5.6 Sample container for handheld XRFPlastic container suitable for simple sample pretreatment and direct XRF measurement. The concentration of target elements i
44、n the container shall be negligible.5.7 Drying device (optional)A portable electric drying oven, hot plate etc. that are powered by batteries, a portable generator or a heater driven by exothermic chemical reactions, e.g. hydration of calcium oxide.2 ISO 2013 All rights reservedBS EN ISO 13196:2015I
45、SO 13196:2013(E)6 Procedure6.1 GeneralHandheld XRF instruments can be used for direct in situ soil measurement to receive qualitative results. Handheld and portable XRF instruments in combination with limited sample pretreatment will give semiquantitative results.If quantitative results are needed,
46、a complete set of sample pretreatment with homogenization and particle size reduction is necessary (see EN 15309).Before starting calibration and measurements, define the parameters to be analysed. Check if the level of concentration to be measured is within the working range of your instrument. Use
47、 the manufacturers instructions and perform tests with samples of known composition.For further details of sampling and measurement concepts, see ISO 12404.6.2 Performance check of instrumentBefore analysis, follow the instrument manufacturers instructions for setup, conditioning, preparation and ma
48、intenance. Additionally, the performance control of the instrument has to be carried out at least once a day to ensure the stability of the instrument.X-ray fluorescence spectrometry would have spectral overlap interferences. In order to confirm the performance of the instrument and interference-cor
49、rection software, it is recommended that the instrument be tested by using multi-element reference samples having elemental compositions similar to those of actual soils.6.3 CalibrationUsually, calibration is not necessary and the pre-installed manufacturers calibration is sufficient. If specific calibration is needed, follow the manufacturers instructions.If site-specific calibration graphs are to be used, measurement shall be done under the same operation and sample conditions that were employed in the calibration. For sam
