DIN EN ISO 13196-2015 Soil quality - Screening soils for selected elements by energy-dipersive X-ray fluorescence spectrometry using a handheld or portable instrument (ISO 13196 20.pdf

1、November 2015 English price group 12No 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 13.080.10!%GF“2363527www.din.de

2、DIN EN ISO 13196Soil quality Screening soils for selected elements by energy-dispersive X-ray fluorescence spectrometry using a handheld or portable instrument (ISO 13196:2013);English version EN ISO 13196:2015,English translation of DIN EN ISO 13196:2015-11Bodenbeschaffenheit Screening ausgewhlter

3、Elemente in Bden mit handhaltbaren oder tragbaren Rntgenfluoreszenzspektrometern (ISO 13196:2013);Englische Fassung EN ISO 13196:2015,Englische bersetzung von DIN EN ISO 13196:2015-11Qualit du sol Analyse rapide dune slection dlments dans les sols laide dun spectromtre de fluorescence X dispersion d

4、nergie portable ou portatif (ISO 13196:2013);Version anglaise EN ISO 13196:2015,Traduction anglaise de DIN EN ISO 13196:2015-11www.beuth.deDocument comprises 20 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.10.15 DIN EN ISO 1

5、3196:2015-11 2 A comma is used as the decimal marker. National foreword The text of ISO 13196:2013 has been prepared by Technical Committee ISO/TC 190 “Soil quality” and has been taken over as EN ISO 13196:2015 by Technical Committee CEN/TC 345 “Characterization of soils” (Secretariat: NEN, Netherla

6、nds). The responsible German body involved in its preparation was the DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-02-21 AK Vor-Ort-Verfahren. WARNING The use of this standard involves the use of hazardous equipment. In particular, such hazard

7、s are as follows: As a rule, commercially available X-ray fluorescence spectrometers (XRF) are fully protected devices that are subject to governmental approval conditions. This ensures that, when such equipment is correctly operated, the user is not exposed to radiation. However, carrying out measu

8、rements in the field directly on the sample can generate secondary radiation. Therefore, safety precautions are to be taken when performing XRF measurements in the field. The person carrying out the measurement should always be aware that X-rays can be generated during the measurement and that the n

9、ational safety provisions are to be observed. The DIN Standards corresponding to the European and International Standards referred to in this document are as follows: EN 15309 DIN EN 15309 ISO 5725-2 DIN ISO 5725-2 ISO 10381-5 DIN ISO 10381-5 ISO 12404 DIN EN ISO 12404 DIN EN ISO 13196:2015-11 3 Nat

10、ional Annex NA (informative) Bibliography DIN EN 15309, Characterization of waste and soil Determination of elemental composition by X-ray fluorescence DIN EN ISO 12404, Soil quality Guidance on the selection and application of screening methods DIN ISO 5725-2, Accuracy (trueness and precision) of m

11、easurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 10381-5, Soil quality Sampling Part 5: Guidance on the procedure for the investigation of urban and industrial sites with regard to soil contaminati

12、on DIN EN ISO 13196:2015-11 4 This page is intentionally blank EUROPEAN 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 portabl

13、e instrument (ISO 13196:2013) Qualit du sol - Analyse 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 in Bden mit handhaltbaren oder tragbaren Rntgenfluore

14、szenzspektrometern (ISO 13196:2013) This European Standard 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-d

15、ate 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 three official versions (English, French, German). A version in any other language made by translatio

16、n 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 standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Fo

17、rmer 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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION C O

18、M I T EUR O P EN D E NOR M A L I S ATI O N EUR O P I S C HES KOM I T E E F R NOR M UNG 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 E Contents

19、PageEuropean Foreword .3Introduction 41 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 65 Apparatus . 65.1 X-ray fluorescence spectrometer (XRF) 65.2 Container for sampling and preparation 65.3 Spoon . 65.4 Sieve (optional) 65.5 Sample cup for portable XRF 65.6 Sample contai

20、ner for handheld XRF . 65.7 Drying device (optional) . 66 Procedure. 76.1 General . 76.2 Performance check of instrument 76.3 Calibration 76.4 In situ measurement . 76.5 Analysis of soil with sampling . 87 Quality control 87.1 Performance test by standard reference material 87.2 Energy calibration 9

21、8 Test report . 9Annex A (informative) Precision data 10Bibliography .16EN ISO 13196:2015 (E) DIN EN ISO 13196:2015-11 2 European foreword The text of ISO 13196:2013 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardization (ISO) and has

22、 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, either by publication of an identical text or by endorsement, at the latest by January

23、 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 and/or CENELEC shall not be held responsible for identifying any or all such patent ri

24、ghts. 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, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, Franc

25、e, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 13196:2013 has been approved by CEN as EN ISO

26、13196:2015 without any modification. EN ISO 13196:2015 (E) DIN EN ISO 13196:2015-11 3 IntroductionX-ray fluorescence spectrometry (XRF) is a quick method for determination of total elemental compositions of soil samples. Unlike analyses by atomic absorption spectroscopy and inductively coupled plasm

27、a spectroscopy, XRF needs no digestion step to prepare a test solution to be analysed. Factory pre-set calibrations can 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 ar

28、e Cr, As, Se, Cd, Hg and Pb, depending on the instrument. For in situ or abbreviated preparation analyses at a site, a 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 o

29、btain semiquantitative results. It is often impracticable to carry out calibration using reference materials at the site 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 eleme

30、nts, including heavy metals, using battery-powered handheld or portable energy-dispersive XRF (EDXRF).EN ISO 13196:2015 (E) DIN EN ISO 13196:2015-11 4 WARNING Soil samples may contain toxic contaminants. Avoid direct contact of soil samples with exposed parts of the body. Appropriate measures shall

31、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 X-ray fluorescence analysis shall qualify for m

32、anaging 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-dispersive XRF spectrometers are used. This quick me

33、thod 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 results can be expected (see e.g. Reference4).T

34、his 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 performance of the instruments used, the concent

35、ration 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 the requirements (limit or threshold values) s

36、et 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) methods like atomic absorption spectrometry (

37、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 undated references, the latest edition of the ref

38、erenced 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 and definitionsFor the purposes of this document,

39、 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 entry: The calculation of the theoretical X-ray

40、fluorescence intensities is carried out based on assumed element composition, theoretical parameters and pre-determined sensitivity coefficients of the X-ray fluorescence spectrometer.EN ISO 13196:2015 (E) DIN EN ISO 13196:2015-11 5 3.2handheld XRF spectrometerXRF spectrometer which can be used for

41、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 selected elements in soil is determined using a handheld or portable XRF in the field. Element concentrations ar

42、e 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-ray fluorescence spectrometer (EDXRF).5.2 Container for sampling and preparationA plastic cup or tray that c

43、an 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, ceramic) to take soil samples from sites and to disaggregate the sample.5.4 Sieve (optional)A sieve of size 2 mm

44、.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. Alternatively, for heavy metals a plastic bag may be used. The concentration of target elements in the cup or plastic

45、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 in the container shall be negligible.5.7 Drying device (optional)A portable electric drying oven, hot plate

46、 etc. that are powered by batteries, a portable generator or a heater driven by exothermic chemical reactions, e.g. hydration of calcium oxide.EN ISO 13196:2015 (E) DIN EN ISO 13196:2015-11 6 6 Procedure6.1 GeneralHandheld XRF instruments can be used for direct in situ soil measurement to receive qu

47、alitative results. Handheld and portable XRF instruments in combination with limited sample pretreatment will give semiquantitative results.If quantitative results are needed, a complete set of sample pretreatment with homogenization and particle size reduction is necessary (see EN 15309).Before sta

48、rting 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 the manufacturers instructions and perform tests with samples of known composition.For further details of sampling and measurement concepts, see ISO 12404.6.2 Perf