1、January 2017 English price group 13No 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 13.030.01; 13.080.10!%_C“2605932
2、www.din.deDIN EN 16171Sludge, treated biowaste and soil Determination of elements using inductively coupled plasma mass spectrometry (ICPMS);English version EN 16171:2016,English translation of DIN EN 16171:2017-01Schlamm, behandelter Bioabfall und Boden Bestimmung von Elementen mittels Massenspektr
3、ometrie mit induktiv gekoppeltem Plasma (ICPMS);Englische Fassung EN 16171:2016,Englische bersetzung von DIN EN 16171:2017-01Boues, biodchets traits et sols Dtermination des lments en traces par spectromtrie de masse avec plasma induit par haute frquence (ICPMS);Version anglaise EN 16171:2016,Traduc
4、tion anglaise de DIN EN 16171:2017-01SupersedesDIN CEN/TS 16171(DIN SPEC 91256):201303www.beuth.deDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.Document comprises 27 pages 01.17 2 A comma is used as the decimal marker. National fo
5、reword This document (EN 16171:2016) has been prepared by Technical Committee CEN/TC 444 “Test methods for the characterization of solid matrices” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Wasserwesen (DIN Standards Committee Wat
6、er Practice), Working Committee NA 119-01-02-02 UA Chemische und physikalische Verfahren, Working Group 119-01-02-02-04 AK Elementanalytik. Amendments This standard differs from DIN CEN/TS 16171 (DIN SPEC 91256):2013-03 as follows: a) “Repeatability and reproducibility data” from a European interlab
7、oratory comparison study have been added (see Annex A); b) the standard has been editorially revised. Previous editions DIN CEN/TS 16171 (DIN SPEC 91256): 2013-03 DIN EN 16171:2017-01 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16171 October 2016 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 1
8、6171:2012English Version Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma mass spectrometry (ICP-MS) Boues, bio-dchets traits et sols - Dtermination des lments en traces par spectromtrie de masse avec plasma induit par haute frquence (ICP-MS) Schlamm, be
9、handelter Bioabfall und Boden - Bestimmung von Elementen mittels Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP-MS) This European Standard was approved by CEN on 19 March 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givi
10、ng 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 three offi
11、cial 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 standards bodies of
12、 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, Slovenia, Spain,
13、Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for
14、 CEN national Members. Ref. No. EN 16171:2016 EEN 16171:2016 (E) 2 Contents Page European foreword . 4 Introduction 5 1 Scope 6 2 Normative references 6 3 Principle . 6 4 Interferences 7 4.1 General 7 4.2 Spectral interferences . 7 4.2.1 Isobaric elemental interferences 7 4.2.2 Isobaric molecular an
15、d doubly-charged ion interferences . 7 4.2.3 Non-spectral interferences 7 5 Reagents . 8 6 Apparatus 11 6.1 General requirements 11 6.2 Mass spectrometer 11 6.3 Mass-flow controller . 11 6.4 Nebuliser with variable speed peristaltic pump 11 6.5 Gas supply . 11 6.6 Storage bottles for the stock, stan
16、dard, calibration and sample solutions. 12 7 Procedure 12 7.1 Test sample solution . 12 7.2 Test solution 12 7.3 Instrument set-up 12 7.4 Calibration 13 7.4.1 Linear calibration function . 13 7.4.2 Standard addition calibration . 13 7.4.3 Determination of correction factors . 13 7.4.4 Variable isoto
17、pe ratio . 13 7.5 Sample measurement . 13 8 Calculation 14 9 Expression of results . 14 10 Performance characteristics 15 10.1 Blank . 15 10.2 Calibration check . 15 10.3 Internal standard response 15 10.4 Interference . 15 10.5 Recovery 15 10.6 Performance data . 16 11 Test report 16 Annex A (infor
18、mative) Repeatability and reproducibility data . 17 DIN EN 16171:2017-01 EN 16171:2016 (E) 3 Annex B (informative) Selected isotopes and spectral interferences for quadrupole ICP-MS instruments 24 Bibliography . 25 DIN EN 16171:2017-01 EN 16171:2016 (E) 4 European foreword This document (EN 16171:20
19、16) has been prepared by Technical Committee CEN/TC 444 “Test methods for environmental characterization of solid matrices”, 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,
20、 at the latest by April 2017, and conflicting national standards shall be withdrawn at the latest by April 2017. 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
21、or all such patent rights. This document supersedes CEN/TS 16171:2012. The preparation of the previous edition of this analytical method by CEN is based on a mandate by the European Commission (Mandate M/330), which assigned the development of standards on sampling and analytical methods for hygieni
22、c and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. This document contains the following technical changes in comparison with the previous edition: repeatabil
23、ity and reproducibility data have been added from a European interlaboratory comparison organized by the German Federal Institute for Materials Research and Testing BAM in 2013 (see Annex A). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following cou
24、ntries 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, Netherlands, Norway, P
25、oland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16171:2017-01 EN 16171:2016 (E) 5 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see Annex A for the results of vali
26、dation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Compost Soil Soil WARNING Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does n
27、ot purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted acc
28、ording to this European Standard be carried out by suitably trained staff. DIN EN 16171:2017-01 EN 16171:2016 (E) 6 1 Scope This European Standard specifies a method for the determination of the following elements in aqua regia or nitric acid digests of sludge, treated biowaste and soil: Aluminium (
29、Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), cesium (Cs), chromium (Cr), cobalt (Co), copper (Cu), dysprosium (Dy), erbium (Er), europium (Eu), gadolinium (Gd), gallium (Ga), germanium (Ge), gold (Au), hafnium (Hf),
30、holmium (Ho), indium (In), iridium (Ir), iron (Fe), lanthanum (La), lead (Pb), lithium (Li), lutetium (Lu), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), palladium (Pd), phosphorus (P), platinum (Pt), potassium (K), praseodymium (Pr), rhenium (Re), rhodi
31、um (Rh), rubidium (Rb), ruthenium (Ru), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), terbium (Tb), thallium (Tl), thorium (Th), thulium (Tm), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), ytterbiu
32、m (Yb), yttrium (Y), zinc (Zn), and zirconium (Zr). The working range depends on the matrix and the interferences encountered. The method detection limit of the method is between 0,1 mg/kg dry matter and 2,0 mg/kg dry matter for most elements. The limit of detection will be higher in cases where the
33、 determination is likely to be interfered (see Clause 4) or in case of memory effects (see e.g. EN ISO 17294-1:2006, 8.3). The method has been validated for the elements given in Table A.1 (sludge), Table A.2 (compost) and Table A.3 (soil). The method is applicable for the other elements listed abov
34、e, provided the user has verified the applicability. 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 ed
35、ition of the referenced document (including any amendments) applies. EN 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue or water content EN 16173, Sludge, treated biowaste and soil Digestion of nitric acid soluble fractions of ele
36、ments EN 16174, Sludge, treated biowaste and soil Digestion of aqua regia soluble fractions of elements EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) EN ISO 17294-1:2006, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) P
37、art 1: General guidelines (ISO 17294-1:2004) 3 Principle Digests of sludge, treated biowaste or soil with nitric acid or aqua regia (see EN 16173 and EN 16174) are analysed by ICP-MS to get a multi-elemental determination of analytes. The method measures ions produced by a radio-frequency inductivel
38、y coupled plasma. Analyte species originating in the digest solution are nebulised and the resulting aerosol is transported by argon gas into the plasma. The ions produced by the high temperatures of the plasma are entrained in the plasma gas and introduced, by means of an interface, into a mass spe
39、ctrometer, sorted according to their mass-to-charge ratios and quantified with a detector (e.g. channel electron multiplier). DIN EN 16171:2017-01 EN 16171:2016 (E) 7 NOTE For the determination of tin only aqua regia extraction applies (EN 16174). 4 Interferences 4.1 General Interferences shall be a
40、ssessed and valid corrections applied. Interference correction shall include compensation for background ions contributed by the plasma gas, reagents, and constituents of the sample matrix. Detailed information on spectral and non-spectral interferences is given in EN ISO 17294-1:2006, Clause 6. 4.2
41、 Spectral interferences 4.2.1 Isobaric elemental interferences Isobaric elemental interferences are caused by isotopes of different elements of closely matched nominal mass-to-charge ratio and which cannot be separated due to an insufficient resolution of the mass spectrometer in use (e.g. 114Cd and
42、 114Sn). Element interferences from isobars may be corrected by taking into account the influence from the interfering element (see EN ISO 17294-1:2006). The isotopes used for correction shall be free of interference if possible. Correction options are often included in the software supplied with th
43、e instrument. Common isobaric interferences are given in Table B.1. 4.2.2 Isobaric molecular and doubly-charged ion interferences Isobaric molecular and doubly-charged ion interferences in ICP-MS are caused by ions consisting of more than one atom or charge, respectively. Examples include 40Ar35Cl+a
44、nd 40Ca35Cl+ion on the 75As signal or 98Mo16O+ions on the 114Cd+signal. Natural isotope abundances are available from the literature. The accuracy of correction equations is based upon the constancy of the observed isotopic ratios for the interfering species. Corrections that presume a constant frac
45、tion of a molecular ion relative to the “parent“ ion have not been found to be reliable, e.g. oxide levels can vary with operating conditions. If a correction for an oxide ion is based upon the ratio of parent-to-oxide ion intensities, this shall be determined by measuring the interference solution
46、just before the sequence is started. The validity of the correction coefficient should be checked at regular intervals within a sequence. Another possibility to remove isobaric molecular interferences is the use of an instrument with collision/reaction cell technology. The use of high resolution ICP
47、-MS allows the resolution of these interferences and additionally double-charged ion interferences. The response of the analyte of interest shall be corrected for the contribution of isobaric molecular and doubly charged interferences if their impact can be higher than three times the detection limi
48、t or higher than half the lowest concentration to be reported. More information about the use of correction factors is given in EN ISO 17294-1. 4.2.3 Non-spectral interferences Physical interferences are associated with sample nebulisation and transport processes as well as with ion-transmission eff
49、iciencies. Nebulisation and transport processes can be affected if a matrix component causes a change in surface tension or viscosity. Changes in matrix composition can cause DIN EN 16171:2017-01 EN 16171:2016 (E) 8 significant signal suppression or enhancement. Solids can be deposited on the nebuliser tip of a pneumatic nebuliser and on the cones. It is recommended to keep the level of total dissolved solids below 0,2 % (2 000 mg/l) to minimise deposition of
