DIN EN 16170-2017 Sludge treated biowaste and soil - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) German version EN 16170 2016.pdf

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!%_B“2605931

2、www.din.deDIN EN 16170Sludge, treated biowaste and soil Determination of elements using inductively coupled plasma optical emission spectrometry (ICPOES);English version EN 16170:2016,English translation of DIN EN 16170:2017-01Schlamm, behandelter Bioabfall und Boden Bestimmung von Elementen mittels

3、 optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICPOES);Englische Fassung EN 16170:2016,Englische bersetzung von DIN EN 16170:2017-01Boues, biodchets traits et sols Dtermination des lments en traces par spectromtrie dmission optique avec plasma induit par haute frquence (ICPOES);V

4、ersion anglaise EN 16170:2016,Traduction anglaise de DIN EN 16170:2017-01SupersedesDIN CEN/TS 16170(DIN SPEC 91255):201302www.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 use

5、d as the decimal marker. National foreword This document (EN 16170:2016) 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 Wass

6、erwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-02-02 UA Chemische und physikalische Verfahren, Working Group 119-01-02-02-04 AK Elementanalytik. The following changes have been made to the ISO Standard as regards application in Germany: Errors in the English reference

7、version have been corrected in this document by national footnotes. Amendments This standard differs from DIN CEN/TS 16170 (DIN SPEC 91255):2013-02 as follows: a) Annex A (informative) “Repeatability and reproducibility data” from a European interlaboratory comparison study has been added; b) the st

8、andard has been editorially revised. Previous editions DIN CEN/TS 16170 (DIN SPEC 91255): 2013-02 DIN EN 16170:2017-01 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16170 October 2016 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 16170:2012 English Version Sludge, treated biowaste and soil - Det

9、ermination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) Boues, bio-dchets traits et sols - Dtermination des lments en traces par spectromtrie dmission optique avec plasma induit par haute frquence (ICP-OES) Schlamm, behandelter Bioabfall und Boden - Bestimmung

10、 von Elementen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) This European Standard was approved by CEN on 19 March 2016. This European Standard was corrected and reissued by the CEN-CENELEC Management Centre on 9 November 2016. CEN members are bound to comply wi

11、th 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 national standards may be obtained on application to the CEN-CENELEC Mana

12、gement 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 language and notified to the CEN-CENELEC Management Centre has the same st

13、atus 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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Mal

14、ta, 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 NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CE

15、N All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16170:2016 E EN 16170:2016 (E) 2 Contents Page European foreword . 3 Introduction 4 1 Scope 5 2 Normative references 5 3 Principle . 5 4 Interferences 5 5 Reagents . 6 6 Apparatus . 8 7

16、 Procedure. 9 7.1 Test sample solution 9 7.2 Test solution . 9 7.3 Instrument set-up . 9 7.4 Calibration 10 7.5 Sample measurement . 10 8 Calculation 11 9 Expression of results . 11 10 Performance characteristics 11 10.1 Calibration check . 11 10.2 Interference . 12 10.3 Recovery 12 10.4 Performance

17、 data . 12 11 Test report 12 Annex A (informative) Repeatability and reproducibility data . 13 Annex B (informative) Wavelengths, spectral interferences and estimated instrumental detection limits . 19 Annex C (informative) Inter-element correction . 23 Bibliography . 25 DIN EN 16170:2017-01 EN 1617

18、0:2016 (E) 3 European foreword This document (EN 16170:2016) 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, eith

19、er by publication of an identical text or by endorsement, 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 C

20、ENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 16170:2012. 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

21、 standards on sampling and analytical methods for hygienic 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 ch

22、anges in comparison with the previous edition: repeatability 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,

23、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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Lat

24、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16170:2017-01 EN 16170:2016 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as

25、indicated in Table 1 (see Annex A for the results of validation). 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

26、 usual laboratory practice. This European Standard does not 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. IMPO

27、RTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16170:2017-01 EN 16170:2016 (E) 5 1 Scope This European Standard specifies a method for the determination of the following elements in aqua regia or nitric acid

28、digest solutions of sludge, treated biowaste and soil: Aluminium (Al), antimony (Sb), arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), boron (B), cadmium (Cd), calcium (Ca), cerium (Ce), chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga), indium (In), iron (Fe), lanthanum (La), lead (Pb),

29、 lithium (Li), magnesium (Mg), manganese (Mn), mercury (Hg), molybdenum (Mo), neodymium (Nd), nickel (Ni), phosphorus (P), potassium (K), praseodymium (Pr), samarium (Sm), scandium (Sc), selenium (Se), silicon (Si), silver (Ag), sodium (Na), strontium (Sr), sulfur (S), tellurium (Te), thallium (Tl),

30、 thorium (Th), tin (Sn), titanium (Ti), tungsten (W), uranium (U), vanadium (V), zinc (Zn) and zirconium (Zr). The method has been validated for the elements given in Table A.1. The method is applicable for the other elements listed above, provided the user has verified the applicability. 2 Normativ

31、e 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 of the referenced document (including any amendments) app

32、lies. 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 elements EN 16174, Sludge, treated biowaste and soil Digestion of

33、aqua regia soluble fractions of elements EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Principle Digests of sludge, treated biowaste or soil with nitric acid or aqua regia (see EN 16173 and EN 16174) are analysed by inductively coupled plasma optical em

34、ission spectrometry (ICP-OES) using sequential or simultaneous optical systems and axial or radial viewing of the plasma. The instrument measures characteristic emission spectra by optical spectrometry. Analyte species originating in the digest solution are nebulised and the resulting aerosol is tra

35、nsported to the plasma torch. Element-specific emission spectra are produced by a radio-frequency inductively coupled plasma. The spectra are dispersed by a grating spectrometer, and the intensities of the emission lines are monitored by photosensitive devices. NOTE For the determination of tin only

36、 aqua regia extraction applies (EN 16174). 4 Interferences Background correction is required for trace element determination. Background correction is not required in cases of line broadening where a background correction measurement would actually degrade the analytical result. Additional interfere

37、nces and matrix effects shall be recognised and appropriate corrections made. Tests for their presence are described below. DIN EN 16170:2017-01 EN 16170:2016 (E) 6 Spectral interferences are caused by background emission from continuous or recombination phenomena, stray light which causes backgroun

38、d increase or overlap of a spectral line from another element, or unresolved overlap of molecular band spectra. Background emission and stray light can usually be compensated for by subtracting the background emission determined by measurements adjacent to the analyte wavelength peak. Spectral scans

39、 of samples compared with single element solutions in the analyte regions may indicate when alternate wavelengths are desirable because of severe spectral interference. These scans will also show whether the most appropriate estimate of the background emission is provided by an interpolation from me

40、asurements on both sides of the wavelength peak or by measured emission on only one side. The locations selected for the measurement of background intensity will be determined by the complexity of the spectrum adjacent to the wavelength peak. The locations used for routine measurement shall be free

41、of off-line spectral interference (inter-element or molecular) or adequately corrected to reflect the same change in background intensity as occurs at the wavelength peak. Spectral overlaps may be avoided by using an alternate wavelength. Alternatively they can be corrected by multiple dimensional s

42、pectra fitting methods or by equations that correct for inter-element contributions. Instruments that use equations for inter-element correction require the interfering elements to be analysed at the same time as the element of interest. When operative and uncorrected, interferences will produce fal

43、se positive determinations and would be reported as analyte concentrations. The interferences are listed in Table B.1. If available, the user should apply multiple dimensional spectra fitting methods provided by the manufacturer, as a corrective action. In this case, the selection of background poin

44、ts for correction is not necessary, since all adjacent wavelengths are processed. Physical interferences are effects associated with the sample nebulisation and transport processes. Changes in viscosity and surface tension can cause significant inaccuracies, especially in samples containing high dis

45、solved solids or high acid concentrations. If physical interferences are present, they shall be reduced by diluting the sample, matching the acid concentration, matrix-matching, or a high solid nebuliser. They can be corrected for by using an internal standard. Chemical interferences include molecul

46、ar compound formation, ionisation effects, and solute vaporisation effects. Normally, these effects are not significant with the ICP technique, but if observed, can be minimised by careful selection of operating conditions (e. g. radio frequency (RF) power, observation position, gas flow rate and so

47、 forth), by buffering of the sample, by matrix matching, and by standard addition procedures. Chemical interferences are highly dependent on matrix type and the specific analyte element. Memory interferences result when analytes in a previous sample contribute to the signals measured in a new sample

48、. Memory effects can result from sample deposition in the uptake tubing or to the nebuliser and from the build-up of sample material in the plasma torch and spray chamber. The occurrence memory effects depend on the element and can be minimised by flushing the system with a rinse blank between sampl

49、es. The possibility of memory interferences should be recognised within an analytical run and suitable rinse times should be used to reduce them. The rinse times necessary for a particular element shall be estimated prior to analysis during method development. 5 Reagents For the determination of elements at trace and ultra-trace level, the reagents shall be of adequate purity. The concentration of the analyte or interfering substances in the reagents and t