1、Sludge, treated biowasteand soil Determination ofelements using inductivelycoupled plasma opticalemission spectrometry(ICP-OES)BS EN 16170:2016Incorporating corrigendum .BSDI2017BSI Standards PublicationBS EN 16170:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation
2、of EN 16170:2016.BSI, as a member of CEN, is obliged to publish EN 16170 as a British Standard. However, attention is drawn to the fact that during the development of this European Standard, the UK committee voted against its approval as a European Standard.The UK committee is concerned that some of
3、 the conditions attached to the validation trials lack clarity.It is also the opinion of the UK committee that validation trials for horizontal methods should include conditions for the preparation and extraction of the original sample.The UK participation in its preparation was entrusted by Technic
4、al Committee H/-, Health and Environment Sector Policy and Strategy Committee, to Subcommittee H/-/4, Environmental Testing Programmes.A list of organizations represented on this subcommittee can be obtained on request to its secretary.This publication does not purport to include all the necessary p
5、rovisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017. Published by BSI Standards Limited 2017ISBN 978 0 580 97516 5ICS 13.030.01; 13.080.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Stand
6、ard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2016.Amendments/corrigenda issued since publicationDate Text affected .BSDI 2017 Implementation of CEN Correction Notice 9 November 2016: Table A.2 correctedEUROPEAN STANDARD NORME EUROPENNE EUROPISCH
7、E NORM EN 16170 October 2016 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 16170:2012 English Version Sludge, treated biowaste and soil - Determination of elements using inductively coupled plasma optical emission spectrometry (ICP-OES) Boues, bio-dchets traits et sols - Dtermination des lments en trac
8、es par spectromtrie dmission optique avec plasma induit par haute frquence (ICP-OES) Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) This European Standard was approved by CEN on 19 March 2016. Thi
9、s European Standard was corrected and reissued by the CEN-CENELEC Management Centre on 9 November 2016. 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.
10、 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 official versions (English, French, German). A version in any other language made by tr
11、anslation 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, Fin
12、land, 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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZAT
13、ION 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 CEN national Members. Ref. No. EN 16170:2016 EBS EN 16170:2016EN 16170:2016 (E) 2
14、 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 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 Calculati
15、on 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 data . 12 11 Test report 12 Annex A (informative) Repeatability and reproducibility data . 13 Annex B (informative) Wavelengths, spectral interfer
16、ences and estimated instrumental detection limits . 19 Annex C (informative) Inter-element correction . 23 Bibliography . 25 BS EN 16170:2016g8g17g3g883g888g883g889g882g483g884g882g883g888g3g525g8g526EN 16170:2016 (E) 3 European foreword This document (EN 16170:2016) has been prepared by Technical C
17、ommittee 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, at the latest by April 2017, and co
18、nflicting 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 or all such patent rights. This docu
19、ment 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 standards on sampling and analytical methods for hygienic and biological parameters as well
20、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: repeatability and reproducibility data have be
21、en 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 countries are bound to implement this E
22、uropean 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, Poland, Portugal, Romania, Slovakia,
23、Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16170:2016g8g17g3g883g888g883g889g882g483g884g882g883g888g3g525g8g526EN 16170:2016 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see Annex A for t
24、he 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 usual laboratory practice. This Europe
25、an 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. IMPORTANT It is absolutely essential that t
26、ests conducted according to this European Standard be carried out by suitably trained staff. BS EN 16170:2016g8g17g3g883g888g883g889g882g483g884g882g883g888g3g525g8g526EN 16170:2016 (E) 5 1 Scope This European Standard specifies a method for the determination of the following elements in aqua regia
27、or nitric acid 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 (
28、La), lead (Pb), 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),
29、 thallium (Tl), 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 applicabil
30、ity. 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 edition of the referenced document (including any
31、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 elements EN 16174, Sludge, treated biowaste and soi
32、l Digestion of 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 pl
33、asma optical emission 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
34、 aerosol is transported 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 determinat
35、ion of tin only 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. Addit
36、ional interferences and matrix effects shall be recognised and appropriate corrections made. Tests for their presence are described below. BS EN 16170:2016g8g17g3g883g888g883g889g882g483g884g882g883g888g3g525g8g526EN 16170:2016 (E) 6 Spectral interferences are caused by background emission from cont
37、inuous or recombination phenomena, stray light which causes background 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
38、 measurements adjacent to the analyte wavelength peak. Spectral scans 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 estima
39、te of the background emission is provided by an interpolation from measurements 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 wavel
40、ength peak. The locations used for routine measurement shall be free 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 wave
41、length. Alternatively they can be corrected by multiple dimensional spectra 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 int
42、erest. When operative and uncorrected, interferences will produce false 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, a
43、s a corrective action. In this case, the selection of background points 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 caus
44、e significant inaccuracies, especially in samples containing high dissolved 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
45、by using an internal standard. Chemical interferences include molecular 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. r
46、adio frequency (RF) power, observation position, gas flow rate and so 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
47、 a previous sample contribute to the signals measured in a new sample. 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
48、 be minimised by flushing the system with a rinse blank between samples. 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 analys
49、is 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 the water should be negligible compared to the lowest concentration to be determined. 5.1 Water, grade 2 as specified in EN ISO 3696 for all sample preparations and dilutions. 5.2 Nitric acid, HNO3, g591(HNO3) = 1,4g/ml, c(HNO3) = 15 mol/l, w(HNO3) = 650 g/kg. BS EN 16170:2016g8g17g3g883g888g883g889g882g483g8
