1、BS EN 16175-1:2016Sludge, treated biowasteand soil Determination ofmercuryPart 1: Cold-vapour atomic absorptionspectrometry (CV-AAS)BSI Standards PublicationBS EN 16175-1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 16175-1:2016.BSI, as a member of CEN,
2、is obliged to publish EN 16175-1 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 the conditions attached to the validati
3、on 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 Technical Committee H/-, Health and Environment
4、 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 provisions of a contract. Users are respo
5、nsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 91017 3ICS 13.030.01; 13.080.10Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of
6、 the Standards Policy and Strategy Committee on 30 November 2016.Amendments/corrigenda issued since publicationDate Text affectedBS EN 16175-1:2016g3g3g3g8g24g21g18g19g8g4g17g3g22g23g4g17g7g4g21g7g3g17g18g21g16g8g3g8g24g21g18g19g50g8g17g17g8g3g8g24g21g18g19g34g12g22g6g11g8g3g17g18g21g16g3EN 16175-1
7、g3 g3g3g18g133g150g145g132g135g148g3g884g882g883g888g3g12g6g22g3g883g885g484g882g885g882g484g882g883g482g3g883g885g484g882g890g882g484g883g882g3 g22g151g146g135g148g149g135g134g135g149g3g6g8g17g512g23g22g3g883g888g883g889g887g486g883g483g884g882g883g885g8g144g137g142g139g149g138g3g25g135g148g149g139
8、g145g144g3g3g22g142g151g134g137g135g481g3g150g148g135g131g150g135g134g3g132g139g145g153g131g149g150g135g3g131g144g134g3g149g145g139g142g3g486g3g7g135g150g135g148g143g139g144g131g150g139g145g144g3g145g136g3g143g135g148g133g151g148g155g3g486g3g19g131g148g150g3g883g483g3g6g145g142g134g486g152g131g146g1
9、45g151g148g3g131g150g145g143g139g133g3g131g132g149g145g148g146g150g139g145g144g3g149g146g135g133g150g148g145g143g135g150g148g155g3g523g6g25g486g4g4g22g524g3g5g145g151g135g149g481g3g132g139g145g486g134g177g133g138g135g150g149g3g150g148g131g139g150g177g149g3g135g150g3g149g145g142g149g3g486g3g7g177g150
10、g135g148g143g139g144g131g150g139g145g144g3g134g151g3g143g135g148g133g151g148g135g3g486g3g19g131g148g150g139g135g3g883g483g3g22g146g135g133g150g148g145g143g177g150g148g139g135g3g134g821g131g132g149g145g148g146g150g139g145g144g3g131g150g145g143g139g147g151g135g3g134g135g3g152g131g146g135g151g148g3g136
11、g148g145g139g134g135g3g523g22g4g4g486g25g19g524g3g3 g22g133g138g142g131g143g143g481g3g132g135g138g131g144g134g135g142g150g135g148g3g5g139g145g131g132g136g131g142g142g3g151g144g134g3g5g145g134g135g144g3g486g3g5g135g149g150g139g143g143g151g144g137g3g152g145g144g3g20g151g135g133g141g149g139g142g132g135
12、g148g3g486g3g23g135g139g142g3g883g483g3g14g131g142g150g134g131g143g146g136g486g4g150g145g143g131g132g149g145g148g146g150g139g145g144g149g149g146g135g141g150g148g145g143g135g150g148g139g135g3g523g6g25g486g4g4g22g524g3g23g138g139g149g3g8g151g148g145g146g135g131g144g3g22g150g131g144g134g131g148g134g3g1
13、53g131g149g3g131g146g146g148g145g152g135g134g3g132g155g3g6g8g17g3g145g144g3g883g891g3g16g131g148g133g138g3g884g882g883g888g484g3g3g3g6g8g17g3g143g135g143g132g135g148g149g3g131g148g135g3g132g145g151g144g134g3g150g145g3g133g145g143g146g142g155g3g153g139g150g138g3g150g138g135g3g6g8g17g512g6g8g17g8g15g8
14、g6g3g12g144g150g135g148g144g131g142g3g21g135g137g151g142g131g150g139g145g144g149g3g153g138g139g133g138g3g149g150g139g146g151g142g131g150g135g3g150g138g135g3g133g145g144g134g139g150g139g145g144g149g3g136g145g148g3g137g139g152g139g144g137g3g150g138g139g149g3g8g151g148g145g146g135g131g144g3g22g150g131g
15、144g134g131g148g134g3g150g138g135g3g149g150g131g150g151g149g3g145g136g3g131g3g144g131g150g139g145g144g131g142g3g149g150g131g144g134g131g148g134g3g153g139g150g138g145g151g150g3g131g144g155g3g131g142g150g135g148g131g150g139g145g144g484g3g24g146g486g150g145g486g134g131g150g135g3g142g139g149g150g149g3g1
16、31g144g134g3g132g139g132g142g139g145g137g148g131g146g138g139g133g131g142g3g148g135g136g135g148g135g144g133g135g149g3g133g145g144g133g135g148g144g139g144g137g3g149g151g133g138g3g144g131g150g139g145g144g131g142g3g149g150g131g144g134g131g148g134g149g3g143g131g155g3g132g135g3g145g132g150g131g139g144g135
17、g134g3g145g144g3g131g146g146g142g139g133g131g150g139g145g144g3g150g145g3g150g138g135g3g6g8g17g486g6g8g17g8g15g8g6g3g16g131g144g131g137g135g143g135g144g150g3g6g135g144g150g148g135g3g145g148g3g150g145g3g131g144g155g3g6g8g17g3g143g135g143g132g135g148g484g3g3g23g138g139g149g3g8g151g148g145g146g135g131g1
18、44g3g22g150g131g144g134g131g148g134g3g135g154g139g149g150g149g3g139g144g3g150g138g148g135g135g3g145g136g136g139g133g139g131g142g3g152g135g148g149g139g145g144g149g3g523g8g144g137g142g139g149g138g481g3g9g148g135g144g133g138g481g3g10g135g148g143g131g144g524g484g3g4g3g152g135g148g149g139g145g144g3g139g1
19、44g3g131g144g155g3g145g150g138g135g148g3g142g131g144g137g151g131g137g135g3g143g131g134g135g3g132g155g3g150g148g131g144g149g142g131g150g139g145g144g3g151g144g134g135g148g3g150g138g135g3g148g135g149g146g145g144g149g139g132g139g142g139g150g155g3g145g136g3g131g3g6g8g17g3g143g135g143g132g135g148g3g139g14
20、4g150g145g3g139g150g149g3g145g153g144g3g142g131g144g137g151g131g137g135g3g131g144g134g3g144g145g150g139g136g139g135g134g3g150g145g3g150g138g135g3g6g8g17g486g6g8g17g8g15g8g6g3g16g131g144g131g137g135g143g135g144g150g3g6g135g144g150g148g135g3g138g131g149g3g150g138g135g3g149g131g143g135g3g149g150g131g15
21、0g151g149g3g131g149g3g150g138g135g3g145g136g136g139g133g139g131g142g3g152g135g148g149g139g145g144g149g484g3g3g6g8g17g3g143g135g143g132g135g148g149g3g131g148g135g3g150g138g135g3g144g131g150g139g145g144g131g142g3g149g150g131g144g134g131g148g134g149g3g132g145g134g139g135g149g3g145g136g3g4g151g149g150g1
22、48g139g131g481g3g5g135g142g137g139g151g143g481g3g5g151g142g137g131g148g139g131g481g3g6g148g145g131g150g139g131g481g3g6g155g146g148g151g149g481g3g6g156g135g133g138g3g21g135g146g151g132g142g139g133g481g3g7g135g144g143g131g148g141g481g3g8g149g150g145g144g139g131g481g3g9g139g144g142g131g144g134g481g3g9g
23、145g148g143g135g148g3g28g151g137g145g149g142g131g152g3g21g135g146g151g132g142g139g133g3g145g136g3g16g131g133g135g134g145g144g139g131g481g3g9g148g131g144g133g135g481g3g10g135g148g143g131g144g155g481g3g10g148g135g135g133g135g481g3g11g151g144g137g131g148g155g481g3g12g133g135g142g131g144g134g481g3g12g14
24、8g135g142g131g144g134g481g3g12g150g131g142g155g481g3g15g131g150g152g139g131g481g3g15g139g150g138g151g131g144g139g131g481g3g15g151g154g135g143g132g145g151g148g137g481g3g16g131g142g150g131g481g3g17g135g150g138g135g148g142g131g144g134g149g481g3g17g145g148g153g131g155g481g3g19g145g142g131g144g134g481g3g
25、19g145g148g150g151g137g131g142g481g3g21g145g143g131g144g139g131g481g3g22g142g145g152g131g141g139g131g481g3g22g142g145g152g135g144g139g131g481g3g22g146g131g139g144g481g3g22g153g135g134g135g144g481g3g22g153g139g150g156g135g148g142g131g144g134g481g3g23g151g148g141g135g155g3g131g144g134g24g144g139g150g1
26、35g134g3g14g139g144g137g134g145g143g484g3g3g3g3g3g8g24g21g18g19g8g4g17g3g6g18g16g16g12g23g23g8g8g3g9g18g21g3g22g23g4g17g7g4g21g7g12g29g4g23g12g18g17g3g6g18g16g12g23g50g3g8g24g21g18g19g50g8g17g3g7g8g3g17g18g21g16g4g15g12g22g4g23g12g18g17g3g8g24g21g18g19g34g12g22g6g11g8g22g3g14g18g16g12g23g8g8g3g9g111
27、g21g3g17g18g21g16g24g17g10g3g3g3g3CEN-CENELECg3Management Centre: Avenue Marnix 17, B-1000 Brussels g825g3g884g882g883g888g3g6g8g17g3 g4g142g142g3g148g139g137g138g150g149g3g145g136g3g135g154g146g142g145g139g150g131g150g139g145g144g3g139g144g3g131g144g155g3g136g145g148g143g3g131g144g134g3g132g155g3g1
28、31g144g155g3g143g135g131g144g149g3g148g135g149g135g148g152g135g134g3g153g145g148g142g134g153g139g134g135g3g136g145g148g3g6g8g17g3g144g131g150g139g145g144g131g142g3g16g135g143g132g135g148g149g484g3g21g135g136g484g3g17g145g484g3g8g17g3g883g888g883g889g887g486g883g483g884g882g883g888g3g8BS EN 16175-1:2
29、016EN 16175-1:2016 (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 . 7 6.1 Usual laboratory apparatus. 7 6.2 Atomic absorption spectrometer (AAS) 7 6.3 Automated sample introduction system 8 6.4
30、Cold-vapour generator, batch system or an automated flow injection analysis system (FIA) . 8 7 Procedure. 8 7.1 Test solution . 8 7.2 Test blank solution . 8 7.3 Preparation of the calibration solutions 8 7.4 Calibration . 8 7.5 Measurement of test sample . 9 8 Calculation and expression of results
31、9 8.1 Calculation . 9 8.2 Expression of results 9 9 Performance data 9 10 Test report 10 Annex A (informative) Repeatability and reproducibility data . 11 A.1 Materials used in the interlaboratory comparison study . 11 A.2 Interlaboratory comparison results . 11 Bibliography . 13 BS EN 16175-1:2016E
32、N 16175-1:2016 (E) 3 European foreword This document (EN 16175-1:2016) 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 stan
33、dard, either 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. CE
34、N and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes CEN/TS 16175-1:2013. 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 de
35、velopment of 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. EN 16175, Sludge, treated biowaste an
36、d soil Determination of mercury comprises the following parts: Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS); Part 2: Cold-vapour atomic fluorescence spectrometry (CV-AFS). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countrie
37、s 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, Poland
38、, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16175-1:2016EN 16175-1:2016 (E) 4 Introduction This European Standard is applicable and validated for several types of matrices as indicated in Table 1 (see Annex A for the results of validation
39、). 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 not pur
40、port 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 according
41、 to this European Standard be carried out by suitably trained staff. BS EN 16175-1:2016EN 16175-1:2016 (E) 5 1 Scope This European Standard specifies a method for the determination of mercury in aqua regia or nitric acid digests of sludge, treated biowaste and soil, obtained according to EN 16173 or
42、 EN 16174 using cold-vapour atomic absorption spectrometry (CV-AAS). The lower working range limit is 0,03 mg/kg (dry matter basis). 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 r
43、eferences, only the edition cited applies. For undated references, the latest edition 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, Slu
44、dge, treated biowaste and soil Digestion of nitric acid soluble fractions of elements 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) 3 Principle Mono- and div
45、alent mercury is reduced to the elemental form by tin(II) chloride or sodium borohydride in acid medium. Elemental mercury is stripped off from the solution in a closed system. The mercury vapour, in the form of an atomic gas, passes through a cell positioned in the light path of an atomic absorptio
46、n spectrometer. Its absorbance at a wavelength of 253,7 nm is measured. The absorbance signal is a function of mercury concentration, and the concentrations are calculated using a calibration curve. NOTE The matrix of the solution analysed is dominated by the acids used in the digestion step. Tin(II
47、) chloride as a reduction substance is recommended in this European Standard, because sodium borohydride reduces many elements commonly found in soil, sludge and waste extract solutions, to the elemental state, which may cause matrix problems under particular circumstances. However, it is still poss
48、ible to use sodium borohydride as reduction agent. The concentration range 1 g/l to 10 g/l in the digested solution, corresponding to 0,03 g/g to 0,3 g/g of mercury when a 3,0 g sample has been digested, can be determined directly. Higher concentrations can be determined if the digested solution is
49、diluted. Sensitivity can be increased by the amalgamation technique. 4 Interferences Because the samples are digested with oxidizing, strong acids before determination of mercury starts, there are no interferences with organic substances in the gas phase that can absorb in the UV range. Neither are there any interferences with mercury compounds which cannot be fully reduced with tin(II) chloride alone. The interferences due to the presence of other elements in the matrix depend on their concentrations. Element concentrations exceeding those listed in Table 2 may ca
