1、December 2016 English price group 10No 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!%A“2599130
2、www.din.deDIN EN 16175-1Sludge, treated biowaste and soil Determination of mercury Part 1: Coldvapour atomic absorption spectrometry (CVAAS);English version EN 161751:2016,English translation of DIN EN 16175-1:2016-12Schlamm, behandelter Bioabfall und Boden Bestimmung von Quecksilber Teil 1: Kaltdam
3、pfAtomabsorptionsspektrometrie (CVAAS);Englische Fassung EN 161751:2016,Englische bersetzung von DIN EN 16175-1:2016-12Boues, biodchets traits et sols Dtermination du mercure Partie 1: Spectromtrie dabsorption atomique de vapeur froide (SAAVP);Version anglaise EN 161751:2016,Traduction anglaise de D
4、IN EN 16175-1:2016-12SupersedesDIN CEN/TS 161751(DIN SPEC 912641):201304www.beuth.deDocument comprises 15 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN 16175-1:2016-12 2 A comma is used as the decimal marker. Nat
5、ional foreword This document (EN 16175-1:2016) 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 Com
6、mittee Water Practice), Working Group NA 119-01-02-02-04 AK Elementanalytik of Working Committee NA 119-01-02-02 UA Chemische und physikalische Verfahren. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-2 DIN ISO 5725-2 Amendments Thi
7、s standard differs from DIN CEN/TS 16175-1 (DIN SPEC 91264-1):2013-04 as follows: a) Repeatability and reproducibility data from a European interlaboratory comparison study have been added (see Annex A); b) the standard has been editorially revised. Previous editions DIN CEN/TS 16175-1 (DIN SPEC 912
8、64-1): 2013-04 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISC
9、HE NORM EN 16175-1 October 2016 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 16175-1:2013English Version Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS) Boues, bio-dchets traits et sols - Dtermination du mercure - Partie 1: Spe
10、ctromtrie dabsorption atomique de vapeur froide (SAA-VP) Schlamm, behandelter Bioabfall und Boden - Bestimmung von Quecksilber - Teil 1: Kaltdampf-Atomabsorptionsspektrometrie (CV-AAS) This European Standard was approved by CEN on 19 March 2016. CEN members are bound to comply with the CEN/CENELEC I
11、nternal 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 Management Centre or to
12、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 status as the official
13、 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, Malta, Netherlands, Nor
14、way, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, 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 explo
15、itation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16175-1:2016 EEN 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 laborator
16、y apparatus. 7 6.2 Atomic absorption spectrometer (AAS) 7 6.3 Automated sample introduction system 8 6.4 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 so
17、lutions 8 7.4 Calibration . 8 7.5 Measurement of test sample . 9 8 Calculation and expression of results 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 interlaborator
18、y comparison study . 11 A.2 Interlaboratory comparison results . 11 Bibliography . 13 DIN EN 16175-1:2016-12 EN 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”
19、, 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 conflicting national standards shall be withdrawn at the latest by April 2017. Attention
20、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 document supersedes CEN/TS 16175-1:2013. The preparation of the previous edition of this an
21、alytical 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 as inorganic and organic determinants, aiming to make these standards applicable to s
22、ludge, treated biowaste and soil as far as this is technically feasible. EN 16175, Sludge, treated biowaste and 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). Acc
23、ording 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, France, German
24、y, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16175-1:2016-12 EN 16175-1:2016 (E) 4 Introduction This European Standard is applic
25、able and validated for several types of matrices as 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
26、using this European Standard should be familiar with 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 comp
27、liance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 16175-1:2016-12 EN 16175-1:2016 (E) 5 1 Scope This European Standard specifies a method for the determination
28、 of mercury in aqua regia or nitric acid digests of sludge, treated biowaste and soil, obtained according to EN 16173 or 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,
29、 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) applies. EN 15934, Sludge, treated biowa
30、ste, 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 aqua regia soluble fractions of eleme
31、nts EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Principle Mono- and divalent 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
32、 mercury vapour, in the form of an atomic gas, passes through a cell positioned in the light path of an atomic absorption 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
33、calibration curve. NOTE The matrix of the solution analysed is dominated by the acids used in the digestion step. Tin(II) 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 solu
34、tions, to the elemental state, which may cause matrix problems under particular circumstances. However, it is still possible 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 sa
35、mple has been digested, can be determined directly. Higher concentrations can be determined if the digested solution is diluted. Sensitivity can be increased by the amalgamation technique. 4 Interferences Because the samples are digested with oxidizing, strong acids before determination of mercury s
36、tarts, 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 depe
37、nd on their concentrations. Element concentrations exceeding those listed in Table 2 may cause negative bias. Fewer interferences arise from heavy metals when tin(II) chloride is used rather than sodium borohydride. When flow systems are used, interference effects due to heavy metals may be less tha
38、n indicated in Table 2. DIN EN 16175-1:2016-12 EN 16175-1:2016 (E) 6 Table 2 Tolerable concentrations of some matrix elements Element Acceptable concentration in the test solution mg/l Cu(II) 500 Ni(II) 500 Ag(I) 1 5 Reagents For the determination of mercury at trace and ultra-trace level, the reage
39、nts shall be of adequate purity. The concentration of mercury or interfering substances in the reagents and the water should be negligible compared to the lowest concentration of mercury to be determined. 5.1 Water quality 2 according to EN ISO 3696 for all sample preparations and dilutions. 5.2 Car
40、rier gas, argon or nitrogen, with a purity of 99,99 %. 5.3 Hydrochloric acid, HCl, (HCl) = 1,18 g/ml, c(HCl) = 12 mol/l, w(HCl) = 370 g/kg. The same batch of hydrochloric acid shall be used throughout the procedure. 5.4 Nitric acid, HNO3, (HNO3) = 1,4 g/ml, c(HNO3) = 15 mol/l, w(HNO3) = 650 g/kg. Th
41、e same batch of nitric acid shall be used throughout the procedure. 5.5 Nitric acid, diluted solution. Add 10 ml nitric acid (5.4) to 500 ml of water in a 1 000 ml volumetric flask, mix and fill to the mark with water. 5.6 Nitric acid, c(HNO3) = 2 mol/l, rinsing solution for glassware. Add 150 ml of
42、 nitric acid (5.4) to about 500 ml of water, and dilute with water to 1 000 ml. 5.7 Aqua regia, diluted solution. Add 21 ml hydrochloric acid (5.3) and 7 ml nitric acid (5.4) to 500 ml of water in a 1 000 ml volumetric flask, mix and fill to the mark with water. 5.8 Tin(II) chloride solution, (SnCl2
43、 2 H2O) = 100 g/l. Dissolve 10 g of SnCl2 2 H2O in 30 ml of hydrochloric acid (5.3), transfer to a 100 ml volumetric flask and fill to the mark with water. The blank concentration of mercury can be reduced by bubbling a stream of nitrogen through the solution for 30 min, if necessary. Prepare this s
44、olution on the day of use. A solution of lower concentration, e. g. 0,5 g in 100 ml, may be used with flow systems. Prepare this latter solution freshly on the day of use from the more concentrated solution by diluting with water. Follow the recommendations of the manufacturer of the spectrometer. D
45、IN EN 16175-1:2016-12 EN 16175-1:2016 (E) 7 5.9 Sodium borohydride solution, NaBH4, (NaBH4) = 30 g/l. 1 g sodium hydroxide, NaOH, is weighed into a 100 ml volumetric flask and dissolved in water. 3 g sodium borohydride, NaBH4, are weighed into a 100 ml volumetric flask, dissolved and diluted to the
46、mark with the sodium hydroxide solution. A solution of lower concentration, e. g. 3 g/l may be used with flow systems. Prepare this latter solution freshly on the day of use from the more concentrated solution by diluting with water. Follow the recommendations of the manufacturer of the spectrometer
47、. 5.10 Mercury standard stock solution, 1 000 mg/l. Use a commercially available quantitative stock solution with a mercury concentration of (1 000 2) mg/l. This solution is considered to be stable for at least one year, but in reference to guaranteed stability, see the recommendations of the manufa
48、cturer. 5.11 Mercury, standard solution I, 100 mg/l. Pipette 10 ml of the mercury standard stock solution (5.10) into a 100 ml volumetric flask, add 10 ml nitric acid (5.4), mix and fill to the mark with water. This solution is stable for one month. 5.12 Mercury, standard solution II, 1 mg/l. Pipett
49、e 1 ml of the mercury standard solution I (5.11) into a 100 ml volumetric flask, add 10 ml nitric acid (5.4), mix and fill to the mark with water. This solution is stable for 7 days. 5.13 Mercury, standard solution III, 100 g/l. Pipette 10 ml of the mercury standard solution II (5.12) into a 100 ml volumetric flask, add 10 ml nitric acid (5.4), mix and fill to the mark with water. This solution shall be freshly prepared on the day of
