DIN EN 16175-2-2016 Sludge treated biowaste and soil - Determination of mercury - Part 2 Cold-vapour atomic fluorescence spectrometry (CV-AFS) German version EN 16175-2 2016《污泥、处理的.pdf

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1、December 2016 English price group 9No 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!%“2599129ww

2、w.din.deDIN EN 16175-2Sludge, treated biowaste and soil Determination of mercury Part 2: Coldvapour atomic fluorescence spectrometry (CVAFS);English version EN 161752:2016,English translation of DIN EN 16175-2:2016-12Schlamm, behandelter Bioabfall und Boden Bestimmung von Quecksilber Teil 2: Kaltdam

3、pfAtomfluoreszenzspektrometrie (CVAFS);Englische Fassung EN 161752:2016,Englische bersetzung von DIN EN 16175-2:2016-12Boues, biodchets traits et sols Dtermination du mercure Partie 2: Spectromtrie de fluorescence atomique de vapeur froide (SFAVP);Version anglaise EN 161752:2016,Traduction anglaise

4、de DIN EN 16175-2:2016-12SupersedesDIN CEN/TS 161752(DIN SPEC 912642):201304www.beuth.deDocument comprises 14 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN 16175-2:2016-12 2 A comma is used as the decimal marker.

5、 National foreword This document (EN 16175-2:2016) 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

6、 Committee 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. Amendments This standard differs from DIN CEN/TS 16175-2 (DIN SPEC 91264-2):2013-04 as follows: a) repeatability and reproducibility data fro

7、m a European interlaboratory comparison study have been added (see Annex A); b) the standard has been editorially revised. Previous editions DIN CEN/TS 16175-2 (DIN SPEC 91264-2): 2013-04 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16175-2 October 2016 ICS 13.030.01; 13.080.10 Supersedes CE

8、N/TS 16175-2:2013English Version Sludge, treated biowaste and soil - Determination of mercury - Part 2: Cold-vapour atomic fluorescence spectrometry (CV-AFS) Boues, biodchets traits et sols - Dtermination du mercure - Partie 2: Spectromtrie de fluorescence atomique de vapeur froide (SFA-VP) Schlamm,

9、 behandelter Bioabfall und Boden - Bestimmung von Quecksilber - Teil 2: Kaltdampf-Atomfluoreszenzspektrometrie (CV-AFS) 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 giving thi

10、s 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 official v

11、ersions (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 Austr

12、ia, 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, Sweden

13、, 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 CEN n

14、ational Members. Ref. No. EN 16175-2:2016 EEN 16175-2:2016 (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 7 Procedure. 8 7.1 Test solution . 8 7.2 Test blank solution . 8 7.3 Preparation of

15、the calibration solutions 8 7.4 Calibration . 8 7.5 Measurement of test sample . 8 8 Calculation and expression of results 9 8.1 Calculation . 9 8.2 Expression of results 9 9 Performance data 9 10 Test report . 9 Annex A (informative) Repeatability and reproducibility data . 11 Bibliography . 12 DIN

16、 EN 16175-2:2016-12 EN 16175-2:2016 (E) 3 European foreword This document (EN 16175-2:2016) 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 stat

17、us 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 is drawn to the possibility that some of the elements of this document may be the subject

18、 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 16175-2:2013. The preparation of the previous edition of this analytical method by CEN is based on a mandate by the European Commission (Mandate M/330),

19、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 sludge, treated biowaste and soil as far as this is technically feasible. This document co

20、ntains the following technical changes 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). EN 16175, Sludge,

21、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). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the

22、 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, Latvia, Lithuania, Luxembourg, Malta, Netherla

23、nds, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16175-2:2016-12 EN 16175-2:2016 (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. DIN EN 16175-2:2016-12 EN 16175-2:2016 (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, obta

27、ined according to EN 16173 or EN 16174 using cold-vapour atomic fluorescence spectrometry (CV-AFS). The lower working range limit is 0,003 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

28、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 biowaste, soil and waste Calculation of dry matter fraction after determination of dry residu

29、e 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 elements EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO

30、 3696) 3 Principle Mono- and divalent mercury is reduced to the elemental form by tin(II) chloride solution or sodium borohydride in acid medium. Elemental mercury is stripped off from the solution in a closed system, by means of a stream of argon or nitrogen. The mercury vapour is injected into the

31、 cell of an atomic fluorescence spectrometer where the mercury atoms are excited by radiation of a specific wavelength, usually about 254 nm. The intensity of the fluorescence radiation is a function of mercury concentration. The concentrations are calculated using a calibration curve. NOTE The matr

32、ix 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 solutions, to the elemental state, w

33、hich may cause matrix problems under particular circumstances. However, it is still possible to use sodium borohydride as reduction agent. The concentration range 0,1 g/l to 10 g/l in the test solution, corresponding to 0,003 mg/kg to 0,3 mg/kg of mercury, when a 3,0 g sample has been digested, can

34、be determined directly. Higher concentrations can be determined if the test solution is diluted. Sensitivity can be increased by the amalgamation technique. 4 Interferences The presence of water vapour or aerosol in the fluorescence cell may cause suppression due to quenching. Water vapour should be

35、 removed from the carrier gas stream using a hygroscopic membrane before entering the detector. The noble metals, such as gold and silver, amalgamate with mercury and, therefore, may cause suppression. Also anions, for instance sulfide, iodide and bromide, which complex strongly with mercury, can ca

36、use suppression. 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 than indicated in Table 2. DIN EN 16175-2:2016-12 EN 16175-2:2016 (E) 6 Table 2 Tolerable concen

37、trations 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 reagents shall be of adequate purity. The concentration of mercury or interfering substances in th

38、e 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 Hydrochloric acid, HCl, (HCl) = 1,18 g/ml, c(HCl) = 12 mol/l, w(HCl) = 370 g/kg. The same batch

39、of hydrochloric acid shall be used throughout the procedure. 5.3 Nitric acid, HNO3, (HNO3) = 1,4 g/ml, c(HNO3) = 15 mol/l w(HNO3) = 650 g/kg. The same batch of nitric acid shall be used throughout the procedure. 5.4 Nitric acid, diluted solution. Add 10 ml nitric acid (5.3) to 500 ml of water in a 1

40、 000 ml volumetric flask, mix and fill to the mark with water. 5.5 Nitric acid, c(HNO3) = 2 mol/l, rinsing solution for glassware. Add 150 ml of nitric acid (5.3) to about 500 ml of water, and dilute with water to 1 000 ml. 5.6 Aqua regia, diluted solution. Add 21 ml hydrochloric acid (5.2) and 7 ml

41、 nitric acid (5.3) to 500 ml of water in a 1 000 ml volumetric flask, mix and fill to the mark with water. 5.7 Tin(II) chloride solution, (SnCl2 2 H2O) = 100 g/l. Dissolve 10 g of SnCl2 2 H2O in 30 ml of hydrochloric acid (5.2), transfer to a 100 ml volumetric flask and fill to the mark with water.

42、The blank concentration of mercury can be reduced by bubbling a stream of nitrogen through the solution for 30 min, if necessary. Prepare this solution 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

43、the day of use from the more concentrated solution by diluting with water. 5.8 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

44、, dissolved and diluted to the mark with the sodium hydroxide solution. 5.9 Mercury standard stock solution, 1 000 mg/l DIN EN 16175-2:2016-12 EN 16175-2:2016 (E) 7 Use a commercially available quantitative stock solution with a mercury concentration of (1 000 2) mg/l. This solution is considered to

45、 be stable for at least one year, but in reference to guaranteed stability, see the recommendations of the manufacturer. 5.10 Mercury, standard solution I, 100 mg/l. Pipette 10 ml of the mercury standard stock solution (5.9) into a 100 ml volumetric flask, add 10 ml nitric acid (5.3), mix and fill t

46、o the mark with water. This solution is stable for one month. 5.11 Mercury, standard solution II, 1 mg/l. Pipette 1 ml of the mercury standard solution I (5.10) into a 100 ml volumetric flask, add 10 ml nitric acid (5.3), mix and fill to the mark with water. This solution is stable for 7 days. 5.12

47、Mercury, standard solution III, 100 g/l Pipette 10 ml of the mercury standard solution II (5.11) into a 100 ml volumetric flask, add 10 ml nitric acid (5.3), mix and fill to the mark with water. This solution shall be freshly prepared on the day of use. 5.13 Carrier gas, argon or nitrogen, with a pu

48、rity of 99,99 %. 6 Apparatus 6.1 Usual laboratory apparatus All glassware shall be carefully cleaned for low trace element determinations, e. g. by immersion in nitric acid rinsing solution (5.5) for a minimum of 6 h, followed by rinsing with water before use. The nitric acid shall be replaced each

49、week. 6.2 Atomic fluorescence spectrometer (AFS) Equipped with a specific Hg lamp, a fixed 254 nm filter, a photomultiplier tube for the detection of fluorescence radiation and a suitable software for processing the output signal. Operate at a current recommended by the lamp or the instrument manufacturer. The gas supply (argon or nitrogen) should be equipped with a two stage regulator. The use of a gas purifier consisting of activated ca