Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS)

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 EN 16174 using cold-vapour atomic absorption spectrometry (CV-AAS). The lower working range limit is 0,03 mg/kg (dry matter basis).

Schlamm, behandelter Bioabfall und Boden - Bestimmung von Quecksilber - Teil 1: Kaltdampf-Atomabsorptionsspektrometrie (CV-AAS)

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Quecksilber in Königswasser  oder Salpetersäureaufschlusslösungen von Schlamm, behandeltem Bioabfall und Boden, hergestellt nach EN 16173 oder EN 16174, durch Kaltdampf Atomabsorptionsspektrometrie (CV-AAS) fest. Die untere Bestimmungsgrenze liegt bei 0,03 mg/kg (Trockenmasse).

Boues, bio-déchets traités et sols - Détermination du mercure - Partie 1: Spectrométrie d'absorption atomique de vapeur froide (SAA-VP)

La présente Norme européenne spécifie une méthode de détermination du mercure soluble dans l'eau régale ou l'acide nitrique des boues, des bio-déchets traités et des sols, obtenus conformément à l’EN 16173 ou à l’EN 16174, par spectrométrie d'absorption atomique en vapeur froide (SAA-VP). La limite inférieure de la plage de travail est de 0,03 mg/kg (par rapport à la matière sèche).

Blato, obdelani biološki odpadki in tla - Določevanje živega srebra - 1. del: Metoda atomske absorpcijske spektrometrije s tehniko hladnih par (CV-AAS)

Ta evropski standard določa metodo za določevanje živega srebra v zlatotopki ali izvlečku dušikove kisline blata, obdelanih bioloških odpadkov in tal, pridobljenega v skladu s standardom EN 16173 ali EN 16174, z uporabo metode atomske absorpcijske spektrometrije s tehniko hladnih par (CV-AAS). Spodnja meja delovnega razpona je 0,03 mg/kg (suha osnova).

General Information

Status
Published
Public Enquiry End Date
03-Jan-2016
Publication Date
13-Mar-2017
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Feb-2017
Due Date
09-Apr-2017
Completion Date
14-Mar-2017

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Schlamm, behandelter Bioabfall und Boden - Bestimmung von Quecksilber - Teil 1: Kaltdampf-Atomabsorptionsspektrometrie (CV-AAS)Boues, bio-déchets traités et sols - Détermination du mercure - Partie 1: Spectrométrie d'absorption atomique de vapeur froide (SAA-VP)Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16175-1:2016SIST EN 16175-1:2017en,fr,de01-april-2017SIST EN 16175-1:2017SLOVENSKI

STANDARDSIST-TS CEN/TS 16175-1:20131DGRPHãþD
SIST EN 16175-1:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16175-1
October
t r s x English Version
Sludgeá treated biowaste and soil æ Determination of mercury æ Part

sã Coldævapour atomic absorption Bouesá bioædéchets traités et sols æ Détermination du mercure æ Partie

sã Spectrométrie d 5absorption
Schlammá behandelter Bioabfall und Boden æ Bestimmung von Quecksilber æ Teil
sã KaltdampfæThis European Standard was approved by CEN on
s { March
t r s xä

egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä

translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels

t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s x s y wæ sã t r s x ESIST EN 16175-1:2017

EN 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 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 ...................................................................................................... 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

SIST EN 16175-1:2017

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”, 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 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 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 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 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 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 16175-1:2017

EN 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). 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 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 tests conducted according to this European Standard be carried out by suitably trained staff. SIST EN 16175-1:2017

EN 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 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 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 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 elements 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 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 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 solutions, 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 µg/l to 10 µg/l in the digested solution, corresponding to 0,03 µg/g to 0,3 µg/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 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 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 than indicated in Table 2. SIST EN 16175-1:2017

EN 16175-1:2016 (E) 6 Table 2 — Tolerable concentrations of s
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