SIST-TS CEN/TS 16175-1:2013
(Main)Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS)
Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS)
This Technical Specification 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)
Die folgenden zitierten Dokumente sind für die Anwendung dieses Dokuments erforderlich. Bei datierten Ver-weisungen gilt nur die in Bezug genommene Ausgabe. Bei undatierten Verweisungen gilt die letzte Ausgabe des in Bezug genommenen Dokuments (einschließlich aller Änderungen).
EN ISO 3696, Wasser für analytische Zwecke — Anforderungen und Prüfungen
prEN 16173, Schlamm behandelter Bioabfall und Boden — Aufschluss von mit Salpetersäure löslichen Anteilen von Elementen
prEN 16174, Schlamm behandelter Bioabfall und Boden — Aufschluss von mit Königswasser löslichen Anteilen von Elementen
Boues, biodéchets traités et sols - Détermination du mercure - Partie 1: Spectrométrie d'absorption atomique de vapeur froide (SAA-VP)
La présente Spécification technique spécifie une méthode de détermination du mercure soluble dans l'eau
régale ou l'acide nitrique des boues, des biodéchets 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 tehnična specifikacija 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). Meja spodnjega delovnega obsega znaša 0,03 mg/kg (suha osnova).
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 16175-1:2013
01-julij-2013
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHåLYHJDVUHEUDGHO 0HWRGD
DWRPVNHDEVRUSFLMVNHVSHNWURPHWULMHVWHKQLNRKODGQLKSDU &9$$6
Sludge, treated biowaste and soil - Determination of mercury - Part 1: Cold-vapour
atomic absorption spectrometry (CV-AAS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Quecksilber - Teil 1:
Kaltdampf-Atomabsorptionsspektrometrie (CV-AAS)
Boues, biodéchets traités et sols - Détermination du mercure - Partie 1: Spectrométrie
d'absorption atomique de vapeur froide (SAA-VP)
Ta slovenski standard je istoveten z: CEN/TS 16175-1:2013
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST-TS CEN/TS 16175-1:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 16175-1:2013
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SIST-TS CEN/TS 16175-1:2013
TECHNICAL SPECIFICATION
CEN/TS 16175-1
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
January 2013
ICS 13.030.01; 13.080.10
English Version
Sludge, treated biowaste and soil - Determination of mercury -
Part 1: Cold-vapour atomic absorption spectrometry (CV-AAS)
Boues, biodéchets traités et sols - Détermination du Schlamm, behandelter Bioabfall und Boden - Bestimmung
mercure - Partie 1: Spectrométrie d'absorption atomique de von Quecksilber - Teil 1: Kaltdampf-
vapeur froide (SAA-VP) Atomabsorptionsspektrometrie (CV-AAS)
This Technical Specification (CEN/TS) was approved by CEN on 16 June 2012 for provisional application.
The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.
CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.
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, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16175-1:2013: E
worldwide for CEN national Members.
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CEN/TS 16175-1:2013 (E)
Contents Page
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 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 Precision 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 . 12
Bibliography . 13
2
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Foreword
This document (CEN/TS 16175-1:2013) has been prepared by Technical Committee CEN/TC 400 “Project
Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by
DIN.
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 has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association, and supports essential requirements of EU Directive(s).
The preparation of this document 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.
CEN/TS 16175, Sludge, treated biowaste and soil — Determination of mercury, is comprised of 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 organisations of the following
countries are bound to announce this Technical Specification: 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.
3
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Introduction
This Technical Specification is validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of validation).
Table 1 — Matrices for which this Technical Specification is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Compost
Soil Agricultural soil
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification 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 Technical
Specification be carried out by suitably trained staff.
4
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1 Scope
This Technical Specification 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 Technical Specification, 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.
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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
...
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