SIST-TS CEN/TS 16172:2013
(Main)Sludge, treated biowaste and soil - Determination of elements using graphite furnace atomic absorption spectrometry (GF-AAS)
Sludge, treated biowaste and soil - Determination of elements using graphite furnace atomic absorption spectrometry (GF-AAS)
This Technical Specification specifies the determination of trace elements in aqua regia or nitric acid digest solutions of sludge, treated biowaste and soil, using atomic absorption spectrometry with electrothermal atomisation in a graphite furnace. The method is applicable for the determination of the following elements: Arsenic (As), cadmium (Cd), cobalt (Co), lead (Pb), antimony (Sb), thallium (Tl), vanadium (V). This method may be applied to other elements. The lower working range is approximately 0,1 mg/kg to 0,01 mg/kg, depending on the element to be determined.
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels Graphitofen-Atomabsorptionsspektrometrie (GF-AAS)
Diese Europäische Norm legt die Bestimmung von Spuren¬elementen in Königswasser- und Salpetersäure-Aufschlusslösungen von Schlamm, behandeltem Bioabfall und Boden unter Anwendung von Atomabsorptionsspektrometrie mit elektrothermischer Atomisierung in einem Graphitrohrofen fest. Das Verfahren ist anwendbar auf die Bestimmung der folgenden Elemente:
Silber (Ag),Cadmium (Cd), Cobalt (Co), Chrom (Cr), Kupfer (Cu), Nickel (Ni), Blei (Pb), Antimon (Sb), Thallium (Tl), Vanadium (V).
Boue, biodéchets traités et sols - Détermination des éléments par spectrométrie d'absorption atomic avec four en graphite (GF-AAS)
La présente Norme européenne spécifie la détermination des éléments en traces solubles dans l'eau régale et l'acide nitrique, dans les boues, les bio-déchets traités et les sols, en utilisant la spectrométrie d'absorption atomique avec atomisation électrothermique dans un four graphite. La méthode est applicable pour la détermination des éléments suivants :
Argent (Ag), cadmium (Cd), cobalt (Co), chrome (Cr), cuivre (Cu), nickel (Ni), plomb (Pb), antimoine (Sb), thallium (Tl), vanadium (V).
Blato, obdelani biološki odpadki in tla - Določevanje elementov z metodo atomske absorpcijske spektrometrije z grafitno pečjo (GF-AAS)
Ta tehnična specifikacija opredeljuje določevanje elementov v sledeh v zlatotopki ali izvlečku dušikove kisline blata, obdelanih bioloških odpadkov in tal z metodo atomske absorpcijske spektrometrije z grafitno pečjo. Metoda se uporablja za določevanje naslednjih elementov: arzen (As), kadmij (Cd), kobalt (Co), svinec (Pb), antimon (Sb), talij (Tl), vanadij (V). Ta metoda se lahko uporablja tudi za določevanje drugih elementov. Spodnji delovni obseg znaša približno od 0,1 mg/kg do 0,01 mg/kg, odvisno od elementa za določevanje.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 16172:2013
01-julij-2013
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHHOHPHQWRY]PHWRGRDWRPVNH
DEVRUSFLMVNHVSHNWURPHWULMH]JUDILWQRSHþMR *)$$6
Sludge, treated biowaste and soil - Determination of elements using graphite furnace
atomic absorption spectrometry (GF-AAS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen mittels
Graphitofen-Atomabsorptionsspektrometrie (GF-AAS)
Boue, biodéchets traités et sols - Détermination des éléments par spectrométrie
d'absorption atomic avec four en graphite (GF-AAS)
Ta slovenski standard je istoveten z: CEN/TS 16172:2013
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST-TS CEN/TS 16172:2013 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 16172:2013
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SIST-TS CEN/TS 16172:2013
TECHNICAL SPECIFICATION
CEN/TS 16172
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
January 2013
ICS 13.080.10; 13.030.01
English Version
Sludge, treated biowaste and soil - Determination of elements
using graphite furnace atomic absorption spectrometry (GF-
AAS)
Boues, bio-déchets traités et sols - Détermination des Schlamm, behandelter Bioabfall und Boden - Bestimmung
éléments par spectrométrie d'absorption atomique avec von Elementen mittels Graphitrohrofen-
four en graphite (GF-AAS) Atomabsorptionsspektrometrie (GF-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 16172:2013: E
worldwide for CEN national Members.
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Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Principle .5
4 Interferences and sources of error .6
5 Reagents .6
6 Apparatus .8
7 Procedure .9
7.1 Graphite furnace programme .9
7.2 Test solution .9
7.3 Test blank solution . 10
7.4 Determination . 10
7.5 Calibration . 10
7.5.1 Standard calibration technique . 10
7.5.2 Standard addition technique . 10
8 Calculation . 11
9 Expression of results . 11
10 Test report . 12
Annex A (informative) Examples of instrumental parameter settings . 13
Bibliography . 14
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Foreword
This document (CEN/TS 16172:2013) 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.
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.
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Introduction
This Technical Specification is applicable for several types of matrices as indicated in Table 1.
Table 1 — Matrices for which this Technical Specification is applicable
Matrix Materials tested
Sludge Municipal sludge
Biowaste Compost
Fresh 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.
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1 Scope
This Technical Specification specifies the determination of trace elements in aqua regia or nitric acid digest
solutions of sludge, treated biowaste and soil, using atomic absorption spectrometry with electrothermal
atomisation in a graphite furnace. The method is applicable for the determination of the following elements:
Arsenic (As), cadmium (Cd), cobalt (Co), lead (Pb), antimony (Sb), thallium (Tl), vanadium (V).
This method may be applied to other elements. The lower working range is approximately 0,1 mg/kg to
0,01 mg/kg, depending on the element to be determined.
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
In graphite furnace atomic absorption spectrometry (GF-AAS) (also known as electrothermal atomic
absorption spectrometry, ET-AAS), discrete sample aliquots are dispensed into a graphite tube (of which there
are several types), which can be heated to over 2 500 °C very rapidly and in a controlled manner. By
increasing the temperature stepwise, the processes of drying, thermal decomposition of the matrix and
thermal dissociation into free atoms occurs. Atomic absorption spectrometry is based on the ability of free
atoms to absorb light. A light source emits light specific for a certain element (or elements). When the light
beam passes through the atom cloud in the heated graphite furnace, the light is selectively absorbed by atoms
of the chosen element(s). The decrease in light intensity is measured with a detector at a specific wavelength.
The concentration of an element in the sample is determined by comparing the absorbance of the sample with
the absorbance of calibration solutions. The signal-peak produced is, under optimum conditions, sharp and
symmetrical, and of narrow half-width. The peak area is for most elements proportional to the concentration of
the element in solution. The measurements are made at the wavelengths given in Table 2.
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Table 2 — Wavelengths of the elements
Element Wavelength
nm
Arsenic 193,7
Cadmium 228,8
Cobalt 240,7
Lead 217,0
Antimony 217,6
Thallium 276,8
Vanadium 318,4
Zeeman background correction and platform use is common practice.
If necessary, interferences may be overcome by adding a matrix modifier to the samples before analysis, or
by performing the calibration with standard addition technique.
The results are given as the mass of analyte (micrograms or milligrams) per kilogram of dried sample material.
4 Interferences and sources of error
The sample solutions prepared from digestion of samples may contain large amounts of substances that may
affect the results. High concentrations of chloride may cause low results, because the volatility of many
elements is increased and analyte loss may occur during the pyrolysis step. This effect is particularly
pronounced for thallium, so for determination of this analyte avoid aqua regia digestions and use only nitric
acid digestion according to EN 16173. Matrix effects may be overcome, partially or completely, by optimisation
of the temperature programme, the use of pyrolytically coated tubes or platforms, the use of chemical
modifiers, the standard addition technique and/or the use of background correction.
5 Reagents
Use only reagents of recognised analytical grade and water grade 1 as specified in EN ISO 3696.
For the determination of elements at trace and ultra-trace level, the reagents shall be of adequate purity. The
concentration of the analyte or interfering substances in the reagents and the water should be negligible
compared to the lowest concentration to be determined.
5.1 Hydrochloric acid, HCl, ρ(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.
5.2 Nitric acid, HNO , ρ(HNO ) = 1,4 g/ml, c(HNO ) = 15 mol/l, w(HNO ) = 650 g/kg.
3 3 3 3
The same batch of nitric acid shall be used throughout the procedure.
5.3 Nitric acid, diluted.
Add 250 ml of nitric acid (5.2) to 500 ml of water in a 1 000 ml volumetric flask and fill to the mark with water.
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5.4 Aqua regia, diluted.
Dilute 210 ml of hydrochloric acid (5.1) and 70 ml of nitric acid (5.2) with about 500 ml of water in a 1 000 ml
volumetric flask, and dilute to the mark.
5.5 Standard stock solutions
Both single-element standard stock solutions and multi-element standard stock solutions with a concentration
of 1 000 mg/l, stating the acid used, are commercially available. These solutions are considered to be stable
for more than one year, but in reference to guaranteed stability, the recommendations of the manufacturer
should be considered.
Alternatively, the standard stock solutions may be prepared in the laboratory using pure metals or salts of
known stoichiometry and purity.
5.6 Standard solutions
When preparing the standard and the calibration solutions, use the same acids as for the digestion
procedures according to EN 16173 or EN 16174.
5.6.1 Standard solution corresponding to 10 mg/l of element
Pipette 10 ml of the actual standard stock solution (5.5) into a 1 000 ml volumetric flask.
...
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