SIST-TS CEN/TS 16188:2012
(Main)Sludge, treated biowaste and soil - Determination of elements in aqua regia and nitric acid digests - Flame atomic absorption spectrometry method (FAAS)
Sludge, treated biowaste and soil - Determination of elements in aqua regia and nitric acid digests - Flame atomic absorption spectrometry method (FAAS)
This Technical Specification specifies the determination of metals in aqua regia and nitric acid digests of sludge, treated biowaste and soil samples, using flame atomic absorption spectrometry. The method is applicable for the determination of the following elements:
Chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), manganese (Mn), Nickel (Ni), zinc (Zn).
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen in Königswasser- und Salpetersäure-Aufschlusslösungen - Flammen-Atomabsorptionsspektrometrie (FAAS)
Diese Technische Spezifikation legt ein Verfahren zur Bestimmung von Metallen in Königswasser und Salpetersäureaufschlüssen von Schlamm-, behandelten Bioabfall- und Bodenproben mit der Flammen-Atomabsorptionsspektrometrie fest. Das Verfahren ist für die Bestimmung der folgenden Elemente geeignet:
Chrom (Cr), Kobalt (Co), Kupfer (Cu), Eisen (Fe), Mangan (Mn), Nickel (Ni), Zink (Zn).
Boues, bio-déchets traités et sols - Détermination des éléments solubles dans l'eau régale et l'acide nitrique - Spectrométrie d'absorption atomique dans la flamme (SAA))
La présente Spécification technique définit une méthode pour la détermination de métaux solubles dans l'eau régale et l'acide nitrique, présents dans les échantillons de boues, de biodéchets traités et de sols, par spectrométrie d'absorption atomique dans la flamme. La méthode est applicable pour la détermination des éléments suivants :
Chrome (Cr), cobalt (Co), cuivre (Cu), fer (Fe), manganèse (Mn), nickel (Ni), zinc (Zn).
Blato, obdelani biološki odpadki in tla - Določevanje elementov po razklopih z zlatotopko in dušikovo kislino - Metoda plamenske atomske absorpcijske spektrometrije (FAAS)
Ta tehnična specifikacija opredeljuje določevanje kovin po razklopih z zlatotopko in dušikovo kislino v blatu, obdelanih bioloških odpadkih in tleh s plamensko atomsko absorpcijsko spektometrijo. Metoda se uporablja za določevanje naslednjih elementov: krom (Cr), kobalt (Co), baker (Cu), železo (Fe), mangan (Mn), nikelj (Ni), cink (Zn).
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 16188:2012
01-junij-2012
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHHOHPHQWRYSRUD]NORSLK]
]ODWRWRSNRLQGXãLNRYRNLVOLQR0HWRGDSODPHQVNHDWRPVNHDEVRUSFLMVNH
VSHNWURPHWULMH )$$6
Sludge, treated biowaste and soil - Determination of elements in aqua regia and nitric
acid digests - Flame atomic absorption spectrometry method (FAAS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Elementen in
Königswasser- und Salpetersäure-Aufschlusslösungen - Flammen-
Atomabsorptionsspektrometrie (FAAS)
Boues, bio-déchets traités et sols - Détermination des éléments solubles dans l'eau
régale et l'acide nitrique - Spectrométrie d'absorption atomique dans la flamme (SAA))
Ta slovenski standard je istoveten z: CEN/TS 16188:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST-TS CEN/TS 16188:2012 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 16188:2012
TECHNICAL SPECIFICATION
CEN/TS 16188
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2012
ICS 13.030.01
English Version
Sludge, treated biowaste and soil - Determination of elements in
aqua regia and nitric acid digests - Flame atomic absorption
spectrometry method (FAAS)
Boues, biodéchets traités et sols - Détermination des Schlamm, behandelter Bioabfall und Boden - Bestimmung
éléments solubles dans l'eau régale et l'acide nitrique - von Elementen in Königswasser- und Salpetersäure-
Spectrométrie d'absorption atomique dans la flamme (SAA) Aufschlusslösungen - Flammen-
Atomabsorptionsspektrometrie (FAAS)
This Technical Specification (CEN/TS) was approved by CEN on 24 April 2011 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, 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
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16188:2012: E
worldwide for CEN national Members.
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CEN/TS 16188:2012 (E)
Contents Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Principle .4
4 Interferences .5
5 Reagents .5
6 Apparatus .6
6.1 Usual laboratory equipment .6
6.2 Atomic absorption spectrometer .6
7 Procedure .7
7.1 Test sample solution .7
7.2 Test blank solution .7
7.3 Calibration and determination .7
7.4 Determination of the element content of the test sample solution .7
7.5 Special precautions .8
7.5.1 Chromium .8
7.5.2 Manganese .8
7.5.3 Nickel .8
8 Calculation and expression of results .8
8.1 Calculation .8
8.2 Expression of results .9
9 Test report .9
Annex A (informative) Preparation of standard stock solutions, 1 000 mg/l . 10
A.1 General information . 10
A.2 Cobalt (Co) and copper (Cu) standard stock solution . 10
A.3 Iron (Fe) standard stock solution . 10
A.4 Manganese (Mn) standard stock solution . 11
A.5 Nickel (Ni) standard stock solution . 11
A.6 Zinc (Zn) standard stock solution . 11
Bibliography . 12
2
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Foreword
This document (CEN/TS 16188:2012) 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.
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.
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.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, 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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1 Scope
This Technical Specification specifies the determination of metals in aqua regia and nitric acid digests of
sludge, treated biowaste and soil samples, using flame atomic absorption spectrometry. The method is
applicable for the determination of the following elements:
Chromium (Cr), cobalt (Co), copper (Cu), iron (Fe), manganese (Mn), nickel (Ni), zinc (Zn).
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 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
The method is based on the atomic absorption spectrometric measurement of the concentration of the
elements in an aqua regia or nitric acid extract of the sample, prepared in accordance with EN 16173 or
EN 16174, using the instrumental conditions given in Table 1.
Table 1 — General conditions for flame atomic absorption spectrometry
Element Wavelength Flame type Lanthanum Main Background
nm chloride interference correction
Chromium 357,9 reduced or neutral Yes Fe, Si Deuterium
air/acetylene or
acetylene/N O No
2
(recommended)
Cobalt 240,7 Oxidizing air/acetylene No Deuterium
Copper 324,8 Oxidizing air/acetylene No Deuterium
Iron 248,3 Oxidizing air/acetylene No Co, Ni, Si Deuterium
Manganese 279,5 Oxidizing air/acetylene or Yes Fe, Si Deuterium
acetylene/N O No
2
Nickel 232,0 Oxidizing air/acetylene No Fe Deuterium
Zinc 213,9 Oxidizing air/acetylene No Deuterium
NOTE The wavelengths given are the most sensitive. The use of less sensitive lines to avoid the dilution step before
measurement is suitable especially for determination of Fe (e. g. 372,0 nm) and Mn (e. g. 403,1 nm) in soil extracts.
Interferences are generally lower if the nitrous oxide (N O) flame is used for the determination of chromium and
2
manganese. Users should be aware that small changes in gas volume ratios can have significant effects on the intensity
of the analytical signal, and can also change the linearity of the instrument response. Also difference in acid strength,
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which will vary slightly from digest to digest, can have a measurable effect on some elements. Users should, therefore,
familiarize themselves with these aspects of their instrument’s performance.
4 Interferences
Digests of soils may contain large amounts of substances that may affect the results. Matrix effects may be
overcome, partially or completely, by the use of a chemical modifier like lanthanum, the standard addition
technique, and the use of background correction.
5 Reagents
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 Water quality 1 according to EN ISO 3696 for all sample preparations and dilutions.
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 1 + 3 (volume fraction).
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.
5.4 Hydrochloric acid, HCl, ρ(HCl) = 1,17 g/ml, c(HCl) = 12 mol/l, w(HCl) = 370 g/kg.
The same batch of hydrochloric acid shall be used throughout the procedure.
5.5 Aqua regia, diluted 1 + 3 (volume fraction).
Add 210 ml of hydrochloric acid (5.4) and 70 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.
5.6 Standard stock solutions
5.6.1 General information
Both single-element standard
...
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