CEN/TS 15411:2006
(Main)Solid recovered fuels - Methods for the determination of the content of trace elements (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
Solid recovered fuels - Methods for the determination of the content of trace elements (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
This Technical Specification specifies three methods of digestion for solid recovered fuels:
a) microwave assisted digestion with hydrofluoric, nitric and hydrochloric acid mixture;
b) hot water bath digestion of with hydrofluoric, nitric and hydrochloric acid mixture, after ashing of the SRFs sample;
c) oven digestion with nitric, perchloric and hydrofluoric acid mixture.
Instrumental determination of As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn, Mo, Ni, Sb, Se, Tl, V, Zn is performed by Inductively Coupled Plasma with optical or mass detection or graphite furnace Atomic Absorption Spectrometry. Hg can be analysed only after the microwave assisted procedure or, alternatively, by a direct analysis method.
The effectiveness of the digestion can be verified by qualitative X-ray fluorescence (XRF) analysis on the remaining residue. If necessary an alternative digestion method (among those proposed) is used.
Method a) is recommended for general use, but the amount of the test portion can be very low in case of high concentration of organic matter.
Method b) is recommended for SRFs with high organic matter concentration that can be difficult to digest with the other methods. This method is not suitable for mercury.
Method c) is recommended for SRFs samples for which the other methods leave a significant insoluble residue.
Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Spurenelementen (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
Combustibles solides de récupération - Méthodes pour la détermination de la teneur en éléments traces (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V et Zn)
Trdno alternativno gorivo - Metode za določevanje elementov v sledovih (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V in Zn)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2007
7UGQRDOWHUQDWLYQRJRULYR0HWRGH]DGRORþHYDQMHHOHPHQWRYYVOHGRYLK $V%D
%H&G&R&U&X+J0R0Q1L3E6E6H7O9LQ=Q
Solid recovered fuels - Methods for the determination of the content of trace elements
(As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an
Spurenelementen (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
Combustibles solides de récupération - Méthodes pour la détermination de la teneur en
éléments traces (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V et Zn)
Ta slovenski standard je istoveten z: CEN/TS 15411:2006
ICS:
75.160.10 Trda goriva Solid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 15411
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
September 2006
ICS 75.160.10
English Version
Solid recovered fuels - Methods for the determination of the
content of trace elements (As, Ba, Be, Cd, Co, Cr, Cu, Hg, Mo,
Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
Combustibles solides de récupération - Méthodes pour la Feste Sekundärbrennstoffe - Verfahren zur Bestimmung
détermination de la teneur en éléments traces (As, Ba, Be, des Gehaltes an Spurenelementen (As, Ba, Be, Cd, Co, Cr,
Cd, Co, Cr, Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V et Zn) Cu, Hg, Mo, Mn, Ni, Pb, Sb, Se, Tl, V and Zn)
This Technical Specification (CEN/TS) was approved by CEN on 25 March 2006 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, 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 and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15411:2006: E
worldwide for CEN national Members.
Contents Page
Foreword.3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Safety remarks .6
5 Principle.6
6 Apparatus .6
7 Reagents.7
8 Procedure .8
9 Digestion procedure.8
10 Analysis of the digestion solutions .9
11 Expression of results .9
12 Quality control.10
13 Performance characteristics .10
14 Test report .10
Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis
of SRF .11
Bibliography .13
Foreword
This document (CEN/TS 15411:2006) has been prepared by Technical Committee CEN/TC 343 “Solid
Recovered Fuels”, the secretariat of which is held by SFS.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this CEN Technical Specification: Austria, Belgium, 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 and United Kingdom.
Introduction
Accurate determination of trace element content in solid recovered fuels is important for environmental and
technical reasons both in the production and combustion stage. After digestion of the solid recovered fuels
using different methods, a number of analytical techniques can be used for the quantification of the trace
element content. They include Inductively Coupled Plasma with optical or mass detection, graphite furnace
Atomic Absorption Spectrometry and, when available, dedicated specific method (e.g. for mercury).
1 Scope
This Technical Specification specifies three methods of digestion for solid recovered fuels:
a) microwave assisted digestion with hydrofluoric, nitric and hydrochloric acid mixture;
b) hot water bath digestion with hydrofluoric, nitric and hydrochloric acid mixture, after ashing of the SRFs
sample;
c) oven digestion with nitric, perchloric and hydrofluoric acid mixture.
Instrumental determination of As, Ba, Be, Cd, Cr, Co, Cu, Pb, Mn, Mo, Ni, Sb, Se, Tl, V, Zn is performed by
Inductively Coupled Plasma with optical or mass detection or graphite furnace Atomic Absorption
Spectrometry. Hg can be analysed only after the microwave assisted procedure or, alternatively, by a direct
analysis method.
The effectiveness of the digestion can be verified by qualitative X-ray fluorescence (XRF) analysis on the
remaining residue. If necessary an alternative digestion method (among those proposed) is used.
Method a) is recommended for general use, but the amount of the test portion can be very low in case of high
concentration of organic matter.
Method b) is recommended for SRFs with high organic matter concentration that can be difficult to digest with
the other methods. This method is not suitable for mercury.
Method c) is recommended for SRFs samples for which the other methods leave a significant insoluble
residue.
2 Normative references
The following referenced documents are indispensable for the application of this Technical Specification. For
dated references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
EN 13656, Characterization of waste — Microwave assisted digestion with hydrofluoric (HF), nitric (HNO )
and hydrochloric (HCI) acid mixture for subsequent determination of elements
CEN/TS 15357:2006, Solid recovered fuels — Terminology, definitions and descriptions
prCEN/TS 15403, Solid recovered fuels — Methods for the determination of the ash content
CEN/TS 15413, Solid recovered fuels — Methods for the preparation of the test sample from the laboratory
sample
prCEN/TS 15414-3, Solid recovered fuels — Determination of moisture content using the oven dry method —
Part 3: Moisture in general analysis sample
EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)
3 Terms and definitions
For the purposes of this Technical Specification, the terms and definitions given in CEN/TS 15357:2006 and
the following apply.
3.1
digestion
mineralization of the organic matter of a sample and dissolution of its mineral part, more or less completely,
when reacted with a reagent mixture
3.2
microwave unit
whole microwave digestion system (oven and associated equipment)
4 Safety remarks
The safety in handling of potentially hazardous materials is dealt with in relevant national and European
regulations, which every laboratory should refer to.
In addition the following information is given:
only experienced personnel can use the microwave apparatus, following the operating instructions
described in the manufacturer manual;
most of reagents used within this Technical Specification are strongly corrosive and toxic. Safety
precautions are absolutely necessary due to strong corrosive reagents, high temperature and high
pressure;
all procedures have to be performed in a hood or in closed force-ventilated equipment. By the use of
strong oxidising reagents the formation of explosive organic intermediates is possible especially when
dealing with samples with a high organic content. Do not open pressurised vessels before they have
cooled down. Avoid contact with the chemicals and the gaseous reaction products.
5 Principle
The test portion is digested using one of the proposed methods with a suitable acid mixture. The digested
sample is then analysed by the most appropriate spectrometric technique, such as atomic absorption or
emission spectroscopy.
6 Apparatus
6.1 Microwave unit
Intended for laboratory use and preferably equipped with temperature control.
6.2 Resistance heating oven
A resistance heated oven or heating block that can be used at a temperature of at least 220 °C and an
accuracy of ± 10 °C.
6.3 Digestion vessels
The vessels used in the microwave unit shall be equipped with a pressure relieve valve or another technical
equipment which avoids the bursting of the vessels at suddenly occurring excess pressure. The material of
the vessels has to be inert to the acids used for digestion. The digestion vessel shall withstand the pressure of
at least 8 bar. If the amount of organic carbon exceeds 100 mg it has to be ensured that the digestion vessel
is capable of withstanding higher pressures.
6.4 Inductively coupled plasma
Normal commercial instrumentation with optical or mass spectrometric detector (ICP-OES, ICP-MS).
6.5 Atomic absorption spectrophotometer
Normal commercial instrumentation, equipped with graphite furnace or hydride generation systems or cold
vapour (GF-AAS, HG-AAS, CV-AAS).
6.6 X-ray fluorescence spectrometer
Energy or wavelength dispersion system suitable for qualitative analysis of the elements listed in this
Technical Specification (with the exception of beryllium).
6.7 Balances
Analytical balance resolution ± 0,1 mg.
6.8 General equipment
General laboratory equipment, including volumetric graduated flasks and pipettes of adequate size.
Filter equipment of adequate chemical resistance and purity or centrifuge.
The use of glass ware shall be excluded when free hydrofluoric acid is present.
The glassware used in the digestion procedure should be carefully pre-cleaned with, for example, 10 % nitric
acid solution.
7 Reagents
All reagents shall be at least of analytical grade and suitable for their specific purposes.
Other specific reagents are listed and described in the reference methods for digestion or instrumental
determination listed in Clause 2.
NOTE Acids used in the preparation of standards and for sample processing are of high purity. Redistilled acids are
recommended because of the high sensitivity of ICP-MS. Nitric acid at less than 2 % (v/v) is recommended for ICP-MS to
minimize damage to the interface and to minimize isobaric molecular-ion interferences with the analytes. Many more
molecular-ion interferences are observed when hydrochloric and sulfuric acids are used.
7.1 Water of grade 1 as specified by EN ISO 3696:1995.
7.2 Nitric acid (HNO ), 65 % (w/w), ρ 1,40 g/ml.
7.3 Hydrofluoric acid (HF), 40 % (w/w), ρ 1,14 g/ml.
7.4 Perchloric acid (HClO ), 70 % (w/w), ρ 1,62 g/ml.
7.5 Hydrochloric acid (HCl), 65 % (w/w), ρ 1,40 g/ml.
8 Procedure
8.1 Sample conservation and pre-treatment
The laboratory samples shall be stored according to guidelines defined in Annex A.
It is advisable to contact the people performing the sampling in order to agree a procedure for the laboratory
sample preparation and storage before delivering to the laboratory. In particular, any treatment procedure
which can increase the temperature of the material above 40 °C should be avoided, in order to avoid
significant loss of mercury or other volatile compounds.
Furthermore any possible source of contamination during the laboratory sample preparation (e.g. grinding with
metallic appa
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