EN 13656:2002
(Main)Characterization of waste - Microwave assisted digestion with hydrofluoric (HF), nitric (HNO3) and hydrochloric (HCl) acid mixture for subsequent determination of elements
Characterization of waste - Microwave assisted digestion with hydrofluoric (HF), nitric (HNO3) and hydrochloric (HCl) acid mixture for subsequent determination of elements
This European Standard specifies methods of microwave assisted digestion with hydrofluoric (HF), nitric (HNO3)and hydrochloric (HCL) acid mixture. Solutions produced by the methods are suitable for analysis e.g.by atomic absorption spectometry (FLAAS,HGAAS,CVAAS,GFAAS), inductively coupled plasma emission spectometry(ICP-OES) and inductive coupled plasma mass spectometry(ICP-MS). The method is applicable to the microwave assisted acid digestion of waste for example for the following elements:Al,Sb,As,B,Ba,Be,Cd,Cr,Cu,Fe,Pb,Mg,Mn,Hg,Mo, Ni,P,K,Se,Ag,S,Na,Sr,Te,Ti,Tl,V,Zn.
Charakterisierung von Abfällen - Aufschluss mittels Mikrowellengerät mit einem Gemisch aus Fluorwasserstoffsäure (HF), Salpetersäure (HNO3) und Salzsäure (HCI) für die anschließende Bestimmung der Elemente im Abfall
Diese Norm legt Verfahren für den Aufschluß mittels Mikrowellengerät mit einem Gemisch aus Fluorwasserstoffsäure, Salpetersäure und Salzsäure fest. Die nach den Verfahren hergestellten Lösungen sind z.B. für Analysen mittels Flammen-Atomabsorptionsspektrometrie (FAAS), Hydrid-Atomabsorptions- spektrometrie (HGAAS), Kaltdampf-Atomabsorptionsspektrometrie (CVAAS), Graphitrohrofen-Atomabsorptionsspektrometrie (GFAAS), optischer Emissions- spektrometrie mit induktiv gekoppeltem Plasma (ICP-OES) und induktiv gekoppelterPlasma-Emission-Massenspektrometrie (ICP-MS) geeignet.
Caractérisation des déchets - Digestion assistée par micro-ondes avec un mélange d'acides fluorhydrique (HF), nitrique (HNO3) et chlorhydrique (HCI) pour la détermination ultérieure d'éléments contenus dans les déchets
La présente Norme européenne décrit des méthodes de digestion assistée par micro-ondes avec un mélange d'acides fluorhydrique (HF), nitrique (HNO3) et chlorhydrique (HCl). Les solutions produites par ces méthodes conviennent à l'analyse, par exemple par spectrométrie d'absorption atomique (FLAAS, HGAAS, CVAAS, GFAAS), spectrométrie d'émission par un plasma à couplage inductif (ICP-OES) et spectrométrie de masse par un plasma à couplage inductif (ICP-MS).
La méthode est applicable pour la digestion acide assistée par micro-ondes des déchets, par exemple pour les éléments suivants : Al, Sb, As, B, Ba, Be, Ca, Cd, Cr, Co, Cu, Fe, Pb, Mg, Mn, Hg, Mo, Ni, P, K, Se, Ag, S, Na, Sr, Sn, Te, Ti, Tl, V, Zn.
Karakterizacija odpadkov - Mikrovalovni razklop z zmesjo fluorovodikove (HF), klorovodikove (HCl) in dušikove(V) kisline (HNO3) za določanje elementov
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2004
.DUDNWHUL]DFLMDRGSDGNRY0LNURYDORYQLUD]NORS]]PHVMRIOXRURYRGLNRYH +)
NORURYRGLNRYH +&O LQGXãLNRYH 9 NLVOLQH +12 ]DGRORþDQMHHOHPHQWRY
Characterization of waste - Microwave assisted digestion with hydrofluoric (HF), nitric
(HNO3) and hydrochloric (HCl) acid mixture for subsequent determination of elements
Charakterisierung von Abfällen - Aufschluss mittels Mikrowellengerät mit einem Gemisch
aus Fluorwasserstoffsäure (HF), Salpetersäure (HNO3) und Salzsäure (HCI) für die
anschließende Bestimmung der Elemente im Abfall
Caractérisation des déchets - Digestion assistée par micro-ondes avec un mélange
d'acides fluorhydrique (HF), nitrique (HNO3) et chlorhydrique (HCI) pour la détermination
ultérieure d'éléments contenus dans les déchets
Ta slovenski standard je istoveten z: EN 13656:2002
ICS:
13.030.40 Naprave in oprema za Installations and equipment
odstranjevanje in obdelavo for waste disposal and
odpadkov treatment
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EUROPEAN STANDARD
EN 13656
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2002
ICS 13.030.40
English version
Characterization of waste - Microwave assisted digestion with
hydrofluoric (HF), nitric (HNO ) and hydrochloric (HCl) acid
mixture for subsequent determination of elements
Caractérisation des déchets - Digestion assistée par micro- Charakterisierung von Abfällen - Aufschluss mittels
ondes avec un mélange d'acides fluorhydrique (HF), Mikrowellengerät mit einem Gemisch aus
nitrique (HNO ) et chlorhydrique (HCI) pour la Fluorwasserstoffsäure (HF), Salpetersäure (HNO ) und
3 3
détermination ultérieure d'éléments contenus dans les Salzsäure (HCI) für die anschließende Bestimmung der
déchets Elemente im Abfall
This European Standard was approved by CEN on 19 August 2002.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, 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
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 13656:2002 E
worldwide for CEN national Members.
Contents
page
Foreword . 3
1 Scope. 5
2 Normative references . 5
3 Terms and definitions. 5
4 Safety remarks . 6
5 Sample. 6
5.1 Sample pre-treatment. 6
5.2 Mass of test portion . 7
6 Equipment. 7
6.1 Closed vessel system . 7
6.1.1 Microwave unit. 7
6.1.2 Digestion vessels . 7
6.2 Semi-open vessel system. 7
6.2.1 Microwave unit. 7
6.2.2 Digestion vessels . 8
6.3 General equipment . 8
7 Reagents . 8
8 Interferences and sources of error . 8
8.1 General informations . 8
8.2 Closed vessel system . 9
8.3 Semi-open vessel system. 9
9 Procedure. 9
9.1 Blank test . 9
9.2 Procedure for closed vessels. 9
9.2.1 Amount of samples and reagents. 10
9.2.2 Digestion. 10
9.2.3 Complexation of HF. 10
9.2.4 Preparation of the solution for analysis . 10
9.3 Procedure for semi-open vessels . 11
9.3.1 Amount of samples. 11
9.3.2 Digestion and complexation of HF . 11
9.3.3 Preparation of the solution for analysis . 11
10 Test report. 12
Annex A (normative) Calibration of the power adjustment. 13
Annex B (informative) Validation. 14
Bibliography. 25
Foreword
This document EN 13656:2002 has been prepared by Technical Committee CEN/TC 292 "Characterization of
waste", 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 2003, and conflicting national standards shall be withdrawn at the latest
by April 2003.
In this European Standard the annex A is normative and the annexe B is informative.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark,
Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,
Spain, Sweden, Switzerland and the United Kingdom.
Introduction
The purpose of the method is to bring the elements to be determined in many types of waste into solution to
provide a rapid digestion for analysis. Elements extractable by this procedure can in many instances be described
as „total“. On another hand they cannot be regarded as available for leaching, as the extraction procedure is too
vigorous to represent natural processes.
1 Scope
This European Standard specifies methods of microwave assisted digestion with hydrofluoric (HF), nitric (HNO )
and hydrochloric (HCl) acid mixture. Solutions produced by the methods are suitable for analysis e.g. by atomic
absorption spectrometry (FLAAS, HGAAS, CVAAS, GFAAS), inductively coupled plasma emission spectrometry
(ICP-OES) and inductive coupled plasma mass spectrometry (ICP-MS).
The method is applicable to the microwave assisted acid digestion of waste for example for the following
elements: Al, Sb, As, B, Ba, Be, Ca, Cd, Cr, Co, Cu, Fe, Pb, Mg, Mn, Hg, Mo, Ni, P, K, Se, Ag, S, Na, Sr, Sn, Te,
Ti, Tl, V, Zn.
2 Normative references
This European Standard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
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 European Standard, the following terms and definitions 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
sample
portion of material selected from a larger quantity of material
[ENV 12506:2001]
3.3
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
[ENV 12506:2001]
3.4
test sample; analytical sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or analysis
[ENV 12506:2001]
3.5
test portion; analytical portion
quantity of material of proper size for measurement of the concentration or other properties of interest, removed
from the test sample
[ENV 12506:2001]
NOTE 1 The test portion may be taken from the laboratory sample directly if no preparation of sample is required (e.g. with
liquids), but usually it is taken from the prepared test sample.
NOTE 2 A unit or increment of proper homogeneity, size and fineness, needing no further preparation, may be a test portion.
3.6
dry residue
dry matter expressed as a percentage by mass after drying at 105 °C ± 5 °C to the constancy of weight
3.7
digestion vessel
special flask where the test portion and the acid mixture are filled in and the digestion is performed
3.8
microwave unit
whole microwave digestion system (oven and associated equipment)
3.9
microwave unit cavity
inner part of the microwave unit in which the digestion vessel is located and the microwave digestion is performed
3.10
focused microwave unit
microwave unit in which a precise control of the electric field is made by using a wave guide
NOTE Microwaves are focused at the bottom part of the digestion vessel.
4 Safety remarks
All this work has to be performed by skilled persons.
The reagents used within this European Standard are strongly corrosive and partly very 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. Samples and solutions have to be disposed of
according to regulations.
People performing the test shall be informed on the specific risk of HF.
5 Sample
5.1 Sample pre-treatment
The test portion should be transferred into the vessel as it is without any pre-treatment if possible.This is
applicable only if the test portion is representative for the laboratory sample and the effectiveness of the digestion
is proven.
If these conditions are not met a pre-treatment of the laboratory sample is necessary. This procedure shall not
change the concentration of the elements of interest.
NOTE Pr
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