SIST EN 62321-4:2014
(Main)Determination of certain substances in electrotechnical products - Part 4: Determination of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS
Determination of certain substances in electrotechnical products - Part 4: Determination of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS
EN-IEC 62321-4 describes test methods for mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS. This standard specifies the determination of the levels of mercury (Hg) contained in electrotechnical products. These materials are polymers, metals and electronics (e.g. printed wiring boards, cold cathode fluorescent lamps, mercury switches). Batteries containing Hg should be handled as described in [1]1. The interlaboratory study has only evaluated these test methods for plastics, other matrices were not covered. This standard refers to the sample as the object to be processed and measured. What the sample is or how to get to the sample is defined by the entity carrying out the tests. Further guidance on obtaining representative samples from finished electronic products to be tested for levels of regulated substances may be found in IEC 62321-2. It is noted that the selection and/or determination of the sample may affect the interpretation of the test results. This standard describes the use of four methods, namely CV-AAS (cold vapour atomic absorption spectrometry), CV-AFS (cold vapour atomic fluorescence spectrometry) ICP-OES (inductively coupled plasma optical emission spectrometry), and ICP-MS (inductively coupled plasma mass spectrometry) as well as several procedures for preparing the sample solution from which the most appropriate method of analysis can be selected by experts. Analysis by CV-AAS, CV-AFS, ICP-OES and ICP-MS allows the determination of the target element, mercury, with high precision (uncertainty in the low per cent range) and/or high sensitivity (down to the μg/kg level). The test procedures described in this standard are intended to provide the highest level of accuracy and precision for concentrations of mercury in the range from 4 mg/kg to 1 000 mg/kg. The procedures are not limited for higher concentrations. For direct analysis, using thermal decomposition-gold amalgamation in conjunction with CV-AAS (TD(G)-AAS) can be also applied for mercury analysis without sample digestion, although the detection limits are higher than other methods due to the reduced sample size.
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 4: Bestimmung von Quecksilber in Polymeren, Metallen und Elektronik mit CV-AAS, CV-AFS, ICP-OES und ICP-MS
Détermination de certaines substances dans les produits électrotechniques - Partie 4: Détermination du mercure dans les polymères, métaux et produits électroniques part CV-AAS, CV-AFS, ICP-OES et ICP-MS
La CEI 62321-4:2013 décrit l'utilisation de quatre méthodes d'essai pour le mercure dans les polymères, à savoir CV-AAS (spectrométrie d'absorption atomique à vapeur froide), CV-AFS (spectrométrie de fluorescence atomique à vapeur froide, cold vapour atomic fluorescence spectrometry), ICP-OES (spectrométrie d'émission optique couplée à un plasma induit) et ICP-MS (spectrométrie de masse couplée à un plasma induit), ainsi que plusieurs procédures de préparation de la solution d'échantillon à partir de laquelle les experts peuvent choisir la méthode d'analyse la plus appropriée.
Določevanje posameznih snovi v elektrotehničnih izdelkih - 4. del: Določevanje živega srebra v polimerih, kovinah in elektroniki s CV-AAS, CV-AFS, ICP-OES in ICP-MS (IEC 62321-4:2013)
Standard 62321-4 opisuje preskusne metode za določanje živega srebra v polimerih, kovinah in elektroniki z metodami: atomska absorpcijska spektrometrija hladnih par (CV-AAS), atomska fluorescentna spektrometrija hladnih par (CV-AFS), optična emisijska spektrometrija z induktivno sklopljeno plazmo (ICP-OES) in masna spektrometrija z induktivno sklopljeno plazmo (ICP-MS). Ta standard opisuje določanje vsebnosti živega srebra (Hg) v elektrotehničnih izdelkih. Ti materiali so polimeri, kovine in elektronika (npr. plošče s tiskanim vezjem, hladnokatodne fluorescentne luči, živosrebrova stikala). Z baterijami, ki vsebujejo Hg, je treba ravnati, kot je opisano v [1]1. Medlaboratorijska študija je ocenila le te preskusne metode za plastiko. Druge matrice niso zajete. Ta standard se nanaša na vzorec kot predmet, ki se obdela in meri. Kaj ta vzorec je ali kako ga pridobiti, določa subjekt, ki izvaja preskuse. Dodatna navodila o pridobivanju reprezentativnih vzorcev iz končnih elektronskih izdelkov za testiranje ravni reguliranih snovi je mogoče najti v standardu IEC 62321-2. Opozoriti je treba, da lahko izbira in/ali določanje vzorca vpliva na razlago rezultatov preskusa. Ta standard opisuje uporabo štirih metod, in sicer CV-AAS (atomska absorpcijska spektrometrija hladnih par), CV-AFS (atomska fluorescentna spektrometrija hladnih par), ICP-OES (optična emisijska spektrometrija z induktivno sklopljeno plazmo) in ICP-MS (masna spektrometrija z induktivno sklopljeno plazmo), kot tudi več postopkov za pripravo vzorčne raztopine, s pomočjo katere lahko strokovnjaki izberejo najbolj primerno metodo analize. Analiza z metodami CV-AAS, CV-AFS, ICP-OES in ICP-MS omogoča določitev ciljnega elementa živega srebra z visoko natančnostjo (negotovost v nizkoodstotnem območju) in/ali visoko občutljivostjo (do ravni μg/kg). Testni postopki, opisani v tem standardu, so namenjeni zagotavljanju najvišje stopnje pravilnosti in natančnosti za vsebnosti živega srebra v območju od 4 mg/kg do 1000 mg/kg. Postopki se lahko uporabljajo tudi za višje koncentracije. Za neposredno analizo se lahko uporabi tudi toplotna razgradnja-amalgamiranje zlata v povezavi s CV-AAS (TD(G)-AAS) za analizo živega srebra brez prebave vzorca, čeprav so meje zaznavanja višje kot pri drugih postopkih zaradi zmanjšane velikosti vzorca.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 62321-4:2014
01-junij-2014
1DGRPHãþD
SIST EN 62321:2009
'RORþHYDQMHSRVDPH]QLKVQRYLYHOHNWURWHKQLþQLKL]GHONLKGHO 'RORþHYDQMH
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Determination of certain substances in electrotechnical products - Part 4: Determination
of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-
MS
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik
- Teil 4: Bestimmung von Quecksilber in Polymeren, Metallen und Elektronik mit CV-
AAS, CV-AFS, ICP-OES und ICP-MS
Détermination de certaines substances dans les produits électrotechniques - Partie 4:
Détermination du mercure dans les polymères, métaux et produits électroniques part CV
-AAS, CV-AFS, ICP-OES et ICP-MS
Ta slovenski standard je istoveten z: EN 62321-4:2014
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
SIST EN 62321-4:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 62321-4:2014
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SIST EN 62321-4:2014
EUROPEAN STANDARD
EN 62321-4
NORME EUROPÉENNE
April 2014
EUROPÄISCHE NORM
ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially)
English version
Determination of certain substances in electrotechnical products -
Part 4: Mercury in polymers, metals and electronics by CV-AAS, CV-AFS,
ICP-OES and ICP-MS
(IEC 62321-4:2013)
Détermination de certaines substances Verfahren zur Bestimmung von
dans les produits électrotechniques - bestimmten Substanzen in Produkten der
Partie 4: Mercure dans les polymères, Elektrotechnik -
métaux et produits électroniques par CV- Teil 4: Quecksilber in Polymeren, Metallen
AAS, CV-AFS, ICP-OES et ICP-MS und Elektronik mit CV-AAS, CV-AFS, ICP-
(CEI 62321-4:2013) OES und ICP-MS
(IEC 62321-4:2013)
This European Standard was approved by CENELEC on 2013-11-15. CENELEC 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 CEN-CENELEC Management Centre or to any CENELEC 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 CENELEC member into its own language and notified
to the CEN-CENELEC Management Centre has the same status as the official versions.
CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus,
the Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
CENELEC
European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für Elektrotechnische Normung
CEN-CENELEC Management Centre: Avenue Marnix 17, B - 1000 Brussels
© 2014 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.
Ref. No. EN 62321-4:2014 E
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SIST EN 62321-4:2014
EN 62321-4:2014 - 2 -
Foreword
The text of document 111/299/FDIS, future edition 1 of IEC 62321-4, prepared by IEC/TC 111
"Environmental standardization for electrical and electronic products and systems" was submitted to the
IEC-CENELEC parallel vote and approved by CENELEC as EN 62321-4:2014.
The following dates are fixed:
(dop) 2014-10-25
• latest date by which the document has
to be implemented at national level by
publication of an identical national
standard or by endorsement
(dow) 2016-11-15
• latest date by which the national
standards conflicting with the
document have to be withdrawn
EN 62321-4:2014 is a partial replacement of EN 62321:2009, forming a structural revision and replacing
Clause 7 and Annex E.
Future parts in the EN 62321 series will gradually replace the corresponding clauses in EN 62321:2009.
Until such time as all parts are published, however, EN 62321:2009 remains valid for those clauses not
yet re-published as a separate part.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CENELEC [and/or CEN] shall not be held responsible for identifying any or all such patent
rights.
Endorsement notice
The text of the International Standard IEC 62321-4:2013 was approved by CENELEC as a European
Standard without any modification.
In the official version, for Bibliography, the following note has to be added for the standard indicated:
IEC 62321-5 NOTE Harmonised as EN 62321-5.
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Annex ZA
(normative)
Normative references to international publications
with their corresponding European publications
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.
NOTE When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD
applies.
Publication Year Title EN/HD Year
IEC 62321-1 - Determination of certain substances in EN 62321-1 -
electrotechnical products -
Part 1: Introduction and overview
IEC 62321-2 - Determination of certain substances in EN 62321-2 -
electrotechnical products -
Part 2: Disassembly, disjunction and
mechanical sample preparation
IEC 62321-3-1 - Determination of certain substances in EN 62321-3-1 -
electrotechnical products -
Part 3-1: Screening electrotechnical products
for lead, mercury, cadmium, total chromium
and total bromine using X-ray Fluorescence
Spectrometry
IEC 62554 - Sample preparation for measurement of EN 62554 -
mercury level in fluorescent lamps
ISO 3696 - Water for analytical laboratory use - EN ISO 3696 -
Specification and test methods
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SIST EN 62321-4:2014
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SIST EN 62321-4:2014
IEC 62321-4
®
Edition 1.0 2013-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
Determination of certain substances in electrotechnical products –
Part 4: Mercury in polymers, metals and electronics
by CV-AAS, CV-AFS, ICP-OES and ICP-MS
Détermination de certaines substances dans les produits électrotechniques –
Partie 4: Mercure dans les polymères, métaux et produits électroniques par
CV-AAS, CV-AFS, ICP-OES et ICP-MS
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
PRICE CODE
INTERNATIONALE
CODE PRIX U
ICS 13.020; 43.040.10 ISBN 978-2-83220-841-0
Warning! Make sure that you obtained this publication from an authorized distributor.
Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.
® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
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SIST EN 62321-4:2014
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CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions and abbreviations . 8
3.1 Terms and definitions . 8
3.2 Abbreviations . 9
4 Reagent and materials. 9
4.1 General . 9
4.2 Reagents . 9
4.3 Materials . 11
5 Apparatus . 11
5.1 General . 11
5.2 Apparatus . 11
6 Sampling and test portion . 12
7 Procedure. 12
7.1 Wet digestion (digestion of electronics) . 12
7.2 Microwave digestion . 13
7.3 Thermal decomposition-gold amalgamation system . 13
7.4 Preparation of reagent blank solution . 14
8 Calibration . 14
8.1 General . 14
8.2 Development of the calibration curve . 14
8.3 Measurement of the sample . 15
9 Calculation . 15
10 Precision . 16
11 Quality assurance and control . 16
11.1 General . 16
11.2 Limits of detection (LOD) and limits of quantification (LOQ) . 17
Annex A (informative) Practical application of determination of mercury in polymers,
metals and electronics by CV-AAS, AFS, ICP-OES and ICP-MS . 19
Annex B (informative) Results of international interlaboratory study Nos. 2 (IIS2) and
4A (IIS 4A) . 24
Bibliography . 25
Figure A.1 – Heating digester equipped with reaction vessel, reflux cooler and
absorption vessel . 19
Figure A.2 – Configuration of equipment with AAS (example) . 20
Figure A.3 – Mercury collecting tube (example) . 21
Figure A.4 – Configuration (example) of the thermal decomposition/atomic absorption
spectrometer for CCFL. 22
Table 1 – Repeatability and reproducibility . 16
Table 2 – Acceptance criteria of items for the quality control . 17
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Table 3 – Method detection limit = t × s . 18
n–1
Table A.1 – Program for microwave digestion (example) of samples (power output for
five vessels). 20
Table B.1 – Statistical data for TD(G)-AAS . 24
Table B.2 – Statistical data for CV-AAS . 24
Table B.3 – Statistical data for CV-AFS . 24
Table B.4 – Statistical data for ICP-OES . 24
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INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 4: Mercury in polymers, metals and electronics
by CV-AAS, CV-AFS, ICP-OES and ICP-MS
FOREWORD
1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising
all national electrotechnical committees (IEC National Committees). The object of IEC is to promote
international co-operation on all questions concerning standardization in the electrical and electronic fields. To
this end and in addition to other activities, IEC publishes International Standards, Technical Specifications,
Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC
Publication(s)”). Their preparation is entrusted to technical committees; any IEC National Committee interested
in the subject dealt with may participate in this preparatory work. International, governmental and non-
governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely
with the International Organization for Standardization (ISO) in accordance with conditions determined by
agreement between the two organizations.
2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international
consensus of opinion on the relevant subjects since each technical committee has representation from all
interested IEC National Committees.
3) IEC Publications have the form of recommendations for international use and are accepted by IEC National
Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC
Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any
misinterpretation by any end user.
4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications
transparently to the maximum extent possible in their national and regional publications. Any divergence
between any IEC Publication and the corresponding national or regional publication shall be clearly indicated in
the latter.
5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity
assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any
services carried out by independent certification bodies.
6) All users should ensure that they have the latest edition of this publication.
7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and
members of its technical committees and IEC National Committees for any personal injury, property damage or
other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and
expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC
Publications.
8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is
indispensable for the correct application of this publication.
9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of
patent rights. IEC shall not be held responsible for identifying any or all such patent rights.
International Standard IEC 62321-4 has been prepared by IEC technical committee 111:
Environmental standardization for electrical and electronic products and systems.
The first edition of IEC 62321:2008 was a 'stand alone' standard that included an Introduction,
an overview of test methods, a mechanical sample preparation as well as various test method
clauses.
This first edition of IEC 62321-4 is a partial replacement of IEC 62321, forming a structural
revision and replacing Clause 7 and Annex E.
Future parts in the IEC 62321 series will gradually replace the corresponding clauses in
IEC 62321:2008. Until such time as all parts are published, however, IEC 62321:2008 remains
valid for those clauses not yet re-published as a separate part.
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SIST EN 62321-4:2014
62321-4 © IEC:2013 – 5 –
The text of this standard is based on the following documents:
FDIS Report on voting
111/299/FDIS 111/309/RVD
Full information on the voting for the approval of this standard can be found in the report on
voting indicated in the above table.
This publication has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 62321 series can be found on the IEC website under the general
title: Determination of certain substances in electrotechnical products
The committee has decided that the contents of this publication will remain unchanged until
the stability date indicated on the IEC web site under "http://webstore.iec.ch" in the data
related to the specific publication. At this date, the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
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SIST EN 62321-4:2014
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INTRODUCTION
The widespread use of electrotechnical products has drawn increased attention to their impact
on the environment. In many countries this has resulted in the adaptation of regulations
affecting wastes, substances and energy use of electrotechnical products.
The use of certain substances (e.g. lead (Pb), cadmium (Cd) and polybrominated diphenyl
ethers (PBDEs)) in electrotechnical products, is a source of concern in current and proposed
regional legislation.
The purpose of the IEC 62321 series is therefore to provide test methods that will allow the
electrotechnical industry to determine the levels of certain substances of concern in
electrotechnical products on a consistent global basis.
WARNING – Persons using this International Standard should be familiar with normal
laboratory practice. This standard 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.
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62321-4 © IEC:2013 – 7 –
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 4: Mercury in polymers, metals and electronics
by CV-AAS, CV-AFS, ICP-OES and ICP-MS
1 Scope
This part of IEC 62321 describes test methods for mercury in polymers, metals and
electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS.
This standard specifies the determination of the levels of mercury (Hg) contained in
electrotechnical products. These materials are polymers, metals and electronics (e.g. printed
wiring boards, cold cathode fluorescent lamps, mercury switches). Batteries containing Hg
1
should be handled as described in [1] . The interlaboratory study has only evaluated these
test methods for plastics, other matrices were not covered.
This standard refers to the sample as the object to be processed and measured. What the
sample is or how to get to the sample is defined by the entity carrying out the tests. Further
guidance on obtaining representative samples from finished electronic products to be tested
for levels of regulated substances may be found in IEC 62321-2. It is noted that the selection
and/or determination of the sample may affect the interpretation of the test results.
This standard describes the use of four methods, namely CV-AAS (cold vapour atomic
absorption spectrometry), CV-AFS (cold vapour atomic fluorescence spectrometry) ICP-OES
(inductively coupled plasma optical emission spectrometry), and ICP-MS (inductively coupled
plasma mass spectrometry) as well as several procedures for preparing the sample solution
from which the most appropriate method of analysis can be selected by experts.
Analysis by CV-AAS, CV-AFS, ICP-OES and ICP-MS allows the determination of the target
element, mercury, with high precision (uncertainty in the low per cent range) and/or high
sensitivity (down to the µg/kg level). The test procedures described in this standard are
intended to provide the highest level of accuracy and precision for concentrations of mercury
in the range from 4 mg/kg to 1 000 mg/kg. The procedures are not limited for higher
concentrations.
For direct analysis, using thermal decomposition-gold amalgamation in conjunction with
CV-AAS (TD(G)-AAS) can be also applied for mercury analysis without sample digestion,
although the detection limits are higher than other methods due to the reduced sample size.
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.
IEC 62321-1, Determination of levels of certain substances in electrotechnical products –
Part 1: Introduction and overview
______________
1
Figures in square brackets refer to the bibliography.
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IEC 62321-2, Determination of levels of certain substances in electrotechnical products –
2
Part 2: Disassembly, disjointment and mechanical sample preparation
IEC 62321-3-1, Determination of certain substances in electrotechnical products – Part 3-1:
Screening – Lead, mercury, cadmium, total chromium and total bromine by X-ray fluorescence
spectrometry
IEC 62554, Sample preparation for measurement of mercury level in fluorescent lamps
ISO 3696, Water for analytical laboratory use – Specification and test methods
3 Terms, definitions and abbreviations
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in IEC 62321-1 as well as
the following, apply.
3.1.1
accuracy
closeness of agreement between a test result and an accepted reference value
3.1.2
blank calibration solution
calibration solution without analyte
3.1.3
calibration standard
substance in solid or liquid form with known and stable concentration(s) of the analyte(s) of
interest used to establish instrument response (calibration curve) with respect to analyte(s)
concentration(s)
3.1.4
calibration solution
solution used to calibrate the instrument prepared either from (a) stock solution(s) or from a
(certified) reference material
3.1.5
certified reference material
reference material, accompanied by documentation issued by an authoritative body and
providing one or more specified property values with associated uncertainties and
traceabilities using valid precedures
3.1.6
laboratory control sample
known matrix spiked with compound(s) representative of the target analytes, used to
document laboratory performance
[SOURCE: US EPA SW-846] [2]
3.1.7
reagent blank solution
prepared by adding to the solvent the same amounts of reagents as those added to the test
sample solution (same final volume)
______________
2
To be published.
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62321-4 © IEC:2013 – 9 –
3.1.8
stock solution
solution with accurately known analyte concentartion(s), prepared from “pure chemicals”
3.1.9
test portion
quantity of material drawn from the test sample (or from the laboratory sample if both are the
same) and on which the test or observation is actually carried out
[SOURCE ISO 6206:1979] [3]
3.1.10
test sample solution
solution prepared with the test portion of the test sample according to the appropriate
specifications such that it can be used for the envisaged measurement
3.2 Abbreviations
CRM Certified reference material
CCFL Cold cathode fluorescent lamp
CCV Continuing calibration verification
CV-AAS Cold vapour atomic absorption spectrometry
CV-AFS Cold vapour atomic fluorescence spectrometry
LCS Laboratory control sample
LOD Limits of detection
LOQ Limits of quantification
MDL Method detection limit
TD(G)-AAS Thermal decomposition – Gold amalgamation – Atomic absorption spectrometry
NOTE TD(G)-AAS is commonly referred to as a direct mercury analysis or DMA technique.
4 Reagent and materials
4.1 General
For the determination of elements at trace level, the reagents shall be of adequate purity.
Contamination can be a major source of error when working in the 1 ng range with the
instruments. Cautious handling of the apparatus and careful technique will minimize this
problem. Therefore, only grade 1 water (4.2 a) shall be used. Care shall be taken that all
materials in contact with the water are Hg-free.
Chemicals used for sample preparation can be a major source of contamination. Only
reagents that are mercury-free shall be used. It is therefore highly recommended that the
blank values of the reducing agents and the other chemicals be measured before using them
for sample preparation.
4.2 Reagents
The following reagents are used:
a) Water: Grade 1, as defined in ISO 3696, shall be used for preparation and dilution of all
sample solutions.
b) Nitric acid (concentrated nitric acid): ρ(HNO ) = 1,4 g/ml , a mass fraction of 65 %, trace
3
metal grade.
c) Nitric acid, a mass fraction of 50 %, trace metal grade.
d) Nitric acid, 0,5 mol/l, trace metal grade.
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SIST EN 62321-4:2014
– 10 – 62321-4 © IEC:2013
e) Nitric acid, a mass fraction of 1 %, trace metal grade.
f) Nitric acid, a mass fraction of 1,5 %, trace metal grade.
g) Nitric acid, a mass fraction of 5 % , trace metal grade.
h) Fluoroboric acid: HBF a mass fraction of 50 %, trace metal grade (for microwave
4,
digestion).
i) Hydrogen peroxide: H O a mass fraction of 30 %, trace metal grade (for microwave
2 2,
digestion).
j) Stock solution with 1 000 mg/L of mercury, trace metal grade.
k) Potassium tetrahydridoborate (potassium borohyride): KBH , trace metal grade.
4
l) Potassium permanganate: KMnO , a mass fraction of 5 % solution, trace metal grade.
4
Dissolve 5 g of potassium permanganate in 100 ml of water (4.2 a).
m) Sodium tetrahydridoborate (sodium borohydride), NaBH , trace metal grade.
4
n) Sodium hydroxide, NaOH trace metal grade.
o) Hydrogen tetrachloroaurate (Ⅲ) tetra hydrate, HAuCl ･ 4H2O trace metal grade.
4
p) Internal standard stock solution, trace metal grade:
– Internal standard elements that do not interfere with the target element are used for
ICP-OES and ICP-MS. Also, the presence of these internal standard elements in the
sample solution shall be at negligible levels. Sc, In, Tb, Lu, Re, Rh, Bi and Y may be
used as internal standard elements.
– For use with ICP-OES, Sc or Y is recommended. The recommended concentration is
1 000 mg/L.
– For use with ICP-MS, Rh is recommended. The recommended concentration is
1 000 µg/l.
q) Reducing agent for CV-AAS: a mass fraction of 3 % NaBH in a mass fraction of 1 %
4
NaOH.
Dissolve 10,0 g sodium hydroxide (4.2 n) into approximately 700 ml of water (4.2 a) in a
beaker and stir until dissolved. Add 30,0 g of sodium tetrahydridoborate powder (4.2 m)
into the beaker and stir until dissolved. Finally transfer to a 1 l volumetric flask and fill up
to the mark with water (4.2 a) and filter. Prepare daily.
Reductant solution containing sodium t
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