SIST ENV 14138:2004

Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation by co-precipitation

This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-ES) for the determination of elements at low content in lead for the ranges given in Table 1.
Higher contents than those listed in Table 1 should be determined according to ENV 13800.
These methods are intended as the definitive methods in case of dispute for the determination of elements at low content in lead. They are also recommended for the analysis of Certified Reference Materials (CRM) and Reference Materials (RM) which are used in analysis according to ENV 12908.

Blei und Bleilegierungen - Analyse durch Flammen-Atomabsorptionsspektrometrie (FAAS) oder Emission-Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES), nach Abtrennung durch Mitfällung

Diese Europäische Vornorm legt ein flammen-atomabsorptionsspektrometrisches Verfahren (FAAS) und ein emissionsspektrometrisches Verfahren mit induktiv gekoppeltem Plasma (ICP-ES) für die Bestimmung niedriger Elementgehalte in Blei fest, deren Bereiche in Tabelle 1 gegeben sind.
Höhere Gehalte als die in Tabelle 1 angegebenen, sollten nach ENV 13800 bestimmt werden.
Diese Verfahren sind vorgesehen als Schiedsverfahren im Falle von Streitigkeiten für die Bestimmung von niedrigen Elementgehalten in Blei. Sie werden ebenfalls empfohlen für die Analyse von zertifizierten Referenzmaterialien (ZRM) und Referenzmaterialien (RM), welche in der Analytik entsprechend ENV 12908 eingesetzt werden.

Plomb et alliages de plomb - Analyse par spectrométrie d'absorption atomique dans la flamme (FAAS) ou par spectrométrie d'émission a plasma inductif couplé (ICP-ES), apres séparation par co-précipitation

Svinec in svinčeve zlitine – Analiza s plamensko atomsko absorpcijsko spektrometrijo (FAAS) ali emisijsko spektrometrijo z induktivno sklopljeno plazmo (IC-ES) po ločenju elementov s soobarjanjem

General Information

• Status: Published
• Publication Date: 31-Dec-2003
• ICS: 77.120.60 - Lead, zinc, tin and their alloys
• Technical Committee: INEK - Nonferrous metals
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Jan-2004
• Due Date: 01-Jan-2004
• Completion Date: 01-Jan-2004
• Ref Project: ENV 14138:2001 - Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation by co-precipitation

Standards Content (Sample)

SLOVENSKI STANDARD
SIST ENV 14138:2004
01-januar-2004
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VSHNWURPHWULMR)$$6DOLHPLVLMVNRVSHNWURPHWULMR]LQGXNWLYQRVNORSOMHQRSOD]PR
,&(6SRORþHQMXHOHPHQWRYVVRREDUMDQMHP
Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or
inductively coupled plasma emission spectrometry (ICP-ES), after separation by co-
precipitation
Blei und Bleilegierungen - Analyse durch Flammen-Atomabsorptionsspektrometrie
(FAAS) oder Emission-Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES), nach
Abtrennung durch Mitfällung
Plomb et alliages de plomb - Analyse par spectrométrie d'absorption atomique dans la
flamme (FAAS) ou par spectrométrie d'émission a plasma inductif couplé (ICP-ES),
apres séparation par co-précipitation
Ta slovenski standard je istoveten z: ENV 14138:2001
ICS:
77.120.60 Svinec, cink, kositer in Lead, zinc, tin and their
njihove zlitine alloys
SIST ENV 14138:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ENV 14138:2004

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SIST ENV 14138:2004
EUROPEAN PRESTANDARD
ENV 14138
PRÉNORME EUROPÉENNE
EUROPÄISCHE VORNORM
December 2001
ICS 77.120.60
English version
Lead and lead alloys - Analysis by flame atomic absorption
spectrometry (FAAS) or inductively coupled plasma emission
spectrometry (ICP-ES), after separation by co-precipitation
Plomb et alliages de plomb - Analyse par spectrométrie Blei und Bleilegierungen - Analyse durch Flammen-
d'absorption atomique dans la flamme (FAAS) ou par Atomabsorptionsspektrometrie (FAAS) oder Emission-
spectrométrie d'émission à plasma inductif couplé (ICP- Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES),
ES), après séparation par co-précipitation nach Abtrennung durch Mitfällung
This European Prestandard (ENV) was approved by CEN on 18 November 2001 as a prospective standard for provisional application.
The period of validity of this ENV 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 ENV can be converted into a European Standard.
CEN members are required to announce the existence of this ENV in the same way as for an EN and to make the ENV available promptly
at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the ENV) until the final
decision about the possible conversion of the ENV into an EN is reached.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, 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
© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. ENV 14138:2001 E
worldwide for CEN national Members.

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SIST ENV 14138:2004
ENV 14138:2001 (E)
Contents
page
Foreword.4
1 Scope .5
2 Normative references .5
3 Principle.5
3.1 Preparation of the test solution.5
3.2 Instrumental techniques .6
3.2.1 Flame atomic absorption spectrometry (FAAS) .6
3.2.2 Inductively coupled plasma emission spectrometry (ICP-ES).6
4 Apparatus .6
4.1 General.6
4.2 Volumetric glassware .6
4.3 Filtration system .6
4.4 Instruments.6
4.4.1 Flame atomic absorption spectrometer .6
4.4.2 Inductively coupled plasma emission spectrometer .7
5 Reagents.7
5.1 General.7
5.2 Nitric acid (HNO ) .7
3
5.2.1 Concentrated nitric acid.7
5.2.2 Nitric acid 1:1 (V/V) .7
5.2.3 Nitric acid 1:2 (V/V) .7
5.3 Hydrochloric acid (HCl) .7
5.3.1 Concentrated hydrochloric acid.7
5.3.2 Hydrochloric acid 1:1 (V/V) .7
5.4 Ammonia solution.7
5.5 Pure lead.7
5.6 Manganese nitrate solution .8
5.7 Potassium permanganate solution .8
5.8 Standard solutions .8
5.8.1 Standard solutions (1g/l).8
5.8.2 Standard solutions (100 mg/l).8
5.8.3 Standard solutions (10 mg/l).9
5.8.4 Multi-element solutions (either 10 mg/l or 100 mg/l).9
6 Sampling and sample preparation .9
7 Procedure .9
7.1 Preparation of the test solution.9
7.1.1 Dissolution.9
7.1.2 Co-precipitation with manganese dioxide.9
7.1.3 Test solution.9
7.2 Preparation of the synthetic test solution.9
7.3 Preparation of the blank test solution .10
7.4 Preparation of calibration solutions .10
8 Determination of elements by FAAS.10
8.1 General.10
8.2 Calibration and measurement of the test solution.11
8.3 Expression of results .11
8.3.1 Analyte recovery rate .11
8.3.2 Analyte content in the sample.11
9 Determination of elements by ICP-ES .12
9.1 General.12
9.2 Calibration and measurement of the test solution.12
2

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SIST ENV 14138:2004
ENV 14138:2001 (E)
9.3 Expression of results .13
9.3.1 Analyte recovery rate .13
9.3.2 Analyte content in the sample.13
10 Test report .13
Bibliography .14
3

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SIST ENV 14138:2004
ENV 14138:2001 (E)
Foreword
This European Prestandard has been prepared by Technical Committee CEN /TC 306, "Lead and lead alloys", the
secretariat of which is held by AFNOR.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this European Prestandard: Austria, Belgium, Czech Republic, Denmark, Finland,
France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden,
Switzerland and the United Kingdom.
CAUTION FOR SAFETY AND TRAINING
The methods in this Prestandard are recommended for the certification of reference materials and as umpire
methods in cases of a dispute. The importance of either application, and the paramount issue of safety, requires
that they should only be carried out by fully-trained analysts who are experienced in all relevant techniques and the
precautions necessary in the inherently hazardous environs of a laboratory, especially those required when using
particularly hazardous apparatus and reagents used in some of these methods.
Where a particular hazard exists, this is given as a DANGER adjacent to the point in the text where the apparatus
or reagent is referenced.
4

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SIST ENV 14138:2004
ENV 14138:2001 (E)
1 Scope
This European Prestandard specifies methods using flame atomic absorption spectrometry (FAAS) and inductively
coupled plasma emission spectrometry (ICP-ES) for the determination of elements at low content in lead for the
ranges given in Table 1.
Higher contents than those listed in Table 1 should be determined according to ENV 13800.
Table 1 — Ranges of application for the determination of elements
Element Ranges of applications
(% m/m)
FAAS ICP-ES
As 0,0002 - 0,005 0,00005 - 0,005
Sb 0,0002 - 0,0025 0,0002 - 0,0025
Se 0,0002 - 0,005 0,0002 - 0,005
Sn 0,0005 - 0,005 0,0002 - 0,005
Te 0,00002 - 0,0025 0,00002 - 0,0025
These methods are intended as the definitive methods in case of dispute for the determination of elements at low
content in lead. They are also recommended for the analysis of Certified Reference Materials (CRM) and
Reference Materials (RM) which are used in analysis according to ENV 12908.
2 Normative references
This European Prestandard 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
Prestandard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
EN 12402, Lead and lead alloys - Methods of sampling for analysis.
ENV 12908, Lead and lead alloys - Analysis by Optical Emission Spectrometry (OES) with spark excitation.
ENV 13800, Lead and lead alloys – Analysis by flame atomic absorption spectrometry (FAAS) or inductively
coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrix.
ISO 648, Laboratory glassware – One-mark pipettes.
EN ISO 1042, Laboratory glassware – One-mark volumetric flasks (ISO 1042:1998).
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).
3 Principle
3.1 Preparation of the test solution
Dissolution of a test portion in nitric acid.
Separation of analyte by co-precipitation with manganese dioxide.
Dissolution of the precipitate, made up to a defined volume.
Determination of the analyte concentration using one of the two techniques described in 3.2.
5

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SIST ENV 14138:2004
ENV 14138:2001 (E)
3.2 Instrumental techniques
3.2.1 Flame atomic absorption spectrometry (FAAS)
The analyte concentration in the test solution is obtained by :

nebulization of the test solution into the flame of an atomic absorption spectrometer ;

measurement of the absorption of the resonance line energy of the spectrum from the element at the relevant
wavelength (absorbance) ;

comparison with that of calibration solutions of the same element.
3.2.2 Inductively coupled plasma emission spectrometry (ICP-ES)
The analyte concentration in the test solution is obtained by :

nebulization of the test solution into the plasma of an inductively coupled plasma optical emission
spectrometer ;

measurement of the intensity of the emission signal from the spectrum of the element to be determined at the
relevant wavelength ;

comparison with that of calibration solutions of the same element.
4 Apparatus
4.1 General
Use ordinary apparatus as available in a chemical laboratory.
All glassware to be used shall be cleaned with diluted hydrochloric acid (5.3.2) and thoroughly rinsed with water.
4.2 Volumetric glassware
4.2.1 One-mark volumetric flasks of capacities 25 ml, 100 ml, 500 ml and 1 000 ml
...