SIST ENV 14029:2002

SLOVENSKI STANDARD
SIST ENV 14029:2002
01-februar-2002
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Lead and lead alloys - Analysis by flame atomic absorption spectrometry (FAAS) or
inductively coupled plasma emission spectrometry (ICP-ES), after separation of the lead
matrix
Blei und Bleilegierungen - Analyse durch Flammen-Atomabsorptionsspektrometrie
(FAAS) oder Emissions-Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES), nach
Abtrennung der Bleimatrix
Plomb et alliages de plomb - Analyse par spectrométrie d'absorption atomique dans la
flamme (FAAS) ou spectrométrie d'émission atomique a plasma inductif couplé (ICP-
ES), apres séparation de la matrice plomb
Ta slovenski standard je istoveten z: ENV 14029:2001
ICS:
77.120.60 Svinec, cink, kositer in Lead, zinc, tin and their
njihove zlitine alloys
SIST ENV 14029:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST ENV 14029:2002

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SIST ENV 14029:2002
EUROPEAN PRESTANDARD
ENV 14029
PRÉNORME EUROPÉENNE
EUROPÄISCHE VORNORM
July 2001
ICS 77.040.30; 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 of the lead matrix
Plomb et alliages de plomb - Analyse par spectrométrie Blei und Bleilegierungen - Analyse durch Flammen-
d'absorption atomique dans la flamme (FAAS) ou Atomabsorptionsspektrometrie (FAAS) oder Emissions -
spectrométrie d'émission atomique à plasma inductif Spektrometrie mit induktiv gekoppeltem Plasma (ICP-ES),
couplé (ICP-ES), après séparation de la matrice plomb nach Abtrennung der Bleimatrix
This European Prestandard (ENV) was approved by CEN on 9 June 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 14029:2001 E
worldwide for CEN national Members.

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SIST ENV 14029:2002
ENV 14029:2001 (E)
Contents
page
Foreword.3
1 Scope.4
2 Normative references .5
3 Principle .5
3.1 Preparation of the test solution.5
3.2 Instrumental techniques.5
4 Apparatus .6
4.1 General.6
4.2 Volumetric glassware .6
4.3 Filtration system .6
4.4 Instruments.6
5 Reagents .6
5.1 General.6
5.2 Nitric acid (HNO ) .7
3
5.3 Hydrochloric acid (HCl) .7
5.4 Pure lead .7
5.5 Standard solutions.7
6 Sampling and sample preparation .9
7 Procedure .9
7.1 Preparation of the test solution.9
7.2 Preparation of the synthetic test solution.9
7.3 Preparation of the blank test solution .9
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.12
9 Determination of elements by ICP-ES.13
9.1 General.13
9.2 Calibration and measurement of the test solution.14
9.3 Expression of results.14
10 Test report .14
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SIST ENV 14029:2002
ENV 14029:2001 (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.
CAUTION FOR SAFETY AND TRAINING
The methods in this standard 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.
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.
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SIST ENV 14029:2002
ENV 14029:2001 (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
Ag 0,00001 - 0,001 0,00001 - 0,001
Al 0,0001 - 0,005 0,00005 - 0,005
As 0,0002 - 0,005 0,00005 - 0,005
Bi 0,00005 - 0,0025 0,00005 - 0,0025
Ca 0,00005 - 0,001 0,00001 - 0,001
Cd 0,00005 - 0,001 0,00001 - 0,001
Co 0,00005 - 0,001 0,00005 - 0,001
Cr 0,00005 - 0,001 0,00005 - 0,001
Cu 0,00001 - 0,001 0,00001 - 0,001
Fe 0,00005 - 0,001 0,00005 - 0,001
Mg 0,00005 - 0,001 0,00005 - 0,001
Mn 0,00005 - 0,001 0,00005 - 0,001
Na 0,00005 - 0,001 0,00001 - 0,001
Ni 0,00005 - 0,001 0,00001 - 0,001
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
TI 0,00002 - 0,0025 0,00002 - 0,0025
Zn 0,00001 - 0,001 0,00001 - 0,001
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.
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SIST ENV 14029:2002
ENV 14029:2001 (E)
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 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 648:1977, Laboratory glassware – One-mark pipettes.
ISO 1042:1998, Laboratory glassware – One-mark volumetric flasks.
ISO 3696, Water for analytical laboratory use - Specification and test methods.
3 Principle
3.1 Preparation of the test solution
Dissolution of a test portion in nitric acid.
Separation of lead by crystallisation as lead nitrate.
Reduction of the test solution to a defined volume, and determination of the analyte concentration using one of the
two techniques described in 3.2.
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 matrix-matched 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 matrix-matched calibration solutions of the same element.
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SIST ENV 14029:2002
ENV 14029:2001 (E)
4 Apparatus
4.1 General
Use ordinary apparatus as available in a chemical laboratory.
All glassware to be used shall be cleaned with diluted nitric acid (5.2.2) and thoroughly rinsed with water.
4.2 Volumetric glassware
4.2.1 One-mark volumetric flasks of capacities 20 ml, 200 ml, 500 ml, and 1 000 ml in accordance with ISO
1042:1998 class A.
4.2.2 One-mark pipettes of capacities 2 ml, 5 ml, 10 ml, and 50 ml in accordance with ISO 648:1977 class A.
4.3 Filtration system
Vacuum filtration system with a filter membrane of PTFE, or other material inert to nitric acid, of about 5 μm
porosity (filtering diameter 20 mm to 50 mm).
4.4 Instruments
4.4.1 Flame atomic absorption spectrometer
Flame atomic absorption spectrometer (FAAS) equipped with laminar flow burners suitable for acetylene-air,
hydrogen-air or acetylene-nitrous oxide flames, and with radiation sources such as hollow cathode lamps (HCL) or
electrode-less discharge lamps (EDL) as appropriate to the element to be determined.
The instrument shall be used in accordance with the manufacturer's instructions and the performance checked (see
also the ISO documents in preparation, numbers 00023056 and 00023057).
DANGER To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be
exhausted externally.
4.4.2 Inductively coupled plasma emission spectrometer
Inductively coupled plasma emission spectrometer (ICP-ES), either a simultaneous instrument with the relevant
wavelengths installed or a sequential instrument where a monochromator system allows the selection of
wavelengths (see also the ISO document in preparation number 00021288).
The instrument shall be used in accordance with the manufacturer's instructions and the performances checked
(see also the ISO document in preparation, number 00023058).
DANGER To avoid any risk to personnel due to emission of acid and lead fumes, the off-gas shall be
exhausted externally.
5 Reagents
5.1 General
For all stages of analysis, unless otherwise stated, use only reagents suitable for trace analysis of recognised
analytical grade, preferably with an actual analysis, and only water of at least grade 2, as specified in ISO 3696.
Prepare all solutions using the same container of each reagent.
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SIST ENV 14029:2002
ENV 14029:2001 (E)
5.2 Nitric acid (HNO )
3
5.2.1 Concentrated nitric acid
Nitric acid of high purity, which  = 1,41 g/ml.
20
5.2.2 Nitric acid 1:1 (v/v)
Add to one volume of water, in a suitable container , the same volume of nitric acid (5.2.1) and mix thoroughly. This
diluted acid is also used to clean the laboratory ware.
5.2.3 Nitric acid 1:2 (v/v)
Add 200 ml nitric acid (5.2.1) to 400 ml water in a 1 000 ml beaker and mix thoroughly.
5.3 Hydrochloric acid (HCl)
Hydrochloric acid of high purity, which  = 1,18 g/ml.
20
5.4 Pure lead
For the determination of the recovery rate of the analyte (see 7.2), very pure lead (99,9999 % m/m) should be
used. However, lead of lower purity may be used provided that the analyte is not present in an amount that could
be significant to the determination required.
5.5 Standard solutions
5.5.1 Standard solutions (1 g/l)
5.5.1.1 General
Either use commercially available certified standard solutions or prepare standard solutions as described in 5.5.1.2
to 5.5.1.10.
5.5.1.2 Solutions for silver, bismuth, cadmium, cobalt, chromium, iron, manganese, magnesium, copper,
nickel, thallium and zinc
Weigh (1,0 ± 0,001) g of the relevant metal (99,99 % m/m minimum purity) and transfer into a 250 ml beaker. Add
75 ml of nitric acid (5.2.3), cover with a watch glass and heat gently until dissolution is complete. Allow to cool, then
transfer into a 1 000 ml volumetric flask (4.2.1), then make up to the mark with water and mix thoroughly.
Store the s
...