SIST EN 10181:2019
(Main)Steels - Determination of lead content - Flame atomic absorption spectrometric method (FAAS)
Steels - Determination of lead content - Flame atomic absorption spectrometric method (FAAS)
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of lead content in non-alloy and low alloy steels.
The method is applicable to lead contents between 0,005 % and 0,5 %.
The method can be adapted to lower or higher lead contents by changing the test portion or the dilution process, provided the criteria in 5.2.2 and 5.2.3 are still met.
Stahl - Bestimmung des Bleianteils - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Dieses Dokument legt ein Verfahren zur Bestimmung des Bleigehalts in unlegierten und niedriglegierten Stählen mittels Flammenatomabsorptionsspektroskopie (FAAS) fest.
Dieses Verfahren ist anwendbar für Stähle mit Bleianteilen von 0,005 % (Massengehalt) bis 0,5 % (Massengehalt).
Dieses Verfahren kann für niedrigere als auch höhere Bleigehalte angewandt werden, wenn die Probengrößen und Lösungsvorgänge angepasst werden, sofern die in 6.2.2 und 6.2.3 angegebenen Kriterien erfüllt werden.
Aciers - Détermination de la teneur en plomb - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
Le présent document spécifie une méthode par spectrométrie d'absorption atomique dans la flamme (SAAF) pour la détermination des teneurs en plomb dans les aciers non alliés et faiblement alliés.
La méthode s'applique aux teneurs en plomb comprises entre 0,005 % et 0,5 %.
La méthode peut être adaptée à des teneurs en plomb inférieures ou supérieures en modifiant la prise d'essai ou le facteur de dilution, sous réserve que les critères énoncés en 6.2.2 et 6.2.3 soient respectés.
Jeklo - Določevanje svinca - Metoda s plamensko atomsko absorpcijsko spektrometrijo (FAAS)
Ta dokument določa metodo plamenske atomske absorpcijske spektrometrije (FAAS) za določevanje svinca v nelegiranih in malolegiranih jeklih.
Ta metoda se uporablja za vsebnosti svinca med 0,005 % in 0,5 %.
Metodo je mogoče prilagoditi nižjim ali višjim vsebnostim svinca s spreminjanjem preskusne količine ali procesa redčenja, če so kriteriji iz točk 5.2.2 in 5.2.3 še vedno izpolnjeni.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 10181:2019
01-september-2019
Nadomešča:
SIST EN 10181:1997
Jeklo - Določevanje svinca - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (FAAS)
Steels - Determination of lead content - Flame atomic absorption spectrometric method
(FAAS)
Stahl - Bestimmung des Bleianteils - Flammenatomabsorptionsspektrometrisches
Verfahren (FAAS)
Aciers - Détermination de la teneur en plomb - Méthode par spectrométrie d'absorption
atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: EN 10181:2019
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
SIST EN 10181:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 10181:2019
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SIST EN 10181:2019
EN 10181
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 77.040.30 Supersedes EN 10181:1989
English Version
Steels - Determination of lead content - Flame atomic
absorption spectrometric method (FAAS)
Aciers - Détermination de la teneur en plomb - Stahl - Bestimmung des Bleianteils -
Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches
dans la flamme (SAAF) Verfahren (FAAS)
This European Standard was approved by CEN on 22 April 2019.
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 CEN-CENELEC 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 CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 10181:2019 E
worldwide for CEN national Members.
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SIST EN 10181:2019
EN 10181:2019 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sampling . 6
8 Procedure. 6
8.1 Test portion . 6
8.2 Blank test . 6
8.3 Determination . 7
8.3.1 Preparation of the test solution . 7
8.3.2 Preparation of the calibration solutions . 7
8.3.3 Adjustment of the atomic absorption spectrometer . 8
8.3.4 Spectrometric measurements . 8
9 Expression of results . 9
9.1 Use of the calibration curve . 9
9.2 Use of bracketing method . 10
10 Test report . 10
Annex A (informative) Samples tested . 11
Bibliography . 12
2
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SIST EN 10181:2019
EN 10181:2019 (E)
European foreword
This document (EN 10181:2019) has been prepared by Technical Committee CEN/TC 459 “ECISS -
1
European Committee for Iron and Steel Standardization” , the secretariat of which is held by AFNOR.
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 December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 10181:1989.
In comparison with EN 10181:1989, the following significant technical changes were made:
— Clause 1: lower limit of the scope changed;
— Normative references: revised;
— Clause 4: possibility for using aqua regia for the dissolution and other suitable radiation sources
added;
— Clause 5: preparation of lead standard solution, 0,05 g/l and iron base solution added;
— 8.3.2: calibration solutions expanded;
— 8.3.3: background correction specified;
— 8.3.4 and Clause 9: bracketing method for the spectrometric measurements added;
— Clause 10: editorially updated;
— Bibliography: added.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
1
Through its subcommittee SC 2 “Methods of chemical analysis for iron and steel” (secretariat: SIS)
3
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SIST EN 10181:2019
EN 10181:2019 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of lead content in non-alloy and low alloy steels.
The method is applicable to lead contents between 0,005 % (weight percent) and 0,5 % (weight
percent).
The method can be adapted to lower or higher lead contents by changing the test portion or the dilution
process, provided the criteria in 6.2.2 and 6.2.3 are still met.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 648, Laboratory glassware — Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)
EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition (ISO 14284)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
Dissolution of a test portion in hydrochloric acid followed by oxidation with nitric acid.
NOTE 1 Aqua regia can be used for simultaneous dissolution and oxidation of the test portion.
Nebulization of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 283,3 nm spectral line emitted by a lead
hollow-cathode lamp.
NOTE 2 Other suitable radiation sources can also be used and measurements can also be carried out at
217,0 nm, provided the criteria in 6.2.2 and 6.2.3 are still met.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water
of equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into
account in 8.3 and Clause 9.
5.1 Pure iron, with lead content < 0,001 %.
4
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SIST EN 10181:2019
EN 10181:2019 (E)
5.2 Hydrochloric acid solution, 1 + 1.
Add 500 ml of hydrochloric acid (ρ = 1,19 g/ml, approximately) to 500 ml of water and mix.
20
5.3 Nitric acid solution, 4 + 6.
Add 400 ml of nitric acid (ρ = 1,40 g/ml, approximately) to 600 ml of water and mix.
20
5.4 Lead standard solution, 0,5 g/l.
Weigh (0,500 ± 0,001) g of lead (Pb ≥ 99,99 %) and transfer into a heat-resistant glassware of suitable
size. Add 25 ml of nitric acid (ρ = 1,40 g/ml, approximately), diluted 1 + 4.
20
Cover with a watch glass, and, if necessary, heat gently to assist dissolution. When dissolution is
complete boil to remove nitrogen oxides.
Allow to cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 0,5 mg of lead.
5.5
...
SLOVENSKI STANDARD
oSIST prEN 10181:2018
01-september-2018
-HNOR'RORþHYDQMHVYLQFD3ODPHQVNDDWRPVNDDEVRUSFLMVNDVSHNWURPHWULþQD
PHWRGD )$$6
Steels - Determination of lead content - Flame atomic absorption spectrometric method
(FAAS)
Stahl - Bestimmung des Bleianteils - Flammenatomabsorptionsspektrometrisches
Verfahren (FAAS)
Aciers - Détermination de la teneur en plomb - Méthode par spectrométrie d'absorption
atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: prEN 10181
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
oSIST prEN 10181:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 10181:2018
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oSIST prEN 10181:2018
DRAFT
EUROPEAN STANDARD
prEN 10181
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2018
ICS 77.040.30 Will supersede EN 10181:1989
English Version
Steels - Determination of lead content - Flame atomic
absorption spectrometric method (FAAS)
Aciers - Détermination de la teneur en plomb - Stahl - Bestimmung des Bleianteils -
Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches
dans la flamme (SAAF) Verfahren (FAAS)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
ECISS/TC 102.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 10181:2018 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 10181:2018
prEN 10181:2018 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sampling . 6
8 Procedure. 6
9 Expression of results . 9
10 Test report . 10
Annex A (informative) Samples tested . 11
Bibliography . 12
2
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oSIST prEN 10181:2018
prEN 10181:2018 (E)
European foreword
This document (prEN 10181:2018) has been prepared by Technical Committee ECISS/TC 102 “Methods
of chemical analysis for iron and steel”, the secretariat of which is held by SIS.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 10181:1989.
3
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oSIST prEN 10181:2018
prEN 10181:2018 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of lead content in non-alloy and low alloy steels.
The method is applicable to lead contents between 0,005 % and 0,5 %.
The method can be adapted to lower or higher lead contents by changing the test portion or the dilution
process, provided the criteria in 6.2.2 and 6.2.3 are still met.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
Dissolution of a test portion in hydrochloric acid followed by oxidation with nitric acid.
NOTE 1 Aqua regia can be used for simultaneous dissolution and oxidation of the test portion.
Nebulization of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 283,3 nm spectral line emitted by a lead
hollow-cathode lamp.
NOTE 2 Other suitable radiation sources can also be used and measurements can also be carried out at 217,0 nm,
provided the criteria in 6.2.2 and 6.2.3 are still met.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of
equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into account
in 8.3 and Clause 9.
5.1 Pure iron, with lead content < 0,001 %.
5.2 Hydrochloric acid solution, 1 + 1.
Add 500 ml of hydrochloric acid (ρ = 1,19 g/ml, approximately) to 500 ml of water and mix.
20
5.3 Nitric acid solution, 4 + 6.
Add 400 ml of nitric acid (ρ = 1,40 g/ml, approximately) to 600 ml of water and mix.
20
4
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oSIST prEN 10181:2018
prEN 10181:2018 (E)
5.4 Lead standard solution, 0,5 g/l.
Weigh (0,500 ± 0,001) g of lead (Pb ≥ 99,99 %) and transfer into a heat-resistant glassware of suitable
size. Add 25 ml of nitric acid (ρ = 1,40 g/ml, approximately), diluted 1 + 4.
20
Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolution is complete
boil to remove nitrogen oxides.
Allow to cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 0,5 mg of lead.
5.5 Lead standard solution, 0,05 g/l.
Transfer 10,0 ml of lead standard solution (5.4) into a 100 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,05 mg of lead.
5.6 Iron base solution, 40 g/l.
Weigh, to the nearest 0,01 g, 10,00 g of pure iron (5.1) and transfer into a heat-resistant glassware of
suitable size. Add 100 ml of hydrochloric acid (5.2), cover the beaker with a watch glass and heat gently
until the reaction ceases. Oxidise with 20 ml of nitric acid (5.3), then boil the solution for 5 min to remove
nitrogen oxides.
Allow to cool and transfer the solution quantitatively into a 250 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
6 Apparatus
6.1 Ordinary laboratory apparatus
All volumetric glassware shall be class A, in accordance with EN ISO 648 or EN ISO 1042, as appropriate.
6.2 Atomic absorption spectrometer
6.2.1 General
The spectrometer shall be equipped with a lead hollow-cathode lamp or other suitable radiation source
and supplied with air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water
and oil, and free from lead.
The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.3, the
limit of detection and characteristic concentration are in reasonable agreement with the values given by
the manufacturer and it meets the performance criteria given in 6.2.2 and 6.2.3.
6.2.2 Minimum precision
The s
...
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