EN 10181:2019

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 % (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.

Stähle - Bestimmung des Bleigehalts - 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 % (pourcentage en masse) et 0,5 % (pourcentage en masse).
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

• Status: Published
• Publication Date: 11-Jun-2019
• Withdrawal Date: 30-Dec-2019
• ICS: 77.040.30 - Chemical analysis of metals
• Technical Committee: ECISS/TC 102 - Methods of chemical analysis for iron and steel
• Drafting Committee: ECISS/TC 102/WG 3 - Determination of environmentally sensitive elements in steel
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 09-Jan-2025
• Completion Date: 14-Apr-2025
• Mandate: M/BC/CEN/87/15 - ECISS - 2nd programme
• Ref Project: SIST EN 10181:2019 - Steels - Determination of lead content - Flame atomic absorption spectrometric method (FAAS)

Relations

• Replaces: EN 10181:1989 - Chemical analysis of ferrous materials - Determination of lead in steels - Flame atomic absorption spectrometric method
• Effective Date: 19-Jun-2019

Overview

EN 10181:2019 is a European standard established by CEN that specifies a flame atomic absorption spectrometric method (FAAS) for determining the lead content in non-alloy and low alloy steels. This analytical technique is designed to accurately measure lead concentrations typically ranging from 0.005% to 0.5% by weight. The method can be adjusted for lead levels outside this range by altering sample preparation steps such as test portion size or solution dilution, ensuring flexibility while maintaining accuracy.

The standard replaces the earlier EN 10181:1989 version and introduces significant technical enhancements including updated calibration procedures, the option to use aqua regia for sample dissolution, and refined spectrometric measurement protocols. EN 10181:2019 ensures reliable and reproducible results critical for quality control and regulatory compliance within the steel manufacturing and processing industries.

Key Topics

• Scope and Applicability
  Applies to non-alloy and low alloy steels to quantify lead content within the specified concentration range. Adaptable to broader lead content levels with adjusted sample handling.

• Analytical Principle

  • Sample dissolution using hydrochloric acid followed by oxidation with nitric acid or aqua regia.
  • Introduction of the dissolved sample into an air/acetylene flame within an atomic absorption spectrometer.
  • Measurement of lead atomic absorption at 283.3 nm using a lead hollow-cathode lamp or equivalent radiation sources.

• Equipment and Reagents

  • Use of class A volumetric glassware for precise measurements.
  • Requirement of a lead hollow-cathode lamp spectrometer with background correction and stable flame conditions.
  • High purity reagents including hydrochloric acid, nitric acid, pure iron, and calibrated lead standard solutions.

• Calibration and Measurement

  • Preparation of calibration solutions tailored to the sample's lead content range, ensuring linearity and precision.
  • Implementation of the bracketing method to enhance measurement accuracy.
  • Stringent instrument performance checks including limit of detection (<0.3 µg/ml) and characteristic concentration (<0.6 µg/ml).

• Sampling and Sample Preparation

  • Adherence to EN ISO 14284 for steel sampling procedures.
  • Test portion typically around 2 grams, digested chemically for complete dissolution.
  • Filtration and dilution ensuring clear solutions for accurate spectrometric readings.

Applications

• Quality Control in Steel Production
  Accurate monitoring of lead content is vital in steel manufacturing to prevent contamination and ensure mechanical properties meet specifications.

• Regulatory Compliance
  Supports manufacturers in meeting environmental and safety regulations concerning heavy metals in steel products.

• Material Certification
  Enables steel producers and users to verify chemical composition for certification and traceability purposes.

• Research and Development
  Facilitates experimental studies requiring precise quantification of lead in steel alloys for new material development.

Related Standards

• EN ISO 14284 – Sampling and preparation of steel and iron samples for chemical analysis.
• EN ISO 648 – Standards for single-volume pipettes used in laboratory measurements.
• EN ISO 1042 – Standards for volumetric flasks essential for the preparation of calibration solutions.
• Additional CEN standards on chemical analysis methods for metals contribute to a comprehensive quality management system in metallurgy.

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By following EN 10181:2019, laboratories and steel manufacturers gain access to a robust and validated FAAS method for lead determination, ensuring precision, repeatability, and compliance with European regulatory frameworks. This standard plays a crucial role in controlling lead contamination, protecting end-users, and maintaining the high quality standards of steel products worldwide.

Standards Content (Sample)

SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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.

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

European foreword
This document (EN 10181:2019) has been prepared by Technical Committee CEN/TC 459 “ECISS -
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.

Through its subcommittee SC 2 “Methods of chemical analysis for iron and steel” (secretariat: SIS)
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 %.
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.
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.
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.
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
...