EN 10181:2019

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 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 glassware with a watch glass and heat
gently until the reaction ceases. Oxidize 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 standard deviation of 10 measurements of the absorbance of the most concentrated calibration
solution shall not exceed 1,5 % of the mean absorbance of this solution.
The standard deviation of 10 measurements of the absorbance of the least concentrated calibration
solution (excluding the zero member) shall not exceed 0,5 % of the mean absorbance of the most
concentrated calibration solution.
6.2.3 Additional performance requirements
6.2.3.1 General
The instrument should also conform to the additional performance requirements given in 6.2.3.2 and
6.2.3.3.
6.2.3.2 Characteristic concentration
The characteristic concentration for lead in a matrix similar to the final test solution shall be lower than
0,6 µg/ml.
6.2.3.3 Limit of detection
The limit of detection is a number, expressed in units of concentration (or amount) that describes the
lowest concentration level (or amount) of an element that can be determined to be statistically different
from an analytical blank.
The limit of detection of lead in a matrix similar to the final test solution shall be less than 0,3 µg/ml.
7 Sampling
Carry out sampling in accordance with EN ISO 14284 or appropriate national standards for steels.
8 Procedure
NOTE The following concentrations, amounts and glassware volumes can be modified, provided the changes
are taken into account in all appropri
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