Steel and cast iron - Determination of copper content - Flame atomic absorption spectrometric method (ISO 4943:2022)

This document specifies a flame atomic absorption spectrometric method for the determination of
copper in steel and cast iron.
The method is applicable to copper contents in the range of 0,003 % (mass fraction) to 3,0 % (mass
fraction).

Stahl und Gusseisen - Bestimmung des Kupfergehalts - Flammenatomabsorptionsspektrometrisches Verfahren (ISO 4943:2022)

Dieses Dokument ist anzuwenden für ein Verfahren zur Bestimmung von Kupfer in Stahl und Gusseisen mittels Flammenatomabsorptionsspektrometrie (FAAS).
Das Verfahren ist auf Kupfergehalte im Bereich von 0,003 % (Massenanteil) bis 3,0 % (Massenanteil) anwendbar.

Aciers et fontes - Détermination de la teneur en cuivre - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 4943:2022)

Le présent document spécifie une méthode par spectrométrie d'absorption atomique dans la flamme pour la détermination du cuivre dans les aciers et les fontes.
Cette méthode est applicable aux teneurs en cuivre comprises entre 0,003 % (en masse) et 3,0 % (en masse).

Jeklo in lito železo - Določevanje bakra - Plamenska atomska absorpcijska spektrometrična metoda (ISO 4943:2022)

Ta dokument določa plamensko atomsko absorpcijsko spektrometrično metodo za določevanje
bakra v jeklu in litem železu.
Metoda se uporablja za vsebnost bakra med 0,003 % (masni delež) in 3,0 % (masni
delež).

General Information

Status
Published
Public Enquiry End Date
17-Jan-2022
Publication Date
09-Oct-2022
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
28-Sep-2022
Due Date
03-Dec-2022
Completion Date
10-Oct-2022

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SLOVENSKI STANDARD
SIST EN ISO 4943:2022
01-november-2022
Nadomešča:
SIST EN 24943:1997
SIST EN 24943:1997/AC:1997
Jeklo in lito železo - Določevanje bakra - Plamenska atomska absorpcijska
spektrometrična metoda (ISO 4943:2022)
Steel and cast iron - Determination of copper content - Flame atomic absorption
spectrometric method (ISO 4943:2022)
Stahl und Gusseisen - Bestimmung des Kupfergehalts -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO 4943:2022)

Aciers et fontes - Détermination de la teneur en cuivre - Méthode par spectrométrie

d'absorption atomique dans la flamme (ISO 4943:2022)
Ta slovenski standard je istoveten z: EN ISO 4943:2022
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.01 Železne kovine na splošno Ferrous metals in general
SIST EN ISO 4943:2022 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN ISO 4943:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 4943:2022
EN ISO 4943
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2022
EUROPÄISCHE NORM
ICS 77.080.01 Supersedes EN 24943:1990, EN 24943:1990/AC:1991
English Version
Steel and cast iron - Determination of copper content -
Flame atomic absorption spectrometric method (ISO
4943:2022)

Aciers et fontes - Détermination de la teneur en cuivre - Stahl und Gusseisen - Bestimmung des Kupfergehalts -

Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches

dans la flamme (ISO 4943:2022) Verfahren (ISO 4943:2022)
This European Standard was approved by CEN on 5 August 2022.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye 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

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4943:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 4943:2022
EN ISO 4943:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

---------------------- Page: 4 ----------------------
SIST EN ISO 4943:2022
EN ISO 4943:2022 (E)
European foreword

This document (EN ISO 4943:2022) has been prepared by Technical Committee ISO/TC 17 "Steel" in

collaboration with Technical Committee CEN/TC 459/SC 2 “Methods of chemical analysis for iron and

steel ” the secretariat of which is held by SIS.

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 March 2023, and conflicting national standards shall

be withdrawn at the latest by March 2023.

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 24943:1990, EN 24943:1990/AC:1991.

Any feedback and questions on this document should be directed to the users’ national standards

body/national committee. A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the

United Kingdom.
Endorsement notice

The text of ISO 4943:2022 has been approved by CEN as EN ISO 4943:2022 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 4943:2022
---------------------- Page: 6 ----------------------
SIST EN ISO 4943:2022
INTERNATIONAL ISO
STANDARD 4943
Second edition
2022-08
Steel and cast iron — Determination
of copper content — Flame atomic
absorption spectrometric method
Aciers et fontes — Détermination de la teneur en cuivre — Méthode
par spectrométrie d'absorption atomique dans la flamme
Reference number
ISO 4943:2022(E)
© ISO 2022
---------------------- Page: 7 ----------------------
SIST EN ISO 4943:2022
ISO 4943:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on

the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below

or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 4943:2022
ISO 4943:2022(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus .................................................................................................................................................................................................................... 2

6.1 Atomic absorption spectrometer ........................................................................................................................................... 2

6.1.1 Minimum precision .......................................................................................................................................................... 3

6.1.2 Limit of detection ............................................................................................................................................................... 3

6.1.3 Calibration linearity ........................................................................................................................................................ 3

6.1.4 Characteristic concentration ................................................................................................................................... 3

6.2 Ancillary equipment .......................................................................................................................................................................... 3

7 Sampling ....................................................................................................................................................................................................................... 3

8 Procedure ....................................................................................................................................................................................................................3

8.1 Test portion ............................................................................................................................................................................................... 3

8.2 Blank test ..................................................................................................................................................................................................... 4

8.3 Determination ......................................................................................................................................................................................... 4

8.3.1 Preparation of the test solution ............................................................................................................................ 4

8.3.2 Preparation of the calibration solutions ....................................................................................................... 4

8.3.3 Adjustment and optimization of atomic absorption spectrometer ...................................... 6

8.3.4 Spectrometric measurements ................................................................................................................................ 7

8.4 Plotting the calibration curve ................................................................................................................................................... 7

9 Expression of results ....................................................................................................................................................................................... 7

10 Precision ....................................................................................................................................................................................................................... 8

11 Test report .................................................................................................................................................................................................................. 8

Annex A (normative) Procedures for the determination of instrumental criteria ........................................10

Annex B (informative) Additional information on the international interlaboratory

precision test ........................................................................................................................................................................................................13

Annex C (informative) Graphical representation of precision data ................................................................................14

Bibliography .............................................................................................................................................................................................................................15

iii
© ISO 2022 – All rights reserved
---------------------- Page: 9 ----------------------
SIST EN ISO 4943:2022
ISO 4943:2022(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to

the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see

www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods

of determination of chemical composition, in collaboration with the European Committee for

Standardization (CEN) Technical Committee CEN/TC 459/SC 2, Methods of chemical analysis for iron

and steel, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna

Agreement).

This second edition cancels and replaces the first edition (ISO 4943:1985), which has been technically

revised. The main changes are as follows:
— extension of the determination range;
— re-organization of a precision test;
— re-assessment of the precision data.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
© ISO 2022 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 4943:2022
INTERNATIONAL STANDARD ISO 4943:2022(E)
Steel and cast iron — Determination of copper content —
Flame atomic absorption spectrometric method
1 Scope

This document specifies a flame atomic absorption spectrometric method for the determination of

copper in steel and cast iron.

The method is applicable to copper contents in the range of 0,003 % (mass fraction) to 3,0 % (mass

fraction).
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.

ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods

ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical

composition
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle

Dissolution of a test portion in a mixture of hydrochloric, nitric and perchloric acids.

Nebulization of the test solution into an air/acetylene flame of an atomic absorption spectrometer.

Spectrometric measurement of the atomic absorption of the 324,7 nm or 327,4 nm spectral line emitted

by a copper hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used.
5 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

grade 2 water as specified in ISO 3696.

5.1 Pure iron, containing less than 0,000 5 % (mass fraction) of copper or having a very low and

known copper content.
© ISO 2022 – All rights reserved
---------------------- Page: 11 ----------------------
SIST EN ISO 4943:2022
ISO 4943:2022(E)
5.2 Hydrochloric acid-nitric acid mixture.

Mix three parts by volume of hydrochloric acid (ρ about 1,19 g/ml), one part by volume of nitric acid (ρ

about 1,40 g/ml), and two parts by volume of water.
Prepare this mixture immediately before use.
5.3 Hydrochloric, nitric and perchloric acids mixture.

Mix 20 ml of hydrochloric acid (ρ about 1,19 g/ml) with 55 ml of nitric acid (ρ about 1,40 g/ml) and

75 ml of perchloric acid (ρ about 1,54 g/ml).

NOTE Perchloric acid (ρ about 1,67 g/ml) can also be used. 100 ml of perchloric acid (ρ about 1,54 g/ml) are

equivalent to 79 ml of perchloric acid (ρ about 1,67 g/ml).
5.4 Copper standard solution, 1,0 g/l.

Weigh (1,000 ± 0,001) g of copper [purity >99,95 % (mass fraction)]. Transfer into a 400 ml beaker,

add 25 ml of nitric acid (ρ about 1,40 g/ml, diluted 1 + 4) and cover with a watch-glass. Heat gently

to complete dissolution. Allow to cool, 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 standard solution contains 1 mg of Cu.
5.5 Copper standard solution, 20 mg/l.

Transfer 20,0 ml of the standard solution (5.4) into a 1 000 ml one-mark volumetric flask, dilute to the

mark with water and mix.
1 ml of this standard solution contains 20 μg of Cu.
Prepare this standard solution immediately before use.
6 Apparatus

All volumetric glassware shall be class A, in accordance with ISO 648 or ISO 1042 as appropriate.

All glassware shall first be washed in hydrochloric acid (ρ about 1,19 g/ml, diluted 1 + 1), and then

in water. The quantity of copper present in the beakers and flasks can be checked by measuring the

absorption of distilled water introduced in the glassware after the acid wash.
Ordinary laboratory apparatus and the following shall be used.
6.1 Atomic absorption spectrometer

The spectrometer shall be equipped with a copper hollow-cathode lamp, and supplied with air and

acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from

copper.
NOTE Other suitable radiation sources can also be used.

The atomic absorption spectrometer used will be satisfactory if, after optimization in accordance with

8.3.4, the limit of detection and characteristic concentration are in reasonable agreement with the

values given by the manufacturer and it meets the precision criteria given in 6.1.1 to 6.1.3.

The instrument should also conform to the additional performance requirement given in 6.1.4.

© ISO 2022 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 4943:2022
ISO 4943:2022(E)
6.1.1 Minimum precision

Use the procedures described in Annex A. Calculate the standard deviation of 10 measurements of the

absorbance of the most concentrated calibration solution. This standard deviation shall not exceed

1,0 % of the mean absorbance.

Calculate the standard deviation of 10 measurements of the absorbance of the least concentrated

calibration solution (excluding the zero member). This standard deviation shall not exceed 0,5 % of the

mean absorbance of the most concentrated calibration solution.
6.1.2 Limit of detection
Use the procedures described in Annex A. The li
...

SLOVENSKI STANDARD
oSIST prEN ISO 4943:2022
01-januar-2022
Jeklo in lito železo - Določevanje bakra - Plamenska atomska absorpcijska
spektrometrična metoda (ISO/DIS 4943:2021)
Steel and cast iron - Determination of copper content - Flame atomic absorption
spectrometric method (ISO/DIS 4943:2021)
Stahl und Gusseisen - Bestimmung des Kupfergehalts -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO/DIS 4943:2021)

Aciers et fontes - Détermination du cuivre - Méthode par spectrométrie d'absorption

atomique dans la flamme (ISO/DIS 4943:2021)
Ta slovenski standard je istoveten z: prEN ISO 4943
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.01 Železne kovine na splošno Ferrous metals in general
oSIST prEN ISO 4943:2022 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN ISO 4943:2022
---------------------- Page: 2 ----------------------
oSIST prEN ISO 4943:2022
DRAFT INTERNATIONAL STANDARD
ISO/DIS 4943
ISO/TC 17/SC 1 Secretariat: JISC
Voting begins on: Voting terminates on:
2021-10-27 2022-01-19
Steel and cast iron — Determination of copper content —
Flame atomic absorption spectrometric method

Aciers et fontes — Dosage du cuivre — Méthode par spectrométrie d'absorption atomique dans la flamme

ICS: 77.080.01
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 4943:2021(E)
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. ISO 2021
---------------------- Page: 3 ----------------------
oSIST prEN ISO 4943:2022
ISO/DIS 4943:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 4943:2022
ISO/DIS 4943:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

6.1 Atomic absorption spectrometer ............................................................................................................................................ 2

6.1.1 Minimum precision (see Annex A) ................................................................................................................... 3

6.1.2 Limit of detection (see Annex A) ........................................................................................................................ 3

6.1.3 Calibration linearity (see Annex A) ................................................................................................................. 3

6.1.4 Characteristic concentration (see Annex A) ............................................................................................ 3

6.2 Ancillary equipment. ......................................................................................................................................................................... 3

7 Sampling ........................................................................................................................................................................................................................ 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Test Portion ................................................................................................................................................................................................ 3

8.2 Blank test ..................................................................................................................................................................................................... 4

8.3 Determination ......................................................................................................................................................................................... 4

8.3.1 Preparation of the test solution .......................................................................................................................... 4

8.3.2 Preparation of the calibration solutions ...................................................................................................... 4

8.3.3 Adjustment and optimization of atomic absorption spectrometer ..................................... 6

8.3.4 Spectrometric measurements .............................................................................................................................. 7

8.4 Plotting the calibration curve ..................................................................................................................................................... 7

9 Expression of results ........................................................................................................................................................................................ 7

10 Precision ....................................................................................................................................................................................................................... 8

11 Test report ................................................................................................................................................................................................................... 8

Annex A (normative) Procedures for the determination of instrumental criteria ...........................................10

Annex B (informative) Additional information on the international interlaboratory test.......................13

Annex C (informative) Graphical representation of precision data ..................................................................................14

Bibliography .............................................................................................................................................................................................................................15

© ISO 2021 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 4943:2022
ISO/DIS 4943:2021(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2. www .iso .org/ directives

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received. www .iso .org/ patents

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO's adherence to the World Trade Organization (WTO)

principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword

.html.

This document was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of

determination of chemical composition.

This second edition cancels and replaces the first edition (ISO 4943:1985), which has been technically

revised. The main changes compared to the previous edition are:
— extension of the determination range;
— re-organization of a precision test;
— re-assessment of the precision data.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST prEN ISO 4943:2022
DRAFT INTERNATIONAL STANDARD ISO/DIS 4943:2021(E)
Steel and cast iron — Determination of copper content —
Flame atomic absorption spectrometric method
1 Scope

This document specifies a flame atomic absorption spectrometric method for the determination of

copper in steel and cast iron.

The method is applicable to copper contents in the range of 0,003 % (mass fraction) to 3,0 % (mass

fraction).
2 Normative references

The following documents are referred to in the text 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.

ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods

ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical

composition
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle

Dissolution of a test portion in a mixture of hydrochloric, nitric and perchloric acids.

Nebulisation of the test solution into an air/acetylene flame of an atomic absorption spectrometer.

Spectrometric measurement of the atomic absorption of the 324,7 nm or 327,4 nm spectral line emitted

by a copper hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used.
5 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

grade 2 water as specified in ISO 3696.

5.1 Pure iron, containing less than 0,000 5 % (mass fraction) of copper or of low and known copper

content.
© ISO 2021 – All rights reserved 1
---------------------- Page: 7 ----------------------
oSIST prEN ISO 4943:2022
ISO/DIS 4943:2021(E)
5.2 Hydrochloric acid-nitric acid mixture.

Mix three parts by volume of hydrochloric acid (ρ about 1,19 g/ml), one part by volume of nitric acid (ρ

about 1,40 g/ml), and two parts by volume of water.
Prepare this mixture immediately before use.
5.3 Hydrochloric acid-nitric acid-perchloric acid mixture.

Mix 20 ml of hydrochloric acid (ρ about 1,19 g/ml) with 55 ml of nitric acid (ρ about 1,40 g/ml) and

75 ml of perchloric acid (ρ about 1,54 g/ml).

NOTE Perchloric acid (ρ about 1,67 g/ml) may also be used. 100 ml of perchloric acid (ρ about 1,54 g/ml) are

equivalent to 79 ml of perchloric acid (ρ about 1,67 g/ml).
5.4 Copper standard solution, 1,0 g/l.

Weigh (1,000 ± 0,001) g of copper [purity > 99,95 % (mass fraction)]. Transfer into a 400 ml beaker,

add 25 ml of nitric acid (ρ about 1,40 g/ml, diluted 1 + 4) and cover with a watch-glass. Heat gently

to complete dissolution. Allow to cool, 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 standard solution contains 1 mg of Cu.
5.5 Copper standard solution, 20 mg/l.

Transfer 20,0 ml of the standard solution (5.4) into a 1 000 ml one-mark volumetric flask, dilute to the

mark with water and mix.
1 ml of this standard solution contains 20 μg of Cu.
Prepare this standard solution immediately before use.
6 Apparatus

All volumetric glassware shall be class A, in accordance with ISO 648 or ISO 1042 as appropriate.

All glassware shall first be washed in hydrochloric acid (ρ about 1,19 g/ml, diluted 1 + 1), and then

in water. The quantity of copper present in the beakers and flasks can be checked by measuring the

absorption of distilled water introduced in the glassware after the acid wash.
Ordinary laboratory apparatus and the following shall be used.
6.1 Atomic absorption spectrometer

The spectrometer shall be equipped with a copper hollow-cathode lamp, and supplied with air and

acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from

copper.
NOTE Other suitable radiation sources can also be used.

The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.4,

the limit of detection and characteristic concentration are in reasonable agreement with the values

given by the manufacturer and it meets the precision criteria given in 6.1.1 to 6.1.3.

The instrument should also conform to the additional performance requirement given in 6.1.4.

2 © ISO 2021 – All rights reserved
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oSIST prEN ISO 4943:2022
ISO/DIS 4943:2021(E)
6.1.1 Minimum precision (see Annex A)

Calculate the standard deviation of 10 measurements of the absorbance of the most concentrated

calibration solution. This standard deviation shall not exceed 1,0 % of the mean absorbance.

Calculate the standard deviation of 10 measurements of the absorbance of the least concentrated

calibration solution (excluding the zero member). This standard deviation shall not exceed 0,5 % of the

mean absorbance of the most concentrated calibration solution.
6.1.2 Limit of detection (see Annex A)

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 copper in a matrix similar to the final test portion solution shall be better than

0,05 µg/ml.
6.1.3 Calibration linearity (see Annex A)

The slope of the calibration curve covering the top 20 % of the concentration range (expressed as a

change in absorbance) shall not be less than 0,7 times the value of the slope for the bottom 20 % of the

concentration range (expressed as a change in absorbance) determined in the same way.

For instruments with automatic calibration using two or more standards, it shall be established prior

to the analysis, by obtaining absorbance readings, that the above requirements for graph linearity are

fulfilled.
6.1.4 Characteristic concentration (see Annex A)

The characteristic concentration for copper in a matrix similar to the final test portion solution shall be

better than 0,08 µg/ml for 324,7 nm.
6.2 Ancillary equipment.

Scale expansion can be used until the noise observed is greater than the read-out error and is always

recommended for absorbances below 0,1. If scale expansion has to be used and the instrument does not

have the means to read the value of the scale expansion factor, the value can be calculated by measuring

a suitable solution with and without scale expansion and then dividing the signal obtained.

7 Sampling

Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel and cast

iron.
8 Procedure

WARNING — Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous

fumes or organic matter in general. All evaporations shall be carried out in fume cupboards

suitable for use with
...

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