Unalloyed steel - Determination of low carbon content - Part 2: Infrared absorption method after combustion in an induction furnace (with preheating) (ISO 15349-2:2021)

This document specifies an infrared absorption method after combustion in an induction furnace for
the determination of the low carbon content in unalloyed steel.
The method is applicable to carbon contents between 0,000 3 % (mass fraction) and 0,009 % (mass
fraction).

Unlegierter Stahl - Bestimmung niedriger Kohlenstoffgehalte - Teil 2: Verfahren mit Infrarotabsorption nach Verbrennung im Induktionsofen (mit Vorwärmung) (ISO 15349-2:2021)

Dieses Dokument legt ein Verfahren mit Infrarotabsorption nach Verbrennung im Induktionsofen zur Bestimmung niedriger Kohlenstoffgehalte in unlegiertem Stahl fest.
Das Verfahren ist auf Kohlenstoffgehalte zwischen 0,000 3 % (Massenanteil) und 0,009 % (Massenanteil) anwendbar.

Acier non alliés - Détermination des faibles teneurs en carbone - Partie 2: Méthode par absorption dans l'infrarouge après combustion dans un four à induction (avec préchauffage) (ISO 15349-2:2021)

Nelegirana jekla - Določevanje ogljika v majhnih količinah - 2. del: Metoda z infrardečo absorpcijo po zgorevanju v indukcijski peči (s predgrevanjem) (ISO 15349-2:2021)

General Information

Status
Published
Public Enquiry End Date
14-Jun-2020
Publication Date
24-Aug-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
04-Aug-2021
Due Date
09-Oct-2021
Completion Date
25-Aug-2021

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SLOVENSKI STANDARD
SIST EN ISO 15349-2:2021
01-oktober-2021
Nadomešča:
SIST EN ISO 15349-2:2003
Nelegirana jekla - Določevanje ogljika v majhnih količinah - 2. del: Metoda z
infrardečo absorpcijo po zgorevanju v indukcijski peči (s predgrevanjem) (ISO
15349-2:2021)

Unalloyed steel - Determination of low carbon content - Part 2: Infrared absorption

method after combustion in an induction furnace (with preheating) (ISO 15349-2:2021)

Unlegierter Stahl - Bestimmung niedriger Kohlenstoffgehalte - Teil 2: Verfahren mit

Infrarotabsorption nach Verbrennung im Induktionsofen (mit Vorwärmung) (ISO 15349-

2:2021)

Acier non alliés - Détermination des faibles teneurs en carbone - Partie 2: Méthode par

absorption dans l'infrarouge après combustion dans un four à induction (avec
préchauffage) (ISO 15349-2:2021)
Ta slovenski standard je istoveten z: EN ISO 15349-2:2021
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.140.45 Nelegirana jekla Non-alloyed steels
SIST EN ISO 15349-2:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN ISO 15349-2:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 15349-2:2021
EN ISO 15349-2
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2021
EUROPÄISCHE NORM
ICS 77.080.20 Supersedes EN ISO 15349-2:2003
English Version
Unalloyed steel - Determination of low carbon content -
Part 2: Infrared absorption method after combustion in an
induction furnace (with preheating) (ISO 15349-2:2021)

Acier non alliés - Détermination des faibles teneurs en Unlegierter Stahl - Bestimmung niedriger

carbone - Partie 2: Méthode par absorption dans Kohlenstoffgehalte - Teil 2: Verfahren mit

l'infrarouge après combustion dans un four à induction Infrarotabsorption nach Verbrennung im

(avec préchauffage) (ISO 15349-2:2021) Induktionsofen (mit Vorwärmung) (ISO 15349-

2:2021)
This European Standard was approved by CEN on 11 July 2021.

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, 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

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15349-2:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 15349-2:2021
EN ISO 15349-2:2021 (E)
Contents Page

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

---------------------- Page: 4 ----------------------
SIST EN ISO 15349-2:2021
EN ISO 15349-2:2021 (E)
European foreword

This document (EN ISO 15349-2:2021) 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 January 2022, and conflicting national standards shall

be withdrawn at the latest by January 2022.

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 ISO 15349-2:2003.

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 websites.

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, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 15349-2:2021 has been approved by CEN as EN ISO 15349-2:2021 without any

modification.
---------------------- Page: 5 ----------------------
SIST EN ISO 15349-2:2021
---------------------- Page: 6 ----------------------
SIST EN ISO 15349-2:2021
INTERNATIONAL ISO
STANDARD 15349-2
Second edition
2021-07
Unalloyed steel — Determination of
low carbon content —
Part 2:
Infrared absorption method after
combustion in an induction furnace
(with preheating)
Aciers non alliés — Détermination des faibles teneurs en carbone —
Partie 2: Méthode par absorption dans l'infrarouge après combustion
dans un four à induction (avec préchauffage)
Reference number
ISO 15349-2:2021(E)
ISO 2021
---------------------- Page: 7 ----------------------
SIST EN ISO 15349-2:2021
ISO 15349-2:2021(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: 8 ----------------------
SIST EN ISO 15349-2:2021
ISO 15349-2:2021(E)
Contents Page

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

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

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

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

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

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 3

7 Sampling and preparation of the test samples ..................................................................................................................... 4

8 Procedure..................................................................................................................................................................................................................... 4

8.1 General ........................................................................................................................................................................................................... 4

8.2 Test portion ................................................................................................................................................................................................ 5

8.3 Blank test ..................................................................................................................................................................................................... 5

8.4 Determination ......................................................................................................................................................................................... 5

8.4.1 Pre-treatment of the test portion ...................................................................................................................... 5

8.4.2 Combustion of the test portion ........................................................................................................................... 6

8.5 Establishment of the calibration curve .............................................................................................................................. 6

8.5.1 Calibration with sucrose standard solutions ........................................................................................... 6

8.5.2 Calibration with calcium carbonate ................................................................................................................ 7

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

9.1 Method of calculation ........................................................................................................................................................................ 7

9.2 Precision ....................................................................................................................................................................................................... 8

10 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Features of commercial induction furnaces and infrared carbon analysers 9

Annex B (informative) Additional information on the international inter-laboratory test ....................11

Annex C (informative) Graphical representation of precision data ..................................................................................12

Bibliography .............................................................................................................................................................................................................................13

© ISO 2021 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 15349-2:2021
ISO 15349-2:2021(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 (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 15349-2:1999), which has been

technically revised. The main changes compared to the previous edition are as follows:

— normative references have been revised;
— the precision data has been updated;
— the former Table B.3 has been deleted;
— the text has been improved editorially.
A list of all parts in the ISO 15349 series can be found on the ISO website.

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: 10 ----------------------
SIST EN ISO 15349-2:2021
INTERNATIONAL STANDARD ISO 15349-2:2021(E)
Unalloyed steel — Determination of low carbon content —
Part 2:
Infrared absorption method after combustion in an
induction furnace (with preheating)
1 Scope

This document specifies an infrared absorption method after combustion in an induction furnace for

the determination of the low carbon content in unalloyed steel.

The method is applicable to carbon contents between 0,000 3 % (mass fraction) and 0,009 % (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 terminological databases for use in standardization at the following addresses:

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

Pre-heating of a test portion at low temperature followed by its combustion in presence of an accelerator

at a high temperature in an induction furnace in a current of pure oxygen.
Transformation of carbon into carbon dioxide and/or carbon monoxide.

Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide evolved from the

sample and carried by a current of pure oxygen.
The calibration is carried out using sucrose or calcium carbonate.
© ISO 2021 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 15349-2:2021
ISO 15349-2:2021(E)
5 Reagents

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

water with a low content of organic matter, i.e. grade 2 water as specified in ISO 3696.

5.1 Water, free from carbon dioxide.

Boil water for 30 min, cool to room temperature and bubble oxygen (5.2) or a high purity inert gas

through it for 15 min. Prepare just before use.
5.2 Oxygen, minimum purity 99,95 % (volume fraction).

When the presence of organic contaminants is suspected in oxygen, an oxidation catalyst [copper(II)

oxide or platinum] tube heated to a temperature above 450 °C shall be used prior to the purifying unit.

The pressure of oxygen in the furnace is controlled by a pressure regulator designed especially for this

purpose.

5.3 Pure iron, containing less than 0,000 3 % (mass fraction) of carbon or having a very low and

known carbon content.

5.4 Solvent, appropriate for cleaning greasy or dirty test samples, for example, acetone.

5.5 Accelerator, common accelerators are copper, tungsten-tin mixture, iron, tungsten or nickel.

Copper, tungsten-tin mixture or tungsten containing less than 0,000 3 % carbon (mass fraction) may be

used.

Copper plate or pellet type tin and granular tungsten mixture containing less than 0,000 3 % (mass

fraction) of carbon or having a very low and known carbon content.

Plate shape or granular copper (about 0,1 g/plate) should be used after the following treatment. Heat

the copper plate at 450 °C to 600 °C for 10 min in a current of oxygen or air and cool in a desiccator

without grease. This treatment shall be carried out just before use.

If necessary, wash three times with acetone by decantation to remove organic contaminants and dry at

room temperature.

Pellet type tin (about 0,2 g/pellet) and granular tungsten, 1,68 mm (12 mesh) to 0,853 mm (20 mesh)

should be used after the following treatment. Heat the tungsten at 450 °C in air for 10 min and cool in

a desiccator without grease. Clean the tin for more than 5 min with hydrochloric acid in an ultrasonic

cleaner, rinse with water and dry in air. These treatments shall be carried out just before use.

5.6 Sucrose, standard solutions

Weigh, to the nearest 0,1 mg, the masses of sucrose (C H O ) indicated in Table 1, previously dried

12 22 11

at 100 °C to 105 °C for 2,5 h and cooled in a desiccator, and transfer to a series of seven 100 ml beakers.

Add 30 ml of water (5.1) to dissolve, transfer quantitatively into a series of 100 ml one-mark volumetric

flasks, dilute to the mark with water (5.1) and mix.
2 © ISO 2021 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 15349-2:2021
ISO 15349-2:2021(E)
Table 1 — Standard solution series of sucrose
Standard solution Mass of sucrose Corresponding mass of Carbon content in 1 g of
added carbon the test portion
reference number g
µg % mass fraction
1 0 0 0
2 0,010 0 4,21 0,000 42
3 0,025 0 10,53 0,001 05
4 0,060 0 25,26 0,002 53
5 0,120 0 50,53 0,005 05
6 0,180 0 75,79 0,007 58
7 0,240 0 101,1 0,010 11
Zero member.
5.7 Calcium carbonate

Dry calcium carbonate [minimum purity: 99,9 % (mass fraction)] at 180 °C for 1 h and cool in a

desiccator before use.

5.8 Magnesium perchlorate, anhydrous, [Mg(ClO ) ], particle size: from 0,7 mm to 2,0 mm.

4 2
Phosphorous pentoxide may also be used by some instrument manufacturers.

5.9 Inert ceramic (attapulgus clay), impregnated with sodium hydroxide, particle size: from 0,6 mm

to 1,2 mm.
6 Apparatus
The apparatus required for combustion in an inductio
...

SLOVENSKI STANDARD
oSIST prEN ISO 15349-2:2020
01-junij-2020
Nelegirana jekla - Določevanje ogljika v majhnih količinah - 2. del: Metoda z

infrardečo absorpcijo po zgorevanju v indukcijski peči (s predgrevanjem) (ISO/DIS

15349-2:2020)

Unalloyed steel - Determination of low carbon content - Part 2: Infrared absorption

method after combustion in an induction furnace (with preheating) (ISO/DIS 15349-

2:2020)

Unlegierter Stahl - Bestimmung niedriger Kohlenstoffgehalte - Teil 2: Verfahren mit

Infrarotabsorption nach Verbrennung im Induktionsofen (mit Vorwärmung) (ISO/DIS
15349-2:2020)

Acier non alliés - Détermination des faibles teneurs en carbone - Partie 2: Méthode par

absorption dans l'infrarouge après combustion dans un four à induction (avec
préchauffage) (ISO/DIS 15349-2:2020)
Ta slovenski standard je istoveten z: prEN ISO 15349-2
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.140.45 Nelegirana jekla Non-alloyed steels
oSIST prEN ISO 15349-2:2020 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN ISO 15349-2:2020
---------------------- Page: 2 ----------------------
oSIST prEN ISO 15349-2:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 15349-2
ISO/TC 17/SC 1 Secretariat: JISC
Voting begins on: Voting terminates on:
2020-03-23 2020-06-15
Unalloyed steel — Determination of low carbon content —
Part 2:
Infrared absorption method after combustion in an
induction furnace (with preheating)
Acier non allié — Détermination des faibles teneurs en carbone —

Partie 2: Méthode par absorption dans l'infrarouge après combustion dans un four à induction (avec

préchauffage)
ICS: 77.080.20
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 15349-2:2020(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 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(E)
Contents Page

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

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

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

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

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

5 Reagent ........................................................................................................................................................................................................................... 2

6 Apparatus ..................................................................................................................................................................................................................... 3

7 Sampling and preparation of the test samples ..................................................................................................................... 4

8 Procedure..................................................................................................................................................................................................................... 4

8.1 General ........................................................................................................................................................................................................... 4

8.2 Test portion ................................................................................................................................................................................................ 4

8.3 Blank test ..................................................................................................................................................................................................... 5

8.4 Determination ......................................................................................................................................................................................... 5

8.4.1 Pre-treatment of the test portion ...................................................................................................................... 5

8.4.2 Combustion of the test portion ........................................................................................................................... 5

8.5 Establishment of the calibration curve .............................................................................................................................. 6

8.5.1 Calibration with sucrose standard solutions (5.6) ............................................................................. 6

8.5.2 Calibration with calcium carbonate (5.7) .................. ................................................................................. 6

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

9.1 Method of calculation ........................................................................................................................................................................ 7

9.2 Precision ....................................................................................................................................................................................................... 7

10 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Features of commercial induction furnaces and infrared carbon analysers 9

Annex B (informative) Additional information on international cooperative tests ........................................11

Annex C (informative) Graphical representation of precision data ..................................................................................13

Bibliography .............................................................................................................................................................................................................................14

© ISO 2020 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(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.

This second edition cancels and replaces the first edition (ISO 15349-2:1999), which has been

technically revised in order to re-assess the precision data.
A list of all parts in the ISO 15349 series can be found on the ISO website.
iv © ISO 2020 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST prEN ISO 15349-2:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 15349-2:2020(E)
Unalloyed steel — Determination of low carbon content —
Part 2:
Infrared absorption method after combustion in an
induction furnace (with preheating)
1 Scope

This document specifies an infrared absorption method after combustion in an induction furnace for

the determination of the low carbon content in unalloyed steel.

The method is applicable to carbon mass fraction contents between 0,000 3 % and 0,009 % .

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 terminological databases for use in standardization at the following addresses:

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

Pre-heating of a test portion at low temperature followed by its combustion in presence of an accelerator

at a high temperature in an induction furnace in a current of pure oxygen.
Transformation of carbon into carbon dioxide and/or carbon monoxide.

Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide evolved from steel

and carried by a current of pure oxygen.
The calibration is carried out using sucrose or calcium carbonate.
© ISO 2020 – All rights reserved 1
---------------------- Page: 7 ----------------------
oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(E)
5 Reagent

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

water with a low content of organic matter, i.e. grade 2 water as specified in ISO 3696.

5.1 Water, free from carbon dioxide

Boil water for 30 min, cool to room temperature and allow oxygen (5.2) or a high purity inert gas to

bubble through it for 15 min. Prepare just before use.
5.2 Oxygen, minimum purity 99,95 % (mass fraction)

An oxidation catalyst [copper(II) oxide or platinum] tube heated to a temperature above 450 °C shall be

used prior to a purifying unit, when the presence of organic contaminants in the oxygen is suspected.

The pressure of oxygen in the furnace is controlled by a pressure regulator designed especially for this

purpose.

5.3 Pure iron, containing less than 0,000 3 % mass fraction of carbon or having very low and known

carbon content.

5.4 Solvent, appropriate for cleaning greasy or dirty test samples, for example, acetone

5.5 Accelerator, copper plate (see NOTE 1) or pellet type tin and granular tungsten mixture (see NOTE

2) containing less than 0,000 3 % mass fraction of carbon or having very low and known carbon content.

NOTE 1 Plate shape or granular copper (about 0,1 g/plate) should be used after the following treatment. Heat

the copper plate at 450 °C to 600 °C for 10 min in a current of oxygen or air and cool in a desiccator without

grease. This treatment shall be carried out just before use.

NOTE 2 Pellet type tin (about 0,2 g/pellet) and granular tungsten, 12 mesh to 20 mesh should be used after

the following treatment. Heat the tungsten at 450 °C in air for 10 min and cool in a desiccator without grease.

Clean the tin for more than 5 min by use of hydrochloric acid in an ultrasonic cleaner, rinse with water and dry in

air. These treatments shall be carried out just before use.
5.6 Sucrose, standard solutions

Weigh, to the nearest 0,1 mg, the seven masses of sucrose (C H O ) (analytical standard grade)

12 22 11

indicated in Table 1, previously dried at 100 °C to 105 °C for 2,5 h and cooled in a desiccator, and transfer

to seven 100 ml beakers.

Add 30 ml of water (5.1) to dissolve, transfer to seven 100 ml one-mark volumetric flasks quantitatively,

dilute to the mark with water (5.1) and mix.
Table 1 — Standard solution series of sucrose
Standard solution Mass of sucrose Corresponding mass of Carbon content in 1 g of
added carbon the test portion
reference number g
µg % mass fraction
1 0 0 0
2 0,010 0 4,21 0,000 42
3 0,025 0 10,53 0,001 05
4 0,060 0 25,26 0,002 53
5 0,120 0 50,53 0,005 05
6 0,180 0 75,79 0,007 58
Zero member
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oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(E)
Table 1 (continued)
Standard solution Mass of sucrose Corresponding mass of Carbon content in 1 g of
added carbon the test portion
reference number g
µg % mass fraction
7 0,240 0 101,1 0,010 11
Zero member
5.7 Calcium carbonate

Dry calcium carbonate [minimum purity: 99,9 % (mass fraction)] at 180 °C for 1 h and cool in a

desiccator before use.

5.8 Magnesium perchlorate, anhydrous, [Mg(ClO4) ], particle size: from 0,7 mm to 1,2 mm

5.9 Inert ceramic (attapulgus clay) impregnated with sodium hydroxide, particle size: from 0,6

mm to 1,2 mm
6 Apparatus

The apparatus required for combustion in an induction furnace and the subsequent infrared absorption

measurement of the evolved carbon dioxide and/or carbon monoxide may be obtained commercially

from a number of manufacturers. Follow the manufacturer’s instructions for the operation of the

instrument.
Common features of such systems are described in annex A.

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

Common features of such systems are discussed in annex A.
Ordinary laboratory apparatus and the following should be used.
6.1 Ceramic crucible, capable of withstanding combustion in an induction furnace

Just before use, ignite crucibles in an electric furnace in a current of oxygen or air for not less than 2 h at

more than 1 200 °C and keep in a desiccator or closed container before use.

NOTE For the determination of low carbon contents it is advisable to ignite crucibles at 1 350 °C in a current

of oxygen.

6.2 Tin capsule, about 6 mm in diameter, 18 mm in height, 0,3 g in mass and approximately 0,4 ml

in volume of known and very low carbon content less than 0,000 3 % mass fraction of carbon or having

very low and known carbon content.
Tin capsules should be used after the following treatment.

Rinse the capsule in hydrochloric acid (ρ approximately = 1,19 g/ml, diluted 1+1) for 5 min while

shaking frequently, wash it thoroughly with water and dry. Store it in a clean glass bottle.

6.3 Glass-fiber filter, 21 mm in diameter
Glass-fiber filters should be used after the following treatment.

Heat the glass-fiber filter at 500 °C to 550 °C for 30 min and more in air and cool in a desiccator without

grease. Store it in a clean glass bottle.
6.4 Micropipette, 100 µl, limit of error should be less than 1 µl.
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oSIST prEN ISO 15349-2:2020
ISO/DIS 15349-2:2020(E)
6.5 Microbalance, weighing to the nearest 0,1 µg.
6.6 Muffle or wire-wound furnace, regulated at 400 °C to 500 °C.
7 Sampling and preparation of the test samples

Sampling and preparation of the samples shall be carried out in accordance with ISO 14284 or

appropriate national standards. The chip size of test sample should be between 0,75 mm and 2,0 mm.

8 Procedure

SAFETY INSTRUCTIONS The risks related to combustion analysis are mainly burns in pre-igniting the ceramic

crucible and in the combustion. Use crucible tongs at all times and suitable containers for the used crucibles.

Normal precautions for handling oxygen cylinders shall be taken. Oxygen from the combustion process shall be

removed effectively from the apparatus since a high concentration of oxygen in a confined space can present a

fire hazard.
8.1 General
Purify the oxygen supp
...

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