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

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

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

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Status
Not Published
Current Stage
6055 - CEN Ratification completed (DOR) - Publishing
Due Date
11-Jul-2021
Completion Date
11-Jul-2021

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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.

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oSIST prEN ISO 15349-2:2020
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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
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FOR COMMENT AND APPROVAL. IT IS
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ISO/DIS 15349-2:2020(E)
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PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
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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

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ii © ISO 2020 – All rights reserved
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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
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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
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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
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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
2 © ISO 2020 – All rights reserved
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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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