ISO 17053:2005
(Main)Steel and iron — Determination of oxygen — Infrared method after fusion under inert gas
Steel and iron — Determination of oxygen — Infrared method after fusion under inert gas
ISO 17053:2005 specifies an infrared method after fusion under inert gas for the determination of oxygen in steel and iron. The method is applicable to mass fractions of oxygen between 0,000 75 % and 0,01 %.
Acier et fonte — Dosage de l'oxygène — Méthode par infrarouge après fusion sous gaz inerte
General Information
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 17053
First edition
2005-02-01
Steel and iron — Determination of
oxygen — Infrared method after fusion
under inert gas
Acier et fonte — Dosage de l'oxygène — Méthode par infrarouge après
fusion sous gaz inerte
Reference number
ISO 17053:2005(E)
©
ISO 2005
---------------------- Page: 1 ----------------------
ISO 17053:2005(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2005
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2005 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 17053:2005(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references . 1
3 Principle . 1
4 Reagents and materials. 1
5 Apparatus. 3
6 Sampling . 3
7 Procedure. 3
8 Expression of results. 6
9 Test report. 7
Annex A (informative) Additional information on international cooperative test. 8
Annex B (informative) Graphical representation of precision data. 9
© ISO 2005 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 17053:2005(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
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.
ISO 17053 was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of
determination of chemical composition.
iv © ISO 2005 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 17053:2005(E)
Steel and iron — Determination of oxygen — Infrared method
after fusion under inert gas
1 Scope
This International Standard specifies an infrared method after fusion under inert gas for the determination of
oxygen in steel and iron.
The method is applicable to mass fractions of oxygen between 0,000 75 % and 0,01 %.
2 Normative references
The following referenced documents are indispensable for the application 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 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic
method for the determination of repeatability and reproducibility of a standard measurement method
ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results — Part 3:
Intermediate measures of the precision of a standard measurement method
ISO 14284:1996, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition
3 Principle
Fusion of a test portion in a single-use graphite crucible under helium gas at a minimum temperature of
2 000 °C. Combination of the oxygen from the sample with carbon from the crucible to form carbon monoxide.
Eventually, transformation of carbon monoxide into carbon dioxide.
Measurement of infrared absorption of the carbon monoxide or dioxide, against a calibration curve made of
potassium nitrate.
4 Reagents and materials
4.1 General
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade.
4.2 Helium, of high purity, total impurity content 0,000 5 % (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 is suspected in the helium.
© ISO 2005 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 17053:2005(E)
4.3 Magnesium perchlorate, Mg (ClO ) , (commercial designation: anhydrone), particle size from 1,2 mm
4 2
to 2,0 mm, or anhydrous calcium sulfate, (commercial designation: drierite), particle size from 0,6 mm to
0,85 mm.
4.4 Sodium hydroxide, on granulated support, (commercial designation: ascarite), particule size from
0,7 mm to 1,2 mm.
4.5 Copper oxide, CuO.
4.6 Tin or nickel capsules, for example diameter 5 mm, length 13 mm, mass 160 mg, with low mass
fraction of oxygen, less than 0,1 µg/mg of oxygen.
Cut off the upper part of the tin capsule to reduce the mass to 50 mg or the length to 8 mm in order to remove
the contaminated part.
4.7 Water of high purity, deionised, prepared just before use.
4.8 Potassium nitrate, KNO , of high purity, maximum total impurity content 0,000 5 % by mass.
3
Dry before use at 100°C to 105°C for 2 h, and allow to cool in a dessicator.
4.9 Potassium nitrate stock solution, corresponding to 4 mg/ml of oxygen.
Weigh, to the nearest 0,1 mg, 8,416 g of potassium nitrate (4.8).
Place in a 100 ml beaker and dissolve in about 50 ml of water (4.7).
Transfer quantitatively to a 1 000 ml volumetric flask, dilute to the mark with water (4.7), and mix.
1 ml of the potassium nitrate stock solution contains 4 mg of oxygen as potassium nitrate.
4.10 Potassium nitrate diluted stock solution, corresponding to 0,4 mg/ml of oxygen.
This solution must be prepared freshly before use.
Transfer 10 ml of the potassium nitrate stock solution to a 100 ml volumetric flask, dilute to the mark with
water (4.7), and mix.
1 ml of the potassium nitrate stock solution contains 0,4 mg of oxygen as potassium nitrate.
4.11 Potassium nitrate standard solutions
These solutions must be prepared freshly before use.
Transfer the volume listed in Table 1 of the potassium nitrate stock solution (4.9) and of the potassium nitrate
diluted stock solution (4.10) to a series of nine 100 ml volumetric flasks, dilute to the mark with water (4.7),
and mix.
100 µl of each of the potassium nitrate standard solutions contain the mass of oxygen (as potassium nitrate)
listed in the last column of Table 1.
4.12 Graphite powder, of high purity, with low oxygen content.
2 © ISO 2005 – All rights reserved
---------------------- Page: 6 ----------------------
ISO 17053:2005(E)
Table 1 — Potassium nitrate standard solution
Potassium nitrate Volume of potassium nitrate Mass of oxygen in 1 ml
Mass of oxygen in 100 µµµµl of the
standard solution stock solution (4.9) added of the potassium nitrate potassium nitrate standard
standard solution
solution
(except for solution 4.11.2)
a
4.11.1 0 ml 0 mg 0 µg
4.11.2 3 ml of potassium nitrate diluted 0,012 mg 1,2 µg
stock solution (4.10)
4.11.3 1,0 ml 0,04 mg
4 µg
4.11.4 2,0 ml 0,08 mg
8 µg
4.11.5 3,0 ml 0,12 mg 12 µg
4.11.6 5,0 ml 0,20 mg 20 µg
4.11.7 10,0 ml 0,40 mg 40 µg
4.11.8 20,0 ml 0,80 mg
80 µg
4.11.9 30,0 ml 1,20 mg
120 µg
a
Zero member: The standard solution (4.11.1) is in fact the water (4.7) used for preparing the solutions.
5 Apparatus
5.1 General
The apparatus required for fusion of the test portion, and measurement of the carbon monoxide or dioxide
extracted, may be obtained commercially from a number of manufacturers. Follow the manufacturer's
instructions for the operation of the instrument.
5.2 Graphite crucible, single-use.
Use high-purity crucibles suited to the apparatus.
5.3 Crucible tongs, for handling the crucibles used.
5.4 Glass-wool filters.
5.5 Micropipette, 100 µl, the limit of error shall be less than 1 µl.
6 Sampling
Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel.
7 Procedure
SAFETY INSTRUCTIONS — The risk involved when using an apparatus for fusing the test portion are
mainly risks of burns. It is therefore necessary to use crucible tongs (5.3) and appropriate containers
for the used crucibles.
7.1 General instructions
Check that glass-wool filters (5.4) are clean and change them as often as necessary.
© ISO 2005 – All rights reserved 3
---------------------- Page: 7 ----------------------
ISO 17053:2005(E)
If the electricity supply has been switched off for a long time, allow the instrument to stabilize for the time
recommended by the manufacturer.
After changing the filters (5.4) and/or reagents (4.3, 4.4 and 4.5), or when the apparatus has been inoperative
for a period, stabilize the instrument by carrying out trial analyses, the results of which are to be disregarded.
Then proceed with blank, calibration and preparation tests, as indicated in 7.3, 7.4 and 7.5, before analysing
the sample.
If the instrument used provides a direct reading in per
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.