Metallic powders - Determination of oxygen content by reduction methods - Part 4: Total oxygen by reduction-extraction (ISO 4491-4:2019)

This document specifies a method for the determination of the total oxygen content of metallic powders by reduction-extraction at high temperature.
By agreement, this method is also applicable to the determination of the total oxygen content of sintered metal materials.
The method is applicable to all powders of metals, alloys, carbides, and mixtures thereof which are non-volatile under the test conditions. The sample can be in powder or compact form.
The analysis is carried out on the powder as supplied, but the method is not applicable if the powder contains a lubricant or binder. If such substances are present, the method may be used only if they can first be completely removed by a method not affecting the oxygen content of the powder.
This document is to be read in conjunction with ISO 4491-1.

Metallpulver - Bestimmung des Sauerstoffgehaltes durch Reduktionsverfahren - Teil 4: Gesamt-Sauerstoffgehalt durch Reduktionsextraktion (ISO 4491-4:2019)

Dieses Dokument legt ein Verfahren zur Bestimmung des Gesamt-Sauerstoffgehalts von Metallpulvern durch Reduktionsextraktion bei hoher Temperatur fest.
Nach Vereinbarung ist dieses Verfahren auch zur Bestimmung des Gesamt-Sauerstoffgehalts von Sinter-metallwerkstoffen anwendbar.
Dieses Verfahren gilt für alle Pulver aus Metallen, Legierungen, Carbiden und deren Mischungen, die unter den Prüfbedingungen nicht flüchtig sind. Die Probe kann im Pulverzustand oder als Presskörper vorliegen.
Die Analyse wird auf das Pulver im Anlieferungszustand angewendet, jedoch ist dieses Verfahren nicht anwendbar, wenn das Pulver Gleitmittel oder Bindemittel enthält. Sind derartige Substanzen vorhanden, darf das Verfahren nur dann angewendet werden, wenn diese Substanzen vorher vollständig durch ein Verfahren entfernt werden können, das den Sauerstoffgehalt des Pulvers nicht beeinträchtigt.
Dieses Dokument dient zur Verwendung in Verbindung mit ISO 4491-1.

Poudres métalliques - Dosage de l'oxygène par les méthodes de réduction - Partie 4: Oxygène total par réduction-extraction (ISO 4491-4:2019)

Le présent document spécifie une méthode de dosage de l'oxygène total présent dans les poudres métalliques. Cette méthode procède par réduction, puis extraction de l'échantillon à haute température.
Par accord, cette méthode peut également être appliquée au dosage de l'oxygène total dans les matériaux métalliques frittés.
La présente méthode est applicable à toutes les poudres de métaux, d'alliages, de carbures et de mélanges de ces composés non volatils dans les conditions de l'essai. L'échantillon peut se trouver à l'état de poudre ou de comprimé.
L'analyse est menée sur la poudre à l'état de livraison, mais la méthode n'est pas applicable si la poudre contient un lubrifiant ou un liant. Si de telles substances sont présentes, la méthode ne peut être utilisée que si ces substances peuvent être totalement éliminées au préalable par une méthode n'affectant pas la teneur de la poudre en oxygène.
Le présent document est prévu pour être utilisé conjointement avec l'ISO 4491-1.

Kovinski prah - Ugotavljanje deleža kisika z redukcijskimi metodami - 4. del: Skupni delež kisika z redukcijo-ekstrakcijo (ISO 4491-4:2019)

Ta dokument določa metodo za ugotavljanje skupnega deleža kisika v kovinskem prahu
z redukcijo-ekstrakcijo pri visoki temperaturi.
Po dogovoru se ta metoda uporablja tudi za ugotavljanje skupnega deleža kisika v sintranih
kovinskih materialih.
Metoda se uporablja za vse kovinske prahe, zlitine, karbide in njihove mešanice, ki so v preskusnih pogojih nehlapne. Vzorec je lahko v obliki prahu ali v trdni obliki.
Analiza se izvaja na dobavljenem prahu, vendar se metoda ne uporablja, če prah vsebuje mazivo ali vezivo. Če so takšne snovi prisotne, je mogoče metodo uporabiti samo, če je te snovi mogoče popolnoma odstraniti z metodo, ki ne vpliva na delež kisika v prahu.
Ta dokument se uporablja v povezavi s standardom ISO 4491-1.

General Information

Status
Published
Public Enquiry End Date
28-Feb-2019
Publication Date
21-May-2019
Technical Committee
I13 - Imaginarni 13
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
10-May-2019
Due Date
15-Jul-2019
Completion Date
22-May-2019

Relations

Effective Date
08-May-2019
Effective Date
21-Nov-2018

Overview

EN ISO 4491-4:2019 specifies a standardized laboratory method for measuring the total oxygen content of metallic powders by high-temperature reduction–extraction. The method is applicable to powders of metals, alloys, carbides and their mixtures that are non‑volatile under test conditions, and - by agreement - to sintered metal materials. This part of the ISO 4491 series is intended to be read in conjunction with ISO 4491‑1 (general guidelines).

Key topics and technical requirements

  • Principle: sample oxygen is converted to carbon oxides during high‑temperature reduction in a graphite crucible; the resulting CO or CO2 is extracted and quantitatively measured.
  • Test environments: extraction can be carried out under vacuum or in a flow of inert gas (e.g., nitrogen, argon, helium).
  • Reaction media & heating:
    • Dry (solid state) or metal bath (fusible metal to accelerate reduction).
    • Continuous heating (preheated crucible) or pulse heating (rapid high‑power pulse).
  • Apparatus & materials:
    • High‑purity graphite crucibles (individual or cumulative use).
    • Devices for crucible degassing, sample introduction, gas extraction, and a purification train to remove water.
    • Measuring systems for CO / CO2: volumetric, chromatography, infrared absorption, thermal conductivity, or coulometry.
    • Calibration gases (CO, CO2) or certified reference materials for instrument calibration.
  • Sample preparation:
    • Powder tested as supplied (unless lubricant/binder is present - must be completely removed without changing oxygen content).
    • Test portion can be weighed directly, compacted (uniaxial pressing without binders), or enclosed in a capsule.
  • Quality practice:
    • Carry out blank tests and calibration.
    • Use at least two test portions if no gauge repeatability and reproducibility (R&R) study is performed.
    • Report results with stated tolerances and test details.

Applications and who uses this standard

  • Powder metallurgy manufacturers and suppliers verifying oxygen limits in metal powders (iron, nickel, titanium, etc.).
  • Materials testing and QA/QC laboratories performing compositional control for powders and sintered parts.
  • R&D labs optimizing powder processing, sintering behavior and powder storage/handling.
  • Fabricators of additive manufacturing feedstocks where oxygen affects mechanical properties and powder stability.

Keywords: metallic powders, oxygen determination, reduction‑extraction, total oxygen, powder metallurgy, graphite crucible, CO, CO2, inert gas, calibration.

Related standards

  • ISO 4491‑1 - General guidelines for oxygen determination methods.
  • ISO 4491‑2 and ISO 4491‑3 - other reduction methods (note: these do not determine total oxygen; see ISO 4491‑4 for total oxygen by reduction‑extraction).
Standard

SIST EN ISO 4491-4:2019

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Frequently Asked Questions

SIST EN ISO 4491-4:2019 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Metallic powders - Determination of oxygen content by reduction methods - Part 4: Total oxygen by reduction-extraction (ISO 4491-4:2019)". This standard covers: This document specifies a method for the determination of the total oxygen content of metallic powders by reduction-extraction at high temperature. By agreement, this method is also applicable to the determination of the total oxygen content of sintered metal materials. The method is applicable to all powders of metals, alloys, carbides, and mixtures thereof which are non-volatile under the test conditions. The sample can be in powder or compact form. The analysis is carried out on the powder as supplied, but the method is not applicable if the powder contains a lubricant or binder. If such substances are present, the method may be used only if they can first be completely removed by a method not affecting the oxygen content of the powder. This document is to be read in conjunction with ISO 4491-1.

This document specifies a method for the determination of the total oxygen content of metallic powders by reduction-extraction at high temperature. By agreement, this method is also applicable to the determination of the total oxygen content of sintered metal materials. The method is applicable to all powders of metals, alloys, carbides, and mixtures thereof which are non-volatile under the test conditions. The sample can be in powder or compact form. The analysis is carried out on the powder as supplied, but the method is not applicable if the powder contains a lubricant or binder. If such substances are present, the method may be used only if they can first be completely removed by a method not affecting the oxygen content of the powder. This document is to be read in conjunction with ISO 4491-1.

SIST EN ISO 4491-4:2019 is classified under the following ICS (International Classification for Standards) categories: 77.160 - Powder metallurgy. The ICS classification helps identify the subject area and facilitates finding related standards.

SIST EN ISO 4491-4:2019 has the following relationships with other standards: It is inter standard links to SIST EN ISO 4491-4:2014, SIST EN ISO 4491-4:2014. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

You can purchase SIST EN ISO 4491-4:2019 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of SIST standards.

Standards Content (Sample)


SLOVENSKI STANDARD
01-julij-2019
Nadomešča:
SIST EN ISO 4491-4:2014
Kovinski prah - Ugotavljanje deleža kisika z redukcijskimi metodami - 4. del:
Skupni delež kisika z redukcijo-ekstrakcijo (ISO 4491-4:2019)
Metallic powders - Determination of oxygen content by reduction methods - Part 4: Total
oxygen by reduction-extraction (ISO 4491-4:2019)
Poudres métalliques - Dosage de l'oxygène par les méthodes de réduction - Partie 4:
Oxygène total par réduction-extraction (ISO 4491-4:2019)
Ta slovenski standard je istoveten z: EN ISO 4491-4:2019
ICS:
77.160 Metalurgija prahov Powder metallurgy
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 4491-4
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2019
EUROPÄISCHE NORM
ICS 77.160 Supersedes EN ISO 4491-4:2013
English Version
Metallic powders - Determination of oxygen content by
reduction methods - Part 4: Total oxygen by reduction-
extraction (ISO 4491-4:2019)
Poudres métalliques - Dosage de l'oxygène par les
méthodes de réduction - Partie 4: Oxygène total par
réduction-extraction (ISO 4491-4:2019)
This European Standard was approved by CEN on 25 April 2019.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4491-4:2019 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 4491-4:2019) has been prepared by Technical Committee ISO/TC 119 "Powder
metallurgy" in collaboration with Technical Committee CEN/SS M11 “Powder metallurgy” the
secretariat of which is held by CCMC.
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 November 2019, and conflicting national standards
shall be withdrawn at the latest by November 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 4491-4:2013.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 4491-4:2019 has been approved by CEN as EN ISO 4491-4:2019 without any
modification.
INTERNATIONAL ISO
STANDARD 4491-4
Third edition
2019-04
Metallic powders — Determination
of oxygen content by reduction
methods —
Part 4:
Total oxygen by reduction-extraction
Poudres métalliques — Dosage de l'oxygène par les méthodes de
réduction —
Partie 4: Oxygène total par réduction-extraction
Reference number
ISO 4491-4:2019(E)
©
ISO 2019
ISO 4491-4:2019(E)
© ISO 2019
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
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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 2019 – All rights reserved

ISO 4491-4:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Apparatus and materials. 2
6 Test portion . 3
7 Procedure. 3
7.1 General . 3
7.2 Blank test and calibration . 4
7.3 Test . 4
8 Expression of results . 4
8.1 Permissible tolerances . 4
8.2 Final result . 4
9 Test report . 4
Annex A (informative) Examples of conditions of extraction for selected metal powders .6
ISO 4491-4:2019(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 119, Powder metallurgy, Subcommittee
SC 2, Sampling and testing methods for powders (including powders for hardmetals).
This third edition cancels and replaces the second edition (ISO 4491-4:2013), of which it constitutes a
minor revision. The changes compared to the previous edition are as follows:
— addition of Clause 3 (Terms and definitions);
— Clause 6, changing from 0,1 mg to 0,000 1 g;
— changing carbon monoxide to CO and carbon dioxide to CO .
A list of all parts in the ISO 4491 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 2019 – All rights reserved

ISO 4491-4:2019(E)
Introduction
The determination of the oxygen content of metallic powders is of the utmost importance in many fields
of powder metallurgy.
The standard methods described in ISO 4491-2 and ISO 4491-3 do not give the total oxygen content of
the sample, as some oxygen-containing
...

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