Steel and cast iron - Determination of vanadium content - Potentiometric titration method (ISO 4947:2020)

This document specifies a potentiometric titration method for the determination of vanadium in steel
and cast iron.
The method is applicable to vanadium contents between 0,04 % (mass fraction) and 2 % (mass fraction).

Stahl und Gusseisen - Bestimmung des Vanadium-Gehaltes - Potentiometrisches Titrierverfahren (ISO 4947:2020)

Dieses Dokument legt ein Verfahren zur Bestimmung des Vanadiumgehalts in Stahl und Gusseisen mittels potentiometrischer Titration fest.
Das Verfahren ist anwendbar für die Bestimmung von Massenanteilen von Vanadium zwischen 0,04 % (Masseanteil) und 2 % (Masseanteil).

Aciers et fontes - Dosage du vanadium - Méthode par titrage potentiométrique (ISO 4947:2020)

Le présent document spécifie une méthode de détermination du vanadium par titrage potentiométrique dans l'acier et la fonte.
La méthode est applicable aux teneurs en vanadium comprises entre 0,04 % (en masse) et 2 % (en masse).

Jeklo in lito železo - Določevanje vanadija - Potenciometrijska metoda titracije (ISO 4947:2020)

General Information

Status
Published
Public Enquiry End Date
30-Oct-2019
Publication Date
28-Jul-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
23-Jul-2020
Due Date
27-Sep-2020
Completion Date
29-Jul-2020

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SLOVENSKI STANDARD
SIST EN ISO 4947:2020
01-oktober-2020
Nadomešča:
SIST EN 24947:1998
Jeklo in lito železo - Določevanje vanadija - Potenciometrijska metoda titracije (ISO
4947:2020)
Steel and cast iron - Determination of vanadium content - Potentiometric titration method
(ISO 4947:2020)
Stahl und Gusseisen - Bestimmung des Vanadium-Gehaltes - Potentiometrisches
Titrierverfahren (ISO 4947:2020)
Aciers et fontes - Dosage du vanadium - Méthode par titrage potentiométrique (ISO
4947:2020)
Ta slovenski standard je istoveten z: EN ISO 4947:2020
ICS:
77.080.01 Železne kovine na splošno Ferrous metals in general
SIST EN ISO 4947:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 4947:2020

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SIST EN ISO 4947:2020


EN ISO 4947
EUROPEAN STANDARD

NORME EUROPÉENNE

July 2020
EUROPÄISCHE NORM
ICS 77.080.01 Supersedes EN 24947:1991
English Version

Steel and cast iron - Determination of vanadium content -
Potentiometric titration method (ISO 4947:2020)
Acier et fonte - Détermination des teneurs en Stahl und Gusseisen - Bestimmung des Vanadium-
vanadium - Méthode par titrage potentiométrique (ISO Gehaltes - Potentiometrisches Titrierverfahren (ISO
4947:2020) 4947:2020)
This European Standard was approved by CEN on 9 May 2020.

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
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4947:2020 E
worldwide for CEN national Members.

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SIST EN ISO 4947:2020
EN ISO 4947:2020 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 4947:2020
EN ISO 4947:2020 (E)
European foreword
This document (EN ISO 4947:2020) 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 2021, and conflicting national standards shall
be withdrawn at the latest by January 2021.
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 24947:1991.
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 4947:2020 has been approved by CEN as EN ISO 4947:2020 without any modification.

3

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SIST EN ISO 4947:2020

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SIST EN ISO 4947:2020
INTERNATIONAL ISO
STANDARD 4947
Second edition
2020-06
Steel and cast iron — Determination of
vanadium content — Potentiometric
titration method
Acier et fonte — Détermination des teneurs en vanadium — Méthode
par titrage potentiométrique
Reference number
ISO 4947:2020(E)
©
ISO 2020

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SIST EN ISO 4947:2020
ISO 4947:2020(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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved

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SIST EN ISO 4947:2020
ISO 4947:2020(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 . 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 Oxidation of chromium and vanadium . 4
8.3.3 Preparation of the solution for titration . 4
8.3.4 Oxidation of vanadium . . . 5
8.4 Titration . 5
9 Expression of results . 6
9.1 Method of calculation . 6
9.2 Precision . 6
10 Test report . 6
Annex A (informative) Additional information on the international interlaboratory test.8
Annex B (informative) Graphical representation of precision data . 9
Bibliography .10
© ISO 2020 – All rights reserved iii

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SIST EN ISO 4947:2020
ISO 4947:2020(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 4947:1986), which has been technically
revised. The main changes compared to the previous edition are as follows:
— introduction of an optional electrode;
— re-assessment of 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 2020 – All rights reserved

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SIST EN ISO 4947:2020
INTERNATIONAL STANDARD ISO 4947:2020(E)
Steel and cast iron — Determination of vanadium content
— Potentiometric titration method
1 Scope
This document specifies a potentiometric titration method for the determination of vanadium in steel
and cast iron.
The method is applicable to vanadium contents between 0,04 % (mass fraction) and 2 % (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 385, Laboratory glassware — Burettes
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 http:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle
Dissolution of a test portion with appropriate acids. Addition of hydrofluoric acid to keep tungsten in
solution.
Oxidation of chromium and vanadium by potassium peroxydisulfate. Partial oxida
...

SLOVENSKI STANDARD
oSIST prEN ISO 4947:2019
01-oktober-2019
Jeklo in lito železo - Določanje vanadija - Potenciometrijska metoda titracije
(ISO/DIS 4947:2019)
Steel and cast iron - Determination of vanadium content - Potentiometric titration method
(ISO/DIS 4947:2019)
Stahl und Gusseisen - Bestimmung des Vanadium-Gehaltes - Potentiometrisches
Titrierverfahren (ISO/DIS 4947:2019)
Aciers et fontes - Dosage du vanadium - Méthode par titrage potentiométrique (ISO/DIS
4947:2019)
Ta slovenski standard je istoveten z: prEN ISO 4947
ICS:
77.080.01 Železne kovine na splošno Ferrous metals in general
oSIST prEN ISO 4947:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 4947:2019

---------------------- Page: 2 ----------------------
oSIST prEN ISO 4947:2019
DRAFT INTERNATIONAL STANDARD
ISO/DIS 4947
ISO/TC 17/SC 1 Secretariat: JISC
Voting begins on: Voting terminates on:
2019-08-16 2019-11-08
Steel and cast iron — Determination of vanadium content
— Potentiometric titration method
Aciers et fontes — Dosage du vanadium — Méthode par titrage potentiométrique
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 4947:2019(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 2019

---------------------- Page: 3 ----------------------
oSIST prEN ISO 4947:2019
ISO/DIS 4947:2019(E)

COPYRIGHT PROTECTED DOCUMENT
© 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
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 2019 – All rights reserved

---------------------- Page: 4 ----------------------
oSIST prEN ISO 4947:2019
ISO/DIS 4947:2019(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
5 Apparatus . 3
6 Sampling . 3
7 Procedure. 3
7.1 Test Portion . 3
7.2 Blank test . 3
7.3 Determination . 4
7.3.1 Preparation of the test solution . 4
7.3.2 Oxidation of chromium and vanadium . 4
7.3.3 Preparation of the solution for measurement . 4
7.3.4 Oxidation of vanadium . . . 5
7.4 Titration . 5
8 Expression of results . 5
8.1 Method of calculation . 5
8.2 Precision . 6
9 Test report . 6
Annex A (informative) Additional information on the international interlaboratory test.7
Annex B (informative) Graphical representation of precision data . 8
Bibliography . 9
© ISO 2019 – All rights reserved iii

---------------------- Page: 5 ----------------------
oSIST prEN ISO 4947:2019
ISO/DIS 4947:2019(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. 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 WTO principles in the Technical
Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information
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 4947:1986), which has been revised in
order to re-assess the precision data.
iv © ISO 2019 – All rights reserved

---------------------- Page: 6 ----------------------
oSIST prEN ISO 4947:2019
DRAFT INTERNATIONAL STANDARD ISO/DIS 4947:2019(E)
Steel and cast iron — Determination of vanadium content
— Potentiometric titration method
1 Scope
This International Standard specifies a potentiometric titration method for the determination of
vanadium in steel and cast iron.
The method is applicable to vanadium contents between 0,04 % (mass fraction) to 2 % (mass fraction).
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 385, Laboratory glassware - Burettes
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 Principle
Dissolution of a test portion with appropriate acids. Addition of hydrofluoric acid to keep tungsten in
solution.
Oxidation of chromium and vanadium by potassium peroxydisulfate. Partial oxidation of chromium.
While checking the potential of the solution:
— reduction of chromium(VI) and vanadium(V) by ammonium iron(II) sulphate;
— oxidation of vanadium by a slight excess of potassium permanganate; reduction of the excess of
permanganate by sodium nitrite, and reduction of the excess of sodium nitrite by sulfamic acid.
Potentiometric titration of vanadium with an ammonium iron(II) sulfate standard solution.
4 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 2 water as specified in ISO 3696, free from reducing or oxidizing activity.
4.1 Potassium peroxydisulfate (K S O ).
2 2 8
4.2 Hydrochlorit acid, ρ = 1,19 g/ml approximately.
4.3 Nitrit acid, ρ = 1,40 g/ml approximately.
© ISO 2019 – All rights reserved 1

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oSIST prEN ISO 4947:2019
ISO/DIS 4947:2019(E)

4.4 Hydrofluoric acid, ρ = 1,15 g/ml approximately.
4.5 Sulfuric acid, ρ = 1,84 g/ml approximately, diluted 1 + 4.
4.6 Sulfuric acid, ρ = 1,84 g/ml approximately, diluted 1 + 50.
4.7 Orthophosphoric acid, ρ = 1,70 g/ml approximately.
4.8 Ammonium iron(II) sulfate [Fe(NH ) (S0 ) ·6H 0] solution in sulfuric acid medium.
4 2 4 2 2
Dissolve 40 g of ammonium iron(II) sulfate hexahydrate in approximately 500 ml of water, add 20 ml
of sulfuric acid, ρ 1,84 g/ml approximately, cool, make up the volume to 1 000 ml with water and mix.
4.9 Potassium permanganate, 5 g/l.
4.10 Sodium nitrite, 3 g/l.
4.11 Sulfamic acid (NH SO H), 100 g/l.
2 3
This solution is stable for only one week.
4.12 Potassium dichromate, standard solution.
Weigh, to the nearest 0,001 g, approximately 1 g of potassium dichromate (high purity grade) previously
dried at 150 °C until a co
...

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