SIST EN ISO 9647:2022
(Main)Steel - Determination of vanadium content - Flame atomic absorption spectrometric method (FAAS) (ISO 9647:2020)
Steel - Determination of vanadium content - Flame atomic absorption spectrometric method (FAAS) (ISO 9647:2020)
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the vanadium content in steel.
The method is applicable to vanadium contents between 0,01 % (mass fraction) and 0,80 % (mass fraction), provided that the tungsten content in a 1,0 g test portion is not higher than 1,0 % and/or the titanium content is not higher than 0,5 %.
Stahl - Bestimmung des Vanadiumgehaltes - Flammen-Atomextinktionsspektrometrisches Verfahren (FAAS) (ISO 9647:2020)
Dieses Dokument legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS) zur Bestimmung des Vanadiumgehalts in Stahl fest.
Das Verfahren ist für Vanadiumgehalte zwischen 0,01 % (Massenanteil) und 0,80 % (Massenanteil) anwendbar, vorausgesetzt, der Wolframgehalt in einer 1,0-g-Prüfportion ist nicht höher als 1,0 % und/oder der Titangehalt ist nicht höher als 0,5 %.
Aciers - Détermination des teneurs en vanadium - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF) (ISO 9647:2020)
Le présent document spécifie une méthode par spectrométrie d'absorption atomique dans la flamme (SAAF) pour la détermination des teneurs en vanadium dans l'acier.
La méthode est applicable aux teneurs en vanadium comprises entre 0,01 % (en masse) et 0,80 % (en masse), sous réserve que la teneur en tungstène dans une prise d'essai de 1,0 g ne soit pas supérieure à 1,0 % et/ou que la teneur en titane ne soit pas supérieure à 0,5 %.
Jeklo - Določevanje vanadija - Metoda s plamensko atomsko absorpcijsko spektrometrijo (FAAS) (ISO 9647:2020)
Ta dokument določa metodo s plamensko atomsko absorpcijsko spektrometrijo (FAAS) za določevanje vanadija v jeklu.
Metoda se uporablja za vsebnosti vanadija med 0,01 % (masni delež) in 0,80 % (masni delež) pod pogojem, da vsebnost volframa v preskusni količini 1,0 g ni višja od 1,0 % in/ali vsebnost titana ne presega 0,5 %.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 9647:2022
01-maj-2022
Jeklo - Določevanje vanadija - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (FAAS) (ISO 9647:2020)
Steel - Determination of vanadium content - Flame atomic absorption spectrometric
method (FAAS) (ISO 9647:2020)
Stahl - Bestimmung des Vanadiumgehaltes - Flammen-
Atomextinktionsspektrometrisches Verfahren (FAAS) (ISO 9647:2020)
Aciers - Détermination des teneurs en vanadium - Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF) (ISO 9647:2020)
Ta slovenski standard je istoveten z: EN ISO 9647:2022
ICS:
77.080.20 Jekla Steels
SIST EN ISO 9647:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST EN ISO 9647:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 9647:2022
EN ISO 9647
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2022
EUROPÄISCHE NORM
ICS 77.080.01
English Version
Steel - Determination of vanadium content - Flame atomic
absorption spectrometric method (FAAS) (ISO 9647:2020)
Aciers - Détermination des teneurs en vanadium - Stahl - Bestimmung des Vanadiumgehaltes - Flammen-
Méthode par spectrométrie d'absorption atomique Atomextinktionsspektrometrisches Verfahren (FAAS)
dans la flamme (SAAF) (ISO 9647:2020) (ISO 9647:2020)
This European Standard was approved by CEN on 20 March 2022.
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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 9647:2022 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 9647:2022
EN ISO 9647:2022 (E)
Contents Page
European foreword . 3
2
---------------------- Page: 4 ----------------------
SIST EN ISO 9647:2022
EN ISO 9647:2022 (E)
European foreword
The text of ISO 9647:2020 has been prepared by Technical Committee ISO/TC 17 "Steel” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 9647:2022 by
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 September 2022, and conflicting national standards
shall be withdrawn at the latest by September 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.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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 9647:2020 has been approved by CEN as EN ISO 9647:2022 without any modification.
3
---------------------- Page: 5 ----------------------
SIST EN ISO 9647:2022
---------------------- Page: 6 ----------------------
SIST EN ISO 9647:2022
INTERNATIONAL ISO
STANDARD 9647
Second edition
2020-02
Steel — Determination of vanadium
content — Flame atomic absorption
spectrometric method (FAAS)
Aciers — Détermination des teneurs en vanadium — Méthode par
spectrométrie d'absorption atomique dans la flamme (SAAF)
Reference number
ISO 9647:2020(E)
©
ISO 2020
---------------------- Page: 7 ----------------------
SIST EN ISO 9647:2022
ISO 9647:2020(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: 8 ----------------------
SIST EN ISO 9647:2022
ISO 9647:2020(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
6.1 Atomic absorption spectrometer . 3
6.1.1 Minimum precision (see Annex C) . 3
6.1.2 Limit of detection (see Annex C) . 3
6.1.3 Calibration linearity (see Annex C) . 3
6.1.4 Characteristic concentration (see Annex C) . 3
6.2 Ancillary equipment . 4
7 Sampling . 4
8 Procedure. 4
8.1 Test portion . 4
8.2 Blank test . 4
8.3 Determination . 4
8.3.1 Preparation of the test solution . 4
8.3.2 Preparation of the calibration solutions . 4
8.3.3 Adjustment of the atomic absorption spectrometer. 5
8.3.4 Spectrometric measurements . 6
9 Expression of results . 7
9.1 Use of the calibration curve . 7
9.2 Use of bracketing method . 8
10 Precision . 8
11 Test report . 9
Annex A (informative) Additional information on the international interlaboratory test.10
Annex B (informative) Graphical representation of precision data .13
Annex C (normative) Procedures for the determination of instrumental criteria.14
Bibliography .16
© ISO 2020 – All rights reserved iii
---------------------- Page: 9 ----------------------
SIST EN ISO 9647:2022
ISO 9647:2020(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 on 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 the following URL: 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 9647:1989), which has been technically
revised. The main changes compared to the previous edition are as follows:
— a complete revaluation of the precision data;
— amendment of the field of application.
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
---------------------- Page: 10 ----------------------
SIST EN ISO 9647:2022
INTERNATIONAL STANDARD ISO 9647:2020(E)
Steel — Determination of vanadium content — Flame
atomic absorption spectrometric method (FAAS)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of the vanadium content in steel.
The method is applicable to vanadium contents between 0,01 % (mass fraction) and 0,80 % (mass
fraction), provided that the tungsten content in a 1,0 g test portion is not higher than 1,0 % and/or the
titanium content is not higher than 0,5 %.
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
Dissolution of a test portion in hydrochloric, nitric and perchloric acids.
Addition of an aluminium chloride solution as spectrochemical buffer.
Nebulisation of the test solution into an acetylene/nitrous oxide flame of an atomic absorption
spectrometer.
Spectrometric measurement of the atomic absorption of the 318,4 nm spectral line emitted by a
vanadium hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used.
© ISO 2020 – All rights reserved 1
---------------------- Page: 11 ----------------------
SIST EN ISO 9647:2022
ISO 9647:2020(E)
5 Reagents
During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and
only grade 2 water as specified in ISO 3696.
5.1 Pure iron, containing <0,000 5 % of vanadium or of low and known vanadium content.
5.2 Hydrochloric acid, ρ approximately 1,19 g/ml.
5.3 Nitric acid, ρ approximately 1,40 g/ml.
5.4 Perchloric acid, ρ approximately 1,67 g/ml.
WARNING — Perchloric acid vapour can cause explosions in the presence of ammonia, nitrous
fumes or organic material in general.
5.5 Hydrochloric acid solution, 1 + 50.
Add 10 ml of hydrochloric acid (5.2) to 500 ml of water and mix.
5.6 Aluminium solution, 20 g/l.
Dissolve 90 g of aluminium chloride hexahydrate (AlCl ·6H O) in about 300 ml of water, add 5 ml of
3 2
hydrochloric acid (5.2), dilute to 500 ml with water and mix.
5.7 Vanadium standard solution, 2,0 g/l.
5.7.1 Preparation using vanadium metal
Weigh (1,000 ± 0,001) g of vanadium (V ≥ 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of a
mixture of three volumes of hydrochloric acid (5.2) and one volume of nitric acid (5.3).
Cover with a watch glass and if necessary, heat gently to assist dissolution. When dissolution is complete
evaporate the solution to just before dryness and add 20 ml of hydrochloric acid (5.2).
Allow to cool to room temperature and transfer the solution quantitatively into a 500 ml one-mark
volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 2,0 mg of vanadium.
5.7.2 Preparation using ammonium metavanadate
Dry several grams of ammonium metavanadate (NH VO ) (purity >99,9 %) in an oven at 100 °C to
4 3
105 °C for at least one hour and allow to cool to room temperature in a desiccator.
NOTE A drying temperature over 110 °C will cause decomposition of ammonium metavanadate. Keep
strictly to the drying temperature specified.
Weight 2,296 g of the dried product into a 600 ml beaker, add about 400 ml of hot water and gently
simmer to dissolve.
Allow to cool, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
1 ml of this solution contains 2,0 mg of vanadium.
2 © ISO 2020 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 9647:2022
ISO 9647:2020(E)
5.8 Vanadium standard solution, 0,08 g/l.
Transfer 10,0 ml of vanadium standard solution (5.7) into a 250 ml one-mark volumetric flask. Dilute to
the mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,08 mg of vanadium.
6 Apparatus
All volumetric glassware shall be class A, in accordance with ISO 648 or ISO 1042, as appropriate.
Ordinary laboratory apparatus and the following shall be used.
6.1 Atomic absorption spectrometer
The spectrometer shall be equipped with a vanadium hollow-cathode lamp and supplied with dinitrogen
monoxide and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil,
and free from vanadium.
The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.3,
the limit of detection and characteristic concentration are in reasonable agreement with the values
given by the manufacturer and it meets the performance criteria given in 6.1.1 to 6.1.3.
The instrument should also conform to the additional performance requirement given in 6.1.4.
6.1.1 Minimum precision (see Annex C)
The standard deviation of 10 measurements of the absorbance of the most concentrated calibration
...
SLOVENSKI STANDARD
oSIST prEN ISO 9647:2022
01-januar-2022
Jeklo - Določevanje vanadija - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (FAAS) (ISO 9647:2020)
Steel - Determination of vanadium content - Flame atomic absorption spectrometric
method (FAAS) (ISO 9647:2020)
Stahl - Bestimmung des Vanadiumgehaltes - Flammen-
Atomextinktionsspektrometrisches Verfahren (FAAS) (ISO 9647:2020)
Aciers - Détermination des teneurs en vanadium - Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF) (ISO 9647:2020)
Ta slovenski standard je istoveten z: prEN ISO 9647
ICS:
77.080.20 Jekla Steels
oSIST prEN ISO 9647:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
oSIST prEN ISO 9647:2022
---------------------- Page: 2 ----------------------
oSIST prEN ISO 9647:2022
INTERNATIONAL ISO
STANDARD 9647
Second edition
2020-02
Steel — Determination of vanadium
content — Flame atomic absorption
spectrometric method (FAAS)
Aciers — Détermination des teneurs en vanadium — Méthode par
spectrométrie d'absorption atomique dans la flamme (SAAF)
Reference number
ISO 9647:2020(E)
©
ISO 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 9647:2022
ISO 9647:2020(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 9647:2022
ISO 9647:2020(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
6.1 Atomic absorption spectrometer . 3
6.1.1 Minimum precision (see Annex C) . 3
6.1.2 Limit of detection (see Annex C) . 3
6.1.3 Calibration linearity (see Annex C) . 3
6.1.4 Characteristic concentration (see Annex C) . 3
6.2 Ancillary equipment . 4
7 Sampling . 4
8 Procedure. 4
8.1 Test portion . 4
8.2 Blank test . 4
8.3 Determination . 4
8.3.1 Preparation of the test solution . 4
8.3.2 Preparation of the calibration solutions . 4
8.3.3 Adjustment of the atomic absorption spectrometer. 5
8.3.4 Spectrometric measurements . 6
9 Expression of results . 7
9.1 Use of the calibration curve . 7
9.2 Use of bracketing method . 8
10 Precision . 8
11 Test report . 9
Annex A (informative) Additional information on the international interlaboratory test.10
Annex B (informative) Graphical representation of precision data .13
Annex C (normative) Procedures for the determination of instrumental criteria.14
Bibliography .16
© ISO 2020 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 9647:2022
ISO 9647:2020(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 on 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 the following URL: 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 9647:1989), which has been technically
revised. The main changes compared to the previous edition are as follows:
— a complete revaluation of the precision data;
— amendment of the field of application.
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
---------------------- Page: 6 ----------------------
oSIST prEN ISO 9647:2022
INTERNATIONAL STANDARD ISO 9647:2020(E)
Steel — Determination of vanadium content — Flame
atomic absorption spectrometric method (FAAS)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of the vanadium content in steel.
The method is applicable to vanadium contents between 0,01 % (mass fraction) and 0,80 % (mass
fraction), provided that the tungsten content in a 1,0 g test portion is not higher than 1,0 % and/or the
titanium content is not higher than 0,5 %.
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
Dissolution of a test portion in hydrochloric, nitric and perchloric acids.
Addition of an aluminium chloride solution as spectrochemical buffer.
Nebulisation of the test solution into an acetylene/nitrous oxide flame of an atomic absorption
spectrometer.
Spectrometric measurement of the atomic absorption of the 318,4 nm spectral line emitted by a
vanadium hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used.
© ISO 2020 – All rights reserved 1
---------------------- Page: 7 ----------------------
oSIST prEN ISO 9647:2022
ISO 9647:2020(E)
5 Reagents
During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and
only grade 2 water as specified in ISO 3696.
5.1 Pure iron, containing <0,000 5 % of vanadium or of low and known vanadium content.
5.2 Hydrochloric acid, ρ approximately 1,19 g/ml.
5.3 Nitric acid, ρ approximately 1,40 g/ml.
5.4 Perchloric acid, ρ approximately 1,67 g/ml.
WARNING — Perchloric acid vapour can cause explosions in the presence of ammonia, nitrous
fumes or organic material in general.
5.5 Hydrochloric acid solution, 1 + 50.
Add 10 ml of hydrochloric acid (5.2) to 500 ml of water and mix.
5.6 Aluminium solution, 20 g/l.
Dissolve 90 g of aluminium chloride hexahydrate (AlCl ·6H O) in about 300 ml of water, add 5 ml of
3 2
hydrochloric acid (5.2), dilute to 500 ml with water and mix.
5.7 Vanadium standard solution, 2,0 g/l.
5.7.1 Preparation using vanadium metal
Weigh (1,000 ± 0,001) g of vanadium (V ≥ 99,9 %) and transfer it into a 400 ml beaker. Add 30 ml of a
mixture of three volumes of hydrochloric acid (5.2) and one volume of nitric acid (5.3).
Cover with a watch glass and if necessary, heat gently to assist dissolution. When dissolution is complete
evaporate the solution to just before dryness and add 20 ml of hydrochloric acid (5.2).
Allow to cool to room temperature and transfer the solution quantitatively into a 500 ml one-mark
volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 2,0 mg of vanadium.
5.7.2 Preparation using ammonium metavanadate
Dry several grams of ammonium metavanadate (NH VO ) (purity >99,9 %) in an oven at 100 °C to
4 3
105 °C for at least one hour and allow to cool to room temperature in a desiccator.
NOTE A drying temperature over 110 °C will cause decomposition of ammonium metavanadate. Keep
strictly to the drying temperature specified.
Weight 2,296 g of the dried product into a 600 ml beaker, add about 400 ml of hot water and gently
simmer to dissolve.
Allow to cool, transfer the solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
1 ml of this solution contains 2,0 mg of vanadium.
2 © ISO 2020 – All rights reserved
---------------------- Page: 8 ----------------------
oSIST prEN ISO 9647:2022
ISO 9647:2020(E)
5.8 Vanadium standard solution, 0,08 g/l.
Transfer 10,0 ml of vanadium standard solution (5.7) into a 250 ml one-mark volumetric flask. Dilute to
the mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,08 mg of vanadium.
6 Apparatus
All volumetric glassware shall be class A, in accordance with ISO 648 or ISO 1042, as appropriate.
Ordinary laboratory apparatus and the following shall be used.
6.1 Atomic absorption spectrometer
The spectrometer shall be equipped with a vanadium hollow-cathode lamp and supplied with dinitrogen
monoxide and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil,
and free from vanadium.
The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.3,
the limit of detection and characteristic concentration are in reasonable agreement with the values
given by the manufacturer and it meets the performance criteria given in 6.1.1 to 6.1.3.
The instrument should also conform to the additional performance requirement given in 6.1.4.
6.1.1 Minimum precision (see Annex C)
The standard deviation of 10 measurements of the absorbance of the most concentrated calibration
solution shall not exceed 1,0 % of the mean absorbance of this solution.
The standard deviation of 10 measurements of the absorbance of the least concentrated calibration
solution (excluding the zero member) shall not exceed 0,5 % of the mean absorbance of the most
concentrated calibration solution.
6.1.2 Limit of detection (see Annex C)
The limit of detection is a number, expressed in units of concentration (or amount) that describes the
lowest concentration level (or amount) of an element that can be determined to be statistically different
from an analytical blank.
The limit of detection of vanadium in a matrix similar to the final test solution shall be less than 0,3 µg/ml.
6.1.3 Calibration linearity (see Annex C)
The slope of the calibration line covering the top 20 % of the concentration range (expressed as a
change in absorbance) shall not be less than 0,7 times the value of the slope for the bottom 20 % of the
concentration range determined in the same way.
For instruments with automatic calibration using two or more standard solutions, it shall be established
prior to the analysis, by obtaining absorbance readings, that the above requirements for calibration
linearity are fulfilled.
6.1.4 Characteristic concentration (see Annex C)
The characteristic concentration for vanadium in a matrix similar to the final test solution shall be
greater than 1 µg/ml.
© ISO 2020 – All rights reserved 3
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oSIST prEN ISO 9647:2022
ISO 9647:2020(E)
6.2 Ancillary equipment
Scale expansion can be used until the noise observed is greater than the readout error and is always
recommended for absorbances below 0,1. If scale expansion has to be used and the instrument does not
have the means to read the value of the scale expansion factor, the value can be calculated by measuring
a suitable solution with and without scale expansion and then dividing the signals obtained.
7 Sampling
Carry out sampling in accordance with ISO 14284 or appropriate national standards for steels.
8 Procedure
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