Steels - Determination of niobium - Spectrophotometric method

This document specifies a spectrophotometric method for the determination of niobium in steels.
The method is applicable to all grades of steels with niobium contents up to 1,3 % (by mass), with a lower limit of detection of 0,002 % (by mass).

Stähle - Bestimmung von Niob - Photometrisches Verfahren

Dieses Dokument legt ein photometrisches Verfahren zur Bestimmung von Niob in Stählen fest.
Das Verfahren ist anwendbar für alle Stahlsorten mit Niobgehalten bis zu 1,3 Masse-%, mit einer unteren Nachweisgrenze von 0,002 % (Masse).

Aciers - Détermination du niobium - Méthode spectrophotométrique

Le présent document spécifie une méthode spectrophotométrique de détermination du niobium dans les aciers.
La méthode est applicable à tous les types d’acier pour des teneurs en niobium allant jusqu’à 1,3 % (en masse), avec une limite inférieure de détection de 0,002 % (en masse).

Jekla - Določevanje niobija - Spektrofotometrična metoda

General Information

Status
Published
Public Enquiry End Date
09-Sep-2023
Publication Date
01-Jul-2024
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
27-Jun-2024
Due Date
01-Sep-2024
Completion Date
02-Jul-2024

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SLOVENSKI STANDARD
01-september-2024
Jekla - Določevanje niobija - Spektrofotometrična metoda
Steels - Determination of niobium - Spectrophotometric method
Stähle - Bestimmung von Niob - Photometrisches Verfahren
Aciers - Détermination du niobium - Méthode spectrophotométrique
Ta slovenski standard je istoveten z: EN 10178:2024
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 10178
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2024
EUROPÄISCHE NORM
ICS 77.040.30 Supersedes EN 10178:1989
English Version
Steels - Determination of niobium - Spectrophotometric
method
Aciers - Détermination du niobium - Méthode Stähle - Bestimmung von Niob - Photometrisches
spectrophotométrique Verfahren
This European Standard was approved by CEN on 29 April 2024.

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, Türkiye 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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 10178:2024 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 6
7 Sampling . 6
8 Procedure . 6
8.1 Test portion . 6
8.2 Blank test . 6
8.3 Determination . 6
8.3.1 Preparation of the test solution . 6
8.3.2 Separation of the niobium . 6
8.3.3 Development of the colour . 7
8.3.4 Spectrophotometric measurement . 7
8.4 Establishment of the calibration curve . 7
8.4.1 Preparation of the calibration solutions . 7
8.4.2 Spectrophotometric measurements . 8
8.4.3 Plotting the calibration curve . 8
9 Expression of results . 9
10 Test report . 9
Annex A (informative) Precision data . 11
Bibliography . 12

European foreword
This document (EN 10178:2024) has been prepared 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 December 2024, and conflicting national standards shall
be withdrawn at the latest by December 2024.
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 10178:1989.
In comparison with the previous edition, the following technical modifications have been made:
— normative references: updated;
— Clause 3 Terms and definitions: added;
— reference 5.13: added;
— reference 5.18: title simplified;
— Clause 6: developed and subclauses 6.1 and 6.2, added;
— Clause 7: updated;
— former subclause 7.3.3: included in 8.3.2;
— Clause 10: updated;
— Bibliography: added.
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 organisations 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, Türkiye and the United
Kingdom.
1 Scope
This document specifies a spectrophotometric method for the determination of niobium in steels.
The method is applicable to all grades of steels with niobium contents up to 1,3 % (by mass), with a lower
limit of detection of 0,002 % (by mass).
The precision data of the present method are given in Annex A.
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.
EN ISO 648, Laboratory glassware — Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)
EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition (ISO 14284)
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
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 https://www.electropedia.org/
4 Principle
Dissolution of a test portion with hydrochloric acid followed by oxidation with hydrogen peroxide.
Precipitation of niobium and tantalum with phenylarsonic acid using zirconium as a carrier.
Formation of a complex of niobium with 4-(2-pyridylazo)-resorcinol (PAR) in a buffered sodium tartrate
medium.
Spectrophotometric measurement of the coloured compound at a wavelength of 550 nm.
5 Reagents
5.1 General
During analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 2 water as specified in EN ISO 3696 or water of equivalent purity.
5.2 Iron, of high purity, free from niobium
5.3 Potassium hydrogen sulphate (KHSO )
5.4 Hydrochloric acid, ρ 1,19 g/ml approximately
5.5 Hydrochloric acid, solution 1 + 4
Carefully add 40 ml of hydrochloric acid (5.4) to 160 ml of water and mix.
5.6 Hydrochloric acid, solution 1 + 9
Carefully add 20 ml of hydrochloric acid (5.4)
...


SLOVENSKI STANDARD
oSIST prEN 10178:2023
01-september-2023
Jekla - Določevanje niobija - Spektrofotometrična metoda
Steels - Determination of niobium - Spectrophotometric method
Stähle - Bestimmung von Niob - Photometrisches Verfahren
Aciers - Détermination du niobium - Méthode spectrophotométrique
Ta slovenski standard je istoveten z: prEN 10178
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
oSIST prEN 10178:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

oSIST prEN 10178:2023
oSIST prEN 10178:2023
DRAFT
EUROPEAN STANDARD
prEN 10178
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2023
ICS 77.040.30 Will supersede EN 10178:1989
English Version
Steels - Determination of niobium - Spectrophotometric
method
Aciers - Détermination du niobium - Méthode Stählen - Bestimmung von Niob - Photometrisches
spectrophotométrique Verfahren
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 459/SC 2.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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, Türkiye and
United Kingdom.
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.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 10178:2023 E
worldwide for CEN national Members.

oSIST prEN 10178:2023
prEN 10178:2023 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
5.1 General. 4
6 Apparatus . 6
7 Sampling . 6
8 Procedure . 6
8.1 Test portion . 6
8.2 Blank test . 6
8.3 Determination . 6
8.3.1 Preparation of the test solution . 6
8.3.2 Separation of the niobium . 6
8.3.3 Development of the colour . 7
8.3.4 Spectrophotometric measurement . 7
8.4 Establishment of the calibration curve . 7
8.4.1 Preparation of the calibration solutions . 7
8.4.2 Spectrophotometric measurements . 8
8.4.3 Plotting the calibration curve . 8
9 Expression of results . 8
10 Test report . 9
Annex A (informative) Precision data . 10
Bibliography . 11

oSIST prEN 10178:2023
prEN 10178:2023 (E)
European foreword
This document (prEN 10178:2023) has been prepared 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 document is currently submitted to the CEN Enquiry.
This document will supersede EN 10178:1989.
In comparison with the previous edition, the following technical modifications have been made:
— Normative references: updated;
— Clause 3 Terms and definitions: added;
— Reference 5.13: added;
— Reference 5.18: title simplified;
— Clause 6: developed and sub Clauses 6.1 and 6.2, added;
— Clause 7: updated;
— Former sub Clause 7.3.3: included in 8.3.2;
— Clause 10: updated;
— Bibliography: added.
oSIST prEN 10178:2023
prEN 10178:2023 (E)
1 Scope
This document specifies a spectrophotometric method for the determination of niobium in steels.
The method is applicable to all grades of steels with niobium contents up to 1,3 % (by mass), with a lower
limit of detection of 0,002 % (by mass).
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.
EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042)
EN ISO 14284, Steel and iron - Sampling and preparation of samples for the determination of chemical
composition (ISO 14284)
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:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle
Dissolution of a test portion with hydrochloric acid followed by oxidation with hydrogen peroxide.
Precipitation of niobium and tantalum with phenylarsonic acid using zirconium as a carrier.
Formation of a complex of niobium with 4-(2-pyridylazo)-resorcinol (PAR) in a buffered sodium tartrate
medium.
Spectrophotometric measurement of the coloured compound at a wavelength of 550 nm.
5 Reagents
5.1 General
During analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 2 water as specified in ISO 3696 or water of equivalent purity.
5.2 Iron, of high purity, free from niobium
5.3 Potassium hydrogen sulphate (KHSO )
5.4 Hydrochloric acid, ρ 1,19 g/ml approximately
5.5 Hydrochloric acid, solution 1 + 4
Carefully add 40 ml of hydrochloric acid (5.4) to 160 ml of water and mix.
oSIST prEN 10178:2023
prEN 10178:2023 (E)
5.6 Hydrochloric acid, solution 1 + 9
Carefully add 20 ml of hydrochloric acid (5.4) to 180 ml of water and mix.
5.7 Sulphuric acid, solution 1 + 1
Carefully add 100 ml of sulphuric acid (ρ 1,84 g/ml approximately) to 200 ml of water.
Allow to cool and mix.
5.8 Sulphuric acid, solution 1 + 4
Carefully add 20 ml of sulphuric acid (ρ 1,84 g/ml approximately) to 80 ml of water.
Allow to cool and mix.
5.9 Ethylenediaminetetraacetic acid di-sodium salt, (EDTA Na ), 15 g/l solution
St
...

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