Steel and iron - Determination of cobalt content - Flame atomic absorption spectrometric method (ISO 11652:1997)

This International Standard specifies a flame atomic absorption spectrometric method for the
determination of the cobalt content in steel and iron.
The method is applicable to cobalt contents between 0,003 % (m/m) and 5,0 % (m/m).

Stahl und Eisen - Bestimmung des Cobaltgehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (ISO 11652:1997)

Diese Internationale Norm legt ein flammenatomabsorptionsspektrometrisches Verfahren zur Bestimmung des Cobaltgehaltes in Stahl und Eisen fest.
Das Verfahren ist anwendbar auf Cobaltgehalte zwischen 0,003 % Massenanteil und 5,0 % Massenanteil.

Aciers et fontes - Dosage du cobalt - Méthode par spectrométrie d'absorption atomique dans la flamme (ISO 11652:1997)

L'IEC 61910-1:2014 s'applique aux rapports structures sur la dose de rayonnement générés par l'appareil a rayonnement X entrant dans le domaine d'application de l'IEC 60601-2-43:2010 ou de l'IEC 60601-2-54:2009. Le présent document n'impose aucune exigence particulière quant à l'exactitude des données consignées ou affichées. Les normes et règlements existants peuvent comporter des exigences applicables en matière d'exactitude et de précision. La présente norme indique les unités et grandeurs spécifiques et précise des formats de stockage de données. Le présent document ne présente aucune exigence quant à l'affichage des informations sur la dose aux opérateurs ou à d'autres individus. La présente Norme internationale a pour objet de spécifier l'ensemble de données minimal à utiliser pour consigner les informations dosimétriques et connexes associées à la production d'images radiologiques de projection. Cette première édition annule et remplace l'IEC/PAS 61910-1, parue en 2007. Cette édition constitue une révision technique qui inclut les modifications techniques majeures suivantes par rapport à l'IEC/PAS 61910-1:2007:
- les trois niveaux de conformité définis précédemment ont été restructurés en deux niveaux;
- la correspondance entre les termes DICOM et IEC est décrite explicitement dans une annexe et est dissociée des exigences relatives au contenu des niveaux de conformité; et le contenu révisé de la définition du RDSR selon la DICOM a été mis à jour de manière générale.

Jeklo in železo - Določevanje kobalta - Metoda s plamensko atomsko absorpcijsko spektrometrijo (ISO 11652:1997)

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SLOVENSKI STANDARD
SIST EN ISO 11652:2022
01-maj-2022
Jeklo in železo - Določevanje kobalta - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (ISO 11652:1997)

Steel and iron - Determination of cobalt content - Flame atomic absorption spectrometric

method (ISO 11652:1997)
Stahl und Eisen - Bestimmung des Cobaltgehaltes -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO 11652:1997)

Aciers et fontes - Dosage du cobalt - Méthode par spectrométrie d'absorption atomique

dans la flamme (ISO 11652:1997)
Ta slovenski standard je istoveten z: EN ISO 11652:2022
ICS:
77.080.10 Železo Irons
77.080.20 Jekla Steels
SIST EN ISO 11652:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 11652:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 11652:2022
EN ISO 11652
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2022
EUROPÄISCHE NORM
ICS 77.080.01
English Version
Steel and iron - Determination of cobalt content - Flame
atomic absorption spectrometric method (ISO
11652:1997)

Aciers et fontes - Dosage du cobalt - Méthode par Stahl und Eisen - Bestimmung des Cobaltgehaltes -

spectrométrie d'absorption atomique dans la flamme Flammenatomabsorptionsspektrometrisches

(ISO 11652:1997) Verfahren (ISO 11652:1997)
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 11652:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 11652:2022
EN ISO 11652:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

---------------------- Page: 4 ----------------------
SIST EN ISO 11652:2022
EN ISO 11652:2022 (E)
European foreword

The text of ISO 11652:1997 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 11652:2022 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 11652:1997 has been approved by CEN as EN ISO 11652:2022 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 11652:2022
---------------------- Page: 6 ----------------------
SIST EN ISO 11652:2022
IS0
INTERNATIONAL
11652
STANDARD
First edition
1997-08-I 5
- Determination of cobalt
Steel and iron
content - Flame atomic absorption
spectrometric method
Aciers et fontes - Dosage du cobalt - Mkthode par spectrom&rie
d’absorption atomique dans la flamme
Reference number
IS0 11652:1997(E)
---------------------- Page: 7 ----------------------
SIST EN ISO 11652:2022
IS0 11652: 1997(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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.
International Standard IS0 11652 was prepared by Technical Committee
ISOnC 17, Steel, Subcommittee SC 1, Methods of determination of
chemical composition.
Annex A forms an integral part of this International Standard. Annexes B
and C are for information only.
0 IS0 1997

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 the publisher.
International Organization for Standardization
Case postale 56 l CH-1211 Geneve 20 l Switzerland
Internet central @ iso.ch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
---------------------- Page: 8 ----------------------
SIST EN ISO 11652:2022
INTERNATIONAL STANDARD @ Iso IS0 11652: 1997(E)
Steel and iron - Determination of cobalt content - Flame atomic
absorption spectrometric method
1 Scope

This International Standard specifies a flame atomic absorption spectrometric method for the determination of the

cobalt content in steel and iron.

The method is applicable to cobalt contents between 0,003 % (m/m) and 5,0 % (m/m).

2 Normative references

The following standards contain provisions which, through reference in this text, constitute provisions of this

International Standard. At the time of publication, the editions indicated were valid. All standards are subject to

revision, and parties to agreements based on this International Standard are encouraged to investigate the

possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain

registers of currently valid International Standards.

IS0 385-l :I 984, Laboratory glassware - Burettes - Part I: Genera/ requirements.

IS0 648:1977, Laboratory glassware - One-mark pipettes.
-I), Laboratory glassware - One-mark volumetric flasks.
IS0 1042:

IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.

IS0 5725-l :I 994, Accuracy (trueness and precision) of measurement methods and results - Par? I: General

principles and definitions.

IS0 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.

IS0 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results - Part 3: Intermediate

measures of the precision of a standard measurement method.

IS0 14284 :I 996, Steel and iron - Sampling and preparation of samples for the determination of chemical

composition.
3 Principle
Dissolution of a test portion in hydrochloric, nitric and perchloric acids.
Spraying of the solution into an air-acetylene flame.

Spectrometric measurement of the atomic absorption of the 240,7 nm spectral line emitted by a cobalt hollow

cathode lamp.
1) To be published. (Revision of IS0 1042:1983)
---------------------- Page: 9 ----------------------
SIST EN ISO 11652:2022
@ IS0
IS01 1652:1997( E)
4 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2

water as specified in IS0 3696.
4.1 Pure iron, containing less than 0,000 3 % (m/m) cobalt.
4.2 Pure nickel, containing less than 0,000 3 % (m/m) cobalt.
4.3 Hydrochloric acid, p about 1,19 g/ml.
4.4 Nitric acid, p about 1,40 g/ml.
4.5 Perchloric acid, p about 1,67 g/ml.
4.6 Cobalt, standard solutions.
4.6.1 Standard solution A, corresponding to I,0 g of Co per litre.

Weigh, to the nearest 0,001 g, 1,000 g of metallic cobalt [purity > 99,9 % (m/m) Co]. Transfer to a 250 ml beaker.

Add 15 ml of water and 15 ml of nitric acid (4.4). Cover the beaker with a watch-glass, heat gently until complete

dissolution has taken place and boil to remove oxides of nitrogen.

Cool to room temperature, transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the

mark with water and mix.
1 ml of this standard solution A contains I,0 mg of Co.
4.6.2 Standard solution B, corresponding to 0,2 g of Co per litre.

Transfer 20,O ml of the standard solution A (4.6.1) to a 100 ml one-mark volumetric flask, dilute to the mark with

water and mix.
1 ml of this standard solution B contains 0,2 mg of Co.
4.6.3 Standard solution C, corresponding to 0,08 g of Co per litre.

Transfer 8,0 ml of the standard solution A (4.6.1) to a 100 ml one-mark volumetric flask, dilute to the mark with

water and mix.
Prepare this standard solution C immediately before use.
1 ml of this standard solution C contains 0,08 mg of Co.
5 Apparatus

All volumetric glassware shall be class A, in accordance with IS0 385-1, IS0 648 or IS0 1042 as appropriate.

Ordinary laboratory apparatus, and

5.1 Atomic absorption spectrometer, equipped with a cobalt hollow cathode lamp and supplied with air and

acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from cobalt.

The atomic absorption spectrometer used will be satisfactory if, after optimization according to 7.3.4, the limit of

detection and characteristic concentration are in reasonable agreement with the values given by the manufacturer

and if it meets the precision criteria given in 5.1 .I to 5.1.3.
---------------------- Page: 10 ----------------------
SIST EN ISO 11652:2022
@ IS0
IS0 11652: 1997(E)

It is also desirable that the instrument should conform to the additional performance requirements given in 51.4.

5.1.1 Minimum precision (see A.l)

Calculate the standard deviation of 10 measurements of the absorbance of the most concentrated calibration

solution. The standard deviation shall not exceed I,5 % of the mean absorbance.

Calculate the standard deviation of IO measurements of the absorbance of the least concentrated calibration

solution (excluding the zero member). The standard deviation shall not exceed 0,5 % of the mean absorbance of

the most concentrated calibration solution.
5.1.2 Limit of detection (see A.2)

This is defined as twice the standard deviation of IO measurements of the absorbance of a solution containing the

appropriate element of a concentration level selected to give an absorbance just above that of the zero member.

The limit of detection of cobalt in a matrix similar to the final test solution shall be better than 0,05 pg of Co per

millilitre, for wavelength 240,7 nm.
51.3 Graph linearity (see A.3)

The slope of the calibration graph 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

(expressed as a change in absorbance) determined in the same way.

For instruments with automatic calibration using two or more standards, it shall be established prior to the analysis,

by obtaining absorbance readings, that the above requirements for graph linearity are fulfilled.

5.t .4 Characteristic concentration (see A.4)

The chlaracteristic concentration of cobalt in a matrix similar to the final test portion solution shall be better than

0,3 pg of Co per millititre, for wavelength 240,7 nm.
5.2 Ancillary equipment

A strip chart recorder and/or digital readout device is recommended to evaluate the criteria of 5.1 .I to 5.1.3 and for

all subsequent measurements.

Scale expansion may be used until the noise observed is greater than the readout error and is always

recommended for absorbances below 0,l. 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 the absorbances

of a suitable solution with and without scale expansion and simply dividing the signal obtained.

A background corrector equipped with a deuterium hollow cathode lamp is advisable for the analysis of highly

alloyed steels, in order to eliminate interference from an Fe0 molecular absorption band at the cobalt wavelength.

6 Sampling

Carry out sampling in accordance with IS0 14284 or appropriate national standards for steel and iron.

7 Procedure

- Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or

WARNING
organic material in general.
---------------------- Page: 11 ----------------------
SIST EN ISO 11652:2022
@ IS0
IS0 11652:1997(E)
7.1 Test portion
Weigh a test portion according to the presumed cobalt content as follows:

a) for cobalt contents up to 2,0 % (mlm), a test portion of about I,0 g, to the nearest 0,001 g;

b) for cobalt contents from 2,0 % (mlm) to 5,0 % (m/m), a test portion of about 0,50 g, to the nearest 0,000 5 g.

7.2 Blank test

In parallel with the determination and following the same procedure, cairy out a blank test for each concentration

range (see 7.1) using the same quantities of all the reagents, including the pure iron(4.1) but omitting the test

portion.
7.3 Determination
7.3.1 Preparation of the test solution
7.3.1.1 Dissolution of the test portion

Transfer the test portion (7.1) to a 250 ml beaker. Add IO ml of hydrochloric acid (4.3) and 4 ml of nitric acid (4.4)

and cover the beaker with a watch-glass. After effervescence ceases, add IO ml of perchloric acid (4.5) and heat.

Heat until dense white fumes of perchloric acid reflux smoothly in the beaker.

Allow to cool, add 30 ml of water and heat gently to dissolve the salts. Cool again and transfer quantitatively to a

100 ml one-mark volumetric flask. Dilute to the mark with water and mix.

Decant the solution through a dry medium-filter paper, to remove any residue or precipitate, for example graphite,

silica or tungstic acid, and collect the filtrate in a dry beaker after discarding the first few millilitres.

7.3.1.2 Dilution of the test solution

Depending on the cobalt content expected in the test portion, prepare the test solution in accordance with a), b), c)

or d), as follows.

a) If the expected cobalt content is up to 0,08 % (m/m), use the filtrate (see 7.3.1 .I) undiluted.

b) If the expected cobalt content is between 0,08 % (m/m) and 0,40 % (m/m), dilute the filtrate as follows.

Transfer 20,O ml of the filtrate to a 100 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

c) If the expected cobalt content is between 0,40 % (m/m) and 2,0 % (m/m), dilute the filtrate as follows.

Transfer IO,0 ml of the filtrate to a 250 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

d) If the expected cobalt content is between 2,0 % (m/m) and 5,0 % (m/m), dilute the filtrate as follows.

Transfer 5,0 ml of the filtrate to a 250 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

NOTE 1 If the filtrate(see 7.3.1 .l) has to be diluted to give the test solution, dilute the blank (see 7.2) in exactly the same

way.
---------------------- Page: 12 ----------------------
SIST EN ISO 11652:2022
@ IS0 IS0 11652:1997(E)
7.3.2 Preparation of the calibration solution
7.3.2.1 Cobalt contents up to 0,08 % (m/m)

Introduce (I,00 + 0,OOl)g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effervescence ceases, cool, then respectively add, using a burette, the volumes of cobalt standard solution C

(4.6.3) given in table 1.

Proceed as specified in 7.3.1 .I from “add IO ml of perchloric acid (4.5) . ..” (omitting the filtration step) to item a) in

7.3. I .2.
Table 1 - Calibration solutions, up to 0,08 % (m/m) cobalt content
Corresponding
Volume of cobalt Corresponding
standard solution C concentration of percentage of
(4.6.3) cobalt in the final cobalt in the
test solution test sample
ml % (m/m)
0 ‘) 0
0,016
116
290
0,032
490
0,048
4,8
690
0,064
694
0,080
890
IO,0
1) Zero member
7.3.2.2 Cobalt contents between 0,08 % (m/m) and 0,40 % (m/m)

Introduce (I,00 & 0,OOl)g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effervescence ceases, cool, t
...

SLOVENSKI STANDARD
oSIST prEN ISO 11652:2022
01-januar-2022
Jeklo in železo - Določevanje kobalta - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (ISO 11652:1997)

Steel and iron - Determination of cobalt content - Flame atomic absorption spectrometric

method (ISO 11652:1997)
Stahl und Eisen - Bestimmung des Cobaltgehaltes -
Flammenatomabsorptionsspektrometrisches Verfahren (ISO 11652:1997)

Aciers et fontes - Dosage du cobalt - Méthode par spectrométrie d'absorption atomique

dans la flamme (ISO 11652:1997)
Ta slovenski standard je istoveten z: prEN ISO 11652
ICS:
77.080.10 Železo Irons
77.080.20 Jekla Steels
oSIST prEN ISO 11652:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 11652:2022
---------------------- Page: 2 ----------------------
oSIST prEN ISO 11652:2022
IS0
INTERNATIONAL
11652
STANDARD
First edition
1997-08-I 5
- Determination of cobalt
Steel and iron
content - Flame atomic absorption
spectrometric method
Aciers et fontes - Dosage du cobalt - Mkthode par spectrom&rie
d’absorption atomique dans la flamme
Reference number
IS0 11652:1997(E)
---------------------- Page: 3 ----------------------
oSIST prEN ISO 11652:2022
IS0 11652: 1997(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
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.
International Standard IS0 11652 was prepared by Technical Committee
ISOnC 17, Steel, Subcommittee SC 1, Methods of determination of
chemical composition.
Annex A forms an integral part of this International Standard. Annexes B
and C are for information only.
0 IS0 1997

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 the publisher.
International Organization for Standardization
Case postale 56 l CH-1211 Geneve 20 l Switzerland
Internet central @ iso.ch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
---------------------- Page: 4 ----------------------
oSIST prEN ISO 11652:2022
INTERNATIONAL STANDARD @ Iso IS0 11652: 1997(E)
Steel and iron - Determination of cobalt content - Flame atomic
absorption spectrometric method
1 Scope

This International Standard specifies a flame atomic absorption spectrometric method for the determination of the

cobalt content in steel and iron.

The method is applicable to cobalt contents between 0,003 % (m/m) and 5,0 % (m/m).

2 Normative references

The following standards contain provisions which, through reference in this text, constitute provisions of this

International Standard. At the time of publication, the editions indicated were valid. All standards are subject to

revision, and parties to agreements based on this International Standard are encouraged to investigate the

possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain

registers of currently valid International Standards.

IS0 385-l :I 984, Laboratory glassware - Burettes - Part I: Genera/ requirements.

IS0 648:1977, Laboratory glassware - One-mark pipettes.
-I), Laboratory glassware - One-mark volumetric flasks.
IS0 1042:

IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.

IS0 5725-l :I 994, Accuracy (trueness and precision) of measurement methods and results - Par? I: General

principles and definitions.

IS0 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.

IS0 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results - Part 3: Intermediate

measures of the precision of a standard measurement method.

IS0 14284 :I 996, Steel and iron - Sampling and preparation of samples for the determination of chemical

composition.
3 Principle
Dissolution of a test portion in hydrochloric, nitric and perchloric acids.
Spraying of the solution into an air-acetylene flame.

Spectrometric measurement of the atomic absorption of the 240,7 nm spectral line emitted by a cobalt hollow

cathode lamp.
1) To be published. (Revision of IS0 1042:1983)
---------------------- Page: 5 ----------------------
oSIST prEN ISO 11652:2022
@ IS0
IS01 1652:1997( E)
4 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2

water as specified in IS0 3696.
4.1 Pure iron, containing less than 0,000 3 % (m/m) cobalt.
4.2 Pure nickel, containing less than 0,000 3 % (m/m) cobalt.
4.3 Hydrochloric acid, p about 1,19 g/ml.
4.4 Nitric acid, p about 1,40 g/ml.
4.5 Perchloric acid, p about 1,67 g/ml.
4.6 Cobalt, standard solutions.
4.6.1 Standard solution A, corresponding to I,0 g of Co per litre.

Weigh, to the nearest 0,001 g, 1,000 g of metallic cobalt [purity > 99,9 % (m/m) Co]. Transfer to a 250 ml beaker.

Add 15 ml of water and 15 ml of nitric acid (4.4). Cover the beaker with a watch-glass, heat gently until complete

dissolution has taken place and boil to remove oxides of nitrogen.

Cool to room temperature, transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the

mark with water and mix.
1 ml of this standard solution A contains I,0 mg of Co.
4.6.2 Standard solution B, corresponding to 0,2 g of Co per litre.

Transfer 20,O ml of the standard solution A (4.6.1) to a 100 ml one-mark volumetric flask, dilute to the mark with

water and mix.
1 ml of this standard solution B contains 0,2 mg of Co.
4.6.3 Standard solution C, corresponding to 0,08 g of Co per litre.

Transfer 8,0 ml of the standard solution A (4.6.1) to a 100 ml one-mark volumetric flask, dilute to the mark with

water and mix.
Prepare this standard solution C immediately before use.
1 ml of this standard solution C contains 0,08 mg of Co.
5 Apparatus

All volumetric glassware shall be class A, in accordance with IS0 385-1, IS0 648 or IS0 1042 as appropriate.

Ordinary laboratory apparatus, and

5.1 Atomic absorption spectrometer, equipped with a cobalt hollow cathode lamp and supplied with air and

acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water and oil, and free from cobalt.

The atomic absorption spectrometer used will be satisfactory if, after optimization according to 7.3.4, the limit of

detection and characteristic concentration are in reasonable agreement with the values given by the manufacturer

and if it meets the precision criteria given in 5.1 .I to 5.1.3.
---------------------- Page: 6 ----------------------
oSIST prEN ISO 11652:2022
@ IS0
IS0 11652: 1997(E)

It is also desirable that the instrument should conform to the additional performance requirements given in 51.4.

5.1.1 Minimum precision (see A.l)

Calculate the standard deviation of 10 measurements of the absorbance of the most concentrated calibration

solution. The standard deviation shall not exceed I,5 % of the mean absorbance.

Calculate the standard deviation of IO measurements of the absorbance of the least concentrated calibration

solution (excluding the zero member). The standard deviation shall not exceed 0,5 % of the mean absorbance of

the most concentrated calibration solution.
5.1.2 Limit of detection (see A.2)

This is defined as twice the standard deviation of IO measurements of the absorbance of a solution containing the

appropriate element of a concentration level selected to give an absorbance just above that of the zero member.

The limit of detection of cobalt in a matrix similar to the final test solution shall be better than 0,05 pg of Co per

millilitre, for wavelength 240,7 nm.
51.3 Graph linearity (see A.3)

The slope of the calibration graph 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

(expressed as a change in absorbance) determined in the same way.

For instruments with automatic calibration using two or more standards, it shall be established prior to the analysis,

by obtaining absorbance readings, that the above requirements for graph linearity are fulfilled.

5.t .4 Characteristic concentration (see A.4)

The chlaracteristic concentration of cobalt in a matrix similar to the final test portion solution shall be better than

0,3 pg of Co per millititre, for wavelength 240,7 nm.
5.2 Ancillary equipment

A strip chart recorder and/or digital readout device is recommended to evaluate the criteria of 5.1 .I to 5.1.3 and for

all subsequent measurements.

Scale expansion may be used until the noise observed is greater than the readout error and is always

recommended for absorbances below 0,l. 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 the absorbances

of a suitable solution with and without scale expansion and simply dividing the signal obtained.

A background corrector equipped with a deuterium hollow cathode lamp is advisable for the analysis of highly

alloyed steels, in order to eliminate interference from an Fe0 molecular absorption band at the cobalt wavelength.

6 Sampling

Carry out sampling in accordance with IS0 14284 or appropriate national standards for steel and iron.

7 Procedure

- Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or

WARNING
organic material in general.
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oSIST prEN ISO 11652:2022
@ IS0
IS0 11652:1997(E)
7.1 Test portion
Weigh a test portion according to the presumed cobalt content as follows:

a) for cobalt contents up to 2,0 % (mlm), a test portion of about I,0 g, to the nearest 0,001 g;

b) for cobalt contents from 2,0 % (mlm) to 5,0 % (m/m), a test portion of about 0,50 g, to the nearest 0,000 5 g.

7.2 Blank test

In parallel with the determination and following the same procedure, cairy out a blank test for each concentration

range (see 7.1) using the same quantities of all the reagents, including the pure iron(4.1) but omitting the test

portion.
7.3 Determination
7.3.1 Preparation of the test solution
7.3.1.1 Dissolution of the test portion

Transfer the test portion (7.1) to a 250 ml beaker. Add IO ml of hydrochloric acid (4.3) and 4 ml of nitric acid (4.4)

and cover the beaker with a watch-glass. After effervescence ceases, add IO ml of perchloric acid (4.5) and heat.

Heat until dense white fumes of perchloric acid reflux smoothly in the beaker.

Allow to cool, add 30 ml of water and heat gently to dissolve the salts. Cool again and transfer quantitatively to a

100 ml one-mark volumetric flask. Dilute to the mark with water and mix.

Decant the solution through a dry medium-filter paper, to remove any residue or precipitate, for example graphite,

silica or tungstic acid, and collect the filtrate in a dry beaker after discarding the first few millilitres.

7.3.1.2 Dilution of the test solution

Depending on the cobalt content expected in the test portion, prepare the test solution in accordance with a), b), c)

or d), as follows.

a) If the expected cobalt content is up to 0,08 % (m/m), use the filtrate (see 7.3.1 .I) undiluted.

b) If the expected cobalt content is between 0,08 % (m/m) and 0,40 % (m/m), dilute the filtrate as follows.

Transfer 20,O ml of the filtrate to a 100 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

c) If the expected cobalt content is between 0,40 % (m/m) and 2,0 % (m/m), dilute the filtrate as follows.

Transfer IO,0 ml of the filtrate to a 250 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

d) If the expected cobalt content is between 2,0 % (m/m) and 5,0 % (m/m), dilute the filtrate as follows.

Transfer 5,0 ml of the filtrate to a 250 ml one-mark volumetric flask, dilute to the mark with water and mix (see

note 1).

NOTE 1 If the filtrate(see 7.3.1 .l) has to be diluted to give the test solution, dilute the blank (see 7.2) in exactly the same

way.
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oSIST prEN ISO 11652:2022
@ IS0 IS0 11652:1997(E)
7.3.2 Preparation of the calibration solution
7.3.2.1 Cobalt contents up to 0,08 % (m/m)

Introduce (I,00 + 0,OOl)g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effervescence ceases, cool, then respectively add, using a burette, the volumes of cobalt standard solution C

(4.6.3) given in table 1.

Proceed as specified in 7.3.1 .I from “add IO ml of perchloric acid (4.5) . ..” (omitting the filtration step) to item a) in

7.3. I .2.
Table 1 - Calibration solutions, up to 0,08 % (m/m) cobalt content
Corresponding
Volume of cobalt Corresponding
standard solution C concentration of percentage of
(4.6.3) cobalt in the final cobalt in the
test solution test sample
ml % (m/m)
0 ‘) 0
0,016
116
290
0,032
490
0,048
4,8
690
0,064
694
0,080
890
IO,0
1) Zero member
7.3.2.2 Cobalt contents between 0,08 % (m/m) and 0,40 % (m/m)

Introduce (I,00 & 0,OOl)g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effervescence ceases, cool, then respectively add, using a burette, the volumes of cobalt standard solution B

(4.6.2) given in table 2.

Proceed as specified in 7.3.1 .I from “add IO ml of perchloric acid (4.5) . ..” (omitting the filtration step) to item b) in

0,08 % (m/m) up to 0,40 % (m/m) cobalt content
Table 2 - Calibration solutions,
Volume of cobalt Corresponding Corresponding
concentration of percentage of
standard solution B
(4.6.2) cobalt in the
cobalt in the final
test sample
test solution
ml % (m/m)
Wml
0 ”
0,080
0,160
870
478 0,240
12,0
694 0,320
16,0
0,400
8'0
20,o
1) Zero member
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oSIST prEN ISO 11652:2022
@ IS0
IS0 11652:1997(E)
7.3.2.3 Cobalt contents between 0,40 % (m/m) and 2,00 % (m/m)

Introduce (I,00 rfr 0,OOl)g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effen/escence ceases, cool, then respectively add, using a burette, the volumes of cobalt standard solution A

(4.6.1) given in table 3.

Proceed as specified in 7.3.1 .I from “add IO ml of perchloric acid (4.5) . ..” (omitting the filtration step) to item c) in

7.3.1.2 .
solutions, 0,40 % (m/m) up to 2,00 % (m/m) cobalt content
Table 3 - Calibration
Volume of cobalt Corresponding Corresponding
concentration of percentage of
standard solution A
cobalt in the final cobalt in the
(4.6.1)
test solution test sample
ml % (m/m)
Wml
0 ” 0 0
W I,6 0,40
890 3,2 0,80
12,0 48 I,20
694 I,60
16,0
890 2,00
20,o
1) Zero member
7.3.2.4 Cobalt contents between 2,0 % (m/m) and 5,0 % (m/m)

Introduce (0,50 + 0,000 5) g of the pure iron (4.1) into a series of six 250 ml beakers. Add IO ml of hydrochloric acid

(4.3) and 5 ml of nitric acid (4.4) to each beaker and cover them with watch-glasses.

After effervescence ceases, cool, then respectively add, using a burette, the volumes of cobalt standard solution A

(4.6.1) given in table 4.
Proceed as spec
...

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