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Språk: engelska/English Utgåva: 1

SS-EN ISO 11652:2022 SVENSK STANDARD

Stål och järn – Bestämning av halt kobolt – Flamatomisk absorptionspektrometrisk metod (ISO 11652:1997)

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

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Fastställd: 2022-04-04 ICS: 77.080.01

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Europastandarden EN ISO 11652:2022 gäller som svensk standard. Detta dokument innehåller den officiella engelska versionen av EN ISO 11652:2022.

The European Standard EN ISO 11652:2022 has the status of a Swedish Standard. This document contains the official version of EN ISO 11652:2022.

This preview is downloaded from www.sis.se. Buy the entire standard via https://www.sis.se/std-80034504

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LÄSANVISNINGAR FÖR STANDARDER

I dessa anvisningar behandlas huvudprinciperna för hur regler och yttre begränsningar anges i standardiseringsprodukter.

KravEtt krav är ett uttryck i ett dokuments innehåll som anger objektivt verifierbara kriterier som ska uppfyllas och från vilka ingen avvikelse tillåts om efterlevnad av dokumentet ska kunna åberopas.Krav uttrycks med hjälpverbet ska (eller ska inte för förbud).

Rekommendation

En rekommendation är ett uttryck i ett dokuments innehåll som anger en valmöjlighet eller ett tillvägagångssätt som bedöms vara särskilt lämpligt utan att nödvändigtvis nämna eller utesluta andra. Rekommendationer uttrycks med hjälpverbet bör (eller bör inte för avrådanden).

Instruktion

Instruktioner anges i imperativ form och används för att ange hur något görs eller utförs. De kan underordnas en annan regel, såsom ett krav eller en rekommendation. De kan även användas självständigt, och är då att betrakta som krav.

Förklaring

En förklaring är ett uttryck i ett dokuments innehåll som förmedlar information. En förklaring kan uttrycka tillåtelse, möjlighet eller förmåga. Tillåtelse uttrycks med hjälpverbet får. Inom standardiseringen saknas rekommenderad nekande motsats till hjälpverbet får, förbud uttrycks med ska inte enligt reglerna för krav. Möjlighet och förmåga uttrycks med hjälpverbet kan (eller motsatsen kan inte).

READING INSTRUCTIONS FOR STANDARDS

These instructions cover the main principles for the use of provisions and external constraints in standardization deliverables.

Requirement

A requirement is an expression, in the content of a document, that conveys objectively verifiable criteria to be fulfilled, and from which no deviation is permitted if conformance with the document is to be claimed. Requirements are expressed by the auxiliary shall (or shall not for prohibition).

Recommendation

A recommendation is an expression, in the content of a document, that conveys a suggested possible choice or course of action deemed to be particularly suitable, without necessarily mentioning or excluding others. Recommendations are expressed by the auxiliary should (or should not for dissuasion).

Instruction

An instruction is expressed in the imperative mood and is used in order to convey an action to be performed. It can be subordinated to another provision, such as a requirement or a recommendation. It can also be used independently and is then to be regarded as a requirement.

Statement

A statement is an expression, in the content of a document, that conveys information. A statement can express permission, possibility or capability. Permission is expressed by the auxiliary may. There is no recommended opposite expression for the auxiliary may in standardization, prohibition is expressed by the use of shall not in accordance with the rules for requirements. Possibility and capability are expressed by the auxiliary can (its opposite being cannot).

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EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM

EN ISO 11652

March 2022

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 spectrométrie d'absorption atomique dans la flamme

(ISO 11652:1997)

Stahl und Eisen - Bestimmung des Cobaltgehaltes - Flammenatomabsorptionsspektrometrisches

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 C O M I T É E U R O P É E N D E N O R M A L I S A T I O N E U R O P Ä I S C H E S K O M I T E E F Ü R N O R M U N G

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

worldwide for CEN national Members. Ref. No. EN ISO 11652:2022 E

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EN ISO 11652:2022 (E)

3

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.

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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

ii

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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.

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

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)

1

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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.

2

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@ 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

WARNING - Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes or organic material in general.

3

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