Alloyed steels - Determination of chromium content - Inductively coupled plasma optical emission spectrometric method

This document specifies an inductively coupled plasma optical emission spectrometric method for the determination of the chromium content (mass fraction) between 5,0 % (m/m) and 27,0 % (m/m) in alloyed steels.
The method doesn't apply to alloyed steels having carbon contents higher than 1 % and niobium and/or tungsten contents higher than 0,1 %.

Stahl - Bestimmung des Chromgehaltes - Optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma Verfahren

Aciers alliés - Détermination du chrome - Méthode par spectrométrie d'émission optique avec source à plasma induit

Le présent document spécifie une méthode de détermination des teneurs en chrome comprises entre 5,0 % (m/m) et 27,0 % (m/m) (en masse) dans les aciers alliés, par spectrométrie d’émission optique avec source à plasma induit.
La méthode ne s’applique pas aux aciers alliés contenant plus de 1 % de carbone et plus de 0,1 % de niobium et/ou de tungstène.

Legirana jekla - Določevanje kroma - Optična emisijska spektrometrija z induktivno sklopljeno plazmo (ICP/OES)

V tem delovnem osnutku je določena metoda optične emisijske spektrometrije z induktivno sklopljeno plazmo za določanje vsebnosti kroma (masni delež) med 5,0 % (m/m) in 27,0 % (m/m) v legiranih jeklih. Metoda se ne uporablja za legirana jekla z vsebnostjo niobija in/ali volframa, višjo od 0,1 %.

General Information

Status
Published
Publication Date
11-Jun-2019
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
12-Jun-2019
Completion Date
12-Jun-2019

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SLOVENSKI STANDARD
SIST-TP CEN/TR 10367:2019
01-september-2019
Legirana jekla - Določevanje kroma - Optična emisijska spektrometrija z
induktivno sklopljeno plazmo (ICP/OES)

Alloyed steels - Determination of chromium content - Inductively coupled plasma optical

emission spectrometric method

Stahl - Bestimmung des Chromgehaltes - Optischer Emissionsspektrometrie mit induktiv

gekoppeltem Plasma Verfahren

Aciers alliés - Détermination du chrome - Méthode par spectrométrie d'émission optique

avec source à plasma induit
Ta slovenski standard je istoveten z: CEN/TR 10367:2019
ICS:
77.080.20 Jekla Steels
SIST-TP CEN/TR 10367:2019 en,fr,de

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

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SIST-TP CEN/TR 10367:2019
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SIST-TP CEN/TR 10367:2019
CEN/TR 10367
TECHNICAL REPORT
RAPPORT TECHNIQUE
June 2019
TECHNISCHER BERICHT
ICS 77.080.20
English Version
Alloyed steels - Determination of chromium content -
Inductively coupled plasma optical emission spectrometric
method

Aciers alliés - Détermination du chrome - Méthode par Stahl - Bestimmung des Chromgehaltes - Optischer

spectrométrie d'émission optique avec source à plasma Emissionsspektrometrie mit induktiv gekoppeltem

induit Plasma Verfahren

This Technical Report was approved by CEN on 19 May 2019. It has been drawn up by the Technical Committee CEN/TC 459/SC

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, North

Macedonia, Norway, Poland, Portugal, 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

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 10367:2019 E

worldwide for CEN national Members.
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CEN/TR 10367:2019 (E)
Contents Page

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

1 Scope .................................................................................................................................................................... 4

2 Normative references .................................................................................................................................... 4

3 Terms and definitions ................................................................................................................................... 4

4 Principle ............................................................................................................................................................. 5

5 Reagents ............................................................................................................................................................. 5

6 Apparatus ........................................................................................................................................................... 6

7 Sampling ............................................................................................................................................................. 6

8 Procedure........................................................................................................................................................... 7

9 Determination .................................................................................................................................................. 9

10 Expression of the results ........................................................................................................................... 10

11 Test report ...................................................................................................................................................... 11

Annex A (informative) Plasma optical emission spectrometer - Suggested performance

criteria to be checked ................................................................................................................................. 13

Annex B (informative) Composition of the samples used for the validation precision test ............. 15

Bibliography ................................................................................................................................................................. 17

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European foreword

This document (CEN/TR 10367:2019) 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.

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.

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1 Scope

This document specifies an inductively coupled plasma optical emission spectrometric method for the

determination of the chromium content (mass fraction) between 5,0 % (m/m) and 27,0 % (m/m) in

alloyed steels.

The method doesn't apply to alloyed steels having carbon contents higher than 1 % and niobium and/or

tungsten contents higher than 0,1 %.
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
EN ISO 1042, Laboratory glassware — One mark volumetric flasks

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 http://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
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4 Principle

Dissolution of a test portion with hydrochloric and nitric acids. Filtration and ignition of the acid

insoluble residue. Removal of silica with hydrofluoric acid. Fusion of the residue with potassium

hydrogen sulphate (or with potassium disulphate), acid dissolution of the melt and addition of this

solution to the reserved filtrate.

After suitable dilution and, if necessary, addition of an internal reference element, nebulisation of the

solution into an inductively coupled plasma optical emission spectrometer and measurement of the

intensity of the emitted light (including, where appropriate, that of the internal reference element).

The method uses a calibration based on a very close matrix matching of the calibration solutions to the

sample and bracketing of the mass fractions between 0,95 to 1,05 of the approximate content of

chromium in the sample to be analysed. The content of all elements in the sample has, therefore, to be

approximately known. If the contents are not known, the sample has to be analysed by some

semi-quantitative method. The advantage with this procedure is that all possible interferences from the

matrix will be compensated, which will result in high accuracy. This is most important for spectral

interferences, which can be severe in very highly alloyed matrixes. All possible interferences shall be

kept at a minimum level. Therefore, it is essential that the spectrometer used meets the performance

criteria specified in the method for the selected analytical lines.

The wavelengths reported in Table 1 have been investigated and the strongest possible interferences

are given. If other wavelengths are used, they shall be carefully checked. The wavelength for the

internal reference element should be selected carefully. The use of scandium at 363,1 nm or yttrium at

371,0 nm is recommended. These wavelengths are interference-free for the elements and contents

generally found in alloyed steels.
5 Reagents

During the analysis, use only reagents of recognized analytical grade and only distilled water or water

of equivalent purity.

The same reagents should be used for the preparation of calibration solutions and of sample solutions.

5.1 Hydrochloric acid, HCl (ρ = 1,19 g/ml).
5.2 Nitric acid, HNO (ρ = 1,33 g/ml).
3 20
5.3 Hydrofluoric acid, HF (ρ = 1,13 g/ml).

WARNING — Hydrofluoric acid is extremely irritating and corrosive to skin and mucous membranes,

producing severe skin burns which are slow to heal. In the case of contact with skin, wash well with

water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate, and seek immediate

medical treatment.
5.4 Sulphuric acid, H SO (ρ = 1,84 g/ml).
2 4 20
5.5 Sulphuric acid, solution 1 + 1.
While cooling, add 25 ml of sulphuric acid (5.4) to 25 ml of water.
5.6 Potassium hydrogen sulphate [KHSO ] or potassium disulphate [K S O ].
4 2 2 7
5.7 Chromium standard solution, 10 g/l.
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Weigh, to the nearest 0,001 g, 2 g of high purity chromium [min 99,9 % (mass fraction)], place it in a

beaker and add 100 ml of hydrochloric acid (5.1). Cover with a watch glass and heat gently until

chromium is completely dissolved. After cooling, transfer the solution quantitatively into a 200 ml one-

mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 10 mg of chromium.
5.8 Chromium standard solution, 5 g/l

Weigh, to the nearest 0,001 g, 1 g of high purity chromium [min 99,9 % (mass fraction)], place it in a

beaker and add 50 ml of hydrochloric acid (5.1). Cover with a watch glass and heat gently until

chromium is completely dissolved. After cooling, transfer the solution quantitatively into a 200 ml one-

mark volumetric flask, dilute to the mark with water and mix well.
1 ml of this solution contains 5 mg of chromium.
5.9 Standard solutions of matrix elements

Prepare standard solutions for each element whose content (mass fraction) in the test sample is higher

than 1 %. Use pure metals or chemical substances with chromium contents (mass fractions) less than

100 μg/g.
5.10 Internal reference element solution, 1 g/l

Choose a suitable element to be added as internal reference and prepare a 1 g/l solution.

NOTE Elements such as Sc and Y are often used for this purpose.
6 Apparatus

All volumetric glassware shall be class A and calibrated in accordance with EN ISO 648 or EN ISO 1042

as appropriate.
6.1 Fine texture filter paper.
6.2 Platinum crucibles.
6.3 Optical emission spectrometer, equipped with inductively coupled plasma.

This shall be equipped with a nebulisation system. The instrument used will be satisfactory if, after

optimizing in accordance with the manufacturer’s instructions, it meets the performance criteria given

in Annex A.

The spectrometer can be either a simultaneous or a sequential one. If a sequential spectrometer can be

equipped with an extra arrangement for simultaneous measurement of the internal reference element

intensity, it can be used with the internal reference method. If the sequential spectrometer is not

equipped with this arrangement, an internal reference cannot be used and an alternative measurement

technique without internal reference element shall be used.
7 Sampling

Sampling shall be carried out in accordance with EN ISO 14284 or with an appropriate national

standard for steels.
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8 Procedure
8.1 Test portion
Weigh 0,5 g of the test sample to the nearest 0,001 g.
8.2 Preparation of the test solution, T
Transfer the test portion (8.1) into a 250 ml beaker.

Add 15 ml of hydrochloric acid (5.1), cover with a watch glass, heat gently until the attack reaction

ceases, and then add dropwise, 10 ml of nitric acid (5.2).

Depending on the composition of each sample, larger amounts of hydrochloric acid can be necessary.

Addition of hydrogen peroxide (H O ) may advantageously help dissolution. The same quantities of the

2 2
dissolution reagents shall be added to the corresponding calibration solutions.

Boil until nitrous fumes have been expelled. After cooling, add about 20 ml of water, filter the solution

through a fine texture filter paper (6.1) and collect the filtrate into a 200 ml one-mark volumetric flask.

Wash the filter paper and its content with hot water slightly acidified with nitric acid (5.2) several times

and collect the washings in the 200 ml one-mark volumetric flask.

Transfer the filter into a platinum crucible (6.2), dry and ignite first at a relatively low temperature

(until all carbonaceous matter is removed) and then at about 800 °C for at least 15 min.

Allow the crucible to cool. Add into the crucible 0,5 to 1,0 ml of sulphuric acid solution (5.5) and 2 ml of

hydrofluoric acid (5.3). Evaporate to dryness and cool.

Add into the crucible 1,00 g of potassium hydrogen sulphate or potassium disulphate (5.6) and fuse

carefully by means of a Meker burner, until a clear melt is obtained.

NOTE 1 For residues containing substantial amounts of chromium carbides, prolonged heating could be

necessary for complete fusion. The potassium hydrogen sulphate or potassium disulphate (5.6) can be

regenerated by allowing the melt to cool, adding some drops of sulphuric acid (5.4) and repeating the fusion until

the residue is fused.

NOTE 2 Depending on the composition of each sample, larger amounts of potassium hydrogen sulphate or

potassium disulphate (5.6) can be used, provided the same amount is added to the corresponding calibration

solutions.

Allow the crucible to cool and add about 10 ml of water and 2 ml of hydrochloric acid (5.1) to the

solidified melt. Heat gently, in order to dissolve the fusion products. Allow the crucible to cool and

quantitatively add the solution to the filtrate in the 200 ml one-mark volumetric flask.

NOTE 3 The volume of hydrochloric acid (5.1) can be increased, provided the same volume is added to the

corresponding calibration solutions.

NOTE 4 If an internal reference element is used, an appropriate volume of the internal reference element

solution (5.10) can be added at this stage. In this case, omit this operation when diluting the sample solution.

Dilute to the mark with water and mix.

Transfer 20 ml of this sample solution into a 100 ml one-mark volumetric flask and add 10 ml of

hydrochloric acid (5.1).

NOTE 5 Depending on the instrument performances, the final concentration of the test solution can be lower

(or higher), provided the corresponding calibration solutions have the same final concentration.

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If an internal reference element is used, add, with a calibrated pipette, 10 ml of the internal reference

element solution (5.10).

NOTE 6 Depending on the instrument performances, the volume and/or the concentration of the internal

reference element solution could be different.
Dilute to the mark with water and mix.
8.3 Predetermination of the test solution

Prepare two calibration solutions labelled K and K , matrix matched to the test sample solution as

28 0
follows:

Add 14 ml of the chromium standard solution (5.7) in a 400 ml beaker, labelled K .

In each 400 ml beaker, K and K , add the volumes of the standard solutions (5.9) necessary to match

28 0
the sample matrix to be tested, for each element whose
...

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