SIST-TP CEN/TR 10367:2019
(Main)Alloyed steels - Determination of chromium content - Inductively coupled plasma optical emission spectrometric method
Alloyed steels - Determination of chromium content - Inductively coupled plasma optical emission spectrometric method
This Working Draft 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 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
Standards Content (Sample)
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
2.
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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SIST-TP CEN/TR 10367:2019
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
2
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SIST-TP CEN/TR 10367:2019
CEN/TR 10367:2019 (E)
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.
3
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SIST-TP CEN/TR 10367:2019
CEN/TR 10367:2019 (E)
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
4
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CEN/TR 10367:2019 (E)
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).
20
5.2 Nitric acid, HNO (ρ = 1,33 g/ml).
3 20
5.3 Hydrofluoric acid, HF (ρ = 1,13 g/ml).
20
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.
5
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SIST-TP CEN/TR 10367:2019
CEN/TR 10367:2019 (E)
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.
6
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CEN/TR 10367:2019 (E)
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
Cr
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.
7
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SIST-TP CEN/TR 10367:2019
CEN/TR 10367:2019 (E)
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 .
28
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
...
SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 10367:2019
01-marec-2019
/HJLUDQDMHNOD'RORþHYDQMHNURPD2SWLþQDHPLVLMVNDVSHNWURPHWULMD]LQGXNWLYQR
VNORSOMHQRSOD]PR ,&32(6
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: FprCEN/TR 10367
ICS:
77.080.20 Jekla Steels
kSIST-TP FprCEN/TR 10367:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TP FprCEN/TR 10367:2019
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kSIST-TP FprCEN/TR 10367:2019
FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 10367
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
January 2019
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 draft Technical Report is submitted to CEN members for Vote. It has been drawn up by the Technical Committee CEN/TC
459/SC 2.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey 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 Technical Report. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a Technical Report.
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. FprCEN/TR 10367:2019 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TP FprCEN/TR 10367:2019
FprCEN/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 . 7
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
A.1 Resolution of a spectrometer . 13
A.2 Short and long-term stability . 14
A.3 Evaluating the Background Equivalent Concentration . 14
Annex B (informative) Composition of the samples used for the validation precision test . 15
Bibliography . 17
2
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kSIST-TP FprCEN/TR 10367:2019
FprCEN/TR 10367:2019 (E)
European foreword
This document (FprCEN/TR 10367:2019) has been prepared by Technical Committee ECISS/TC 102
“Methods of Chemical analysis of iron and steel”, the secretariat of which is held by SIS.
This document is currently submitted to the Vote on TR.
3
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kSIST-TP FprCEN/TR 10367:2019
FprCEN/TR 10367:2019 (E)
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
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 http://www.iso.org/obp
4
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kSIST-TP FprCEN/TR 10367:2019
FprCEN/TR 10367:2019 (E)
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 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
5.1 General
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.
5.2 Hydrochloric acid, HCl (ρ = 1,19 g/ml)
20
5.3 Nitric acid, HNO (ρ = 1,33 g/ml)
3 20
5.4 Hydrofluoric acid, HF (ρ = 1,13 g/ml)
20
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.
5.5 Sulphuric acid, H SO (ρ = 1,84 g/ml)
2 4 20
5.6 Sulphuric acid, solution 1 + 1
While cooling, add 25 ml of sulphuric acid (5.5) to 25 ml of water.
5.7 Potassium hydrogen sulphate [KH SO ] or potassium disulphate [K S O ]
2 4 2 2 7
5
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FprCEN/TR 10367:2019 (E)
5.8 Chromium standard solution, 10 g/l
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 (5.2). 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.
5.9 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 (5.2). 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.
5.10 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.
5.11 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
6.1 General
All volumetric glassware shall be class A and calibrated, in accordance with EN ISO 648 or EN ISO 1042
as appropriate.
6.2 Fine texture filter paper
6.3 Platinum crucibles
6.4 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.
6
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kSIST-TP FprCEN/TR 10367:2019
FprCEN/TR 10367:2019 (E)
7 Sampling
Sampling shall be carried out in accordance with EN ISO 14284 or with an appropriate national
standard for steels.
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
Cr
Transfer the test portion (8.1) into a 250 ml beaker.
Add 15 ml of hydrochloric acid (5.2), cover with a watch glass, heat gently until the attack reaction
ceases, and then add dropwise, 10 ml of nitric acid (5.3).
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 (6.2) 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 (5.3) several times
and collect the washings in the 200 ml one-mark volumetric flask.
Transfer the filter into a platinum crucible (6.3), 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 (5.6) and 2 ml of
hydrofluoric acid (5.4). Evaporate to dryness and cool.
Add into the crucible 1,00 g of potassium hydrogen sulphate or potassium disulphate (5.7) 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 (5.7) can be
regenerated by allowing the melt to cool, adding some drops of sulphuric acid (5.5) 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 (5.7) 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 (5.2) 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 (5.2) can be increased, provide 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 (5.11) can be added at this stage. In this case, omit this operation when diluting the sample solution.
7
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kSIST-TP FprCEN/TR 10367:2019
FprCEN/TR 10367:2019 (E)
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 (5.2).
NOTE 5 Depending on the instrument performances, the final concentration of the test solution can be lower
(or higher), provide the corresponding calibration solutions have the same final concentration.
If an internal reference element is used, add, with a calibrated pipette, 10 ml of the internal reference
element solution (5.11).
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 Pre
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