SIST EN 10136:2019
(Main)Steels and cast irons - Determination of nickel content - Flame atomic absorption spectrometric method (FAAS)
Steels and cast irons - Determination of nickel content - Flame atomic absorption spectrometric method (FAAS)
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of nickel content in steels and cast irons.
The method is applicable to nickel contents between 0,004 % and 2,0 %.
The method can be adapted to lower or higher nickel contents by changing the test portion or the dilution process, provided the criteria in 5.2.2 and 5.2.3 are still met.
Stahl und Eisen Stahl und Eisen - Bestimmung des Nickelanteils - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Flammenatomabsorptionsspektroskopie (FAAS) fest.
Dieses Verfahren ist anwendbar für Nickelgehalte von 0,004 % (Masseanteil) bis 2,0 % (Masseanteil).
Dieses Verfahren kann für niedrigere als auch höhere Nickelgehalte angewandt werden, wenn die Probengrößen oder Lösungsvorgänge angepasst werden, sofern die in 6.2.2 und 6.2.3 angegebenen Kriterien weiterhin erfüllt werden.
Aciers et fontes - Détermination de la teneur en nickel - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
Le présent document spécifie une méthode par spectrométrie d'absorption atomique dans la flamme (SAAF) pour la détermination des teneurs en nickel dans les aciers et les fontes.
La méthode s'applique aux teneurs en nickel comprises entre 0,004 % et 2,0 %.
La méthode peut être adaptée à des teneurs en nickel inférieures ou supérieures en modifiant la prise d'essai ou le facteur de dilution, sous réserve que les critères énoncés en 6.2.2 et 6.2.3 soient respectés.
Jeklene in železove litine - Določevanje niklja - Metoda plamenske atomske absorpcijske spektrometrije (FAAS)
Ta dokument določa metodo plamenske atomske absorpcijske spektrometrije (FAAS) za določevanje niklja v jeklih in železovih litinah.
Ta metoda se uporablja za vsebnosti niklja med 0,004 % in 2,0 %.
Metodo je mogoče prilagoditi nižjim ali višjim vsebnostim niklja s spreminjanjem preskusne količine ali procesa redčenja, če so kriteriji iz točk 5.2.2 in 5.2.3 še vedno izpolnjeni.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 10136:2019
01-september-2019
Nadomešča:
SIST EN 10136:1997
Jeklene in železove litine - Določevanje niklja - Metoda plamenske atomske
absorpcijske spektrometrije (FAAS)
Steels and cast irons - Determination of nickel content - Flame atomic absorption
spectrometric method (FAAS)
Stahl und Eisen Stahl und Eisen - Bestimmung des Nickelanteils -
Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Aciers et fontes - Détermination de la teneur en nickel - Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: EN 10136:2019
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
SIST EN 10136:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 10136:2019
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SIST EN 10136:2019
EN 10136
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 77.040.30 Supersedes EN 10136:1989
English Version
Steels and cast irons - Determination of nickel content -
Flame atomic absorption spectrometric method (FAAS)
Aciers et fontes - Détermination de la teneur en nickel - Stahl und Gusseisen - Bestimmung des Nickelanteils -
Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches
dans la flamme (SAAF) Verfahren (FAAS)
This European Standard was approved by CEN on 22 April 2019.
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, 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.
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. EN 10136:2019 E
worldwide for CEN national Members.
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SIST EN 10136:2019
EN 10136:2019 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 6
6.1 Ordinary laboratory apparatus . 6
6.2 Atomic absorption spectrometer . 6
6.2.1 General . 6
6.2.2 Minimum precision . 6
6.2.3 Additional performance requirements . 6
7 Sampling . 6
8 Procedure. 7
8.1 Test portion . 7
8.2 Blank test . 7
8.3 Determination . 7
8.3.1 Preparation of the test solution . 7
8.3.2 Treatment of the test solution . 7
8.3.3 Preparation of the calibration solutions . 8
8.3.4 Adjustment of the atomic absorption spectrometer . 9
8.3.5 Spectrometric measurements . 9
9 Expression of results . 10
9.1 Use of the calibration curve . 10
9.2 Use of bracketing method . 10
10 Test report . 11
Annex A (informative) Precision . 12
Bibliography . 13
2
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SIST EN 10136:2019
EN 10136:2019 (E)
European foreword
This document (EN 10136:2019) has been prepared by Technical Committee CEN/TC 459 “ECISS -
1
European Committee for Iron and Steel Standardization” , the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 10136:1989.
In comparison with EN 10136:1989, the following significant technical changes were made:
— Clause 1: lower limit of the scope changed;
— Normative references: revised;
— Clause 4: possibility for using other suitable radiation sources added;
— Clause 5: preparation of iron base solutions added;
— 8.3: details regarding the preparation of the test solution added;
— 8.3.3: calibration solutions expanded;
— 8.3.4: background correction specified;
— 8.3.5 and Clause 9: bracketing method for the spectrometric measurements added;
— Clause 10: editorially updated;
— Bibliography: added.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, 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 the United Kingdom.
1
Through its subcommittee SC 2 “Methods of chemical analysis for iron and steel” (secretariat: SIS)
3
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SIST EN 10136:2019
EN 10136:2019 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of nickel content in steels and cast irons.
The method is applicable to nickel contents between 0,004 % (weight percent) and 2,0 % (weight
percent).
The method can be adapted to lower or higher nickel contents by changing the test portion or the
dilution process, provided the criteria in 6.2.2 and 6.2.3 are still met.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 648, Laboratory glassware — Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)
EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition (ISO 14284)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
4 Principle
Dissolution of a test portion in a mixture of appropriate acids and fuming with perchloric acid.
Nebulisation of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 232,0 nm or 352,5 nm spectral line emitted
by a nickel hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used, provided the criteria in 6.2.2 and 6.2.3 are still met.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water
of equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into
account in 8.3 and Clause 9.
5.1 Pure iron, with nickel content < 0,000 5 %.
4
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SIST EN 10136:2019
EN 10136:2019 (E)
5.2 Hydrochloric-nitric acids mixture.
Mix three volumes of hydrochloric acid ( ρ = 1,19 g/ml approximately), one volume of nitric
20
acid (ρ = 1,40 g/ml approximately) and two volumes of water.
20
This mixture shall be prepared immediately before use.
5.3 Nitric-perchloric acids mixture.
Mix 100 ml of nitric acid (ρ = 1,40 g/ml approximately) with 800 ml of perchloric acid (ρ = 1,54 g/ml
20 20
approximately). Dilute to one litre with water and mix.
Perchloric acid (ρ = 1,67 g/ml approximately) may also be used. 100 ml of perchloric
20
acid (ρ = 1,54 g/ml approximately) are equivalent to 79 ml of perchloric acid (ρ = 1,67 g/ml
20 20
approximately).
5.4 Nickel standard solution, 1 g/l.
Weigh (0,500 ± 0,001) g of nickel (Ni ≥ 99,9 %) and transfer into a heat-resistant glassware of suitable
size. Add 25 ml of nitric acid (ρ = 1,40 g/ml approximately), diluted 1 + 1. Cover with a watch glass,
20
and, if necessary, heat gently to assist dissolution. When dissolution is complete, boil to remove
nitrogen oxides. Allow to cool to room temperature and transfer the solution quantitatively into a
500 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1,0 mg of nickel.
5.5 Nickel standard solution, 0,04 g/l.
Transfer 10,0 ml of nickel standard solution (5.4) into a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,04 mg of nickel.
5.6 Iron base solution, 40 g/l.
Weigh, to the nearest 0,01 g, 10,00 g of pure iron (5.1) and transfer into a heat-resistant glassware of
suitable size. Add 100 ml of the hydrochloric-nitric acids mixture (5.2), cover the glassware with a
watch glass and heat gently until the iron is dissolved. Add 150 ml of the nitric-perchloric acids mixture
(5.3) and heat until dense white fumes of perchloric acid appear. Continue heating for one minute and
allow to cool.
In order to get a better mastery of the acidity (volume of free perchloric acid) of the sample solutions
and of the calibration solutions, perchloric fumes may be maintained until iron crystallizes.
Add 100 ml of water and heat gently to dissolve the salts. Cool again and transfer the solution
quantitatively into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix.
5.7 Iron base solution, 2 g/l.
Transfer 10,0 ml of iron base solution (5.6) into a 200 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
5
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SIST EN 10136:2019
EN 10136:2019 (E)
6 Apparatus
6.1 Ordinary laboratory apparatus
All volumetric glassware shall be class A, in accor
...
SLOVENSKI STANDARD
oSIST prEN 10136:2018
01-september-2018
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VSHNWURPHWULþQDPHWRGD )$$6
Steels and cast irons - Determination of nickel content - Flame atomic absorption
spectrometric method (FAAS)
Stahl und Eisen Stahl und Eisen - Bestimmung des Nickelanteils -
Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Aciers et fontes - Détermination de la teneur en nickel - Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: prEN 10136
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
oSIST prEN 10136:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 10136:2018
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oSIST prEN 10136:2018
DRAFT
EUROPEAN STANDARD
prEN 10136
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2018
ICS 77.040.30 Will supersede EN 10136:1989
English Version
Steels and cast irons - Determination of nickel content -
Flame atomic absorption spectrometric method (FAAS)
Aciers et fontes - Détermination de la teneur en nickel - Stahl und Eisen Stahl und Eisen - Bestimmung des
Méthode par spectrométrie d'absorption atomique Nickelanteils -
dans la flamme (SAAF) Flammenatomabsorptionsspektrometrisches
Verfahren (FAAS)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
ECISS/TC 102.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, 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 European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 10136:2018 E
worldwide for CEN national Members.
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oSIST prEN 10136:2018
prEN 10136:2018 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 4
5 Reagents . 4
6 Apparatus . 5
7 Sampling . 6
8 Procedure. 6
9 Expression of results . 10
10 Test report . 11
Annex A (informative) Precision . 12
A.1 General . 12
A.2 Repeatability . 12
A.3 Reproducibility . 12
Bibliography . 13
2
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oSIST prEN 10136:2018
prEN 10136:2018 (E)
European foreword
This document (prEN 10136:2018) has been prepared by Technical Committee ECISS/TC 102 “Methods
of chemical analysis for iron and steel”, the secretariat of which is held by SIS.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 10136:1989.
3
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oSIST prEN 10136:2018
prEN 10136:2018 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of nickel content in steels and cast irons.
The method is applicable to nickel contents between 0,004 % and 2,0 %.
The method can be adapted to lower or higher nickel contents by changing the test portion or the dilution
process, provided the criteria in 6.2.2 and 6.2.3 are still met.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN ISO 648, Laboratory glassware - Single-volume pipettes (ISO 648)
EN ISO 1042, Laboratory glassware - One-mark volumetric flasks (ISO 1042)
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 Principle
Dissolution of a test portion in a mixture of appropriate acids and fuming with perchloric acid.
Nebulisation of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 232,0 nm or 352,5 nm spectral line emitted
by a nickel hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used, provided the criteria in 6.2.2 and 6.2.3 are still met.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of
equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into account
in 8.3 and Clause 9.
5.1 Pure iron, with nickel content < 0,000 5 %.
5.2 Hydrochloric-nitric acids mixture.
Mix three volumes of hydrochloric acid (ρ = 1,19 g/ml, approximately), one volume of nitric
20
acid (ρ = 1,40 g/ml, approximately) and two volumes of water.
20
This mixture shall be prepared immediately before use.
4
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oSIST prEN 10136:2018
prEN 10136:2018 (E)
5.3 Nitric-perchloric acids mixture.
Mix 100 ml of nitric acid (ρ = 1,40 g/ml, approximately) with 800 ml of perchloric acid (ρ = 1,54 g/ml,
20 20
approximately). Dilute to one litre with water and mix.
Perchloric acid (ρ 1,67 g/ml approximately) may also be used. 100 ml of perchloric
20
acid (ρ approximately 1,54 g/ml) are equivalent to 79 ml of perchloric acid (ρ 1,67 g/ml
20 20
approximately).
5.4 Nickel standard solution, 1 g/l.
Weigh (0,500 ± 0,001) g of nickel (Ni ≥ 99,9 %) and transfer into a heat-resistant glassware of suitable
size. Add 25 ml of nitric acid (ρ = 1,40 g/ml, approximately), diluted 1 + 1. Cover with a watch glass and,
20
if necessary, heat gently to assist dissolution. When dissolution is complete boil to remove nitrogen
oxides. Allow to cool to room temperature and transfer the solution quantitatively into a 500 ml one-
mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1,0 mg of nickel.
5.5 Nickel standard solution, 0,04 g/l.
Transfer 10,0 ml of nickel standard solution (5.4) into a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,04 mg of nickel.
5.6 Iron base solution, 40 g/l.
Weigh, to the nearest 0,01 g, 10,00 g of pure iron (5.1) and transfer into a heat-resistant glassware of
suitable size. Add 100 ml of the hydrochloric-nitric acids mixture (5.2), cover the beaker with a watch
glass and heat gently until the iron is dissolved. Add 150 ml of the nitric-perchloric acids mixture (5.3)
and heat until dense white fumes of perchloric acid appear. Continue heating for one minute and allow to
cool.
In order to get a better mastery of the acidity (volume of free perchloric acid) of the sample solutions and
of the calibration solutions, perchloric fumes may be maintained until iron crystallizes.
Add 100 ml of water and heat gently to dissolve the salts. Cool again and transfer the solution
quantitatively into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix.
5.7 Iron base solution, 2 g/l.
Transfer 10,0 ml of iron base solution (5.6) into a 200 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
6 Apparatus
6.1 Ordinary laboratory apparatus
All volumetric glassware shall be class A, in accordance with EN ISO 648 or EN ISO 1042, as appropriate.
5
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oSIST prEN 10136:2018
prEN 10136:2018 (E)
6.2 Atomic absorption spectrometer
6.2.1 General
The spectrometer shall be equipped with a nickel hollow-cathode lamp or other suitable radiation source
and supplied with air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free from water
and oil, and free from nickel.
The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.4, the
limit of detection and characteristic concentration are in reasonable agreement with the values given by
the manufacturer and it meets the performance criteria given in 6.2.2 and 6.2.3.
6.2.2 Minimum precision
The standard deviation of 10 measurements of the absorbance of the most concentrated calibration
solution shall not exceed 1,0 % of the mean absorbance of this solution.
The standard deviation of 10 measurements of the absorbance of the least concentrated calibration
solution (excluding the zero member) shall not exceed 0,5 % of the mean absorbance of the most
concentrated calibration solution.
6.2.3 Additional performance requirements
6.2.3.1 General
It is also desirable that the instrument should conform to the additional performance requirements given
in 6.2.3.2 and 6.2.3.3.
6.2.3.2 Characteristic concentration
The characteristic concentration for nickel in a matrix similar to the final test solution shall be lower than
0,10 µg/ml.
6.2.3.3 Limit of detection
The limit of detection is a number, expressed in units of concentration (or amount) that describes the
lowest concentration level (or amount) of an ele
...
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