SIST EN 10177:2019
(Main)Steels - Determination of calcium content - Flame atomic absorption spectrometric method (FAAS)
Steels - Determination of calcium content - Flame atomic absorption spectrometric method (FAAS)
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of calcium content in non-alloy and low alloy steels.
The method is applicable to calcium contents between 0,000 4 % and 0,012 %.
The method can be adapted to higher calcium 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 - Bestimmung des Calciumgehalt - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Dieses Dokument legt ein Verfahren zur Bestimmung von Calciumin unlegierter und niedrig legierter Stähle mittels Flammenatomabsorptionsspektroskopie (FAAS) fest.
Dieses Verfahren ist anwendbar für Calciumanteile von 4 μg/g bis 120 μg/g.
Diese Verfahren kann für höhere Calciumgehalte angewandt werden, wenn die Probengrößen und Lösungsvorgänge angepasst werden, sofern die in 6.2.2 und 6.2.3 angegebenen Kriterien erfüllt werden.
Aciers - Détermination de la teneur en calcium - 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 calcium dans les aciers non alliés et faiblement alliés.
La méthode s'applique aux teneurs en calcium comprises entre 0,000 4 % et 0,012 %.
La méthode peut être adaptée à des teneurs en calcium 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.
Jeklo - Določevanje kalcija - Metoda s plamensko atomsko absorpcijsko spektrometrijo (FAAS)
Ta dokument določa metodo plamenske atomske absorpcijske spektrometrije (FAAS) za določevanje kalcija v nelegiranih in malolegiranih jeklih.
Ta metoda se uporablja za vsebnosti kalcija med 0,0004 % in 0,012 %.
Metodo je mogoče prilagoditi vsebnostim kalcija 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 10177:2019
01-september-2019
Nadomešča:
SIST EN 10177:1998
Jeklo - Določevanje kalcija - Metoda s plamensko atomsko absorpcijsko
spektrometrijo (FAAS)
Steels - Determination of calcium content - Flame atomic absorption spectrometric
method (FAAS)
Stahl - Bestimmung des Calciumgehalt - Flammenatomabsorptionsspektrometrisches
Verfahren (FAAS)
Aciers - Détermination de la teneur en calcium - Méthode par spectrométrie d'absorption
atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: EN 10177:2019
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
SIST EN 10177:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 10177:2019
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SIST EN 10177:2019
EN 10177
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2019
EUROPÄISCHE NORM
ICS 77.040.30 Supersedes EN 10177:1989
English Version
Steels - Determination of calcium content - Flame atomic
absorption spectrometric method (FAAS)
Aciers - Détermination de la teneur en calcium - Stahl - Bestimmung des Calciumgehalt -
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 10177:2019 E
worldwide for CEN national Members.
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SIST EN 10177:2019
EN 10177:2019 (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 . 5
6.1 Ordinary laboratory apparatus . 5
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. 6
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 . 7
8.3.4 Adjustment of the atomic absorption spectrometer . 8
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 . 10
Annex A (informative) Precision . 11
Bibliography . 12
2
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SIST EN 10177:2019
EN 10177:2019 (E)
European foreword
This document (EN 10177:2019) 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 10177:1989.
In comparison with EN 10177:1989, the following significant technical changes were made:
— Clause 1: limits of the scope changed;
— Normative references: revised;
— Clause 4: possibility for using aqua regia for the dissolution and other suitable radiation sources
added;
— Clause 5: preparation of iron base solution added;
— 8.3: details regarding the preparation of the test solution added
— 8.3.3: calibration solutions expanded;
— 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 10177:2019
EN 10177:2019 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of calcium content in non-alloy and low alloy steels.
The method is applicable to calcium contents between 4 µg/g and 120 µg/g.
The method can be adapted to higher calcium 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 hydrochloric acid followed by oxidation with nitric acid.
NOTE 1 Aqua regia can be used for simultaneous dissolution and oxidation of the test portion.
Addition of a solution of potassium chloride and nebulization of the test solution into an
acetylene/nitrous oxide flame of an atomic absorption spectrometer.
NOTE 2 Potassium chloride is added to suppress ionization of calcium.
Spectrometric measurement of the atomic absorption of the 422,7 nm spectral line emitted by a calcium
hollow-cathode lamp.
NOTE 3 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.
4
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SIST EN 10177:2019
EN 10177:2019 (E)
5.2 Hydrochloric acid solution, 1 + 1.
Add 500 ml of hydrochloric acid (ρ = 1,19 g/ml, approximately) to 500 ml of water and mix.
20
5.3 Nitric acid solution, 4 + 6.
Add 400 ml of nitric acid (ρ = 1,40 g/ml, approximately) to 600 ml of water and mix.
20
5.4 Potassium chloride solution, 190 g/l.
5.5 Calcium standard solution, 1 g/l.
Weigh (2,500 ± 0,001) g of pure calcium carbonate, dried at 105 °C and transfer into glassware of
suitable size. Add 20 ml of water and then, slowly, 20 ml of hydrochloric acid (5.2).
When dissolved, dilute to 100 ml approximately with water and transfer the solution quantitatively into
a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of calcium.
5.6 Calcium standard solution, 0,02 g/l.
Transfer 5,0 ml of calcium standard solution (5.5) 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 0,02 mg of calcium.
5.7 Calcium standard solution, 0,002 g/l.
Transfer 20,0 ml of calcium standard solution (5.6) into a 200 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 0,002 mg of calcium.
5.8 Iron base solution, 50 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 hydrochloric acid (5.2), cover the glassware with a watch glass and heat
gently until the reaction ceases. Oxidize with 25 ml of nitric acid (5.3) and then boil the solution for
5 min to remove nitrogen oxides.
Allow to cool and transfer the solution quantitatively into a 200 ml one-mark volumetric flask.
Add 2,5 ml of potassium chloride (5.4), dilute to the mark with water and mix.
6 Apparatus
6.1 Ordinary laboratory apparatus
All volum
...
SLOVENSKI STANDARD
oSIST prEN 10177:2018
01-september-2018
-HNOR'RORþHYDQMHNDOFLMD0HWRGDVSODPHQVNRDWRPVNRDEVRUSFLMVNR
VSHNWURPHWULMR )$$6
Steels - Determination of calcium content - Flame atomic absorption spectrometric
method (FAAS)
Stahl - Bestimmung des Calciumgehalt - Flammenatomabsorptionsspektrometrisches
Verfahren (FAAS)
Aciers - Détermination de la teneur en calcium - Méthode par spectrométrie d'absorption
atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: prEN 10177
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
oSIST prEN 10177:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 10177:2018
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oSIST prEN 10177:2018
DRAFT
EUROPEAN STANDARD
prEN 10177
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2018
ICS 77.040.30 Will supersede EN 10177:1989
English Version
Steels - Determination of calcium content - Flame atomic
absorption spectrometric method (FAAS)
Aciers - Détermination de la teneur en calcium - Stahl - Bestimmung des Calciumgehalt -
Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches
dans la flamme (SAAF) 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 10177:2018 E
worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 10177:2018
prEN 10177:2018 (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 10177:2018
prEN 10177:2018 (E)
European foreword
This document (prEN 10177:2018) 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 10177:1989.
3
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oSIST prEN 10177:2018
prEN 10177:2018 (E)
1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of calcium content in non-alloy and low alloy steels.
The method is applicable to calcium contents between 0,000 4 % and 0,012 %.
The method can be adapted to higher calcium 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 hydrochloric acid followed by oxidation with nitric acid.
NOTE 1 Aqua regia can be used for simultaneous dissolution and oxidation of the test portion.
Addition of a solution of potassium chloride and nebulization of the test solution into an
acetylene/nitrous oxide flame of an atomic absorption spectrometer.
NOTE 2 Potassium chloride is added to suppress ionization of calcium.
Spectrometric measurement of the atomic absorption of the 422,7 nm spectral line emitted by a calcium
hollow-cathode lamp.
NOTE 3 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.
5.2 Hydrochloric acid solution, 1 + 1.
Add 500 ml of hydrochloric acid (ρ = 1,19 g/ml, approximately) to 500 ml of water and mix.
20
4
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oSIST prEN 10177:2018
prEN 10177:2018 (E)
5.3 Nitric acid solution, 4 + 6.
Add 400 ml of nitric acid (ρ = 1,40 g/ml, approximately) to 600 ml of water and mix.
20
5.4 Potassium chloride solution, 190 g/l.
5.5 Calcium standard solution, 1 g/l.
Weigh (2,500 ± 0,001) g of pure calcium carbonate, dried at 105 °C and transfer into a glassware of
suitable size. Add 20 ml of water and then, slowly, 20 ml of hydrochloric acid (5.2).
When dissolved, dilute to 100 ml approximately with water and transfer the solution quantitatively into
a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1 mg of calcium.
5.6 Calcium standard solution, 0,02 g/l.
Transfer 5,0 ml of calcium standard solution (5.5) 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 0,02 mg of calcium.
5.7 Calcium standard solution, 0,002 g/l.
Transfer 20,0 ml of calcium standard solution (5.6) into a 200 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 0,002 mg of calcium.
5.8 Iron base solution, 50 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 hydrochloric acid (5.2), cover the beaker with a watch glass and heat gently
until the reaction ceases. Oxidise with 25 ml of nitric acid (5.3) and then boil the solution for 5 min to
remove nitrogen oxides.
Allow to cool and transfer the solution quantitatively into a 200 ml one-mark volumetric flask.
Add 2,5 ml of potassium chloride (5.4), 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.
All glassware shall be washed in hydrochloric acid (5.2) and then in water. The quantity of calcium
present in the beakers and the volumetric flasks can be checked by measuring the absorption of distilled
water introduced in the glassware after the acid washing.
5
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oSIST prEN 10177:2018
prEN 10177:2018 (E)
6.2 Atomic absorption spectrometer
6.2.1 General
The spectrometer shall be equipped with a calcium hollow-cathode lamp or other suitable radiation
source and supplied with acetylene and nitrous oxide sufficiently pure to give a steady clear fuel-lean
flame, free from water and oil, and free from calcium.
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 3 % 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 1 % 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
...
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