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

Status
Published
Public Enquiry End Date
05-Sep-2018
Publication Date
01-Jul-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Jun-2019
Due Date
25-Aug-2019
Completion Date
02-Jul-2019

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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

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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 -

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.

Through its subcommittee SC 2 “Methods of chemical analysis for iron and steel” (secretariat: SIS)

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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.
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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.

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.

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
...

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