SIST EN 15024-2:2018
(Main)Copper and copper alloys - Determination of zinc content - Part 2: Flame atomic absorption spectrometric method (FAAS)
Copper and copper alloys - Determination of zinc content - Part 2: Flame atomic absorption spectrometric method (FAAS)
This part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the zinc content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having zinc mass fractions between 0,000 5 % and 6,0 %.
Kupfer und Kupferlegierungen - Bestimmung des Zinkgehaltes - Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Dieser Teil dieser Europäischen Norm legt ein flammenatomabsorptionsspektrometrisches Verfahren (FAAS) für die Bestimmung des Zinkgehaltes in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als plastisch oder nicht plastisch geformte Produkte vorliegen.
Das Verfahren ist geeignet für Produkte mit Zink-Massenanteilen zwischen 0,000 5 % und 5,0 %.
Cuivre et alliages de cuivre - Dosage du zinc - Partie 2 : Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
La présente partie de cette Norme européenne spécifie une méthode par spectrométrie d’absorption atomique dans la flamme (SAAF) pour la détermination des teneurs en zinc dans le cuivre et les alliages de cuivre sous forme de produits non corroyés, corroyés ou moulés.
La méthode est applicable aux produits ayant une teneur en zinc comprise entre 0,000 5 % et 5,0 %.
Baker in bakrove zlitine - Določevanje cinka - 2. del: Metoda s plamensko atomsko absorpcijsko spektrometrijo (FAAS)
Del tega evropskega standarda določa metodo s plamensko atomsko absorpcijsko spektrometrijo (FAAS) za določevanje cinka v bakru in bakrovih zlitinah v negnetenih, gnetenih in ulitih proizvodih. Ta metoda se uporablja za proizvode z masnim deležem cinka med 0,0005 % in 6 %.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Bestimmung des Zinkgehaltes - Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)Cuivre et alliages de cuivre - Dosage du zinc - Partie 2 : Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)Copper and copper alloys - Determination of zinc content - Part 2: Flame atomic absorption spectrometric method (FAAS)77.120.30Baker in bakrove zlitineCopper and copper alloysICS:Ta slovenski standard je istoveten z:EN 15024-2:2018SIST EN 15024-2:2018en01-junij-2018SIST EN 15024-2:2018SLOVENSKI
STANDARDSIST EN 15024-2:20071DGRPHãþD
SIST EN 15024-2:2018
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15024-2
April
t r s z ICS
y yä s t rä u r Supersedes EN
s w r t væ tã t r r xEnglish Version
Copper and copper alloys æ Determination of zinc content æPart
tã Flame atomic absorption spectrometric method Cuivre et alliages de cuivre æ Détermination de la teneur en zinc æ Partie
t ã Méthode par spectrométrie
Kupfer und Kupferlegierungen æ Bestimmung des Zinkgehaltes æ Teil
tã Flammenatomabsorptionsspektrometrisches This European Standard was approved by CEN on
s z January
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels
9
t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s w r t væ tã t r s z ESIST EN 15024-2:2018
EN 15024-2:2018 (E) 2 Contents Page European foreword . 3 1 Scope . 4 2 Normative references . 4 3 Principle . 4 4 Reagents . 4 5 Apparatus . 5 6 Sampling . 5 7 Procedure. 5 7.1 Preparation of the test portion solution . 5 7.2 Blank test . 6 7.3 Check test . 6 7.4 Establishment of the calibration curve . 7 7.5 Determination . 9 8 Expression of results . 10 8.1 Use of the calibration curve . 10 8.2 Use of bracketing method . 11 9 Precision . 11 10 Test report . 13 Bibliography . 14
SIST EN 15024-2:2018
EN 15024-2:2018 (E)
3 European foreword This document (EN 15024-2:2018) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. 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 October 2018, and conflicting national standards shall be withdrawn at the latest by October 2018. 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 15024-2:2006. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis” to prepare the following standard: EN 15024-2, Copper and copper alloys — Determination of zinc content — Part 2: Flame atomic absorption spectrometric method (FAAS) This is one of two parts of the standard for the determination of zinc content in copper and copper alloys. The other part is: prEN 15024-1, Copper and copper alloys — Determination of zinc content — Part 1: Titrimetric method In comparison with EN 15024-2:2006, the following significant changes were made: a) The upper limit of the zinc mass fraction has been reduced from 6,0 % to 5,0 %; b) Fluoroboric-nitric acid mixture has been replaced by a solution of hydrochloric and nitric acids for the dissolution of the test portion; c) The concentrations of the zinc stock solution and the copper base solutions have been modified; d) The use of a continuum source xenon short arc lamp has been added as an alternative to the use of a zinc hollow-cathode lamp; e) The precision data have been updated. 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. SIST EN 15024-2:2018
EN 15024-2:2018 (E) 4 1 Scope This part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the zinc content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having zinc mass fractions between 0,000 5 % and 5,0 %. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1811-1, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 1: Sampling of cast unwrought products ISO 1811-2, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 2: Sampling of wrought products and castings 3 Principle Dissolution of a test portion in hydrochloric and nitric acid solution followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 213,8 nm line emitted by a zinc hollow-cathode lamp or a continuum source xenon short arc lamp. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid = 1,19 g/ml). 4.2 Hydrochloric acid solution, 1 + 1. Add 500 ml of hydrochloric acid (4.1) to 500 ml of water. 4.3 Nitric acid, HNO3
= 1,40 g/ml). 4.4 Nitric acid solution, 1 + 1. Add 500 ml of nitric acid (4.3) to 500 ml of water. 4.5 Zinc stock solution, 1 g/l Zn. Weigh (1 ± 0,001) g of zinc (Zn
· 99,99 %) and transfer it into a 250 ml beaker. Add 50 ml of hydrochloric acid solution (4.2). Cover with a watch glass and heat gently to assist dissolution. When dissolution is complete, cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Zn. SIST EN 15024-2:2018
EN 15024-2:2018 (E)
5 4.6 Zinc standard solution, 0,01 g/l Zn. Transfer 5,0 ml of the zinc stock solution (4.5) into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 0,01 mg of Zn. 4.7 Zinc standard solution, 0,001 g/l Zn. Transfer 25,0 ml of the zinc standard solution (4.6) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 0,001 mg of Zn. 4.8 Copper base solution, 50 g/l Cu. Transfer 50,0 g of zinc-free copper (Cu
· 99,99 %) into a 2 000 ml beaker. Add 500 ml of hydrochloric acid (4.1) and, by small fractions, 250 ml of nitric acid (4.3). Cover with a watch glass and heat gently until the copper has been completely dissolved, then heat up to the boiling point until the nitrous fumes have been expelled. Cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9 Copper base solution, 2 g/l Cu Transfer 10,0 ml of copper base solution (4.8) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.2 Zinc hollow-cathode lamp or a continuum source xenon short arc lamp. 6 Sampling Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2, as appropriate. Test samples shall be in the form of fine drillings, chips or millings, with a maximum thickness of 0,5 mm. 7 Procedure 7.1 Preparation of the test portion solution 7.1.1 Test portion Weigh (1 ± 0,001) g of the test sample. 7.1.2 Test portion solution Transfer the test portion (7.1.1) into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, and wash the beaker cover and the sides of the beaker with water. SIST EN 15024-2:2018
EN 15024-2:2018 (E) 6 7.1.3 Zinc mass fractions between 0,000 5 % and 0,01 % Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. NOTE The validation inter-laboratory
test of this method showed that for zinc mass fractions near 0,01 % results are better when the determination is carried out following 7.1.3. 7.1.4 Zinc mass fractions between 0,01 % and 0,10 % Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 10,0 ml of this solution, into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. NOTE The validation inter-laboratory test of this method showed
...
SLOVENSKI STANDARD
oSIST prEN 15024-2:2016
01-december-2016
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Copper and copper alloys - Determination of zinc content - Part 2: Flame atomic
absorption spectrometric method (FAAS)
Kupfer und Kupferlegierungen - Bestimmung des Zinkgehaltes - Teil 2:
Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)
Cuivre et alliages de cuivre - Dosage du zinc - Partie 2 : Méthode par spectrométrie
d'absorption atomique dans la flamme (SAAF)
Ta slovenski standard je istoveten z: prEN 15024-2
ICS:
77.120.30 Baker in bakrove zlitine Copper and copper alloys
oSIST prEN 15024-2:2016 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 15024-2:2016
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oSIST prEN 15024-2:2016
DRAFT
EUROPEAN STANDARD
prEN 15024-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2016
ICS 77.120.30 Will supersede EN 15024-2:2006
English Version
Copper and copper alloys - Determination of zinc content -
Part 2: Flame atomic absorption spectrometric method
(FAAS)
Cuivre et alliages de cuivre - Dosage du zinc - Partie 2 : Kupfer und Kupferlegierungen - Bestimmung des
Méthode par spectrométrie d'absorption atomique Zinkgehaltes - Teil 2:
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
CEN/TC 133.
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, 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: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15024-2:2016 E
worldwide for CEN national Members.
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oSIST prEN 15024-2:2016
prEN 15024-2:2016 (E)
Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Principle . 4
4 Reagents . 4
5 Apparatus . 5
6 Sampling . 5
7 Procedure. 5
7.1 Preparation of the test portion solution . 5
7.1.1 Test portion . 5
7.1.2 Test portion solution . 5
7.1.3 Zinc mass fractions between 0,000 5 % and 0,01 % . 5
7.1.4 Zinc mass fractions between 0,01 % and 0,10 % . 6
7.1.5 Zinc mass fractions between 0,10 % and 1,00 % . 6
7.1.6 Zinc mass fractions between 1,0 % and 5,0 % . 6
7.2 Blank test . 6
7.3 Check test . 6
7.4 Establishment of the calibration curve . 6
7.4.1 Preparation of the calibration solutions . 6
7.4.2 Adjustment of the atomic absorption spectrometer . 9
7.4.3 Spectrometric measurement of the calibration solutions . 9
7.4.4 Calibration curve . 9
7.5 Determination . 9
7.5.1 General . 9
7.5.2 Preliminary spectrometric measurement . 9
7.5.3 Spectrometric measurements . 10
8 Expression of results . 10
8.1 Use of the calibration curve . 10
8.2 Use of bracketing method . 10
9 Precision . 11
Bibliography . 13
2
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oSIST prEN 15024-2:2016
prEN 15024-2:2016 (E)
European foreword
This document (prEN 15024-2:2016) has been prepared by Technical Committee CEN/TC 133 “Copper and
copper alloys”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 15024-2:2006.
Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods
of analysis” to prepare the following standard:
EN 15024-2, Copper and copper alloys — Determination of zinc content — Part 2: Flame atomic absorption
spectrometric method (FAAS)
This is one of two parts of the standard for the determination of zinc content in copper and copper alloys.
The other part is:
prEN 15024-1, Copper and copper alloys — Determination of zinc content — Part 1: Titrimetric method
In comparison with EN 15024-2:2006, the following significant changes were made:
a) The upper limit of the zinc mass fraction has been reduced from 6,0 % to 5,0 %;
b) Fluoroboric-nitic acid mixture has been replaced by a solution of hydrochloric and nitric acid for the
dissolution of the test portion;
c) The concentrations of the zinc stock solution and the copper base solutions have been modified;
d) The use of a continuum source xenon short arc lamp has been added as an alternative to the use of a zinc
hollow-cathode lamp;
e) The precision data have been updated.
3
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oSIST prEN 15024-2:2016
prEN 15024-2:2016 (E)
1 Scope
This part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for
the determination of the zinc content of copper and copper alloys in the form of unwrought, wrought and
cast products.
The method is applicable to products having zinc mass fractions between 0,000 5 % and 5,0 %.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
ISO 1811-1, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 1:
Sampling of cast unwrought products
ISO 1811-2, Copper and copper alloys — Selection and preparation of samples for chemical analysis — Part 2:
Sampling of wrought products and castings
3 Principle
Dissolution of a test portion in hydrochloric and nitric acid solution followed, after suitable dilution, by
aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption
of the 213,8 nm line emitted by a zinc hollow-cathode lamp or a continuum source xenon short arc lamp.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of
equivalent purity.
4.1 Hydrochloric acid, HCl (ρ = 1,19 g/ml)
4.2 Hydrochloric acid solution, 1 + 1
Add 500 ml of hydrochloric acid (4.1) to 500 ml of water.
4.3 Nitric acid, HNO (ρ = 1,40 g/ml)
3
4.4 Nitric acid solution, 1 + 1
Dilute 500 ml of nitric acid (4.3) in 500 ml of water
4.5 Zinc stock solution, 1 g/l Zn
Weigh (1 ± 0,001) g of zinc (Zn ≥ 99,99 %) and transfer it into a 250 ml beaker. Add 50 ml of hydrochloric
acid (4.2). Cover with a watch glass and heat gently to assist dissolution. When dissolution is complete, cool
to room temperature 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 Zn.
4.6 Zinc standard solution, 0,01 g/l Zn
Transfer 5,0 ml of the zinc stock solution (4.5) into a 500 ml one-mark volumetric flask. Dilute to the mark
with water and mix well.
1 ml of this solution contains 0,01 mg of Zn.
4
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oSIST prEN 15024-2:2016
prEN 15024-2:2016 (E)
4.7 Zinc standard solution, 0,001 g/l Zn
Transfer 25,0 ml of the zinc standard solution (4.6) into a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix well.
1 ml of this solution contains 0,001 mg of Zn.
4.8 Copper base solution, 50 g/l Cu
Transfer 50,0 g of zinc-free copper (Cu ≥ 99,99 %) into a 2 000 ml beaker. Add 500 ml of hydrochloric acid
(4.1) and, by small fractions, 250 ml of nitric acid (4.3). Cover with a watch glass and heat gently until the
copper has been completely dissolved, then heat up to the boiling point until the nitrous fumes have been
expelled. Cool to room temperature and transfer the solution quantitatively into a 1 000 ml one-mark
volumetric flask, dilute to the mark with water and mix.
4.9 Copper base solution, 2 g/l Cu
Transfer 10,0 ml of copper base solution (4.8) into a 250 ml one-mark volumetric flask. Dilute to the mark
with water and mix.
5 Apparatus
5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner.
5.2 Zinc hollow-cathode lamp or a continuum source xenon short arc lamp
6 Sampling
Sampling shall be carried out in accordance with ISO 1811-1 or ISO 1811-2, as appropriate.
Test samples shall be in the form of fine drillings, chips or millings, with a maximum thickness of 0,5 mm.
7 Procedure
7.1 Preparation of the test portion solution
7.1.1 Test portion
Weigh (1 ± 0,001) g of the test sample.
7.1.2 Test portion solution
Transfer the test portion into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric
acid solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved
and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature,
and wash the beaker cover and the sides of the beaker with water.
7.1.3 Zinc mass fractions between 0,000 5 % and 0,01 %
Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to
t
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