EN 15024-2:2018

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

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
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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

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of an identical text or by endorsement, at the latest by October 2018, and conflicting national standards shall be withdrawn at the latest by October 2018.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

= 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

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

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 that for zinc mass fractions near 0,1 % results are better when the determination is carried out following 7.1.4. 7.1.5 Zinc mass fractions between 0,10 % and 1,00 % 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 2,0 ml of this solution, into a 200 ml one-mark volumetric flask and add 10,0 ml of hydrochloric acid (4.1). 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 1,0 % results are better when the determination is carried out following 7.1.5. 7.1.6 Zinc mass fractions between 1,0 % and 5,0 % Transfer the test portion solution (7.1.2) quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 2,5 ml of this solution into a 200 ml one-mark volumetric flask and add 10,0 ml of hydrochloric acid (4.1). Dilute to the mark with water and mix well. 7.2 Blank test Carry out a blank test simultaneously with the determination, following the same procedure and using the same quantities of all reagents as used for the determination, but substituting pure copper for the test portion. 7.3 Check test Make a preliminary check of the apparatus by preparing a solution of a reference material or a synthetic sample containing a known amount of zinc and of a composition similar to the material to be analysed. Carry out the procedure specified in 7.5. SIST EN 15024-2:2018

7 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, copper, chloride and nitrate concentrations, and acidity in the calibration solutions shall be similar to those of the test portion solutions. The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the test portion solution. Normally no similar a
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