Copper and copper alloys - Determination of silver content - Flame atomic absorption spectrometric method (FAAS)

This European Standard specifies two flame atomic absorption spectrometric methods (FAAS) for the determination of the silver content of copper and copper alloys in the form of unwrought, wrought and cast products. The methods are applicable to products having silver mass fractions between 0,01 % and 2,0 %.
a) Method A is applicable to copper and copper alloys having silver mass fractions between 0,01 % and 1,0 % and containing antimony or tin not greater than 0,005 0 % or silicon not greater than 0,010 %.
b) Method B is applicable to copper and copper alloys having silver mass fractions between 0,01 % and 2,0 % and antimony or tin greater than 0,005 % and silicon greater than 0,010 %.

Kupfer und Kupferlegierungen - Bestimmung des Silbergehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)

Diese Europäische Norm legt zwei flammenatomabsorptionsspektrometrische Verfahren (FAAS) für die Bestimmung von Silbergehalten in Kupfer und Kupferlegierungen fest, die als Gussstücke oder als plastisch oder nicht plastisch geformte Produkte vorliegen.
Die Verfahren sind geeignet für Produkte mit Silber-Massenanteilen zwischen 0,01 % und 2,0 %.
a)   Verfahren A ist anwendbar auf Kupfer und Kupferlegierungen mit Silber-Massenanteilen zwischen 0,01 % und 1,0 %, die Antimon oder Zinn bis 0,005 0 % oder Silicium bis 0,010 % enthalten.
b)   Verfahren B ist anwendbar auf Kupfer und Kupferlegierungen mit Silber-Massenanteilen zwischen 0,01 % und 2,0 %, die Antimon oder Zinn über 0,005 % und Silicium über 0,010 % enthalten.

Cuivre et alliages de cuivre - Dosage de l'argent - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)

La présente Norme européenne spécifie deux méthodes par spectrométrie d’absorption atomique dans la
flamme (SAAF) pour le dosage de l’argent dans le cuivre et les alliages de cuivre, sous forme de produits non
corroyés, corroyés et moulés.
Ces méthodes s’appliquent aux produits en cuivre et en alliages de cuivre ayant des teneurs en argent
comprises entre 0,01 % et 2,0 %.
- La méthode A s’applique aux cuivres et alliages de cuivre ayant des teneurs en argent comprises entre
0,01 % et 1,0 %, et contenant de l’antimoine ou de l’étain dans des proportions inférieures ou égales à
0,005 0 %, ou contenant du silicium dans des proportions inférieures ou égales à 0,010 %.
- La méthode B s’applique aux cuivres et alliages de cuivre ayant des teneurs en argent comprises entre
0,01 % et 2,0 %, et contenant de l’antimoine ou de l’étain dans des proportions supérieures à 0,005 %, et
contenant du silicium dans des proportions supérieures à 0,010 %.

Baker in bakrove zlitine - Določevanje srebra - Metoda z uporabo spektrometrije s plamensko atomsko absorpcijo (FAAS)

Ta evropski standard določa metodi z uporabo spektrometrije s plamensko atomsko absorpcijo (FAAS) za določevanje srebra v bakru in bakrovih zlitinah v obliki negnetenih, gnetenih in ulitih polizdelkov. Metoda velja za polizdelke z masnim deležem srebra med 0,01 % in 2,0 %.
a) Metoda A se uporablja za baker in bakrove zlitine, ki imajo masni delež srebra med 0,01 in 1,0 % ter vsebujejo antimon ali kositer, ki ne presega 0.0050 %, ali silicij, ki ne presega 0,010 %.
b) Metoda B se uporablja za baker in bakrove zlitine, ki imajo masni delež srebra med 0,01 in 2,0 % ter vsebujejo antimon ali kositer, ki presega 0,0050 %, in silicij, ki presega 0,010 %.

General Information

Status
Published
Public Enquiry End Date
04-Jun-2009
Publication Date
13-Sep-2010
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Sep-2010
Due Date
06-Nov-2010
Completion Date
14-Sep-2010

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kupfer und Kupferlegierungen - Bestimmung des Silbergehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)Cuivre et alliages de cuivre - Dosage de l'argent - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)Copper and copper alloys - Determination of silver content - Flame atomic absorption spectrometric method (FAAS)77.120.30Baker in bakrove zlitineCopper and copper alloys77.040.30Kemijska analiza kovinChemical analysis of metalsICS:Ta slovenski standard je istoveten z:EN 15915:2010SIST EN 15915:2010en,de01-oktober-2010SIST EN 15915:2010SLOVENSKI
STANDARD



SIST EN 15915:2010



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15915
July 2010 ICS 77.040.30; 77.120.30 English Version
Copper and copper alloys - Determination of silver content - Flame atomic absorption spectrometric method (FAAS)
Cuivre et alliages de cuivre - Détermination de l'argent - Méthode par spectrométrie d'absorption atomique dans la flamme (SAAF)
Kupfer und Kupferlegierungen - Bestimmung des Silbergehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 19 June 2010.
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 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 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15915:2010: ESIST EN 15915:2010



EN 15915:2010 (E) 2 Contents Page Foreword . 31Scope . 42Normative references . 43Principle . 44Reagents . 45Apparatus . 66Sampling . 67Procedure . 67.1Preparation of the test portion solution — Method A . 67.1.1General . 67.1.2Test portion . 67.1.3Test portion solution . 67.2Blank test . 67.3Check test . 67.4Establishment of the calibration curve . 77.4.1Preparation of the calibration solutions . 77.4.2Adjustment of the atomic absorption spectrometer . 87.4.3Spectrometric measurement of the calibration solutions . 87.4.4Calibration curve. 87.5Determination . 87.5.1General . 87.5.2Preliminary spectrometric measurement . 87.5.3Spectrometric measurements . 97.6Preparation of the test portion solution — Method B . 97.6.1General . 97.6.2Test portion . 97.6.3Test portion solution . 97.7Blank test . 97.8Check test . 107.9Establishment of the calibration curve . 107.9.1Preparation of the calibration solutions . 107.9.2Adjustment of the atomic absorption spectrometer . 117.9.3Spectrometric measurement of the calibration solutions . 127.9.4Calibration curve. 127.10Determination . 127.10.1General . 127.10.2Preliminary spectrometric measurement . 127.10.3Spectrometric measurement . 128Expression of results . 128.1Use of the calibration curve . 128.2Use of bracketing method . 139Precision . 1310Test report . 15Bibliography . 16
SIST EN 15915:2010



EN 15915:2010 (E) 3 Foreword This document (EN 15915:2010) 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 January 2011, and conflicting national standards shall be withdrawn at the latest by January 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 "Methods of analysis" to prepare the following document: EN 15915, Copper and copper alloys — Determination of silver content — Flame atomic absorption spectrometric method (FAAS). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. SIST EN 15915:2010



EN 15915:2010 (E) 4 1 Scope This European Standard specifies two flame atomic absorption spectrometric methods (FAAS) for the determination of the silver content of copper and copper alloys in the form of unwrought, wrought and cast products. The methods are applicable to products having silver mass fractions between 0,01 % and 2,0 %. a) Method A is applicable to copper and copper alloys having silver mass fractions between 0,01 % and 1,0 % and containing antimony or tin not greater than 0,005 0 % or silicon not greater than 0,010 %. b) Method B is applicable to copper and copper alloys having silver mass fractions between 0,01 % and 2,0 % and antimony or tin greater than 0,005 % and silicon greater than 0,010 %. 2 Normative references The following referenced documents are indispensable for the application 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. 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 an appropriate acid solution followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 328,1 nm line emitted by a silver hollow-cathode or electrodeless discharge lamp. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. WARNING — Special care shall be taken to strictly exclude chlorine and chloride ions from all operations, reagents, equipment and the laboratory air. For that reason all reagents indicated hereafter shall be freshly prepared and not stored after analysis. 4.1 Nitric acid, HNO3 (ρ
= 1,40 g/ml). 4.2 Nitric acid solution, 1 + 1. Add 500 ml of nitric acid (4.1) into 500 ml of water. 4.3 Boric acid, H3BO3 (40 g/l solution). 4.4 Hydrofluoric acid, HF, 48 % (ρ
= 1,14 g/ml). WARNING — Hydrofluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. 4.5 Fluoroboric-nitric acid mixture. SIST EN 15915:2010



EN 15915:2010 (E) 5 In a 500 ml one-mark volumetric flask introduce:  150 ml of boric acid (4.3);  20 ml of hydrofluoric acid (4.4);  300 ml of nitric acid solution (4.2). Dilute to the mark with water and mix well. 4.6 Silver stock solution, 1,0 g/l Ag. Weigh (0,5 ± 0,001) g of silver (Ag ≥ 99,99 %) and transfer it into a 250 ml beaker. Add 50 ml of the nitric acid solution (4.2) and cover with a watch glass. Heat gently until the silver is dissolved and then boil or alternatively heat the solution in a boiling water bath until nitrous fumes have been expelled. Cool to room temperature, transfer the solution into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1 mg of Ag. 4.7 Silver standard solution, 0,050 g/l Ag. Transfer 10,0 ml of the silver stock solution (4.6) into a 200 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 0,050 mg of Ag. 4.8 Silver standard solution, 0,020 g/l Ag. Transfer 5,0 ml of the silver stock 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 0,020 mg of Ag. 4.9 Copper base solution A, 10 g/l Cu. For method A. Weigh 5,0 g of pure copper (Ag ≤ 0,000 5 %) and transfer it into a 600 ml beaker. Add 100 ml of the nitric acid solution (4.2) and cover with a watch glass. Heat gently until the copper is completely dissolved, then boil or alternatively heat the solution in a boiling water bath until nitrous fumes have been expelled. 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 well. 4.10 Copper base solution B, 10 g/l Cu. For method B. Weigh 5,0 g of pure copper (Ag ≤ 0,000 5 %) and transfer it into a 600 ml plastic beaker. Add 75 ml of water, 10 ml of hydrofluoric acid (4.4) and by small fractions, 75 ml of nitric acid (4.1) and cover with a watch glass. Heat gently until the copper is completely dissolved, then heat the solution in a boiling water bath until nitrous fumes have been expelled. Cool to room temperature and transfer the solution quantitatively into a 500 ml plastic one-mark volumetric flask and add 75 ml of boric acid (4.3). Dilute to the mark with water and mix well. SIST EN 15915:2010



EN 15915:2010 (E) 6 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.2 Silver hollow-cathode or electrodeless discharge 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 — Method A 7.1.1 General Method A is applicable to products having silver mass fractions between 0,01 % and 1,0 % and containing antimony or tin not greater than 0,005 0 % or silicon not greater than 0,010 %. 7.1.2 Test portion Weigh (0,5 ± 0,001) g of the test sample. 7.1.3 Test portion solution 7.1.3.1 General Transfer the test portion (7.1.2) into a 200 ml conical flask and add 20 ml of the nitric acid solution (4.2). Warm gently until dissolution is complete, then boil or alternatively heat the solution in a boiling water bath until nitrous fumes have been expelled. Cool to room temperature. 7.1.3.2 Silver mass fractions below 0,2 % Transfer the dissolved test portion (7.1.3.1) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.3.3 Silver mass fractions between 0,1 % and 1,0 % Transfer the dissolved test portion (7.1.3.1) into a 500 ml one-mark volumetric flask. 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 (7.1.2). 7.3 Check test Make a prelimi
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