1、December 2010 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).I
2、CS 77.120.30!$lc“1735964www.din.deDDIN EN 15915Copper and copper alloys Determination of silver content Flame atomic absorption spectrometric method (FAAS)English translation of DIN EN 15915:2010-12Kupfer und Kupferlegierungen Bestimmung des Silbergehaltes Flammenatomabsorptionsspektrometrisches Ver
3、fahren (FAAS)Englische bersetzung von DIN EN 15915:2010-12Cuivre et alliages de cuivre Dtermination de largent Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Traduction anglaise de DIN EN 15915:2010-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language origin
4、al shall be considered authoritative.1811.10 DIN EN 15915:2010-12 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its preparation
5、 was the Normenausschuss Nichteisenmetalle (Nonferrous Metals Standards Committee), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN
6、ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part
7、2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME E
8、UROPENNE EUROPISCHE 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 - Dtermination de largent - Mthode par spectromtrie dabsorption atomique
9、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 cond
10、itions 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 thr
11、ee 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
12、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.
13、EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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: EEN 15915:20
14、10 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents . 45 Apparatus . 66 Sampling . 67 Procedure . 67.1 Preparation of the test portion solution Method A 67.1.1 General 67.1.2 Test portion 67.1.3 Test portion solution . 67.2 Blank test 67.3 Check test . 67.4 Esta
15、blishment of the calibration curve . 77.4.1 Preparation of the calibration solutions 77.4.2 Adjustment of the atomic absorption spectrometer 87.4.3 Spectrometric measurement of the calibration solutions . 87.4.4 Calibration curve 87.5 Determination . 87.5.1 General 87.5.2 Preliminary spectrometric m
16、easurement 87.5.3 Spectrometric measurements 97.6 Preparation of the test portion solution Method B 97.6.1 General 97.6.2 Test portion 97.6.3 Test portion solution . 97.7 Blank test 97.8 Check test . 107.9 Establishment of the calibration curve . 107.9.1 Preparation of the calibration solutions 107.
17、9.2 Adjustment of the atomic absorption spectrometer 117.9.3 Spectrometric measurement of the calibration solutions . 127.9.4 Calibration curve 127.10 Determination . 127.10.1 General 127.10.2 Preliminary spectrometric measurement 127.10.3 Spectrometric measurement 128 Expression of results 128.1 Us
18、e of the calibration curve 128.2 Use of bracketing method . 139 Precision . 1310 Test report 15Bibliography 16DIN EN 15915:2010-12 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 he
19、ld 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
20、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
21、 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 Standar
22、d: 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 Ki
23、ngdom. DIN EN 15915:2010-12 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
24、 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 cop
25、per 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 edit
26、ion 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 alloy
27、s 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.
28、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 stric
29、tly 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( = 1,40 g/ml). 4.2 Nitric acid solution, 1 + 1. Add 500 ml of nitric
30、 acid (4.1) into 500 ml of water. 4.3 Boric acid, H3BO3(40 g/l solution). 4.4 Hydrofluoric acid, HF, 48 % ( = 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. DIN EN 15915:2010-
31、12 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 %) an
32、d 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
33、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 wit
34、h 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
35、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 soluti
36、on 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 (
37、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
38、 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. DIN EN 15915:2010-12 EN 15915:2010 (E) 6 5 Apparatus 5.1 Atomic absorpti
39、on 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 maximu
40、m 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 po
41、rtion 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 boilin
42、g 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
43、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
44、 the determination, but substituting pure copper for the test portion (7.1.2). 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 silver and of composition similar to the material to be analysed.
45、 Carry out the procedure specified in 7.5. DIN EN 15915:2010-12 EN 15915:2010 (E) 7 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibration solutions The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the test solutio
46、n. Normally no similar additions are required to compensate for the effect of alloying elements. If an alloying element is present in the material to be analysed in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The volumes of copper base solutio
47、n A added (4.9) have been calculated to compensate for chemical interaction effects of copper in test solutions of copper or high-copper alloys. Overcompensation may occur if the same volumes are added when the test samples are copper-based alloys where the percentage of copper is lower. In these ca
48、ses the volumes of copper base solution shall be decreased to match the copper content of the test sample in solution. NOTE The range of calibration solutions is appropriate for most current models of equipment of average performance. The range and operating conditions should be selected for optimum
49、 measurements by the particular equipment available. Into each of a series of 100 ml one-mark volumetric flasks, introduce the volumes of silver standard solution (4.7), nitric acid solution (4.2) and copper base solution A (4.9) shown in Tables 1 or 2 depending on the expected silver content. Dilute to the mark with water and mix well. Table 1
