EN 15915-2010 en Copper and copper alloys - Determination of silver content - Flame atomic absorption spectrometric method (FAAS)《铜及铜合金 银含量的测定 火焰原子光谱吸收法(FAAS)》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15915:2010Copper and copper alloys Determination of silver content Flame atomic absorptionspectrometric method (FAAS)BS EN 15915:2010 BRITISH STANDARDNational forewordThis

2、British Standard is the UK implementation of EN 15915:2010.The UK participation in its preparation was entrusted to TechnicalCommittee NFE/34, Copper and copper alloys.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport t

3、o include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 66410 6ICS 77.040.30; 77.120.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theS

4、tandards Policy and Strategy Committee on 31 August 2010Amendments issued since publicationDate Text affectedBS EN 15915:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15915 July 2010 ICS 77.040.30; 77.120.30 English Version Copper and copper alloys - Determination of silver content - Flam

5、e atomic absorption spectrometric method (FAAS) Cuivre et alliages de cuivre - Dtermination de largent - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Silbergehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This Eur

6、opean 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 con

7、cerning 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

8、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, Lat

9、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Bruss

10、els 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15915:2010: EBS EN 15915:2010EN 15915:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents . 45 Apparatus . 66 Sampling . 67 Procedure

11、. 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 Establishment of the calibration curve . 77.4.1 Preparation of the calibration solutions 77.4.2 Adjustment of the atomic absorption spectr

12、ometer 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 measurement 87.5.3 Spectrometric measurements 97.6 Preparation of the test portion solution Method B 97.6.1 General 97.6.2 Test portion

13、 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 107.9.2 Adjustment of the atomic absorption spectrometer 117.9.3 Spectrometric measurement of the calibration solutions . 127.9.4 Calibrat

14、ion 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 Use of the calibration curve 128.2 Use of bracketing method . 139 Precision . 1310 Test report 15Bibliography 16BS EN 15915:2010EN 15915

15、: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 endors

16、ement, 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 identi

17、fying 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)

18、. 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, Irela

19、nd, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15915:2010EN 15915:2010 (E) 4 1 Scope This European Standard specifies two flame atomic absorption spectrometric methods (FAAS

20、) 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 fracti

21、ons 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,

22、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

23、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

24、 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 ana

25、lysis, 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 h

26、ereafter 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 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 a

27、cid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. 4.5 Fluoroboric-nitric acid mixture. BS EN 15915:2010EN 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 nitri

28、c 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 dissolv

29、ed 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 Silv

30、er 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

31、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 ni

32、tric 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 on

33、e-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 nit

34、ric 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

35、and add 75 ml of boric acid (4.3). Dilute to the mark with water and mix well. BS EN 15915:2010EN 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

36、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 ma

37、ss 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 an

38、d 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 porti

39、on (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 Ca

40、rry 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 preliminary check of the apparatus by preparing a sol

41、ution of a reference material or a synthetic sample containing a known amount of silver and of composition similar to the material to be analysed. Carry out the procedure specified in 7.5. BS EN 15915:2010EN 15915:2010 (E) 7 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibra

42、tion solutions The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the test solution. 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 analys

43、ed in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The volumes of copper base solution A added (4.9) have been calculated to compensate for chemical interaction effects of copper in test solutions of copper or high-copper alloys. Overcompensati

44、on 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 cases 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

45、is appropriate for most current models of equipment of average performance. The range and operating conditions should be selected for optimum measurements by the particular equipment available. Into each of a series of 100 ml one-mark volumetric flasks, introduce the volumes of silver standard solut

46、ion (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 Calibration for silver mass fractions between 0,01 % and 0,2 % Silver standard solution volume (4.7) Correspondi

47、ng silver mass Corresponding silver concentration Nitric acidsolution (4.2) Copper base solution A(4.9) Corresponding copper mass Correspondingsilver mass fraction of sample ml mg mg/mlbml ml g % 0a0 0 10 50 0,5 0 1 0,05 0,000 5 10 50 0,5 0,01 2 0,10 0,001 0 10 50 0,5 0,02 5 0,25 0,002 5 10 50 0,5 0

48、,05 7 0,35 0,003 5 10 50 0,5 0,07 10 0,50 0,005 0 10 50 0,5 0,1015 0,75 0,007 5 10 50 0,5 0,15 20 1,00 0,010 0 10 50 0,5 0,20aBlank test on reagents for calibration curve. bAfter final dilution. BS EN 15915:2010EN 15915:2010 (E) 8 Table 2 Calibration for silver mass fractions between 0,1 % and 1,0 %

49、 Silver standard solution volume (4.7) Corresponding silver mass Correspondingsilver concentration Nitric acid solution (4.2) Copper basesolution A(4.9) Corresponding copper mass Correspondingsilver mass fraction of sample ml mg mg/mlbml ml g % 0a0 0 2 10 0,1 0 2 0,10 0,001 0 2 10 0,1 0,10 5 0,25 0,002 5 2 10 0,1 0,25 7 0,35 0,003 5 2 10 0,1 0,35 10 0,50 0,005 0