DIN EN 15022-4-2012 Copper and copper alloys - Determination of tin content - Part 4 Medium tin content - Flame atomic absorption spectrometric method (FAAS) German version EN 1502.pdf

1、January 2012 Translation by DIN-Sprachendienst.English price group 9No 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).ICS

2、 77.120.30!$y+a“1860862www.din.deDDIN EN 15022-4Copper and copper alloys Determination of tin content Part 4: Medium tin content Flame atomic absorption spectrometricmethod (FAAS)English translation of DIN EN 15022-4:2012-01Kupfer und Kupferlegierungen Bestimmung des Zinngehaltes Teil 4: Mittlerer Z

3、inngehalt Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)Englische bersetzung von DIN EN 15022-4:2012-01Cuivre et alliages de cuivre Dtermination de la teneur en tain Partie 4: tain en moyenne teneur Mthode par spectromtrie dabsorption atomiquedans la flamme (SAAF)Traduction anglaise de DIN

4、EN 15022-4:2012-01SupersedesDIN CEN/TS 15022-4:2007-02www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1301.12 DIN EN 15022-4:2012-01 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Tech

5、nical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Nichteisenmetalle (Nonferrous Metals Standards Committee), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle. The DIN Sta

6、ndards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 Amendments This standard differs from DIN CEN/TS 15022-4:2007-02 as follows: a) the standard has been adopted as a European S

7、tandard; b) Clause 9 “Precision” has been completely revised including the results of the precision test. Previous editions DIN CEN/TS 15022-4: 2007-02 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General pr

8、inciples and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 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

9、results Part 3: Intermediate measures of the precision of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15022-4 November 2011 ICS 77.120.30 Supersedes CEN/TS 15022-4:2006English Version Copper and copper alloys - Determination of tin content - Part 4: Medium tin

10、content - Flame atomic absorption spectrometric method (FAAS) Cuivre et alliages de cuivre - Dtermination de la teneur en tain - Partie 4: tain en moyenne teneur - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Zinngehaltes - Teil 4:

11、Mittlerer Zinngehalt - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 24 September 2011. 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

12、national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A

13、 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, Cypr

14、us, 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 CO

15、MIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15022-4:2011: EEN 15022-4:2011 (E) 2 Contents Page Foreword 31 Sc

16、ope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .57.1 Preparation of the test portion solution 57.1.1 Test portion 57.1.2 Test portion solution .57.2 Blank test 57.3 Check test .57.4 Establishment of the calibration curve .67.4.1 Preparation of the calib

17、ration solutions 67.4.2 Adjustment of the atomic absorption spectrometer 67.4.3 Spectrometric measurement of the calibration solutions .77.4.4 Calibration curve77.5 Determination .77.5.1 General 77.5.2 Preliminary spectrometric measurement 77.5.3 Spectrometric measurements 78 Expression of results 8

18、8.1 Use of calibration curve 88.2 Use of bracketing method .89 Precision .810 Test report 9Bibliography . 11DIN EN 15022-4:2012-01 EN 15022-4:2011 (E) 3 Foreword This document (EN 15022-4:2011) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which i

19、s 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 May 2012, and conflicting national standards shall be withdrawn at the latest by May 2012. Attention is drawn to the possibility that

20、 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. This document supersedes CEN/TS 15022-4:2006. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/

21、WG 10 “Methods of analysis“ to prepare the revision of the following document: CEN/TS 15022-4:2006, Copper and copper alloys Determination of tin content Part 4: Medium tin content Flame atomic absorption spectrometry method (FAAS). In comparison with the first edition of CEN/TS 15022-4:2006, the fo

22、llowing significant technical changes were made: a) conversion into a European Standard; b) Clause 9 completely revised and the results of the precision test included. This is one of four parts of the standard for the determination of tin content in copper and copper alloys. The other parts are: prE

23、N 15022-1, Copper and copper alloys Determination of tin content Part 1: Titrimetric method (Part 1 will be the subject of a future work); CEN/TS 15022-2, Copper and copper alloys Determination of tin content Part 2: Spectrophotometric method; EN 15022-3, Copper and copper alloys Determination of ti

24、n content Part 3: Low tin content Flame atomic absorption spectrometry 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 R

25、epublic, 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. DIN EN 15022-4:2012-01 EN 15022-4:2011 (E) 4 1 S

26、cope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the tin content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having medium tin mass fractions between 0,2 % an

27、d 3,0 %. 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, Coppe

28、r 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 te

29、st portion in hydrochloric acid and hydrogen peroxide followed, after suitable dilution, by aspiration into a nitrous oxide/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 286,3 nm line emitted by a tin hollow-cathode lamp. 4 Reagents Use only reagents of r

30、ecognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml). 4.2 Hydrochloric acid solution, 7 + 3. Add 700 ml of hydrochloric acid (4.1) to 300 ml of water. 4.3 Hydrogen peroxide, H2O230 % (mass fraction) solution, free from tin base

31、stabilizers. Hydrogen peroxide may be stabilized by products containing some tin. It is therefore necessary to use exactly the same volume of hydrogen peroxide for the dissolution of the test sample as for the preparation of the corresponding blank test. 4.4 Tin stock solution, 1 g/ l Sn. Weigh (1 0

32、,001) g of tin (Sn 99 %) and transfer it into a 250 ml beaker. Dissolve it in 100 ml hydrochloric acid (4.1) and several drops of hydrogen peroxide (4.3) and cover with a watch glass. Heat gently until the metal is dissolved. Cool to room temperature and transfer the solution quantitatively into a 1

33、 000 ml one-mark volumetric flask. Dilute to the mark with water and mix. 1 ml of this solution contains 1 mg of Sn. DIN EN 15022-4:2012-01 EN 15022-4:2011 (E) 5 4.5 Copper base solution, 20 g/ l Cu. Weigh 10,0 g of electrolytic copper (Cu 99,95 %) into a 600 ml beaker. Add 250 ml of the hydrochlori

34、c acid solution (4.2) and cover with a watch glass. Cool to room temperature and add successively 5 ml hydrogen peroxide portions (4.3) until dissolution is complete, waiting after each addition until all effervescence ceases. Heat to eliminate the excess of hydrogen peroxide. Cool to room temperatu

35、re and transfer this solution quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with a nitrous oxide/acetylene burner. 5.2 Tin hollow-cathode lamp. 6 Sampling Sampling shall be carried out in accordan

36、ce 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

37、Transfer the test portion (7.1.1) into a 250 ml beaker and cover with a watch glass. Add 25 ml of hydrochloric acid solution (4.2), cool and add 5 ml of hydrogen peroxide (4.3). Cool until the violent reaction has ceased and add, if necessary, 2 ml of hydrogen peroxide to continue the dissolution. R

38、epeat this addition several times as necessary to complete the dissolution of the test portion. Heat to eliminate the excess of hydrogen peroxide and cool to room temperature. Transfer the dissolved test portion into a 100 ml one-mark volumetric flask. Add 3,5 ml of hydrochloric acid (4.1). Dilute t

39、o the mark with water and mix. 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 c

40、heck of the apparatus by preparing a solution of a reference material or a synthetic sample containing a known amount of tin and of a composition similar to the material to be analysed. Carry out the procedure specified in 7.5. DIN EN 15022-4:2012-01 EN 15022-4:2011 (E) 6 7.4 Establishment of the ca

41、libration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, copper and chloride 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 chemi

42、cal interaction effects of copper in the test portion 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 analysed in mass fraction 10 %, an appropriate mass of this element shall be added to

43、the calibration solutions. The volumes of copper base solution added (4.5) 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

44、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. The tin concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so

45、that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Tin mass fractions between 0,2 % and 3,0 % Into each of a series of eight 100 ml one-mark volumetric flasks, introduce the volumes of the tin stock solution (4.4), the copper base solution (4.5) and hydrochloric

46、acid (4.1) shown in Table 1. Dilute to the mark with water and mix. Table 1 Calibration for tin mass fractions between 0,2 % and 3,0 % Tin stock solution volume Correspondingtin mass Correspondingtin concentration after final dilution Copper base solution volume Correspondingcopper mass Hydrochloric

47、 acid volume Correspondingtin mass fractionof sample (4.4) (4.5) (4.1) ml mg mg/ml ml g ml %0 a0 0 50 1 3,5 0 2 2 0,02 50 1 3,3 0,20 5 5 0,05 50 1 3,0 0,50 10 10 0,10 50 1 2,5 1,0015 15 0,15 50 1 2,0 1,50 20 20 0,20 50 1 1,5 2,0025 25 0,25 50 1 1,0 2,50 30 30 0,30 50 1 0,5 3,00aBlank test on reagent

48、s for calibration curve. 7.4.2 Adjustment of the atomic absorption spectrometer Fit the tin hollow-cathode lamp (5.2) into the atomic absorption spectrometer (5.1), switch on the current and allow it to stabilize. Adjust the wavelength in the region of 286,3 nm to minimum absorbance. Following the DIN EN 15022-4:2012-01 EN 15022-4:2011 (E) 7 manufacturers instructions, fit the