DIN EN 15916-2-2010 Copper and copper alloys - Determination of tellurium content - Part 2 Medium tellurium content - Flame atomic absorption spectrometric method (FAAS) German ver.pdf

1、December 2010 Translation by DIN-Sprachendienst.English price group 8No 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).IC

2、S 77.120.30!$ld“1735965www.din.deDDIN EN 15916-2Copper and copper alloys Determination of tellurium content Part 2: Medium tellurium content Flame atomic absorptionspectrometric method (FAAS)English translation of DIN EN 15916-2:2010-12Kupfer und Kupferlegierungen Bestimmung des Tellurgehaltes Teil

3、2: Mittlerer Tellurgehalt Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)Englische bersetzung von DIN EN 15916-2:2010-12Cuivre et alliages de cuivre Dtermination du tellure Partie 2: Tellure en moyenne teneur Mthode par spectromtrie dabsorption atomiquedans la flamme (SAAF)Traduction anglais

4、e de DIN EN 15916-2:2010-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1211.10 DIN EN 15916-2:2010-12 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 133 “C

5、opper 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 Standards corresponding to the I

6、nternational 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 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principl

7、es 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 result

8、s Part 3: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15916-2 July 2010 ICS 77.040.30; 77.120.30 English Version Copper and copper alloys - Determination of tellurium content - Part 2: Medium tellurium content - Flame

9、 atomic absorption spectrometric method (FAAS) Cuivre et alliages de cuivre - Dtermination du tellure - Partie 2: Tellure en moyenne teneur - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Tellurgehalte - Teil 2: Mittlerer Tellurgehal

10、t - 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 withou

11、t 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 m

12、ade 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, Fi

13、nland, 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES

14、 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 15916-2:2010: EsEN 15916-2:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principl

15、e 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .57.1 Preparation of the test portion solution 57.2 Blank test 57.3 Check test .57.4 Establishment of the calibration curve .67.5 Determination .78 Expression of results 78.1 Use of calibration curve 78.2 Use of bracketing method .89 Precision .

16、810 Test report 9Bibliography . 10DIN EN 15916-2:2010-12 EN 15916-2:2010 (E) 3 Foreword This document (EN 15916-2:2010) 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 natio

17、nal 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 paten

18、t 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 15916-2, Copper and copper alloys Determinatio

19、n of tellurium content Part 2: Medium tellurium content Flame atomic absorption spectrometric method (FAAS). This is one of two parts of the standard for the determination of tellurium content in copper and copper alloys. The other standard is: FprCEN/TS 15916-1, Copper and copper alloys Determinati

20、on of tellurium content Part 1: Low tellurium 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, Cro

21、atia, 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. DIN EN 15916-2:2010-12 EN 1

22、5916-2:2010 (E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the tellurium content of copper and copper alloys in form of castings or unwrought or wrought products. The method is applicable to products having tellurium mass

23、 fractions between 0,20 % and 1,00 %. 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 amendment

24、s) 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

25、Principle Dissolution of a test portion in nitric acid followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 214,3 nm line emitted by a tellurium hollow-cathode lamp. 4 Reagents During the analysis, use

26、 only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Nitric acid, HNO3( = 1,40 g/ml). 4.2 Hydrochloric acid, HCl ( = 1,19 g/ml). 4.3 Nitric acid solution, 2 + 1. Add 200 ml of nitric acid (4.1) to 100 ml of water. 4.4 Hydrochloric acid solution, H

27、Cl (2 mol/l). In a 1 000 ml one-mark volumetric flask containing about 500 ml of water, add 165 ml of hydrochloric acid (4.2). Dilute to the mark with water and mix well. 4.5 Tellurium stock solution, 1 g/l Te. Weigh (0,5 0,001) g of tellurium (Te 99,9 %) and transfer it into a 250 ml beaker. Add 10

28、 ml of nitric acid solution (4.3) and dissolve on a water bath. Evaporate to a wet residue, and then dissolve in 10 ml of hydrochloric acid solution (4.4). Transfer to a 500 ml one-mark volumetric flask, dilute to the mark with hydrochloric acid solution (4.4) and mix well. 1 ml of this solution con

29、tains 1,0 mg of Te. DIN EN 15916-2:2010-12 EN 15916-2:2010 (E) 5 4.6 Copper base solution, 10 g/l Cu. Weigh 10,0 g of pure electrolytic copper (Cu 99,95 %) and transfer it into a 600 ml beaker. Add 200 ml of nitric acid (4.1). Heat gently until copper is dissolved, then heat until all nitrous fumes

30、are expelled. Dilute with hydrochloric acid (4.2). Cool to room temperature. Transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with hydrochloric acid (4.2) and mix well. 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burn

31、er. 5.2 Tellurium hollow-cathode 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 solu

32、tion 7.1.1 Test portion Weigh (0,5 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 nitric acid (4.1). Cover with a watch glass and heat gently until the test portion is completely dissolved and then heat until all nitrous

33、fumes have been expelled. Add 40 ml of hydrochloric acid (4.2) and transfer the test solution quantitatively into a 100 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

34、and using the same quantities of all reagents as used for the determination, but omitting 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 tellurium and of composition similar

35、 to the material to be analysed. Carry out the procedure specified in 7.5. DIN EN 15916-2:2010-12 EN 15916-2:2010 (E) 6 7.4 Establishment of the calibration curve 7.4.1 Preparation of calibration solutions 7.4.1.1 General In all cases, copper, chloride and nitrate concentrations, and acidity in the

36、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 solution. Normally no similar additions are required to compensate for the effect of alloying elements

37、. 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 solution added (4.6) have been calculated to compensate for chemical interaction effects of copper in

38、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 cases the volumes of copper base solution shall be decreased to match the copper content of the tes

39、t sample in solution. The tellurium concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Tellurium mass fraction between 0,20 % and 1,0 % Into each of

40、a series of six 100 ml one-mark volumetric flasks, introduce the volumes of tellurium stock solution (4.5) and copper base solution (4.6) shown in Table 1. Dilute to the mark with water and mix well. Table 1 Calibration for tellurium mass fractions between 0,20 % and 1,0 % Tellurium standard solutio

41、n volume (4.5) Corresponding tellurium mass Corresponding tellurium concentration after final dilution Copper base solution volume (4.6) Corresponding copper mass Corresponding tellurium mass fraction of sample ml mg g/ml ml g % 0a0 0 50 0,5 0 1 1,0 10 50 0,5 0,2 2 2,0 20 50 0,5 0,4 3 3,0 30 50 0,5

42、0,6 4 4,0 40 50 0,5 0,8 5 5,0 50 50 0,5 1,0 aBlank test on reagents for calibration curve. 7.4.2 Adjustment of the atomic absorption spectrometer Fit the tellurium hollow-cathode lamp (5.2) into the atomic absorption spectrometer (5.1), switch on the current and allow it to stabilize. Adjust the wav

43、elength in the region of 214,3 nm to minimum absorbance. Following the manufacturers instructions, fit the correct burner, light the flame and allow the burner temperature to stabilize. The flame shall be set up on oxidising conditions. Taking careful note of the manufacturers instructions regarding

44、 the minimum flow rate of acetylene, aspirate the calibration solution of highest concentration of analyte and adjust the burner configuration and gas flows to obtain maximum absorbance. DIN EN 15916-2:2010-12 EN 15916-2:2010 (E) 7 7.4.3 Spectrometric measurement Aspirate the series of calibration s

45、olutions (7.4.1.2) in succession into the flame and measure the absorbance for each solution. Take care to keep the aspiration rate constant throughout the preparation of the calibration curve. Spray water through the burner after each measurement. NOTE For certain types of apparatus, instead of wat

46、er it is preferable to use a solution containing the attack reagents, in the same concentrations as in the test portion solutions. 7.4.4 Calibration curve Establish the calibration curve using measured absorbances and corresponding analyte amounts. Use appropriate spectrometer software or an off-lin

47、e computer for regression calculations or prepare a graphical representation. 7.5 Determination 7.5.1 General The analyses shall be carried out independently, in duplicate. 7.5.2 Preliminary spectrometric measurement Carry out a preliminary measurement on the test portion solution (7.1.2) following

48、the procedure specified in 7.4.3 at the same time as the spectrometric measurements are carried out on the standard calibration solutions (7.4.1). Estimate the preliminary analyte amount by using the calibration curve according to 7.4.4. NOTE In presence of silver a precipitate of AgCl will occur. F

49、ilter before any spectrometric measurement. 7.5.3 Spectrometric measurements 7.5.3.1 Use of the calibration curve Repeat the measurements and calculate the concentration directly using the calibration curve. 7.5.3.2 Use of bracketing method Carry out a second measurement on the test portion solution (7.1.2) following the procedure specified in 7.4.3, by bracketing between two calibration solutions of composition similar to that of the calibration s