DIN EN 14938-2-2010 Copper and copper alloys - Determination of bismuth content - Part 2 Flame atomic absorption spectrometric method (FAAS) German version EN 14938-2 2010《铜和铜合金 铋含.pdf

1、December 2010 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).IC

2、S 77.120.30!$ld,“1736509www.din.deDDIN EN 14938-2Copper and copper alloys Determination of bismuth content Part 2: Flame atomic absorption spectrometric method (FAAS)English translation of DIN EN 14938-2:2010-12Kupfer und Kupferlegierungen Bestimmung des Bismutgehaltes Teil 2: Flammenatomabsorptions

3、spektrometrisches Verfahren (FAAS)Englische bersetzung von DIN EN 14938-2:2010-12Cuivre et alliages de cuivre Dtermination du bismuth Partie 2: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Traduction anglaise de DIN EN 14938-2:2010-12SupersedesDIN CEN/TS 14938-2:2006-12www.beuth

4、.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1312.10 DIN EN 14938-2:2010-12 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” (Secretaria

5、t: 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 International Standards referred to i

6、n 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 14938-2:2006-12 as follows: a) the status of the Technical Specification/prestandard has been changed to that of a full standard; b) informat

7、ive text has been added to Subclause 7.4.1.1 “General”; c) Clause 9 “Precision” has been completely revised. Previous editions DIN CEN/TS 14938-2: 2006-12 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General

8、 principles 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 a

9、nd results Part 3: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 14938-2 July 2010 ICS 77.120.30 Supersedes CEN/TS 14938-2:2006English Version Copper and copper alloys Determination of bismuth content Part 2: Flame atom

10、ic absorption spectrometric method (FAAS)Cuivre et alliages de cuivre Dtermination du bismuth Partie 2: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen Bestimmung des Bismutgehaltes Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This

11、European Standard was approved by CEN on 12 June 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references c

12、oncerning 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 it

13、s own language and notified to the CEN Management Centre has the same status as theofficial 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

14、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 Brusse

15、ls 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14938-2:2010: EEN 14938-2:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents . 45 Apparatus . 56 Sampling . 57 Procedure . 58 Expressi

16、on of results 89 Precision . 910 Test report 9Bibliography 11DIN EN 14938-2:2010-12 EN 14938-2:2010 (E) 3 Foreword This document (EN 14938-2:2010) 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

17、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

18、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 14938-2:2006. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare

19、the revision of the following document: CEN/TS 14938-2:2006, Copper and copper alloys Determination of bismuth content Part 2: FAAS method In comparison with the first edition of CEN/TS 14938-2:2006, the following significant technical changes were made: Revision from a Technical Specification to a

20、European Standard; Subclause 7.4.1.1 - text added; Clause 9 Precision - completely revised. This is one of two parts of the standard for the determination of bismuth content in copper and copper alloys. The other part is: EN 14938-1, Copper and copper alloys Determination of bismuth content Part 1:

21、Spectrophotometric method Part 1 will be the subject of future work. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following coun-tries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark

22、, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxem-bourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 14938-2:2010-12 EN 14938-2:2010 (E) 4 1 Scope This European

23、Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the bismuth content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having bismuth mass fractions between 0,01 % and 0,25 %. 2 Norma

24、tive references The following referenced documents are indispensable for the application of this European Standard. 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 c

25、opper 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 port

26、ion in a mixture of hydrochloric acid/hydrogen peroxide and nitric acid solutions followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 223,1 nm line emitted by a bismuth hollow-cathode or electrodeless

27、 discharge lamp. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml) 4.2 Nitric acid, HNO3( = 1,40 g/ml) 4.3 Hydrogen peroxide, H2O230 % (mass fraction) solution 4.4 Bismuth

28、 stock solution, 1,0 g/ l Bi Weigh (0,25 0,001) g of bismuth (Bi 99,999 9 %) and transfer it into a 250 ml beaker. Add 50 ml of nitric acid (4.2) and cover with a watch glass. Heat gently until the bismuth is dissolved and then bring to the boiling point until the nitrous fumes have been expelled. C

29、ool to room temperature and transfer the solution quantitatively into a 250 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 1,0 mg of Bi. 4.5 Bismuth standard solution, 0,1 g/l Bi Transfer 25,0 ml of the bismuth stock solution (4.4) into a 250

30、 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,1 mg of Bi. DIN EN 14938-2:2010-12 EN 14938-2:2010 (E) 5 4.6 Copper base solution, 20 g/l Cu Into a 600 ml tall beaker weigh 10,0 g of bismuth-f

31、ree copper (Bi 0,005 %). Add 50 ml of distilled water and, in small portions, 50 ml of nitric acid (4.2). Cover and heat gently until the copper is completely dissolved, then con-tinue heating to the boiling point. Cool to room temperature. Wash the beaker cover and the sides of the beaker with wate

32、r. Transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.2 Bismuth hollow-cathode or electrodeless discharge lamp. 6 Sampling Sampling shall be c

33、arried 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 7.1.1 Test portion Weigh (1 0,001) g of the test sample. 7.1.2 T

34、est portion solution Transfer the test portion (7.1.1) into a 250 ml beaker. Add 10 ml of distilled water, 0,5 ml of nitric acid (4.2), 0,5 ml of hydrogen peroxide (4.3) and 20 ml of hydrochloric acid (4.1). Cover with a watch glass and heat gently until the test portion is completely dissolved, the

35、n continue heating to the boiling point. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test portion 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 simultaneous

36、ly with the determination, following the same procedure 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 containin

37、g a known amount of bismuth and of composition similar to the material to be analysed. Carry out the pro-cedure specified in 7.5. DIN EN 14938-2:2010-12 EN 14938-2:2010 (E) 6 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, coppe

38、r and chloride concentrations in the calibration solutions shall be similar to those of the test por-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 compensa

39、te for the effect of alloying elements. If an al-loying element is present in the material to be analysed in mass fraction 10 %, an appropriate mass of this ele-ment shall be added to the calibration solutions. The volumes of copper base solution added (4.6) have been cal-culated to compensate for c

40、hemical 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 cases the volumes of copper base solution shall be decreas

41、ed to match the copper content of the test sample in solution. The bismuth concentration of the calibration solutions shall be adjusted to suit the sensitivity of the apparatus used, so that the curve of absorbance as a function of concentration is a straight line. NOTE The amount of HNO3in the samp

42、le solutions is different from that in the calibration solutions. This does not effect the measurement. 7.4.1.2 Bismuth mass fractions between 0,01 % and 0,05 % Into each of a series of five 100 ml one-mark volumetric flasks, introduce 20,0 ml of hydrochloric acid (4.1) and the volumes of the bismut

43、h standard solution (4.5) and of the copper base solution (4.6) shown in Table 1. Dilute to the mark with water and mix well. Table 1 Calibration for bismuth mass fractions between 0,01 % and 0,05 % Bismuth Corresponding Corresponding Copper Corresponding Correspondingstandard bismuth bismuth base c

44、opper bismuthsolution volume mass concentration after solution volume mass mass fraction(4.5) final dilution (4.6) of sampleml mg mg/ml ml g % 0a0 0 50 1,000 0 1 0,10 0,001 0 50 1,000 0,010 2 0,20 0,002 0 50 1,000 0,0203 0,30 0,003 0 50 1,000 0,030 5 0,50 0,005 0 50 1,000 0,050aBlank test on reagent

45、s for calibration curve. 7.4.1.3 Bismuth mass fractions between 0,050 % and 0,25 % Into each of a series of five 100 ml one-mark volumetric flasks, introduce 20,0 ml of hydrochloric acid (4.1) and the volumes of the bismuth stock solution (4.4) and of the copper base solution (4.6) shown in Table 2.

46、 Dilute to the mark with water and mix well. DIN EN 14938-2:2010-12 EN 14938-2:2010 (E) 7 Table 2 Calibration for bismuth mass fractions between 0,05 % and 0,25 % Bismuth stock solution volume (4.4) Corresponding bismuth mass Correspondingbismuth concentration after final dilution Copper base soluti

47、on volume(4.6) Corresponding copper mass Correspondingbismuth mass fraction of sample ml mg mg/ml ml g % 0a0 0 50 1,00 0 0,5 0,50 0,005 50 1,00 0,050 1,0 1,00 0,010 50 1,00 0,101,5 1,50 0,015 50 1,00 0,15 2,5 2,50 0,025 50 1,00 0,25aBlank test on reagents for calibration curve. 7.4.2 Adjustment of t

48、he atomic absorption spectrometer Fit the bismuth hollow-cathode or electrodeless discharge 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 223,1 nm to minimum absorbance. Following the manufacturers instructions, fit the correct burner, light the flame and allow the burner temperature to stabilize. Taking careful note of the manufacturers instructi