DIN EN 15023-3-2010 Copper and copper alloys - Determination of nickel content - Part 3 Flame atomic absorption spectrometric method (FAAS) German version EN 15023-3 2010《铜和铜合金 镍含量.pdf

1、December 2010 Translation by DIN-Sprachendienst.English price group 10No 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!$lUM“1735042www.din.deDDIN EN 15023-3Copper and copper alloys Determination of nickel content Part 3: Flame atomic absorption spectrometric method (FAAS)English translation of DIN EN 15023-3:2010-12Kupfer und Kupferlegierungen Bestimmung des Nickelgehaltes Teil 3: Flammenatomabsorptions

3、spektrometrisches Verfahren (FAAS)Englische bersetzung von DIN EN 15023-3:2010-12Cuivre et alliages de cuivre Dtermination du nickel Partie 3: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Traduction anglaise de DIN EN 15023-3:2010-12SupersedesDIN CEN/TS 15023-3:2007-03www.beuth.

4、deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1512.10 DIN EN 15032-3:2010-12 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

5、: 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 in

6、 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 15023-3:2007-03 as follows: a) the status of the Technical Specification/prestandard has been changed to that of a full standard; b) Clause 4

7、has been renumbered; c) new text has been added in Subclause 7.4.1.1; d) Clause 9 “Precision” has been completely revised. Previous editions DIN CEN/TS 15023-3: 2007-03 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results P

8、art 1: General 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 measure

9、ment methods and results Part 3: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15023-3 July 2010 ICS 77.120.30 Supersedes CEN/TS 15023-3:2006English Version Copper and copper alloys Determination of nickel content Part

10、3: Flame atomic absorption spectrometric method (FAAS)Cuivre et alliages de cuivre Dtermination du nickel Partie 3: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen Bestimmung des Nickelgehaltes Teil 3: Flammenatomabsorptionsspektrometrisches Verfahren

11、(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 EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical

12、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 made by translation under the responsibility of a CEN me

13、mber into its 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

14、, 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 KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B

15、-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15023-3:2010: EEN 15023-3:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .57.

16、1 Preparation of the test portion solution 57.1.1 General 57.1.2 Nickel mass fractions between 0,001 % and 0,012 5 % .67.1.3 Nickel mass fractions between 0,01 % and 0,25 % 67.1.4 Nickel mass fractions between 0,2 % and 6,0 % 67.2 Blank test 67.3 Check test .67.4 Establishment of the calibration cur

17、ve .77.4.1 Preparation of the calibration solutions 77.4.2 Adjustment of the atomic absorption spectrometer 97.4.3 Spectrometric measurement of the calibration solutions .97.4.4 Calibration curve97.5 Determination .97.5.1 General 97.5.2 Preliminary spectrometric measurement 97.5.3 Spectrometric meas

18、urements 98 Expression of results . 108.1 Use of calibration curve . 108.2 Use of bracketing method 109 Precision 1110 Test report . 12Bibliography . 13DIN EN 15032-3:2010-12 EN 15023-3:2010 (E) 3 Foreword This document (EN 15023-3:2010) has been prepared by Technical Committee CEN/TC 133 “Copper an

19、d 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 endorsement, at the latest by January 2011, and conflicting national standards shall be withdrawn at the latest by Janu

20、ary 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 identifying any or all such patent rights. This document supersedes CEN/TS 15023-3:2006. Within its programme of work,

21、Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the revision of the following document: CEN/TS 15023-3:2006, Copper and copper alloys Determination of nickel content Part 3: Flame atomic absorption spectrometry method (FAAS). In comparison with the first ed

22、ition of CEN/TS 15023-3:2006, the following significant technical changes were made: Transformation into a European Standard; In 7.4.1.1, text added; Clause 9, Precision - completely revised. This is one of the three parts of the standard for the determination of nickel content in copper and copper

23、alloys. The other parts are: prEN 15023-1, Copper and copper alloys Determination of nickel content Part 1: Spectrophotometric method; prEN 15023-2, Copper and copper alloys Determination of nickel content Part 2: Titrimetric method. Part 1 and Part 2 will be the subjects of future work. According t

24、o 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, Ireland, Italy, La

25、tvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15032-3:2010-12 EN 15023-3:2010 (E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for t

26、he determination of the nickel content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having a nickel mass fractions between 0,001 % and 6,0 %. 2 Normative references The following referenced documents are indispensable for the a

27、pplication 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 and copper alloys Selection and preparation of samples for chemical analysis Part 1: Samplin

28、g 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 portion in hydrochloric and nitric acid solution followed, after suitable dilution and the

29、addition of lanthanum chloride to mask the effect of interfering ions, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 232,0 nm or the 352,4 nm line emitted by a nickel hollow-cathode lamp. 4 Reagents During the analysis, use only

30、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 Nitric acid solution, 1 + 1. Add 500 ml of nitric acid (4.2) to 500 ml of water. 4.4 Lanthanum (III) chloride solution,

31、100 g/l. Dissolve 50 g of lanthanum (III) chloride heptahydrate (LaCl3 7H2O) in a 400 ml beaker with water and transfer the solution into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. 4.5 Nickel stock solution, 1,0 g/l Ni. Weigh (1 0,001) g of nickel (Ni 99,8 %) and tran

32、sfer it into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.3). Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolution is complete, cool to room temperature and transfer the solution quantitatively into a 1 000

33、ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this solution contains 1,0 mg of Ni. 4.6 Nickel standard solution, 0,1 g/l Ni. DIN EN 15032-3:2010-12 EN 15023-3:2010 (E) 5 Transfer 20,0 ml of nickel stock solution (4.5) into a 200 ml one-mark volumetric flask. Dilute to

34、the mark with water and mix. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,1 mg of Ni. 4.7 Nickel standard solution, 0,01 g/l Ni. Transfer 5,0 ml of nickel stock solution (4.5) into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. Prepare

35、this solution immediately prior to use. 1 ml of this solution contains 0,01 mg of Ni. 4.8 Copper base solution, 40 g/l Cu. Transfer 20,0 g of nickel-free copper (Cu 99,95 %) into an 1 000 ml beaker. Add 100 ml of hydrochloric acid (4.1) and, cautiously, 200 ml of nitric acid solution (4.3). Cover wi

36、th a watch glass and heat gently until the copper has been completely dissolved, then heat up to the boiling point until the 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

37、mix. 4.9 Copper base solution, 2 g/l Cu. Transfer 25,0 ml of copper base solution (4.8) into a 500 ml one-mark volumetric flask. Add 95 ml of hydrochloric acid (4.1) and 190 ml of nitric acid solution (4.3). Dilute to the mark with water and mix. 5 Apparatus 5.1 Atomic absorption spectrometer, fitte

38、d with an air/acetylene burner. 5.2 Nickel 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 Preparatio

39、n of the test portion solution 7.1.1 General Prepare test portion solutions in accordance with 7.1.2, 7.1.3 or 7.1.4 depending on the expected nickel content of the test sample. 4.6 Nickel standard solution, 0,1 g/l Ni. DIN EN 15032-3:2010-12 EN 15023-3:2010 (E) 6 Transfer the test portion into a 25

40、0 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 20 ml of the nitric acid solution (4.3). Cover with a watch glass and heat gently until the test portion is completely dissolved. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test

41、portion quantitatively into a 100 ml one-mark volumetric flask. Add 10 ml of the lanthanum (III) chloride solution (4.4). Dilute to the mark with water and mix. 7.1.3 Nickel mass fractions between 0,01 % and 0,25 % Weigh (1 0,001) g of the test sample. Transfer the test portion into a 250 ml beaker.

42、 Add 5 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.3). Cover with a watch glass and heat gently until the test portion is completely dissolved. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test portion quant

43、itatively into a 100 ml one-mark volumetric flask. Add 10 ml of the lanthanum (III) chloride solution (4.4). Dilute to the mark with water and mix. NOTE The validation exercise of this standard method showed that for nickel mass fractions between 0,2 % and 0,25 % results are better when the determin

44、ation is carried out following 7.1.3. 7.1.4 Nickel mass fractions between 0,2 % and 6,0 % Weigh (1 0,001) g of the test sample. Transfer the test portion into a 250 ml beaker. Add 5 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.3). Cover with a watch glass and heat gently un

45、til the test portion is completely dissolved. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test portion quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 10,0 ml of this solut

46、ion into a 200 ml one-mark volumetric flask. Add 10 ml of hydrochloric acid (4.1), 20 ml of the nitric acid solution (4.3) and 20 ml of the lanthanum (III) chloride solution (4.4). Dilute to the mark with water and mix. 7.2 Blank test Carry out a blank test simultaneously with the determination, fol

47、lowing 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 reference material or a synthetic sample containing a known amount of nickel and o

48、f a composition similar to the material to be analysed. Carry out the procedure specified in 7.5. 7.1.2 Nickel mass fractions between 0,001 % and 0,012 5 % Weigh (2 0,001) g of the test sample. DIN EN 15032-3:2010-12 EN 15023-3:2010 (E) 7 7.4 Establishment of the calibration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, copper, chl