BS EN 15023-3-2010 Copper and copper alloys n Determination of nickel ncontent nPart 3 Flame atomic absorption nspectrometric method (FAAS)《铜和铜合金 镍含量测定 第3部分 火焰原子吸收光谱法(FAAS)》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15023-3:2010Copper and copper alloys Determination of nickelcontentPart 3: Flame atomic absorptionspectrometric method (FAAS)BS EN 15023-3:2010 BRITISH STANDARDNational for

2、ewordThis British Standard is the UK implementation of EN 15023-3:2010.It supersedes DD CEN/TS 15023-3:2006 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee NFE/34, Copper and copper alloys.A list of organizations represented on this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 beobta

3、ined on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 66409 0ICS 77.120.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This B

4、ritish Standard was published under the authority of theStandards Policy and Strategy Committee on 31 August 2010Amendments issued since publicationDate Text affectedBS EN 15023-3:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15023-3 July 2010 ICS 77.120.30 Supersedes CEN/TS 15023-3:2006E

5、nglish Version Copper and copper alloys - Determination of nickel content - Part 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 - B

6、estimmung des Nickelgehaltes - Teil 3: 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 s

7、tatus of a national standard without 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)

8、. A version in any other language made 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, C

9、zech 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 COMIT E

10、UROPEN DE NORMALISATION EUROPISCHES 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 15023-3:2010: EBS EN 15023-3:2010EN 15023-3:2010 (E) 2 Contents Page F

11、oreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .57.1 Preparation of the test portion solution 57.1.1 General 57.1.2 Nickel mass fractions between 0,001 % and 0,012 5 % .57.1.3 Nickel mass fractions between 0,01 % and 0,25 % 67.1.4 Nickel ma

12、ss fractions between 0,2 % and 6,0 % 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 spectrometer 97.4.3 Spectrometric measurement of the calibration solutions .97.4.4 Calibration

13、 curve97.5 Determination .97.5.1 General 97.5.2 Preliminary spectrometric measurement 97.5.3 Spectrometric measurements 98 Expression of results . 108.1 Use of calibration curve . 108.2 Use of bracketing method 109 Precision 1110 Test report . 12Bibliography . 13BS EN 15023-3:2010EN 15023-3:2010 (E)

14、 3 Foreword This document (EN 15023-3:2010) 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 endorsement,

15、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 identifying a

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

17、nickel content Part 3: Flame atomic absorption spectrometry method (FAAS). In comparison with the first edition 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. Th

18、is is one of the three parts of the standard for the determination of nickel content in copper and copper 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 nic

19、kel content Part 2: Titrimetric method. Part 1 and Part 2 will be the subjects of future work. 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

20、, 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. BS EN 15023-3:2010EN 15023-3:2010 (E) 4

21、 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the 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 0,0

22、01 % and 6,0 %. 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

23、, 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 Principle Dissolution

24、of a test portion in hydrochloric and nitric acid solution followed, after suitable dilution and the 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

25、 the 352,4 nm line emitted by a nickel hollow-cathode 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 Nitric acid solutio

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

27、ater and mix. 4.5 Nickel stock solution, 1,0 g/l Ni. Weigh (1 0,001) g of nickel (Ni 99,8 %) and transfer 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 dis

28、solution is complete, cool to room temperature and transfer the solution quantitatively into a 1 000 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. BS EN 15023-3:2010EN 15023-3:2010 (E) 5 Tra

29、nsfer 20,0 ml of nickel stock solution (4.5) into a 200 ml one-mark volumetric flask. Dilute to 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 solutio

30、n (4.5) into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix. Prepare 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 1

31、00 ml of hydrochloric acid (4.1) and, cautiously, 200 ml of nitric acid solution (4.3). Cover with 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 sol

32、ution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and 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.

33、3). Dilute to the mark with water and mix. 5 Apparatus 5.1 Atomic absorption spectrometer, fitted 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 f

34、ine 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 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. 7.1.2 Nickel mass fraction

35、s between 0,001 % and 0,012 5 % Weigh (2 0,001) g of the test sample. BS EN 15023-3:2010EN 15023-3:2010 (E) 6 Transfer the test portion into a 250 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 port

36、ion 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. Add 10 ml of the lanthanum (III) chloride solution (4.4). Dilute to the mark with water and

37、 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. 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 comple

38、tely 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. Add 10 ml of the lanthanum (III) chloride solution (4.4). Dilute to the mark with water and mix. NOTE Th

39、e validation exercise of this standard method showed that for nickel mass fractions between 0,2 % and 0,25 % results are better when the determination 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 i

40、nto 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 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 dissolve

41、d 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 solution 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)

42、 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, 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

43、 preliminary check of the apparatus by preparing a solution of reference material or a synthetic sample containing a known amount of nickel and of a composition similar to the material to be analysed. Carry out the procedure specified in 7.5. BS EN 15023-3:2010EN 15023-3:2010 (E) 7 7.4 Establishment

44、 of the calibration curve 7.4.1 Preparation of the calibration solutions 7.4.1.1 General In all cases, copper, chloride and nitrate 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 co

45、mpensates 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 analysed in mass fraction 10 %, an appropriate mass of this element shall b

46、e added to the calibration solutions. The volumes of copper base solutions added (4.8 and 4.9) 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 sampl

47、es 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. The nickel concentration of the calibration solutions shall be adjusted to suit the sensitivity of the

48、 spectrometer used, so that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Nickel mass fractions between 0,001 % and 0,012 5 % Into each of a series of seven 100 ml one-mark volumetric flasks, introduce the volumes of nickel standard solution (4.7) and copper base

49、 solution (4.8) shown in Table 1. Add 10 ml of lanthanum (III) chloride solution (4.4). Dilute to the mark with water and mix. Table 1 Calibration for nickel mass fractions between 0,001 % and 0,012 5 % Nickel Corresponding Corresponding Copper Corresponding Correspondingstandard nickel nickel base copper nickelsolution volume mass concentration solution volume mass mass fraction(4.7) after final dilution (4.8) of sa