EN 15024-2-2018 Copper and copper alloys - Determination of zinc content - Part 2 Flame atomic absorption spectrometric method (FAAS).pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Copper and copper alloys - Determination of zinc contentPart 2: Flame atomic absorption spectrometric method (FAAS)BS EN 150242:2018National forewordThis British Standard is the UK implementation of EN 150242:2018. It s

2、upersedes BS EN 150242:2006, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include

3、 all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 95728 4ICS 77.120.30Compliance with a British Standard cannot confer immunity from legal obligations.This Briti

4、sh Standard was published under the authority of the Standards Policy and Strategy Committee on 30 April 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 150242:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15024-2April 2018ICS 77.120.30 Supersedes E

5、N 150242:2006EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN 150242:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN nation

6、al MembersCopper and copper alloys Determination of zinc content Part 2: Flame atomic absorption spectrometric method (FAAS)Cuivre et alliages de cuivre Dtermination de la teneur en zinc Partie 2 : Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Kupfer und Kupferlegierungen Bestimm

7、ung des Zinkgehaltes Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS)This European Standard was approved by CEN on 18 January 2018.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of

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

9、ersion 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, Cyprus,

10、 Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and Unite

11、d Kingdom.English VersionEN 15024-2:2018 (E)European foreword 31 Scope . 42 Normative references 43 Principle 44 Reagents 45 Apparatus . 55.2 Zinc hollowcathode lamp or a continuum source xenon short arc lamp. 56 Sampling 57 Procedure. 57.1 Preparation of the test portion solution . 57.1.1 Test port

12、ion 57.1.2 Test portion solution 57.1.3 Zinc mass fractions between 0,000 5 % and 0,01 % 67.1.4 Zinc mass fractions between 0,01 % and 0,10 % 67.1.5 Zinc mass fractions between 0,10 % and 1,00 % 67.1.6 Zinc mass fractions between 1,0 % and 5,0 % . 67.2 Blank test . 67.3 Check test . 67.4 Establishme

13、nt of the calibration curve 67.4.1 Preparation of the calibration solutions 67.4.2 Adjustment of the atomic absorption spectrometer. 87.4.3 Spectrometric measurement of the calibration solutions . 97.4.4 Calibration curve . 97.5 Determination . 97.5.1 General 97.5.2 Preliminary spectrometric measure

14、ment 97.5.3 Spectrometric measurements 98 Expression of results .108.1 Use of the calibration curve 108.2 Use of bracketing method . 109 Precision 1010 Test report 11Bibliography .132Contents PageBS EN 150242:2018EN 15024-2:2018 (E)European forewordThis document (EN 150242:2018) has been prepared by

15、 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, at the latest by October 2018, and conflicting national standards

16、 shall be withdrawn at the latest by October 2018.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights.This document supersedes EN 150242:2006.Within its p

17、rogramme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis” to prepare the following standard:EN 150242, Copper and copper alloys Determination of zinc content Part 2: Flame atomic absorption spectrometric method (FAAS)This is one of two parts of the standard fo

18、r the determination of zinc content in copper and copper alloys. The other part is:prEN 150241, Copper and copper alloys Determination of zinc content Part 1: Titrimetric methodIn comparison with EN 15024-2:2006, the following significant changes were made:a) The upper limit of the zinc mass fractio

19、n has been reduced from 6,0 % to 5,0 %;b) Fluoroboricnitric acid mixture has been replaced by a solution of hydrochloric and nitric acids for the dissolution of the test portion;c) The concentrations of the zinc stock solution and the copper base solutions have been modified;d) The use of a continuu

20、m source xenon short arc lamp has been added as an alternative to the use of a zinc hollowcathode lamp;e) The precision data have been updated.According to the CENCENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standa

21、rd: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Sloven

22、ia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.3BS EN 150242:2018EN 15024-2:2018 (E)1 ScopeThis part of this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the zinc content of copper and copper alloys in the form of unwrought

23、, wrought and cast products.The method is applicable to products having zinc mass fractions between 0,000 5 % and 5,0 %.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, onl

24、y the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 18111, Copper and copper alloys Selection and preparation of samples for chemical analysis Part 1: Sampling of cast unwrought productsISO 18112, Copper and copper

25、 alloys Selection and preparation of samples for chemical analysis Part 2: Sampling of wrought products and castings3 PrincipleDissolution of a test portion in hydrochloric and nitric acid solution followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption s

26、pectrometer. Measurement of the absorption of the 213,8 nm line emitted by a zinc hollowcathode lamp or a continuum source xenon short arc lamp.4 ReagentsDuring the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity.4.1 Hydrochloric acid

27、, HCl ( = 1,19 g/ml).4.2 Hydrochloric acid solution, 1 + 1.Add 500 ml of hydrochloric acid (4.1) to 500 ml of water.4.3 Nitric acid, HNO3( = 1,40 g/ml).4.4 Nitric acid solution, 1 + 1.Add 500 ml of nitric acid (4.3) to 500 ml of water.4.5 Zinc stock solution, 1 g/l Zn.Weigh (1 0,001) g of zinc (Zn 9

28、9,99 %) and transfer it into a 250 ml beaker. Add 50 ml of hydrochloric acid solution (4.2). Cover with a watch glass and heat gently to assist dissolution. When dissolution is complete, cool to room temperature and transfer the solution quantitatively into a 1 000 ml onemark volumetric flask, dilut

29、e to the mark with water and mix well.1 ml of this solution contains 1 mg of Zn.4 BS EN 150242:2018EN 15024-2:2018 (E)4.6 Zinc standard solution, 0,01 g/l Zn.Transfer 5,0 ml of the zinc stock solution (4.5) into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well.1 ml of t

30、his solution contains 0,01 mg of Zn.4.7 Zinc standard solution, 0,001 g/l Zn.Transfer 25,0 ml of the zinc standard solution (4.6) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix well.1 ml of this solution contains 0,001 mg of Zn.4.8 Copper base solution, 50 g/l Cu.Tran

31、sfer 50,0 g of zinc-free copper (Cu 99,99 %) into a 2 000 ml beaker. Add 500 ml of hydrochloric acid (4.1) and, by small fractions, 250 ml of nitric acid (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 nitrou

32、s fumes have been expelled. 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 well.4.9 Copper base solution, 2 g/l CuTransfer 10,0 ml of copper base solution (4.8) into a 250 ml one-mark volumetric flask

33、. Dilute to the mark with water and mix well.5 Apparatus5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner.5.2 Zinc hollow-cathode lamp or a continuum source xenon short arc lamp.6 SamplingSampling shall be carried out in accordance with ISO 18111 or ISO 18112, as appropriate.Te

34、st samples shall be in the form of fine drillings, chips or millings, with a maximum thickness of 0,5 mm.7 Procedure7.1 Preparation of the test portion solution7.1.1 Test portionWeigh (1 0,001) g of the test sample.7.1.2 Test portion solutionTransfer the test portion (7.1.1) into a 250 ml beaker. Ad

35、d 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, and wash the beaker cover

36、and the sides of the beaker with water.5BS EN 150242:2018EN 15024-2:2018 (E)7.1.3 Zinc mass fractions between 0,000 5 % and 0,01 %Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well.NOTE The validation interlab

37、oratory test of this method showed that for zinc mass fractions near 0,01 % results are better when the determination is carried out following 7.1.3.7.1.4 Zinc mass fractions between 0,01 % and 0,10 %Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. D

38、ilute to the mark with water and mix well.Transfer 10,0 ml of this solution, into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well.NOTE The validation interlaboratory test of this method showed that for zinc mass fractions near 0,1 % results are better when the determin

39、ation is carried out following 7.1.4.7.1.5 Zinc mass fractions between 0,10 % and 1,00 %Transfer the test portion solution (7.1.2) quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well.Transfer 2,0 ml of this solution, into a 200 ml one-mark volumetric fl

40、ask and add 10,0 ml of hydrochloric acid (4.1). Dilute to the mark with water and mix well.NOTE The validation interlaboratory test of this method showed that for zinc mass fractions near 1,0 % results are better when the determination is carried out following 7.1.5.7.1.6 Zinc mass fractions between

41、 1,0 % and 5,0 %Transfer the test portion solution (7.1.2) quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well.Transfer 2,5 ml of this solution into a 200 ml one-mark volumetric flask and add 10,0 ml of hydrochloric acid (4.1). Dilute to the mark with w

42、ater and mix well.7.2 Blank testCarry 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 testMake a preliminary check of the appa

43、ratus by preparing a solution of a reference material or a synthetic sample containing a known amount of zinc and of a composition similar to the material to be analysed. Carry out the procedure specified in 7.5.7.4 Establishment of the calibration curve7.4.1 Preparation of the calibration solutions

44、7.4.1.1 GeneralIn all cases, copper, chloride and nitrate concentrations, and acidity in the calibration solutions shall be similar to those of the test portion solutions.6 BS EN 150242:2018EN 15024-2:2018 (E)The presence of copper in the calibration solutions compensates for chemical interaction ef

45、fects 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 the calibration so

46、lutions. The volumes of copper base solution added (4.8 or 4.9) have been calculated to compensate for chemical interaction effects of copper in test solutions of copper or highcopper alloys. Overcompensation may occur if the same volumes are added when the test samples are copperbased alloys where

47、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 zinc concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the cur

48、ve of absorbance as a function of concentration is a straight line.7.4.1.2 Zinc mass fractions between 0,000 5 % and 0,01 %Into each of a series of seven 100 ml one-mark volumetric flasks, introduce the volumes of zinc standard solutions (4.6 or 4.7) and copper base solution (4.8) as shown in Table

49、1. Dilute to the mark with water and mix well.Table 1 Calibration for zinc mass fractions between 0,000 5 % and 0,01 %Zinc standard solutions volume (4.6) or (4.7)mlCorresponding zinc massmgCorresponding zinc concentra-tion after final dilutionmg/mlCopper base solution volume (4.8)mlCorresponding copper massmgCorresponding zinc mass frac-tion of sample%0a0 0 20 1 000 05 (4.7) 0,005 0,000 05 20 1 000 0,000 510 (4.7) 0,010 0,000 1 20 1 000 0,00120 (4.7) 0,020 0,000 2 20 1 000 0,0025 (4.6) 0,050 0,000 5 20 1