BS EN 14937-2-2006 Copper and copper alloys - Determination of antimony content - FAAS method《铜和铜合金 锑含量的测定 FAAS法》.pdf

1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Part 2: FAAS methodThe European Standard EN 14937-2:2006 has the status of a British StandardICS 77

2、.120.30Copper and copper alloys Determination of antimony content BRITISH STANDARDBS EN14937-2:2006BS EN 14937-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2006 BSI 2006ISBN 0 580 49065 3Cross-referencesThe British Standard

3、s which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This pub

4、lication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pagesThis document comprises a front cover, an inside front cove

5、r, the EN title page, pages 2 to 11 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsA list of organizations represented on this committee can be obtained on request to its secret

6、ary. present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.National forewordThis British Standard is the official

7、English language version of EN 14937-2:2006. The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys, which has the responsibility to: aid enquirers to understand the text;EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14937-2June 2006ICS 77.1

8、20.30English VersionCopper and copper alloys - Determination of antimony content -Part 2: FAAS methodCuivre et alliages de cuivre - Dosage de lantimoine - Partie2 : Mthode par spectromtrie dabsorption atomique dansla flamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desAntimongehaltes - Teil 2:

9、Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)This European Standard was approved by CEN on 15 May 2006.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 alt

10、eration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by transl

11、ationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungar

12、y, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue

13、de Stassart, 36 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14937-2:2006: EEN 14937-2:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus

14、.5 6 Sampling.5 7 Procedure .5 8 Expression of results 8 9 Precision.9 10 Test report 10 Bibliography11 EN 14937-2:2006 (E) 3 Foreword This document (EN 14937-2:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. This Europea

15、n Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2006, and conflicting national standards shall be withdrawn at the latest by December 2006. Within its programme of work, Technical Committee CEN/TC 13

16、3 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 14937-2, Copper and copper alloys Determination of antimony content Part 2: FAAS method This is one of two parts of the standard for the determination of antimony content in copper and copper alloys. The other p

17、art is: EN 14937-1, Copper and copper alloys Determination of antimony content Part 1: Spectrophotometric method 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, Cyprus

18、, Czech Republic, Denmark, Esto-nia, 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. EN 14937-2:2006 (E) 4 1 Scope This part of

19、 this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the de-termination of the antimony content of copper and copper alloys in the form of unwrought, wrought and cast prod-ucts. The method is applicable to products having antimony mass fractions between 0,02 %

20、and 2,0 %. 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, Cop

21、per 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 NOTE Informative references t

22、o documents used in the preparation of this standard, and cited at the appropriate places in the text, are listed in the Bibliography. 3 Principle Dissolution of a test portion in aqua regia followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrom

23、eter. Measurement of the absorption of the 217,6 nm line emitted by an antimony hollow-cathode or electrodeless discharge lamp. 4 Reagents and materials 4.1 General During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.2 Hydro

24、chloric acid, HCl ( = 1,19 g/ml). 4.3 Nitric acid, HNO3( = 1,40 g/ml). 4.4 Nitric acid solution, 1 + 1 Dilute 500 ml of nitric acid (4.3) in 500 ml of water. 4.5 Antimony stock solution, 1,000 g/l Sb a) Weigh (1 0,001) g of antimony (Sb 99,90 %). Transfer it into a 250 ml beaker. Cover with a watch

25、glass. Add 100 ml of hydrochloric acid (4.2) and 50 ml of nitric acid solution (4.4). Heat very gently until the antimony is completely dissolved. Cool to room temperature. Transfer it into a 1 000 ml one-mark volumetric flask, containing 200 ml of hydrochloric acid (4.2), dilute to the mark with wa

26、ter and mix well, or b) Weigh 2,743 0 g of pure potassium antimony(III) oxide tartrate hemihydrate K(SbO)C4H4O6 1/2H2O and dis-solve it in water. Transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of either solution contai

27、ns 1,0 mg of Sb. EN 14937-2:2006 (E) 5 4.6 Antimony standard solution, 0,050 g/l Sb Transfer 10,0 ml of the antimony stock solution (4.5) into a 200 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 contain

28、s 0,050 mg of Sb. 4.7 Antimony standard solution, 0,200 g/l Sb Transfer 20,0 ml of the antimony stock solution (4.5) into a 100 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 0,200 mg of Sb. 4.8

29、 Copper base solution, 50 g/l Cu Weigh 25,0 g of antimony-free copper (Cu 99,5 %) and transfer it into an 800 ml beaker. Add 125 ml of hydro-chloric acid (4.2) and, cautiously, 250 ml of nitric acid solution (4.4). Cover with a watch glass and heat gently until the copper is completely dissolved, th

30、en continue heating to the boiling point. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 50 mg of Cu 4.9 C

31、opper base solution, 10 g/l Cu Transfer 50,0 ml of the copper base solution (4.8) into a 250 ml one-mark volumetric flask. Add 45 ml of hydro-chloric acid (4.2) and 90 ml of nitric acid solution (4.4). Dilute to the mark with water and mix well. 1 ml of this solution contains 10 mg of Cu 5 Apparatus

32、 5.1 Ordinary laboratory apparatus. 5.2 Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.3 Antimony hollow-cathode or electrodeless discharge 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

33、 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. EN 14937-2:2006 (E) 6 7.1.2 Antimony mass fractions between 0,02 % and 0,10 % Transfer the test portion (7.

34、1.1) into a 250 ml beaker. Add 5 ml of the hydrochloric acid (4.2) and 10 ml of the nitric acid solution (4.4). Cover and heat gently until the test portion is completely dissolved, then continue heating to the boiling point. Cool to room temperature. Wash the beaker cover and the sides of the beake

35、r with water. Transfer quantitatively the dissolved test portion into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.3 Antimony mass fractions between 0,10 % and 2,0 % Transfer the test portion (7.1.1) into a 250 ml beaker. Add 5 ml of the hydrochloric acid (4.2)

36、 and 10 ml of the nitric acid solution (4.4). Cover and heat gently until the test portion is completely dissolved, then continue heating to the boiling point. Cool to room temperature. Wash the beaker cover and the sides of the beaker with water. Transfer quantitatively the dissolved test portion i

37、nto a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 20 ml of this solution 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 pro

38、cedure 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 standard material or a synthetic sample containing a known amount of antimony and of composition si

39、milar to the material to be analysed. Carry out the procedure specified in 7.5. 7.4 Establishment 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 simila

40、r to those of the test portion solutions. The presence of copper in the standard calibration solutions compensates for chemical interaction effects of copper in the test portion solution. Normally no similar additions are required to compensate for the effect of alloying ele-ments. If an alloying el

41、ement 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 antimony concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the curve of abs

42、orbance as a function of concentration is a straight line. 7.4.1.2 Antimony mass fractions between 0,02 % and 0,10 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of the antimony standard solution (4.6) and of the copper base solution (4.8) shown in Table 1. D

43、ilute to the mark with water and mix well. EN 14937-2:2006 (E) 7 Table 1 Calibration for antimony mass fractions between 0,02 % and 0,10 % Antimony standard solution volume (4.6) Corresponding antimony mass Correspondingantimony concentration after final dilution Copper base solution volume(4.8) Cor

44、responding copper mass Correspondingantimony mass fraction of sample ml mg mg/ml ml g % 0a0 0 20 1,000 0 4 0,20 0,002 0 20 1,000 0,020 5 0,25 0,002 5 20 1,000 0,025 10 0,50 0,005 0 20 1,000 0,050 15 0,75 0,007 5 20 1,000 0,075 20 1,00 0,010 20 1,000 0,100 aBlank test on reagents for calibration curv

45、e. 7.4.1.3 Antimony mass fractions between 0,10 % and 2,0 % Into each of a series of nine 100 ml one-mark volumetric flasks, introduce the volumes of the antimony standard solution (4.7) and of the copper base solution (4.9) shown in Table 2. Dilute to the mark with water and mix well. Table 2 Calib

46、ration for antimony mass fractions between 0,10 % and 2,0 % Antimony standard solution volume (4.7) Corresponding antimony mass Correspondingantimony concentration after final dilution Copper base solution volume(4.9) Corresponding copper mass Correspondingantimony mass fraction of sample ml mg mg/m

47、l ml g % 0a0 0 20 0,2 0 1 0,20 0,002 0 20 0,2 0,10 2 0,40 0,004 0 20 0,2 0,20 4 0,80 0,008 0 20 0,2 0,40 6 1,2 0,012 20 0,2 0,60 8 1,6 0,016 20 0,2 0,80 10 2,0 0,020 20 0,2 1,00 15 3,0 0,030 20 0,2 1,50 20 4,0 0,040 20 0,2 2,0 aBlank test on reagents for calibration curve. 7.4.2 Adjustment of the at

48、omic absorption spectrometer Fit the antimony hollow-cathode or electrodeless discharge lamp (5.3) into the atomic absorption spectrometer (5.2), switch on the current and allow to stabilize. Following the manufacturers instructions, fit the correct burner, light the flame and allow the burner tempe

49、rature to stabilize. Taking careful note of the manufacturers instructions regarding 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. EN 14937-2:2006 (E) 8 7.4.3 Spectrometric measurement of the calibration solutions Aspirate the relevant series of calibration solutions (see 7.4.1.2 or 7.4.1.3 depending on the expected antimony content) in succession into the flame an