BS EN 14942-2-2006 Copper and copper alloys - Determination of arsenic content - FAAS method《铜和铜合金 砷含量的测定 FAAS法》.pdf

1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Part 2: FAAS methodThe European Standard EN 14942-2:2006 has the status of a British StandardICS 77

2、.120.30Copper and copper alloys Determination of arsenic content BRITISH STANDARDBS EN14942-2:2006BS EN 14942-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2006 BSI 2006ISBN 0 580 49079 3Cross-referencesThe British Standards

3、 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 publ

4、ication 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 cover

5、, 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 secreta

6、ry. 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 E

7、nglish language version of EN 14942-2:2006. 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 14942-2June 2006ICS 77.12

8、0.30English VersionCopper and copper alloys - Determination of arsenic content -Part 2: FAAS methodCuivre et alliages de cuivre - Dosage de larsenic - Partie 2: Mthode par spectromtrie dabsorption atomique dans laflamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desArsengehaltes - Teil 2:Flamme

9、natomabsorptionsspektrometrisches 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 alteratio

10、n. 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 translationu

11、nder 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, Hungary, Ice

12、land, 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 de Sta

13、ssart, 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 14942-2:2006: EEN 14942-2:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 S

14、ampling.5 7 Procedure .5 8 Expression of results 9 9 Precision.10 10 Test report 10 Bibliography11 EN 14942-2:2006 (E) 3 Foreword This document (EN 14942-2:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. This European Sta

15、ndard 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 133 req

16、uested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 14942-2, Copper and copper alloys Determination of arsenic content Part 2: FAAS method This is one of two parts of the standard for the determination of arsenic content in copper and copper alloys. The other part is:

17、 prEN 14942-1, Copper and copper alloys Determination of arsenic content Part 1: Spectrometric 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, Czech Rep

18、ublic, 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 14942-2:2006 (E) 4 1 Scope This part of this Europ

19、ean Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the arsenic content of copper and copper alloys in the form of unwrought, wrought and cast prod-ucts. The method is applicable to products having arsenic mass fractions between 0,01 % and 1,5 %. 2 N

20、ormative 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, Copper and copper

21、 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 to documents us

22、ed 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 hydrochloric acid and hydrogen peroxide followed, after suitable dilution, by aspira-tion into an air/acetylene flame of an atomic abs

23、orption spectrometer. Measurement of the absorption of the 193,7 nm line emitted by an arsenic 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 pu

24、rity. 4.2 Hydrochloric acid, HCl ( = 1,19 g/ml). 4.3 Hydrochloric acid solution, 7 + 3 Dilute 700 ml of hydrochloric acid (4.2) in 300 ml of water. 4.4 Hydrogen peroxide, H2O230 % (mass fraction) solution. 4.5 Potassium hydroxide, KOH 20 % solution Weigh 20,0 g of potassium hydroxide pellets and dis

25、solve gently in 50 ml of water. Cool to room temperature and dilute to 100 ml with water. 4.6 Arsenic stock solution, 1,000 g/l As Weigh (1,320 0,001) g of primary standard arsenious oxide (As2O3 purity 99,5 %) and dissolve it in 25 ml of the potassium hydroxide solution (4.5). Transfer the solution

26、 quantitatively into a 1 000 ml one-mark polyethylene volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 1,000 mg of As. EN 14942-2:2006 (E) 5 4.7 Arsenic standard solution, 0,050 g/l As Transfer 10,0 ml of the arsenic stock solution (4.6) into a 200 ml one-

27、mark polyethylene volumetric flask. Dilute to the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,050 mg of As. 4.8 Arsenic standard solution, 0,500 g/l As Transfer 50,0 ml of the arsenic stock solution (4.6) into a 100 ml one-mark polye

28、thylene volumetric flask. Dilute to the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,500 mg of As. 4.9 Copper base solution, 50 g/l Cu Weigh 31,294 g of copper II oxide (CuO 98 %, As 0,000 2 %) or 25 g copper (Cu 99,90 %, As 0,000 2 %

29、) and transfer into a 800 ml beaker. Dissolve it gently with 100 ml of hydrochloric acid solution (4.3) previously cooled. Add slowly hydrogen peroxide (4.4) in small portions while cooling (approximately 50 ml total) until the dis-solution is complete. Cover and heat to the boiling point. Cool to r

30、oom 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, add 250 ml of hydrochloric acid solution (4.3), dilute to the mark with water and mix well. 5 Apparatus 5.1 Ordinary laboratory apparatus. 5.2

31、Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.3 Arsenic 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 form of fine drillings, chips or milling

32、s 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 14942-2:2006 (E) 6 7.1.2 Arsenic mass fractions less than 0,10 % Transfer the test portion (7.1.1) into a 250 ml beaker. Add 15 ml of hydrochlori

33、c acid solution (4.3) and, drop by drop, 10 ml of hydrogen peroxide (4.4). Cool until the violent reaction has ceased. When the test portion is com-pletely dissolved, heat the solution to boil gently for 1 min. Cool to room temperature, transfer the solution quantita-tively into a 100 ml volumetric

34、flask, dilute to the mark with water and mix well. 7.1.3 Arsenic mass fractions between 0,10 % and 1,5 % Transfer the test portion (7.1.1) into a 250 ml beaker. Add 15 ml of hydrochloric acid solution (4.3) and, drop by drop, 10 ml of hydrogen peroxide (4.4). Cool until the violent reaction has ceas

35、ed. When the test portion is com-pletely dissolved, heat the solution to boil gently for 1 min. Cool to room temperature, transfer quantitatively the so-lution into a 200 ml volumetric flask, add 10 ml of the hydrochloric solution (4.3). Dilute to the mark with water and mix well. 7.2 Blank test Car

36、ry 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 preliminary check of the apparatus by preparing a solution of a reference material

37、 or a synthetic sample containing a known amount of arsenic and of composition similar to the material to be analysed. Carry out the pro-cedure 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 and chlorid

38、e concentrations and acidity in the calibration solutions shall be similar 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 requi

39、red to compensate for the effect of alloying ele-ments. 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 solutions. The arsenic concentration of the calibration solutions shall be adjusted to

40、 suit the sensitivity of the apparatus used, so that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Arsenic mass fractions between 0,01 % and 0,10 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of the arsenic standard solu-

41、tion (4.7) and of the copper base solution (4.9) shown in Table 1. Dilute to the mark with water and mix well. EN 14942-2:2006 (E) 7 Table 1 Calibration for arsenic mass fractions between 0,01 % and 0,10 % Arsenic Corresponding Corresponding Copper Corresponding Corresponding standard arsenic arseni

42、c base copper arsenic solution volume mass concentration after solution volume mass mass fraction (4.7) final dilution (4.9) of sample ml mg mg/ml ml g % 0a0 0 20 1,000 0 2 0,10 0,001 0 20 1,000 0,010 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

43、 0,010 20 1,000 0,100 aBlank test on reagents for calibration curve. 7.4.1.3 Arsenic mass fractions between 0,10 % and 1,5 % Into each of a series of eight 100 ml one-mark volumetric flasks, introduce the volumes of the arsenic standard solution (4.8) and of the copper base solution (4.9) shown in T

44、able 2. Dilute to the mark with water and mix well. Table 2 Calibration for arsenic mass fractions between 0,10 % and 1,5 % Arsenic Corresponding Corresponding Copper Corresponding Corresponding standard arsenic arsenic base copper arsenic solution volume mass concentration after solution volume mas

45、s mass fraction (4.8) final dilution (4.9) of sample ml mg mg/ml ml g % 0a0 0 10 0,500 0 1 0,5 0,005 0 10 0,500 0,10 2 1 0,010 10 0,500 0,20 4 2 0,020 10 0,500 0,40 6 3 0,030 10 0,500 0,60 8 4 0,040 10 0,500 0,80 10 5 0,050 10 0,500 1,00 15 7,5 0,075 10 0,500 1,50 aBlank test on reagents for calibra

46、tion curve. EN 14942-2:2006 (E) 8 7.4.2 Adjustment of the atomic absorption spectrometer Fit the arsenic 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

47、 correct burner, light the flame and allow the burner temperature 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

48、to obtain maximum absorbance. 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 arsenic con-tent) in succession into the flame and measure the absorbance for each. Take care to keep the

49、 aspiration rate con-stant throughout the preparation of the calibration curve. Spray water through the burner after each measurement, see note. NOTE For certain types of apparatus, instead of water it is preferable to use a solution containing the attack reagents, in the same concentrations as in the test portion solutions. 7.4.4 Calibration curve Establish the calibration curve using measured absorbances and corresponding analyte amounts. Use appropriate spectrometer software or off-line computer