EN 14936-2-2006 en Copper and copper alloys - Determination of aluminium content - Part 2 FAAS method《铜和铜合金 测定铝含量 第2部分 FAAS法》.pdf

1、BRITISH STANDARDBS EN14936-2:2006Copper and copper alloys Determination of aluminium content Part 2: FAAS methodThe European Standard EN 14936-2:2006 has the status of a British StandardICS 77.120.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g

2、59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14936-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2006 BSI 2006ISBN 0 580 49064 5National forewordThis British Standa

3、rd is the official English language version of EN 14936-2:2006. The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secr

4、etary.Cross-referencesThe British Standards 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 Catalog

5、ue or of British Standards Online.This publication 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. aid enquirers to understand the

6、text; 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.Summary of pagesThis document comprises a front cover,

7、 an inside front cover, 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 CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14936-2June 2006ICS 77.

8、120.30English VersionCopper and copper alloys - Determination of aluminium content -Part 2: FAAS methodCuivre et alliages de cuivre - Dosage de laluminium -Partie 2 : Mthode par spectromtrie dabsorption atomiquedans la flamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desAluminiumgehaltes - Tei

9、l 2: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

10、 alteration. 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 tr

11、anslationunder 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, Hu

12、ngary, 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:

13、rue 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 14936-2:2006: EEN 14936-2:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Appara

14、tus .5 6 Sampling.5 7 Procedure .5 8 Expression of results 9 9 Precision.10 10 Test report 10 Bibliography11 EN 14936-2:2006 (E) 3 Foreword This document (EN 14936-2:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of which is held by DIN. This Eu

15、ropean 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/

16、TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 14936-2, Copper and copper alloys Determination of aluminium content Part 2: FAAS method This is one of two parts of the standard for the determination of aluminium content in copper and copper alloys. The

17、other part is: EN 14936-1, Copper and copper alloys Determination of aluminium content Part 1: Titrimetric method According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus

18、, 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 United Kingdom. EN 14936-2:2006 (E) 4 1 Scope This part of

19、this European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the aluminium content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having aluminium mass fractions between 0,010 %

20、and 2,5 %. 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 a nitrous oxide/ acetylene flame of an atomic absorptio

23、n spectrometer. Measurement of the absorption of the 309,3 nm line emitted by an aluminium hollow-cathode 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 Hydrochloric acid, HC

24、l ( = 1,19 g/ml). 4.3 Hydrochloric acid solution, 1 + 1 Dilute 500 ml of hydrochloric acid (4.2) in 500 ml of water. 4.4 Nitric acid, HNO3( = 1,40 g/ml). 4.5 Nitric acid solution, 1 + 1 Dilute 500 ml of nitric acid (4.4) in 500 ml of water. 4.6 Aluminium stock solution, 1,000 g/l Al Weigh (1 0,001)

25、g of aluminium (Al 99,9 %) and dissolve it in 50 ml of the hydrochloric acid solution (4.3). Transfer the solution into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 1,000 mg of Al. EN 14936-2:2006 (E) 5 4.7 Aluminium standard soluti

26、on, 0,050 g/l Al Transfer 10,0 ml of the aluminium stock solution (4.6) 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 contains 0,050 mg of Al. 4.8 Aluminium standard solution, 0,200 g/l Al Tr

27、ansfer 20,0 ml of the aluminium stock solution (4.6) 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 Al. 4.9 Copper base solution, 50 g/l Cu Weigh 25,0 g of aluminium-free

28、copper (Cu 99,95 %) and transfer it into an 800 ml beaker. Add 125 ml of hydrochloric acid (4.2) and, cautiously, 250 ml of nitric acid solution (4.5). Cover with a watch glass and heat gently until the copper is completely dissolved, then continue heating to the boiling point. Cool to room temperat

29、ure. 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. 4.10 Copper base solution, 10 g/l Cu Transfer 40,0 ml of the copper base solution (4.9) into a 200 ml one-mark

30、volumetric flask. Add 45 ml of hydrochloric acid (4.2) and 90 ml of nitric acid solution (4.5). Dilute to the mark with water and mix well. 5 Apparatus 5.1 Ordinary laboratory apparatus. 5.2 Atomic absorption spectrometer, fitted with a nitrous oxide/acetylene burner. 5.3 Aluminium hollow-cathode la

31、mp. 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 Preparation of the test portion solution 7.1.1 Test portion Weigh (1 0,

32、001) g of the test sample. EN 14936-2:2006 (E) 6 7.1.2 Aluminium mass fractions between 0,01 % and 0,10 % Transfer the test portion (7.1.1) into a 250 ml beaker. Add 5 ml of the hydrochloric acid (4.2) and 10 ml of the nitric acid solution (4.5). Cover and heat gently until the test portion is compl

33、etely 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 the dissolved test portion into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.3 Aluminium mass fractions

34、 between 0,10 % and 2,5 % Transfer the test portion (7.1.1) into a 250 ml beaker. Add 5 ml of the hydrochloric acid (4.2) and 10 ml of the nitric acid solution (4.5). Cover and heat gently until the test portion is completely dissolved, then continue heating to the boiling point. Cool to room temper

35、ature. Wash the beaker cover and the sides of the beaker with water. Transfer the dissolved test portion into a 500 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 procedure and

36、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 aluminium and of composition similar to t

37、he 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 similar to those

38、 of the test portion solutions. The presence of copper in the 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 elements. If an alloying element is present in

39、the material to be analysed in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The aluminium concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the curve of absorbance as a functi

40、on of concentration is a straight line. 7.4.1.2 Aluminium 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 aluminium standard solution (4.7) and of the copper base solution (4.9) shown in Table 1. Dilute to the mark

41、 with water and mix well. EN 14936-2:2006 (E) 7 Table 1 Calibration for aluminium mass fractions between 0,01 % and 0,10 % Aluminium Corresponding Corresponding Copper Corresponding Corresponding standard aluminium aluminium base copper aluminium solution volume mass concentration solution volume ma

42、ss mass fraction (4.7) after 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 0,010 20 1,000 0,100 aBlank test on reagents for calibration curve. 7.4.1.

43、3 Aluminium mass fractions between 0,10 % and 2,5 % Into each of a series of fifteen 100 ml one-mark volumetric flasks, introduce the volumes of the aluminium standard solution (4.8) and of the copper base solution (4.10) shown in Table 2. Dilute to the mark with water and mix well. Table 2 Calibrat

44、ion for aluminium mass fractions between 0,10 % and 2,5 % Aluminium Corresponding Corresponding Copper Corresponding Corresponding standard aluminium aluminium base copper aluminium solution volume mass concentration solution volume mass mass fraction (4.8) after final dilution (4.10) of sample ml m

45、g mg/ml ml g % 0a0 0 20 0,200 0 1 0,20 0,002 0 20 0,200 0,10 2 0,40 0,004 0 20 0,200 0,20 4 0,80 0,008 0 20 0,200 0,40 6 1,2 0,012 20 0,200 0,60 8 1,6 0,016 20 0,200 0,80 10 2,0 0,020 20 0,200 1,00 12 2,4 0,024 20 0,200 1,20 14 2,8 0,028 20 0,200 1,40 16 3,2 0,032 20 0,200 1,60 18 3,6 0,036 20 0,200

46、 1,80 20 4,0 0,040 20 0,200 2,00 22 4,4 0,044 20 0,200 2,20 24 4,8 0,048 20 0,200 2,40 25 5,0 0,050 20 0,200 2,50 aBlank test on reagents for calibration curve. EN 14936-2:2006 (E) 8 7.4.2 Adjustment of the atomic absorption spectrometer Fit the aluminium hollow-cathode lamp (5.3) into the atomic ab

47、sorption 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 temperature to stabilize. Taking careful note of the manufacturers instructions regarding the minimum flow rate of acetyle

48、ne, aspirate the calibration solution of highest concentration of analyte and adjust the burner configuration and gas flows to obtain maximum absorbance. 7.4.3 Spectrometric measurement of the calibration solutions Aspirate the relevant series of calibration solutions (7.4.1.2 or 7.4.1.3 depending o

49、n the expected aluminium content) in succession into the flame and measure the absorbance for each. Take care to keep the aspiration rate constant 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 a