1、BRITISH STANDARDBS EN14939:2006Copper and copper alloys Determination of beryllium content FAAS methodThe European Standard EN 14939:2006 has the status of a British StandardICS 77.120.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g
2、55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14939:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2006 BSI 2006ISBN 0 580 49067 XNational forewordThis British Standard is the offi
3、cial English language version of EN 14939:2006. 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 secretary.Cross-refe
4、rencesThe 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 Catalogue or of British
5、 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 text; present to
6、 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, an inside front
7、 cover, the EN title page, pages 2 to 12, an inside back cover 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 14939June 2006ICS
8、 77.120.30English VersionCopper and copper alloys - Determination of beryllium content -FAAS methodCuivre et alliages de cuivre - Dosage du bryllium -Mthode par spectromtrie dabsorption atomique dans laflamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desBerylliumgehaltes -Flammenatomabsorption
9、sspektrometrisches 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 alteration. Up-to-date l
10、ists 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 translationunder the respon
11、sibility 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, Iceland, Ireland,
12、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 Stassart, 36 B-105
13、0 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14939:2006: EEN 14939:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 Sampling.6 7 Procedu
14、re .6 8 Expression of results 9 9 Precision.10 10 Test report 11 Bibliography12 EN 14939:2006 (E) 3 Foreword This document (EN 14939:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper al-loys”, the secretariat of which is held by DIN. This European Standard shall be given t
15、he 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 requested CEN/TC 133/WG 1
16、0 “Methods of analysis“ to prepare the following standard: EN 14939, Copper and copper alloys Determination of beryllium content FAAS method According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following coun-tries are bound to implement this European Standa
17、rd: Austria, Belgium, Cyprus, 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 14939:2006
18、(E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the beryllium content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having beryllium mass fractions be
19、tween 0,01 % and 3,0 %. 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. IS
20、O 1811-1, 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 NOTE Informative
21、 references to 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 hydrochloric/nitric acid mixture followed, after suitable dilution, by aspiration into a ni-trous oxide/ace
22、tylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 234,8 nm line emitted by a beryllium hollow-cathode lamp. 4 Reagents and materials WARNING Beryllium is an extremely poisonous metal and the inhalation of dust can cause cancer. 4.1 General During the analysis, u
23、se only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.2 Hydrochloric acid, HCl ( = 1,19 g/ml). 4.3 Hydrochloric acid solution, 1 + 1 Dilute 1 000 ml of hydrochloric acid (4.2) in 1 000 ml of water. 4.4 Nitric acid, HNO3( = 1,40 g/ml). 4.5 Nitric ac
24、id solution, 1 + 1 Dilute 1 000 ml of nitric acid (4.4) in 1 000 ml of water. EN 14939:2006 (E) 5 4.6 Beryllium stock solution, 1,000 g/l Be Weigh (1 0,001) g of beryllium (Be 99,9 %) and transfer it into a 250 ml beaker. Add 20 ml of hydrochloric acid (4.2). Cover and heat gently until the berylliu
25、m is completely dissolved. Cool to room temperature, transfer the solu-tion quantitatively 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 Be. 4.7 Beryllium standard solution, 0,010 g/l Be Transfer 5,0 ml of the beryll
26、ium stock solution (4.6) into a 500 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 0,010 mg of Be. 4.8 Beryllium standard solution, 0,005 g/l Be Transfer 50,0 ml of the beryllium standard soluti
27、on (4.7) 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 0,005 mg of Be. 4.9 Copper base solution, 5 g/l Cu Weigh (5 0,001) g of beryllium-free copper (Be 0,001 5 %) and transfer it in
28、to a 400 ml beaker. Add 50 ml of hydrochloric acid solution (4.3) and, cautiously, 50 ml of nitric acid solution (4.5). Heat gently until the copper is dis-solved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitat
29、ively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Cu. 4.10 Copper base solution, 1 g/l Cu Transfer 50,0 ml of the copper base solution (4.9) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mi
30、x well. 1 ml of this solution contains 1 mg of Cu. 5 Apparatus 5.1 Ordinary laboratory apparatus. 5.2 Atomic absorption spectrometer, fitted with a nitrous oxide/acetylene burner. 5.3 Beryllium hollow-cathode lamp. EN 14939:2006 (E) 6 6 Sampling Sampling shall be carried out in accordance with ISO 1
31、811-1 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 0,001) g of the test sample. 7.1.2 Test portion solution Transfer the t
32、est portion (7.1.1) into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.2) and 10 ml of the nitric acid solution (4.5). Cover with a watch glass and heat gently until the test portion is completely dissolved, then heat at a temperature of approximately 90 C until brown fumes have been expelled.
33、Allow to cool. 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 Beryllium mass fractions between 0,01 % and 0,10 % Transfer 10 ml of the test portion solution (
34、7.1.2) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.4 Beryllium mass fractions between 0,10 % and 0,5 % Transfer 2,5 ml of the test portion solution (7.1.2) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.5 Berylliu
35、m mass fractions between 0,4 % and 3,0 % Transfer 10 ml of the test portion solution (7.1.2) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 5 ml of this solution into a 200 ml one-mark volumetric flask. Add 5 ml of the 1 g/l copper solution (4.10), dilu
36、te 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 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
37、 apparatus by preparing a solution of a standard material or a synthetic sample containing a known amount of beryllium and of composition similar to the material to be analysed. Carry out the procedure specified in 7.5. EN 14939:2006 (E) 7 7.4 Establishment of the calibration curve 7.4.1 Preparation
38、 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 standard calibration solutions compensates for chemical interaction
39、effects of copper in the test portion solution. Normally no similar additions are required to compensate for the effects of alloying ele-ments. If any 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 calibratio
40、n solutions. The beryllium concentration of the calibration solutions shall be adjusted to 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 Beryllium mass fractions between 0,01 % and 0,10 % Into each of a series o
41、f six 100 ml one-mark volumetric flasks, introduce the volumes of standard beryllium solu-tions (4.7) and copper base solutions (4.9) as shown in Table 1. Dilute to the mark with water and mix well. Table 1 Calibration for beryllium mass fractions between 0,01 % and 0,10 % Beryllium Corresponding Co
42、rresponding Copper Corresponding Corresponding standard beryllium beryllium base copper beryllium solution volume mass concentration after solution volume mass mass fraction (4.7) final dilution (4.9) of sample ml mg mg/ml ml mg % 0a0 0 20 100 0 1 0,01 0,000 1 20 100 0,010 2,5 0,025 0,000 25 20 100
43、0,025 5 0,05 0,000 50 20 100 0,050 7,5 0,075 0,000 75 20 100 0,075 10 0,10 0,001 0 20 100 0,10 aBlank test on reagents for calibration curve. 7.4.1.3 Beryllium mass fractions between 0,10 % and 0,50 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of standard b
44、eryllium solu-tions (4.7) and copper base solutions (4.10) as shown in Table 2. Dilute to the mark with water and mix well. EN 14939:2006 (E) 8 Table 2 Calibration for beryllium mass fractions between 0,10 % and 0,50 % Beryllium Corresponding Corresponding Copper Corresponding Corresponding standard
45、 beryllium beryllium base copper beryllium solution volume mass concentration after solution volume mass mass fraction (4.7) final dilution (4.10) of sample ml mg mg/ml ml mg % 0a0 0 25 25 0 2,5 0,025 0,000 25 25 25 0,1 5 0,05 0,000 50 25 25 0,2 7,5 0,075 0,000 75 25 25 0,3 10 0,10 0,001 0 25 25 0,4
46、 12,5 0,125 0,001 25 25 25 0,5 aBlank test on reagents for calibration curve. 7.4.1.4 Beryllium mass fractions between 0,4 % and 3,0 % Into each of a series of nine 100 ml one-mark volumetric flasks, introduce the volumes of standard beryllium solu-tions (4.8) and copper base solutions (4.10) as sho
47、wn in Table 3. Dilute to the mark with water and mix well. Table 3 Calibration for beryllium mass fractions between 0,4 % and 3,0 % Beryllium Corresponding Corresponding Copper Corresponding Corresponding standard beryllium beryllium base copper beryllium solution volume mass concentration after sol
48、ution volume mass mass fraction (4.8) final dilution (4.10) of sample ml mg mg/ml ml mg % 0a0 0 5 5 0 2 0,01 0,000 1 5 5 0,40 4 0,020 0,000 2 5 5 0,80 6 0,030 0,000 3 5 5 1,20 8 0,040 0,000 4 5 5 1,60 10 0,050 0,000 5 5 5 2,00 12 0,060 0,000 6 5 5 2,40 14 0,070 0,000 7 5 5 2,80 15 0,075 0,000 75 5 5
49、 3,00 aBlank test on reagents for calibration curve. 7.4.2 Adjustment of the atomic absorption spectrometer Fit the beryllium hollow-cathode 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 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 a
