1、BRITISH STANDARDBS EN 15024-2:2006Copper and copper alloys Determination of zinc content Part 2: Flame atomic absorption spectrometry method (FAAS)The European Standard EN 15024-2:2006 has the status of a British StandardICS 77.120.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g
2、51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 15024-2:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 March 2007 BSI 2007ISBN 978 0 580 50309
3、 2National forewordThis British Standard was published by BSI. It is the UK implementation of EN 15024-2:2006.The UK participation in its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys.A list of organizations represented on NFE/34 can be obtained on request to its
4、secretary.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 cannot confer immunity from legal obligations.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STAN
5、DARDNORME EUROPENNEEUROPISCHE NORMEN 15024-2November 2006ICS 77.120.30English VersionCopper and copper alloys - Determination of zinc content - Part2: Flame atomic absorption spectrometry method (FAAS)Cuivre et alliages de cuivre - Dosage du zinc - Partie 2 :Mthode par spectromtrie dabsorption atomi
6、que dans laflamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desZinkgehaltes - Teil 2:Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)This European Standard was approved by CEN on 18 September 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate
7、the conditions for giving this EuropeanStandard the status of a national standard without any 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
8、three official versions (English, French, German). A version in any other language made by translationunder 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 Au
9、stria, Belgium, Cyprus, 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.EUROPEAN COMMITTEE FOR S
10、TANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: 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 15024-2:2006: EEN 15024-2:2006 (E) 2 Contents Page
11、Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 Sampling.5 7 Procedure .6 8 Expression of results 11 9 Precision.12 10 Test report 13 Bibliography 14 EN 15024-2:2006 (E) 3 Foreword This document (EN 15024-2:2006) has been prepared by Technical Co
12、mmittee 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 May 2007, and conflicting national standards shall be withdr
13、awn at the latest by May 2007. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 15024-2, Copper and copper alloys Determination of zinc content Part 2: Flame atomic absorption spec-trometry method (FAA
14、S) This is one of two parts of the standard for the determination of zinc content in copper and copper alloys. The other part is: prEN 15024-1, Copper and copper alloys Determination of zinc content Part 1: Titrimetric method According to the CEN/CENELEC Internal Regulations, the national standards
15、organizations of the following coun-tries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Esto-nia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Roman
16、ia, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 15024-2:2006 (E) 4 1 Scope This 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, wro
17、ught and cast products. The method is applicable to products having zinc mass fractions between 0,000 5 % and 6,0 %. 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 ref
18、erences, the latest edition of the referenced document (including any amendments) applies. ISO 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 sam
19、ples for chemical analysis Part 2: Sampling of wrought products and castings 3 Principle Dissolution of a test portion in a fluoroboric-nitric acid mixture followed, after suitable dilution, by aspiration into an air/ acetylene flame of an atomic absorption spectrometer. Measurement of the absorptio
20、n of the 213,8 nm line emitted by a zinc 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 Fluoroboric-nitric acid mixture Mix together 300 ml of boric acid, H3BO
21、3, 40 g/l solution, 30 ml of hydrofluoric acid, HF, ( = 1,13 g/l), 500 ml of ni-tric acid, HNO3( = 1,40 g/ml) and 150 ml of water. 4.3 Nitric acid, HNO3( = 1,40 g/ml) 4.4 Nitric acid solution, 1 + 1 Dilute 1 000 ml of nitric acid (4.3) in 1 000 ml of water 4.5 Zinc stock solution, 5 g/l Zn Weigh (2,
22、5 0,001) g of zinc (Zn 99,99 %) and transfer it into a 250 ml tall-form beaker. Add 50 ml of the nitric acid solution (4.4), cover and heat gently until the zinc is completely dissolved. Boil the solution for several minutes to expel the nitrous fumes. Allow it to cool and transfer the solution quan
23、titatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 5 mg of Zn. 4.6 Zinc standard solution, 0,5 g/l Zn Transfer 10 ml of the zinc stock solution (4.5) into a 100 ml one-mark volumetric flask. Dilute to the mark with water and
24、 mix well. EN 15024-2:2006 (E) 5 1 ml of this solution contains 0,5 mg of Zn. 4.7 Zinc standard solution, 0,05 g/l Zn Transfer 10,0 ml of the zinc stock solution (4.5) into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 0,05 mg of Zn.
25、 4.8 Zinc standard solution, 0,01 g/l Zn Transfer 5,0 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 0,01 mg of Zn. 4.9 Zinc standard solution, 0,001 g/l Zn Transfer 5,0 ml of the zinc standar
26、d solution (4.7) 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. 4.10 Copper base solution, 20 g/l Cu Weigh 10,0 g of pure copper containing not more than 0,000 2 % mass fraction zinc into a 1 000 ml polytetrafluore-
27、thylene, polypropylene or low-pressure polyethylene beaker. Add 400 ml of fluoroboric-nitric acid mixture (4.2). Heat gently until the copper is completely dissolved, then boil until the nitrous fumes have been expelled. In the case of polyethylene or polypropylene beakers, use a water bath for heat
28、ing. Allow to cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. 50 ml of this solution contains 1 g of Cu and 40 ml of attack solution (4.2). 4.11 Copper base solution, 2 g/l Cu Transfer, by means of a calibrated pipett
29、e, 10,0 ml of the copper base solution (4.10) into a 100 ml PTFE one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 2 mg of Cu. 5 Apparatus 5.1 Ordinary laboratory apparatus 5.2 Burette, graduated in 0,05 ml or calibrated pipette. 5.3 Atomic absorpt
30、ion spectrometer, fitted with an air/acetylene burner. 5.4 Zinc hollow-cathode 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 millings, with a maximum thickness of 0,5 mm. EN 150
31、24-2:2006 (E) 6 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 test portion (7.1.1) into a 250 ml PTFE, polypropylene or low-pressure polyethylene beaker. Add 40 ml of the attack reagent (4.2)
32、. 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 the nitrous fumes have been expelled. Wash the beaker cover and the sides of the beaker with water and cool. 7.1.3 Zinc mass fractions between 0,000 5 % a
33、nd 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. 7.1.4 Zinc mass fractions between 0,005 % and 0,06 % Transfer the test portion solution (7.1.2) quantitatively into a 200 ml one-mark volumetric fl
34、ask. Dilute to the mark with water and mix well. 7.1.5 Zinc mass fractions between 0,05 % and 0,60 % Transfer the test portion solution (7.1.2) quantitatively into a 200 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 10,0 ml of this solution, by means of a 25 ml b
35、urette or a calibrated pipette, into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 7.1.6 Zinc mass fractions between 0,5 % and 6 % Transfer the test portion solution (7.1.2) quantitatively into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mi
36、x well. Transfer 2,50 ml of this solution, by means of a 25 ml burette or a calibrated pipette, 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 procedure and using the
37、 same quantities of all reagents and of pure copper 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 zinc and of a composition simil
38、ar 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, nitrate, fluoride and borate concentrations, and acidity in the calibration solutions shall be
39、 simi-lar to those 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 effects of alloying elements. EN 15024-2:2006 (E
40、) 7 If any alloying element is present in the material to be analysed in a mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The zinc concentration of the calibration solutions shall be adjusted to suit the sensitivity of the spectrometer used, so t
41、hat the absorbance curve as a function of concentration, is a straight line. 7.4.1.2 Zinc mass fractions between 0,000 5 % and 0,001 % Into each of a series of three 100 ml one-mark volumetric flasks, introduce the volumes of zinc standard solutions (4.9) and copper base solutions (4.10) as shown in
42、 Table 1. Dilute to the mark with water and mix well. Table 1 Calibration for zinc mass fractions between 0,000 5 % and 0,001 % Zinc Corresponding Corresponding Copper Corresponding Corresponding standard zinc zinc base copper Zinc solution volume mass concentration after solution volume mass mass f
43、raction (4.9) final dilution (4.10) of sample ml mg mg/ml ml mg % 0a0 0 50 1 000 0 5 0,005 0,000 05 50 1 000 0,000 5 10 0,010 0,000 1 50 1 000 0,001 aBlank test on reagents for calibration curve. EN 15024-2:2006 (E) 8 7.4.1.3 Zinc mass fractions between 0,001 % and 0,01 % Into each of a series of fo
44、ur 100 ml one-mark volumetric flasks, introduce the volumes of zinc standard solutions (4.8) and copper base solutions (4.10) as shown in Table 2. Dilute to the mark with water and mix well. Table 2 Calibration for zinc mass fractions between 0,001 % and 0,01% Zinc Corresponding Corresponding Copper
45、 Corresponding Corresponding standard zinc zinc base copper Zinc solution volume mass concentration after solution volume mass mass fraction (4.8) final dilution (4.10) of sample ml mg mg/ml ml mg % 0a0 0 50 1 000 0 1 0,01 0,000 1 50 1 000 0,001 5 0,05 0,000 5 50 1 000 0,005 10 0,10 0,001 50 1 000 0
46、,01 aBlank test on reagents for calibration curve. 7.4.1.4 Zinc mass fractions between 0,005 % and 0,06 % Into each of a series of six 200 ml one-mark volumetric flasks, introduce the volumes of zinc standard solutions (4.7) and copper base solutions (4.10) as shown in Table 3. Dilute to the mark wi
47、th water and mix well. Table 3 Calibration for zinc mass fractions between 0,005 % and 0,006 % Zinc Corresponding Corresponding Copper Corresponding Corresponding standard zinc zinc base copper Zinc solution volume mass concentration after solution volume mass mass fraction (4.7) final dilution (4.1
48、0) of sample ml mg mg/ml ml mg % 0a0 0 50 1 000 0 1 0,05 0,000 25 50 1 000 0,005 2 0,1 0,000 5 50 1 000 0,01 4 0,2 0,001 50 1 000 0,02 8 0,4 0,002 50 1 000 0,04 12 0,6 0,003 50 1 000 0,06 aBlank test on reagents for calibration curve. EN 15024-2:2006 (E) 9 7.4.1.5 Zinc mass fractions between 0,05 %
49、and 0,60 % Into each of a series of six 200 ml one-mark volumetric flasks, introduce the volumes of zinc standard solutions (4.6) and copper base solutions (4.10) as shown in Table 4. Dilute to the mark with water and mix well. Transfer 10,0 ml of these solutions into each of six 100 ml one-mark volumetric flasks. Dilute to the mark with water and mix well. Table 4 Calibration for zinc mass fractions between 0,05 % and 0,60% Zinc Corresponding Corresponding Copper Corresponding Corresponding standard zinc zinc base copper Zinc solution volume ma
