1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58copper ET AAS methodThe European Standard EN 14935:2006 has the status of a British StandardICS 77.
2、120.30Copper and copper alloys Determination of impurities in pure BRITISH STANDARDBS EN14935:2006BS EN 14935:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2006 BSI 2006ISBN 0 580 49062 9Cross-referencesThe British Standards w
3、hich 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 public
4、ation 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 19 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 secretary
6、. 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 Eng
7、lish language version of EN 14935:2006. 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 14935June 2006ICS 77.120.30En
8、glish VersionCopper and copper alloys - Determination of impurities in purecopper - ET AAS methodCuivre et alliages de cuivre - Dosage des impurets dans lecuivre pur - Mthode par spectromtrie dabsorptionatomique lectrothermiqueKupfer und Kupferlegierungen - Bestimmung derVerunreinigungen in reinem K
9、upfer - ElektrothermalesAtomabsorptionsspektrometrie-Verfahren (ET-AAS)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
10、 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 three official versions (English, French, German). A version in any other languag
11、e 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 Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany
12、, 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagem
13、ent 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 14935:2006: EEN 14935:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle5 4 Reagents and materials 5
14、5 Apparatus .9 6 Sampling.9 7 Procedure .10 8 Expression of results 15 9 Precision.16 10 Test report 17 Annex A (informative) Matrix modifiers 18 Bibliography19 EN 14935:2006 (E) 3 Foreword This document (EN 14935:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”,
15、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 December 2006, and conflicting national standards shall be withdrawn at the latest by December 2006. Within
16、 its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 14935:2006, Copper and copper alloys Determination of impurities in pure copper ET AAS method According to the CEN/CENELEC Internal Regulations, the national
17、standards 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, Portu
18、gal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 14935:2006 (E) 4 1 Scope This European Standard specifies two different electrothermal atomization atomic absorption spectrometric meth-ods (ET AAS) for the determination of silver, arsenic, bismuth, cadmium, cobalt,
19、 chromium, iron, manganese, nickel, lead, antimony, selenium, tin, tellurium and zinc in copper (greater than 99,85 %) in the form of unwrought, wrought and cast products. The standard specifies two methods depending on range of impurity concentrations, see Table 1. Table 1 Concentration range in g/
20、g Element Method A Method B from up to andincluding from up to and including Ag 1 30 0,02 1,0 As 1 20 0,04 1,0 Bi 1 5 0,09 1,0 Cd 1 5 0,001 1,0 Co 1 10 0,04 1,0 Cr 1 10 0,04 1,0 Fe 1 10 0,01 1,0 Mn 1 10 0,02 1,0 Ni 1 30 0,01 1,0 Pb 1 10 0,01 1,0 Sb 1 10 0,2 1,0 Se 1 10 0,05 1,0 Sn 1 10 0,02 1,0 Te 1
21、 10 0,05 1,0 Zn 1 10 0,01 1,0 Method B (method of additions) is applicable to products containing impurity elements at concentrations below 1,0 g/g. This method uses special ET AAS equipment fitted with background correction by means of the Zeemann effect. 2 Normative references The following refere
22、nced 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 alloys Selection and preparation of sam
23、ples 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 used in the preparation of this standard,
24、and cited at the appropriate places in the text, are listed in the Bibliography. EN 14935:2006 (E) 5 3 Principle Dissolution of a test portion in nitric acid followed, after suitable dilution, by injection into electrothermal atomization equipment of an atomic absorption spectrometer with a suitable
25、 background corrector. Measurement of the absorption of the following lines emitted by the relevant hollow-cathode or electrodeless discharge lamps, see Table 2. Table 2 Element Wave length nm Ag 328,1 As 193,7 Bi 223,1 Cd 228,8 Co 240,7 Cr 357,9 Fe 248,3 Mn 279,5 Ni 232,0 Pb 283,3 Sb 217,6 Se 196,0
26、 Sn 224,6 Te 214,3 Zn 213,9 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, HCl ( = 1,19 g/ml). 4.3 Nitric acid, HNO3( = 1,40 g/ml). 4.4 Nitric acid solution, 1 +
27、 1 Dilute 500 ml of nitric acid (4.3) in 500 ml of water. 4.5 Nitric acid solution, 1 + 3 Dilute 250 ml of nitric acid (4.3) in 750 ml of water. 4.6 Pure sodium hydroxide, NaOH 1 mol/l. EN 14935:2006 (E) 6 4.7 Sulfuric acid, H2SO40,5 mol/l. 4.8 Hydrofluoric acid, HF ( = 1,13 g/ml). 4.9 Metal stock s
28、olutions, containing 1,000 g/l element. NOTE All these stock solutions have limited life (3 months max.) and should be cold and dark stored. 4.9.1 Silver a) Weigh (1 0,001) g of silver (Ag 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solu-tion (4.4). Heat gently until the
29、silver has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. b) Weigh 1,5748 g of pure silver
30、nitrate (AgNO3) and dissolve it in 100 ml of water previously acidified with 20 ml of nitric acid solution (4.4). Transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.2 Arsenic a) Weigh 0,660 g of pure arsenic trioxide (As2O3
31、) and transfer it into a 250 ml PTFE beaker. Add 50 ml of sodium hydroxide (4.6) and, after complete dissolution, add 150 ml of sulfuric acid (4.7). Transfer the solution quantita-tively into a 500 ml one-mark volumetric flask, dilute to the mark with water and mix well. b) Weigh 4,1650 g of pure so
32、dium arsenate (Na2HAsO4 7H2O) and dissolve it in 200 ml of water. Transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.3 Bismuth Weigh (1 0,001) g of bismuth (Bi 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nit
33、ric acid solution (4.4). Heat gently until the bismuth has been completely dissolved and then bring to the boiling point until the ni-trous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with wate
34、r and mix well. 4.9.4 Cadmium Weigh (1 0,001) g of cadmium (Cd 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solu-tion (4.4). Heat gently until the cadmium has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to
35、room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.5 Cobalt Weigh (1 0,001) g of cobalt (Co 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solution (4.4). Heat gently until the cob
36、alt has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.6 Chromium Weigh (1 0,001) g of
37、chromium (Cr 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solu-tion (4.4). Heat gently until the chromium has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitat
38、ively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.7 Iron Weigh (1 0,001) g of iron (Fe 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solution (4.4). Heat gently until the iron has been completely dissolved and then bring to the
39、 boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. EN 14935:2006 (E) 7 4.9.8 Manganese Weigh (1 0,001) g of manganese (Mn 99,90 %) and transfe
40、r it into a 250 ml beaker. Add 40 ml of nitric acid so-lution (4.4). Heat gently until the manganese has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark v
41、olumetric flask, dilute to the mark with water and mix well. 4.9.9 Nickel Weigh (1 0,001) g of nickel (Ni 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solution (4.4). Heat gently until the nickel has been completely dissolved and then bring to the boiling point until the n
42、itrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.10 Lead Weigh (1 0,001) g of lead (Pb 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid sol
43、ution (4.4). Heat gently until the lead has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well.
44、4.9.11 Antimony Weigh (1 0,001) g of antimony (Sb 99,90 %) and transfer it into a 250 ml beaker. Add 25 ml of hydrochloric acid (4.2) and 50 ml of nitric acid solution (4.4). Heat gently until the antimony has been completely dissolved. Cool to room temperature. Transfer the solution quantitatively
45、into a 1 000 ml of one-mark volumetric flask. Add 100 ml of hydrocloric acid (4.2). Dilute to the mark with water and mix well. 4.9.12 Selenium Weigh (1 0,001) g of selenium (Se 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solu-tion (4.4). Heat gently until the selenium ha
46、s been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.13 Tin Weigh (1 0,001) g of tin (Sn 99
47、,90 %) and transfer it into a 250 ml PTFE beaker. Add 40 ml of nitric acid solu-tion (4.4) and 2 ml of hydrofluoric acid (4.8). After dissolution, transfer it quantitatively into a 1 000 ml plastics one-mark volumetric flask containing 500 ml of water. Dilute to the mark with water and mix well. 4.9
48、.14 Tellurium Weigh (1 0,001) g of tellurium (Te 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solution (4.4). Heat gently until the tellurium has been completely dissolved and then bring to the boiling point until the ni-trous fumes have been expelled. Cool to room tempera
49、ture, transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask, dilute to the mark with water and mix well. 4.9.15 Zinc Weigh (1 0,001) g of zinc (Zn 99,90 %) and transfer it into a 250 ml beaker. Add 40 ml of nitric acid solution (4.4). Heat gently until the zinc has been completely dissolved and then bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transfer the solution quantitatively int
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