DIN EN 15025-2010 Copper and copper alloys - Determination of magnesium content - Flame atomic absorption spectrometric method (FAAS) German version EN 15025 2010《铜和铜合金 镁含量的测定 火焰原子.pdf

1、December 2010 Translation by DIN-Sprachendienst.English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC

2、S 77.120.30!$l“1735959www.din.deDDIN EN 15025Copper and copper alloys Determination of magnesium content Flame atomic absorption spectrometric method (FAAS)English translation of DIN EN 15025:2010-12Kupfer und Kupferlegierungen Bestimmung des Magnesiumgehaltes Flammenatomabsorptionsspektrometrisches

3、 Verfahren (FAAS)Englische bersetzung von DIN EN 15025:2010-12Cuivre et alliages de cuivre Dtermination du magnsium Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Traduction anglaise de DIN EN 15025:2010-12SupersedesDIN CEN/TS 15025:2007-02www.beuth.deDocument comprises pagesIn ca

4、se of doubt, the German-language original shall be considered authoritative.1411.10 DIN EN 15025:2010-12 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible

5、German body involved in its preparation was the Normenausschuss Nichteisenmetalle (Nonferrous Metals Standards Committee), Working Committee NA 066-02-06 AA Analysenverfahren fr NE-Metalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: IS

6、O 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 Amendments This standard differs from DIN CEN/TS 15025:2007-02 as follows: a) the status of the Technical Specification/prestandard has been changed to that of a full standard; b) Clause 4 has been renumbered; c) new text ha

7、s been added in Subclause 7.4.1.1; d) Clause 9 “Precision” has been completely revised. Previous editions DIN CEN/TS 15025: 2007-02 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definit

8、ions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Inte

9、rmediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15025 July 2010 ICS 77.120.30 Supersedes CEN/TS 15025:2006English Version Copper and copper alloys - Determination of magnesium content - Flame atomic absorption spectrometric m

10、ethod (FAAS) Cuivre et alliages de cuivre - Dtermination du magnsium - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Magnesiumgehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by

11、CEN on 19 June 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards

12、 may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to th

13、e CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Mal

14、ta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of expl

15、oitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15025:2010: EEN 15025:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 43 Principle 44 Reagents .45 Apparatus .56 Sampling .57 Procedure .57.1 Preparation of the test portion solution 57.

16、1.1 Test portion 57.1.2 Test portion solution .57.2 Blank test 67.3 Check test .67.4 Preparation of the calibration curve 67.4.1 Preparation of the calibration solutions 67.4.2 Adjustment of the atomic absorption spectrometer 77.4.3 Spectrometric measurement of the calibration solutions .87.4.4 Cali

17、bration curve87.5 Determination .87.5.1 General 87.5.2 Preliminary spectrometric measurement 87.5.3 Spectrometric measurements 88 Expression of results 88.1 Use of calibration curve 88.2 Use of bracketing method .99 Precision .910 Test report . 10Bibliography . 12DIN EN 15025:2010-12 EN 15025:2010 (

18、E) 3 Foreword This document (EN 15025:2010) has been prepared by Technical Committee 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,

19、at the latest by January 2011, and conflicting national standards shall be withdrawn at the latest by January 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying a

20、ny or all such patent rights. This document supersedes CEN/TS 15025:2006. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the revision of the following document: CEN/TS 15025:2006, Copper and copper alloys Determination of magn

21、esium content Flame atomic absorption spectrometry method (FAAS). In comparison with the first edition of CEN/TS 15025:2006, the following significant technical changes were made: Transformation into a European Standard; In 7.4.1.1, text added; Clause 9, Precision - completely revised. According to

22、the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latv

23、ia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15025:2010-12 EN 15025:2010 (E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the det

24、ermination of magnesium content of copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having magnesium mass fractions between 0,001 % and 0,20 %. 2 Normative references The following referenced documents are indispensable for the applic

25、ation 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 samples for chemical analysis Part 1: Sampling of

26、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 3 Principle Dissolution of a test portion in a hydrochloric-nitric acid mixture followed, after suitable dilution, by aspiration i

27、nto an air/acetylene flame of an atomic absorption spectrometer. Determination of the magnesium content by measuring the absorption of the 285,2 nm line emitted by a magnesium hollow-cathode lamp. 4 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled wat

28、er or water of equivalent purity. 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml). 4.2 Nitric acid, HNO3( = 1,40 g/ml). 4.3 Nitric acid solution, 1 + 1. Add 100 ml of nitric acid (4.2) to 100 ml of water. 4.4 Magnesium stock solution, 0,5 g/l Mg. Weigh (0,5 0,001) g of magnesium (Mg 99,9 %) and transfer i

29、t into a 250 ml beaker. Add 20 ml of the nitric acid solution (4.3) in small amounts. Cover with a watch glass and heat gently until the magnesium is completely dissolved. Boil the solution until nitrous fumes have been expelled. Cool to room temperature and transfer the solution quantitatively into

30、 a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 0,5 mg of Mg. 4.5 Magnesium standard solution, 0,01 g/l Mg. Transfer 5 ml of the magnesium stock solution (4.4) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and

31、 mix well. DIN EN 15025:2010-12 EN 15025:2010 (E) 5 Prepare this solution immediately prior to use. 1 ml of this solution contains 0,01 mg of Mg. 4.6 Magnesium standard solution, 0,000 5 g/l Mg. Transfer 5 ml of the magnesium standard solution (4.5) into a 100 ml one-mark volumetric flask. Dilute to

32、 the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,000 5 mg of Mg. 4.7 Lanthanum (III) chloride solution, 200 g/l. Dissolve 100 g of lanthanum chloride heptahydrate (LaCl37H2O) in a 1 000 ml beaker with approximately 400 ml of water. T

33、ransfer the solution into a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 4.8 Copper base solution, 10 g/l Cu. Weigh (10 0,01) g of electrolytic copper and transfer it into a 1 000 ml beaker. Add 100 ml of hydrochloric acid (4.1) and, in small amounts, 100 ml of the n

34、itric acid solution (4.3). Cover with a watch glass and heat gently until the copper is dissolved, then boil until the nitrous fumes have been expelled. Cool to room temperature and transfer the solution into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 5 Apparat

35、us 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner. 5.2 Magnesium 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

36、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 test portion (7.1.1) into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the nitric acid solution (4.3).

37、 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 nitrous fumes have been expelled. Cool to room temperature. Wash the cover and the sides of the beaker with water. Transfer the solution to a 100 ml one-ma

38、rk volumetric flask. Dilute to the mark with water and mix well. DIN EN 15025:2010-12 EN 15025:2010 (E) 6 Select an aliquot portion from the test portion solution according to the expected magnesium mass fraction as indicated in Table 1. Table 1 Aliquot solution Magnesium (mass fraction) Aliquot of

39、the test portion solution (7.1.2) Lanthanum (III) chloride solution volume (4.7) Final volume of diluted solution % ml ml ml0,001 to 0,05 10 10 100 0,05 to 0,2 5 10 100 7.2 Blank test Carry out a blank test simultaneously with the determination, following the same procedure and using the same quanti

40、ties 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 or a synthetic sample containing a known amount of magnesium and of a composition similar to the material to be

41、analysed. Carry out the procedure specified in 7.5. 7.4 Preparation 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 of the test portio

42、n solutions. The presence of copper in the calibration solutions compensates for chemical interaction effects of copper in the test solution. Normally no similar additions are required to compensate for the effect of alloying elements. If an alloying element is present in the material to be analysed

43、 in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The volumes of copper base solution added (4.8) have been calculated to compensate for chemical interaction effects of copper in test solutions of copper or high-copper alloys. Overcompensation m

44、ay occur if the same volumes are added when the test samples are copper-based alloys where the percentage of copper is lower. In these cases the volumes of copper base solution shall be decreased to match the copper content of the test sample in solution. The magnesium concentration of the calibrati

45、on solutions shall be adjusted to suit the sensitivity of the spectrometer used, so that the curve of absorbance as a function of concentration is a straight line. 7.4.1.2 Magnesium mass fractions between 0,001 % and 0,20 % Into each of a series of 100 ml one-mark volumetric flasks, introduce the vo

46、lumes of magnesium standard solution (4.5 or 4.6) and of copper base solution (4.8) shown in Tables 2 or 3, depending on the expected magnesium content, followed by 10 ml of lanthanum (III) chloride solution (4.7). Dilute to the mark with water and mix well. The range of calibration solutions is app

47、ropriate for most current models of equipment of average performance. The range and operating conditions shall be selected for optimum measurements by the particular equipment available. DIN EN 15025:2010-12 EN 15025:2010 (E) 7 Table 2 Calibration for magnesium mass fractions between 0,001 % and 0,0

48、5 % Magnesium standard solution volume Corresponding magnesium mass Correspondingmagnesium concentration after final dilution Copper base solution volumeCorresponding copper mass Correspondingmagnesium mass fractionof sample (4.6) (4.5) (4.8) ml ml mg mg/ml ml g % 0a 0 0 10 0,1 0 2 0,001 0,000 01 10

49、 0,1 0,001 4 0,002 0,000 02 10 0,1 0,002 10 0,005 0,000 05 10 0,1 0,005 20 0,01 0,000 1 10 0,1 0,010 2 0,02 0,000 2 10 0,1 0,020 3 0,03 0,000 3 10 0,1 0,030 4 0,04 0,000 4 10 0,1 0,040 5 0,05 0,000 5 10 0,1 0,050 aBlank test on reagents for calibration curve. Table 3 Calibration for magnesium mass fractions between 0,05 % and 0,20 % Magnesium standard solution volume (4.5) Corresponding magne