DIN EN 15703-2-2015 Copper and copper alloys - Determination of manganese content - Part 2 Flame atomic absorption spectrometric method (FAAS) German version EN 15703-2 2014《铜和铜合金 .pdf

1、March 2015 Translation by DIN-Sprachendienst.English price group 10No 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).ICS

2、77.120.30; 77.040.30!%AR#“2304700www.din.deDDIN EN 15703-2Copper and copper alloys Determination of manganese content Part 2: Flame atomic absorption spectrometric method (FAAS);English version EN 15703-2:2014,English translation of DIN EN 15703-2:2015-03Kupfer und Kupferlegierungen Bestimmung des M

3、angangehaltes Teil 2: Flammenatomabsorptionsspektrometrisches Verfahren (FAAS);Englische Fassung EN 15703-2:2014,Englische bersetzung von DIN EN 15703-2:2015-03Cuivre et alliages de cuivre Dtermination de manganse Partie 2: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF);Version a

4、nglaise EN 15703-2:2014,Traduction anglaise de DIN EN 15703-2:2015-03www.beuth.deDocument comprises 16 pagesIn case of doubt, the German-language original shall be considered authoritative.02.15 DIN EN 15703-2:2015-03 2 A comma is used as the decimal marker. National foreword This document (EN 15703

5、-2:2014) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the DIN-Normenausschuss Nichteisenmetalle (DIN Standards Committee Nonferrous Metals), Working Committee NA 066-02-06 AA An

6、alysenverfahren fr NE-Metalle. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5725-3 DIN ISO 5725-3 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and

7、 precision) of measurement methods and results Part 1: General principles and definitions 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

8、-3, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15703-2 December 2014 ICS 77.040.30; 77.120.30 English Version Copper and copper alloys - Dete

9、rmination of manganese content - Part 2: Flame atomic absorption spectrometric method (FAAS)Cuivre et alliages de cuivre - Dtermination de manganse -Partie 2: Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Mangangehaltes - Teil 2: Fla

10、mmenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 8 November 2014. 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 an

11、y alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other langua

12、ge made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC 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,

13、 Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR

14、 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15703-2:2014 EEN 15703-2:2014 (E)

15、2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Principle 4 4 Reagents .4 4.1 Hydrochloric acid, HCl ( = 1,19 g/ml) .4 4.2 Nitric acid, HNO3( = 1,40 g/ml) 4 4.3 Hydrofluoric acid, HF ( = 1,13 g/ml) .4 4.4 Nitric acid solution, 1 + 1 4 4.5 Lanthanum(III) chloride solution, 100 g/l .4

16、4.6 Sulphuric acid, H2SO4( = 1,84 g/ml) .4 4.7 Sulphuric acid solution, 1 + 9 .5 4.8 Manganese stock solution, 1,0 g/l Mn .5 4.9 Manganese standard solution, 0,10 g/l 5 4.10 Manganese standard solution, 0,010 g/l 5 4.11 Copper matrix solution, 20 g/l Cu 5 4.12 Copper matrix solution, 2 g/l Cu 5 5 Ap

17、paratus .5 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner .5 5.2 Manganese hollow-cathode lamp 6 6 Sampling .6 7 Procedure .6 7.1 Preparation of the test portion solution 6 7.2 Blank test 7 7.3 Check test .7 7.4 Establishment of the calibration curve .7 7.5 Determination 10

18、8 Expression of results . 10 8.1 Use of the calibration curve . 10 8.2 Use of the bracketing method . 11 9 Precision 12 10 Test report . 13 Bibliography . 14 DIN EN 15703-2:2015-03 EN 15703-2:2014 (E) 3 Foreword This document (EN 15703-2:2014) has been prepared by Technical Committee CEN/TC 133 “Cop

19、per 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 June 2015 and conflicting national standards shall be withdrawn at the latest by Ju

20、ne 2015. 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 any or all such patent rights. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC

21、 133/WG 10 “Methods of analysis” to prepare the following standard: EN 15703-2, Copper and copper alloys Determination of manganese content Part 2: Flame atomic absorption spectrometric method (FAAS) This is one of two Parts of the standard/Technical Specification for the determination of manganese

22、content in copper and copper alloys. The other Part is: CEN/TS 15703-1, Copper and copper alloys Determination of manganese content Part 1: Spectrophotometric method According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implem

23、ent this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,

24、Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15703-2:2015-03 EN 15703-2:2014 (E) 4 1 Scope This European Standard specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the manganese content of copper and copper alloys in the

25、 form of unwrought, wrought and cast products. The method is applicable to products having manganese mass fractions between 0,001 0 % and 6,0 %. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application.

26、 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 cast unwrought products

27、 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 hydrochloric acid and nitric acid followed, after suitable dilution and the addition of lanthanum chloride t

28、o mask the effect of interfering ions, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 279,5 nm or 403,1 nm line emitted by a manganese hollow-cathode lamp. 4 Reagents During the analysis, use only reagents of recognized analytical

29、 grade and only distilled water 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 Hydrofluoric acid, HF ( = 1,13 g/ml) WARNING Hydrofluoric acid is extremely irritating and corrosive to skin and mucous membranes producing severe skin bur

30、ns which are slow to heal. In the case of contact with skin, wash well with water, apply a topical gel containing 2,5 % (mass fraction) calcium gluconate, and seek immediate medical treatment. 4.4 Nitric acid solution, 1 + 1 Add 500 ml of nitric acid (4.2) to 500 ml of water. 4.5 Lanthanum(III) chlo

31、ride solution, 100 g/l Dissolve 100 g of lanthanum(III) chloride (LaCl3 7H2O) in a 600 ml beaker with water and transfer the solution into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 4.6 Sulphuric acid, H2SO4( = 1,84 g/ml) DIN EN 15703-2:2015-03 EN 15703-2:2014

32、(E) 5 4.7 Sulphuric acid solution, 1 + 9 Add 20 ml of sulphuric acid (4.6) in 180 ml water. 4.8 Manganese stock solution, 1,0 g/l Mn 4.8.1 Cleaning of manganese metal Transfer several grams of electrolytic manganese (purity 99,9 %) into a 250 ml beaker containing about 150 ml of sulphuric acid solut

33、ion (4.7). Stir, then allow the manganese to settle for several minutes. Decant and discard the sulphuric acid solution. Rinse several times with water and finally with acetone. Dry the metal for about 2 min at 100C and cool in a desiccator. 4.8.2 Preparation of stock solution Weigh, (1 0,001) g, of

34、 manganese cleaned as in 4.8.1 and transfer it into a 250 ml beaker. Add 20 ml of hydrochloric acid (4.1) and 20 ml of the nitric acid solution (4.4). Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolution is complete, allow to cool and transfer the solution

35、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 1,0 mg of Mn. 4.9 Manganese standard solution, 0,10 g/l Transfer 20,0 ml of manganese stock solution (4.8) into a 200 ml one-mark volumetric flask. Dilute to the mark

36、with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,10 mg of Mn. 4.10 Manganese standard solution, 0,010 g/l Transfer 5,0 ml of manganese stock solution (4.8) to a 500 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Prep

37、are this solution immediately prior to use. 1 ml of this solution contains 0,010 mg of Mn. 4.11 Copper matrix solution, 20 g/l Cu Transfer (10 0,01) g of manganese-free copper (Cu 99,95 %) into a 600 ml beaker. Add 100 ml of hydrochloric acid (4.1) and, cautiously, 100 ml of the nitric acid solution

38、 (4.4). Cover with a watch glass and heat gently until the copper has been completely dissolved, then heat up to the boiling point until the nitrous fumes have been expelled. Allow to cool and transfer the solution quantitatively into a 500 ml one-mark volumetric flask, dilute to the mark with water

39、 and mix well. 4.12 Copper matrix solution, 2 g/l Cu Transfer 50,0 ml of the copper matrix solution (4.11) into a 500 ml one-mark volumetric flask. Add 90 ml of hydrochloric acid (4.1) and 90 ml of the nitric acid solution (4.4). Dilute to the mark with water and mix well. 5 Apparatus 5.1 Atomic abs

40、orption spectrometer, fitted with an air/acetylene burner DIN EN 15703-2:2015-03 EN 15703-2:2014 (E) 6 5.2 Manganese 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

41、 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 test portion (7.1.1) into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.1) and 10 ml of the ni

42、tric acid solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved. Allow to cool. If undissolved matter remains, indicating the presence of silicon, filter the solution. Place the filter and retained residues in a platinum crucible and ash, taking care

43、 that the filter does not flame. Calcine at about 550 C. Allow to cool and add 5 ml of hydrofluoric acid (4.3) and five drops of nitric acid (4.2). Evaporate to dryness and calcine again for several minutes at about 700 C to completely volatilize the silicon. Cool, and then dissolve the residue with

44、 the least possible volume of nitric acid solution (4.4). Filter, if necessary, and add this filtrate quantitatively to the original filtrate. 7.1.3 Manganese mass fractions between 0,001 % and 0,020 % Transfer the dissolved test portion or the combined filtrates quantitatively into a 100 ml one-mar

45、k volumetric flask. Add 10 ml of the lanthanum(III) chloride solution (4.5), dilute to the mark with water and mix well. NOTE The validation exercise of this method showed that for manganese mass fractions between 0,015 % and 0,020 % results are better when the determination is carried out following

46、 7.1.3. 7.1.4 Manganese mass fractions between 0,020 % and 0,50 % Transfer the dissolved test portion or the combined filtrates quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 5,0 ml of this solution into a 100 ml one-mark volumetric flask

47、. Add 4,5 ml of hydrochloric acid (4.1), 4,5 ml of the nitric acid solution (4.4) and 10 ml of the lanthanum(III) chloride solution (4.5). Dilute to the mark with water and mix well. 7.1.5 Manganese mass fractions between 0,50 % and 2,0 % Transfer the dissolved test portion or the combined filtrates

48、 quantitatively into a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Transfer 10,0 ml of this solution into a 100 ml one-mark volumetric flask. Add 9 ml of hydrochloric acid (4.1), 9 ml of the nitric acid solution (4.4) and 10 ml of the lanthanum(III) chloride solution (4.5). Dilute to the mark with water and mix well. NOTE The validation exercise of this method showed that for manganese mass fractions near 0,5 % results are better when the determination is carried o