BS EN 15690-2-2009 Copper and copper alloys - Determination of iron content - Flame atomic absorption spectrometric method (FAAS)《铜和铜合金 铁含量的测定 火焰原子吸收光谱法(FAAS)》.pdf

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1、BS EN15690-2:2009ICS 77.040.30; 77.120.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCopper and copperalloys Determinationof iron contentPart 2: Flame atomic absorptionspectrometric method (FAAS)This British Standardwas published under theauthority of the St

2、andardsPolicy and StrategyCommittee on 31 March2009 BSI 2009ISBN 978 0 580 58647 7Amendments/corrigenda issued since publicationDate CommentsBS EN 15690-2:2009National forewordThis British Standard is the UK implementation of EN 15690-2:2009.The UK participation in its preparation was entrusted to T

3、echnicalCommittee NFE/34, Copper and copper alloys.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance wit

4、h a British Standard cannot confer immunityfrom legal obligations.BS EN 15690-2:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15690-2February 2009ICS 77.040.30; 77.120.30English VersionCopper and copper alloys - Determination of iron content - Part2: Flame atomic absorption spectrometric met

5、hod (FAAS)Cuivre et alliages de cuivre - Dosage du fer - Partie 2 :Mthode par spectromtrie dabsorption atomique dans laflamme (SAAF)Kupfer und Kupferlegierungen - Bestimmung desEisengehaltes - Teil 2:Flammenatomabsorptionsspektrometrisches Verfahren(FAAS)This European Standard was approved by CEN on

6、 26 December 2008.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 lists and bibliographical references concerning such nationalstandards may

7、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 translationunder the responsibility of a CEN member into its own language and notified to the CEN M

8、anagement Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, No

9、rway, 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-1050 Brussels 2009 CEN All rights of exploitation in any form a

10、nd by any means reservedworldwide for CEN national Members.Ref. No. EN 15690-2:2009: EBS EN 15690-2:2009EN 15690-2:2009 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Principle 4 4 Reagents and materials 4 5 Apparatus .6 6 Sampling .6 7 Procedure .6 8 Expression of results . 10

11、9 Precision 11 10 Test report . 12 Bibliography . 13 BS EN 15690-2:2009EN 15690-2:2009 (E) 3 Foreword This document (EN 15690-2:2009) 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 sta

12、tus of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2009, and conflicting national standards shall be withdrawn at the latest by August 2009. Attention is drawn to the possibility that some of the elements of this document may be the subj

13、ect 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 133/WG 10 “Methods of analysis“ to prepare the following standard: EN 15690-2, Copper and copper alloys

14、Determination of iron content Part 2: Flame atomic absorption spectrometric method (FAAS) This is one of two Parts of the standard for the determination of iron content in copper and copper alloys. The other Part is: EN 15690-1, Copper and copper alloys Determination of iron content Part 1: Titrimet

15、ric method Part 1 will be the subject of future work. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, Franc

16、e, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15690-2:2009EN 15690-2:2009 (E) 4 1 Scope This Part of this European Standard speci

17、fies a flame atomic absorption spectrometric method (FAAS) for the determination of the iron content of copper and copper alloys in the form of castings or unwrought or wrought products. The method is applicable to products having iron mass fractions between 0,005 % and 5,0 %. 2 Normative references

18、 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. ISO 1811-1, Copper and copper alloys Selection a

19、nd 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 references to documents used in the preparati

20、on 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 a hydrochloric and nitric acid mixture followed, after suitable dilution and the addition of lanthanum chloride to mask the effect of interfering ions, b

21、y aspiration of the test solution into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 248,3 nm or the 372,0 nm line emitted by an iron hollow-cathode lamp. 4 Reagents and materials 4.1 General During the analysis, use only reagents of recognized ana

22、lytical grade and only distilled water or water of equivalent purity. Avoid any contamination with iron during the mechanical preparation steps. 4.2 Hydrochloric acid, HCl ( = 1,19 g/ml) 4.3 Nitric acid, HNO3( = 1,40 g/ml) 4.4 Nitric acid, (1 + 1) Add 500 ml of nitric acid (4.3) into 500 ml of water

23、. 4.5 Hydrofluoric acid, HF ( = 1,13 g/ml) WARNING Hydrofluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. BS EN 15690-2:2009EN 15690-2:2009 (E) 5 4.6 Lanthanum(III) chloride solution, 100 g/l Weigh 100 g of lanthanum(III) chloride (LaCl3 7H

24、2O) in a 600 ml beaker, transfer it into a 1 000 ml one-mark volumetric flask and dissolve it with water. Dilute to the mark with water and mix well. 4.7 Iron stock solution, 0,5 g/l Fe a) Weigh (0,5 0,001) g of high purity iron and transfer it into a 250 ml beaker. Dissolve it in 50 ml of hydrochlo

25、ric acid (4.2), 25 ml water and 2,5 ml nitric acid (4.3). Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolution is complete, allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and m

26、ix well; or b) Weigh (0,715 0,000 1) g of high purity iron(III) oxide (Fe2O3), previously dried and transfer it into a 250 ml beaker. Add 50 ml of hydrochloric acid (4.2). Cover with a watch glass and, if necessary, heat gently to assist dissolution. When dissolution is complete, allow to cool and t

27、ransfer the solution 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 0,5 mg of Fe. 4.8 Iron standard solution, 0,05 g/l Fe Transfer 20,0 ml of iron stock solution (4.7) into a 200 ml one-mark volumetric flask. Add 5

28、 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. 1 ml of this solution contains 0,05 mg of Fe. 4.9 Iron standard solution, 0,01 g/l Fe Transfer 10,0 ml of iron stock solution (4.7) into a 500 ml one-mark volumetric flask. Add 10 ml of hydrochloric acid (4.2), dilute to the

29、 mark with water and mix well. 1 ml of this solution contains 0,01 mg of Fe. 4.10 Copper base solution, 20 g/l Cu Transfer (10 0,01) g of iron-free copper (Cu 99,95 %) after etching into a 600 ml beaker. Add 100 ml of hydrochloric acid (4.2) and, cautiously, 100 ml of nitric acid solution (4.4). Cov

30、er 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 and mix we

31、ll. 1 ml of this solution contains 0,02 g of Cu. 4.11 Copper base solution, 2,0 g/l Cu Transfer quantitatively 25 ml of copper base solution (4.10) into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 1 ml of this solution contains 2,0 mg of Cu. BS EN 15690-2:2009EN 1

32、5690-2:2009 (E) 6 5 Apparatus 5.1 Atomic absorption spectrometer, fitted with an air/acetylene burner 5.2 Iron 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 milli

33、ngs 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 (4.2) and 10 ml of the nitric

34、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 paper and contained salts in a platinum crucible and ash, taking care

35、that the filter does not flame. Calcine at about 550 C. Cool and add 5 ml of hydrofluoric acid (4.5) and five drops of nitric acid (4.3). 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 the least

36、 possible volume of nitric acid solution (4.4). Filter, if necessary, and add this filtrate quantitatively to the original filtrate. 7.1.3 Iron mass fractions between 0,005 % and 0,025 % Transfer the dissolved test portion or the combined filtrates quantitatively into a 100 ml one-mark volumetric fl

37、ask. Add 10 ml of the lanthanum(III) chloride solution (4.6) and 1 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. 7.1.4 Iron mass fractions between 0,025 % and 0,5 % Transfer the dissolved test portion or the combined filtrates quantitatively into a 100 ml one-mark volume

38、tric flask. Dilute to the mark with water and mix well. Transfer 20 ml of this solution into a 100 ml one-mark volumetric flask. Add 10 ml of the lanthanum(III) chloride solution (4.6) and 1 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. 7.1.5 Iron mass fractions between

39、0,5 % and 5 % 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 ml of this solution into a 250 ml one-mark volumetric flask. Add 25 ml of the lanthanum(III) chloride solution (4

40、.6) and 1 ml of hydrochloric acid (4.2), dilute to the mark with water and mix well. BS EN 15690-2:2009EN 15690-2:2009 (E) 7 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 determi

41、nation, by pure copper for the test portion (7.1.1). Correct the result obtained from the determination in accordance with the result of the blank. 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

42、of iron and of composition similar to the material to be analysed. Carry out the procedure 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, salts concentration and the pH-values of the calibration soluti

43、ons shall be similar 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 solution. Normally no similar additions are required to compensate for the effect of alloying elements. If an alloying e

44、lement is present in the material to be analysed in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The volumes of copper base solution added (4.10 and 4.11) have been calculated to compensate for chemical interaction effects of copper in test sol

45、utions of copper or high-copper alloys. Overcompensation may 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

46、 in solution. The iron concentration of the calibration 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. BS EN 15690-2:2009EN 15690-2:2009 (E) 8 7.4.1.2 Calibration for iron mass fractions

47、 between 0,005 % and 0,025 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of iron standard solution (4.9) and of copper base solution (4.10) as shown in Table 1. Introduce also 10 ml of lanthanum(III) chloride solution (4.6). Dilute to the mark with water and

48、 mix well. Table 1 Calibration for iron mass fractions between 0,005 % and 0,025 % Iron standard solution volume (4.9) Corresponding iron mass Hydrochloric acid volume (4.2) Correspondingiron concentration after final dilution Copper basesolution volume (4.10) Corresponding copper mass Corresponding

49、 iron mass fraction of test sample ml mg ml mg/ml ml g % 0a0 1 0 50 1 0 5 0,05 0,9 0,000 5 50 1 0,005 10 0,10 0,8 0,001 0 50 1 0,010 15 0,15 0,7 0,001 5 50 1 0,015 20 0,20 0,6 0,002 0 50 1 0,020 25 0,25 0,5 0,002 5 50 1 0,025 aBlank test on reagents for calibration curve. 7.4.1.3 Calibration for iron mass fractions between 0,025 % and 0,5 % Into each of a series of seven 100 ml one-mark volumetric flasks, introduce the volumes of iron standard solution (4.8) and of copper base solution (4.10) as shown in Table 2. Introduce also 10 ml of