EN 15622-2010 en Copper and copper alloys - Determination of lead content - Flame atomic absorption spectrometric method (FAAS)《铜和铜合金 铅含量的测定 火焰原子吸收光谱法测定法(FAAS)》.pdf

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1、BS EN 15622:2010ICS 77.120.30NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCopper andcopper alloys Determination oflead content Flameatomic absorptionspectrometric method(FAAS)This British Standardwas published under theauthority of the StandardsPolicy and Str

2、ategyCommittee on 31 March2010 BSI 2010ISBN 978 0 580 58190 8Amendments/corrigenda issued since publicationDate CommentsBS EN 15622:2010National forewordThis British Standard is the UK implementation of EN 15622:2010.The UK participation in its preparation was entrusted to TechnicalCommittee NFE/34,

3、 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 with a British Standard cann

4、ot confer immunityfrom legal obligations.BS EN 15622:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15622 March 2010 ICS 77.120.30 English Version Copper and copper alloys - Determination of lead content - Flame atomic absorption spectrometric method (FAAS) Cuivre et alliages de cuivre - D

5、osage du plomb - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegierungen - Bestimmung des Bleigehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 23 January 2010. CEN members are bound to comply wit

6、h 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 may be obtained on application to the CEN Management Ce

7、ntre 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 the CEN Management Centre has the same status as the offic

8、ial 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, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slov

9、akia, 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 exploitation in any form and by any means reserved worldwide

10、 for CEN national Members. Ref. No. EN 15622:2010: EBS EN 15622:2010EN 15622:2010 (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 57.1.1 Test portion 57.1.2 Test portion sol

11、ution .57.1.3 Lead mass fractions between 0,01 % and 0,15 % .67.1.4 Lead mass fractions between 0,1 % and 0,75 % .67.1.5 Lead mass fractions between 0,5 % and 5,0 % .67.2 Blank test 67.3 Check test .67.4 Establishment of the calibration curve .67.4.1 Preparation of the calibration solutions 67.4.2 A

12、djustment of the atomic absorption spectrometer 87.4.3 Spectrometric measurement 87.4.4 Calibration curve87.5 Determination .87.5.1 General 87.5.2 Preliminary spectrometric measurement 97.5.3 Spectrometric measurements 98 Expression of results 98.1 Use of calibration curve 98.2 Use of bracketing met

13、hod .99 Precision 1010 Test report . 11Bibliography . 12BS EN 15622:2010EN 15622:2010 (E) 3 Foreword This document (EN 15622:2010) 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

14、 of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2010, and conflicting national standards shall be withdrawn at the latest by September 2010. Attention is drawn to the possibility that some of the elements of this document may be the s

15、ubject 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 European Standard: EN 15622, Copper and copp

16、er alloys Determination of lead content Flame atomic absorption spectrometric method (FAAS). 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, Croatia, Cyprus,

17、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 the United Kingdom. BS EN 15622:2010EN 15622:2010 (E) 4 1 Sco

18、pe This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination of the lead in copper and copper alloys in the form of unwrought, wrought and cast products. The method is applicable to products having lead mass fractions between 0,01 % and 5,0 %. 2 Normative re

19、ferences 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 Sel

20、ection 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 samples for chemical analysis Part 2: Sampling of wrought products and castings 3 Principle Dissolution of a test portion in fluorobor

21、ic-nitric acid mixture followed, after suitable dilution, by aspiration of the test solution into an air/acetylene flame of an atomic absorption spectrometer. Measurement of the absorption of the 217,0 nm line emitted by a lead hollow-cathode lamp. NOTE During the validation exercise of this standar

22、d method some laboratories have also carried out the measurements at 283 nm line. These measurements showed a satisfactory trueness. However, the number of results produced was too few and, therefore, insufficient for the estimation of the corresponding precision data. 4 Reagents During the analysis

23、, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Nitric acid, HNO3( = 1,40 g/ml). 4.2 Nitric acid solution (1 + 1). Add 100 ml of nitric acid (4.1) to 100 ml of water. 4.3 Hydrofluoric acid, HF, 40 % solution ( = 1,13 g/ml). WARNING Hydro

24、fluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume hood. 4.4 Boric acid, H3BO3, 40 g/l solution. 4.5 Fluoroboric-nitric acid mixture. Add 300 ml of boric acid (4.4), 30 ml of hydrofluoric acid (4.3) and 500 ml of nitric acid (4.1) to 150 ml of wat

25、er and mix well. 4.6 Lead stock solution, 1,0 g/l Pb. BS EN 15622:2010EN 15622:2010 (E) 5 Weigh (1 0,001) g of lead (Pb 99,9 %) and transfer it into a 250 ml beaker. Add 20 ml of nitric acid solution (4.2), cover with a watch glass and heat gently until the lead is completely dissolved and then brin

26、g 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, add 100 ml of water and 9 ml of nitric acid solution (4.2). Dilute to the mark with water and mix well. 1 ml of this solution c

27、ontains 0,001 g of Pb. 4.7 Lead standard solution, 0,1 g/l Pb. Transfer 25,0 ml of the lead stock solution (4.6) into a 250 ml one-mark volumetric flask, add 100 ml of water and 9 ml of nitric acid solution (4.2). Dilute to the mark with water and mix well. 1 ml of this solution contains 0,1 mg of P

28、b. 4.8 Copper base solution, 20 g/l Cu. Weigh (10 0,01) g of pure, lead-free copper (Pb 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

29、 in test solutions 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 th

30、e test sample in solution. The lead 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 15622:2010EN 15622:2010 (E) 7 7.4.1.2 Lead mass fractions betwee

31、n 0,01 % and 0,15 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce the volumes of lead standard solution (4.7) and of copper base solution (4.8) shown in Table 1. Dilute to the mark with water and mix well. Table 1 Calibration for lead mass fractions between 0,01 % and 0,1

32、5 % Lead standard solution volume (4.7) Corresponding lead mass Correspondinglead concentration after final dilution Copper base solution volume(4.8) Corresponding copper mass Correspondinglead mass fractionof sample ml mg mg/ml ml g % 0a0 0 50 1,000 0 1 0,1 0,001 50 1,000 0,01 2 0,2 0,002 50 1,000

33、0,02 5 0,5 0,005 50 1,000 0,05 10 1,0 0,010 50 1,000 0,1015 1,5 0,015 50 1,000 0,15 aBlank test on reagents for calibration curve. 7.4.1.3 Lead mass fractions between 0,1 % and 0,75 % Into each of a series of five 100 ml one-mark volumetric flask, introduce the volumes of lead standard solution (4.7

34、) and of copper base solution (4.8) as shown in Table 2. Dilute to the mark with water and mix well. Table 2 Calibration for lead mass fractions between 0,1 % and 0,75 % Lead standard solution volume (4.7) Corresponding lead mass Correspondinglead concentration after final dilution Copper base solut

35、ion volume(4.8) Corresponding copper mass Correspondinglead mass fractionof sample ml mg mg/ml ml g % 0a0 0 10 0,200 0 2 0,2 0,002 10 0,200 0,10 5 0,5 0,005 10 0,200 0,25 10 1,0 0,010 10 0,200 0,5015 1,5 0,015 10 0,200 0,75 aBlank test on reagents for calibration curve. 7.4.1.4 Lead mass fractions b

36、etween 0,5 % and 5,0 % Into each of a series of six 100 ml one-mark volumetric flask, introduce the volumes of lead standard solution (4.7) and of copper base solution (4.8) as shown in Table 3. Dilute to the mark with water and mix well. BS EN 15622:2010EN 15622:2010 (E) 8 Table 3 Calibration for l

37、ead mass fractions between 0,5 % and 5,0 % Lead standard solution volume (4.7) Corresponding lead mass Correspondinglead concentrationafter final dilution Copper base solution volume(4.8) Corresponding copper mass Correspondinglead mass fraction of sample ml mg mg/ml ml g %0a0 0 2 0,040 0 2 0,2 0,00

38、2 2 0,040 0,50 5 0,5 0,005 2 0,040 1,25 10 1,0 0,010 2 0,040 2,5015 1,5 0,015 2 0,040 3,75 20 2,0 0,020 2 0,040 5,00aBlank test on reagents for calibration curve. 7.4.2 Adjustment of the atomic absorption spectrometer Fit the lead hollow-cathode lamp (5.4) into the atomic absorption spectrometer (5.

39、3), switch on the current and allow it to stabilize. Adjust the wavelength in the region of 217,0 nm to minimum absorbance (see NOTE in Clause 3). Following the manufacturers instructions, fit the correct burner, light the flame and allow the burner temperature to stabilize. Taking careful note of t

40、he manufacturers instructions regarding the minimum flow rate of acetylene, aspirate the calibration solution of highest concentration of analyte and adjust the burner configuration and gas flows to obtain maximum absorbance. 7.4.3 Spectrometric measurement Aspirate the relevant series of calibratio

41、n solutions (7.4.1.2, 7.4.1.3 or 7.4.1.4 depending on the expected lead content) in succession into the flame and measure the absorbance for each solution. Take care to keep the aspiration rate constant throughout the preparation of the calibration curve. Spray water through the burner after each me

42、asurement, see NOTE. NOTE For certain types of spectrometer, instead of water it is preferable to use a solution containing the attack reagents, in the same concentrations as in the test portion solutions. 7.4.4 Calibration curve Establish the calibration curve using measured absorbances and corresp

43、onding analyte amounts. Use appropriate spectrometer software or an off-line computer for regression calculations or prepare a graphical representation. 7.5 Determination 7.5.1 General The analyses shall be carried out independently, in duplicate. BS EN 15622:2010EN 15622:2010 (E) 9 7.5.2 Preliminar

44、y spectrometric measurement Carry out a preliminary measurement on the test portion solutions (7.1.3, 7.1.4, 7.1.5) following the procedure specified in 7.4.2 and 7.4.3 at the same time as the spectrometric measurements are carried out on the calibration solutions (see 7.4.1.2, 7.4.1.3 or 7.4.1.4).

45、Estimate the preliminary analyte amount by using the calibration curve (7.4.4). 7.5.3 Spectrometric measurements 7.5.3.1 Use of the calibration curve Repeat the measurements and determine the concentration directly using the appropriate calibration curve. 7.5.3.2 Use of bracketing method Carry out a

46、 second measurement on the test portion solutions (7.1.3, 7.1.4 or 7.1.5) following the procedure specified in 7.4.3, by bracketing between two new calibration solutions with a composition similar to that of the calibration solutions (see 7.4.1), but having lead contents slightly higher and slightly

47、 lower ( 10 %) than the estimated lead concentration of the test portion solution. To prepare these calibration solutions, follow the procedure specified in 7.4.1 using, however, suitable quantities of lead standard solution (4.7). 8 Expression of results 8.1 Use of calibration curve Calculate the l

48、ead mass fraction, in percent (%), as follows: w(Pb) = 100f1 Vmc(1) where w(Pb) is the lead mass fraction in per cent (%); c1is the lead concentration from the calibration curve, in milligram per millilitre (mg/ml); m is the mass of the test portion in milligram (mg); Vfis the total1)volume of the t

49、est portion solution (7.1.3, 7.1.4, 7.1.5), in millilitre (ml). 8.2 Use of bracketing method Calculate the lead mass fraction, in percent (%), as follows: w(Pb) = 100f2 Vmc(2) 1) Is the final volume corrected by a dilution ratio (if the case). BS EN 15622:2010EN 15622:2010 (E) 10 where c2is the lead concentration, calculated using Formula (3), in milligram per millilitre (mg/ml); m is the mass of the test portion in milligra