1、June 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).ICS 77
2、.120.30!$i,*“1700907www.din.deDDIN EN 15622Copper and copper alloys Determination of lead content Flame atomic absorption spectrometric method (FAAS)English translation of DIN EN 15622:2010-06Kupfer und Kupferlegierungen Bestimmung des Bleigehaltes Flammenatomabsorptionsspektrometrisches Verfahren (
3、FAAS)Englische bersetzung von DIN EN 15622:2010-06Cuivre et alliages de cuivre Dosage du plomb Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF)Traduction anglaise de DIN EN 15622:2010-06www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be cons
4、idered authoritative.1406.10 DIN EN 15622:2010-06 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 German body involved in its preparation was the Normena
5、usschuss 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: ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5
6、725-3 DIN ISO 5725-3 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (trueness and 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
7、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: Intermediate measures of the precision of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPIS
8、CHE 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 - Dosage du plomb - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kup
9、ferlegierungen - Bestimmung des Bleigehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This European Standard was approved by CEN on 23 January 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Sta
10、ndard 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 Centre or to any CEN member. This European Standard exists in three official versions (English, Fren
11、ch, 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 official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia
12、, Cyprus, 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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZAT
13、ION 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 for CEN national Members. Ref. No. EN 15622:2010: EEN 15622:2010 (E) 2 Contents Page Foreword 31
14、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 solution .57.1.3 Lead mass fractions between 0,01 % and 0,15 % .67.1.4 Lead mass fractions between 0,1 % and 0,75 % .
15、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 Adjustment of the atomic absorption spectrometer 87.4.3 Spectrometric measurement 87.4.4 Calibration curve87.5 Dete
16、rmination .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 method .99 Precision 1010 Test report . 11Bibliography . 12DIN EN 15622:2010-06 EN 15622:2010 (E) 3 Foreword This doc
17、ument (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 of a national standard, either by publication of an identical text or by endorsement, at the latest by Septe
18、mber 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 subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such pat
19、ent 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 copper alloys Determination of lead content Flame atomic absorption spectrometric method (FAAS). According to the
20、 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, Latvia,
21、 Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. DIN EN 15622:2010-06 EN 15622:2010 (E) 4 1 Scope This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination o
22、f 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 references The following referenced documents are indispensable for the application of this document. For
23、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 ISO
24、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 fluoroboric-nitric acid mixture followed, after suitable dilution, by aspiration of the test solution into an air
25、/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 standard method some laboratories have also carried out the measurements at 283 nm line. These measurements sho
26、wed 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, use only reagents of recognized analytical grade and only distilled water or water of equivalent purit
27、y. 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 Hydrofluoric acid is a hazardous substance. Care shall be taken and it shall be used under an efficient fume
28、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 water and mix well. 4.6 Lead stock solution, 1,0 g/l Pb. DIN EN 15622:2010-06 EN 15622:2010 (E) 5 Weigh (1
29、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 bring to the boiling point until the nitrous fumes have been expelled. Cool to room temperature, transf
30、er 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 contains 0,001 g of Pb. 4.7 Lead standard solution, 0,1 g/l Pb. Transfer 25,0 ml of the lead stock s
31、olution (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 Pb. 4.8 Copper base solution, 20 g/l Cu. Weigh (10 0,01) g of pure, lead-free copper (Pb 10 %, an ap
32、propriate 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 may occur if the same volumes
33、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 lead concentration of the calibration solutions shall be adjusted to
34、 suit the sensitivity of the spectrometer used, so that the curve of absorbance as a function of concentration is a straight line. DIN EN 15622:2010-06 EN 15622:2010 (E) 7 7.4.1.2 Lead mass fractions between 0,01 % and 0,15 % Into each of a series of six 100 ml one-mark volumetric flasks, introduce
35、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 0,15 % Lead standard solution volume (4.7) Corresponding lead mass Correspondinglead concentratio
36、n 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 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 tes
37、t 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) and of copper base solution (4.8) as shown in Table 2. Dilute to the mark with water and mix
38、 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 solution volume(4.8) Corresponding copper mass Correspondinglead mass fractionof sample ml mg mg/ml
39、 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 between 0,5 % and 5,0 % Into each of a series of six 100 ml one-mark volumetric flask, introduc
40、e 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. DIN EN 15622:2010-06 EN 15622:2010 (E) 8 Table 3 Calibration for lead mass fractions between 0,5 % and 5,0 % Lead standard solution volume (4.7) Correspond
41、ing 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 0,002 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 3,7
42、5 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 (5.3), switch on the current and allow it to stabilize. Adjust the wavelength in the region
43、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 the manufacturers instructions regarding the minimum flow rate of acetylene, aspirate the
44、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 calibration solutions (7.4.1.2, 7.4.1.3 or 7.4.1.4 depending on the expected lead content) in succe
45、ssion 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 measurement, see NOTE. NOTE For certain types of spectrometer, instead of water it is prefe
46、rable 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 corresponding analyte amounts. Use appropriate spectrometer software or an off-line computer for
47、 regression calculations or prepare a graphical representation. 7.5 Determination 7.5.1 General The analyses shall be carried out independently, in duplicate. DIN EN 15622:2010-06 EN 15622:2010 (E) 9 7.5.2 Preliminary spectrometric measurement Carry out a preliminary measurement on the test portion
48、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). Estimate the preliminary analyte amount by using the calibration curve (7.4.4). 7.5.
49、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 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 t
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