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1、DRAFT FOR DEVELOPMENT DD CEN/TS 15025:2006 Copper and copper alloys Determination of magnesium content Flame atomic absorption spectrometry method (FAAS) ICS 77.120.30 ? Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy,
2、(c) BSI DD CEN/TS 15025:2006 This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 31 January 2007 BSI 2007 ISBN 978-0-580-49913-5 National foreword This Draft for Development was published by BSI. It is the UK implementation of CEN/TS 15025:2
3、006. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical application can be obtained. C
4、omments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated not later than 3 years after its publication by the Europe
5、an organization so that a decision can be taken on its status. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period, the responsible BSI Committee will decide whe
6、ther to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL. The UK participation in
7、 its preparation was entrusted to Technical Committee NFE/34, Copper and copper alloys. A list of organizations represented on NFE/34 can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its co
8、rrect application. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15025
9、November 2006 ICS 77.120.30 English Version Copper and copper alloys - Determination of magnesium content - Flame atomic absorption spectrometry method (FAAS) Cuivre et alliages de cuivre - Dosage de magnsium - Mthode par spectromtrie dabsorption atomique dans la flamme (SAAF) Kupfer und Kupferlegie
10、rungen - Bestimmung des Magnesiumgehaltes - Flammenatomabsorptionsspektrometrisches Verfahren (FAAS) This Technical Specification (CEN/TS) was approved by CEN on 12 September 2006 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years
11、the members of CEN will be requested to submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard. CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available promptly at nation
12、al level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech
13、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 STANDARDIZATION COMIT EUROPE
14、N DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15025:2006: E Licensed Copy: London South Bank University, London Sout
15、h Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Principle4 4 Reagents and materials 4 5 Apparatus .5 6 Sampling.5 7 Procedure .6 8 Expression of results 9 9 Precision.10 10 Test report10 Bibliography12 CE
16、N/TS 15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 3 Foreword This document (CEN/TS 15025:2006) has been prepared by Technical Committee CEN/TC 133 “Copper and copper alloys”, the secretariat of wh
17、ich is held by DIN. Within its programme of work, Technical Committee CEN/TC 133 requested CEN/TC 133/WG 10 “Methods of analysis“ to prepare the following Technical Specification: CEN/TS 15025, Copper and copper alloys Determination of magnesium content Flame atomic absorption spectrometry method (F
18、AAS) According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to announce this Technical Specification: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
19、Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. CEN/TS 15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled C
20、opy, (c) BSI 4 1 Scope This Technical Specification specifies a flame atomic absorption spectrometric method (FAAS) for the determination 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 f
21、ractions between 0,001 % and 0,20 %. 2 Normative references The following referenced documents are indispensable for the application of this Technical Specification. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including
22、 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 1811-2, Copper and copper alloys Selection and preparation of samples for chemical analysis Part 2: Sampling of wrought products a
23、nd castings 3 Principle Dissolution of a test portion in a hydrochloric-nitric acid mixture followed, after suitable dilution, by aspiration into an air/acetylene flame of an atomic absorption spectrometer. Determination of the magnesium content by measuring the absorption of the 285,2 nm line emitt
24、ed by a magnesium hollow-cathode lamp. 4 Reagents and materials 4.1 General During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.2 Hydrochloric acid, HCl ( = 1,19 g/ml) 4.3 Nitric acid, HNO3 ( = 1,40 g/ml) 4.4 Nitric acid sol
25、ution, 1 + 1 Dilute 100 ml of nitric acid (4.3) in 100 ml of water. 4.5 Magnesium stock solution, 0,5 g/l Mg Weigh (0,5 0,001) g of magnesium (Mg 99,9 %) and transfer it into a 250 ml beaker. Add 20 ml of the nitric acid solution (4.4) in small amounts. Cover with a watch glass and heat gently until
26、 the magnesium is completely dissolved. Boil the solution until nitrous fumes have been expelled. Cool to room temperature, transfer 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 Mg. CEN/TS
27、15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 5 4.6 Magnesium standard solution, 0,01 g/l Mg Using a calibrated pipette, transfer 5 ml of the magnesium stock solution (4.5) into a 250 ml one-mark v
28、olumetric flask. Dilute to the mark with water and mix well. Prepare this solution immediately prior to use. 1 ml of this solution contains 0,01 mg of Mg. 4.7 Magnesium standard solution, 0,000 5 g/l Mg Using a calibrated pipette, transfer 5 ml of the magnesium standard solution (4.6) into a 100 ml
29、one-mark volumetric flask. Dilute to 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. 4.8 Lanthanum (III) chloride solution, 200 g/l Dissolve 200 g of lanthanum chloride heptahydrate (LaCl37H2O) in a 2 000 ml beaker wi
30、th approximately 800 ml of water. Transfer the solution into a 1 000 ml one-mark volumetric flask. Dilute to the mark with water and mix well. 4.9 Copper base solution, 50 g/l Cu Weigh (50 0,01) g of electrolytic copper and transfer it into a 2 000 ml beaker. Add 500 ml of hydrochloric acid (4.2) an
31、d, in small amounts, 250 ml of the nitric acid solution (4.4). 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 mar
32、k with water and mix well. 4.10 Copper base solution, 10 g/l Cu Transfer 50 ml of the copper base solution (4.9) into a 250 ml one-mark volumetric flask, add 15 ml of the nitric acid solution (4.4). Dilute to the mark with water and mix well. 1 ml of this solution contains 0,01 g of Cu. 5 Apparatus
33、5.1 Ordinary laboratory apparatus 5.2 Atomic absorption spectrometer, fitted with an air/acetylene burner 5.3 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
34、 or millings, with a maximum thickness of 0,3 mm. CEN/TS 15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 6 7 Procedure 7.1 Preparation of the test portion solution 7.1.1 Test portion Weigh (1 0,001)
35、g of the test sample. 7.1.2 Test portion solution Transfer the test portion (7.1.1) into a 250 ml beaker (5.2). Add 10 ml of hydrochloric acid (4.2) and 10 ml of the nitric acid solution (4.4). Cover with a watch glass and heat gently until the test portion is completely dissolved, then heat at a te
36、mperature of approximately 90 C until brown fumes have been expelled. Wash the cover and the sides of the beaker with water. Cool to room temperature. Transfer the solution to a 100 ml one-mark volumetric flask. Dilute to the mark with water and mix well. Select an aliquot portion from the test port
37、ion solution according to the expected magnesium mass fraction as indicated in Table 1. Table 1 Aliquot solution Magnesium (mass fraction) Aliquot of the test portion solution (7.1.2) Lanthanum chloride(III) solution volume (4.8) Final volume of diluted solution % ml ml ml 0,001 to 0,05 10 10 100 0,
38、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 quantities 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 prepari
39、ng a solution of a standard material or a synthetic sample containing a known amount of magnesium and of a composition similar to the material to be 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 Gen
40、eral In all cases, copper, chloride and nitrate concentrations, and acidity in the calibration solutions 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,
41、 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 in mass fraction 10 %, an appropriate mass of this element shall be added to the calibration solutions. The magnesium concentration of the calibratio
42、n solutions shall be adjusted to suit the sensitivity of the spectrome- ter used, so that the curve of absorbance as a function of concentration is a straight line. CEN/TS 15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncont
43、rolled Copy, (c) BSI 7 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 volumes of magnesium standard solution (4.6 or 4.7) and of copper base solution (4.10) shown in Tables 2 or 3, depending on the expected magnes
44、ium content, followed by 10 ml of lanthanum (III) chloride solution (4.8). Dilute to the mark with water and mix well. The range of calibration solutions is appropriate for most current models of equipment of average performance. The range and operating conditions shall be selected for optimum measu
45、rements by the particular equipment available. Table 2 Calibration for magnesium mass fractions between 0,001 % and 0,05 % Magnesium standard solution volume Corresponding magnesium mass Corresponding magnesium concentration after final dilution Copper base solution volume Corresponding copper mass
46、Corresponding magnesium mass fraction of sample (4.7) (4.6) (4.10) ml ml mg mg/ml ml g % 0 a 0 0 10 0,1 0 2 0,001 0,000 01 10 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
47、0,1 0,040 5 0,05 0,000 5 10 0,1 0,050 a Blank test on reagents for calibration curve. Table 3 Calibration for magnesium mass fractions between 0,05 % and 0,20 % Magnesium standard solution volume (4.6) Corresponding magnesium mass Corresponding magnesium concentration after final dilution Copper bas
48、e solution volume (4.10) Corresponding copper mass Corresponding magnesium mass fraction of sample ml mg mg/ml ml g % 0 a 0 0 5 0,050 0 2,5 0,025 0,000 25 5 0,050 0,05 5 0,050 0,000 50 5 0,050 0,10 7,5 0,075 0,000 75 5 0,050 0,15 10,0 0,1 0,001 5 0,050 0,20 a Blank test on reagents for calibration c
49、urve. CEN/TS 15025:2006 Licensed Copy: London South Bank University, London South Bank University, Thu Jan 18 01:23:06 GMT+00:00 2007, Uncontrolled Copy, (c) BSI 8 7.4.2 Adjustment of the atomic absorption spectrometer Fit the magnesium hollow-cathode lamp (5.3) into the atomic absorption spectrometer (5.2), switch on the current and allow it to stabilize. Adjust the wavelength in the region of 285,2 nm to minimum absorbance. Following the manufacture