1、BRITISH STANDARDBS EN 725-2:2007Advanced technical ceramics Methods of test for ceramic powders Part 2: Determination of impurities in barium titanateThe European Standard EN 725-2:2007 has the status of a British StandardICS 81.060.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3
2、g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 725-2:2007This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2007 BSI 2007ISBN 978 0 580 552
3、03 8National forewordThis British Standard is the UK implementation of EN 725-2:2007. It supersedes DD ENV 725-2:1994 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee RPI/13, Advanced technical ceramics.A list of organizations represented on this commit
4、tee 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 correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since publicat
5、ionAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 725-2November 2007ICS 81.060.30 Supersedes ENV 725-2:1994 English VersionAdvanced technical ceramics - Methods of test for ceramicpowders - Part 2: Determination of impurities in barium titanateCramiques techniques avances -
6、Mthodes dessai pourpoudres cramiques - Partie 2 : Dtermination desimpurets dans le titanate de baryumHochleistungskeramik - Prfverfahren fr keramischePulver - Teil 2: Bestimmung von Verunreinigungen inBariumtitanatpulvernThis European Standard was approved by CEN on 23 September 2007.CEN members are
7、 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 be obtained on application to the
8、 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 Management Centre has the same sta
9、tus 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, Norway, Poland, Portugal,Romania, S
10、lovakia, 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 2007 CEN All rights of exploitation in any form and by any means reservedworldwide
11、 for CEN national Members.Ref. No. EN 725-2:2007: EEN 725-2:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents.4 5 Apparatus .5 6 Preparation of sample solution5 6.1 Sample calcination 5 6.2 Test sample 5 6.3 Dissolution of the test sample5 7 Calibration 6
12、7.1 Standard addition method 6 7.2 Calibration method 6 8 Procedure .6 8.1 ICP spectrometer operation6 8.2 Standard addition method 7 8.3 Calibration method 7 9 Test report 7 EN 725-2:2007 (E) 3 Foreword This document (EN 725-2:2007) has been prepared by Technical Committee CEN/TC 184 “Advanced tech
13、nical ceramics”, the secretariat of which is held by BSI. 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 May 2008, and conflicting national standards shall be withdrawn at the latest by May 2008.
14、 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. This document supersedes ENV 725-2:1994. EN 725 Advanced technical ceramics Methods o
15、f test for ceramic powders was prepared in Parts as follows: Part 1: Determination of impurities in alumina Part 2: Determination of impurities in barium titanate Part 3: Determination of the oxygen content of non-oxides by thermal extraction with a carrier gas Part 4: Determination of oxygen conten
16、t in aluminium nitride by XRF analysis Part 5 Determination of particle size distribution Part 6: Determination of the specific surface area withdrawn Part 7: Determination of the absolute density withdrawn Part 8: Determination of tapped bulk density Part 9: Determination of un-tapped bulk density
17、Part 10: Determination of compaction properties Part 11: Determination of densification on natural sintering Part 12: Chemical analysis of zirconia Part 6 and part 7 of this series were superseded in 2005 by EN ISO 18757 and EN ISO 18753. According to the CEN/CENELEC Internal Regulations, the nation
18、al standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Po
19、land, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. EN 725-2:2007 (E) 4 1 Scope This part of EN 725 describes a method for the determination of impurities in barium titanate powders using inductively coupled plasma optical emission spectroscopy (ICP-OES).
20、The method is applicable only to stoichiometric barium titanate. The maximum concentrations measured for each impurity are as follows: Sr 4 mg/g (4 000 ppm) Ca 500 g/g (500 ppm) K 200 g/g (200 ppm) Na, Mg, Al, Fe, Nb 100 g/g (100 ppm) The minimum concentration or detection limits are from 1 g/g to 5
21、 g/g (1 ppm to 5 ppm). 2 Normative references 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. EN
22、ISO/IEC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Principle Calcined barium titanate powder is dissolved in a mixture of hydrochloric acid and hydrogen peroxide, and the impurities in the solution are determined by ICP-OES analysis,
23、 using an addition method of synthetic matrix matched solutions for the calibration. 4 Reagents Spectroscopic grades of the following reagents shall be used. 4.1 Quartz distilled water or water of equivalent purity. 4.2 Hydrochloric acid, density = 1,18 g/cm. 4.3 Hydrogen peroxide, 110 V/V. 4.4 Bari
24、um chloride solution, 99,999 % purity. 4.5 Titanium chloride, TiCl4, in solution, 99,999 % purity. 4.6 Reagents for calibration A commercial solution, or solution obtained by dissolution of a pure chemical compound, of concentration 1g/l shall be used for each of the following: strontium; calcium; p
25、otassium; sodium; magnesium; aluminium; iron; and niobium. EN 725-2:2007 (E) 5 5 Apparatus 5.1 Spectrometer for inductively coupled plasma atomic emission, with a quartz torch hand pneumatic cross-flow nebulizer. 5.2 Muffle furnace, for operation at 900 C 50 C. 5.3 Platinum or platinum/gold crucible
26、 and lid. 5.4 Balance, to weigh to 0,001 g. 5.5 PTFE beakers, 100 ml, with paraffin film. 5.6 Polyethylene pipettes, micro-pipettes and 100 ml volumetric flasks. 5.7 Hot plate, with magnetic stirrer. 5.8 Dessicator. 5.9 Double boiler. 6 Preparation of sample solution 6.1 Sample calcination Weigh abo
27、ut 1,2 g to an accuracy of 0,001 g of the sample into a platinum crucible. Calcine the sample for 2 h in the muffle furnace at 900 C 50 C. Remove it from the hot furnace and allow it to cool in the desiccator. 6.2 Test sample Weigh 1 000 g 0,001 g of the calcined powder from 6.1 and place this test
28、sample into a 100 ml PTFE beaker. 6.3 Dissolution of the test sample Place the magnetic bar (5.7) in the beaker containing the test sample and carefully add 25 ml of water (4.1), 25 ml of hydrochloric acid (4.2) and 8 ml of hydrogen peroxide (4.3). Cover the beaker with paraffin film. Heat the beake
29、r to 60 C 10 C and maintain at this temperature while stirring, until either the sample is dissolved or the amount of residue is constant. NOTE A double boiler is recommended for heating. If there is residue, remove this by filtration and repeat the dissolution procedure. Transfer the cool solution
30、to a 100 ml volumetric flask and make up to volume with the distilled water. Use the solution for the analysis (clause 8) within 48 h. EN 725-2:2007 (E) 6 7 Calibration 7.1 Standard addition method For non-routine samples with unknown impurity levels, standard addition, as follows, can be used to de
31、termine the concentration of impurities. Prepare the final test solutions by diluting the sample solution (6.3) so that: a) final test solutions with added amounts of standard solutions (4.6) are in the concentration range given in Table 1; b) the amount of standard solution added is similar to the
32、amount of each impurity in the final test solution. 7.2 Calibration method Routine samples with known impurity levels shall be calibrated by a synthetic calibration method. This method uses solutions which are matrix-matched with BaCl2, TiCl4, HCl and H2O2. The concentration of matrix components in
33、these solutions shall be such that the concentration of the impurities is within the range given in the scope. Table 1 Concentration range for impurities Element Concentration range (106gml1) Na 0 to 10 K 0 to 5 Mg 0 to 0,3 Ca 0 to 3 Sr 0 to 5 A1 0 to 10 Fe 0 to 1 Nb 0 to 15 8 Procedure 8.1 ICP spec
34、trometer operation Adjust the ICP spectrometer (5.1) to provide a stable plasma, a high signal-to-noise ratio and a separation of spectral overlaps for the impurities being determined. Follow the manufacturers instructions for igniting the plasma. NOTE Use of UV eye protectors is necessary. Use the
35、wavelengths given in Table 2 for the determination of each impurity. EN 725-2:2007 (E) 7 Table 2 Wavelengths for each impurity Element Wavelength (nm) Na 589,59 K 766,47 Mg 279,55 Ca 422,67 or 393,37 Sr 346,44 or 407,77 Al 396,15 Fe 259,94 Nb 309,42 or 316,34 8.2 Standard addition method Aspirate th
36、e blank solution and then the samples in order of increasing signal. Extrapolate the signal back to give the concentration of impurity in ppm, after the blank value has been subtracted. 8.3 Calibration method Aspirate the blank solution and then the calibration solutions in order of increasing signa
37、l. Aspirate the equivalent hydrochloric acid solution (4.2) between each of these solutions and record the readings when stable responses are reached. Take three measurements and calculate the mean. Prepare calibration graphs for each element by plotting the signal values against quantities of impur
38、ity in the test sample, expressed as ppm. Use these calibration graphs to convert the signal values, after the blank value has been subtracted, of the test solution into concentration of impurities in the test sample (see 6.2). Aspirate the test solutions and read the intensity values from the graph
39、s. Express the results in ppm of the test sample. 9 Test report The test report shall be in accordance with the reporting provisions of EN ISO/IEC 17025 and shall include at least the following information: a) name and address of the testing establishment; b) date of the test; c) on each page, a uni
40、que report identification and page number; d) customer name and address; e) reference to this standard, i.e. determined in accordance with EN 725-2:2007; f) authorizing signature; g) any deviation from the method described, with appropriate validation, i.e. demonstrated to be acceptable to the parti
41、es involved; EN 725-2:2007 (E) 8 h) description of the powder (e.g. material type, manufacturer code, batch or code number); i) details of the ICP-OES equipment used; j) any information on the decomposition of the sample; k) calibration procedure used; l) relevant test parameters; m) reproducibility
42、 and repeatability of the method; n) results of individual determinations, mean results and standard deviations; o) any unusual features noted during the determination; p) any comments about the test or test results. blankBS EN 725-2:2007BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards Ins
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