1、January 2008DEUTSCHE NORM English price group 7No part of this standard 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 81.060.30!$Ki“1409470ww
2、w.din.deDDIN EN 725-2Advanced technical ceramics Methods of test for ceramic powders Part 2: Determination of impurities in barium titanateEnglish version of DIN EN 725-2:2008-01Hochleistungskeramik Prfverfahren fr keramische Pulver Teil 2: Bestimmung von Verunreinigungen in BariumtitanatpulvernEngl
3、ische Fassung DIN EN 725-2:2008-01SupersedesDIN V ENV 725-2:1994-03www.beuth.deDocument comprises 10 pagesDIN EN 725-2:2008-01 2 National foreword This standard has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics” (Secretariat: BSI, United Kingdom). At present a DIN comm
4、ittee does not exist for this standard since the parties concerned have not shown any interest in work on the subject. The Normenausschuss Materialprfung (Materials Testing Standards Committee) is obliged to publish the standard, however, as the subject falls in its domain. Amendments This standard
5、differs from DIN V ENV 725-2:1994-03 as follows: a) The standard has been extensively revised. b) The prestandard status has been changed to that of a full standard. Previous editions DIN V ENV 725-2: 1994-03 EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 725-2November 2007ICS 81.060.30 Supersede
6、s ENV 725-2:1994 English VersionAdvanced technical ceramics - Methods of test for ceramicpowders - Part 2: Determination of impurities in barium titanateCramiques techniques avances - Mthodes dessai pourimpurets dans le titanate de baryumHochleistungskeramik - Prfverfahren fr keramischePulver - Teil
7、 2: Bestimmung von Verunreinigungen inBariumtitanatpulvernThis European Standard was approved by CEN on 23 September 2007.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 withou
8、t any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may 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 mad
9、e by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management 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,
10、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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNG
11、Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 725-2:2007: Epoudres cramiques - Partie 2: Dtermination desEN 725-2:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative
12、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 7.1 Standard addition method 6 7.2 Calibration method 6 8 Procedure .6 8.1 ICP spectrometer operation6 8.2 Standard a
13、ddition method 7 8.3 Calibration method 7 9 Test report 7 DIN EN 725-2:2008-01 -2: - EN 725-2:2007 (E) 3 Foreword This document (EN 725-2:2007) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is held by BSI. This European Standard shall be
14、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. Attention is drawn to the possibility that some of the elements of this document may be t
15、he 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 of test for ceramic powders was prepared in Parts as follows: Part 1: Determination of impu
16、rities 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 content in aluminium nitride by XRF analysis Part 5 Determination of particle size distribution
17、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 Part 10: Determination of compaction properties Part 11: Determination of densification on
18、 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 national standards organizations of the following countries are bound to implement this European
19、 Standard: 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, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kin
20、gdom. - DIN EN 725-2:2008-01 -2:- :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). The method is applicable only to stoichiometric barium titana
21、te. 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 g/g (1 ppm to 5 ppm). 2 Normative references The following r
22、eferenced 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 ISO/IEC 17025, General requirements for the competence of tes
23、ting 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, using an addition method of synthetic matrix matched solutio
24、ns 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 Barium chloride solution, 99,999 % purity. 4.5 Titanium chloride,
25、 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; potassium; sodium; magnesium; aluminium; iron; and niobium. DI
26、N EN 725-2:2008-01 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 and lid. 5.4 Balance, to weigh to 0,001
27、 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 about 1,2 g to an accuracy of 0,001 g of th
28、e 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 sample into a 100 ml PTFE beaker. 6.3 Di
29、ssolution 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 beaker to 60 C 10 C and maintain at this temp
30、erature 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 to a 100 ml volumetric flask and make up
31、 to volume with the distilled water. Use the solution for the analysis (clause 8) within 48 h. DIN EN 725-2:2008-01 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 determine the concent
32、ration 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 amount of each impu
33、rity 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 these solutions sha
34、ll 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 spectrometer operation
35、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 wavelengths given i
36、n Table 2 for the determination of each impurity. DIN EN 725-2:2008-01 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
37、the 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 sig
38、nal. 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 imp
39、urity 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 gra
40、phs. 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 u
41、nique 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 par
42、ties involved; DIN EN 725-2:2008-01 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 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. DIN EN 725-2:2008-01
