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1、BRITISH STANDARD BS EN 725-5:2007 Advanced technical ceramics Methods of test for ceramic powders Part 5: Determination of particle size distribution The European Standard EN 725-5:2007 has the status of a British Standard ICS 81.060.30 ? Licensed Copy: London South Bank University, London South Ban
2、k University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI BS EN 725-5:2007 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 September 2007 BSI 2007 ISBN 978 0 580 54526 9 National foreword This British Standard is the UK
3、implementation of EN 725-5:2007, incorporating corrigendum August 2007. It supersedes BS EN 725-5:1996 which is withdrawn.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 committee can be ob
4、tained 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 publication Amd. N
5、o. DateComments Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 725-5 January 2007 ICS 81.060.30Supersedes EN 725-5:1996 English Version Advanced technical c
6、eramics - Methods of test for ceramic powders - Part 5: Determination of particle size distribution Cramiques techniques avances - Mthodes dessais pour poudre cramiques - Partie 5: Dtermination de la distribution granulomtrique Hochleistungskeramik - Prfverfahren fr keramische Pulver - Teil 5: Besti
7、mmung der Teilchengrenverteilung This European Standard was approved by CEN on 2 December 2006. CEN members are bound to comply with 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-d
8、ate 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, French, German). A version in any other language made by translation under
9、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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hu
10、ngary, 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 EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Cen
11、tre: rue de Stassart, 36 B-1050 Brussels 2007 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 725-5:2007: E Incorporating corrigendum August 2007 Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05
12、02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references4 3 Apparatus .4 4 Preparation of the suspension.4 5 Calibration5 6 Procedure .5 7 Expression of results 6 8 Test report6 Annex A (informative) Suspending liquids and dispe
13、rsing agents7 Annex B (informative) Certified reference materials11 Annex C (informative) Suspension and dispersion data.12 Annex D (informative) Example of particle size distribution.13 Annex E (informative) Presentation of particle size distribution data.14 Bibliography15 Licensed Copy: London Sou
14、th Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 3 Foreword This document (EN 725-5:2007) has been prepared by Technical Committee CEN/TC 184 “Advanced technical ceramics”, the secretariat of which is held by BSI. This
15、 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 July 2007, and conflicting national standards shall be withdrawn at the latest by July 2007. This document supersedes EN 725-5:1996. EN 725 Advanced tec
16、hnical ceramics Methods of 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: Deter
17、mination of oxygen content 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
18、of un-tapped bulk density Part 10: Determination of compaction properties Part 11: Determination of densification on natural sintering Part 12: Chemical analysis of zirconia Parts 6 and 7 of the series were superseded in 2005 by EN ISO 18757 and EN ISO 18753 respectively. According to the CEN/CENELE
19、C Internal Regulations, the national 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, Luxembou
20、rg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 4 1 Scope This Par
21、t of EN 725 describes the preparation of suspensions and calibration of apparatus, prior to the measurement of particle size distribution of powders used for advanced technical ceramics. The preparation described is appropriate for measurements either by the sedimentation method or the laser light s
22、cattering method. 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 ISO/I
23、EC 17025, General requirements for the competence of testing and calibration laboratories (ISO/IEC 17025:2005) 3 Apparatus 3.1 Glass microscope slides and cover slips. 3.2 Optical microscope. 3.3 Beaker, 50 ml to 100 ml. 3.4 Ultrasonicator. 3.5 Magnetic stirrer. 3.6 Particle size analyser. 4 Prepara
24、tion of the suspension 4.1 Selection of liquid The dispersing liquid for the suspension shall not react with or dissolve the powder. For the sedimentation method of analysis, the density of the liquid shall be less than that of the powder by at least 0,5 g/cm. For the laser light scattering method o
25、f analysis, the liquid shall be optically transparent for the wavelength used. NOTE 1 This is generally 633 nm. The liquid shall have a refractive index which is substantially different from that of the sample. NOTE 2 Any specific manufacturers instructions regarding the refractive index of the disp
26、ersing liquid should be taken into account. Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 5 The liquid for the suspension shall be selected, together with any dispersing agent, from those gi
27、ven in Annex A. NOTE 3 Additional information is given in the bibliographical references listed. The dispersion of powder in the liquid shall be checked by one of the methods given in 4.2. 4.2 Dispersion checking 4.2.1 Optical microscopic examination Place a drop of the prepared suspension on the gl
28、ass slide (3.1) of a microscope (3.2) and carefully cover with a cover slip (3.1). Observe the preparation under a suitable magnification, to determine if particles are completely separated and well dispersed, or if they are gathered together in chains or clusters. NOTE This method is not suitable f
29、or powders with particle diameters of less than 5 m. 4.2.2 Qualitative test by sedimentation Allow the suspension to stand. A correctly dispersed suspension settles less rapidly than a suspension which flocculates, and shows no clear border line between the liquid which becomes clear and the layer w
30、hich is still turbid as sedimentation proceeds. The sediment obtained is compact and of a minimal volume. 4.2.3 Scanning electron microscope (S.E.M.) examination Check the correlation of the particle size distribution obtained with the mean size of the ultimate particles observed by S.E.M. If the su
31、spension is not sufficiently dispersed, particles are partially aggregated and particle size distribution measurements thus give values much higher than the mean size of the ultimate particles observed. 4.2.4 Quantitative test by sedimentation Perform the quantitative tests, while allowing a variati
32、on of the various parameters liable to influence the dispersion quality. Choose the dispersion procedure which gives the smallest mean particle diameter. An examination of the shape of the distribution can give an indication of the presence of agglomerates. 5 Calibration Check the working order of t
33、he apparatus, by analysing standard powders regularly. NOTE Information on available standard reference powders is provided in Annex B. 6 Procedure 6.1 Determine the quantity of powder, the type and quantity of suspending liquid and the dispersing agent to be used. NOTE In principle, and within the
34、limits imposed by the instrument, the sample mass to be dispersed has no influence on the results. However, it is preferable to use dilute suspensions. 6.2 For the sedimentation method, ensure that the volume concentration is less than or equal to 0,2 %. 6.3 For the laser Iight scattering method, fo
35、r all determinations to be accurate, ensure that all particles present in the pencil rays are separate and diffract independently from each other. Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (
36、E) 6 NOTE This condition should be fulfilled when each particle with a radius a is in the centre of a circle with a radius R = a, when there is no secant circle and when no particle casts a shadow on the others. 6.4 In a 50 ml to 100 ml beaker (3.3) prepare a first test sample. Mix the suspending li
37、quid and the dispersing agent, add the powder while stirring the suspension, and disperse using the ultrasonicator (3.4) until free of agglomerates. Continue stirring with a magnetic stirrer (3.5) until the start of the analysis. 6.5 Read the technical instructions of the instrument for general adju
38、stments prior to the test and follow the manufacturers recommendations for using the instrument when performing the test. 6.6 Repeat the procedure on a second test sample and plot the particle size distribution curves. If the curves are similar, it may be deduced that the dispersion is stable and th
39、at no mistake has been made during the test. If the curves are not similar, check the dispersion again (see 4.2). 7 Expression of results Record the suspension and dispersion conditions in a table similar to the example given in Annex C. Present the results either in graphic form as in Annex D, with
40、 the cumulative particle size distribution curve obtained automatically on the measurement sheet of the instrument, specifying test conditions in the appropriate part of the sheet, or as a table of results: a recommended layout example is given in Annex E. 8 Test report The test report shall be in a
41、ccordance 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 unique report identification and page number; d) customer name and address; e) reference to this
42、 standard, i.e. determined in accordance with EN 725-5; f) authorising signature; g) any deviation from the method described, with appropriate validation, i.e. demonstrated to be acceptable to the parties involved; h) description of the test material (manufacturer, type, batch or code number, date o
43、f receipt) including any treatment before testing; i) suspension and dispersion conditions in the form of a table similar to the example given in Annex C; j) reference powder used to calibrate the instrument (see clause 5) and the results obtained on a given date; k) for the sedimentation method onl
44、y, the apparent density of the powder, apparent density and viscosity of the suspending liquid, displacement rate of the cell, temperature of the suspension and the initial diameter; l) comments about the test or test results. Licensed Copy: London South Bank University, London South Bank University
45、, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 7 Annex A (informative) Suspending liquids and dispersing agents The following alphabetical list in Table A.1 gives examples of suspending liquids and dispersing agents most commonly used for the main technical cerami
46、c powders. Surface characteristics, and consequently dispersion behaviour, depend on the powder type, but also on its manufacturing process. Therefore, the suspending liquid and dispersing agent may vary among powders of the same type. Among the dispersing agents listed in the third column of Table
47、A.1, 9 are designated by a number (d.a No. 1 to No 9). Their chemical composition is as follows: d.a. No 1 Dioctylsulfosuccinates; d.a. No 2 Trimethylcetyl ammonium bromide; d.a. No 3 Polyoxyethylene nonylphenol; d.a. No 4 Linear polyethoxy derivates; d.a. No 5 Sodium alkylnaphthalene sulfonate; d.a
48、. No 6 Sorbitol monolaurate; d.a. No 7 Polyoxyethylene alkylphenol; d.a. No 8 Sodium alkylsulfonate; d.a. No 9 Polyoxyethylene octylphenol. Licensed Copy: London South Bank University, London South Bank University, Fri Oct 05 02:49:17 GMT+00:00 2007, Uncontrolled Copy, (c) BSI EN 725-5:2007 (E) 8 Ta
49、ble A.1 - Suspending liquids and dispersing agents Material Suspending liquid Dispersing agent (0,5 g/l to 1,0 g/l, unless otherwise stated) Alumina see aluminium (oxide) Aluminium (oxide) water Sodium pyrophosphate water Sodium pyrophosphate water Sodium tartrate water d.a. No 3 or No 4 or No 5 or No 9 water hydrochloric acid (pH 3) n-butanol n-butylamine linseed oil/xylene iso-octane d.a. No 6 Barium carbonate cyclohexanol, methanol Barium titanate water d.a. No 8 Boron (am
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