1、Designation: C 690 03Standard Test Method forParticle Size Distribution of Alumina or Quartz Powders byElectrical Sensing Zone Technique1This standard is issued under the fixed designation C 690; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method, one of several found valuable for themeasurement of particle size, covers
3、the determination of theparticle size distribution of alumina or quartz powders (0.6 to56.0 m) using electrical sensing zone particle size analyzers.These instruments use an electric current path of small dimen-sions which is modulated by individual particle passagethrough an aperture, and produces
4、individual pulses of ampli-tude proportional to the particle volume.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of thesafety problems, if any, associated with its use. It is theresponsibility of the user of this standard to es
5、tablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Summary of Test Method2.1 A carefully dispersed, dilute suspension of the powderin a beaker filled with an electrolyte is placed on the instrumentsample stand. The suspension i
6、s forced through a restrictingaperture. Each particle passing generates an electric pulse thatis recorded on an electronic counter.2.2 The instrument response is essentially related to particlevolume (liquid displacement). Equivalent spherical diameter iscommonly used to express the particle size. (
7、Comparisons withother techniques have been found to be good for sphericalparticles; for non-spherical particles results may differ.)3. Significance and Use3.1 This test method is useful to both sellers and purchasersof alumina and quartz powders for determining particle sizedistributions for materia
8、ls specifications, manufacturing con-trol, and development and research.4. Apparatus4.1 Electrical Sensing Zone Particle Counter. CoulterCounter Models MSII, MS IIe, and MS 324.2 Aperture Tubes, diameter ranging from approximately30 to 140 m. The diameter required is dependent upon theparticle size
9、distribution of the sample. Generally any giventube will cover a particle size range from 2 to 60 % of itsaperture diameter.NOTE 1In certain cases, apertures up to 280 m are usable.4.3 Sample Beaker, capable of maintaining all particlesuniformly in suspension (for example, round-bottom).4.4 Blender,
10、 capacity 1-Lglass container.Ameans to controlspeed is required.4.5 Beakers, 100, 500, and 1000-mL.4.6 Pipet.4.7 Wash Bottles.4.8 Membrane Filtering Device, rated at 0.45-m filters orfiner.35. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated
11、, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit
12、its use without lessening theaccuracy of the determination.1This test method is under the jurisdiction ofASTM Committee C21 on CeramicWhitewares and Related Products and is the direct responsibility of SubcommitteeC21.07 on Nonplastics.Current edition approved Oct. 1, 2003. Published November 2003.
13、Originallyapproved in 1971. Last previous edition approved in 1997 as C 690 86 (1997)e1.2The sole source of supply of the apparatus known to the committee at this timeis Beckman Coulter, Inc., Miami, FL 33196. If you are aware of alternativesuppliers, please provide this information to ASTM Internat
14、ional Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee1, which you may attend.3The membrane filters may be the Millipore, Pall metal type, or other equivalent.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemica
15、l Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, VWR International Ltd., U.K., and the United States Pharmacopoeia,USPC, Rockville, MD1Copyright ASTM International, 100 Barr Harbor Drive, P
16、O Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Dispersing MediaTen percent solution of purified orreagent grade sodium hexametaphosphate in distilled watertwice filtered through the membrane filtering device.NOTE 2Deionized water may be substituted for distilled water.NOTE 3This liq
17、uid should not be retained longer than 1 month andshould not be pH modified or heated.5.3 ElectrolyteDissolve 10.0 g of reagent grade sodiumchloride (NaCl) in 1000 mL of distilled water and filter twicethrough the membrane filtering device.5.4 Wash WaterDistilled water twice filtered through thememb
18、rane filtering device.5.5 Calibration ParticlesNIST or NIST traceable mono-sized particle standards.6. Procedure6.1 SummaryDisperse the test powder in the electrolytewith a blender. Transfer a representative portion to the samplebeaker that contains filtered electrolyte. Place sample beaker inthe ap
19、paratus and obtain particle size distribution in a chosensize range. Obtain relative weight fraction by assuming con-stant particle density.6.2 Precalibrate the aperture and electrolyte combinationfollowing the manufacturers instruction manual.NOTE 4Calibration should be performed in accordance with
20、 theinstruction manual. Monosized NIST or NIST traceable calibrationstandards should be selected from Fig. A1.1. Mutual agreement on thesource and size of calibration standards is necessary for interlaboratorycomparisons.6.3 Check background counts by filling the sample beakerwith filtered electroly
21、te and taking counts without any sampleadded. Follow 6.6, 6.7, and 6.8.6.4 Disperse approximately 0.7 g of sample in 200 mL ofelectrolyte containing 5 drops of dispersing media, by mixingat high speed on the blender or its equivalent for 5 min.NOTE 5The proper dispersion conditions for a given mixer
22、 or blendershould be predetermined by obtaining a time-speed versus mediandiameter curve (see typical curve in Fig. A1.2) while ensuring thatgrinding does not occur. The position of the plateau will indicate theproper dispersion conditions for the sample. Experience has shown thatfull speed on the W
23、aring Blender may cause size reduction. Slightly lessthan full speed should be used. For some suspensions ultrasonic treatmentfrom 1 to 5 min is effective.6.5 With a pipet, transfer an appropriate aliquot of dispersedsample into the sample beaker containing electrolyte withdispersing media added in
24、the ratio of 3 drops/200 mL ofelectrolyte. The aliquot size is dependent on the aperture sizeused. Wash down the pipet by rinsing with electrolyte severaltimes (see 6.9.3).NOTE 6The blender or mixer should be stirring just rapidly enough tomaintain a uniform particle suspension while withdrawing the
25、 sample. Thepipet should deliver all of the withdrawn slurry to ensure a representativetransfer of sample in the event of any size classification during thetransfer.6.6 Place the sample beaker in position on the sample stand.6.7 Adjust the speed of the stirrer to furnish sufficientagitation to maint
26、ain a uniform particle suspension, but belowair bubble generation speeds.6.8 Use the apparatus control software to set the measure-ment parameters. Make three measurements in which eachmeasurement counts and measures at least 5000 particles.Average the particle size distribution from the three measu
27、re-ments and report the statistical parameters from the averagedresults.6.9 Precautions:6.9.1 Before each analysis, using wash bottle and filteredwash water, wash all surfaces coming in contact with sample.6.9.2 Ensure that the calibration of the instrument is correctby checking the calibration fact
28、or at least once a week.6.9.3 The number of particles per unit volume in the samplebeaker should not exceed that which will give a 5 % coinci-dence correction for the aperture tube being used (see Fig.A1.1).7. Presentation of Data7.1 Convert data to cumulative weight percent greater thanstated parti
29、cle size according to instrument instruction manual.Coincidence is insignificant if total counts are limited to Fig.A1.1.NOTE 7For all electrical sensing zone counters the conversion isactually to volume percent. If all particles in the sample have the samedensity the volume percent and weight perce
30、nt are interchangeable.7.2 Report size distribution graphs, tables, and statisticssuch as: weight percent, count percent, volume percent, mean,median, mode, quartiles, and standard deviation.8. Precision and Bias8.1 Intralaboratory, Same OperatorExperience of severallaboratories indicates that the t
31、est method is capable of aprecision of 61 % (95 % confidence level) for all size values.8.2 InterlaboratoryExperience of several laboratories in-dicates that the test method is capable of a precision of 63%(95 % confidence level) for all size values.8.3 BiasInstrument calibrations shall be performed
32、 usingNIST or NIST traceable uniform spheres with relative standarddeviation of 5 % or less.9. Keywords9.1 alumina; particle size; quartz; sensing zoneC690032ANNEX(Mandatory Information)A1. APERTURE CHART AND DISPERSION CURVEFigs.A1.1 andA1.2 are examples of the charts that should beemployed in conj
33、unction with this test method.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof in
34、fringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this stan
35、dard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your v
36、iews known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contac
37、ting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).Aperture Size,mTotal Cumulative Count for 5 %Coincidence CorrectionApproximate Particle Size Rangein Equivalent Spherical DiameterSuggested Calibration
38、ParticlesAManometer Volumem Diameter, m50 L 500 L 2000 L30 74 100AA0.6 to 12.0 1.5 to 6.050 15 950 159 500A1.0 to 20.0 2.5 to 10.070 5 810 58 100 232 400 1.4 to 28.0 3.5 to 14.0100 2 000 20 000 80 000 2.0 to 40.0 5.0 to 20.0140 725 7 250 29 000 2.8 to 56.0 7.0 to 28.0200280AA2500A10 0003 6304.0 to 80.05.6 to 112.010.0 to 40.014.0 to 56.0AAperture size and manometer volume combination not recommended.FIG. A1.1 Typical Aperture ChartBlender Dispersion Time (Minutes)FIG. A1.2 Example of a Sample Dispersion CurveC690033
