1、Designation: C690 09 (Reapproved 2014)Standard Test Method forParticle Size Distribution of Alumina or Quartz Powders byElectrical Sensing Zone Technique1This standard is issued under the fixed designation C690; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method, one of several found valuable for themeasurement of partic
3、le size, covers 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 apertur
4、e, and produces individual pulses of ampli-tude proportional to the particle volume.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety problems, if any, associated
5、with its use. It is theresponsibility of the user of this standard to establish 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
6、an electrolyte is placed on the instrumentsample stand. The suspension is 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). Equiv
7、alent spherical diameter iscommonly used to express the particle size. (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 a
8、nd quartz powders for determining particle sizedistributions for materials specifications, manufacturingcontrol, and development and research.4. Apparatus4.1 Electrical Sensing Zone Particle Counter.4.2 Aperture Tubes, diameter ranging from approximately30 to 140 m. The diameter required is dependen
9、t upon theparticle size 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 300 m are usable.4.3 Sample Beaker, capable of maintaining all particlesuniformly in suspension (for example, ro
10、und-bottom).4.4 Blender, 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.5. Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unl
11、ess otherwise indicated, 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.2Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently
12、 high purity to permit its use without lessening theaccuracy of the determination.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 distille
13、d water.NOTE 3This liquid should not be retained longer than 1 month andshould not be pH modified or heated.1This test method is under the jurisdiction ofASTM Committee C21 on CeramicWhitewares and Related Productsand is the direct responsibility of SubcommitteeC21.04 on Raw Materials.Current editio
14、n approved Dec. 1, 2014. Published December 2014. Originallyapproved in 1971. Last previous edition approved in 2009 as C690 09. DOI:10.1520/C0690-09R14.2Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents
15、 notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, VWR International Ltd., U.K., and the United States Pharmacopoeia,USPC, Rockville, MD*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box
16、 C700, West Conshohocken, PA 19428-2959. United States15.3 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 themembrane filtering device.5.5 Calib
17、ration 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 apparatus and obtain particle siz
18、e 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 theinstruction manual. Monosiz
19、ed 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 electrolyte and taking counts without an
20、y 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 or blendershould be predetermi
21、ned 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 Waring Blender may cause size re
22、duction. 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 the ratio of 3 drops/200 mL ofe
23、lectrolyte. 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 sample. Thepipet should delive
24、r 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 maintain a uniform particle suspensi
25、on, 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 measure-ments and report the statist
26、ical 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 factor at least once a week.6.9.3 T
27、he 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 particle size according to instrumen
28、t 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 percent are interchangeable.7.2 Repo
29、rt 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 test method is capable of apreci
30、sion 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 usingNIST or NIST traceable un
31、iform spheres with relative standarddeviation of 5 % or less.9. Keywords9.1 alumina; particle size; quartz; sensing zoneC690 09 (2014)2ANNEX(Mandatory Information)A1. APERTURE CHART AND DISPERSION CURVEFigs. A1.1 and A1.2 are examples of the charts that shouldbe employed in conjunction with this tes
32、t method.SUMMARY OF CHANGESCommittee C21 has identified the location of selected changes to this standard since the last issue (C69003)that may impact the use of this standard.Nominal Aperture Size,mTotal Cumulative Count for 5 %Coincidence CorrectionApproximate ParticleSize Rangein Equivalent Spher
33、i-cal DiameterSuggested Calibra-tionParticlesAManometer 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
34、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 CurveC690 09 (2014)3(1) Instruments are available from
35、multiple suppliers and thusreference to particular instruments in sections 4.1 and 4.8,along with footnotes 2 and 3 must be removed according toASTM policy. All other footnotes are renumbered accordingly.(2) Note 1 is revised to indicate aperture openings up to 300mmay be used, instead of 280m, sinc
36、e 300m are now availablewith performance essentially the same as 280m tubes.(3) The word “Nominal” has been added to the heading for thefirst column in Fig. A1.1 since aperture tubes are available insizes slightly different from those given in the table.ASTM International takes no position respectin
37、g 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 infringement of such rights, are entirely their own responsibility.This standa
38、rd 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 standard or for additional standardsand should be addressed to ASTM Internationa
39、l 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 views known to the ASTM Committee on Standards, at the address shown below.Th
40、is 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 contacting 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 09 (2014)4
