1、Designation: C1730 17Standard Test Method forParticle Size Distribution of Advanced Ceramics by X-RayMonitoring of Gravity Sedimentation1This standard is issued under the fixed designation C1730; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of particlesize distribution of advanced ceramic po
3、wders. Experience hasshown that this test method is satisfactory for the analysis ofsilicon carbide, silicon nitride, and zirconium oxide in the sizerange of 0.1 up to 50 m.1.1.1 However, the relationship between size and sedimen-tation velocity used in this test method assumes that particlessedimen
4、t within the laminar flow regime. It is generallyaccepted that particles sedimenting with a Reynolds number of0.3 or less will do so under conditions of laminar flow withnegligible error. Particle size distribution analysis for particlessettling with a larger Reynolds number may be incorrect due tot
5、urbulent flow. Some materials covered by this test methodmay settle in water with a Reynolds number greater than 0.3 iflarge particles are present. The user of this test method shouldcalculate the Reynolds number of the largest particle expectedto be present in order to judge the quality of obtained
6、 results.Reynolds number (Re) can be calculated using the followingequation:Re 5D3 2 0!0g182(1)where:D = the diameter of the largest particle expected to bepresent, in cm, = the particle density, in g/cm3,0= the suspending liquid density, in g/cm3,g = the acceleration due to gravity, 981 cm/sec2, an
7、d = the suspending liquid viscosity, in poise.1.1.2 A table of the largest particles that can be analyzedwith a suggested maximum Reynolds number of 0.3 or less inwater at 35 C is given for a number of materials in Table 1.Acolumn of the Reynolds number calculated for a 50-m particlesedimenting in t
8、he same liquid system is also given for eachmaterial. Larger particles can be analyzed in dispersing mediawith viscosities greater than that for water. Aqueous solutionsof glycerine or sucrose have such higher viscosities.1.2 The procedure described in this test method may beapplied successfully to
9、other ceramic powders in this generalsize range, provided that appropriate dispersion procedures aredeveloped. It is the responsibility of the user to determine theapplicability of this test method to other materials. Notehowever that some ceramics, such as boron carbide and boronnitride, may not ab
10、sorb X-rays sufficiently to be characterizedby this analysis method.1.3 The values stated in cgs units are to be regarded as thestandard, which is the long-standing industry practice. Thevalues given in parentheses are for information only.1.4 This standard does not purport to address all of thesafe
11、ty concerns, if any, associated 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. Specific hazardinformation is given in Section 8.1.5 This international st
12、andard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2.
13、 Referenced Documents2.1 ASTM Standards:2C1145 Terminology of Advanced CeramicsE1617 Practice for Reporting Particle Size CharacterizationData3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology C1145.1This test method is under the jurisdiction of ASTM Committee C
14、28 onAdvanced Ceramics and is the direct responsibility of Subcommittee C28.03 onPhysical Properties and Non-Destructive Evaluation.Current edition approved July 1, 2017. Published July 2017. Originally approvedin 2017. DOI: 10.1520/C1730-17.2For referenced ASTM standards, visit the ASTM website, ww
15、w.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis i
16、nternational standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT)
17、 Committee.14. Summary of Test Method4.1 A carefully dispersed homogeneous suspension of thepowder is permitted to settle in a cell scanned by a collimatedX-ray beam of constant intensity. The net X-ray signal isinversely proportional to the sample concentration in thedispersing medium, and the part
18、icle diameter is related to theposition of the X-ray beam relative to the top of the cell.Cumulative mass percent versus equivalent spherical diameterare recorded to yield a particle size distribution curve.5. Significance and Use5.1 This test method is useful to both suppliers and users ofpowders,
19、as outlined in 1.1 and 1.2, in determining particle sizedistribution for product specifications, manufacturing control,development, and research.5.2 Users should be aware that sample concentrations usedin this test method may not be what are considered ideal bysome authorities, and that the range of
20、 this test method extendsinto the region where Brownian movement could be a factor inconventional sedimentation. Within the range of this testmethod, neither the sample concentration nor Brownian move-ment is believed to be significant. Standard reference materialstraceable to national standards, of
21、 chemical composition spe-cifically covered by this test method, are available from NIST,3and perhaps other suppliers.5.3 Reported particle size measurement is a function of theactual particle dimension and shape factor as well as theparticular physical or chemical properties being measured.Caution
22、is required when comparing data from instrumentsoperating on different physical or chemical parameters or withdifferent particle size measurement ranges. Sample acquisition,handling, and preparation can also affect reported particle sizeresults.5.4 Suppliers and users of data obtained using this tes
23、tmethod need to agree upon the suitability of these data toprovide specification for and allow performance prediction ofthe materials analyzed.6. Apparatus6.1 X-Ray Gravitational Sedimentation Particle SizeAnalyzerThe analyzer shall utilize extinction of collimatedX-rays to determine particle mass c
24、oncentration as a homoge-neous dispersion of sample sediments under the influence ofgravity.46.2 Ultrasonic Probe, consisting of a 200 to 300 W powerunit, ultrasonic transducer, and 13-mm (12-in.) diameter probe.6.3 Balance, top-loading, accurate to 100 6 0.1 g.6.4 Stirrer, magnetic, with 19-mm (34-
25、in.) stirrer bar.7. Reagents and Materials7.1 Purity of ReagentsReagent-grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specification
26、s are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Typical Dispersing MediaDissolve 5.0 g of sodiumhexametaphosphate (NaPO3)6 in 1000 mL of distilled ordeio
27、nized water. Alternately, dissolve 5.0 g Darvan C6(ammo-nium salt of polymethacrylic acid) in 95 mL of distilled ordeionized water. This latter solution is typically used afterdilution of 0.03 g per 20 mL of distilled or deionized water.7.3 pH AdjustersFresh ammonium hydroxide (NH4OH) at5 to 10 weig
28、ht % strength is a common reagent used to raisepH, while fresh nitric acid (HNO3) at 5 to 10 weight % strengthis a common reagent to lower pH.7.4 Cleaning SolutionPrepare a 0.1 % solution by volumeof Triton X-100 using distilled or deionized water,7or othersuitable laboratory cleaning solution.3Nati
29、onal Institute of Standards and Technology (NIST), 100 Bureau Dr., Stop2300, Gaithersburg, MD 20899-2300, http:/www.nist.gov.4The sole instrument of this type known to the committee at this time is theSediGraph X-ray gravity sedimentation particle size analyzer, available fromMicromeritics Instrumen
30、t Corporation, 4356 Communications Drive, Norcross, GA30093. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.5Reag
31、ent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand
32、 National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.6Darvan C is a trademarked product of R.T. Vanderbilt Company, Inc., Norwalk,CT 06856-5150.7Triton X-100 is a trademarked product of Rohm gravity sedimentation; particle sizedistribution; silicon carbide; silicon nitride;
33、zirconium oxideASTM 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 infringement of s
34、uch 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 standard or for add
35、itional 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 views known to t
36、he 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 contacting ASTM at th
37、e 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:/ by special request from the NIST Research Library via the NISTwebsite at www.nist.org.C1730 174
