1、Designation: D 4699 03 (Reapproved 2008)Standard Test Method forVibratory Packing Density of Large Formed Catalyst andCatalyst Carrier Particles1This standard is issued under the fixed designation D 4699; the number immediately following the designation indicates the year oforiginal adoption or, in
2、the case 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 covers the determination of the vibra-tory packing density of form
3、ed catalyst and catalyst carrierparticles that will not break up significantly under test condi-tions. For the purpose of this test, catalyst particles are definedas extrudates, spheres or formed pellets greater than 4.8 mm(316 in.).1.2 The values stated in SI units are to be regarded as thestandard
4、. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety 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-bil
5、ity of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 3766 Terminology Relating to Catalysts and CatalysisE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 456 Terminology Relating to Quality and StatisticsE 691 Practice for Conducting an I
6、nterlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 DefinitionsSee Terminology D 3766.4. Summary of Test Method4.1 A known sample of environmentally equilibratedformed catalyst or catalyst carrier particles is vibrated in agraduated cylinder. The vibratory packing densit
7、y is deter-mined for a specified drying condition.5. Significance and Use5.1 This test method is used for measuring the vibratorypacking density of formed particles used in fixed bed reactors,driers, and so forth.6. Apparatus6.1 Graduated Cylinder, capacity 2000-mL.6.2 Vibratory Plate.36.3 Desiccato
8、r, with a desiccant grade molecular sieve suchas 4A.6.4 Balance having a sensitivity of 1.0 g.6.5 Balance having a sensitivity of 0.1 g.6.6 Drying Oven.7. Procedure7.1 Equilibrate test sample to laboratory environment for 4h.7.2 Pour between 1000 to 2000 mL of the test specimencarefully into a tared
9、 beaker and weigh to the nearest 1 g.Record as W.7.3 Separately weigh to the nearest tenth of a gram about100 g of additional test sample, WI, that will be used formoisture loss. Heat this sample at 400 6 15C for not less than3 h. Normally, this treatment can take place in air; however, inthe case o
10、f materials that might react with air at elevatedtemperature (such as prereduced catalysts) the heat treatmentshould take place in an inert atmosphere. After heating, coolthe test sample in a desiccator or other suitable container toeliminate the possibility of moisture adsorption prior to weigh-ing
11、. Weigh the sample to the nearest tenth of a gram, WH.NOTE 1The conditions may not be appropriate for all materials.NOTE 2Since many catalyst formulations are strong adsorbents, theuse of a 4A indicating (cobalt-treated) molecular sieve as a desiccatingmedium is recommended. The desiccant should be
12、regenerated at 220 to260C, as required.1This test method is under the jurisdiction of ASTM Committee D32 onCatalysts and is the direct responsibility of Subcommittee D32.02 on Physical-Mechanical Properties.Current edition approved April 1, 2008. Published April 2008. Originallyapproved in 1987. Las
13、t previous edition approved in 2003 as D 469903.2For referenced ASTM standards, visit the ASTM website, www.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.3The sole sou
14、rce of supply of the Syntron Vibrating Machine, Model V-2-B withPower Pulse Controller, known to the committee at this time is FMC Technologies,57 Cooper Ave., Homer City, PA 157489234. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Your
15、comments will receive careful consideration at a meeting of the responsibletechnical committee1, which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 3Multiple samples can be pretreated but must be desiccatedprio
16、r to analysis.7.4 Clamp the cylinder to the vibratory plate (see exampleFig. 1).7.5 Start vibrator at a setting at the midpoint of the rheostatrange and pour the 1000 to 2000-mL test specimen carefullyinto the graduated cylinder using a funnel. The entire transfertime should be between 90 and 120 s.
17、 Those vibrating platemachines that operate at a frequency other than 60 Hz willrequire appropriate adjustment of the vibrating time.7.6 Continue vibrating for 5 min.7.7 When vibration is completed, read the packed volume,V, to the nearest 1 mL by estimating the average level of thecatalyst surface
18、in the cylinder.8. Calculation8.1 Calculate the moisture loss as follows:L 5 WI2 WH!/WI(1)where:L = mass fraction moisture loss,WI= initial mass prior to drying, g, andWH= mass after drying, g8.2 Calculate the vibratory packing density as follows:VPD 51 2 L!WV(2)where:VPD = vibratory packing density
19、, g/mL,W = mass of equilibrated catalyst particles, g, andV = volume occupied by particles in measuring cylin-der, mL.8.3 Report the average of two or more runs.9. Precision and Bias49.1 Test ProgramAn interlaboratory study was conductedin which the named property was measured in three separatetest
20、materials in four separate laboratories. Practice E 691,modified for non-uniform data sets, was followed for the datareduction. Analysis details are in the research report.9.2 PrecisionPairs of test results obtained by the proce-dure described in the method are expected to differ in absolutevalue by
21、 less than 2.772 S, where 2.772 S is the 95 %probability limit on the difference between two test results, andS is the appropriate estimate of standard deviation. Definitionsand usage are given in Terminology E 456 and Practice E 177,respectively.Test Result(ConsensusMean) g/mL95 % Repeatability Lim
22、it(Within Laboratory),g/mL (% of mean)95 % ReproducibilityLimit(Between Laboratories)g/mL (% of mean)1.308 0.029 (2.2) 0.093 (7.1)0.998 0.004 (0.4) 0.058 (5.8)0.829 0.011 (1.3) 0.091 (11.0)9.3 BiasThe procedure described for measuring vibratorypacking density has no bias because the value of the vib
23、ratorypacking density can be defined only in terms of the testmethods.10. Keywords10.1 catalyst; large; packing density; vibratory4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D321022.FIG. 1 Example of Components of Vibratory
24、 Stand for Large Diameter PelletsD 4699 03 (2008)2ASTM 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 right
25、s, and the riskof infringement 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 r
26、evision of this standard 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 y
27、ou shouldmake your views 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 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).D 4699 03 (2008)3
