1、Designation: D4699 03 (Reapproved 2018)1Standard Test Method forVibratory Packing Density of Large Formed Catalyst andCatalyst Carrier Particles1This standard is issued under the fixed designation D4699; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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.1NOTEKeywords updated editorially in May 2018.1. Scope1.1 This test method covers the determinati
3、on of the vibra-tory packing density of formed 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.1.2 The values stated in SI unit
4、s 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 concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and env
5、ironmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Stand
6、ards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D3766 Terminology Relating to Catalysts and CatalysisE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE456 Terminolog
7、y Relating to Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 DefinitionsSee Terminology D3766.4. Summary of Test Method4.1 A known sample of environmentally equilibratedformed catalyst or catalyst carrier partic
8、les is vibrated in agraduated cylinder. The vibratory packing density 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 Gra
9、duated Cylinder, capacity 2000-mL.6.2 Vibratory Plate.36.3 Desiccator, 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 P
10、our between 1000 to 2000 mL of the test specimencarefully into a tared 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 for1This test method is under the jurisdiction of ASTM Committee D32
11、onCatalysts and is the direct responsibility of Subcommittee D32.02 on Physical-Mechanical Properties.Current edition approved May 1, 2018. Published June 2018. Originallyapproved in 1987. Last previous edition approved in 2013 as D469903(2013).DOI: 10.1520/D4699-03R18.2For referenced ASTM standards
12、, 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 source of supply of the Syntron Vibrating Machine, Model V-2-B withPower Pulse Co
13、ntroller, 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 comments will receive careful consideration at a meeting of the responsibletec
14、hnical committee1, which you may attend.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision o
15、n Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1moisture loss. Heat this sample at 400 6 15C for not less than3 h. Normally, this treatment can take place in air; however, inthe
16、 case of 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 we
17、igh-ing. 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 sho
18、uld be regenerated at 220 to260C, as required.NOTE 3Multiple samples can be pretreated but must be desiccatedprior 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 spec
19、imen carefullyinto the graduated cylinder using a funnel. The entire transfertime should be between 90 and 120 s. 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
20、 completed, read the packed volume,V, to the nearest 1 mL by estimating the average level of thecatalyst surface 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 dryi
21、ng, g8.2 Calculate the vibratory packing density as follows:VPD 51 2 L!WV(2)where:VPD = vibratory packing density, g/mL,W = mass of equilibrated catalyst particles, g, andV = volume occupied by particles in measuring cylinder,mL.8.3 Report the average of two or more runs.9. Precision and Bias49.1 Te
22、st ProgramAn interlaboratory study was conductedin which the named property was measured in three separatetest materials in four separate laboratories. Practice E691,modified for non-uniform data sets, was followed for the datareduction. Analysis details are in the research report.9.2 PrecisionPairs
23、 of test results obtained by the proce-dure described in the method are expected to differ in absolutevalue by 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 gi
24、ven in Terminology E456 and Practice E177,respectively.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D32-1022.FIG. 1 Example of Components of Vibratory Stand for Large Diameter PelletsD4699 03 (2018)12Test Result(ConsensusMean
25、) g/mL95 % Repeatability Limit(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
26、because the value of the vibratorypacking density can be defined only in terms of the testmethods.10. Keywords10.1 catalyst; large; packing density; vibratoryASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standa
27、rd. 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 standard is subject to revision at any time by the responsible technical committee and must be reviewe
28、d 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 International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible
29、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.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consh
30、ohocken, 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:/ 03 (2018)13
