ASTM_D_4699_-_03_2013.pdf

Designation:D469903(Reapproved 2013)Standard 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 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.Scope1.1 This test method covers the determination 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 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 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.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 Terminology 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 particles 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 Graduated 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 Pour 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 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 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 weigh-ing.Weigh the sample to the nearest tenth of a gram,WH.NOTE1The conditions may not be appropriate for all materials.NOTE2Since many catalyst formulations are strong adsorbents,theuse of a 4A indicating(cobalt-treated)molecular sieve as a desiccating1This 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 March 1,2013.Published March 2013.Originallyapproved in 1987.Last previous edition approved in 2008 as D469903(2008).DOI:10.1520/D4699-03R13.2For 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 source 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 comments will receive careful consideration at a meeting of the responsibletechnical committee1,which you may attend.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 medium is recommended.The desiccant should be regenerated at 220 to260C,as required.NOTE3Multiple 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 specimen 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 completed,read the packed volume,V,to the nearest 1 mL by estimating the av