ASTM_D_4164_-_13.pdf

Designation:D416413Standard Test Method forMechanically Tapped Packing Density of Formed Catalystand Catalyst Carriers1This standard is issued under the fixed designation D4164;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 me-chanically tapped density of formed catalyst and catalystcarriers.For the purpose of this test method,catalyst particlesare defined as extrudates,spheres,or formed pellets of 0.8 to4.8-mm(132to316-in.)nominal diameter.1.2 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 MethodE1272 Specification for Laboratory Glass Graduated Cylin-ders3.Terminology3.1 DefinitionsSee Terminology D3766.4.Summary of Test Method4.1 A preconditioned sample of formed catalyst or catalystcarrier is tapped in a graduated cylinder.The mechanicallytapped packing density is determined from the known mass andtapped volume.5.Significance and Use5.1 This test method is to be used for measuring themechanically tapped packing density of formed particles thatwill not break up during sampling,filling,or tapping of themeasuring cylinder under test conditions.6.Apparatus6.1 Graduated Cylinder,capacity 250 mL,conforming toSpecification E1272,Class A,with a base designed to accom-modate the cylinder holder.6.2 Cylinder Holder,weighing approximately 1 lb(454 g).6.3 Tapping Device,consisting of a base-plate with wormdrive,reduction ratio 15:1,nominal cam shaft speed of 250r/min,tapping stroke travel18in.(3.2 mm).6.4 Four Digit Adjustable Counter,which can be preset todeliver any number of taps between 1 and 9999.6.5 Desiccator,with a desiccant grade molecular sieve suchas No.4A.6.6 Balance having a sensitivity of 0.1 g.6.7 Drying Oven.7.Procedure7.1 Heat an adequate sample(s)at 400 6 15C for not lessthan 3 h.Normally,this treatment can take place in air.However,in the case of materials that might react with air atelevated temperatures(such as prereduced catalysts)the heattreatment should take place in an inert atmosphere.Afterheating,cool the test sample(s)in a desiccator or other suitablecontainer to eliminate the possibility of moisture adsorptionprior to testing.NOTE1These conditions may not be appropriate for all materials.NOTE2Since many catalyst formulations are strong adsorbents,theuse of No.4Aindicating(cobalt-treated)molecular sieves as a desiccatingmedium is suggested.The desiccant should be regenerated at 493 K(220C)to 533 K(260C),as required.7.2 Pour between 240 and 250 mL of the test specimencarefully into the tared graduated cylinder using a funnel.Toensure proper level,rotate the funnel while pouring the testspecimen.Weigh immediately to the nearest 0.1 g.7.3 Preset the counter to 1000 taps.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 Dec.1,2013.Published December 2013.Originallyapproved in 1988.Last previous edition approved in 2008 as D4164 03(2008).DOI:10.1520/D4164-13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.4 Start the tapping device.7.5 When tapping is completed,read the tapped volume,V,to the nearest 1 mL by estimating the average level of thecatalyst or catalyst carrier surface in the cylinder.8.Calculation8.1 Calculate mechanically tapped packing density MTD asfollows:MTD5 W/V(1)where:W=mass of catalyst particles,g,andV=volume occupied by particles in measuring cylinder,mL.9.Precision and Bias39.1 Test ProgramAn interlaboratory study was conductedin which the named property was measured in two separate testmaterials in three separate laboratories.Practice E691,modi-fied for non-uniform data sets,was followed for the datareduction.9.2 PrecisionPairs of test results obtained by a proceduresimilar to that described in the study are expected to differ inabsolute value by less than 2.772 S,where 2.772 S is the 95%probability interval