ASTM_D_5153_-_22.pdf

Designation:D515322Standard Test Method forPalladium in Molecular Sieve Catalyst by Atomic AbsorptionSpectrophotometry1This standard is issued under the fixed designation D5153;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 palladiumin molecular sieve-containing fresh catalysts with about 0.5weight%of palladium.1.2 UnitsThe values stated in SI units are to be regardedas standard.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 environmental 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 Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD7442 Practice for Sample Preparation of Fluid CatalyticCracking Catalysts and Zeolites for ElementalAnalysis byInductively Coupled Plasma Optical Emission Spectros-copyE177 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-ders2.2 U.S.Federal Specification:3Federal Spec.NNN-P-395C Tolerance for Class A Pipets3.Summary of Test Method3.1 WarningThis test method requires the use of anextremely hazardous substance,hydrofluoric acid.Please referto Appendix X1 and Appendix X2 for additional safetyrequirements.3.2 The test sample is treated with a mixture of sulfuric andhydrofluoric acids.Upon dissolution,the excess hydrofluoricacid is expelled.Aqua regia and lanthanum chloride are addedand the solution is diluted to a specific volume.Palladiumconcentration is determined by atomic absorption spectropho-tometry.Absorbance of the samples is bracketed using a set ofnarrow range,matrix matched standards.A second sample,taken at the same time as the analysis sample,is used todetermine loss on ignition.4.Significance and Use4.1 This test method provides a means of determining thepalladium content in fresh catalysts containing molecularsieves.4.2 This test method is not intended to cover samplescontaining precious metals other than palladium.5.Apparatus5.1 Analytical Balance,capable of weighing to nearest0.1 mg.5.2 Atomic Absorption Spectrophotometer.5.3 Beakers,TFE-fluorocarbon,100 mL.5.4 Crucibles,porcelain,10 mL.5.5 Crucible Cover,porcelain,for 10 mL crucible.5.6 Desiccator.5.7 Flasks,Erlenmeyer,2000 mL.5.8 Graduated Cylinders,glass,5 mL,10 mL,25 mL,50 mL,250 mL,500 mL,1000 mL(see Specification E1272).1This test method is under the jurisdiction of ASTM Committee D32 onCatalysts and is the direct responsibility of Subcommittee D32.03 on ChemicalComposition.Current edition approved Aug.1,2022.Published August 2022.Originallyapproved in 1991.Last previous edition approved in 2016 as D5153 10(2016).DOI:10.1520/D5153-22.2For 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.3Available from Standardization Documents Order Desk,DODSSP,Bldg.4,Section D,700 Robbins Ave.,Philadelphia,PA 19111-5098.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 on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.15.9 Graduated Cylinder,plastic,10 mL.5.10 Hot Plate.5.11 Muffle Furnace,electrically heated,capable of1000 C.5.12 Pipets,4 mL,6 mL,8 mL,10 mL.5.13 Volumetric Flasks,100 mL,500 mL.5.14 Watch Glasses,TFE-fluorocarbon,for 100 mL beaker.5.15 Weighing Papers.5.16 Fume Hood suitable for use with hydrofluoric acid.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other gr