ASTM_D_5153_-_10_2016.pdf

Designation:D515310(Reapproved 2016)Standard Test Method forPalladium in Molecular Sieve Catalyst by AtomicAbsorption1This 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 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:2D1193 Specification for Reagent WaterE177 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 MethodD7442 Practice for Sample Preparation of Fluid CatalyticCracking Catalysts and Zeolites for ElementalAnalysis byInductively Coupled Plasma Atomic Emission Spectros-copy2.2 U.S.Federal Specification:Federal Spec.NNN-P-395C Tolerance for Class A Pipets33.Summary of Test Method3.1 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.5.9 Graduated Cylinder,plastic,10-mL.5.10 Hot Plate.5.11 Muffle Furnace,electrically heated,capable of 1000C.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.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended that1This 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 Jan.1,2016.Published January 2016.Originallyapproved in 1991.Last previous edition approved in 2010 as D515310.DOI:10.1520/D5153-10R16.2For 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 States1 all reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Specification D1193.6.3 Hydrochloric Acid,concentrated,36.538.0 wt.%or 12M,sp gr 1.18.6.4 Hydrofluoric Acid,concentrated,48.051.0 wt.%or28.9 M,sp gr 1.17.NOTE1Refer to Section 8 of Practice D7442-08 for hazards associ-ated with handling of acids.6.5 Nitric Acid,concentrated,69.071.0 wt.%or 15.7 M,spgr 1.41.6.6 Sulfuric Acid,concentrated,95.098.0 wt.%or 18 M,sp gr 1.84.6.7 Aluminum Oxide(Al2O3).6.8 Lanthanum Chloride(LaCl37H2O).6.9 Palladium Wire,99.99%.6.10 Aqua RegiaMix three parts by volume of concen-trated hydrochloric acid(12 M)and one part by volume ofconcentrated nitric acid(15.7 M)immediately before use.6.11 Sulfuric Acid,15.816.3 wt.%or 3M.Cautiously add250 mL of concentr