ASTM_D_7442_-_22.pdf

Designation:D744222Standard Practice forSample Preparation of Fluid Catalytic Cracking Catalysts,Catalytic Materials,and Zeolites for Elemental Analysis byInductively Coupled Plasma Optical EmissionSpectroscopy1This standard is issued under the fixed designation D7442;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.Scope*1.1 This practice covers uniform dissolution techniques forpreparing samples of fluid catalytic cracking catalysts(FCC)and exchanged zeolitic materials for analysis by InductivelyCoupled Plasma Optical Emission Spectroscopy(ICP-OES).These techniques describe standardized approaches to well-known,widely used laboratory practices of sample preparationutilizing acid digestions and borate salt fusions.This practice isapplicable to fresh and equilibrium FCC catalysts,catalyticmaterials used to manufacture catalyst,and exchanged zeolitematerials.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:2D3766 Terminology Relating to Catalysts and CatalysisD7260 Practice for Optimization,Calibration,and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry(ICP-AES)for Elemental Analysis of Petro-leum Products and LubricantsE1272 Specification for Laboratory Glass Graduated Cylin-ders3.Terminology3.1 Acronyms:As per Terminology D3766.3.1.1 FCCFluid Catalytic Cracking3.1.2 FCCUFluid Catalytic Cracking Unit3.1.3 ICP-OESInductively-CoupledPlasma-OpticalEmission Spectroscopy4.Summary of Practice4.1 Three preparation techniques are presented for convert-ing solid,power samples into clear,dilute acid solutionssuitable for analysis by ICP-OES.The three techniques pre-sented are Perchloric Acid Digestion,Sulfuric Acid Digestion,and Lithium-Borate Fused Dissolution.Other techniques maybe possible;however,these three approaches are established,widely used laboratory techniques for preparing FCC catalystand catalytic materials.4.2 Powder samples are heat-treated for 1 to 3 h to removevolatile components prior to further preparation by any of thesethree techniques.4.3 The Perchloric Acid and Sulfuric Acid techniques in-volve dissolving small aliquots of heat-treated sample in therespective acid liquors and diluting the resulting solutions tothe appropriate analytical volume.These techniques requireboiling acid solutions in platinum or polytetrafluoroethylene(PTFE)labware and shall be used in appropriate fume hoods.The PerchloricAcid Digestion shall never be used in a standardfume hood.4.4The Lithium Borate Fused Dissolution technique in-volves dissolving small aliquots of heat-treated sample in amolten flux of lithium metaborate and lithium tetraborate salts,dissolving the resulting flux solution in a dilute nitric acidsolution,and diluting the clear,concentrated specimen solution1This practice is under the jurisdiction of ASTM Committee D32 on Catalystsand is the direct responsibility of Subcommittee D32.03 on Chemical Composition.Current edition approved Aug.1,2022.Published August 2022.Originallyapproved in 2008.Last previous edition approved in 2016 as D7442 16.DOI:10.1520/D7442-22.2For 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.*A Summary of Changes section appears at the end of this standardCopyright 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.1to an appropriate analytical volume.This technique must beperformed in an operational fume hood and can be performedmanually or may utilize the advantages of an automated fluxer.The optimal ratio of flux to sample,as well as fusiontemperature needed,