ASTM_D_7442_-_16.pdf

Designation:D744216Standard Practice forSample Preparation of Fluid Catalytic Cracking Catalystsand Zeolites for Elemental Analysis by Inductively CoupledPlasma Optical Emission Spectroscopy1This 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 and ex-changed zeolite materials.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:2D7260 Practice for Optimization,Calibration,and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry(ICP-AES)for Elemental Analysis of Petro-leum Products and Lubricants3.Terminology3.1 Acronyms: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 catalyst-like samples.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 solutionto 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,will vary depending on sample matrix.5.Significance and Use5.1 The chemical composition of catalyst and catalyst ma-terials is an important indicator of catalyst performance and isa valuable tool for assessing parameters in a FCCU process.This practice will be useful to catalyst manufacturers andpetroleum refiners for quality verification and performance1This 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 March 1,2016.Published April 2016.Originallyapproved in 2008.Last previous edition approved in 2008 as D744208a.DOI:10.1520/D7442-16.2For 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 States1 evaluation,and to environmental authorities at the state andfederal levels for evaluation and verification of various com-pliance programs.3,4,55.2 Catalysts and catalyst type materials are difficult toprepare for analysis by ICP,and although the techniquespresented in this practice are common,there is wide variationamong laboratories in sample pretreatment and digestionrecipes.This practice is intended to standardize these variablesin order to facilitate the utility of comparative data amongm