ASTM_D_1977_-_22.pdf

Designation:D197722Standard Test Method forNickel and Vanadium in FCC Equilibrium Catalysts byHydrofluoric/Sulfuric Acid Decomposition and AtomicSpectroscopic Analysis1This standard is issued under the fixed designation D1977;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 nickel andvanadium in equilibrium catalysts where the vanadium andnickel concentrations are greater than 50 and 25 mg kg,respectively.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 WaterD3766 Terminology Relating to Catalysts and CatalysisD4481 Test Method for Total Nickel in Fresh Alumina-BaseCatalystsD7442 Practice for Sample Preparation of Fluid CatalyticCracking Catalysts and Zeolites for ElementalAnalysis byInductively Coupled Plasma Optical Emission Spectros-copyE105 Guide for Probability Sampling of MaterialsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE288 Specification for Laboratory Glass Volumetric FlasksE456 Terminology Relating to Quality and StatisticsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 U.S.Federal Specification:3Federal Specification NNN-P-395C Tolerance for Class APipets3.Terminology3.1 DefinitionsSee Terminology D3766.4.Summary of Test Method4.1 The test specimen(as received)is decomposed withhydrofluoric and sulfuric acids.After complete volatilization ofthe hydrofluoric acid and cooling,the sulfate salts are diluted tothe appropriate concentration range for analysis by flameatomic absorption,direct current plasma emission,or induc-tively coupled plasma emission spectroscopies.The instrumentis calibrated with matrix-matched standards.Solutions of thetest specimen are analyzed.5.Significance and Use5.1 This test method is a procedure by which catalystsamples may be compared on an inter-or intra-laboratorybasis.Catalyst producers and user should find this test methodto be of value.6.Interferences6.1 The enhancement of alumina in the samples are over-come by using matrix-matched standards.Any dilutionsneeded to achieve the working ranges for vanadium and nickelmust contain the same Al2O3(7800 ppm)concentration as thestandards.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 D1977 16.DOI:10.1520/D1977-22.2For 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 DLA Document Services,Building 4/D,700 Robbins Ave.,Philadelphia,PA 19111-5094,http:/quicksearch.dla.mil.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.16.2 If using optical emission,consult tables showing inter-fering line near analyte lines;if significant overlap occurs,onemust apply interelement correction or choose an alternateemission line.7.Apparatus7.1 Analytical Balance,capable of weighing to nearest0.1 mg.7.2 Hot Plate,capable of maintaining 250 6 10 C atsurface.7.3 PTFE Fluorocarbon Beaker,250 mL and PTFE watchglass.7.4 Volumetric Flasks,borosilicate glass,50,100,250,500,and 1000 mL capacity conforming to Specification E288.7.5 Pipettes,borosilicate glass,5,10,and 25 mL,conform-ing to Federal Specification NNN-P-395C.7.6 Bottles,polyethylene,100 and 1000 mL.7.7 Laboratory Fume Hood suitable for use with hydroflu-oric acid.8.Reagen