ASTM_D_1977_-_03.pdf

Designation:D 1977 03Standard Test Method forNickel and Vanadium in FCC Equilibrium Catalysts byHydrofluoric/Sulfuric Acid Decomposition and AtomicSpectroscopic Analysis1This standard is issued under the fixed designation D 1977;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(e)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 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.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:2D 1193 Specification for Reagent WaterD 3766 Terminology Relating to Catalysts and CatalysisE 105 Practice for Probability Sampling of MaterialsE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 288 Specification for Laboratory Glass Volumetric FlasksE 456 Terminology Relating to Quality and StatisticsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2U.S.Federal SpecificationFederal Spec NNN-P-395C Tolerance for Class A Pipets33.Terminology3.1 DefinitionsSee Terminology D 3766.4.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.6.2 If using optical emission,consult tables showing inter-fering line near analyte lines;if significant overlap occurs,onemust apply inter-element correction or choose an alternateemission line.7.Apparatus7.1 Analytical Balance,capable of weighing to nearest 0.1mg.7.2 Hot Plate,capable of maintaining 250 6 10C atsurface.7.3 TFE Fluorocarbon Beaker,250 mL.7.4 Volumetric Flasks,borosilicate glass,50,100,250,500,and 1000-mL capacity conforming to Specification E 288.1This 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 Oct.1,2003.Published October 2003.Originallyapproved in 1991.Last previous edition approved in 1998 as D 197798.2For 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,Bldg.4 Section D,700Robbins Ave.,Philadelphia,PA 19111-5094,Attn:NPODS.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.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.8.Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientpurity to permit its use without lessening the accuracy of thedetermination.8.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean type IV reagent water,asdefined in Specification D 1193.8.3 Required Reagents:8.3.1 Hydrofluoric Acid(HF),concentrated,48%.8.3.2 Sulfuric Acid,(H2SO4),concentrated,98%.8.3.3 Sulfuric Acid,49 volume%,add slowly,while stirring,one part of concentrated H2SO4(98%)to one part of water,then cool.8.3.4 Hydrochloric Acid,concentrated,38%.8.3.5 Hydrochloric Acid,19 volume%,add slowly,whilestirring,one part of concentrated HCl(38%)to one part ofwater,the