ASTM_D_4481_-_10.pdf

Designation:D448110Standard Test Method forTotal Nickel in Fresh Alumina-Base Catalysts1This standard is issued under the fixed designation D4481;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 infresh alumina-base catalysts and has been tested at nickelconcentrations from 2.5 to 60 weight%,expressed as nickeloxide(NiO).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 its use.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD7442 Practice for Sample Preparation of Fluid CatalyticCracking Catalysts and Zeolites for ElementalAnalysis byInductively Coupled Plasma Atomic Emission Spectros-copyE105 Practice for Probability Sampling of MaterialsE177 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 Method3.Summary of Test Method3.1 The test specimen(as received)is treated with concen-trated hydrochloric acid to solubilize the nickel.If necessary,nickel is recovered from any insoluble residue by potassiumpyrosulfate fusion,after hydrofluoric-sulfuric acid treatment toremove silica.Ammonium citrate is added to complex thealuminum and buffer the solution.Nickel is precipitated asnickel dimethylglyoxime,Ni(C4H7O2N2)2,at a weakly alka-line pH.The precipitate is washed and weighed as Ni(C4H7O2N2)2after drying at 120C.3.2 A separate test specimen is taken to determine loss onignition(LOI)at 550C.The value is used to calculate thenickel as percent nickel oxide(NiO)on a 550C dry basis.4.Significance and Use4.1 This test method sets forth a procedure by whichcatalyst samples can be compared either on an interlaboratoryor intralaboratory basis.It is anticipated that catalyst producersand users will find this method of value.5.Interferences5.1 Cobalt,molybdenum,and aluminum do not interfere.Interferences by elements that precipitate as hydroxides,suchas iron,chromium,aluminum,lead,tin,manganese,titanium,and zirconium,are avoided by the addition of ammoniumcitrate before making the solutions ammoniacal.Copper,pres-ent in the 2 to 10%range,tends to be co-precipitated with thenickel dimethylglyoxime.The only other metal ions precipi-tated by dimethylglyoxime are palladium,gold,and bismuth.6.Apparatus6.1 Beakers,600-mL,150-mL.6.2 Hotplate.6.3 Furnace,electric muffle.Calibrated and capable ofmaintaining temperatures of 550 6 25C,and 950 6 25C.6.4 Platinum Dishes,100-mL3capacity.6.5 Mortar and Pestle,agate,or equivalent mechanicalgrinder.6.6 Crucibles,sintered-glass,30-mL,medium porosity frit.6.7 Fiberglass Filter,3.2 cm.6.8 Drying Oven capable of maintaining a temperature of120C.6.9 Vacuum Filtering Flask,500-mL.6.10 Filter Holder and Filter Disk,Millipore 0.65 m-47-mm diameter.6.11 pH Paper to detect a value of 9.1This test method is under the jurisdiction of Committee D32 on Catalysts andis the direct responsibility of Subcommittee D32.03 on Chemical Composition.Current edition approved April 1,2010.Published May 2010.Originallyapproved in 1985.Last previous edition approved in 2004 as D448104.DOI:10.1520/D4481-10.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.12 Screen,250-m openings,60-mesh.6.13 Analytical Balance,capable of weighing to nearest 0.1mg.6.14 Ashless Filter Pulp.6.15 Desiccator.7.Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other 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.7.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean type IV reagent water asdefined in Specification D1193.7.3 Ammonium Citrate,dibasic crystal,(NH4)2HC6H5O7.7.4 Ammonium Hydroxide,10 and 25%solutions.NOTE1Refer to Se