ASTM_D_4481_-_21.pdf

Designation:D448121Standard 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 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 WaterD7442 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 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 120 C.3.2 A separate test specimen is taken to determine loss onignition(LOI)at 550 C.The value is used to calculate thenickel as percent nickel oxide(NiO)on a 550 C 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 25 C,and 950 6 25 C.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.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 June 1,2021.Published June 2021.Originallyapproved in 1985.Last previous edition approved in 2015 as D4481 10(2015).DOI:10.1520/D4481-21.2For 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 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.16.8 Drying Oven capable of maintaining a temperature of120 C.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 9.6.12 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.6.16 Laboratory Fume Hood,suitable for use with Hydro-fluori