ASTM_D_4642_-_04_2010.pdf

Designation:D464204(Reapproved 2010)Standard Test Method forPlatinum in Reforming Catalysts by Wet Chemistry1This standard is issued under the fixed designation D4642;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 platinum innonzeolitic,fresh reforming catalysts containing platinum asthe only precious metal,in the range of concentration of 0.200to 0.700 weight%.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:2D1193 Specification for Reagent WaterE177 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:NNN-P-395C Tolerance for Class A Pipets33.Summary of Test Method3.1 The ground alumina based reforming catalyst is dis-solved using dilute hydrochloric acid.Stannous chloride isadded to convert the platinum in solution to a yellowish-orange-colored platinum stannous hydrochloride complex.Theabsorbance of the resulting solution is measured comparativelyat 403 nm by spectrophotometry and the platinum content iscalculated from a previously determined value for the absorp-tivity.4.Significance and Use4.1 This test method provides a means of determining theplatinum content of fresh reforming catalysts where the plati-num is supported on an all alumina substrate.44.2 This test method is not intended to cover samplescontaining metals other than platinum.Palladium,rhenium,and rhodium in particular interfere with the spectrophotometricdetermination of platinum.5.Apparatus5.1 Balance,analytical,capable of weighing to the nearest0.1 mg.5.2 Beakers,250-mL,tall form and 600-mL.5.3 Cells,spectrophotometer,1.0 cm,matched.5.4 Crucibles,platinum,or porcelain,50-mL.5.5 Desiccator,vacuum.5.6 Filter Paper,fine,ashless,slow filtering,12.5 cm orequivalent.5.7 Flasks,volumetric,conforming to tolerances specifiedby Specification E288,500-mL and 1000-mL.5.8 Funnel,filtering,fluted bowl,65 mm top diameter,150mm stem.5.9 Graduated Cylinders,10-mL,25-mL,50-mL,250-mL.5.10 Pipets,conforming to tolerances specified by FederalSpecification NNN-P-395C,5-mL,10-mL,15-mL.5.11 Muffle Furnace,capable of 1000 6 25C.5.12 Spectrophotometer,capable of measuring absorbancevalues between 200 to 800 nm with a photometric repeatabilityof 60.002 absolute at 1.0 absolute.5.13 Watch Glass,flat,100 mm.5.14 Watch Glass,ribbed,65 mm.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 Sept.1,2010.Published November 2010.Originallyapproved in 1986.Last previous edition approved in 2004 as D464204.DOI:10.1520/D4642-04R10.2For 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,DODSSP,Bldg.4,Section D,700 Robbins Ave.,Philadelphia,PA 19111-5098.4This test method can be extended to spent reforming catalyst by isolating theplatinum by the methods described in“Assay Procedure for Platinum in ReformingCatalysts,”Analytical Chemistry,Vol 32,No.6,May 1960,p.646.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.15 Wash Bottle,polyethylene,500-mL.5.16 Weighing Vial,25 by 40 mm.6.Reagents6.1 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.Other 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.56.2 Purity of WaterUnless otherwise indicated,all refer-ences to water used as a reagent mean deionized or distilledwater conforming to Specification D1193.6.3 Aluminum Chloride SolutionDissolve 453.6 g ofAlCl36H2O in water and dilute to a litre with water.6.4 Aqua RegiaMix three parts concentrated