ASTM_D_4004_-_06_2012.pdf

Designation:D400406(Reapproved 2012)Standard Test Methods forRubberDetermination of Metal Content by Flame AtomicAbsorption(AAS)Analysis1This standard is issued under the fixed designation D4004;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.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 These test methods cover the determination of lead,zinc,copper,and manganese in raw rubber and rubbercompounds,vulcanized or unvulcanized.The level at whichthe metals are present is taken into account by suitableadjustments of sample mass and dilution.1.2 Certain compounding ingredients,present in the rubbersample will dictate which of the methods should be used.Referto Section 3.Five methods of determination are as follows:SectionsMethod A8Method B9Method C10Method D14-22Method E23-311.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4This 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:2D1076 Specification for RubberConcentrated,AmmoniaPreserved,Creamed,and Centrifuged Natural LatexD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE663 Practice for Flame Atomic Absorption Analysis(With-drawn 1997)32.2 ISO Standards:ISO 1396 RubberCopper ContentPhotometric Technique-Determination4ISO 1655 RubberManganese ContentPhotometric Tech-niqueDetermination43.Summary of Test Methods3.1 Method ADetermination of lead and zinc in rubber notcontaining any halogen;in the case of lead,also not containingany silica filler.See Section 8.3.1.1 In MethodA,the rubber is furnace-dried in a platinumcrucible at 250C,followed by furnace ashing for 1 to 2 h at550C.The ash is dissolved with the aid of concentratedhydrochloric acid(HCl)and the resulting solution suitablydiluted for Atomic Absorption Spectrometric(AAS)determi-nation of the lead and zinc.3.2 Method BDetermination of lead and zinc in rubbercontaining silica filler,but no halogen.See Section 9.3.2.1 In Method B the rubber is ashed in platinum as inMethod A.The ash is then fused with a lithium or sodiumtetraborate or metaborate flux,after which the fused mixture isdissolved with the aid of HCl for subsequent AAS analysis.3.3 Method CDetermination of lead and zinc in rubbercontaining halogen.See Section 10.3.3.1 In Method C the rubber is wet-ashed with the aid ofconcentrated sulfuric acid(H2SO4)and nitric acid(HNO3),evaporated to dryness,and further ashed in a muffle furnace at550C,after which the ash is dissolved as in Method A forsubsequent AAS analysis.3.4 Method DDetermination of copper in raw rubber andrubber latex,both synthetic and natural(see 14.2).3.4.1 In Method D the rubber is ashed at 550C,the ash isthen digested in hydrochloric acid,and copper is determined byAAS analysis.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved May 1,2012.Published May 2012.Originallyapproved in 1981.Last previous edition approved in 2006 as D4004 06.DOI:10.1520/D4004-06R12.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.5 Method EDetermination of manganese in raw naturalrubber and rubber latex,both synthetic and natural(see 23.2).3.5.1 In Method E the rubber is ashed at 550C,the ash isdigested in hydrochloric acid and the manganese is determinedby AAS analysis.3.5.2 See 3.6.3.6 Because this standard does not contain procedures foroptimizing instrument performance,nor does it instruct theanalyst in the basics of flame atomic absorption,it is recom-mended that the references found in Section 2 be studied forthese purposes.4.Significance and Use4.1 These test methods are suitable for process control,forproduct acceptance,and for research and development.5.Apparatus5.1 Laboratory Balance.5.2 Laboratory Muffle Furnace.5.3 Hot Plate.5.4 Platinum Crucibles,25 cm3content minimum.5.5 Common Borosilicate Glassware.5.6 Mek