ASTM_D_4075_-_06_2012.pdf

Designation:D407506(Reapproved 2012)Standard Test Methods forRubber Compounding MaterialsFlame Atomic AbsorptionAnalysisDetermination of Metals1This standard is issued under the fixed designation D4075;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 metals inrubber compounding materials by flame atomic absorption.1.2 The test methods include the following materials:SectionsZinc oxide11-201.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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.(For a specificwarning statement,see 6.1.)2.Referenced Documents2.1 ASTM Standards:2D4004 Test Methods for RubberDetermination of MetalContent by Flame Atomic Absorption(AAS)AnalysisD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE300 Practice for Sampling Industrial Chemicals2.2 Other Documents:2.2.1 Literature pertinent to the particular atomic absorptionspectrophotometric equipment used for the analysis espe-cially the manufacturers recommendations for optimumperformance.Standard texts on atomic absorption byflame technique are also helpful.3.Summary of Test Methods3.1 The compounding material is suitably sampled,pre-pared according to the appropriate sections of these testmethods,and examined by flame absorption spectrophotom-etry for metals.3.2 Sample preparation,procedures,calculations,and pre-cision statements will be found in each section dealing with aparticular compounding material.3.3 The analysis of metals in compounding materials de-pends on the skill of the operator in the use of the flame atomicabsorption equipment.It is,therefore,assumed that the opera-tor is familiar with all aspects of this analytical technique.Nodetails are given here for the proper operation of the equipmentor interpretation of results obtained.3.4 These test methods do not cover the determination ofmetals in raw rubbers or finished products.See Test MethodsD4004 for these methods.4.Significance and Use4.1 These test methods are suitable for process control,forproduct acceptance,and for research and development.5.Apparatus5.1 Balances,capable of weighing accurately to 60.1 mg or60.1 g,depending on sample mass required.5.2 Hot Plate.5.3 Common Borosilicate Glassware,especially 10,100,200 and 500-cm3volumetric flasks.5.4 Pipets,of 1,2,5,and 10-cm3capacity.One cubiccentimetre pipets graduated in tenths and hundredths areespecially useful.5.5 Microlitre Syringes,1 and 10 mm3(L)are recom-mended.5.6 Plastic Bottles,suitable for storage of standard solu-tions.5.7 Atomic Absorption Spectrophotometer,operating in theflame mode.The instrument must be operated according to themanufacturers directions for optimum performance for flameoperation.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 June 2012.Originallyapproved in 1981.Last previous edition approved in 2006 as D4075 06.DOI:10.1520/D4075-06R12.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Reagents6.1 Standard solution for metals to be determined in eachcompounding material may be prepared from pure metals,metallic compounds,or purchased from a chemical supplyhouse as standard solutions.The usual concentrations ofsolutions is 1000 g of the metal per cubic centimetre ofsolution.Suitable dilutions with water will bring these concen-trated solutions into the linear working range of the instrument.It is recommended that standards below 1 g/cm3be preparedfresh,while those above 1 g/cm3may be stored.(WarningObserve all recognized health and safety precautions whilecarrying out this procedure.All reagents shall be of analyticalgrade,and distilled,deionized,or distilled deionized watershall be used for sample preparation and required dilutions.)7.Sampling7.1 Sampling shall be carried out in the best possible way toensure that the sample is representative of the lot(see PracticeE300).7.2 The analyst shall select a t