ASTM_D_4574_-_06_2012.pdf

Designation:D457406(Reapproved 2012)Standard Test Methods forRubber Compounding MaterialsDetermination of AshContent1This standard is issued under the fixed designation D4574;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 These test methods cover the determination of ashcontent of rubber chemicals.1.2 The test methods include the following materials:MaterialSectionSulfur7-13p-Phenylenediamine Antioxidants14-22Benzothiazole Sulfenamide Accel-erators14-221.3 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.2.Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD4676 Classification for Rubber Compounding MaterialsAntidegradants3.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1“lot”samplea production sample representative of astandard production unit,normally referred to as“the sample.”3.1.2 test unitthe actual material used in the analysis.Itmust be representative of the“lot”sample.4.Summary of Test Methods4.1 The ash content is determined by heating a knownquantity of the rubber chemical on a hot plate or over a gasburner to volatilize the sample and then heating in a mufflefurnace to complete the ashing process.4.2 Sample preparation,procedures,calculations,and pre-cision statements will be found in each section dealing with aparticular rubber chemical.5.Significance and Use5.1 These test methods are suitable for the determination ofthe ash content of rubber compounding materials.The testmethods may be used for quality control,product acceptance,or research and development.Classification D4676 prescribespercent ash as an important characteristic of rubber antidegra-dants.6.Apparatus6.1 Muffle Furnace,capable of temperature regulation of625C between 500 and 800C.6.2 Hot Plate(or laboratory gas burner).6.3 Laboratory Fume Hood.6.4 Porcelain Combustion Crucible,capsule form,25-cm3capacity.6.5 Porcelain Crucible,high form,size 0,15-cm3capacity.6.6 Clay Triangle.6.7 Steel Crucible Tongs.6.8 Heat Resistant Gloves.6.9 Desiccator.6.10 Analytical Balance,sensitive to 0.0001 g.6.11 Air Circulating Oven,capable of 70 6 2C.SULFUR7.Scope7.1 This test method is used for the determination of the ashcontent of sulfur.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 1986.Last previous edition approved in 2006 as D4574 06.DOI:10.1520/D4574-06R12.2For 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 8.Summary of Test Method8.1 The ash content of sulfur is determined by the controlledburning of the sulfur,followed by ashing in a furnace at 600C.9.Apparatus9.1 See Section 6.10.Procedure10.1 Dry 6 g or more of sulfur in an oven at 70C for 2 h.Cool in a desiccator.10.2 Weigh a 5-g specimen to the nearest 0.0001 g into apreviously ignited,weighed,25-cm3porcelain crucible.In awell-ventilated hood,place the crucible on a hot plate and heatto 400 to 500C,burning off all of the sulfur;or burn off thesulfur by moderate heating over a gas burner.When all of thesulfur is gone,transfer the crucible to a muffle furnace and heatto 600 6 25C for at least 20 min.Cool in a desiccator andweigh.11.Calculation11.1 Calculate the percent ash as follows:A 5B/C!3100(1)where:A=ash,%,B=mass of ash,g,andC=mass of sample,g.12.Report12.1 Report the following information:12.1.1 Proper identification of the sample,and12.1.2 Results of two individual determinations and theiraverage reported as percent ash to the nearest 0.01%.13.Precision and Bias313.1 This precision and bias section has been prepared inaccordance with Practice D4483.Refer to Practice D4483 forterminology and other statistical details.13.2 The precision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials(rubbers)used in the particular interlaboratory pro-grams as described below.The precision parameters should notbe used for acceptance/rejection t