ASTM_D_4574-06R2017.pdf

This 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 isued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.Designation:D4574-06(Reapproved 2017)INTERNATIONALStandard Test Methods forRubber Compounding Materials-Determination of AshContentThis 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(8)indicates an editorial change since the last revision or reapproval.1.Scope3.Terminology1.1 These test methods cover the determination of ash3.1 Definitions of Terms Specific to This Standard:content of rubber chemicals.3.1.1 lot sample-a production sample representative of astandard production unit,normally referred to as the sample.1.2 The test methods include the following materials:3.1.2 test unit-the actual material used in the analysis.ItMaterialSectionSulfur7-13must be representative of the lot sample.p-Phenylenediamine Antioxidants14-22Benzothiazole Sulfenamide Accel-14-224.Summary of Test Methodserators4.1 The ash content is determined by heating a known1.3 The values stated in SI units are to be regarded asquantity of the rubber chemical on a hot plate or over a gasstandard.No other units of measurement are included in thisburner to volatilize the sample and then heating in a mufflestandard.furnace to complete the ashing process.1.4 This standard does not purport to address all of the4.2 Sample preparation,procedures,calculations,and pre-safety concerns,if any,associated with its use.It is thecision statements will be found in each section dealing with aresponsibility of the user of this standard to establish appro-particular rubber chemical.priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.5.Significance and Use1.5 This international standard was developed in accor-5.1 These test methods are suitable for the determination ofdance with internationally recognized principles on standard-the ash content of rubber compounding materials.The testization established in the Decision on Principles for themethods may be used for quality control,product acceptance,Development of International Standards,Guides and Recom-or research and development.Classification D4676 prescribesmendations issued by the World Trade Organization Technicalpercent ash as an important characteristic of rubber antidegra-Barriers to Trade(TBT)Committee.dants.2.Referenced Documents6.Apparatus2.1 ASTM Standards:26.1 Muffle Furnace,capable of temperature regulation ofD4483 Practice for Evaluating Precision for Test Method25C between 500 and 800C.Standards in the Rubber and Carbon Black Manufacturing6.2 Hot Plate(or laboratory gas burner).IndustriesD4676 Classification for Rubber Compounding Materials-6.3 Laboratory Fume Hood.Antidegradants6.4 Porcelain Combustion Crucible,capsule form,25-cm3capacity.6.5 Porcelain Crucible,high form,size 0,15-cm3 capacity.These test methods are under the jurisdiction of ASTM Committee D11 on6.6 Clay Triangle.Rubber and Rubber-like Materials and are the direct responsibility of SubcommitteeD11.11 on Chemical Analysis.6.7 Steel Crucible Tongs.Current edition approved May 1,2017.Published May 2017.Originallyapproved in 1986.Last previous edition approved in 2012 as D4574-06(2012).6.8 Heat Resistant Gloves.DOI:10.1520/D4574-06R17.6.9 Desiccator.2 For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTM6.10 Analytical Balance,sensitive to 0.0001 g.Standards volume information,refer to the standards Document Summary page onthe ASTM website.6.11 Air Circulating Oven,capable of 70 2C.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesCopyright by ASTM Intl(all rights reserved);Fri Oct 6 09:32:53 EDT 2017Downloaded/printed byUniversity of Edinburgh(University of Edinburgh)pursuant to License Agreement.No further reproductions authorized.D4574-06(2017)TABLE 2 Ash Content,PPD Antidegradants and Accelerators,%Table 2.Two single test results,obtained under normal testWithin Laboratory Between Laboratorymethod procedures,that differ by more than this tabulated rMaterialAver-ageS,SRR(for any given level)must be considered as derived fromM1-6PPD0.020.0120.0330.0130.036different or nonidentical sample populations.M2-IPPD0.010.0040.0130.0090.026M3-BMPPD0.010.0070.0200.0120.03422.8 Reproducibility-The reproducibility,R,of this testM4-DTPD0.020.0050.0150.0080.025method has been established as the appropriate value tabulatedM5-DCBS0.030.0020.0060.0070.020M6-TBBS0.050.0050.0160.0090.027in Table 2.Two single test results obtained in two differentPooled values0.020.0070.0200.0100.028laboratories,under normal test method procedures,that differ S,=repeatability standard deviation.by more than the tabulated R(for any given level)must ber=repeatability(2.83 x the square root of the repeatability variance).considered to have come from different or nonidentical sampleS=reproducibility standard deviation.populations.R=reproducibility(2.83 x the square root of the reproducibility variance).B No values omitted.22.9 The relative repeatability,(r),and reproducibility,(R),have been omitted from Table 2 since the level of values testedwas extremely low and approached the limits of sensitivity of22.6 The precision of this test method may be expressed inthe test method.Under these circumstances the relative valuesthe format of the following statements which use an appro-become trivial.priate value of r,R,(r),or(R),that is,that value to be used in22.10 Bias-In test method terminology,bias is the differ-decisions about test results(obtained with the test method).ence between an average test value and the reference(or true)The appropriate value is that value of r or R associated with atest property value.Reference values have not been evaluatedmean level in Table 2 closest to the mean level underfor this test method.Bias,therefore,cannot be determined.consideration at any given time,for any given material inroutine testing operations.23.Keywords22.7 Repeatability-The repeatability,r,of this test method23.1 accelerators;antidegradants;ash;rubber compoundinghas been established as the appropriate value tabulated inmaterials;sulfurASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.Users of this standard are expressly advised that determination of the validity of any such patent rights,and the riskof infringement of such rights,are entirely their own 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