1、Designation: D 6370 99 (Reapproved 2003)Standard Test Method forRubberCompositional Analysis by Thermogravimetry(TGA)1This standard is issued under the fixed designation D 6370; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the y
2、ear of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method provides a thermogravimetric (TGA)technique to determine the amounts of organics (oil, polyme
3、r),carbon black and ash (filler) in a rubber compound.1.2 The amount of plasticizer/oil may be determined sepa-rately using Test Method D 297.1.3 This test method utilizes previously calibrated, manualor computer assisted TGA instrumentation.1.4 This standard does not purport to address all of thesa
4、fety 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:2D 297 Test Methods for Rubber
5、ProductsChemicalAnalysisD 1566 Terminology Relating to RubberD 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black IndustriesD 6085 Practice for Sampling in Rubber TestingTerminology and Basic ConceptsE 473 Terminology Relating to Thermal AnalysisE 1953 Pr
6、actice for Description of Thermal Analysis Appa-ratus3. Terminology3.1 Definitions:3.1.1 The definitions relating to rubber appearing in Termi-nology D 1566 shall be considered applicable to this testmethod.3.1.2 The terminology relating to sampling appearing inPractice D 6085 shall be considered ap
7、plicable to this testmethod.3.1.3 The definitions for thermal analysis appearing inTerminology E 473 shall be considered applicable to this testmethod.3.1.4 The description of thermal analysis equipment appear-ing in Practice E 1953 shall be considered applicable to thistest method.3.2 Definitions o
8、f Terms Specific to This Standard:3.2.1 ash, nnonvolatile additives (fillers), such as zincoxide, talc, etc.3.2.2 carbon black, ncarbon black.3.2.3 organics, nrubber (polymer), noncarbon black or-ganic additives, such as oil, plasticizer, antioxidants, etc.4. Summary of Test Method4.1 The mass of th
9、e rubber test sample, heated at a con-trolled, specified rate in a controlled, specified environment isrecorded as a function of temperature. The mass loss over thespecified temperature range provides a compositional analysisof the sample.5. Significance and Use5.1 This test method is intended for u
10、se in quality control,material screening, and related problem solving where acompositional analysis, or comparison to a known material, isdesired.5.2 The parameters described are guidelines and may bealtered to suit the analysis of other rubber compounds.5.3 This test method is not suitable for rubb
11、er compoundscontaining filler materials which decompose in the temperaturerange of 50C to 800C, for example, CaCO3,Al(OH)3(3H2O),etc. Analysis of compounds containing fillers of this typerequires knowledge of the filler type and some correction formass loss.6. Apparatus6.1 Thermogravimetric Analyzer
12、A system of related in-struments that are capable of continuously weighing a testsample, at a sensitivity of 6 2 g, and recording the change in1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Curre
13、nt edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 1999. Last previous edition approved in 1999 as D 6370 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume
14、 information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.mass of the test sample under atmospheric control over aspecified temperature range.7. Reagents and Materia
15、ls7.1 An inert compressed gas, such as argon or nitrogen, anda reactive gas, such as air or oxygen.7.2 Compressed gases must be 99.99 % minimum purity.7.3 The inert purge gas must not contain more than 10 g/goxygen.8. Calibration8.1 Calibrate the apparatus, according to the prescribedprocedures or a
16、ppropriate operating manual, at the heat (tem-perature) and purge gas flow rates to be used.9. Procedure9.1 Place a small piece, 10 to 12 mg, of the rubber testsample into the platinum pan of the calibrated Thermogravi-metric Analyzer (TGA).9.2 Apply a 75 cm3/min, or the manufacturers recom-mended f
17、low, argon or nitrogen purge.9.3 Heat to 50C and allow the instrument to equilibrate fora minimum of 2 minutes.9.4 Heat from 50 C to 560 C at 10 C/min.9.5 Cool to 300 C and allow the temperature to equilibratefor a minimum of 2 minutes.9.6 Change the purge gas to air or oxygen and purge at 75cm3/min
18、 or the manufacturers recommended flow.9.7 Heat from 300 C to 800 C at 10 C/min.10. Calculation10.1 Record the percent mass loss for organics, carbonblack, and ash as follows (see Fig. 1):10.2 For EPDM, NR, PE, PP and SBR:Component % Mass LossOrganics 50 to 550 C (nitrogen)Carbon black 310 to 790 C
19、(air)Ash Residue at 790 CFIG. 1 Typical ThermogramD 6370 99 (2003)210.3 For CPE, CR, NBR and PVC:Component % Mass LossOrganics 50 to 550 C (nitrogen)+ 310 to 560 C (air)Carbon black 560 to 790 C (air)Ash Residue at 790 C11. Report11.1 Report the following information:11.1.1 Identification of the tes
20、t sample.11.1.2 Percentsorganics, carbon black, and ash found,each to the nearest 0.1 %.12. Precision and Bias312.1 This precision and bias section has been prepared inaccordance with Practice D 4483. Please refer to this practicefor terminology and other statistical calculation details.12.2 The pre
21、cision results in this precision and bias sectiongive an estimate of the precision of this test method with thematerials (rubbers, etc.) used in the particular interlaboratorytest program (ITP) as described below. The precision param-eters should not be used for acceptance or rejection testing ofany
22、 group of materials without documentation that the param-eters are applicable to the particular group of materials and thespecific testing protocols of the test method.12.3 A Type 1 interlaboratory test program was conductedin 1998 on three materials or compounds (A, B, C) containing35 % carbon blac
23、k; A = EPDM, B = NBR and C = SBR.Thirteen laboratories participated in the ITP conducting dupli-cate tests on each of two successive test days. A test result isthe average of two measurements for each of the testsconducted; % organics, % carbon black and % ash. Thedatabase generated by the ITP was s
24、ubjected to h-outlier andk-outlier analysis as given by Practice D 4483. Several outlyinglaboratories were found for the tests; the outlier values weredeleted and replaced by the average values for all laboratoriesfor that test and material. The revised database (outliersremoved) was then analyzed f
25、or test method precision. Theresults are given in Table 1. The results in the table indicate thatthe precision for the NBR compound is substantially poorerthan for EPDM and SBR.12.4 RepeatabilityThe repeatability r, for each test (or-ganics, carbon black, ash) of this test method has beenestablished
26、 as the value tabulated in Table 1 for each material.Two single test results, obtained under normal test methodprocedures, that differ by more than this tabulated r (for anygiven level) must be considered as derived from different ornonidentical sample populations.12.5 ReproducibilityThe reproducibi
27、lity R, for each test(organics, carbon black, ash) of this test method has beenestablished as the value tabulated in Table 1 for each material.Two single test results obtained in two different laboratories,under normal test method procedures, that differ by more thanthe tabulated R must be considere
28、d to have come from differentor nonidentical sample populations.12.6 The relative repeatability and reproducibility, (r) and(R), also are given in Table 1. These precision parameters havethe same applicability statements as given in 12.4 and 12.5.12.7 BiasIn test method terminology, bias is the diff
29、er-ence between an average test value and the reference (or true)test property value. Reference values do not exist for this testmethod since the value (of the test property) is exclusivelydefined by the test method; therefore, bias cannot be deter-mined.3Supporting data have been filed at ASTM Inte
30、rnational Headquarters and maybe obtained by requesting Research Report RR: D11-1089.TABLE 1 Precision for Thermogravimetric Analysis(Type 1 Precision)NOTE 1No relative precision given for percent ash, mean values close to zero.Part 1Percent OrganicsWithin Laboratories Between LaboratoriesMaterial M
31、ean SrArB(r)CSRDRE(R)FC 63.7 0.171 0.478 0.75 0.248 0.694 1.09B 64.9 0.252 0.705 1.09 1.933 5.41 8.34A 65.4 0.109 0.306 0.47 0.181 0.508 0.78Part 2Percent Carbon BlackWithin Laboratories Between LaboratoriesMaterial Mean Sr r (r) SR R(R)A 34.3 0.113 0.316 0.92 0.157 0.439 1.28B 34.6 0.224 0.628 1.82
32、 1.73 4.850 14.02C 34.6 0.106 0.296 0.86 0.186 0.520 1.50Part 3Percent AshWithin Laboratories Between LaboratoriesMaterial Mean Sr r SR RA 0.26 0.110 0.307 0.134 0.375B 0.31 0.094 0.264 0.158 0.442C 1.64 0.144 0.403 0.244 0.682ASr = repeatability standard deviation, in measured %.Br = repeatability,
33、 in measured %.C(r) = repeatability, relative basis, % of %.DSR = reproducibility standard deviation, in measured %ER = reproducibility, in measured %F(R) = reproducibility, relative basis, % of %D 6370 99 (2003)313. Keywords13.1 ash; carbon black; filler; oil; organics; plasticizer;polymer; rubber;
34、 thermogravimetryASTM 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
35、 such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for a
36、dditional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to
37、 the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 6370 99 (2003)4
