1、Designation: D6370 99 (Reapproved 2014)Standard Test Method forRubberCompositional Analysis by Thermogravimetry(TGA)1This standard is issued under the fixed designation D6370; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the yea
2、r 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 This test method provides a thermogravimetric (TGA)technique to determine the amounts of organics (oil, polymer),
3、carbon black and ash (filler) in a rubber compound.1.2 The amount of plasticizer/oil may be determined sepa-rately using Test Method D297.1.3 This test method utilizes previously calibrated, manualor computer assisted TGA instrumentation.1.4 The values stated in SI units are to be regarded asstandar
4、d. No other units of measurement are included in thisstandard.1.5 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
5、-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D297 Test Methods for Rubber ProductsChemical Analy-sisD1566 Terminology Relating to RubberD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries
6、D6085 Practice for Sampling in Rubber TestingTerminology and Basic ConceptsE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1953 Practice for Description of Thermal Analysis andRheology Apparatus3. Terminology3.1 Definitions:3.1.1 The definitions relating to rubber appearing in Termi-nolo
7、gy D1566 shall be considered applicable to this testmethod.3.1.2 The terminology relating to sampling appearing inPractice D6085 shall be considered applicable to this testmethod.3.1.3 The definitions for thermal analysis appearing inTerminology E473 shall be considered applicable to this testmethod
8、.3.1.4 The description of thermal analysis equipment appear-ing in Practice E1953 shall be considered applicable to this testmethod.3.2 Definitions of 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 org
9、anics, nrubber (polymer), noncarbon black or-ganic additives, such as oil, plasticizer, antioxidants, etc.4. Summary of Test Method4.1 The mass of the rubber test sample, heated at acontrolled, specified rate in a controlled, specified environmentis recorded as a function of temperature. The mass lo
10、ss over thespecified temperature range provides a compositional analysisof the sample.5. Significance and Use5.1 This test method is intended for use in quality control,material screening, and related problem solving where acompositional analysis, or comparison to a known material, isdesired.5.2 The
11、 parameters described are guidelines and may bealtered to suit the analysis of other rubber compounds.5.3 This test method is not suitable for rubber compoundscontaining filler materials which decompose in the temperaturerange of 50 to 800C, for example, CaCO3, Al(OH)3(3H2O),etc. Analysis of compoun
12、ds containing fillers of this typerequires knowledge of the filler type and some correction formass loss.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved Aug. 1, 2014. Publ
13、ished November 2014. Originallyapproved in 1999. Last previous edition approved in 2009 as D6370 99 (2009).DOI: 10.1520/D6370-99R14.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
14、ation, 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 States16. Apparatus6.1 Thermogravimetric AnalyzerA system of related in-struments that are capable of continuously weighin
15、g a testsample, at a sensitivity of 62 g, and recording the change inmass of the test sample under atmospheric control over aspecified temperature range.7. Reagents and Materials7.1 An inert compressed gas, such as argon or nitrogen, anda reactive gas, such as air or oxygen.7.2 Compressed gases must
16、 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 appropriate operating manual, at the heat (tem-perature) and purge gas flow rates to be used.9. Procedure9.1 Place a small pi
17、ece, 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 flow, argon or nitrogen purge.9.3 Heat to 50C and allow the instrument to equilibrate fora minimum of 2 min.9.4 Heat from 50
18、to 560C at 10C/min.9.5 Cool to 300C and allow the temperature to equilibratefor a minimum of 2 min.9.6 Change the purge gas to air or oxygen and purge at 75cm3/min or the manufacturers recommended flow.9.7 Heat from 300 to 800C at 10C/min.10. Calculation10.1 Record the percent mass loss for organics
19、, carbonblack, and ash as follows (see Fig. 1):10.2 For EPDM, NR, PE, PP and SBR:Component % Mass LossOrganics 50 to 550C (nitrogen)Carbon black 310 to 790C (air)Ash Residue at 790C10.3 For CPE, CR, NBR and PVC:Component % Mass LossOrganics 50 to 550C (nitrogen)+ 310 to 560C (air)Carbon black 560 to
20、 790C (air)Ash Residue at 790C11. Report11.1 Report the following information:11.1.1 Identification of the test 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 Practi
21、ce D4483. Please refer to this practicefor terminology and other statistical calculation details.12.2 The precision 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 (IT
22、P) as described below. The precision param-eters should not be used for acceptance or rejection testing of3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D11-1089.FIG. 1 Typical ThermogramD6370 99 (2014)2any group of materials w
23、ithout 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 black; A = EPDM, B = NBR
24、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 subjected to h-outlier
25、 andk-outlier analysis as given by Practice D4483. 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 for test method precisi
26、on. 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(organics, carbon black, ash) of this test method has beenestablished as the value tabulated
27、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 reproducibility R, for each test(or
28、ganics, 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 considered to have come from diff
29、erentor 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 differencebetween an average
30、 test value and the reference (or true) testproperty 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.13. Keywords13.1 ash; carbon black; filler; oil; organics; plasticizer;
31、polymer; rubber; thermogravimetryTABLE 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 Mean SrArB(r)CSRDRE(R)FC 63.7 0.171 0.478 0.75 0.248
32、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 1.73 4.850 14.02C 34.6 0.106 0.296 0.86 0.186 0.520
33、 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, in measured %.C(r) = repeatability, relative basis,
34、 % of %.DSR = reproducibility standard deviation, in measured %ER = reproducibility, in measured %F(R) = reproducibility, relative basis, % of %D6370 99 (2014)3ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this stan
35、dard. 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 responsibility.This standard is subject to revision at any time by the responsible technical committee and must be revie
36、wed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsibl
37、e technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to 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 Con
38、shohocken, 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 99 (2014)4
