Designation: D6370 − 99 (Reapproved 2014)

Standard Test Method for

Rubber—Compositional Analysis by Thermogravimetry
(TGA)1
This standard is issued under the fixed designation D6370; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope 3. Terminology
1.1 This test method provides a thermogravimetric (TGA) 3.1 Definitions:
technique to determine the amounts of organics (oil, polymer), 3.1.1 The definitions relating to rubber appearing in Termi-
carbon black and ash (filler) in a rubber compound. nology D1566 shall be considered applicable to this test
1.2 The amount of plasticizer/oil may be determined sepa- method.
rately using Test Method D297. 3.1.2 The terminology relating to sampling appearing in
Practice D6085 shall be considered applicable to this test
1.3 This test method utilizes previously calibrated, manual method.
or computer assisted TGA instrumentation. 3.1.3 The definitions for thermal analysis appearing in
1.4 The values stated in SI units are to be regarded as Terminology E473 shall be considered applicable to this test
standard. No other units of measurement are included in this method.
standard. 3.1.4 The description of thermal analysis equipment appear-
ing in Practice E1953 shall be considered applicable to this test
1.5 This standard does not purport to address all of the
method.
safety concerns, if any, associated with its use. It is the
3.2 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.2.1 ash, n—nonvolatile additives (fillers), such as zinc
priate safety and health practices and determine the applica-
oxide, talc, etc.
bility of regulatory limitations prior to use.
3.2.2 carbon black, n—carbon black.
2. Referenced Documents 3.2.3 organics, n—rubber (polymer), noncarbon black or-
2.1 ASTM Standards:2 ganic additives, such as oil, plasticizer, antioxidants, etc.
D297 Test Methods for Rubber Products—Chemical Analy- 4. Summary of Test Method
sis
D1566 Terminology Relating to Rubber 4.1 The mass of the rubber test sample, heated at a
D4483 Practice for Evaluating Precision for Test Method controlled, specified rate in a controlled, specified environment
Standards in the Rubber and Carbon Black Manufacturing is recorded as a function of temperature. The mass loss over the
Industries specified temperature range provides a compositional analysis
D6085 Practice for Sampling in Rubber Testing— of the sample.
Terminology and Basic Concepts
E473 Terminology Relating to Thermal Analysis and Rhe- 5. Significance and Use
ology 5.1 This test method is intended for use in quality control,
E1953 Practice for Description of Thermal Analysis and material screening, and related problem solving where a
Rheology Apparatus compositional analysis, or comparison to a known material, is
desired.
5.2 The parameters described are guidelines and may be
1
This test method is under the jurisdiction of ASTM Committee D11 on Rubber altered to suit the analysis of other rubber compounds.
and is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.
Current edition approved Aug. 1, 2014. Published November 2014. Originally 5.3 This test method is not suitable for rubber compounds
approved in 1999. Last previous edition approved in 2009 as D6370 – 99 (2009). containing filler materials which decompose in the temperature
DOI: 10.1520/D6370-99R14.
2
range of 50 to 800°C, for example, CaCO3, Al(OH)3(3H2O),
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
etc. Analysis of compounds containing fillers of this type
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on requires knowledge of the filler type and some correction for
the ASTM website. mass loss.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 D6370 − 99 (2014)

FIG. 1 Typical Thermogram

6. Apparatus 10. Calculation

6.1 Thermogravimetric Analyzer—A system of related in- 10.1 Record the percent mass loss for organics, carbon
struments that are capable of continuously weighing a test black, and ash as follows (see Fig. 1):
sample, at a sensitivity of 62 µg, and recording the change in 10.2 For EPDM, NR, PE, PP and SBR:
mass of the test sample under atmospheric control over a
Component % Mass Loss
specified temperature range.
Organics 50 to 550°C (nitrogen)
7. Reagents and Materials Carbon black 310 to 790°C (air)
Ash Residue at 790°C
7.1 An inert compressed gas, such as argon or nitrogen, and
a reactive gas, such as air or oxygen. 10.3 For CPE, CR, NBR and PVC:
Component % Mass Loss
7.2 Compressed gases must be 99.99 % minimum purity.
Organics 50 to 550°C (nitrogen)
7.3 The inert purge gas must not contain more than 10 µg/g + 310 to 560°C (air)
oxygen. Carbon black 560 to 790°C (air)
Ash Residue at 790°C
8. Calibration
8.1 Calibrate the apparatus, according to the prescribed 11. Report
procedures or appropriate operating manual, at the heat (tem- 11.1 Report the following information:
perature) and purge gas flow rates to be used. 11.1.1 Identification of the test sample.
11.1.2 Percents—organics, carbon black, and ash found,
9. Procedure
each to the nearest 0.1 %.
9.1 Place a small piece, 10 to 12 mg, of the rubber test
sample into the platinum pan of the calibrated Thermogravi- 12. Precision and Bias3
metric Analyzer (TGA).
12.1 This precision and bias section has been prepared in
9.2 Apply a 75 cm3/min, or the manufacturer’s recom- accordance with Practice D4483. Please refer to this practice
mended flow, argon or nitrogen purge. for terminology and other statistical calculation details.
9.3 Heat to 50°C and allow the instrument to equilibrate for 12.2 The precision results in this precision and bias section
a minimum of 2 min. give an estimate of the precision of this test method with the
9.4 Heat from 50 to 560°C at 10°C/min. materials (rubbers, etc.) used in the particular interlaboratory
test program (ITP) as described below. The precision param-
9.5 Cool to 300°C and allow the temperature to equilibrate
eters should not be used for acceptance or rejection testing of
for a minimum of 2 min.
9.6 Change the purge gas to air or oxygen and purge at 75
cm3/min or the manufacturer’s recommended flow. 3
Supporting data have been filed at ASTM International Headquarters and may
9.7 Heat from 300 to 800°C at 10°C/min. be obtained by requesting Research Report RR:D11-1089.