Designation: D3850 − 12

Standard Test Method for

Rapid Thermal Degradation of Solid Electrical Insulating
Materials By Thermogravimetric Method (TGA)1
This standard is issued under the fixed designation D3850; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope E1582 Practice for Calibration of Temperature Scale for

1.1 This test method outlines a procedure for obtaining Thermogravimetry
thermogravimetric (TGA) data on solid polymeric materials
intended for use as electrical insulating materials. 3. Terminology
1.2 Do not use this standard to quantify an estimate of the 3.1 Definitions—Definitions are in accordance with Termi-
long-term thermal capability for any electrical insulating ma- nology D883, Terminology D1711, and Terminology E473.
terial. If a relationship exists between TGA and the long-term 3.2 Abbreviations—Abbreviations are in accordance with
thermal capabilities of a material, then that fact must be Terminology D1600, unless otherwise indicated.
established and made public, preferably by comparing data
between a candidate and another material known to display 4. Summary of Test Method
similar failure modes.
4.1 This thermogravimetric technique uses the record of the
1.3 The values stated in SI units are the standard. mass loss versus the temperature of the specimen during the

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1.4 This standard does not purport to address all of the time of exposure to a specified prescribed environment using a
safety concerns, if any, associated with its use. It is the controlled time rate of heating.
responsibility of the user of this standard to establish appro-
4.2 The record is a TGA curve, with percent of initial mass
priate safety and health practices and determine the applica-
as the ordinate and temperature as the abscissa (see Figs. 1 and
bility of regulatory limitations prior to use.
2).
2. Referenced Documents 4.3 The temperature is measured and recorded at specified
2.1 ASTM Standards: 2 mass loss points (recorded as a TGA curve), using an electronic
D883 Terminology Relating to Plastics chart recorder or other suitable data acquisition device.
D1600 Terminology for Abbreviated Terms Relating to Plas-
tics 5. Significance and Use
D1711 Terminology Relating to Electrical Insulation 5.1 Thermogravimetry is useful in determining the dynamic
D2307 Test Method for Thermal Endurance of Film- functional effect of temperature on the amount of volatile
Insulated Round Magnet Wire materials leaving a specimen as the latter is heated progres-
E220 Test Method for Calibration of Thermocouples By sively to higher temperatures. TGA can be useful for process
Comparison Techniques control, process development, material evaluation, and for
E473 Terminology Relating to Thermal Analysis and Rhe- identification and quality control in specifications.
ology
5.2 The thermal stability of a material can be associated
with the degree and time rate of mass loss as a function of
1
This test method is under the jurisdiction of ASTM Committee D09 on
temperature. TGA curves can, therefore, be used as a prelimi-
Electrical and Electronic Insulating Materials and is the direct responsibility of nary screen method in the evaluation of relative behavior of
Subcommittee D09.17 on Thermal Characteristics. insulating materials of the same generic family.
Current edition approved Jan. 1, 2012. Published February 2012. Originally
approved in 1979. Last previous edition approved in 2006 as D3850 – 94(2006). 5.3 The functional temperature-life relationship of an insu-
DOI: 10.1520/D3850-12.
2
lating material in any given application depends on a number
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
of service and environmental factors. Therefore, the informa-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on tion obtained from TGA curves is not adequate by itself to
the ASTM website. describe the thermal capability of an insulating material.

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

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 D3850 − 12

Sample 8.54 mg Heating Rate 5°C/min Purging Gas Flow 0.8 mL/s

FIG. 1 Curve No. 1, Typical TGA for Polyester Film

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Sample 5.93 mg Heating Rate 5°C/min Purging Gas Flow 0.8 mL/s

FIG. 2 Curve No. 2, Typical TGA for Polyimide Film

5.4 Refer to the Appendix for further discussion of the 6.1.1 Microbalance, of the null type, sensitive to 0.001 mg,
interpretation of TGA data. 6.1.2 Furnace, controllable at a constant rate over a tem-
perature range of interest, typically 25 to 1000°C,
6. Apparatus 6.1.3 Temperature Programmer, capable of providing a
6.1 Thermogravimetric Analyzer—A system of related in- linear rate of rise of the furnace at a predetermined value
struments comprising: (normally 5°C/min) with a tolerance of 6 0.1°C/min,

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 D3850 − 12
6.1.4 Suitable Data Acquisition Device, and 9.8 Start the heating program and record the mass change
6.1.5 Supply of Purging Gas. until there is no further mass loss.
NOTE 1—For many applications, the purging gas is nitrogen or air NOTE 2—Normally the purge rate is 0.7 to 1.6 mL/s.
having a dew point of at or below −10°C.
10. Report
7. Sampling 10.1 Report the following information:
10.1.1 Identification of the sample and apparatus,
7.1 Use sampling plans as described in specifications or test
10.1.2 Curing time and temperature in the case of resin
methods specific to individual electrical insulating materials.
specimens,
10.1.3 Mass, approximate dimensions and form (for
8. Test Specimens example, film, laminate, molded) of the specimen,
8.1 Prepare test specimens in accordance with the test 10.1.4 Heating rate,
method applicable to the material under investigation. 10.1.5 Rate of flow and type of gas used for purging,
8.2 Generally, it is found that specimens of 2 to 20 mg are 10.1.6 TGA curve of material evaluated, and
satisfactory, depending on the configuration and test apparatus. 10.1.7 Temperatures at which losses of initial specimen
Test results depend in part on the size and shape of specimen, mass, if obtained, of 10, 20, 30, 50, and 75 % occur.
due to thermal equilibrium and diffusion effects. NOTE 3—Do not list temperatures that exceed the resolution of the
instrumentation. Normally this is not to be greater than 2.5°C. Report the
8.3 When the specimen is a coating on a substrate, the total resolution.
mass is greater unless the substrate is carefully separated,
because of the mass contribution of the substrate material. 11. Precision and Bias
11.1 This test method is based on the dynamic measurement
9. Procedure of mass loss as a function of increasing temperature. Devia-
9.1 Calibrate the balance at full scale to within 6 0.01 mg, tions in results that affect precision are caused by variations in
following the recommended procedure. a number of complex factors (for example, physical irregulari-
ties of the specimen, variations in the purging gas composition
9.2 Calibrate the temperature-sensing system to within 6 and flow characteristics) and generally will not correlate
1°C (see Method E220), following the recommended proce- simply with changes in these factors.

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dure.
11.2 The repeatability of the mass loss measurements as a
9.2.1 Position the temperature sensor to prevent contact
function of temperature within one laboratory (and one appa-
with specimens which can become distorted during heating.
ratus) is approximately 6 5°C.
9.2.2 Temperature calibration is critical and the method
employed will vary with the apparatus. Calibrate in accordance 11.3 Limited inter-laboratory testing done as a preliminary
with Practice E1582. preparation for this test method indicate that mass loss mea-
surements plotted as a function of temperature have a repro-
9.3 Adjust the purge rate to the specified value. ducibility of 6 25°C.
9.4 Adjust the Y axis (mass) to chart zero. 11.4 This test method has no bias because the thermal
9.5 Adjust the X axis to the required temperature range. degradation characteristic is defined by the method.
9.6 Place the specimen in the specimen holder and record 12. Keywords
the initial mass. 12.1 degradation; insulating; mass loss; polymeric material;
9.7 Set the heating rate to 5°C/min rate of rise. thermogravimetric analysis; TGA

APPENDIX

(Nonmandatory Information)

X1. INTERPRETATION OF THERMOGRAVIMETRIC TEST TECHNIQUE

X1.1 Introduction—Thermogravimetry is the continuous comparison under dynamic conditions.

measurement of mass loss of a specimen as the temperature is
increased at a specific rate. Since the test method requires the X1.2 Calibration—Initial calibration should follow the
continuous measurement of a varying mass and temperature recommended procedure (when available). This procedure
and the control of temperature rate of rise, differences exist should ensure that individual sensors are correct. The relation-
between instruments, experimenters, or both, even when the ship between the temperature sensor, usually a thermocouple,
precision of the individual component sensors are known. and the specimen design and the type of atmosphere, including
Calibration of the instrumentation system is based upon a the rate of flow of the gas through the weighing chamber, will

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 D3850 − 12
affect the overall calibration of the system. TGA curve will provide a reasonably accurate method for
communicating various TGA data. Close attention to the
X1.3 Atmosphere—The rate of mass loss is dependent in overall calibration on a continual basis will ensure good
part upon the atmosphere to which the test specimen is repeatability within one laboratory over a long period of time.
exposed. For the best correlation of test results to end use,
purge with the air or other gas that relates to the end use X1.6 Interpretation of TGA Data—Thermogravimetry is a
conditions. The rate of flow of the gas in the cell will have a relatively fast means of comparing materials. The dynamic
significant effect on the calibration of the system. It is, relationship between mass loss and temperature is the only
therefore, necessary to select the rate of flow, usually 0.7 to 1.6 thermal characteristic considered with TGA. How this
mL/s, prior to calibration of the system. After calibrating the temperature-mass loss characteristic affects the use of an
system, do not change the flow rate. electrical insulation in the application is unknown. The rate of
mass loss affects electrical insulation life. Mass loss that will
X1.4 Specimen Design, is dictated by the material under result in failure varies with material and temperature. In
consideration, material application, and the instrumentation. addition, the mass loss required for a failure varies with the
Use a specimen in the form normally found in use (for failure mode. Due to the many unknown factors in any given
example, film and coatings). The size will depend on the application, the exact relationship between mass loss and
instrumentation to some degree. The surface area will affect the failure mode for each application should be determined experi-
overall results. For instance, if a specimen with a large surface mentally. Generally, material comparisons by TGA have not
is compared to one with smaller surface area, both of the same always been in the same order as the known temperature class.
mass, the small surface area specimen will normally lose mass As an example, the round robin testing performed during the
at a slower rate, due to thermal equilibrium and thermal effects. development of this test method indicated that polyamide film
Select the specimen configuration and mass prior to system was thermally superior to a PET film. Both life tests and
calibration. experience have verified that PET film is thermally superior to
polyamide film in a variety of electrical applications.
X1.5 System Calibration:
X1.6.1 In 1967, Sweitzer and Stugart3 illustrated that an
X1.5.1 System calibration of the TGA instrumentation in-
equivalent polyamide polymer for magnet wire yielded higher
corporates the comparison of specimen temperature to a
TGA data and had a lower thermal life (Test Method D2307) in
measured physical change in the specimen. The weakest point

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comparison to the same polyamide cured under different
in the calibration procedure is the temperature sensor, usually
conditions.
a thermocouple. Thermocouples are nonlinear within the nor-
mal range of operating temperatures, and can drift from X1.6.2 Thermogravimetry is an important tool in observing
calibration. The location of the temperature sensor in the the effect of polymer variation due to changes in one thermal
weighing chamber must be such that it will provide the best characteristic. The relationship between thermogravimetry and
estimate of the specimen temperature. Since no standard application life is unknown.
measurement will provide this location, it is necessary to make NOTE X1.1—The attached Figs. 1 and 2 for polyester film and
a comparison test. polyimide film are illustrative of the original round-robin test work carried
out in the preparation of this test method.
X1.5.2 Practice E1582 can be used for temperature calibra-
tion.
3
Sweitzer and Stugart, “Screening Polymers for Use as Magnet Wire Enamel,”
X1.5.3 Differences between laboratories always exist. Com- Proceeding of the Seventh Electrical Insulation Conference, 1967, Paper No. IEEE
parison to the referenced curves or another mutually selected 32C-79-64.

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