ASTM D4102-82(1999)

Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers

SCOPE
1.1 This test method covers the apparatus and procedure for the determination of the weight loss of carbon fibers, exposed to ambient hot air, as a means of characterizing their oxidative resistance.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard information, see Section 8.

General Information

• Status: Historical
• Publication Date: 09-Oct-1999
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Relations

• Replaced By: ASTM D4102-82(1999)e1 - Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
• Effective Date: 23-Mar-1982
• Referred By: ASTM D4762-18 - Standard Guide for Testing Polymer Matrix Composite Materials
• Effective Date: 10-Oct-1999

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
Designation:D4102–82 (Reapproved 1999)
Standard Test Method for
ThermalOxidativeResistanceofCarbonFibers
This standard is issued under the fixed designation D 4102; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope extended measurement, determining the weight loss resulting
from 500-h exposure in air at 315°C (600°F).
1.1 This test method covers the apparatus and procedure for
the determination of the weight loss of carbon fibers, exposed
5. Significance and Use
to ambient hot air, as a means of characterizing their oxidative
5.1 The test is used to determine the oxidative resistances of
resistance.
carbon fibers as a means of selecting the most stable fibers for
1.2 This standard does not purport to address all of the
incorporation in high-temperature fiber-reinforced composite
safety concerns, if any, associated with its use. It is the
systems. It can be used for quality control, material specifica-
responsibility of the user of this standard to establish appro-
tion, and for research and development of improved carbon
priate safety and health practices and determine the applica-
fibers. Factors that influence the oxidative resistance and
bility of regulatory limitations prior to use. For specific hazard
should be reported are fiber identification, precursor type, fiber
information, see Section 8.
modulus, and any information on impurities, particularly
2. Referenced Documents metals. IAlso note that the presence of finish on the fiber can
affect the oxidative resistance, and thus, alternative specimen
2.1 ASTM Standards:
preparations that enable the evaluation of finish effects are
C 613 TestMethodforResinContentofCarbonandGraph-
included.
ite Prepregs by Solvent Extraction
6. Apparatus
3. Definitions
6.1 Balance, capable of weighing to the nearest 0.1 mg.
3.1 carbon fibers—fibers containing at least 90 % carbon by
6.2 Vacuum Oven, capable of providing vacuum of 10 torr
weight made by pyrolysis from synthetic polymeric or pitch
(1.3 kPa) or less at 80°C (177°F).
fibers and having moduli$70 GPa ($10 psi).
6.3 Circulating Air Oven, with sufficient flow rate and
3.2 precursor—organic fiber from which carbon fibers are
capability to change the ambient air in the chamber once a
prepared via pyrolysis. Polyacrylonitrile (PAN), rayon, and
minute, while maintaining the temperature within 10°C (18°F)
pitch are commonly used.
over the 25°C (77°F) to 375°C (707°F) range.
3.3 fiber finish—surface coating applied to fibers to facili-
6.4 Glass Beakers, borosilicate, 250-mL or other size,
tate handling or provide better wetting and compatibility of
appropriate for the oven (one per sample).
fiber and matrix, or both.
6.5 Wire Mesh Covers, for the beakers to reduce excessive
4. Summary of Test Method air turbulence during the exposure.
6.6 Boiling Flasks or Erlenmeyer Flasks, borosilicate glass,
4.1 The method is composed of two parts. The first one
250- or 500-mL size, with standard-taper joint.
specifies exposure conditions for an accelerated measurement,
6.7 Glass Condensers, borosilicate for the above flasks.
determining weight loss of the carbon fiber after 24 h in air at
6.8 Hot Plate.
375°C (707°F). The second part specifies conditions for an
6.9 Tweezers, stainless steel.
This test method is under the jurisdiction of ASTM Committee D-30 on
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
Constituent/Precursor Properties.
Current edition approved March 23, 1982. Published April 1987. 20-mesh nickel-chromium wire gauze from Fisher Scientific Co. has been
Annual Book of ASTM Standards, Vol 15.03. found satisfactory for this purpose.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact ASTM
International (www.astm.org) for the latest information.
D4102
7. Reagents and Materials 11.3.1 Put the specimen in a dry flask and cover with 100 to
200 mL of methyl ethyl ketone solvent. Place the condenser
7.1 Methyl Ethyl Ketone (2-butanone) 99.5 % pure, boiling
onto the flask and start the cooling water. Heat the flask on the
range 70.0 to 81.0°C, or other suitable solvents recommended
hot plate or heating bath to bring the solvent to boil. Soak the
in Test Method C 613.
specimen in the boiling solvent for 15 min. Take off the
condenser, decant the solvent, and remove the specimen.
8. Hazards
11.3.2 Dry the specimen in the vacuum oven at 77°C
8.1 The methyl ethyl ketone, classified as an irritant and a
(170°F) at a reduced pressure of 10 torr (1.3 kPa) or less for 30
fire hazard, should be handled in a well-ventilated area and
min.
should not be exposed to direct heat or open flame.
11.3.3 Weigh the dried specimen to the nearest 0.1 mg.
Record the weight.
9. Test Specimen and Sampling
11.3.4 Repeat Steps 11.3.1-11.3.3 until the weight remains
9.1 Using clean gloves to prevent any contamination, par-
constant, within 60.1 mg. Record the final weight, W .
e
ticularly with salt, unwrap the outer layers, which may have
11.4 Drying:
been contaminated by previous handling or environmental
11.4.1 Dry each specimen for 16 h in a vacuum oven at
exposure, from the test package of carbon-fiber yarn and
77°C (170°F) at a reduced pressure of 10 torr (1.3 kPa) or less.
discard. Form a small coil of fresh fiber weighing approxi-
11.4.2 After drying, weigh the specimen to the nearest 0.1
mately 2 g around two gloved fingers and tuck the ends in to
mg and record the weight, W . Weigh each specimen in a tared
d
obtain a specimen in the form of an easily handleable loop.
beaker or crucible.
9.2 Number of Specimens—For quality control purposes,
11.5 Testing—Procedure A (Short Term):
test a minimum of two specimens from each sample. For a
11.5.1 Preheat the air oven to 375°C (707°F) and make sure
quantitative assessment of the fiber performance, however, test
that the specimen positions in the oven are at 375 6
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