ASTM D4102-82(2004)
(Test Method)Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
SIGNIFICANCE AND USE
The test is used to determine the oxidative resistances of carbon fibers as a means of selecting the most stable fibers for incorporation in high-temperature fiber-reinforced composite systems. It can be used for quality control, material specification, and for research and development of improved carbon fibers. Factors that influence the oxidative resistance and should be reported are fiber identification, precursor type, fiber modulus, and any information on impurities, particularly metals. Also note that the presence of finish on the fiber can affect the oxidative resistance, and thus, alternative specimen preparations that enable the evaluation of finish effects are included.
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 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversions to inch-pound units which are provided for information only and are not considered standard.
1.3 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
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4102–82 (Reapproved 2004)
Standard Test Method for
Thermal Oxidative Resistance of Carbon Fibers
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 4. Summary of Test Method
1.1 This test method covers the apparatus and procedure for 4.1 The test method is composed of two parts. The first one
the determination of the weight loss of carbon fibers, exposed specifies exposure conditions for an accelerated measurement,
to ambient hot air, as a means of characterizing their oxidative determining weight loss of the carbon fiber after 24 h in air at
resistance. 375°C (707°F). The second part specifies conditions for an
1.2 The values stated in SI units are to be regarded as extended measurement, determining the weight loss resulting
standard. The values given in parentheses are mathematical from 500-h exposure in air at 315°C (600°F).
conversions to inch-pound units which are provided for infor-
5. Significance and Use
mation only and are not considered standard.
1.3 This standard does not purport to address all of the 5.1 The test is used to determine the oxidative resistances of
carbon fibers as a means of selecting the most stable fibers for
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- incorporation in high-temperature fiber-reinforced composite
systems. It can be used for quality control, material specifica-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard tion, and for research and development of improved carbon
fibers. Factors that influence the oxidative resistance and
information, see Section 8.
should be reported are fiber identification, precursor type, fiber
2. Referenced Documents
modulus, and any information on impurities, particularly
2.1 ASTM Standards: metals. Also note that the presence of finish on the fiber can
C 613/C 613M Test Method for Constituent Content of affect the oxidative resistance, and thus, alternative specimen
Composite Prepreg by Soxhlet Extraction preparations that enable the evaluation of finish effects are
included.
3. Definitions
6. Apparatus
3.1 carbon fibers—fiberscontainingatleast90 %carbonby
weight made by pyrolysis from synthetic polymeric or pitch 6.1 Balance, capable of weighing to the nearest 0.1 mg.
fibers and having moduli$70 GPa ($10 psi). 6.2 Vacuum Oven, capable of providing vacuum of 10 torr
3.2 precursor—organic fiber from which carbon fibers are (1.3 kPa) or less at 80°C (177°F).
prepared via pyrolysis. Polyacrylonitrile (PAN), rayon, and 6.3 Circulating Air Oven, with sufficient flow rate and
pitch are commonly used. capability to change the ambient air in the chamber once a
3.3 fiber finish—surface coating applied to fibers to facili- minute, while maintaining the temperature within 10°C (18°F)
tate handling or provide better wetting and compatibility of over the 25°C (77°F) to 375°C (707°F) range.
fiber and matrix, or both. 6.4 Glass Beakers, borosilicate, 250-mL (8.45 oz) or other
size, appropriate for the oven (one per sample).
6.5 Wire Mesh Covers, for the beakers to reduce excessive
This test method is under the jurisdiction of ASTM Committee D30 on air turbulence during the exposure.
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
6.6 Boiling Flasks or Erlenmeyer Flasks, borosilicate glass,
Constituent/Precursor Properties.
250- or 500-mL (8.45- or 16.91-oz) size, with standard-taper
Current edition approved Oct. 1, 2004. Published October 2004. Originally
joint.
approved in 1982. Last previous edition approved in 1999 as D 4102 – 82 (1999).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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 20-mesh nickel-chromium wire gauze from Fisher Scientific Co. has been
the ASTM website. found satisfactory for this purpose.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4102–82 (2004)
6.7 Glass Condensers, borosilicate for the above flasks. C 613M or follow Steps 11.3.1-11.3.4. If finish is not to be
6.8 Hot Plate. removed, skip Steps 11.3.1-11.3.4 and proceed with Step 11.4.
6.9 Tweezers, stainless steel.
11.3 Removal of the Finish:
11.3.1 Put the specimen in a dry flask and cover with 100 to
7. Reagents and Materials
200 mL(3.38 to 6.76 oz) of methyl ethyl ketone solvent. Place
7.1 Methyl Ethyl Ketone (2-butanone) 99.5 % pure, boiling
the condenser onto the flask and start the cooling water. Heat
range 70.0 to 81.0°C (158 to 177.8°F), or other suitable
the flask on the hot plate or heating bath to bring the solvent to
solvents recommended in Test Method C 613/C 613M.
boil. Soak the specimen in the boiling solvent for 15 min.Take
off the condenser, decant the solvent, and remove the speci-
8. Hazards
men.
8.1 The methyl ethyl ketone, classified as an irritant and a
11.3.2 Dry the specimen in the vacuum oven at 77°C
fire hazard, should be handled in a well-ventilated area and
(170°F) at a reduced pressure of 10 torr (1.3 kPa) or less for 30
should not be exposed to direct heat or open flame.
min.
9. Test Specimen and Sampling 11.3.3 Weigh the dried specimen to the nearest 0.1 mg.
Record the weight.
9.1 Using clean gloves to prevent any contamination, par-
11.3.4 Repeat Steps 11.3.1-11.3.3 until the weight remains
ticularly with salt, unwrap the outer layers, which may have
constant, within 60.1 mg. Record the final weight, W .
been contaminated by previous handling or environmental
e
exposure, from the test package of carbon-fiber yarn and
11.4 Drying:
discard. Form a small coil of fresh fiber weighing approxi-
11.4.1 Dry each specimen for 16 h in a vacuum oven at
mately 2 g around two gloved fingers and tuck the ends in to
77°C (170°F) at a reduced pressure of 10 torr (1.3 kPa) or less.
obtain a specimen in the form of an easily handleable loop.
11.4.2 After drying, w
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