ASTM D4102-82(1999)e1

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 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

• Status: Historical
• Publication Date: 22-Mar-1982
• ICS: 59.100.20 - Carbon materials
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Relations

• Replaces: ASTM D4102-82(1999) - Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
• Effective Date: 23-Mar-1982
• Replaced By: ASTM D4102-82(2004) - Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers
• Effective Date: 01-Oct-2004
• Referred By: ASTM D4762-18 - Standard Guide for Testing Polymer Matrix Composite Materials
• Effective Date: 23-Mar-1982

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
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Designation: D 4102 – 82 (Reapproved 1999)
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.
e NOTE—Section 1.2 was added editorially in July 2003 to address SI units, per Part H of the Form and Style for ASTM
Standards. Other editorial changes were made throughout in July 2003.
1. Scope determining weight loss of the carbon fiber after 24 h in air at
375°C (707°F). The second part specifies conditions for an
1.1 This test method covers the apparatus and procedure for
extended measurement, determining the weight loss resulting
the determination of the weight loss of carbon fibers, exposed
from 500-h exposure in air at 315°C (600°F).
to ambient hot air, as a means of characterizing their oxidative
resistance.
5. Significance and Use
1.2 The values stated in SI units are to be regarded as
5.1 The test is used to determine the oxidative resistances of
standard. The values given in parentheses are mathematical
carbon fibers as a means of selecting the most stable fibers for
conversions to inch-pound units which are provided for infor-
incorporation in high-temperature fiber-reinforced composite
mation only and are not considered standard.
systems. It can be used for quality control, material specifica-
1.3 This standard does not purport to address all of the
tion, and for research and development of improved carbon
safety concerns, if any, associated with its use. It is the
fibers. Factors that influence the oxidative resistance and
responsibility of the user of this standard to establish appro-
should be reported are fiber identification, precursor type, fiber
priate safety and health practices and determine the applica-
modulus, and any information on impurities, particularly
bility of regulatory limitations prior to use. For specific hazard
metals. IAlso note that the presence of finish on the fiber can
information, see Section 8.
affect the oxidative resistance, and thus, alternative specimen
2. Referenced Documents preparations that enable the evaluation of finish effects are
included.
2.1 ASTM Standards:
C 613 Test Method for Resin Content of Carbon and Graph-
6. Apparatus
ite Prepregs by Solvent Extraction
6.1 Balance, capable of weighing to the nearest 0.1 mg.
3. Definitions 6.2 Vacuum Oven, capable of providing vacuum of 10 torr
(1.3 kPa) or less at 80°C (177°F).
3.1 carbon fibers—fibers containing at least 90 % carbon by
6.3 Circulating Air Oven, with sufficient flow rate and
weight made by pyrolysis from synthetic polymeric or pitch
capability to change the ambient air in the chamber once a
fibers and having moduli $70 GPa ($10 psi).
minute, while maintaining the temperature within 10°C (18°F)
3.2 precursor—organic fiber from which carbon fibers are
over the 25°C (77°F) to 375°C (707°F) range.
prepared via pyrolysis. Polyacrylonitrile (PAN), rayon, and
6.4 Glass Beakers, borosilicate, 250-mL (8.45 oz) or other
pitch are commonly used.
size, appropriate for the oven (one per sample).
3.3 fiber finish—surface coating applied to fibers to facili-
6.5 Wire Mesh Covers, for the beakers to reduce excessive
tate handling or provide better wetting and compatibility of
air turbulence during the exposure.
fiber and matrix, or both.
6.6 Boiling Flasks or Erlenmeyer Flasks, borosilicate glass,
4. Summary of Test Method 250- or 500-mL (8.45- or 16.91-oz) size, with standard-taper
joint.
4.1 The method is composed of two parts. The first one
6.7 Glass Condensers, borosilicate for the above flasks.
specifies exposure conditions for an accelerated measurement,
6.8 Hot Plate.
6.9 Tweezers, stainless steel.
This test method is under the jurisdiction of ASTM Committee D30 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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 4102 – 82 (1999)
7. Reagents and Materials 11.3.1 Put the specimen in a dry flask and cover with 100 to
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.
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.
11.3.3 Weigh the dried specimen to the nearest 0.1 mg.
9. Test Specimen and Sampling
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 .
e
been contaminated by previous handling or environmental
11.4 Drying:
exposure, from the test package of carbon-fiber yarn and
11.4.1 Dry each specimen for 16 h in a vacuum oven at
discard. Form a small coil of fresh fiber weighing approxi-
77°C (170°F) at a reduced pressure of 10 torr (1.3 kPa) or less.
mately 2 g around two gloved fingers and tuck the ends in to
11.4.2 After drying, weigh the specimen to the nearest 0.1
obtain a specimen in the form of an easily handleable loop.
mg and record the weight, W . Weigh each specimen in a tared
d
9.2 Number of Specimens—For quality control purposes,
beaker or crucible.
test a minimum of two specimens from each sample. For
...