ASTM D4102/D4102M-22

Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers

SIGNIFICANCE AND USE
5.1 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, carbon fiber 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 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
1.2.1 Within the text, the inch-pound units are shown in brackets.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard information, see Section 8.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Published
• Publication Date: 30-Apr-2022
• ICS: 59.100.20 - Carbon materials
• Technical Committee: D30 - Composite Materials
• Drafting Committee: D30.03 - Constituent/Precursor Properties

Relations

• Refers: ASTM D3878-19a - Standard Terminology for Composite Materials
• Effective Date: 15-Oct-2019
• Refers: ASTM D3878-19 - Standard Terminology for Composite Materials
• Effective Date: 15-Apr-2019
• Refers: ASTM D3878-18 - Standard Terminology for Composite Materials
• Effective Date: 01-Apr-2018
• Refers: ASTM D3878-16 - Standard Terminology for Composite Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM D3878-15 - Standard Terminology for Composite Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM D3878-07(2013) - Standard Terminology for Composite Materials
• Effective Date: 01-May-2013
• Refers: ASTM C613/C613M-97(2008) - Standard Test Method for Constituent Content of Composite Prepreg by Soxhlet Extraction
• Effective Date: 01-Mar-2008
• Refers: ASTM D3878-07 - Standard Terminology for Composite Materials
• Effective Date: 01-May-2007
• Refers: ASTM D3878-04a - Standard Terminology for Composite Materials
• Effective Date: 01-May-2004
• Refers: ASTM D3878-04 - Standard Terminology for Composite Materials
• Effective Date: 01-Mar-2004
• Refers: ASTM C613/C613M-97(2003)e1 - Standard Test Method for Constituent Content of Composite Prepreg by Soxhlet Extraction
• Effective Date: 01-Oct-2003
• Refers: ASTM D3878-03a - Standard Terminology for Composite Materials
• Effective Date: 01-Oct-2003
• Refers: ASTM D3878-03 - Standard Terminology for Composite Materials
• Effective Date: 10-Jan-2003
• Refers: ASTM D3878-02a - Standard Terminology for Composite Materials
• Effective Date: 10-Dec-2002
• Refers: ASTM D3878-02 - Standard Terminology for Composite Materials
• Effective Date: 10-May-2002

Overview

ASTM D4102/D4102M-22: Standard Test Method for Thermal Oxidative Resistance of Carbon Fibers is a rigorous protocol developed by ASTM International. This standard specifies the required apparatus and procedures for characterizing the oxidative resistance of carbon fibers by measuring their weight loss after exposure to hot air under controlled conditions. The method is vital for material selection, quality control, and research of high-performance fiber-reinforced composites, where thermal stability is a critical factor.

Carbon fibers are extensively utilized in advanced composites for sectors requiring high strength-to-weight ratios and excellent performance at elevated temperatures, such as aerospace, automotive, and energy applications. ASTM D4102/D4102M-22 assists manufacturers and researchers in quantifying the material's resistance to oxidative environments, ensuring the selection of the most stable and durable fibers.

Key Topics

• Thermal Oxidative Resistance: This test determines how carbon fibers withstand degradation when exposed to high-temperature oxidative environments, a crucial factor for longevity and reliability in composite materials.
• Weight Loss Measurement: The primary metric is the percentage of weight loss in carbon fibers after controlled exposure to ambient hot air, indicating their oxidative stability.
• Test Conditions:
  • Accelerated Exposure: 24 hours at 375°C to simulate short-term thermal stress.
  • Extended Exposure: 500 hours at 315°C to represent long-term oxidative conditions.
• Specimen Preparation: Procedures are included for testing fibers as-received (with finish) and after finish removal, highlighting the influence of surface treatments and finishes on oxidative resistance.
• Variables to Report:
  • Fiber identification and precursor type (e.g., polyacrylonitrile, rayon, pitch)
  • Modulus of the fiber
  • Levels and types of impurities, especially metallic contaminants
  • Presence and type of fiber finish

Applications

The ASTM D4102/D4102M-22 standard serves multiple practical purposes for manufacturers, material scientists, and quality assurance professionals:

• Material Selection: Enables engineers to compare different grades and types of carbon fibers based on their resistance to oxidation, essential for selecting materials for high-temperature composites.
• Quality Control: Factories and suppliers can use this test method to verify the consistency and oxidative stability of fiber lots, ensuring uniformity in production.
• Product Specification: Clients in industries such as aerospace and automotive can require documented performance in oxidative resistance according to this standard.
• Research and Development: Scientists developing new or improved carbon fibers can benchmark performance improvements and understand the effects of precursor chemistry, finishing agents, and processing techniques.
• Assessment of Surface Treatments: By allowing testing with and without fiber finishes, the standard helps evaluate how surface treatments influence long-term stability and compatibility with composite matrices.

Related Standards

• ASTM C613/C613M: Test Method for Constituent Content of Composite Prepreg by Soxhlet Extraction, referenced for solvent extraction procedures and finish removal.
• ASTM D3878: Terminology for Composite Materials, providing definitions relevant to fiber-reinforced materials.
• Additional test methods and guidance may be found in standards concerning composite durability, surface characterization, and environmental performance.

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Keywords: ASTM D4102/D4102M-22, carbon fiber oxidative resistance, thermal stability, fiber-reinforced composites, ASTM carbon fiber standards, weight loss test, high-temperature composite materials, carbon fiber durability, finish effects on carbon fiber, composite material quality control.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4102/D4102M − 22
Standard Test Method for
Thermal Oxidative Resistance of Carbon Fibers
This standard is issued under the fixed designation D4102/D4102M; 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 3. Terminology
3.1 Definitions—Terminology in accordance with Terminol-
1.1 This test method covers the apparatus and procedure for
the determination of the weight loss of carbon fibers, exposed ogy D3878 shall be used where applicable.
to ambient hot air, as a means of characterizing their oxidative
3.2 Definitions of Terms Specific to This Standard:
resistance.
3.2.1 carbon fibers, n—fibers produced by the pyrolysis of
organicprecursorfiberssuchasrayon,polyacrylonitrile(PAN),
1.2 Units—The values stated in either SI units or inch-
and pitch in an inert atmosphere; carbon fibers typically are
pound units are to be regarded separately as standard. The
carbonized at about 1300 °C [2400 °F] and assay at 93 % or
values stated in each system are not necessarily exact equiva-
more carbon.
lents; therefore, to ensure conformance with the standard, each
system shall be used independently of the other, and values
3.2.2 finish, n—a material, with which filaments are treated,
from the two systems shall not be combined.
which contains a coupling agent to improve the bond between
1.2.1 Within the text, the inch-pound units are shown in
the filament surface and the resin matrix in a composite
brackets.
material; in addition, finishes often contain ingredients which
provide lubricity to the filament surface, preventing abrasive
1.3 This standard does not purport to address all of the
damage during handling, and a binder which promotes strand
safety concerns, if any, associated with its use. It is the
integrity and facilitates packing of the filaments.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
3.3 Symbols:
mine the applicability of regulatory limitations prior to use.
%CV—coefficient of variation
For specific hazard information, see Section 8.
N—number of test specimens
1.4 This international standard was developed in accor-
s—standard deviation
dance with internationally recognized principles on standard-
W —specimen weight after the hot air exposure
a
ization established in the Decision on Principles for the
W —specimen weight after drying
d
Development of International Standards, Guides and Recom-
W —percent weight loss in drying
dr
mendations issued by the World Trade Organization Technical
W —final specimen weight after the finish removal
e
Barriers to Trade (TBT) Committee.
W —percent finish on the fiber
f
W —percent weight loss in hot air
h
2. Referenced Documents
W—specimen weight before finish removal
i
X—average
2.1 ASTM Standards:
X—weight loss of the ith specimen
i
C613/C613M Test Method for Constituent Content of Com-
posite Prepreg by Soxhlet Extraction
4. Summary of Test Method
D3878 Terminology for Composite Materials
4.1 The test method is composed of two parts. The first one
specifies exposure conditions for an accelerated measurement,
determining weight loss of the carbon fiber after 24 h in air at
This test method is under the jurisdiction of ASTM Committee D30 on
375 °C [707 °F]. The second part specifies conditions for an
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
Constituent/Precursor Properties.
extended measurement, determining the weight loss resulting
Current edition approved May 1, 2022. Published May 2022. Originally
from 500 h exposure in air at 315 °C [600 °F].
approved in 1982. Last previous edition approved in 2015 as D4102 – 82(2015).
DOI: 10.1520/D4102_D4102M-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5. Significance and Use
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1 The test is used to determine the oxidative resistances of
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. carbon fibers as a means of selecting the most stable fibers for
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4102/D4102M − 22
incorporation in high-temperature fiber-reinforced composite approximately 2 g around two gloved fingers and tuck the ends
systems. It can be used for quality control, material in to obtain a specimen in the form of an easily handleable
specification, and for research and development of improved loop.
carbon fibers. Factors that influence the oxidative resistance
9.2 Number of Specimens—For quality control purposes,
and should be reported are fiber identification, carbon fiber
test a minimum of two specimens from each sample. For a
precursor type, fiber modulus, and any information on
quantitative assessment of the fiber performance, however, test
impurities, particularly metals. Also note that the presence of
a minimum of ten specimens and evaluate the results statisti-
finish on the fiber can affect the oxidative resistance, and thus,
cally as described in 12.4. It is recommended to report the
alternative specimen preparations that enable the evaluation of
method of sampling the specimens from the test package of
finish effects are included.
carbon fiber yarn (or tow); for example, spacing of specimens
or distribution of specimens along the length of the yarn (or
6. Apparatus
tow), or both.
6.1 The accuracy of all measuring equipment shall have
9.3 Finish Removal From the Fiber—Finish materials are
certified calibrations that are current at the time of use of the
generally present at about 1 % levels and are usually not stable
equipment.
at the exposure temperatures prescribed herein. The finish, if
6.2 Balance, capable of weighing to the nearest 0.1 mg. present, may be removed by extraction with hot solvent, such
as methyl ethyl ketone or dimethyl formamide (DMF). Soxhlet
6.3 Vacuum Oven, capable of providing vacuum of 1.3 kPa
extraction as described in Test Method C613/C613M is rec-
[0.19 psi] or less at 80 6 10 °C [177 6 18 °F].
ommended for difficult-to-remove finishes and as a reference
6.4 Circulating Air Oven, with sufficient flow rate and
control. However, other finishes may be extracted by the
capability to change the ambient air in the chamber once a
procedure given in 11.3.1 – 11.3.4.
minute, while maintaining the required temperature within
9.4 Finish Left on the Fiber—Since the fiber will normally
65°C [69 °F] in an operating range of 25 °C [77 °F] to
be used with the finish intact, it is most useful to know the
375 °C [707 °F].
oxidative resistance of the fiber containing finish. To charac-
6.5 Glass Beakers, borosilicate, 250 mL [8.45 oz], or other
terize and select fibers with optimum finishes, it is also very
size, appropriate for the oven (one per sample).
useful to know the relative effects of a variety of finishes. For
6.6 Wire Mesh Covers, for the beakers to reduce excessive this reason, it is desirable to have approaches for the determi-
air turbulence during the exposure. nation of oxidative resistance both with and without
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4102 − 82 (Reapproved 2015) D4102/D4102M − 22
Standard Test Method for
Thermal Oxidative Resistance of Carbon Fibers
This standard is issued under the fixed designation D4102;D4102/D4102M; 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
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 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values
givenstated in parentheses are mathematical conversions to inch-pound units which are provided for information only and are not
considered standard.each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each
system shall be used independently of the other, and values from the two systems shall not be combined.
1.2.1 Within the text, the inch-pound units are shown in brackets.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard information, see Section 8.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
C613/C613M Test Method for Constituent Content of Composite Prepreg by Soxhlet Extraction
D3878 Terminology for Composite Materials
3. Definitions
3.1 carbon fibers—fibers containing at least 90 % carbon by weight made by pyrolysis from synthetic polymeric or pitch fibers
and having moduli ≥70 GPa (≥10 psi).
3.2 precursor—organic fiber from which carbon fibers are prepared via pyrolysis. Polyacrylonitrile (PAN), rayon, and pitch are
commonly used.
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 Nov. 1, 2015May 1, 2022. Published December 2015May 2022. Originally approved in 1982. Last previous edition approved in 20082015 as
D4102 – 82(2008).(2015). DOI: 10.1520/D4102-82R15.10.1520/D4102_D4102M-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4102/D4102M − 22
3.3 fiber finish—surface coating applied to fibers to facilitate handling or provide better wetting and compatibility of fiber and
matrix, or both.
3. Terminology
3.1 Definitions—Terminology in accordance with Terminology D3878 shall be used where applicable.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 carbon fibers, n—fibers produced by the pyrolysis of organic precursor fibers such as rayon, polyacrylonitrile (PAN), and
pitch in an inert atmosphere; carbon fibers typically are carbonized at about 1300 °C [2400 °F] and assay at 93 % or more carbon.
3.2.2 finish, n—a material, with which filaments are treated, which contains a coupling agent to improve the bond between the
filament surface and the resin matrix in a composite material; in addition, finishes often contain ingredients which provide lubricity
to the filament surface, preventing abrasive damage during handling, and a binder which promotes strand integrity and facilitates
packing of the filaments.
3.3 Symbols:
%CV—coefficient of variation
N—number of test specimens
s—standard deviation
W —specimen weight after the hot air exposure
a
W —specimen weight after drying
d
W —percent weight loss in drying
dr
W —final specimen weight after the finish removal
e
W —percent finish on the fiber
f
W —percent weight loss in hot air
h
W —specimen weight before finish removal
i
X—average
X —weight loss of the ith specimen
i
4. Summary of Test Method
4.1 The test method is composed of two parts. The first one specifies exposure conditions for an accelerated measurement,
determining weight loss of the carbon fiber after 24 h in air at 375°C (707°F).375 °C [707 °F]. The second part specifies conditions
for an extended measurement, determining the weight loss resulting from 500-h500 h exposure in air at 315°C (600°F).315 °C
[600 °F].
5. Significance and Use
5.1 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, carbon fiber 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.
6. Apparatus
6.1 The accuracy of all measuring equipment shall have certified calibrations that are current at the time of use of the equipment.
6.2 Balance, capable of weighing to the nearest 0.1 mg.
6.3 Vacuum Oven, capable of providing vacuum of 10 torr (1.3 kPa) 1.3 kPa [0.19 psi] or less at 80°C (177°F).80 6 10 °C [177
6 18 °F].
6.4 Circulating Air Oven, with sufficient flow rate and capability to change the ambient air in the chamber once a minute, while
D4102/D4102M − 22
maintaining the temperature within 10°C (18°F) over the 25°C (77°F) to 375°C (707°F) range.required temperature within 65 °C
[69 °F] in an operating range of 25 °C [77 °F] to 375 °C [707 °F].
6.5 Glass Beakers, borosilicate, 250-mL (8.45 oz) 250 mL [8.45 oz], or other size, appropriate for the oven (one per sample).
6.6 Wire Mesh Covers, for the beakers to reduce excessive air turbulence during the exposure.
6.7 Boiling Flasks or Erlenmeyer Flasks, borosilicate glass, 250- or 500-mL (8.45- or 16.91-oz)250 or 500 mL [8.45 to 16.91 oz]
size, with standard-taper joint.
6.8 Glass Condensers, borosilicate for the above flasks.
6.9 Hot Plate.
6.10 Tweezers, stainless steel.
7. Reagents and Materials
7.1 Methyl Ethyl Ketone (2-butanone) 99.5 % pure, boiling range 70.0 to 81.0°C (15881.0 °C [158 to 177.8°F),177.8 °F], or other
suitable solvents recommended in Test Method C613/C613M.
8. Hazards
8.1 The methyl ethyl ketone, classified as an irritant and a fire hazard, should be handled in a well-ventilated area and should not
be exposed to direct heat or open flame.
9. Test Specimen and Sampling
9.1 Using clean gloves to prevent any contamination, particularly with salt, unwrap the outer layers, which may have been
contaminated by previous handling or environmental exposure, from the test package of carbon-fiber yarn carbon fiber yarn (or
tow) and discard. Form a small coil of fresh fiber weighing approximately 2 g around two gloved fingers and tuck the ends in to
obtain a specimen in the form of an easily handleable loop.
9.2 Number of Specimens—For quality control purposes, test a minimum of two specimens from each sample. For a quantitative
assessment of the fiber performance, however, test a minimum of ten specimens and evaluate the results statistically as
...