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ASTM D3529/D3529M-97(2003)e1

(Test Method)

Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg

Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg

SIGNIFICANCE AND USE
This test method can be used to obtain the matrix content or matrix solids content. Knowledge of the matrix content or matrix solids content is useful in developing optimum manufacturing processes. Where volatiles content is consistent and not critical to process, matrix content shall be used.
This test method is limited to reinforcement constituents that do not lose or gain weight upon exposure to solvent and matrix constituents that do not dissolve in the solvent. Alternative methods or solvents should be used or an agreement should be made with the end user for how to consider the effect of incomplete matrix dissolution or reinforcement weight change for reporting purposes.
SCOPE
1.1 This test method covers the determination of the matrix solids content and matrix content of composite material prepregs. Volatiles content, if appropriate and required, is determined by means of Test Method D 3530/D 3530M.
1.2 This test method focuses on thermosetting matrix material systems for which matrix may be extracted in organic solvent. However, other, unspecified reagents may be used with this test method to extract other matrix material types for the same purposes.
1.3 This test method does not distinguish between hybrid reinforcements or matrices. Its use with hybrids is limited to a determination of total reinforcement or matrix, or the use of a standard factor to be used as the weight of a particular reinforcement or matrix constituent.
1.4 Alternate techniques for determining matrix and reinforcement content include Test Methods C 613/C 613M (Soxhlet extraction) and D 3171 (meant typically for laminates; covering matrix digestion or combustion).
1.5 The values stated in SI units are to be regarded as standard.
1.6 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. Specific precautionary information is given in 8.2.4 and 8.2.5.

General Information

Status
Historical
Publication Date
30-Sep-2003
ICS
83.120 - Reinforced plastics
Technical Committee
D30 - Composite Materials
Drafting Committee
D30.03 - Constituent/Precursor Properties
Current Stage
Ref Project

Relations

Replaces
ASTM D3529/D3529M-97 - Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg
Effective Date
01-Oct-2003
Replaced By
ASTM D3529/D3529M-97(2008) - Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg
Effective Date
01-Mar-2008
Referred By
ASTM C1793-15 - Standard Guide for Development of Specifications for Fiber Reinforced Silicon Carbide-Silicon Carbide Composite Structures for Nuclear Applications
Effective Date
01-Oct-2003
Referred By
ASTM C1783-15 - Standard Guide for Development of Specifications for Fiber Reinforced Carbon-Carbon Composite Structures for Nuclear Applications
Effective Date
01-Oct-2003

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ASTM D3529/D3529M-97(2003)e1 - Standard Test Method for Matrix Solids Content and Matrix Content of Composite PrepregASTM D3529/D3529M-97(2003)e1 - Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg
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ASTM D3529/D3529M-97(2003)e1 - Standard Test Method for Matrix Solids Content and Matrix Content of Composite Prepreg
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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
e1
Designation:D3529/D3529M–97 (Reapproved 2003)
Standard Test Method for
Matrix Solids Content and Matrix Content of Composite
Prepreg
This standard is issued under the fixed designation D3529/D3529M; 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—Warning/precaution notes were moved into text editorially in October 2003.
1. Scope Composite Prepreg by Soxhlet Extraction
D883 Terminology Relating to Plastics
1.1 This test method covers the determination of the matrix
D3171 Test Method for Constituent Content of Composite
solids content and matrix content of composite material
Materials
prepregs. Volatiles content, if appropriate and required, is
D3530/D3530M Test Method for Volatiles Content of
determined by means of Test Method D3530/D3530M.
Composite Material Prepreg
1.2 This test method focuses on thermosetting matrix ma-
D3878 Terminology of Composite Materials
terial systems for which matrix may be extracted in organic
E177 Practice for Use of Terms Precision and Bias in
solvent.However,other,unspecifiedreagentsmaybeusedwith
ASTM Test Methods
this test method to extract other matrix material types for the
E1309 Guide for Identification of Composite Materials in
same purposes.
Computerized Property Databases
1.3 This test method does not distinguish between hybrid
2.2 NFPA Standard:
reinforcements or matrices. Its use with hybrids is limited to a
NFPA 86 Standard for Ovens and Furnaces
determination of total reinforcement or matrix, or the use of a
standard factor to be used as the weight of a particular
3. Terminology
reinforcement or matrix constituent.
3.1 Definitions—TerminologyD3878definestermsrelating
1.4 Alternate techniques for determining matrix and rein-
to composite materials. Terminology D883 defines terms
forcement content include Test Methods C 613/C 613M
relating to plastics. Practice E177 defines terms relating to
(Soxhlet extraction) and D3171 (meant typically for lami-
statistics.Intheeventofaconflictbetweenterms,Terminology
nates; covering matrix digestion or combustion).
D3878 shall have precedence over the other documents.
1.5 The values stated in SI units are to be regarded as
3.1.1 fiber content, n—the amount of fiber present in a
standard.
composite or prepreg expressed either as percent by weight or
1.6 This standard does not purport to address all of the
percent by volume. See Terminology D3878.
safety concerns, if any, associated with its use. It is the
3.1.2 matrix content, n—the amount of matrix present in a
responsibility of the user of this standard to establish appro-
composite or prepreg expressed either as percent by weight or
priate safety and health practices and determine the applica-
percentbyvolume.Forpolymermatrixcompositesthisisresin
bility of regulatory limitations prior to use. Specific precau-
content. See Terminology D3878.
tionary information is given in 8.2.4 and 8.2.5
3.1.3 prepreg, n—the admixture of fibrous reinforcement
2. Referenced Documents andpolymericmatrixusedtofabricatecompositematerials.Its
form may be sheet, tape, or tow. See Terminology D3878.
2.1 ASTM Standards:
3.1.4 reinforcement content, n—the amount of reinforce-
C613/C613M Test Method for Constituent Content of
ment present in a composite or prepreg expressed either as
percent by weight or percent by volume.
1 3.1.4.1 Discussion—If fiber is the sole reinforcement, then
This test method is under the jurisdiction of ASTM Committee D30 on
Composite Materials and is the direct responsibility of Subcommittee D30.03 on fiber content is equal to reinforcement content. See Terminol-
Constituent/Precursor Properties.
ogy D3878.
Current edition approved Oct. 1, 2003. Published October 2003. Originally
3.1.5 resin content, n—see matrix content.
approvedin1976.Lastpreviouseditionapprovedin1997asD3529/D3529M–97.
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 Available from National Fire Protection Association (NFPA), 1 Batterymarch
the ASTM website. Park, Quincy, MA 02269-9101.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
e1
D3529/D3529M–97 (2003)
3.2 Definitions of Terms Specific to This Standard: reagents listed in Section 8 are provided for consideration,
3.2.1 dry resin content, n—a prepreg resin content calcu- particularly with regard to thermosetting materials, but cannot
latedbysubtractingtheaveragemasslossduetovolatilesfrom
be assured to perform well on all material systems within the
the initial test mass.
scope of this test method.
3.2.2 matrix solids content, n—see dry resin content.
6.3 Ability of Solvent to Reach Matrix—Solvents are more
3.2.3 wet resin content, n—aprepregresincontentthatdoes
efficient if the material is spread as a film, rather than a solid
not account for mass loss due to volatiles. This is used
mass. It is recommended that the sample be consolidated as
interchangeably with matrix content and resin content in this
little as possible before introduction into the solvent.Asolvent
test method.
that is satisfactory for a given form may not be adequate with
3.2.4 volatilescontent,n—theamountofvolatilespresentin
the same material of a different form.
a prepreg expressed as percent by weight.
6.4 Solvent Strength—Solvent strength, or the ability to
3.3 Symbols:
rapidlydissolvethematrix,maybeenhancedbyincreasingthe
3.3.1 M —mass of container.
c
amount of solvent, increasing agitation, increasing tempera-
3.3.2 M—initial mass of the specimen.
i
ture,orbyplacingthesampleundervacuum.Theseareoffered
3.3.3 M—final mass of specimen and container at end of
f
as physical alternatives to use of more hazardous solvents, or
test.
combined solvent systems.
3.3.4 W —matrix content of specimen in weight percent.
m
3.3.5 W —matrix solids content of specimen in weight
ms
7. Apparatus
percent.
7.1 Cutting (Grooved) Template—Cutting templates shall
4. Summary of Test Method
vary no more than 0.4 mm from center line when used. This
4.1 Specimens of the prepreg are weighed and subjected to
givesamaximumerrorof2%.Thisisnotrequiredifacutting
solvent, that may be heated, until the matrix is dissolved. The
die is used.
dissolved matrix is rinsed from the reinforcement residue
7.2 Cutting Blade—Die cutting blades are recommended to
whichisthendriedandweighed.Thelossinmassisexpressed
provideaconsistentcutareaerrorfromsampletosampleofno
as matrix content, a percentage of the specimen mass.
greater than 0.05% of the target area. If a die is not available,
4.2 Where applicable, adjacent samples are tested for vola-
a single edged blade will be used.
tiles content according to D 3530/D3530M. A calculation of
7.3 Analytical Balance—The analytical balance shall be
amount of resin in the sample after volatiles content is
capable of reading to within 61 mg.
subtracted is expressed as matrix solids content, a percentage
7.4 Timer, accurate to nearest minute.
of specimen mass. The matrix solids content is applicable
mainly to thermosetting matrices.
7.5 Fume Exhaust Hood.
7.6 Containers (Beakers, Flasks), borosilicate or suitable
5. Significance and Use
plastic that is not dissolved by solvent. The container shall be
5.1 This test method can be used to obtain the matrix
ofasuitablevolumeforthesampleandsolvent(aminimumof
content or matrix solids content. Knowledge of the matrix
250mLissuggested).Othersizesofcontainermayberequired
content or matrix solids content is useful in developing
depending on sample size, and amount of solvent needed to
optimum manufacturing processes. Where volatiles content is
complete the dissolution process.
consistent and not critical to process, matrix content shall be
7.7 Fritted Glass Crucibles or Sample Holder—The fritted
used.
glass crucible filter shall be of a suitable porosity to allow
5.2 Thistestmethodislimitedtoreinforcementconstituents
dissolved matrix to pass while retaining reinforcement.
that do not lose or gain weight upon exposure to solvent and
7.8 Agitator—Mechanical shaker or ultrasonic bath. Mini-
matrix constituents that do not dissolve in the solvent. Alter-
mum shaker speed recommended is 100 agitations or
native methods or solvents should be used or an agreement
revolutions/minute. Minimum frequency for ultrasonic bath
shouldbemadewiththeenduserforhowtoconsidertheeffect
recommended is 40 kHz.
of incomplete matrix dissolution or reinforcement weight
change for reporting purposes.
7.9 Hot Plate—The hot plate shall have adjustable controls
suitable for heating the solvent to its boiling point and be
6. Interferences
capable of controlling the temperature to 615°C.
6.1 Extent of Cure in Thermosetting Systems—The effi-
7.10 Vacuum Pump—Capable of delivering vacuum of at
ciencyofmatrixdissolutionforthermosettingmatrixmaterials
least 50 kPa.
is directly related to the extent of cure of the resin system.
Resins that have started to cross link (such as B-staged resins)
8. Reagents
will be increasingly more difficult to extract as the cure
8.1 Purity of Reagents—As a minimum, a technical-grade
advances. This test method may not be appropriate for such
reagent is required to provide accurate results. However, when
materials; one of the methods of Test Method D3171 is then
recommended. resolvingdisputesorperformingsubsequentanalysisofextract
or residue, a reagent-grade reagent shall be used. Unless
6.2 Reagent Selection—The proper reagent, in a suitable
quantity, must be selected for the constituents under test. The otherwise indicated, it is intended that the reagent conform to
e1
D3529/D3529M–97 (2003)
the specifications of the Committee onAnalytical Reagents of 10. Test Specimens
theAmerican Chemical Society, where such specifications are
10.1 Aminimumofthreespecimensshallbetestedforeach
available.
sample.
8.2 MatrixDissolutionSolvents—Asuitablesolventshallbe
10.2 The
...

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1.3 Units—The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered 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.  
1.4 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.  
1.5 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.

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ASTM
ASTM D7028-07(2024)(Test Method)
Standard Test Method for Glass Transition Temperature (DMA Tg) of Polymer Matrix Composites by Dynamic Mechanical Analysis (DMA)

SIGNIFICANCE AND USE
5.1 This test method is designed to determine the glass transition temperature of continuous fiber reinforced polymer composites using the DMA method. The DMA Tg value is frequently used to indicate the upper use temperature of composite materials, as well as for quality control of composite materials.
SCOPE
1.1 This test method covers the procedure for the determination of the dry or wet (moisture conditioned) glass transition temperature (Tg) of polymer matrix composites containing high-modulus, 20 GPa (> 3 × 106 psi), fibers using a dynamic mechanical analyzer (DMA) under flexural oscillation mode, which is a specific subset of the Dynamic Mechanical Analysis (DMA) method.  
1.2 The glass transition temperature is dependent upon the physical property measured, the type of measuring apparatus and the experimental parameters used. The glass transition temperature determined by this test method (referred to as “DMA Tg”) may not be the same as that reported by other measurement techniques on the same test specimen.  
1.3 This test method is primarily intended for polymer matrix composites reinforced by continuous, oriented, high-modulus fibers. Other materials, such as neat resin, may require non-standard deviations from this test method to achieve meaningful results.  
1.4 The values stated in SI units are standard. The values given in parentheses are non-standard mathematical conversions to common units that are provided for information only.  
1.5 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.  
1.6 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.

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ASTM
ASTM C613-23(Test Method)
Standard Test Method for Constituent Content of Composite Prepreg by Soxhlet Extraction

SIGNIFICANCE AND USE
5.1 The prepreg volatiles content, matrix content, reinforcement content, and filler content of composite prepreg materials are used to control material manufacture and subsequent fabrication processes, and are key parameters in the specification and production of such materials, as well as in the fabrication of products made with such materials.  
5.2 The extraction products resulting from this test method (the extract, the residue, or both) can be analyzed to assess chemical composition and degree of purity.
SCOPE
1.1 This test method covers a Soxhlet extraction procedure to determine the matrix content, reinforcement content, and filler content of composite material prepreg. Volatiles content, if appropriate, and required, is determined by means of Test Method D3530.  
1.1.1 The reinforcement and filler must be substantially insoluble in the selected extraction reagent and any filler must be capable of being separated from the reinforcement by filtering the extraction residue.  
1.1.2 Reinforcement and filler content test results are total reinforcement content and total filler content; hybrid material systems with more than one type of either reinforcement or filler cannot be distinguished.  
1.2 This test method focuses on thermosetting matrix material systems for which the matrix may be extracted by an organic solvent. However, other, unspecified, reagents may be used with this test method to extract other matrix material types for the same purposes.  
1.3 Alternate techniques for determining matrix and reinforcement content include Test Methods D3171 (matrix digestion), D2584 (matrix burn-off/ignition), and D3529 (matrix dissolution and ignition loss). Test Method D2584 is preferred for reinforcement materials, such as glass, quartz, or silica, that are unaffected by high-temperature environments.  
1.4 The technical content of this standard has been stable since 1997 without significant objection from its stakeholders. As there is limited technical support for the maintenance of this standard, changes since that date have been limited to items required to retain consistency with other ASTM D30 Committee standards. The standard therefore should not be considered to include any significant changes in approach and practice since 1997. Future maintenance of the standard will only be in response to specific requests and performed only as technical support allows.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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. Specific precautionary statements are given in Section 9 and 7.2.3 and 8.2.1.  
1.7 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.

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ASTM
ASTM D6484/D6484M-23(Test Method)
Standard Test Method for Open-Hole Compressive Strength of Polymer Matrix Composite Laminates

SIGNIFICANCE AND USE
5.1 Refer to Guide D8509.
SCOPE
1.1 This test method determines the open-hole compressive strength of multidirectional polymer matrix composite laminates reinforced by high-modulus fibers. The composite material forms are limited to continuous-fiber or discontinuous-fiber (tape or fabric, or both) reinforced composites in which the laminate is balanced and symmetric with respect to the test direction. The range of acceptable test laminates and thicknesses are described in 8.2.1.  
1.2 Several related ASTM standards reference the procedures and apparatus described within this test method. In particular, the support fixture described in 7.2 is used by several other standards to stabilize compression-loaded test specimens. These include Practice D6742/D6742M, which covers filled-hole compression testing; Practice D7615/D7615M, which covers open-hole fatigue testing; and Practice D8066/D8066M, which covers unnotched laminate compression testing.  
1.3 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.  
1.3.1 Within the text, the inch-pound units are shown in brackets.  
1.4 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.  
1.5 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.

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