ASTM D3529/D3529M-97
(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
SCOPE
1.1 This test method covers the determination of the resin solids content of epoxy-matrix prepreg tape and sheet. The reinforcement material type is limited to those which are substantially unaffected by the solvents selected for use in dissolving the matrix material.
1.2 The values stated in either SI units or inch-pound units are to be regarded separately as standard. Within the text, the inch-pound units are shown in brackets. The values stated in each system are not exact equivalents; therefore, each system must be used independently of the other. Combining values from the two systems may result in nonconformance with the standard.
1.2 This standard does not purport to address all of the safety problems 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 hazards statements, see Note 1.
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Standards Content (Sample)
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Designation: D 3529/D3529M – 97
Standard Test Method for
Matrix Solids Content and Matrix Content of Composite
Prepreg
This standard is issued under the fixed designation D 3529/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.
1. Scope Composite Material Prepreg
D 3878 Terminology of High-Modulus Reinforcing Fibers
1.1 This test method covers the determination of the matrix
and Their Composites
solids content and matrix content of composite material
E 177 Practice for Use of Terms Precision and Bias in
prepregs. Volatiles content, if appropriate and required, is
ASTM Test Methods
determined by means of Test Method D 3530/D 3530M.
E 1309 Guide for Identification of Composite Materials in
1.2 This test method focuses on thermosetting matrix ma-
Computerized Property Databases
terial systems for which matrix may be extracted in organic
2.2 NFPA Standard:
solvent. However, other, unspecified, reagents may be used
NFPA 86 Standard for Ovens and Furnaces
with this test method to extract other matrix material types for
the same purposes.
3. Terminology
1.3 This test method does not distinguish between hybrid
3.1 Definitions—Terminology D 3878 defines terms relating
reinforcements or matrices. Its use with hybrids is limited to a
to composite materials. Terminology D 883 defines terms
determination of total reinforcement or matrix, or the use of a
relating to plastics. Practice E 177 defines terms relating to
standard factor to be used as the weight of a particular
statistics. In the event of a conflict between terms, Terminology
reinforcement or matrix constituent.
D 3878 shall have precedence over the other documents.
1.4 Alternate techniques for determining matrix and rein-
3.1.1 fiber content, n—the amount of fiber present in a
forcement content include Test Methods C 613 (Soxhlet ex-
composite or prepreg expressed either as percent by weight or
traction) and D 3171 (meant typically for laminates; covering
percent by volume. See Terminology D 3878.
matrix digestion or combustion).
3.1.2 matrix content, n—the amount of matrix present in a
1.5 The values stated in SI units are to be regarded as
composite or prepreg expressed either as percent by weight or
standard.
percent by volume. For polymer matrix composites this is resin
1.6 This standard does not purport to address all of the
content. See Terminology D 3878.
safety concerns, if any, associated with its use. It is the
3.1.3 prepreg, n—the admixture of fibrous reinforcement
responsibility of the user of this standard to establish appro-
and polymeric matrix used to fabricate composite materials. Its
priate safety and health practices and determine the applica-
form may be sheet, tape or tow. See Terminology D 3878.
bility of regulatory limitations prior to use. Specific precau-
3.1.4 reinforcement content, n—the amount of reinforce-
tionary information is given in Notes 1 and 2 and Section 8.
ment present in a composite or prepreg expressed either as
2. Referenced Documents percent by weight or percent by volume.
3.1.4.1 Discussion—If fiber is the sole reinforcement, then
2.1 ASTM Standards:
fiber content is equal to reinforcement content. See Terminol-
C 613 Test Method for Constituent Content of Composite
2 ogy D 3878.
Prepreg by Soxhlet Extraction
3.1.5 resin content, n—see matrix content.
D 883 Terminology Relating to Plastics
3.2 Definitions of Terms Specific to This Standard:
D 3171 Test Method for Fiber Content of Resin-Matrix
3.2.1 dry resin content, n—a prepreg resin content calcu-
Composites by Matrix Digestion
lated by subtracting the average mass loss due to volatiles from
D 3530/D3530M Test Method for Volatiles Content of
the initial test mass.
3.2.2 matrix solids content, n—see dry resin content.
Test Method D 3529/D 3529M is under the jurisdiction of ASTM Committee
D-30 on Composites and is the direct responsibility of Subcommittee D30.03 on
Constituent/Precursor Properties.
Current edition approved Sept. 10, 1997. Published June 1998. Originally Annual Book of ASTM Standards, Vol 14.02.
published as D 3529 – 76. Last previous edition D 3529/D 3529M – 90. Annual Book of ASTM Standards, Vol 14.01.
2 6
Annual Book of ASTM Standards, Vol 15.03. Available from National Fire Protection Association, Batterymarch Park,
Annual Book of ASTM Standards, Vol 08.01. Quincy, MA.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 3529/D3529M
3.2.3 wet resin content, n—a prepreg resin content that does particularly with regard to thermosetting materials, but cannot
not account for mass loss due to volatiles. This is used be assured to perform well on all material systems within the
interchangeably with matrix content and resin content in this scope of this test method.
test method. 6.3 Ability of Solvent to Reach Matrix—Solvents are more
3.2.4 volatiles content, n—the amount of volatiles present in efficient if the material is spread as a film, rather than a solid
a prepreg expressed as percent by weight. mass. It is recommended that the sample be consolidated as
3.3 Symbols: little as possible before introduction into the solvent. A solvent
3.3.1 M —mass of container. that is satisfactory for a given form may not be adequate with
c
3.3.2 M —initial mass of the specimen. the same material of a different form.
i
3.3.3 M —final mass of specimen and container at end of 6.4 Solvent Strength—Solvent strength, or the ability to
f
test. rapidly dissolve the matrix, may be enhanced by increasing the
3.3.4 W —matrix content of specimen in weight percent. amount of solvent, increasing agitation, increasing tempera-
m
3.3.5 W —matrix solids content of specimen in weight ture, or by placing the sample under vacuum. These are offered
ms
percent. as physical alternatives to use of more hazardous solvents, or
combined solvent systems.
4. Summary of Test Method
7. Apparatus
4.1 Specimens of the prepreg are weighed and subjected to
solvent, that may be heated, until the matrix is dissolved. The 7.1 Cutting (Grooved) Template—Cutting templates shall
vary no more than 0.4 mm from center line when used. This
dissolved matrix is rinsed from the reinforcement residue
which is then dried and weighed. The loss in mass is expressed gives a maximum error of 2 %. This is not required if a cutting
as matrix content, a percentage of the specimen mass. die is used.
4.2 Where applicable, adjacent samples are tested for vola- 7.2 Cutting Blade—Die cutting blades are recommended to
tiles content according to D 3530/D 3530M. A calculation of provide a consistent cut area error from sample to sample of no
amount of resin in the sample after volatiles content is greater than 0.05 % of the target area. If a die is not available,
subtracted is expressed as matrix solids content, a percentage a single edged blade will be used.
of specimen mass. The matrix solids content is applicable 7.3 Analytical Balance—The analytical balance shall be
mainly to thermosetting matrices. capable of reading to within 61 mg.
7.4 Timer, accurate to nearest minute.
5. Significance and Use
7.5 Fume Exhaust Hood.
5.1 This test method can be used to obtain the matrix
7.6 Containers (Beakers, Flasks), borosilicate or suitable
content or matrix solids content. Knowledge of the matrix plastic that is not dissolved by solvent. The container shall be
content or matrix solids content is useful in developing of a suitable volume for the sample and solvent (a minimum of
optimum manufacturing processes. Where volatiles content is 250 mL is suggested). Other sizes of container may be required
consistent and not critical to process, matrix content shall be depending on sample size, and amount of solvent needed to
used. complete the dissolution process.
5.2 This test method is limited to reinforcement constituents 7.7 Fritted Glass Crucibles or Sample Holder—The fritted
that do not lose or gain weight upon exposure to solvent and glass crucible filter shall be of a suitable porosity to allow
matrix constituents that do not dissolve in the solvent. Alter- dissolved matrix to pass while retaining reinforcement.
native methods or solvents should be used or an agreement 7.8 Agitator—Mechanical shaker or ultrasonic bath. Mini-
should be made with the end user for how to consider the effect mum shaker speed recommended is 100 agitations or
of incomplete matrix dissolution or reinforcement weight
revolutions/minute. Minimum frequency for ultrasonic bath
change for reporting purposes. recommended is 40 kHz.
7.9 Hot Plate—The hot plate shall have adjustable controls
6. Interferences
suitable for heating the solvent to its boiling point and be
6.1 Extent of Cure in Thermosetting Systems—The effi-
capable of controlling the temperature to 615°C.
ciency of matrix dissolution for thermosetting matrix materials
7.10 Vacuum Pump—Capable of delivering vacuum of at
is directly related to the extent of cure of the resin system.
least 50 kPa.
Resins that have started to cross link (such as B-staged resins)
8. Reagents
will be increasingly more difficult to extract as the cure
advances. This test method may not be appropriate for such 8.1 Purity of Reagents—As a minimum, a technical-grade
materials; one of the methods of Test Method D 3171 is then reagent is required to provide accurate results. However, when
recommended. resolving disputes or performing subsequent analysis of extract
6.2 Reagent Selection—The proper reagent, in a suitable or residue, a reagent-grade reagent shall be used. Unless
quantity, must be selected for the constituents under test. The otherwise indicated, it is intended that the reagent conform to
reagents listed in Section 8 are provided for consideration, the specifications of the Committee on Analytical Reagents of
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 3529/D3529M
the American Chemical Society, where such specifications are 10.2 The specimen size shall be a minimum of 6400 mm .
available. Minimum mass of the specimen shall be 1 g.
8.2 Matrix Dissolution Solvents—A suitable sol
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