ASTM D3529/D3529M-97(2008)
(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
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D3529/D3529M–97 (Reapproved 2008)
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 (´) 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 C613/C613M TestMethodforConstituentContentofCom-
posite Prepreg by Soxhlet Extraction
1.1 This test method covers the determination of the matrix
D883 Terminology Relating to Plastics
solids content and matrix content of composite material
D3171 Test Methods for Constituent Content of Composite
prepregs. Volatiles content, if appropriate and required, is
Materials
determined by means of Test Method D3530/D3530M.
D3530/D3530M TestMethodforVolatilesContentofCom-
1.2 This test method focuses on thermosetting matrix ma-
posite Material Prepreg
terial systems for which matrix may be extracted in organic
D3878 Terminology for Composite Materials
solvent.However,other,unspecifiedreagentsmaybeusedwith
E177 Practice for Use of the Terms Precision and Bias in
this test method to extract other matrix material types for the
ASTM Test Methods
same purposes.
E1309 Guide for Identification of Fiber-Reinforced
1.3 This test method does not distinguish between hybrid
Polymer-Matrix Composite Materials in Databases
reinforcements or matrices. Its use with hybrids is limited to a
2.2 NFPA Standard:
determination of total reinforcement or matrix, or the use of a
NFPA 86 Standard for Ovens and Furnaces
standard factor to be used as the weight of a particular
reinforcement or matrix constituent.
3. Terminology
1.4 Alternate techniques for determining matrix and rein-
3.1 Definitions—Terminology D3878 defines terms relating
forcement content include Test Methods C613/C613M
to composite materials. Terminology D883 defines terms
(Soxhletextraction)andD3171(meanttypicallyforlaminates;
relating to plastics. Practice E177 defines terms relating to
covering matrix digestion or combustion).
statistics.Intheeventofaconflictbetweenterms,Terminology
1.5 The values stated in SI units are to be regarded as
D3878 shall have precedence over the other documents.
standard.
3.1.1 fiber content, n—the amount of fiber present in a
1.6 This standard does not purport to address all of the
composite or prepreg expressed either as percent by weight or
safety concerns, if any, associated with its use. It is the
percent by volume. See Terminology D3878.
responsibility of the user of this standard to establish appro-
3.1.2 matrix content, n—the amount of matrix present in a
priate safety and health practices and determine the applica-
composite or prepreg expressed either as percent by weight or
bility of regulatory limitations prior to use. Specific precau-
percentbyvolume.Forpolymermatrixcompositesthisisresin
tionary information is given in 8.2.4 and 8.2.5
content. See Terminology D3878.
2. Referenced Documents 3.1.3 prepreg, n—the admixture of fibrous reinforcement
andpolymericmatrixusedtofabricatecompositematerials.Its
2.1 ASTM Standards:
form may be sheet, tape, or tow. See Terminology D3878.
3.1.4 reinforcement content, n—the amount of reinforce-
This test method is under the jurisdiction of ASTM Committee D30 on ment present in a composite or prepreg expressed either as
Composite Materials and is the direct responsibility of Subcommittee D30.03 on
percent by weight or percent by volume.
Constituent/Precursor Properties.
3.1.4.1 Discussion—If fiber is the sole reinforcement, then
Current edition approved March 1, 2008. Published April 2008. Originally
fiber content is equal to reinforcement content. See Terminol-
approved in 1976. Last previous edition approved in 2003 as D3529/
´1
D3529M–97(2003) . DOI: 10.1520/D3529_D3529M-97R08.
ogy D3878.
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.
D3529/D3529M–97 (2008)
3.1.5 resin content, n—see matrix content. 6.2 Reagent Selection—The proper reagent, in a suitable
3.2 Definitions of Terms Specific to This Standard: quantity, must be selected for the constituents under test. The
3.2.1 dry resin content, n—a prepreg resin content calcu- reagents listed in Section 8 are provided for consideration,
latedbysubtractingtheaveragemasslossduetovolatilesfrom particularly with regard to thermosetting materials, but cannot
the initial test mass. be assured to perform well on all material systems within the
3.2.2 matrix solids content, n—see dry resin content. scope of this test method.
3.2.3 wet resin content, n—aprepregresincontentthatdoes
6.3 Ability of Solvent to Reach Matrix—Solvents are more
not account for mass loss due to volatiles. This is used
efficient if the material is spread as a film, rather than a solid
interchangeably with matrix content and resin content in this
mass. It is recommended that the sample be consolidated as
test method.
little as possible before introduction into the solvent.Asolvent
3.2.4 volatilescontent,n—theamountofvolatilespresentin
that is satisfactory for a given form may not be adequate with
a prepreg expressed as percent by weight.
the same material of a different form.
3.3 Symbols:
6.4 Solvent Strength—Solvent strength, or the ability to
3.3.1 M —mass of container.
c rapidlydissolvethematrix,maybeenhancedbyincreasingthe
3.3.2 M—initial mass of the specimen.
i amount of solvent, increasing agitation, increasing tempera-
3.3.3 M—final mass of specimen and container at end of
f ture,orbyplacingthesampleundervacuum.Theseareoffered
test.
as physical alternatives to use of more hazardous solvents, or
3.3.4 W —matrix content of specimen in weight percent.
m combined solvent systems.
3.3.5 W —matrix solids content of specimen in weight
ms
percent.
7. Apparatus
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 D3530/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
7.5 Fume Exhaust Hood.
mainly to thermosetting matrices.
7.6 Containers (Beakers, Flasks), borosilicate or suitable
plastic that is not dissolved by solvent. The container shall be
5. Significance and Use
ofasuitablevolumeforthesampleandsolvent(aminimumof
5.1 This test method can be used to obtain the matrix
250mLissuggested).Othersizesofcontainermayberequired
content or matrix solids content. Knowledge of the matrix
depending on sample size, and amount of solvent needed to
content or matrix solids content is useful in developing
complete the dissolution process.
optimum manufacturing processes. Where volatiles content is
7.7 Fritted Glass Crucibles or Sample Holder—The fritted
consistent and not critical to process, matrix content shall be
glass crucible filter shall be of a suitable porosity to allow
used.
dissolved matrix to pass while retaining reinforcement.
5.2 Thistestmethodislimitedtoreinforcementconstituents
7.8 Agitator—Mechanical shaker or ultrasonic bath. Mini-
that do not lose or gain weight upon exposure to solvent and
mum shaker speed recommended is 100 agitations or
matrix constituents that do not dissolve in the solvent. Alter-
revolutions/minute. Minimum frequency for ultrasonic bath
native methods or solvents should be used or an agreement
recommended is 40 kHz.
shouldbemadewiththeenduserforhowtoconsidertheeffect
7.9 Hot Plate—The hot plate shall have adjustable controls
of incomplete matrix dissolution or reinforcement weight
suitable for heating the solvent to its boiling point and be
change for reporting purposes.
capable of controlling the temperature to 615°C.
7.10 Vacuum Pump—Capable of delivering vacuum of at
6. Interferences
least 50 kPa.
6.1 Extent of Cure in Thermosetting Systems—The effi-
ciencyofmatrixdissolutionforthermosettingmatrixmaterials
8. Reagents
is directly related to the extent of cure of the resin system.
Resins that have started to cross link (such as B-staged resins) 8.1 Purity of Reagents—As a minimum, a technical-grade
will be increasingly more difficult to extract as the cure reagent is required to provide accurate results. However, when
advances. This test method may not be appropriate for such resolvingdisputesorperformingsubsequentanalysisofextract
materials; one of the methods of Test Method D3171 is then or residue, a reagent-grade reagent shall be used. Unless
recommended. otherwise indicated, it is intended that the reagent conform to
D3529/D3529M–97 (2008)
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 specimen size shal
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.