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Designation: D3171 − 15

Standard Test Methods for

Constituent Content of Composite Materials1
This standard is issued under the fixed designation D3171; 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 1.2 The values stated in SI units are to be regarded as

standard. No other units of measurement are included in this
1.1 These test methods determine the constituent content of
standard.
composite materials by one of two approaches. Test Method I
physically removes the matrix by digestion or ignition or 1.3 This standard does not purport to address all of the
carbonization by one of eight procedures, leaving the rein- safety concerns, if any, associated with its use. It is the
forcement essentially unaffected and thus allowing calculation responsibility of the user of this standard to establish appro-
of reinforcement or matrix content (by weight or volume) as priate safety and health practices and determine the applica-
well as percent void volume. Test Method II, applicable only to bility of regulatory limitations prior to use. See Section 9 for
laminate materials of known fiber areal weight, calculates additional information.
reinforcement or matrix content (by weight or volume), and the
2. Referenced Documents
cured ply thickness, based on the measured thickness of the
laminate. Test Method II is not applicable to the measurement 2.1 ASTM Standards:2
of void volume. D792 Test Methods for Density and Specific Gravity (Rela-
1.1.1 These test methods are primarily intended for two-part tive Density) of Plastics by Displacement
composite material systems. However, special provisions can D883 Terminology Relating to Plastics
be made to extend these test methods to filled material systems D1505 Test Method for Density of Plastics by the Density-
with more than two constituents, though not all test results can Gradient Technique
be determined in every case. D3878 Terminology for Composite Materials
D5229/D5229M Test Method for Moisture Absorption Prop-
1.1.2 The procedures contained within have been designed erties and Equilibrium Conditioning of Polymer Matrix
to be particularly effective for certain classes of polymer or Composite Materials
metal matrices. The suggested applications are discussed in E12 Terminology Relating to Density and Specific Gravity
Section 4, as well as at the start of each procedure. of Solids, Liquids, and Gases (Withdrawn 1996)3
1.1.3 Test Method I assumes that the reinforcement is E177 Practice for Use of the Terms Precision and Bias in
essentially unaffected by the digestion or ignition medium or ASTM Test Methods
carbonization. A procedure for correction of the results for E1309 Guide for Identification of Fiber-Reinforced
minor changes in the reinforcement is included. Procedures A Polymer-Matrix Composite Materials in Databases
through F are based on chemical removal of the matrix while
Procedure G removes the matrix by igniting the matrix in a 3. Terminology
furnace. Procedure H carbonizes the matrix in a furnace. 3.1 Definitions—Terminology D3878 defines terms relating
1.1.4 Test Method II assumes that the fiber areal weight of to composite materials. Terminology D883 defines terms
the reinforcement material form is known or controlled to an relating to plastics. Terminology E12 defines terms relating to
acceptable tolerance. The presence of voids is not measured. specific gravity. Practice E177 defines terms relating to statis-
Eq 15 and 16 assume zero void content to perform the tics. In the event of a conflict between terms, Terminology
calculation. D3878 shall have precedence over other documents.

1 2
These test methods are under the jurisdiction of ASTM Committee D30 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Composite Materials and are the direct responsibility of Subcommittee D30.04 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Lamina and Laminate Test Methods. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 1, 2015. Published May 2015. Originally the ASTM website.
3
approved in 1973. Last previous edition approved in 2011 as D3171 – 11. DOI: The last approved version of this historical standard is referenced on
10.1520/D3171-15. www.astm.org.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D3171 − 15
3.1.1 fiber content, n—the amount of fiber present in a 4. Summary of Test Method
composite or prepreg expressed either as percent by weight or 4.1 Test Method I—The matrix portion of a material speci-
percent by volume. This is sometimes stated as a fraction. If no men of known mass is removed in a hot liquid medium (for
fillers exist, this is equivalent to reinforcement content. D3878 dissolution) or furnace (for combustion). When dissolving in a
3.1.2 matrix content, n—the amount of matrix present in a hot liquid medium, the remaining residue, containing the
composite or prepreg expressed either as percent by weight or reinforcement, is then filtered, washed, dried, cooled, and
percent by volume. For polymer matrix composites this is resin weighed. The weight percent of the reinforcement is
content. D3878 calculated, and from this value, and if densities of both the
composite and the reinforcement are known, the volume
3.1.3 reinforcement content, n—the amount of nonmatrix percent is calculated. An additional calculation for void volume
material (fiber and filler) in a composite or prepreg expressed may be made if the density of the matrix is known or
either as percent by weight or percent by volume. D3878 determined.
3.1.4 resin content, n—See matrix content. D3878 4.1.1 A correction for weight change of the reinforcement or
3.1.5 void volume, n—the volume in the specimen without retention of the matrix may be made (13.1.2 and 13.1.3), if this
mass, that is identified as neither matrix nor reinforcement. change is sufficiently reproducible under the conditions of the
D3878 test and has the same value for the reinforcement or matrix
alone as for the constituents in the composite.
3.2 Definitions of Terms Specific to This Standard: 4.1.1.1 Procedure A, for matrices such as epoxy resin, steel,
3.2.1 density, ρ23°C—the weight per unit volume measured copper, or others digestible by concentrated nitric acid.
in air, of the impermeable portion of a material at 23°C.
NOTE 1—Many reinforcements are attacked by nitric acid. If reinforce-
3.2.1.1 Discussion—The definition of specific gravity and ment is attacked, an alternative method is recommended, depending on the
density are essentially equivalent to the definitions of apparent matrix. See Annex A1.
specific gravity and apparent density in Terminology E12, 4.1.1.2 Procedure B, for matrices such as epoxy, phenolic,
because no correction is made for buoyancy of the material in polyamide, or thermoplastic resin, or others digestible by an
air. However, this difference is insignificant for most engineer- aqueous mixture of sulfuric acid and hydrogen peroxide. See
ing purposes. Annex A2.
3.2.2 specific gravity, SG23°C—the ratio of the weight in air 4.1.1.3 Procedure C, for matrices such as epoxy resin and
of a unit volume of the impermeable portion of a material at others digestible by a mixture of ethylene glycol and potassium
23°C referenced to the standard unit volume weight of water at hydroxide. See Annex A3.
23°C. NOTE 2—Procedure C is especially applicable to anhydride-cured
3.3 Symbols: epoxy systems containing aramid or carbon reinforcement.
4.1.1.4 Procedure D, for matrices such as aluminum, brass,
A = area of the specimen. or others digestible by sodium hydroxide solution. See Annex
Ar = calculated mass of one layer of reinforcement/unit A4.
area. 4.1.1.5 Procedure E, for matrices such as steel, titanium,
CR = carbonization ratio of the neat resin
copper, aluminum, or others digestible by hydrochloric acid.
ρc = density of the composite specimen.
ρm = density of the cured matrix. See Annex A5.
ρr = density of the reinforcement or fiber. 4.1.1.6 Procedure F, a version of Procedure A for
h = thickness of the specimen. microwave-aided heating. See Annex A6.
hp = cured ply thickness, mm. 4.1.1.7 Procedure G, for reinforcements such as glass, or
mc = mass of the dry crucible for neat resin carbonization ceramic that are not affected by high-temperature
mcr = mass of the dry crucible with carbonized neat resin environments, or reinforcements such as carbon where tem-
md = final mass of the neat resin residue after carbonization perature is adequately controlled so that reinforcement does not
mi = initial mass of the neat resin specimen char. See Annex A7.
Mc = mass of the dry crucible or sintered glass filter. 4.1.1.8 Procedure H, for any reinforcements, particularly
Mcr = mass of the dry crucible or sintered glass filter with carbon, that are not affected at high temperature in a nitrogen
reinforcement residue. atmosphere, and any resin matrix systems. The correction for
Md = final residue mass of the composite specimen the retention of the matrix (13.1.3) is not necessary for this
Mi = initial mass of specimen before digestion or combus- procedure. See Annex A8.
tion.
Mf = final mass of specimen after digestion or combustion. 4.2 Test Method II—The thickness of a relatively flat panel
Mm = mass of the resin matrix in the composite specimen made with reinforcement of known and consistent areal weight
Np = number of plies in the laminate. is measured. By the thickness of the panel, the reinforcement
Vm = volume percent of matrix in specimen. and matrix content is calculated.
Vr = volume percent of reinforcement in the specimen.
Vv = void volume percent in the specimen. 5. Significance and Use
Wm = weight percent of matrix in the specimen. 5.1 A constituent content of a composite material must be
Wr = weight percent of reinforcement in the specimen.
known in order to analytically model the material properties

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 D3171 − 15
(mechanical, physical, thermal, or electrical) of the composite of the limitation of the constituent density measurement would
which are affected by the reinforcement or matrix. Also, be approximately 1 %.
knowledge of the constituent content is required for evaluation 6.4 Mass Change of Reinforcement—Fibers may lose mass
of the quality of a fabricated material and the processes used by any of the techniques in Test Method I. This may be
during fabrication. investigated by subjecting the reinforcement without matrix to
5.2 The void volume of a composite material may signifi- the test conditions of the composite. Once the technique is
cantly affect some of its mechanical properties. Higher void established for a material, no significant changes are expected
volumes usually mean lower fatigue resistance, greater suscep- between samples unless the product or test conditions vary
tibility to moisture penetration and weathering, and increased significantly.
variation or scatter in strength properties. Knowledge of the 6.5 Residual Matrix Retained—Matrix may be retained by
void volume of a composite material is desirable as an any of the techniques of Test Method I. This may be investi-
indication of the quality of a composite. gated quantitatively by subjecting the matrix to the test
5.3 Reinforcement content may be used to normalize me- conditions of the composite. Qualitatively, matrix appears as
chanical properties affected by amount of reinforcement in the hardened pieces in the sample at the end of the test. Once the
coupon. technique is established for a material, no significant changes
are expected between samples unless the product or test
6. Interferences conditions vary significantly.
6.1 Density of Constituents—Calculation of the void volume 6.6 Micrometer Interface—The thickness of the laminate
assumes that reinforcement density and matrix density ob- continuously changes, particularly for surfaces with a release
tained on a lot or material basis are held in the laminate sample. cloth or irregular surface. Test Method II measures the laminate
There is a normal variation in reinforcement and matrix at certain areas. The micrometer gives an indication of the
densities that is dependent on the constituent material. This thickness of the material at a point. The micrometer thickness
assumption used by the void calculation equations is typically measure is dependent on (1) variation in thickness of the panel,
minor, changing the void calculation by less than 0.2 %. One (2) type and diameter of thickness measuring device, (3) ability
indication of this variation is the possibility of obtaining a to hold panel perpendicular to the measurement device, and (4)
negative void volume in low-void volume composites. If sensitivity of the measurement device.
procedural errors can be ruled out, it is reasonable to believe 6.6.1 Ball micrometer geometry tends to give a thickness
that constituent density variation is responsible. Negative void measure for Test Method II that more closely approximates
content is a physical impossibility, but a possibility in these fiber volume if there is a rough surface texture than a flat-faced
calculations. It is useful to report negative void contents to micrometer that tends to overstate laminate thickness. For
assess if constituent density values are incorrect or within a some material forms, such as open weaves, the ball geometry
typical range of material variation. The negative void value is not practical, so that a flat face micrometer is recommended.
then sets an upper bound on error of this test method for any
material. 7. Apparatus
6.2 Coupon Size—Ability to estimate void content is also 7.1 General Requirements:
determined by coupon size and limitations of measuring 7.1.1 Thermal Shock—Laboratory equipment, which is sub-
apparatus. For example, with just limitations of the analytical jected to nonambient temperatures (hot or cold), shall be of
balance (accurate to 0.2 mg), a coupon of 0.2 g with a void tempered glass or polytetrafluoroethylene (PTFE) materials.
volume of 1.0 % would have an uncertainty of 10 % (reported 7.1.2 Post-Test Elemental Analysis—If a post-test elemental
void volume in the range of 0.9 to 1.1 %) on the void volume analysis of the reinforcement residue is to be performed,
calculation as a result of possible balance error. A 1-g sample laboratory equipment contacting the specimen shall be con-
would have an uncertainty of 2 % in the void volume calcula- structed of PTFE, and specimen cutting performed only by
tion (reported void volume in the range of 0.98 to 1.02 %) diamond-tipped tools.
because of possible balance error for the same 1.0 % void 7.2 General Usage:
volume. 7.2.1 Analytical Balance—The analytical balance shall be
6.3 Error in Previous Measures4,5—Ability to estimate void capable of reading to within 60.1 mg.
content is also determined by the accuracy of previous mea- 7.2.2 Laboratory Desiccator.
sures. Density measures of constituents and laminate have 7.3 Test Method I:
some limitations. Good measures of these properties should 7.3.1 Heating Equipment:
have an uncertainty of less than 0.0005 g/cm3. For a typical 7.3.1.1 Constant Heat Source—Heating mantle, hot plate, or
carbon/epoxy laminate, uncertainty in the void volume because controlled temperature bath, capable of heating material to the
required temperature for the particular digestion medium and
4
The interface region in glass fiber-reinforced epoxy resin composites: 1. shall be capable of maintaining the temperature to 610°C.
Sample Preparation, Void Content and Interfacial Strength,Composites , 26, 1995, 7.3.1.2 Microwave, capable of maintaining a constant power
pp. 467–475.
5
output. The microwave setup shall include an overpressure
“A Comparison of Void Measurement Methods for Carbon/Epoxy
Composites,” U.S. Army Materials Technology Laboratory (US Army Research fail-safe device. Used exclusively for Procedure F (see Annex
Laboratory) MTL TR91–13. A6).

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 D3171 − 15
7.3.1.3 Drying Oven, air circulating, capable of maintaining such specifications are available.6 Other grades may be used,
a temperature of 100 6 3°C or other target temperature within provided it is first ascertained that the reagent is of sufficiently
63°C. high purity to permit its use without lessening the accuracy of
7.3.1.4 Muffle Furnace, capable of maintaining a tempera- the determination.
ture where the polymer matrix is removed, but the reinforce- 8.2 Digestion Reagents—A suitable digestion reagent shall
ment is unaffected. This is typically 600 6 30°C minimum. be selected that is compatible with the material system, test
Used exclusively for Procedure G (see Annex A7). method, and apparatus. Read and understand the precautions
7.3.1.5 Nitrogen-Purging Furnace, capable of maintaining a listed in Section 9 before selecting an extraction reagent.
temperature where the polymer matrix is carbonized under Extraction reagents that have been found effective for many
matrices include:
nitrogen environment, but the reinforcement is unaffected. This
8.2.1 Procedures A and F:
is typically 560 6 40°C minimum. Used exclusively for
8.2.1.1 Nitric Acid, HNO3, 70 % aqueous.
Procedure H (see Annex A8). 8.2.2 Procedure B:
7.3.2 Miscellaneous Equipment: 8.2.2.1 Hydrogen Peroxide, H2O2, 30 to 50 % aqueous.
7.3.2.1 Sample Container, beaker, sealed vessel, or flask of (Warning—As of the approval date of this standard, H2O2 was
borosilicate glass or PTFE, minimum size 50 mL. classified by the international agency for Research on Cancer
7.3.2.2 Vacuum Source, capable of 50-kPa (375-mm Hg) as “unknown” (meaning the possibility of this material causing
pressure. cancer in humans is unknown). There is limited evidence of a
cancer risk associated with laboratory animals.)
7.3.2.3 Static Control Device, capable of eliminating static 8.2.2.2 Sulfuric Acid, H2SO4, 96 to 98 % aqueous.
charge from beaker walls. 8.2.3 Procedure C:
7.3.2.4 Filtering Apparatus, this may consist of a filtering 8.2.3.1 Dimethylformamide (DMF), (CH 3 ) 2 NCHO.
flask with crucible holder and sintered glass filter or some other (Warning—As of the approval date of this standard, DMF was
apparatus. listed by the international agency for Research on Cancer in
Group 2B as a “possible human carcinogen” and is considered
NOTE 3—Filter porosity should be sized to filter the smallest expected
a reproductive toxin by the National Toxicology Program. See
reinforcement size. This is particularly important for discontinuous
reinforcements or for materials which have been ground before digestion a recent DMF material safety data sheet for more information.)
(Note 4). If any doubt exists about the filter size selection, successively 8.2.3.2 Ethylene Glycol, HOCH2CH2OH.
finer filters shall be evaluated with the material being tested until 8.2.3.3 Solid Potassium Hydroxide, KOH.
confidence is established in the filter size selected. Resin fillers or other 8.2.4 Procedure D:
constituent materials not destroyed by digestion may be retained both 8.2.4.1 Sodium Hydroxide, NaOH 40 to 80 % aqueous.
within the reinforcement and due to filter size. An estimation of this 8.2.5 Procedure E:
“trapped” matrix may be needed to adjust fiber content. Used in 8.2.5.1 Hydrochloric Acid, HCl 5-10 % aqueous.
Procedures A-F (see Annex A1 – Annex A7).
8.3 Washing Reagents—A suitable washing reagent(s) shall
7.3.2.5 Reflux Condenser, capable of preventing loss of be selected that is compatible with the material system under
digestion medium by allowing volatilized vapors to recondense test and the apparatus. Read and understand the precautions
into the container. Used in Procedures A and C (see Annex A1 listed in Section 9 before selecting a washing reagent. Washing
and Annex A3). reagents that have been found effective include:
7.3.2.6 Other Common Equipment—Other generally avail- 8.3.1 Acetone, CH3COCH3.
able laboratory terms may be needed for the various procedures 8.3.2 Water, distilled or demineralized.
such as beakers, pipettes, watchglasses, and lint-free wipes.
9. Hazards
7.4 Items for Test Method II:
9.1 This test method should be used only by laboratory
7.4.1 Thickness Measuring Device—Micrometer or digital workers with general training in the safe handling of chemi-
indicator (with 6-mm diameter ball/ball measuring ends). cals. A source of useful information is Prudent Practices in the
Device is capable of reaching the center of the laminate test Laboratory: Handling and Disposal of Chemicals, National
specimen surface. Capable of reading to 0.001 mm. Academy Press, 1995, 449 pp., ISBN 0-309-05229-7.
7.4.2 Calipers, capable of reading length or width of the (Warning—In addition to other precautions, consult the ap-
specimen to 0.1 % accuracy. Caliper reading length may vary propriate material safety data sheet for each material used,
depending on specimen size from 75 to over 1500 mm. Optical including caustics, oxidizers, and composite materials for
devices may be used for larger specimens. specific recommendations on safety and

8. Reagents
6
Reagent Chemicals, American Chemical Society Specifications, American
8.1 Purity of Reagents—Reagent grade chemicals shall be Chemical Society, Washington, DC. For suggestions on the testing of reagents not
used in all tests. Unless otherwise indicated, it is intended that listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all reagents conform to the specifications of the Committee on and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Analytical Reagents of the American Chemical Society where MD.

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 D3171 − 15
handling.)(Warning—In addition to other precautions, the 10.1.3 Specimen Cutting—The specimen shall be free from
digestion or combustion process should be performed under a oil, grease, or other foreign matter. If volume percent is to be
suitably vented fume hood. Chemical processes and combus- calculated by measuring the density of the specimen, that
tion processes shall not be performed in the same fume hood.) cutting must not cause the specimen to fray or delaminate. An
9.2 Carry out all oxidations behind a safety shield or hood improperly cut specimen may trap air during submersion,
sash while using a ventilation hood. giving a false density.
10.1.4 Specimen Conditioning—After cutting, the sample
9.3 Use standard procedures for handling acids and caustics. shall be conditioned in accordance with Section 12.
9.4 Store materials by type. Acids especially need to have a 10.2 Test Method II:
containment area by acid type. 10.2.1 Sampling of Test Specimens—The minimum number
9.5 Store 30 to 50 % hydrogen peroxide in a freezer, or in a of recommended test specimens is one.
cool safety hood, in the original container with a vented cap. 10.2.2 Test Specimen Geometry—The specimen may be the
Do not allow contact with any organic material. Flush spills dimensions of the laminate panel. Minimum specimen surface
with copious amounts of water. area is 625 mm2 on one laminate face. The specimen shall be
roughly cylindrical or cuboid in shape.
9.6 If incidental skin contact is made with any reagent 10.2.3 Specimen Cutting—The specimen shall be free from
(except water), wash with copious amounts of water. oil, grease, or other foreign matter.
9.7 No attempt should ever be made to purify hydrogen 10.2.4 Specimen Conditioning—After cutting, the sample
peroxide by distillation. Explosive decomposition is said to shall be conditioned in accordance with Section 12.
occur with boiling solution containing 65 % hydrogen perox-
11. Calibration and Standardization
ide.
11.1 The accuracy of all measuring equipment shall have
9.8 Ensure that all digestion medium is removed before
certified calibrations that are current at the time of use of the
placing the sample in the oven.
equipment.
9.9 Use of mixed digestion reagents, apparatus, or condi-
tions not covered by these test methods may increase hazards 12. Conditioning
as a result of splashing, toxic fumes, overpressurization, or 12.1 Dry the test specimens to an equilibrium condition in
explosion. If conditions from these test methods are altered, accordance with Procedure D of Test Method D5229/D5229M.
follow good laboratory practice for new test method develop- If it may be shown that specimens are dry to within 1 % error,
ment. within a shorter period of time, the reduced drying time may be
9.10 The combination of nitric acid and acetone is specifi- used.
cally cautioned against in the use of these test methods 12.2 Unless otherwise specified, conduct the tests at 23 6
(Procedures A and F) since it may form an explosive media. It 5°C and less than 65 % RH. Test specimens for density within
is good practice to rinse thoroughly so that reactive constitu- 10 min of removal from desiccator.
ents are not combined. Also reactive constituents shall not be
placed in the same (waste) container. 13. Procedure
9.11 Additional nonchemical hazards such as high heat and 13.1 Test Method I:
possibility of glass implosion under vacuum or other glass 13.1.1 General Procedures
breakage exist in these test methods. Follow good laboratory 13.1.1.1 Procedure A—Perform Procedure A in accordance
practice to minimize risks. with Annex A1.
13.1.1.2 Procedure B—Perform Procedure B in accordance
10. Test Specimen with Annex A2.
13.1.1.3 Procedure C—Perform Procedure C in accordance
10.1 Test Method I: with Annex A3.
10.1.1 Sampling of Test Specimens—The minimum number 13.1.1.4 Procedure D—Perform Procedure D in accordance
of recommended test specimens is three. Use the same speci- with Annex A4.
men sized and cut in accordance with 10.1.2 and 10.1.3 for 13.1.1.5 Procedure E—Perform Procedure E in accordance
density (as determined by Test Methods D792 or D1505) and with Annex A5.
reinforcement volume/void content, except in Procedure G, in 13.1.1.6 Procedure F—Perform Procedure F in accordance
which the specimen may need additional dicing to maximize with Annex A6.
surface area for combustion. 13.1.1.7 Procedure G—Perform Procedure G in accordance
10.1.2 Test Specimen Geometry—The specimen shall have a with Annex A7.
minimum mass of 0.5 g for constituent volume only, and 1.0 g 13.1.1.8 Procedure H—Perform Procedure H in accordance
if void content is to be obtained, and any shape not restricted with Annex A8.
by the apparatus. The specimen should contain a representative 13.1.2 Correction for Fiber Weight Change During Test:
volume of the material being evaluated. The same specimen 13.1.2.1 Weigh one blank consisting only of reinforcement.
may be used for density and reinforcement volume determina- The blank mass shall roughly equal the mass of reinforcement
tion. in the test specimens to the nearest 0.0001 g.

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 D3171 − 15
13.1.2.2 Perform the full test procedure on blank. Mf = final mass of the specimen after digestion or
13.1.2.3 The mass difference between the original blank combustion, g.
mass and the mass after digestion or combustion divided by the NOTE 4—The mass of the fiber may be obtained by taking the mass of
original blank mass is the reinforcement fractional loss or gain. the crucible with reinforcement minus the crucible mass (Mf = Mcr – Mc).
13.1.2.4 This fractional loss (or gain), if reproducible, may 14.1.2 Reinforcement Content, Volume Percent—Calculate
be added (or subtracted) to the equation in 14.1.1 or 14.2.3. reinforcement content, in volume percent, in accordance with
13.1.2.5 Only fractional differences larger than 0.005 Eq 2.
(0.5 %) shall be considered significant.
V r 5 ~ M f /M i ! 3 100 3 ρ c /ρ r (2)
13.1.3 Correction for Matrix Weight Change:
13.1.3.1 Weigh one blank consisting only of cured matrix. where:
The blank mass shall roughly equal the mass of matrix in the ρr = density of the reinforcement, g/cm3 and
test specimens to the nearest 0.0001 g. ρc = density of the specimen, g/cm3.
13.1.3.2 Perform the full test procedure on blank.
14.1.3 Matrix Content, Weight Percent—Calculate matrix
13.1.3.3 Since all matrix should be removed, the mass after
content, in weight percent, in accordance with Eq 3.
digestion or combustion divided by the original blank mass is
the matrix residue. This represents matrix material not re- W m 5 ~ M i 2 M f ! /M i 3 100 (3)
moved by digestion or combustion. 14.1.4 Matrix Content, Volume Percent—Calculate matrix
13.1.3.4 This fractional gain, if reproducible, may be added content, in volume percent, in accordance with Eq 4.
to the equation in 14.1.3.
V m 5 ~ M i 2 M f ! /M i 3 ρ c /ρ m 3 100 (4)
13.1.3.5 Only fractional differences larger than 0.005
(0.5 %) shall be considered significant. where:
13.2 Test Method II: ρm = density of the matrix, g/cm3.
13.2.1 Weigh each specimen to the nearest 0.0001 g. 14.1.5 Void Volume—Calculate void volume, in percent, in
13.2.2 Determine the density of each specimen in accor- accordance with Eq 5.
dance with Test Methods D792 or D1505 or use the calculation
V v 5 100 2 ~ V r 1V m ! (5)
shown in 14.3, if fiber volume percent or void percent, or both,
NOTE 5—Negative values of Vv shall be reported. Values of void volume
are required. The preconditioning for D792 or D1505 speci- more negative than –0.2 % indicate a potential testing problem; input
mens is to be in accordance with D3171 Section 12. values and test procedure shall be investigated. See 6.1.
13.2.3 A micrometer with a 4 to 7 mm [0.16 to 0.28 in.] 14.2 Test Method I, Procedure H:
nominal diameter ball interface shall be used to measure the 14.2.1 Carbonization Ratio of the Neat Resin—Calculate
specimen thickness when at least one surface is irregular (such the carbonization ratio of the neat resin, CR, in accordance with
as the bag-side of a laminate). A micrometer with a 4 to 7 mm Eq 6:
[0.16 to 0.28 in.] nominal diameter ball interface or with a flat
anvil interface shall be used to measure the specimen thickness CR 5 m d ⁄m i (6)
when both surfaces are smooth (such as tooled surfaces). where:
Measure thickness in at least ten locations. Take the average md = final mass of the neat resin residue after carbonization,
measurement to determine the specimen thickness. g, and
13.2.4 A micrometer or caliper, with a flat anvil interface, mi = initial mass of the neat resin specimen, g
shall be used to measure the length and the width of the
specimen. The accuracy of the instruments shall be suitable for NOTE 6—The mass of the neat resin residue after carbonization may be
obtained by taking the mass of the crucible with residue minus the crucible
reading to within 1 % of the sample dimensions. For typical
mass (md = mcr– mc). If there is no residue from neat resin specimen after
specimen geometries, an instrument with an accuracy of carbonization, CR is equal to zero since md is equal to zero.
60.0025 mm [60.0001 in.] is adequate for the thickness
14.2.2 Mass of the Resin Matrix in the Composite
measurement, while an instrument with an accuracy of
Specimen—Calculate the mass of the resin matrix in the
60.025 mm [60.001 in.] is adequate for the length and the
composite specimen, in grams, in accordance with Eq 7:
width measurement. Measure the specimen width and length in
at least three locations. Take the average of the measurements M m 5 ~ M i 2 M d ! ⁄ ~ 1 2 CR ! (7)
to determine the length and width. where:
14. Calculation Mi = initial mass of the composite specimen, g, and
Md = final residue mass of the composite specimen, g
14.1 Test Method I, Procedures A through G:
14.1.1 Reinforcement Content, Weight Percent—Calculate NOTE 7—The mass of the composite specimen residue after carboniza-
reinforcement content, in weight percent in accordance with Eq tion may be obtained by taking the mass of the crucible with residue minus
the crucible mass (Md = Mcr–Mc). “M” represents any mass associated
1. with fiber reinforced composite specimens while “m” the mass related to
W r 5 ~ M f /M i ! 3 100 (1) neat resin specimens.

where: 14.2.3 Reinforcement Content, Weight Percent—Calculate

reinforcement content in the composite specimen, in weight
Mi = initial mass of the specimen, g and
percent, in accordance with Eq 8:

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 D3171 − 15
W r 5 ~ M i 2 M m ! ⁄M i 3 100 14.3.6 Cured Ply Thickness, mm—Calculate the cured ply
5 ~ M d 2 M i 3 CR ! ⁄ ~ M i 3 ~ 1 2 CR !! 3 100 (8) thickness from the measured laminate thickness, h, in section
13.2.3, in accordance with Eq 17.
14.2.4 Reinforcement Content, Volume Percent—Calculate
h p 5 h/N p (17)
reinforcement content, in volume percent, in accordance with
Eq 9. where:
V r 5 ~~ M i 2 M m ! ⁄ M i ! 3 100 3 ρ c ⁄ρ r (9) hp = cured ply thickness, mm, and
Np = number of plies in the laminate.
where:
14.4 Statistics—For each series of tests, calculate the aver-
ρr = density of the reinforcement, g/cm3 and
ρc = density of the composite specimen, g/cm3 age value, standard deviation, and coefficient of variation (in
percent) of all values obtained:
14.2.5 Matrix Content, Weight Percent—Calculate matrix
content, in weight percent, in accordance with Eq 10. x̄ 5 S D
n
Σ x i ⁄n
i51
(18)
W m 5 M m ⁄M i 3 100 (10)

14.2.6 Matrix Content, Volume Percent—Calculate matrix S n21 5 ŒS n

i51
D
Σ x i2 2 n x̄ 2 ⁄ ~ n 2 1 ! (19)
content, in volume percent, in accordance with Eq 11. CV 5 100 3 S n21 ⁄x̄ (20)
V m 5 ~ M m ⁄ M i ! 3 100 3 ρ c ⁄ρ m (11)
where:
where: x̄ = sample mean (average),
ρm = density of the matrix, g/cm3 Sn-1 = sample standard deviation,
n = number of specimens,
14.2.7 Void Volume—Calculate void volume, in percent, in xi = measured or derived property, and
accordance with Eq 5. CV = sample coefficient of variation, in percent
NOTE 8—Negative values of Vv shall be reported. Values of void
volume more negative than –0.2 % indicate a potential testing problem; 15. Report
input values and test procedure shall be investigated. See 6.1. 15.1 Report the following information, or references point-
14.3 Test Method II: ing to other documentation containing this information, to the
14.3.1 Specimen Density, g/cm3—Calculate specimen den- maximum extent applicable:
sity in grams per cubic centimeter with Eq 12 or use equivalent 15.1.1 Reporting of terms that are beyond the control of a
test methods such as Test Methods D792 or Test Method given testing laboratory, such as material details, shall be the
D1505. responsibility of the requestor.
15.1.2 Revision level or date of issue of this test method.
ρ c 5 M i / ~ A 3 h 3 1000! (12)
15.1.3 Actual test procedure used.
where: 15.1.4 Any variations to this test method, anomalies noticed
Mi = mass of the specimen, g; during testing, correction factors, or any equipment problems
A = area of the specimen, m2; and that occurred during testing.
h = thickness of the specimen, mm. 15.1.5 Complete identification of the material tested includ-
ing type, source, form, and dimensions (see Guide E1309).
14.3.2 Reinforcement Content, Weight Percent—Calculate
15.1.6 Fiber density values used, and their source.
the reinforcement content in weight percent in accordance with
15.1.7 Individual and average values and standard devia-
Eq 13.
tions of reinforcement and matrix weight and reinforcement
W r 5 ~ A r 3 N 3 0.1! / ~ ρ c 3 h ! (13) and matrix volume percent.
where: 15.1.8 Individual and average value and standard deviation
for void percent.
Ar = mass of one sheet of reinforcement/unit area, g/m2 and
Np = number of sheets/plies in the test specimen. 15.1.9 Matrix density value used and source of value.
15.1.10 Drying times and oven temperature for both origi-
14.3.3 Reinforcement Content, Volume Percent—Calculate nal specimen drying (before density determination and after
the reinforcement content in volume percent in accordance digestion).
with Eq 14. 15.1.11 Exposure time for Procedure A8.
V r 5 ~ A r 3 N 3 0.1! / ~ ρ r 3 h ! (14) 15.1.12 For Test Method II, measurement equipment used,
individual and average laminate thickness width and length
14.3.4 Matrix Content, Weight Percent—Calculate the ma- measures.
trix content in weight percent in accordance with Eq 15. 15.1.13 Cured ply thickness from Test Method II, including
W m 5 100 2 ~~ A r 3 N 3 0.1! / ~ ρ c 3 h !! (15) individual and average values.
14.3.5 Matrix Content, Volume Percent—Calculate the ma- 16. Precision and Bias
trix content in volume percent in accordance with Eq 16. 16.1 Precision—The data required for the development of a
V m 5 W m 3 ρ c /ρ m (16) precision statement is not available for this test method.

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Committee D-30 is currently planning a round-robin test series 17. Keywords
for this test method in order to determine precision. 17.1 composite materials ; fiber content; matrix content;
16.2 Bias—Bias cannot be determined for this test method reinforcement content; resin content; void volume
as no accepted reference standard exists.

ANNEXES

(Mandatory Information)

A1. PROCEDURE A—MATRIX DIGESTION USING NITRIC ACID

Warning—Understand the hazards described in Section 9 A1.5 The maximum time for digestion should be 6 h.
before working with acids. Shorter times are dependent on the composite system. The
matrix is considered fully digested if no trace of the
A1.1 Weigh each specimen, Mi, to the nearest 0.0001 g. reinforcement/matrix laminate combination remains.
A1.2 Determine the density of each specimen in accordance Unfortunately, this is difficult to detect until the specimen has
with Test Methods D792 or Test Method D1505 if fiber volume been removed from the digestion media.
percent or void percent, or both, are required. The precondi-
A1.6 Filter the contents into tared or preweighed (Mc)
tioning for D792 or D1505 specimens is to be in accordance
with D3171 Section 12. sintered glass filters (or filter-lined crucibles) under a vacuum
NOTE A1.1—Specimens may require further dicing or grinding before of 17 kPa or better. Wash the fiber three times with distilled
digestion. After machining, specimens should be reweighed. Care should water. An acetone wash may be used as the final wash after
be taken that the diced or ground specimen represents original sample nitric acid is removed from the specimen to improve drying
composition.
times.
A1.3 Place each specimen in a separate flask or beaker
A1.7 Place the specimen in an oven at 100°C minimum
containing at least 30 mL of 70 % nitric acid.
until the sample is dried (approximately 1 h at 100°C).
A1.4 Constant heating with heating mantle, hot plate, or
controlled temperature bath is recommended. Temperature A1.8 Cool the filter or crucible to room temperature in a
requirements depend on the system to be digested. Generally, desiccator. Weigh the specimen in its holder, Mcr, to the nearest
temperatures should not exceed 80°C. (Warning—Reflux 0.0001 g.
condensers are recommended if the temperature exceeds
40°C.)

A2. PROCEDURE B—MATRIX DIGESTION USING SULFURIC ACID/HYDROGEN PEROXIDE

Warning—Understand the hazards described in Section 9 A2.4 Add a minimum of 20-mL sulfuric acid.
before working with acids. (Warning—Do not use less than 20-mL acid.) Place the beaker
on a hot plate and heat until the mixture starts to fume.
A2.1 Weigh each specimen (Mi) to the nearest 0.0001 g.
A2.5 After the solution is dark (with no appreciable change
A2.2 Determine the density of each specimen in accordance
in color for 5 min) add 50 or 30 % hydrogen peroxide down the
with Test Methods D792 or D1505 if fiber volume percent or
side of the beaker to oxidize the matrix. (Warning—This
void percent, or both, are required. The preconditioning for
procedure increases acid fumes. Wear rubber gloves, labora-
D792 or D1505 specimens is to be in accordance with D3171
Section 12. tory coat, and eye protection.) Typically, about 35 mL or more
of hydrogen peroxide are added. The fibers float to the top of
A2.3 Place each specimen into a 100-mL [minimum] bea- the solution, and the solution appears clear or color intensity
ker. dramatically fades.

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 D3171 − 15
A2.6 Remove the beaker from the hot plate and allow the water. An acetone wash may be used as the final wash after
solution to cool. Cooling may be facilitated by a water or ice sulfuric acid and hydrogen peroxide is removed from the
bath. Any nondigested laminate should be clearly visible at this specimen to improve drying times.
point. If the matrix is not digested, the solution may be filtered,
then reintroduced into the beaker. Steps A2.4 – A2.6 may be A2.8 Place the specimen in an oven at 100°C minimum
repeated. until the sample is dried (approximately 1 h at 100°C).

A2.7 Filter the contents into tared or preweighed, Mc, A2.9 Cool the filter or crucible to room temperature in a
sintered glass filters (or filter-lined crucibles) under a vacuum desiccator. Weigh the specimen in its holder, Mcr, to the nearest
of 17 kPa or better. Wash the fibers three times with distilled 0.0001 g.

A3. PROCEDURE C—MATRIX DIGESTION USING ETHYLENE GLYCOL/POTASSIUM HYDROXIDE

Warning—Understand the hazards described in Section 9 A3.6 Boil until the matrix is completely digested. An
before working with caustics. indicator is when fibers separate and appear to float freely in
the solution.
A3.1 Weigh each specimen, Mi, to the nearest 0.0001 g.
A3.7 Remove the beaker from the reflux condenser.
A3.2 Determine the density of each specimen in accordance
NOTE A3.1—Because potassium hydroxide will attack the glass filter, it
with Test Methods D792 or D1505 if fiber volume percent or is advisable to precondition the filter by pouring a small amount of
void percent, or both, are required. The preconditioning for potassium hydroxide-ethylene glycol solution onto the filter.
D792 or D1505 specimens is to be in accordance with D3171
Section 12. A3.8 Filter the contents into tared or preweighed (Mc)
sintered glass filters under a vacuum of 17 kPa or better. Wash
A3.3 Preparation of Reagent—Prepare a 10 % solution of the fiber two times with dimethylformamide, and three addi-
potassium hydroxide in ethylene glycol. (For example: Place tional times with distilled water. An acetone wash may be used
100 g of solid potassium hydroxide into a 1500-mL volumetric as the final wash after potassium hydroxide-ethylene glycol
flask. Add 500 mL of ethylene glycol. Heat gently to dissolve
solution is removed from the specimen to improve drying
the solid. Then add another 500 mL of ethylene glycol for a
times.
total volume of 1 L.) Label and store flask.
A3.9 Place the specimen in an oven at 100°C minimum
A3.4 Place each specimen into a separate 250-mL flask and
add 100 mL of the potassium hydroxide-ethylene glycol until the sample is dried (approximately 1 h at 100°C).
solution to each flask. Alternate solution volumes may be used A3.10 Cool the filter or crucible to room temperature in a
as long as the ratio of the components remains equivalent. desiccator. Weigh the specimen in its holder, Mcr, to the nearest
A3.5 Connect the flask to a reflux condenser. Start the 0.0001 g.
cooling water flow and adjust the temperature of the hot plate
or heating mantle to bring the solution to a gentle boil.

A4. PROCEDURE D—MATRIX DIGESTION USING SODIUM HYDROXIDE

Warning—Understand the hazards described in Section 9 A4.3 Place each specimen into a suitable beaker.
before working with caustics.
A4.4 Add 20 to 25 mL of 40 to 80 % sodium hydroxide
A4.1 Weigh each specimen, Mi, to the nearest 0.0001 g. solution to the beaker and heat specimen on a hot plate to 80°C
maximum. Heat used depends on the required heat to digest the
A4.2 Determine the density of each specimen in accordance
matrix for the system.
with Test Methods D792 or D1505 if fiber volume percent or
void percent, or both, are required. The preconditioning for A4.5 When the matrix digestion is complete, remove the
D792 or D1505 specimens is to be in accordance with D3171 beaker from the hot plate and allow to cool.
Section 12.

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 D3171 − 15
A4.6 Filter the contents into tared or preweighed, Mc, A4.7 Place the specimen in an oven at 100°C minimum
sintered glass filters (or crucible with glass filter) under a until the sample is dried (approximately 1 h at 100°C).
vacuum of 50 kPa or better. Wash three times with distilled
water. An acetone wash may be used as the final wash after the A4.8 Cool the filter or crucible to room temperature in a
sodium hydroxide is removed from the specimen to improve desiccator. Weigh the specimen in its holder, Mcr, to the nearest
drying times. 0.0001 g.

A5. PROCEDURE E—MATRIX DIGESTION USING HYDROCHLORIC ACID

Warning—Understand the hazards described in Section 9 A5.5 When the matrix digestion is complete, remove the
before working with acids. beaker from the hot plate and allow to cool.
A5.1 Weigh each specimen, Mi, to the nearest 0.0001 g. A5.6 Filter the contents into tared or preweighed, Mc,
sintered glass filters (or crucible with glass filter) under a
A5.2 Determine the density of each specimen in accordance
vacuum of 17 kPa or better. Wash three times with distilled
with Test Methods D792 or D1505 if fiber volume percent or
water. An acetone wash may be used as the final wash after the
void percent, or both, are required. The preconditioning for
sodium hydroxide is removed from the specimen to improve
D792 or D1505 specimens is to be in accordance with D3171
Section 12. drying times.

A5.3 Place each specimen into a suitable beaker. A5.7 Place the specimen in an oven at 100°C minimum
until the sample is dried (approximately 1 h at 100°C).
A5.4 Add 20 to 25 mL of 5 to 10 % hydrochloric acid
solution to the beaker and heat specimen on a hot plate. Heat A5.8 Cool the filter or crucible to room temperature in a
used depends on required heat to digest the matrix for the desiccator. Weigh the specimen in its holder, Mcr, to the nearest
system. 0.0001 g.

A6. PROCEDURE F—MATRIX DIGESTION WITH NITRIC ACID IN A MICROWAVE OVEN

Warning—Understand the hazards described in Section 9 A6.4 Place lid on the vessel and attach tubing so that nitric
before working with acids. acid vapor will be off-gassed to release pressure. Set time and
power requirements of the microwave in accordance with the
A6.1 Weigh each specimen, Mi, to the nearest 0.0001 g. size of specimen and composite system.
A6.2 Determine the density of each specimen in accordance A6.5 The maximum time for digestion should be 30 min.
with Test Methods D792 or D1505 if fiber volume percent or Shorter times are dependent on the system. The matrix is
void percent, or both, are required. The preconditioning for considered fully digested if no trace of the reinforcement/
D792 or D1505 specimens is to be in accordance with D3171 matrix laminate combination remains. Unfortunately, this is
Section 12. difficult to detect until the specimen has been removed from the
NOTE A6.1—Specimens may require further dicing or grinding before
digestion. Specimens in the state to be digested should be reweighed after digestion media.
density determination in this case. Care should be taken that the diced or
ground specimen represents original sample composition. A6.6 Filter the contents into tared or pre-weighed, Mc,
sintered glass filters (or filter-lined crucibles) under a vacuum
A6.3 Place each specimen in a specially designed pressure of 17 kPa or better. Wash the fiber three times with distilled
vessel, which encloses the solution and sample, but allows water. An acetone wash may be used as the final wash after
pressure release.7 Add at least 30 mL of 70 % nitric acid nitric acid is removed from the specimen to improve drying
solution. times.
A6.7 Place the specimen in an oven at 100°C minimum
7
until the sample is dried (approximately 1 h at 100°C).
The sole source of supply of the apparatus known to the committee at this time
is CEM Corp., P.O. Box 200, Matthews, NC 28104. If you are aware of alternative
A6.8 Cool the filter or crucible to room temperature in a
suppliers, please provide this information to ASTM International Headquarters.
Your comments will receive careful consideration at a meeting of the responsible desiccator. Weigh the specimen in its holder, Mcr, to the nearest
technical committee,1 which you may attend. 0.0001 g.

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 D3171 − 15

A7. PROCEDURE G—MATRIX BURNOFF IN A MUFFLE FURNACE

A7.1 Weigh each specimen, Mi, to the nearest 0.0001 g. neously ignite). Heat to 565 6 30°C, or other temperature
compatible with the composite system, that will burn off the
A7.2 Determine the density of each specimen in accordance matrix and leave the reinforcement.
with Test Methods D792 or D1505 if fiber volume percent or NOTE A7.2—Materials placed in such a hot environment may ignite.
void percent, or both, are required. The preconditioning for Specimens may be ignited under a controlled heat flame before entrance
D792 or D1505 specimens is to be in accordance with D3171 into a muffle furnace. If specimens are preignited, the muffle furnace may
Section 12. be set at the actual burn-off temperature.
NOTE A7.1—Specimens may require further dicing or grinding before
burn off. Reweigh specimens after machining. Care should be taken that A7.5 The maximum time for burn off should be 6 h. Shorter
the diced or ground specimen represents original sample composition. times are dependent on the system and specimen size. The
matrix is considered combusted if no matrix/reinforcement
A7.3 Place each specimen in a desiccated preweighed block exists. Ash and reinforcement should be the only items
crucible, Mc. The crucible should be cleaned by heating to 500 visible.
to 600°C or more in a muffle furnace and cooled in a desiccator
before weighing. A7.6 Place the specimen and crucible in a desiccator and
allow to cool to room temperature.
A7.4 Place the crucible into a preheated muffle furnace at
500°C or lower depending on the composite system (a tem- A7.7 Weigh the specimen in its holder, Mcr, to the nearest
perature below the temperature at which samples will sponta- 0.0001 g.

A8. PROCEDURE H—MATRIX CARBONIZATION IN A NITROGEN-PURGING FURNACE

A8.1 Determine the density of each specimen in accordance A8.5 Place the neat resin specimen in a desiccated pre-
with Test Methods D792 or D1505 if fiber volume percent or weighed crucible, mc. The crucible shall be cleaned by heating
void percent, or both, are required. The preconditioning for to 500 to 600°C or more in a furnace and cooled in desiccator
D792 or D1505 specimens is to be in accordance with D3171, before weighing.
Section 12.
A8.6 Place the crucibles into a nitrogen-purging furnace and
A8.2 Weigh each composite specimen, Mi, to the nearest heat to 560 6 40°C. The minimum time for carbonization shall
0.0001 g. be 1 hour at temperature.
A8.3 Weigh neat resin specimen (the same resin used as A8.7 Cool the crucibles to room temperature in the furnace
matrix in the fiber reinforced composite), mi, to the nearest with nitrogen still being purged. Check for residue of the neat
0.0001 g. resin specimen. If any exists, weigh the residue from the neat
resin specimen in its holder, mcr, to the nearest 0.0001g. If no
A8.4 Place the composite specimen in a desiccated pre- residue exists, mcr is equal to mc.
weighed crucible, Mc. The crucible shall be cleaned by heating
to 500 to 600°C or more in a furnace and cooled in desiccator A8.8 Weigh the residue from the composite specimen in its
before weighing. holder, Mcr, to the nearest 0.0001g.

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