Composites 26 (1995) 725-731

~ UTTERWORTH
I N E M A N N
© 1995 Elsevier Science Limited
Printed in Great Britain. All rights reserved
0010-4361/95/$10.00
Research Report

Mass and volume fraction properties of pultruded glass

fibre-reinforced composites

Binshan S. Ye* and Alrik L. Svensont¢

*Federal Highway Administration and tlnformation Dynamics, Inc., Turner-Fairbank Highway
Research Center, McLean, VA 22101, USA

and Lawrence C. Bank

Department of Civil Engineering, The Catholic University of America, Washington, DC 20064,
USA
(Received 2 November 1993; revised 26 February 1995)

With the expansion of pultruded composites into the construction industry, there exists a need for further
studies on the properties of these materials. This paper presents the results from a series of tests on the
physical properties of pultruded composite materials. Specimens cut from structural shapes, plates, grat-
ings and rebars have been tested by using a supplementary procedure to the ASTM D2584-68 Standard
Test Method for Ignition Loss of Cured Reinforced Resins. This supplementary procedure is used to
remove the filler material added to the resin during the pultrusion process. The results from this series of
tests have been used to show the wide variations that exist in specimens cut from similar samples of
pultruded material. Also, pictorial illustrations are given of several representative samples of the post burn-
out fibre architecture of the pultruded composites.

(Keywords: pultroded composites; mass fraction; volume fraction; filler; test method)

INTRODUCTION in pultruded materials, the types of fibre architectures

used in some standard pultruded products and to present
The uses of pultruded composites have proliferated
the experimental results from volume fraction tests of
recently to include a number of new structural applica-
these materials. Although these materials are used exten-
tions. Once only used for specialized parts or secondary
sively in many applications, there are very few published
structural members, composites are now on the brink of
studies which examine these properties. Several types of
being considered competitive with steel and concrete for
pultruded materials from different manufacturers have
construction ~. Pultruded materials have been investi-
been tested, using both the ASTM D2584-68 Standard
gated for use as a reinforcement for concrete2. Pultruded
Test Method for Ignition Loss of Cured Reinforced
columns and beams, used as primary load-carrying
Resins4"5and a procedure to determine the volume frac-
members, are now coming into more widespread service 3,
tion of pultruded composites with filler material outlined
and new, innovative applications of pultruded compo-
by one manufacturer6. The intent is not to endorse any
sites are continuously being developed and put into use.
one product. Rather, the focus here is to expand the
The fact that composites in general can be custom
general understanding of these materials, to illustrate the
tailored to suit individual rbquirements, have desirable
importance of knowing precise volume fraction infor-
properties in corrosive environments, provide higher
mation for design, and to show the ease with which this
strength at a lower weight and have lower life-cycle costs
information can be gained through simple laboratory
has aided in their evolution. These qualities, in addition
tests.
to the ability to monitor the performance of the mater-
The Federal Highway Administration (FHWA) is
ial in the field via embedded sensors (e.g. 'smart struc-
examining glass fibre-reinforced composite materials for
tures'), give composites an edge over conventional
use in roadside safety structures (e.g. barrier, crash cush-
materials I.
ions, signs and lighting supports). Recent research has
With the possibility for unlimited expansion of
investigated the dynamic and static response of these
pultruded composites into the construction industry
composite materials to evaluate their suitability for road-
being so imminent, the need for a full understanding of
side safety structures. As a part of this investigation,
these materials becomes vital. This report intends to
pultruded composite material samples from various
extend the prevalent knowledge of some of the proper-
structural shapes, gratings and rebars have been tested
ties of pultruded composites. The purpose of the report
in both impact and static tests. Results from these inves-
is to show the variations in glass fibre content existing tigations have been published 7-11. Mass fraction tests
have also been performed on the materials under inves-
tigation to determine the exact internal architecture and
~: To w h o m correspondence should be addressed the fibre content of each test specimen. This information

COMPOSITES Volume 26 Number 10 1995 725

Mass and volume fraction of pultruded composites: B.S. Ye et al.

has been used to correlate strength and energy

absoprtion characteristics of a material to lay-up
geometry.
From the results of testing, it has been observed that
pultruded materials vary widely. Specifications given by
manufacturers are often average values for an entire Flange
product line and not a specific item. This is a source of specimens
error when considering small test samples cut from a
structural shape. Further, much of the specific informa-
tion is not published in manufacturers' literature, which
requires the user to conduct the volume fraction tests to vv ~

determine exact information. specimens

MATERIALS CONSIDERED
The materials tested consisted of glass fibre-reinforced
pultruded composites with a polyester or vinyl ester
matrix. The test specimens were cut from standard struc-
tural shapes, plates, gratings or rebars. Specimens were
cut as close in size to the ASTM standard recommen-
dation as possible (25 mm by 25 mm by thickness) 4'5.
For the grating specimens, a complete I-section profile
by a 25 mm depth was used. Table 1 presents the test
specimen specifications for the volume fraction tests
conducted. For the test specimens cut from an I-section
structural shape, Figure 1 illustrates specimen locations
on the I-section.
Specimens designated LV2, LV3, TV3, TV4, LP3 and
TP3 were cut from structural shapes manufactured by
Creative Pultrusions, Inc. in Alum Bank, PA. The IPF
and IPW specimens were manufactured by Morrison
Molded Fiber Glass (MMFG) of Bristol, VA. The
grating specimens designated DP and DV were samples
of the Duradek grating made by Aligned Fiber
Composite, Inc. of Chatfield, MN, and the specimens
designated SP and SV came from Seasafe, Inc. of
Lafayette, LA. The rebar specimens were manufactured
by Creative Pultrusions. For all types 'V' refers to a vinyl
ester and 'P' refers to a polyester matrix.
Visual observation of the pultruded material indicated
significant void content in the structural profile and plate
materials which can be estimated to be ~3 to 5% by
Figure 1 Specimen locations for I-section samples (LV3, TV3, IPF,
IPW specimens)
volume. In the pultruded rebar specimens and grating
bars, voids could not be seen by eye and the void content
was estimated at <1%. In addition, the void density in
the structural profile specimens appeared to vary from
section to section and also by manufacturer.
Reinforcements in pultruded composites typically
consist of unidirectional rovings, continuous strand
mats, and stitched or woven rovings. It is assumed that
the unidirectional rovings exit the pultrusion die at 0 °
orientations, and that woven fabrics exit the die at their
woven orientations (e.g. 0°-90°). In this investigation,
fibre orientations were not specifically measured but were
assumed to be present in the material as intended.
Because the reinforcing materials can 'wander' somewhat
during the pultrusion process, they can vary in orienta-
tion within the same section along the length or through
the thickness.
S U M M A R Y OF TEST METHOD
The specimen is contained in a crucible and is ignited
and burned until only ash and carbon remain. The resid-
ual is then placed in a furnace and degraded, leaving only
reinforcement and filler. Once the resin is completely
removed, analysis of the laminate is performed on the

Table 1 Test specimen specifications

Section
cut Dimensions
Sample Manufacturer from l, w, t (mm) Fibre architecturea

LV2 Creative Pultrusions Channel web 25, 25, 6.4 [C/O/C/O/C/O/C]x

LV3 Creative Pultrusions I-Section flange 25, 25, 9.6 [C/O/C/O/C/O/C/O/C/O/C]T
TV3 Creative Pultrusions l-Section web 25, 25, 9.6 [C/90/C/90/C/90/C/90/C]T
TV4 Creative Pultrusions Plate 25, 25, 1 2 . 7 [C/0-90/90/C/0-90/C/90/0-90/C]T
LP3 Creative Pultrusions Channel web 25, 25, 9.6 [C/C/O/C/O/C/O/C/C]T
TP3 Creative Pultrusions Channel web 25, 25, 9.6 [C/C/90/C/90/C/90/C/C]~
IPF MMFG I-Section flange b [C/C/O/C/O/C/O/C/O/C/C]T
IPW MMFG I-Section web b [C/C/O/C/O/C/O/C/O/C/C]T
DP AFC Grating 25 by c [C/0/C]T
DV AFC Grating 25 by c [C/0/C]T
SP Seasafe Grating 25 by c [C/0/C]T
SV Seasafe Grating 25 by c [C/0/C]T
REP Creative Pultrusions Rebar 38 by a [Spiral/0]

a C, continuous strand mat; 0-90, cross-ply woven roving; 0, longitudinal roving (0° to specimen long axis); 90, transverse roving (90 ° to
specimen long axis)
h Typical size: 1 = 51 mm, w = 38 mm, t = 12.7 mm
c I-section profile (see photo in Figure 2)
a Radius of cylindrical rebar, R = 6.4 (mm)

726 COMPOSITES Volume 26 Number 10 1995

 Mass and volume fraction of pultruded composites: B.S. Ye et al.

burn-out remains. This includes making a detailed

Figure 2 Typicalfibre architecture for a structural shape (LP3) illus-
trating alternatingcontinuousstrand mat and roving layers
diagram of reinforcement type and recording its place-
ment in the laminate. Figures 2-4 depict typical fibre
architecture lay-outs for typical structural shape, grating
and rebar specimens. Hydrochloric or nitric acid or both
is then used to determine the filler type and to separate
the filler from the reinforcement. The complete proce-
dure is presented in Appendix I. Equations for the chem-
ical reactions associated with this process are given in
Appendix II.
The test method presented here, the acid dissolve igni-
tion loss method, is suitable for determining the volume
fraction of pultruded glass-reinforced composites with
filler. Since glass is always a chemically inactive (inert or
noble) material, many different acid types can be selected
to dissolve the fillers. The most commonly used filler

Figure 3 Typicalfibre architecturefor a grating (DP)

Figure 4 Fibrearchitecture for a rebar (REP)

COMPOSITES Volume 26 Number 10 1995 727

Mass and volume fraction of pultruded composites: B.S. Ye et al.
types in industry are kaolin clay, calcium carbonate and
alumina trihydrate (ATH). In the specimens tested, V~=(Ms+ M r + gf)×106
(1)
kaolin clay was the only filler material present. The Pg Pr Pf
chemical procedure to identify the other two and dissolve
them is presented in Appendix 1. is used.
2) The volume fraction for each part is then deter-
mined. The volume fraction for glass fibre is given
CALCULATIONS by
Nomenclature used in calculations
v s _ Ms × 106 (2)
Vs Volume of specimen (mm ~)
Vs Volume of glass (mm 3) Vs Ps xE
Vr Volume of resin (mm3)
Vr Volume of filler (mm 3) the volume fraction for resin is
jog Glass density (kg m -3)
Vr = Mr
Or Resin density (kg m -3) × 106 (3)
pf Filler density (kg m -3) E p XVs
C Mass of crucible (g)
CS Mass of crucible + sample (g) and the volume fraction for filler is
CA Mass of crucible + ash (g)
CG Mass of crucible + glass (g) Vf = 1 Vg (4)
Ms Mass of sample = CS - C (g) K K E
Ma Mass of ash = CA - C (g)
Ms Mass of glass = CG - C (g) where p~ = 1043 for all V (vinyl ester) resin and 1t51
8 Percentage of mass loss of filler (g) for all P (polyester) resin, pg -- 2540 for glass fibre and
M~f Mass of filler after burn-out = Ma - M s (g) Pr = 5900 for filler.
Mf Mass of filler = M~r X (1 + 3) (g)
By using the identifying procedure described in Appendix
Mr Mass of resin = Ms - M r - M s (g)
I, the filler was found to be kaolin clay for all specimens
Assuming that the material densities are known a containing filler. This was confirmed through the use of
priori, then the basic input involves only C, CS, CA and two more advanced techniques, scanning electron
CG. The remaining quantities are derived from these. If microscopy and energy dispersal X-ray fluorescence
the filler type is ATH, one must consider the fact that a analysis 12. The value of the failer density is based on the
6 of 34.6% filler mass will be lost in the bum-out proce- average density for LP3 samples (see Appendix liD.
dure. Likewise, there is a loss for the kaolin clay during
the heat process, 6 = 14% (see Appendix II). This loss
must be taken into account in the calculation. RESULTS
Table 2 presents the test results for mass fraction (some-
Mass fraction nomenclature times referred to as weight fraction) and Table 3 presents
Ms/Ms Mass fraction of glass to sample the volume fraction results for all specimen types tested.
M~/Ms Mass fraction of resin to sample In each row for each specimen, the average of five tests
Mr/Ms Mass fraction of filler to sample +_the standard deviation is given. These values are
presented for the mass and volume fraction of the fibre,
resin and filler in the material. Also, Table 2 provides the
Volume fraction calculations commonly used mass ratio of filler to resin, Mf/Mr, given
The following steps are used to convert the obtained in parts per hundred (pph) of the resin.
mass fraction to volume fraction (assuming that the From Table 3, it can be observed that the calculated
density of filler is known; if not, refer to Appendix III). glass fibre volume fraction values ranged from ~0.22 for
one of the structural shapes to 0.56 for the rebar speci-
1) To get a converted specimen volume, the expression men. The filler content (for those specimens containing

Table 2 Mass fraction results

Sample Mg/Ms M[/Ms M~IMs Mr/Mr

LV2 0.4209 + 0.0051 0.395 i + 0.0068 0.1839 _+0.0061 46.55
LV3 0.5069 + 0.0359 0.3565 + 0.0322 0.1366 + 0.0125 38.31
TV3 0.4119 +0.0047 0.4042 +_0.0059 0.1840 +_0.0015 45.52
TV4 0.3487 +0.0767 0.4715 +_0.0617 0.1798 +_0.0155 40.25
LP3 0.3617 +_0.0233 0.4561 +-0.0246 0.1867 +_0.0020 40.93
IPF 0.4565 _+0.0730 0.3641 +-0.0582 0.1794 +-0.0199 49.27
IPW 0.4405 + 0.0467 0.3899 + 0.0303 0.1696 + 0.0165 43.50
DP 0.6395 +0.0044 0.3605 +-0.0044 0 +0.0 0.0
DV 0.6343 +0.0035 0.3657 +-0.0035 0 +0.0 0.0
SP 0.64 19 + 0.0022 0.3322 +_0.0020 0.0258 + 0.0014 7.77
SV 0.6399 _+0.0051 0.3299 +-0.0065 0.0301 _+0.0014 9.12
REP 0.7564 _+0.0029 0.2436 +-0.0029 0 + 0.0 0.0

728 COMPOSITES Volume 26 Number 10 1995

 Mass and volume fraction of pultruded composites: B.S. Ye et al.
Table 3 Volume fraction results

Sample Vg/V~ Vd V~ Vd Vs

LV2 0.2792 _+0.0047 0.6747 _+0.0056 0.0461 _+0.0021

LV3 0.3465 + 0.0351 0.6184 _+0.0352 0.0352 _+0.0038
TV3 0.2698 _+0.0047 0.6856 _+0.0053 0.0446 _+0.0007
TV4 0.2182 _+0.0570 0.7399 _+0.0550 0.0419 _+0.0023
LP3 0.2449 _+0.0205 0.7074 _+0.0218 0.0477 _+0.0014
IPF 0.3154 _+0.0650 0.6380 + 0.0632 0.0469 + 0.0050
IPW 0.2985 _+0.0378 0.6574 + 0.0340 0.0443 _+0.0038
DP 0.4215 _+0.0046 0.5785 + 0.0046 0 _+0.0
DV 0.4160 _+0.0037 0.5840 _+0.0037 0 + 0.0
SP 0.4371 +0.0022 0.5562 +0.0022 0.0066 +0.0004
SV 0.4372 _+0.0065 0.5550 + 0.0070 0.0078 + 0.0005
REP 0.5604 + 0.0039 0.4396 _+0.0039 0 _+0.0

filler) was approximately 0.044).05 for all specimen types
except the SP and SV grating specimens, which had a
filler content of <0.01.
From the volume fraction values, it was observed that
the rebar and grating specimens had the highest volume
fraction of glass (0.42-0.56) and the lowest amount of
added fillers (04).01). The standard structural shapes
(e.g. I-section and channel) tested had a comparatively
lower glass content (0.224).35) and a substantially higher
filler content (0.04-0.05). The IPF and IPW specimens
varied greatly in both mass and volume fraction values
between the individual specimens of each type. This fact
can be seen in Table 4, which lists the three constituent
tests used to determine the values reported in Table 3.
Composite structure observation
The volume fraction test has uncovered some critical
features in the tested specimens. In addition to volume
fraction, ply layer composition plays an equally impor-
tant role in contributing to the composite strength. A
close observation of the post burn specimen was made
and recorded; refer to Figures 2-4 for the post burn-out
fibre architecture of some representative test specimens.
CONCLUSIONS AND RECOMMENDATIONS
Generally, manufacturers provide only average mass or
volume fraction properties for an entire line of products.
From the data presented here, it can be observed that
filler, fibre and resin contents can vary widely among
samples from a particular manufacturer. These varia-
tions are important to consider since mechanical prop-
erties have been shown to depend on mass and volume
fraction of glass 7. The glass fibre ply architecture is
another important issue to address: for two composites
with the same volume fraction of glass, a cross-ply speci-
men would have half the strength of a comparable all
unidirectional ply composite.
Filler is typically added to improve the fire resistance
and reduce the cost of a composite. It can also reduce
voids and improve processing viscosity. However, the
addition of fillers can reduce the mechanical properties
of the composite. Even small amounts of filler can
severely deteriorate the impact performance of the mate-
rial 7. Using volume fraction test data, it can be explained
why materials with similar fibre architectures can have
differing mechanical properties.
Although filler amounts seem small when Vf/V~ is
calculated, they become significant when examining the
Mf/Mr column in Table 2. This value is usually provided
in manufacturers' literature as filler parts per hundred of
resin. For the material from Creative Pultrusions, this
value ranges from ~38 to 46 pph for the structural shapes
tested, and for the one type of section tested from
M M F G this number varies from 43 to 49 pph.
The modified ignition loss test procedure for
pultruded material used in this investigation allowed the
simple determination of volume fraction results for
several types of pultruded glass fibre composites. It
provided a means for the identification and separation
of filler material from the glass fibres. The procedure,
through the use of acid dissolution of the filler,
was adequate for the kaolin clay found in the material
tested. This method is also appropriate when one of the
other two commonly used fillers, calcium carbonate
and alumina trihydrate, is present exclusively in the
material. However, if two or more fillers are mixed
together, from this method it is difficult to know precisely
the amount of filler lost during ignition loss. In this case,
the ASTM matrix digestion method 5 should be utilized.
In general, the significance of the volume fraction
test is that it yields a simple determination of the exact
fibre, matrix and filler contents in a composite.
This information provides necessary insight to gain a
better understanding of the behaviour of composite
materials.

Table 4 Individual test specimen values for IPF and IPW specimen types

Specimen type Mg/Ms Mr/M~ Mr/M~ Vg/Vs VJ V~ Vf/ V~

IPF Sample 1 0.5348 0.3351 0.4398 0.3801 0.5801 0.0398

Sample 2 0.4480 0.3904 0.4135 0.3051 0.6475 0.0474
Sample 3 0.4398 0.4135 0.1467 0.2912 0.6669 0.0418

IPW Sample 1 0.3837 0.4463 0.1700 0.2485 0.7040 0.0474

Sample 2 0.4735 0.3896 0.1369 0.3197 0.6405 0.0398
Sample 2 0.5085 0.3594 0.1381 0.3559 0.6025 0.0416

COMPOSITES Volume 26 Number 10 1995 729

Mass and volume fraction of pultruded composites: B.S. Ye et al.
REFERENCES
1 Bank, L.C. Civil Engineering January 1993, pp. 64-65
2 Bank, L.C. in 'Fiber Reinforced Plastic (FRP) Reinforcement
for Concrete Structures: Properties and Applications' (Ed. A.
Nanni), Elsevier Science Publishers, Amsterdam, 1993, pp. 59-86
3 Iyer, S.L. and Sen, R. (Eds) 'Advanced Composite Materials in
Civil Engineering Structures', American Society of Civil
Engineers, New York, 1991
4 ASTM Designation: D2584-68 (Reapproved 1985) 'Standard
Test Method for Ignition Loss of Cured Reinforced Resins',
'Annual Book of ASTM Standards', Vol. 8.01, American Society
for Testing and Materials, Philadelphia, PA, pp. 328 329
5 ASTM Designation. D3171-76 (Reapproved 1990) 'Standard
Test Method for Fiber Content of Resin-Matrix Composites by
Matrix Digestion', 'Annual Book of ASTM Standards', Vol.
8.01, American Society for Testing and Materials, Philadelphia,
PA, pp. 123 125
6 'Creative Pultrusions Burnout Procedure', Creative Pultrusions,
Inc., Alum Bank, PA, unpublished internal reference
7 Svenson,A.L. Report No. FHWA-RD-93-090, Federal Highway
Administration, Washington, DC, January 1994
8 Svenson, A.L., Hargrave, M.W. and Bank, L.C. in 'Proc.
Advanced Composite Materials in Bridges and Structures, First
Conference', Sherbrooke, Quebec, Canada, 7-9 October 1992,
pp. 559-568
9 Svenson,A.L., Hargrave, M.W. and Bank, L.C. in 'Proc. SPI
Composites Institute 48th Annual Conference and Exposition',
Cincinnati, OH, 8-11 February 1993, Session 21-D, pp. 1-6
10 Svenson,A.L., Hargrave, M.W., Bank, L.C. and Ye, B.S.J. Test.
Eval. 1994, 22(5), 431
11 Ye, B. Report No. FHWA-RD-94~48, Federal Highway
Administration, Washington, DC, July 1994
12 McCrone, W.C. and Delly, J.G. 'The Particle Atlas Edition Two,
Vol. III, The Electron Microscopy Atlas', Ann Arbor Science
Publishing, Ann Arbor, MI, 1973
APPENDIX I: TEST PROCEDURE
The ignition loss method has been considered a simple
and effective way to determine the volume fraction of
cured resin composite materials. But in many cases, it
has also shown some limitations when fillers have been
added to the material. The fillers, which may be partially
burned out or not burned out at all by the burn-out
process, stay with the glass fibre. This causes difficulties
in determining the fibre volume. Until now, there has
been no standard approach to separate fillers from the
resin and glass fibre of a pultruded composite. In this
appendix, a simple approach to supplement the current
ASTM D2584-68 Standard is presented.
Scope
This method closely follows ASTM D2584-68
(Ignition Loss of Cured Reinforced Resins) 4'5. It has been
adapted to be used on pultruded materials (i.e. materi-
als having varying thickness, filled resin systems, custom
reinforcement location and types, etc.) 6.
Apparatus
A Calipers, used to measure length of samples and
thickness of mats
B Electric muffle furnace, capable of maintaining
a temperature of 565 +28°C (1050 + 50°F), for
burning out specimen
C Gram scale capable of determining mass to
0.01 g
D Nitric and hydrochloric a.cids, used to identify
and dissolve filler from remains
E 100 ml glass beakers, to hold remains and acid
and process the chemical reaction to dissolve
filler
730 COMPOSITES Volume 26 Number 10 1995
G Conditioning oven to dry remains
H Fine screen for washing remains
I Ruler for measuring width of reinforcements
J Crucible, platinum or porcelain, approximately
30 ml capacity
K Desiccator, to cool the crucibles and burn-out
remains
L Safety equipment, such as heatproof gloves and
plastic gloves
Test specimen
The test specimen should be composed of the entire
cross-section of the profile if possible. This is the case
since quite often different reinforcement types will be
engineered into pultruded profiles 6. A representative
sample may be used instead of an entire cross-section if
the part is uniform throughout (e.g. fiat sheet). The speci-
men should be large enough to minimize the chance of
error but small enough for the mass of the specimen to
be determined on the gram balance. In addition, the speci-
men, after being cut, should show ply orientation in the
section.
Pre-test procedure
1) A table is prepared for recording the data.
2) The part name and size, the part it has been cut
from, date and manufacturer's or customer's name
is recorded on the table.
3) The specimen is measured on each side with calipers
(if the specimen is not uniform, multiple points are
measured and averaged) and the measurements are
recorded to the nearest mm.
4) The test method is recorded.
Test method
1) A crucible is heated to 600°C for 10 min or more.
It is then cooled to room temperature in a desicca-
tor and its mass is determined to the nearest 1.0 rag.
This is recorded on the data sheet.
2) The laboratory exhaust fan (or ventilation system)
is turned on.
3) The mass of the specimen and the crucible together
is determined to the nearest 1.0 mg. The crucible and
specimen are heated in a bunsen flame until the
contents ignite. The temperature is maintained such
that the specimen burns at a uniform and moderate
rate until only ash and carbon remain.
4) The specimen and crucible are placed in the furnace.
The heating element is turned on 'medium' (565°C).
The specimen is allowed to remain in the furnace for
a minimum of 2 h or until all carbonaceous mater-
ial has disappeared (extra time is required for thicker
laminates).
5) The crucible and remains are removed from the
furnace and cooled to room temperature in a desic-
cator. Then they are carefully placed on a gram scale
and the post burn-out mass is determined.
6) The laminate is carefully disassembled and a sketch
is made of the construction. The following observa-
tions are made at this time: (a) mat width and thick-
ness; (b) speciality reinforcements; (c) filler remains
present in the laminate; (d) roving placement and
yield (if possible); and (e) number of layers.
7) (a) Each type of reinforcement is segregated and
placed in individual beakers. The beakers are
 Mass and vo/ume fraction of pultruded composites: B.S. Ye et al.
labelled with the part name and the reinforcement
type. (b) If only glass fibre content is needed, all of
the fibre remains from the laminate can be put in
one beaker and be labelled accordingly.
8) If filler was observed in laminate, the following steps
are performed; otherwise, the calculations can now
be initiated. (Note: if a large amount of filler is
found, the disassembled laminates are put in a fine
screen and shaken well until most of the fillers are
removed. Then the following is done.)
(a) A small amount hydrochloric acid is placed in
one of the beakers containing reinforcement. If a
bubbling action occurs, then the filler type is calcium
carbonate. (b) If no bubbling occurs, then nitric acid
is added to the beaker. The ratio of nitric to
hydrochloric acid is ~1:1 (it is necessary that both
acids be present together for the chemical reaction
to occur, see Appendix II). The beaker is heated on
a hot plate for 15 min. If bubbling action occurs, the
filler present is kaolin clay. (c) Since ATH has a
similar chemical structure to kaolin clay, energy
dispersal X-ray fluorescence analysis 12 can be used
to identify one from the other. (d) All remaining
beakers are then treated with the appropriate acid.
(e) The filler type is recorded on the data sheet.
9) Once bubbling action stops, the acid is carefully
drained off. The remains are placed on a fine screen
and washed thoroughly under running water. The
excess water is squeezed out and the remains are
returned to their original crucible. These are then
placed in a conditioning oven at 175°C for a
minimum of 1 h.
Calcium carbonate
Reaction with hydrochloric acid:
CaCO3 + 2HC1 ~ CaCI2 + CO2 + H20
Kaolin clay
When heated to more than 500°C but less than 980°C:
A1203"2SiO2"2H20 heat__)A1203"2SIO2 + 2H20
Reactions when hydrochloric and nitric acid are mixed:
A1203"2SIO2 + 6HC1 ---) 2A1C13 + H20 + 2HzSiO3
A1203"2SIO2 + HNO3 ----) 2AI(NO3)3 + 2H2SIO3 + H20
APPENDIX III: D E T E R M I N A T I O N OF F I L L E R
DENSITY
1) Some regular-shaped specimens are chosen as base
specimens. These are accurately measured by taking
multiple measurements of each dimension and then
averaging to obtain the average length, width and
thickness. High accuracy is necessary in this step
because errors are induced as the density of the filler
is high but its volume is low.
2) The following equation is used to obtain the filler
volume:
vf= v~- Vg-Vr (A1)
Note: voids are accounted for as part of the filler
volume in this formula. By definition, and using the
unit conversion factor, yields

APPENDIX II: C H E M I C A L REACTIONS = •- x 10~ (A2)

~ Dg Or
Alumina trihydrate (or gibbs#e)
When heated to more than 500°C but less than 980°C: 3) The following formula is used to obtain the filler
density:
2AI(OH)3 heat._.)A1203 + 3H20
Reactions when hydrochloric acid and nitric acid are p f = Avg(-~ff / x 106 (A3)
mixed:
A1203 + 6HC1 - - ~ 2A1C13 + 3H20 Once the filler density is determined, it is held constant
for all the volume-converting calculations for the same
A1203 + 6HNO3 --~ 2Al(NO3)3 + 3H20 filler type.

COMPOSITES Volume 26 Number 10 1995 731