Wood Sci Technol 37 (2003) 233–240

DOI 10.1007/s00226-003-0172-x

Original

Analysis of Calcutta bamboo for structural

composite materials: surface characteristics
M. Ahmad, F.A. Kamke

233
Abstract The aim of this work was to assess the technical feasibility of producing
a structural composite from Calcutta bamboo. The approach was to compare
selected chemical, physical and mechanical properties of bamboo to timber
species that are commonly used in the manufacture of structural composites. This
paper addresses pH, buffer capacity, wetting and surface tension. Consideration
was given to the variability of these properties with respect to location along the
length of the bamboo culm, nodes versus internodes, and radial versus tangential
surfaces. Of course, other factors, such as mechanical properties, will also influ-
ence performance in composite materials. However, those issues, as well as the
evaluation of a prototype composite, will be addressed in a companion article.
Calcutta bamboo was found to have similar surface characteristics to commercial
timber species used in North America.

Introduction
Bamboo, as well as other woody materials, has the potential to supplement the use
of timber in structural composite products. The compatibility of alternative fiber
with available adhesive systems, primarily thermosets, is crucial for a successful
introduction into the market. Adhesive bonding of wood and other natural fibers
is influenced by surface characteristics, such as acidity and wettability. Acidity
may be assessed by pH and buffer capacity. Since the rate of cross-linking of most
thermosetting adhesives is pH-dependent, these adhesives will be sensitive to the
pH of the substrate (Blomquist et al. 1981). The formulation of most adhesives is
adapted to the acid range and buffer capacity of the substrate. However, a wide
deviation of this value will create difficulties in providing a superior adhesive
bond.

Received: 7 June 2001

Published online: 10 September 2003

Springer-Verlag 2003

M. Ahmad
Faculty of Applied Science,
Department of Wood Industry and Furniture Technology,
Universiti Teknologi MARA, Shah Alam, 40450, Selangor, Malaysia
F.A. Kamke (&)
Sustainable Engineered Materials Institute,
Virginia Tech, Blacksburg, VA 24061, USA
E-mail: Kamkefa@vt.edu
 Wettability is another factor influencing the formation of an adhesive bond.
Marra (1992) suggested that the five steps of adhesive bond formation in a wood
substance are wetting, flow, transfer, penetration and solidification. Wetting is an
indicator of the relative surface energy of the adhesive and substrate interface. A
convenient method to measure the wetting of a solid surface is through the
determination of the contact angle of a liquid. Fig. 1 illustrates the contact angle
of two liquids on a surface. According to Collett (1972), the contact angle is an
indicator of the affinity of a liquid for a solid. The shape of the liquid drop on a
solid surface is related to the magnitude of the cohesion forces acting between the
three planes: solid, liquid and gas (Bodig 1962). Bodig (1962) and Freeman (1959)
234 used the incline wood plate method, while Wellons (1980) and Kalnins and Feist
(1993) used the sessile liquid drop method to determine the contact angle, which
was referred to as wettability. The sessile drop method, while simple and widely
accepted, is somewhat time-dependent, when it is applied to a porous substrate
like wood or bamboo.
The pH value of several agriculture materials such as hemp, wheat straw, flax
and grass were determined by Hague et al. (1998). The performance of the
materials as panel products, when bonded with UF, was found to be poor. This
poor performance was attributed to the high pH values, which were more than 6
in the case of wheat straw, and more than 7 in the case of hemp. Maloney (1993)
explained that the effect of acidity on cure rate or press times is due to the
combination of pH, buffer capacity and the existing or potential total free volatile
acid content of the material. Knowledge of the chemical condition of a woody
material is a useful guide for selecting an adhesive system. Thus, pH is closely
related to adhesive bond quality and total manufacturing cost, and must be
considered as one of the important factors in determining the suitability of the
raw material.

Experimental

Materials
Calcutta bamboo, Dendrocalamus strictus, was acquired from a Southeast Asian
distributor. This bamboo had an average culm length of 5.5 m (18 ft.), a bottom
diameter of about 3.3 cm (1.3 in.), and a top diameter of about 2.3 cm (0.9 in.).
The average thickness of the culm wall was 0.97 cm (0.38 in.). The average oven-
dry density was 643 kg/m3 (40.1 pcf), while the initial moisture content ranged
from 10 to 11%. The culms were cut into 122 cm (4 ft.) lengths, and placed in a
conditioning chamber (20C and 65% relative humidity) until an equilibrium
moisture content of approximately 9% was reached.

Fig. 1. Finite contact angle (h) of a sessile drop resting on a bamboo surface, showing a
high degree of wetting (A) and a low degree of wetting (B)
Methods
Specimens that were selected from the culms were obtained from four locations
relative to the height in the culm, referred to as Location 1 at the bottom to
Location 4 at the top. The culm sections were split into half and specimens were
randomly selected for the analysis. The specimens were kept in the conditioning
chamber until they were used for testing.

pH
The procedure of pH determination was adapted from the cold extraction method
for hydrogen ion concentration (pH) of paper extracts (TAPPI 1983). Each
specimen was ground to pass a 425-lm (40 mesh) using a milling machine. The 235
specimen (1 g ± 0.01 g) was then transferred into a 100-mL beaker and distilled
water (pH~ 6.7) was added until the specimen was saturated. Distilled water was
added again to bring the total volume to 70 mL. The mixture was stirred well and
allowed to soak for 1 hour at room temperature. The pH meter was calibrated and
the electrode submerged into the unfiltered mixture. The pH value was recorded,
when there was no more drift in the measurement for a period of 30 seconds. An
analysis of variance was performed and Tukey’s Studentized Range (HSD) Test
was used for the comparison procedure.

Buffer capacity
Specimens for buffering capacity were taken from Location 1 of the culm. The
procedure for buffer capacity determination was adapted from the method re-
ported by Maloney (1993). Specimens were again prepared in the milling machine.
30 g of dry fibers were soaked in 400 g of distilled water (20 ± 1C) for 30 minutes.
The mixture was stirred several times. The liquid was then filtered, and 150 g of the
liquid was placed in a beaker. The temperature was maintained at 21C. The pH
meter was again calibrated and used to determine the starting pH value. Titration
was done using 0.01 N hydrochloric acid. The pH value was recorded after each
acid addition. An addition was made at an increment of 0.5 mL up to 10 mL, and
then with increments of 1.0 mL thereafter. A magnetic stirrer was used to mix the
titration solution. The milliequivalent (N x mL) of acid needed to change the pH to
3.5 was calculated as the buffer capacity of Calcutta bamboo.

Wetting
The sessile drop method was used for the contact angle and surface tension
measurement (Zhang et al. 1997; Good, 1992). Specimens for wettability and
surface tension were taken from Locations 1 and 2, while specimens for com-
parisons along the height were taken from Location 1 to 4. Specimens at the nodes
and radial surfaces were also taken for the comparison study (Fig. 2).

Fig. 2. Macroscopic features of the bamboo culm, showing a longitudinal section (A) and a
cross-section view (B)
 All measurements were performed on a freshly prepared, tangential surface,
which was obtained by gently abrading the specimen using 220 grit sandpaper
immediately before testing. All surfaces were sanded at the same rate and tested
within a 2 hour period. A 5 micrometer pipette was used to manually apply the
drops of liquid. Images of the drops were captured by video camera within two
seconds after the drops were applied. The wetting values of the surface were
reported either as the contact angle or by the cosine of the contact angle. Surface
tension, and other components of the surface energy, were determined using
three probe liquids, a-bromonaphthalene (ABN), water and ethylene glycol (EG).
In addition, formamide (Fo) and glycerol (Gl) were used to compare the results.
236 Comparisons between location, section (nodes and internodes) and surface were
done within 10 seconds using glycerol only. At least 30 contact angle measure-
ments were obtained for each liquid probe, and at least 50 measurements were
obtained for Locations 1 to 4 using glycerol. The calculation of the bamboo
surface energy was carried out by using the following equation:
h

þ
1=2

þ 1=2 i
LW 1=2
ð1 þ coshÞcL ¼ 2 cLWs cL þ cs cL þ cs cL ð1Þ

where csLW (Lifshitz van der Waals or apolar), cs+ (acid or electron accepting),
and cs- (base or electron donating) are the solid surface energy components, h is
the contact angle obtained by the sessile drop method for each liquid, cL is the
liquid surface tension, and cLLW, cL+ and cL- are the liquid surface energy com-
ponents. The liquid surface energy components for the probe liquids are given in
Table 1.
All three probe liquids were used to obtain the contact angle measurements.
Then, using the known liquid surface tension parameters from Table 1, the
bamboo surface energy components were calculated by solving a set of three
simultaneous equations. Total surface tension of bamboo cstotal was then calcu-
lated using the following equation:

þ 

 1=
ctotal
s ¼cLW
s þ2½ cs cs  ð2Þ

Analysis of variance was performed and Tukey’s Studentised Range (HSD)

Test was used for the comparison between Locations 1 to 4.

Results and discussion

pH and buffer capacity

Table 2 shows the pH by location in the culm. No significant differences in pH
value between locations were detected (F-value = 4.26). The overall mean pH

Table 1. Surface tension parameters of probe liquids (mJ/m2) used for contact angle
experiment (Good, 1992)

Probe liquid cL cLLW cL+ cL-

a-Bromonaphthalene 44.4 43.5 @0 @0

Water 72.8 21.8 25.5 25.5
Ethylene glycol 48.0 29.0 1.92 47.0
Formamide 58.0 39.0 2.28 39.6
Glycerol 64.0 34.0 3.92 57.4
Table 2. pH and buffer capacity for Calcutta bamboo (by location in culm) and selected
timber species (Fengel and Wegener 1984; Freeman 1959)

Species (culm location) Mean pH Buffer capacity

(Std. dev.) (Milli-equivalent)

Calcutta bamboo (1) 5.13 (0.23) 0.06

Calcutta bamboo (2) 5.13 (0.13) -
Calcutta bamboo (3) 5.17 (0.26) -
Calcutta bamboo (4) 5.44 (0.29) -
Populus spp.(aspen, cottonwood) 5.8 0.230–0.308
Pinus resinosa(red pine) 6.0 -
Pinus sylvestris(scots pine) 5.1 - 237
Pinus strobus(eastern white pine) 4.9 -
Pseudotsuga menziesii(Douglas fir) 3.3 0.03–0.09
Tsuga canadensis(eastern hemlock) 5.5 0.17–0.23
Shorea spp.(meranti or lauan) 4.7 -
Liriodendron tulipifera(yellow poplar) 5.0 -
Quercus alba(white oak) 3.5 0.1
Quercus rubra(red oak) 3.5 -

Table 3. Mean wettability of Calcutta bamboo as determined by five liquid probes

Probe liquid Contact angle Cosine of contact angle

Water 52.2 0.61

a-Bromonaphthalene (ABN) 13.4 0.97
Ethylene glycol (EG) 25.5 0.90
Formamide (Fo) 20.3 0.94
Glycerol (Gl) 97.4 -0.13

value was 5.21. Table 2 also lists the pH values of several timber species that are
commonly used in the composites industry in North America. The pH value of
Calcutta bamboo lies within this range, and is quite similar to yellow poplar,
hemlock, and the pine species listed.
Based on the acid titration analysis for buffer capacity, it takes approximately
6 mL of acid to change the pH of the liquid to 3.5. Thus, the milliequivalent (me.),
or the buffer range, of Calcutta bamboo was 0.06 (0.01 N x 6 mL). Table 2 also
presents the buffer range of several wood species (Graves 1985). Generally, aspen
and hemlock are said to possess a high buffer capacity, while Douglas fir and
white oak have a low buffer capacity. By comparison, Calcutta bamboo would be
considered to have a low buffer capacity. Thus, Calcutta bamboo should not
require any special consideration in regard to catalyst addition and resin cure.

Wettability and surface tension

The wettability of Calcutta bamboo is reported in Table 3 as the mean contact
angle using the probe liquids included in this study. Freeman and Wangaard
(1960) reported the contact angle of water on several timber species using the
incline plate method. Although the method used in this study is different, the
contact angle obtained should be approximately the same, and the values are used
for comparison. Among the timber species included were aspen (Populus trem-
uioides), yellow poplar (Liriodendron tulipifera) and white oak (Quercus alba).
Contact angles of water on these timber species were 38, 51 and 50, respectively.
 The contact angle using water on Calcutta bamboo was 52. The wettability of
Calcutta bamboo was very close to yellow poplar and white oak. The smaller the
contact angle, the better the wettability. In this case, the wettability of Calcutta
bamboo was less than aspen, but very close to yellow poplar and white oak.
The average surface tension of Calcutta bamboo is reported in Table 4 along
with values reported in the literature for several timber species. The total surface
tension of Calcutta bamboo was slightly higher than yellow poplar. From Table 4,
the total surface tension of Calcutta bamboo was 54.3 mJ/m2, while yellow poplar
was 54.0 mJ/m2. When formamide and glyserol were used as the liquid probe, the
total surface energy was 62.1 and 55.4 mJ/m2, respectively. The average of total
238 surface tension, as determined by the three liquid probes (EG, Fo and Gl) was
57.3 mJ/m2.
The surface tension characteristics of Calcutta bamboo were similar to timber,
since it was also dominated by the Lifshitz van der Waals’ component. The value
of the Lifshitz van der Waals’ component of the surface tension for Calcutta
bamboo and yellow poplar were 44.1 and 44.6 mJ/m2, respectively. Calcutta
bamboo had a lower acid-base character than yellow poplar, ash, maple, red oak
and walnut, but was slightly greater than cherry and white oak. The acid-base
character of Calcutta bamboo was dominated by the electron donating sites on its
surface. This is similar to timber, which was also dominated by the electron
donating sites. From the surface tension values determined in this study, Calcutta
bamboo should have similar interactions with the common adhesives used with
the timber species mentioned.
A comparison of the contact angle using glycerol (within 10 seconds) was
made between the location, section and surface in the culm. The analysis of
variance indicated that there were some significant differences between the
locations (F-value = 3.9) and sections (F-value = 49), while there was no signif-
icant difference between the surfaces (Table 5). Location 2 had a significantly
higher contact angle than Location 4 (alpha = 0.01). No other differences by
location were detected. The contact angle of the nodes (77.4) was significantly
greater than the internodes (57.6). An explanation for this behavior may be a
higher extractive content in the nodes compared to the internodes. However, the
extractive content was not investigated here, and no previous studies could be

Table 4. Surface tension parameters of Calcutta bamboo and several timber species (mJ/
m2)

Material csLW cs + cs - cstotal

Calcutta bamboo
EG 44.1 0.89 29.2 54.3
Fo 44.1 3.00 27.1 62.1
Gl 44.1 0.00 30.2 55.4
Yellow-poplar1(Liriodendron tulipifera) 44.6 0.70 31.6 54.0
Ash2(Fraxinus americana L.) 42.6 0.001 67.4 43.2
Cherry2(Prunus serotina Ehrh.) 47.5 0.42 28.0 54.3
Hard maple2(Acer saccharum Marsh.) 45.5 0.46 33.2 53.3
Red oak2(Quercus rubra L.) 39.7 0.46 37.7 48.0
White oak2(Quercus spp.) 34.0 0.39 22.8 40.0
Walnut2(Juglans nigra L.) 37.9 0.09 58.9 42.6
1
Timber species tested at the same venue and time with Calcutta bamboo
2
Gardner (1996)
Table 5. Mean contact angle (standard deviation in parentheses) for glycerol on Calcutta
bamboo, separated by location in the culm, section, and surface

Culm Section Surface Contact angle

Location (degree)

1 Internode Tangential 55.8 (8.79)

2 Internode Tangential 56.6 (6.18)
3 Internode Tangential 54.6 (5.94)
4 Internode Tangential 52.4 (6.63)
1 and 2 Node Tangential 77.4 (14.6)
1 and 2 Internode Tangential 57.6 (7.48)
1 and 2 Internode Radial 57.8 (6.43) 239

found. The anatomical structure of the nodes is different from the internode
sections (Grosser and Liese 1971), which may account for some difference in
contact angle. The nodes have an irregular interwoven texture formed by the
vascular bundles. Fiber strands and lateral sclerenchyma sheaths of the metaxy-
lem vessels are absent. The contact angles of the radial and tangential surfaces
were not significantly different from each other. In general, there was little var-
iability in the contact angle, with the exception of the nodes, due to location and
surface in the culm.

Conclusion
Generally, Calcutta bamboo has a comparable pH, buffer capacity, and wettability
to timber species commonly used in wood-based composite products. These
similarities will allow the use of commonly available thermoset adhesives in the
manufacture of composites from Calcutta bamboo. The wettability of the radial
and tangential surfaces was similar, while the pH and wettability showed little
variability along the length of the culm. From a practical point of view, this is
desirable behavior, because any variation in surface characteristics would com-
plicate the adhesive bonding process. However, the wettability of the nodes was
found to be lower than that of the internodes, which may impose some variability
in adhesive bonding.

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