Advances in Bamboo Science 2 (2023) 100014

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Advances in Bamboo Science

journal homepage: www.journals.elsevier.com/advances-in-bamboo-science

Original article

Assessment of physical, mechanical, and chemical properties of

Dendrocalamus asper bamboo after application of wetting and drying cycles ]]
]]]]]]
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Leo Maia do Amarala, , Conrado de Souza Rodriguesb, Flávia Spitale Jacques Poggialib
⁎

a
University of São Paulo (USP), Department of Biosystems Engineering. Pirassununga, São Paulo, Brazil
b
Federal Centre for Technological Education of Minas Gerais (CEFET-MG), Department of Civil Engineering, Av. Amazonas, 7675, Nova Gameleira, Belo Horizonte, Minas
Gerais, Brazil

A R T I C L E I N F O A B S T R A C T

Keywords: Given the hygroscopic nature of bamboo and its reduction in strength with increasing moisture content, we
Bamboo evaluated the effects of hornification – generated through the application of drying and rewetting cycles – on the
Hornification physical, mechanical, and chemical properties of the culms of Dendrocalamus asper. Our objective was to assess if
Physical properties the treatment would cause a reduction in water uptake, an increase in the dimensional stability of bamboo, and a
Chemical properties
stiffening of the material, increasing its mechanical strength. Specimens were submitted to a maximum of 15
Mechanical properties
cycles, being immersed at room temperature (22 ± 3 °C) and dried at 50 ± 5 °C. Absorption capacity, di-
mensional stability, density as measured with a helium pycnometer, tensile tests, scanning electron microscopy
(SEM) analysis, X-ray diffractometer (XRD) and Fourier-transform infrared spectroscopy (FT-IR) were under-
taken. Hornification increased the dimensional stability of bamboo proportionally to the number of cycles ap-
plied, and a 5.8 % increase in cross section was seen after 264 h for 15 cycles. The control samples increased by
17.8 %. Reduction in the water absorption was not verified for treated bamboo. The elastic modulus was
maintained and the tensile strength after treatment was reduced (258.6 MPa for control and 207.5 MPa after 15
cycles). Chemical analysis and microscopy did not show any significant changes in the composition of the
bamboo after the application of wetting and drying cycles.

1. Introduction Humidity is one of the most important factors to be aware of with

The search for sustainable materials and technologies for the
construction industry is becoming increasingly important because of
the increasing demand for construction materials and the impacts
that extraction of these materials have on the environment
(Drumond and Wiedman, 2017; WBCSD, 2018). Bamboo is a plant
that can be used as an alternative to many other materials as it has
good mechanical performance and is environmentally friendly,
contributing to carbon sequestration, recovery of poor soils during
its growing, and protection from soil erosion and landslides (Janssen,
2000; Rao, 2004).
Interest in bamboo and its use in construction has been growing in
recent decades. Nevertheless, care must be taken as bamboo is a natural
material. Factors such as humidity, insulation, degradation by external
agents (fungi, termites, and beetles) all need to be considered (Liese and
Tang, 2015a; Yu et al., 2018). Consequently, the use of preservative
treatments is required if bamboo’s durability and performance over
time is to be guaranteed.
bamboo as, due to its nature, bamboo tends to reach an equilibrium
with its environment and has a high capacity to adsorb water in the
form of steam. At between 12 % and 30 %, an increase in moisture
content leads to reductions in the mechanical performance of the
structural element (Chung and Yu, 2002; Sánchez and Morales, 2019;
Xu et al., 2014), and causes dimensional changes, mainly in the radial
direction (Azadeh and Ghavami, 2018). Also, higher moisture contents
increase the probability of fungal attack (Liese and Tang, 2015a).
In this context, a treatment based on the application of wetting and
drying cycles is being tested on vegetal fibres to reduce their absorption
capacity, improve their dimensional stability and their ability to bond
to a cementitious matrix (Ballesteros et al., 2015; Ballesteros et al.,
2019; Claramunt et al., 2010; Ferreira et al., 2015; Ferreira et al.,
2017). This process causes an effect called hornification, which was first
observed in the recycling process used by the papermaking industry. It
was observed that the recycled material became stiffer after the re-
moval of water. The changes included a reduction in the volume and
quantity of pores, a stiffening of the polymeric structure of the fibre,

⁎
Corresponding author.
E-mail addresses: leoamaral@usp.br (L.M. do Amaral), crodrigues@cefetmg.br (C.d.S. Rodrigues), flaviaspitale@cefetmg.br (F.S.J. Poggiali).

https://doi.org/10.1016/j.bamboo.2022.100014
Received 5 October 2022; Received in revised form 28 December 2022; Accepted 28 December 2022
2773-1391/© 2022 The Authors. Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali
and a reduction in the water absorption capacity (Diniz et al., 2004;
Stone and Scallan, 1965).
Although there has been a wide range of publications dealing with
the effects of hornification on vegetal fibres, a literature survey re-
vealed only two studies looking at the impacts of wetting and drying
cycles on bamboo. Betz (2018) applied wetting and drying cycles to
Guadua angustifolia Kunth bamboo specimens to simulate the potential
effect of rain on a bridge and found that, in agreement with the results
obtained from vegetal fibres, there is a tendency to reduce the ab-
sorption capacity of the material. Cid et al. (2020) also identified a
reduction in water absorption capacity after 10 cycles on Phyllostachys
edulis J.Houz. (syn. Phyllostachys pubescens Mazel ex j.Houz.) bamboo.
Through four-point bending tests, they also observed a slight increase in
stiffness and, after five cycles, an increase of 65 % in the modulus of
elasticity.
In view of the reported results, this study aimed to explore further
the hornification effect on bamboo, assessing whether the application of
water immersion and drying cycles can increase its dimensional stabi-
lity, reduce its water uptake, and improve the mechanical properties of
the material. Physical, mechanical and chemical tests were applied to
Dendrocalamus asper Backer ex K.Heyne bamboo before and after wet-
ting and drying cycles.
2. Materials and methods
2.1. Materials
Dendrocalamus asper was selected for this study because of its
availability on Brazil in comparison to other commonly used species in
engineering, and because of its good mechanical properties, either in its
natural form (Gauss et al., 2021a) or engineered (Kadivar et al., 2022).
Seven bamboo stem sections, from different culms, with length between
2 and 4 m were provided by the Bamboo and Social Technologies Re-
ference Center (CERBAMBU), located in Ravena, Minas Gerais, Brazil
(19°48′ S; 43°43′ W). The mature culms, aged four years, were har-
vested, and naturally air dried for four months. Following this, they
were stored in a protected environment without further treatment. Two
sections were from the top (external diameter = 88.5 mm, wall
thickness = 8.25 mm), and one from the basal region (external dia-
meter = 91.75 mm, wall thickness = 16.0 mm). These were used only
on the first adjustment step, which comprised the definition of im-
mersion and drying durations. All the other tests were performed on
sections obtained from the middle region of the culms (external dia-
meter = 95.0 mm, wall thickness = 12.0 mm). This reduced the
variability of the material. The internal layer and external bamboo skin
were not removed from the samples.
Tap water at room temperature (22 ± 3 °C) was used to immerse
the bamboo. All drying was done in an oven at a temperature of
50 ± 5 °C. Table 1 summarizes the dimensions and number of samples
used in each test. Further details are provided in the following sections.
Table 1
Sample dimensions, number of samples and tests performed.
Dimensions (L x Ta) (mm) Number of samples
200 × 10 7 -
25 × 25 48
25 × 25 48 (12 per group)
20 × 20 48 (12 per group)
12.5 × 7 4 (2 per group)
Bamboo particlesa 2 (1 per group)
200 × 2 32 (8 per group)
20 × 20 2 (1 per group)
Bamboo particles 2 (1 per group)
Bamboo particles 2 (1 per group)
a
L: longitudinal direction; T: tangential direction (width); Bamboo particles that passed through a 100-mesh sieve; SEM: scanning electron microscopy; XRD: x-ray
diffractometry; FT-IR: Fourier-transform infrared spectroscopy.
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Advances in Bamboo Science 2 (2023) 100014
2.2. Definition of immersion and drying durations
This step aimed to establish how long the material need to be im-
mersed in water to reach a moisture content above the fibre saturation
point (FSP), and the drying time that would guarantee a low moisture
content, as indicated by the closing and reduction of pores.
A moisture content of 30 % represented the minimum value ex-
pected after each wetting step (WL) and was defined based on FSP
values for bamboo. In general, a FSP between 28 % and 32 % for
bamboo is expected (Liese and Tang, 2015b), and for Dendrocalamus
asper a value of 29 % was found in the literature (Silviana, Petermann,
M., 2014).
A limit of 10 % was defined as the maximum moisture content that
the bamboo specimens should have after each drying step (DL). This
ensured that a large part of the water present in the fibres was removed,
causing the hornification effect.
The procedure adopted in the present research was based on the
steps described by Cid et al. (2020). Bamboo specimens were first im-
mersed in water at 22 ± 3 °C for seven days and had their masses
measured in time intervals of 24 h. Immediately after that, they were
dried in an oven at 50 ± 5 °C for seven days and the same time in-
tervals were applied for weighing. The specimens were later dried at
103 ± 2 °C until constant mass and had their moisture content de-
termined by Eq. 1 (ABNT, 2020). The moisture content before the start
of the test was 12.7 % with a standard deviation of 1.9 %.
m m0
MC (%) = x100
m0 (1)
Where m is each weight measure during immersion or drying at
50 ± 5 °C and m 0 is the weight after drying at 103 ± 2 °C.
The weights obtained during each procedure were plotted on a
graph to assess the moisture content variation, and through graphic
analysis, immersion and drying durations were defined to further ap-
plication of wetting and drying cycles on bamboo samples, and as-
sessment of its effects.
2.3. Water absorption
The determination of water absorption followed the Brazilian
Standard – NBR. (2020). With the results from the procedure described
in 2.2, the durations of immersion and drying were defined and applied
to the bamboo samples. After each step of immersion or drying, the
weights of the bamboo samples were measured and, after 15 cycles, the
samples were dried in an oven at 103 ± 2 °C until constant mass to
calculate their moisture content. The variation in absorption capacity
was determined in order to reduce the influence of the moisture content
after drying. Eqs. 2 and 3 indicate how the absorption and retention
capacities were obtained. The Eq. 4 represents the determination of the
variation of absorption capacity.
Number of cycles Test
Definition of immersion and drying durations
1–15 Water absorption
control, 5, 10 and 15
control, 5, 10 and 15 Dimensional analysis
control and 10 Density
control and 10
control, 5, 10 and 15 Tensile
control and 10 SEMa
control and 15 XRDa
control and 15 FT-IRa
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali Advances in Bamboo Science 2 (2023) 100014

Fig. 1. Water absorption sample: A) sample without skin removal; B) sample

cross section.

m wet m 0
ABS (%) = x100
m0 (2)

mdry m0
RET (%) = x100
m0 (3)
Fig. 2. Cross section analysis procedure: A) digital camera photo; B) 8-bit
image; C) threshold for area calculation; D) considered cross-sectional area.
ABSx (%) = ABSx RETx 1 (4)

Where m wet is the weight of bamboo coupons after each wetting step,
mdry is the weight after each drying step, ABSx is the absorption capa-
city in a certain cycle and RETx 1 is the retention value in the previous
cycle.
Another water absorption test was performed to allow comparison
of the results with other treatments applied to bamboo (Gauss et al.,
2021a; Gauss et al., 2021b). Bamboo samples without treatment (con-
trol), were assessed after 5, 10 and 15 cycles. The procedure was similar
to that applied in other research (Gauss et al., 2021a; Gauss et al.,
2021b) and comprised the following steps: Drying in an oven at
50 ± 5 °C for 69 h to reduce the variability of the moisture content;
immersion in water, and mass measurements after 1, 12, 24, 98 and
268 h; the amount of water absorbed was determined in relation to dry
weight obtained in the first step. A sample for water absorption tests is
shown on Fig. 1. Fig. 3. Cross section of prismatic specimens for density assessment using a
helium pycnometer.

2.4. Dimensional variation analysis

The following procedure was used to evaluate the effect of horni-
fication on the dimensional stability of bamboo. Measurements of the
cross section were made after 12, 24, 96 and 264 h of water immersion
and the results compared with the values obtained before immersion,
enabling the calculation of the dimensional variation. All the specimens
were dried for 72 h in an oven at 50 ± 5 °C before being immersed in
water. Images (1200 ×1600 pixels) from each cross section of bamboo
were obtained with a digital camera from a predefined and constant
distance (Fig. 2). ImageJ software (Schneider et al., 2012) was used to
process the images using a threshold-based pixel count measurement,
calculating the cross-sectional area of each sample. We chose to mea-
sure the cross-sectional area of the bamboo using digital image analysis
because of the natural curvature of the material.
2.5. Density measurements with a helium pycnometer
Real density was measured using a helium pycnometer. Two types of
specimens were assessed: First, prismatic specimens 12.5 mm long and
7 mm wide (Fig. 3), without and after treatment (10 cycles), had their
densities measured to verify if the reduction of volume and quantity of
pores could be observed through this test. Later, bamboo particles that
could pass through a 100-mesh sieve were used to compare with the
results obtained in the first step and with values reported in the lit-
erature. Each sample had its density measured 8 times. Before both
tests, the specimens were dried in an oven at 50 ± 5 °C for 70 h.
2.6. Mechanical characterization: tensile test
Tension tests parallel to the fibres were performed based on
Brazilian Standard - NBR (2020), using a universal testing machine
EMIC with 300 kN capacity. A displacement ratio of 1.0 mm.min−1 was
applied and a clip gage was used to gather displacement measures,
allowing the calculation of the modulus of elasticity (Et,0) with higher
accuracy.
The tensile strength was determined by dividing the maximum load
applied by the cross-section area. The modulus of elasticity was cal-
culated through Eq. 5.
Et ,0 = ft / (5)
Where Δft is the difference between the maximum and the minimum
stress within the elastic region, and Δε is the respective difference in
displacement.
Prismatic specimens 4 mm wide were obtained from bamboo in-
ternodes with a chisel and then reduced with a sanding machine to
2 mm. Their length was 200 mm. To ensure the effectiveness of the grip
and to prevent unexpected damage to the specimens, aluminum oxide
sandpaper was placed between the sample and the equipment grip,
following the method proposed by Azadeh (2018).
All the specimens were dried for 72 h in an oven at 50 ± 5 °C before
testing. This reduced the variability of moisture contents between
samples from different groups, as their treatments (control, 5, 10 and
15 cycles) had different time spans. To calculate the moisture content,

3
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali Advances in Bamboo Science 2 (2023) 100014

each group of specimens had a representative sample with dimensions

of 25 × 25 mm, which had its mass measured before each tension test
and after drying at 103 ± 2 °C until constant mass (NBR, 2020). Also,
apparent density was obtained through mass and size measurements of
each sample, with the dimensions being obtained using a digital caliper
(Dixon and Gibson, 2014).

2.7. Scanning electron microscopy (SEM)

Two representative specimens, one without treatment (control) and

the other after 10 cycles, were observed using scanning electron mi-
croscopy. Observations were made in a longitudinal direction, which is
the orientation of the bamboo fibres. The images were obtained by
backscattering electrons through a low vacuum HITACHI TM3000
electron microscope. The specimens were analyzed without any pre-
treatment or coating. Fig. 4. Moisture content of bamboo specimens after immersion and drying.

2.8. X-ray diffraction (XRD)
The objective of this test was to evaluate the bamboo crystallinity
without and after 15 cycles of drying and wetting. A crystallinity index
was calculated using the method proposed by Segal et al. (1959) (Eq.
6).
I002 Iam
Cr . I (%) = x100
I002 (6)
Where I002 is the maximum intensity of the reflection plane (002) to
cellulose type I at approximately 2ϴ = 22.7°, and Iam is the intensity of
the plane to the amorphous region at 2ϴ = 18.0°.
The bamboo particles were obtained after grinding a 25 × 25 mm
bamboo specimen until the particles passed through a 100-mesh sieve.
Before testing, the particles were dried in an oven at 50 ± 5 °C for
72 h. An XRD-7000 Shimadzu diffractometer was used with 40 kV
voltage and 30 mA current. The scanning was made between 5° and 65°
ϴ-2ϴ at a 10°/min rate.
limit of moisture content after the drying phase and WL corresponds to
the inferior limit of moisture content after the immersion phase, as
defined in section 2.2.1. After 24 h the target for immersion (moisture
content of 30 %) was reached. Also, after 24 h of drying (between 168
and 192 h), a moisture content below the target of 10 % for the drying
phase was achieved.
To define the duration of cycles, the moisture contents during ab-
sorption and desorption recorded in this test, and the values applied by
Cid et al. (2020), after 24 h immersion and 48 h drying, were con-
sidered. For the drying phase, low variation of moisture content be-
tween samples, below 10 %, was observed after 72 h (264 h on the
Fig. 4). The immersion and drying durations were set to 96 and 72 h,
respectively, to guarantee the occurrence of the hornification effect and
a low variation after oven drying. The immersion phase occurred in tap
water at ambient temperature (22 ± 3 °C) and the drying phase oc-
curred at 50 ± 5 °C in an oven.
3.2. Water absorption

2.9. Fourier-transform infrared spectroscopy (FT-IR) analysis
Possible chemical changes after hornification were investigated
through Fourier transform infrared spectroscopy. One representative
sample for untreated bamboo and one sample after 15 cycles of wetting
and drying were used. Bamboo particles were obtained using the same
method as in the XRD test, and the samples were dried in an oven at
50 ± 5 °C for 72 h prior to the test. A Shimadzu IRPrestige-21 spec-
trometer was used, and 53 scans were performed along the spectrum
4000–400 cm−1 with a resolution of 2 cm−1.
2.10. Statistical analysis
The moisture contents of the bamboo specimens were measured
during 15 cycles of wetting and drying. Fig. 5 presents the moisture
contents after all immersion phases. To facilitate the analysis of the
results, only comparison between the 2nd cycle (first one being con-
sidered), the 5th cycle (higher moisture content) and 11th cycle (major
decrease) were showed. The complete statistical analysis can be found
in the appendix (Table A.1).
The mean moisture content of the samples after a single immersion
phase was higher in comparison to the following immersion phases.
This occurred because the specimens were not dried prior to the start of
the cycles and had a mean moisture content of 16 %. The first cycle was

Repeated measures analysis of variance (ANOVA) and Bonferroni

post-hoc tests were applied to the water absorption measurements
throughout the application of the wetting and drying cycles. One-way
ANOVA and Tukey post-hoc tests were applied to water absorption, for
the control, 5, 10 and 15 cycles; dimensional analysis; density, to
compare the four different groups; and tensile tests. To verify sig-
nificant differences between densities from prismatic samples (control
and 10 cycles), t-tests were applied. Two assumptions were verified:
normality (Shapiro-Wilk’s test) and equality of variances (Levene’s
test), when applicable.

3. Results and discussion

3.1. Definition of immersion and drying durations

The results related to absorption and desorption of the bamboo

specimens are shown in Fig. 4, in which DL corresponds to the superior Fig. 5. Variation of moisture content during the wetting and drying cycles.

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L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali
Fig. 6. Variation in absorption capacity during cycles.
therefore excluded from the absorption analysis. We suggest that to
allow comparison between all cycles, the treatment should start with
the drying phase.
As shown in Table A.1, statistical differences in the absorption ca-
pacity were tested for all cycles. Moisture contents were the lowest after
2 and 11 cycles, and the highest after 5 cycles (Fig. 5). A gradual in-
crease in water absorption was observed up to the fifth cycle. After that,
a decrease occurred until the 11 cycle, with a new increase then being
observed.
The same behaviour was found by Cid et al. (2020) during an eva-
luation of hornification on Phyllostachys edulis bamboo (moso bamboo).
Although their immersion and drying intervals were different to the
ones we used, an increase in the moisture content up to the fourth cycle
and a subsequent decrease to the tenth cycle were observed. Cid et al.
(2020) attributed the increase in water absorption capacity in the initial
cycles to the removal of water-soluble extractives from the bamboo,
which leads to a higher number of voids in the culm and, consequently,
a greater capacity to absorb water.
Although the drying phase duration was constant, after each phase
different moisture content values were observed (below the defined
target). To reduce the influence of this factor, the variation in absorp-
tion capacity was determined (Eq. 4) and represented graphically
(Fig. 6). The complete statistical analysis is presented in Table A.2.
Similar behaviour to that observed in Fig. 5 can be seen for the
variation in water absorption capacity. The second cycle presented the
lowest variation, being statistically different from cycles 5 and 6, which
presented the highest values. This is consistent with the hypothesis
regarding the removal of water-soluble extractives and an increase in
the number of voids until 5 cycles (Cid et al., 2020). After the sixth
cycle, the variation declines until the ninth cycle, which can be ex-
plained by a continuous reduction in the empty spaces in the bamboo
structure and pore closure, characteristics of the hornification effect.
For vegetable fibres, the reduction in water absorption capacity is ob-
served from the first cycles, implying that pore closure occurs gradually
as the treatment progresses (Amaral et al., 2021). Water absorption
Table 2
Mean values of water absorption for bamboo.
Treatment Mean value of water absorption % (Standard Deviation %)
1h 12 h
No treatment 6.5a (0.7) 22.4a (3.2)
5 cycles 9.8b (1.9) 31.6b (4.0)
10 cycles 10.4b (1.2) 30.4b (3.3)
15 cycles 10.4b (2.1) 30.3b (4.3)
Different letters (a, b) represent statistical difference in the same column (Tukey test, p-value < 0.05).
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Advances in Bamboo Science 2 (2023) 100014
values obtained through immersion of samples in water after 1, 12, 24,
98 and 268 h are shown in Table 2. All the values are expressed as
percentages.
With up to 98 h of immersion, untreated samples absorbed less
water than the others. However, after 268 h, the untreated samples
showed the greatest amount of water absorbed, although the difference
was not statistically significant. The greater amount of water absorbed
with up to 98 h immersion, mainly involving samples that had under-
gone 5 wet and dry cycles, may be explained by an increase in the
number of voids after removal of water-soluble extractives.
When comparing absorption values of untreated samples during the
first 24 h with values found in the literature, differences are apparent.
For instance, Gauss et al. (2021a, 2021b) reported water absorption
values of 41.2 % and 39.7 %, both for Dendrocalamus asper, respec-
tively, which can be explained by the natural variability of bamboo.
3.3. Dimensional analysis
The variation in the cross section of treated and untreated samples
that had been immersed in water was measured (Fig. 7). Samples from
10 and 15 cycles were not measured due to interference in the lighting
at the time of image acquisition, causing changes in area measure-
ments. Untreated samples had the highest variation over time, stabi-
lizing after 264 h (17.8 % increase in cross section area). Although
samples with 5 cycles had a similar behaviour to untreated samples
after 12 h, the same increase was not observed after 24 h. Specimens
treated with 10 and 15 wetting and drying cycles had the highest di-
mensional stability (8.2 % and 5.8 % after 264 h, respectively). Hence,
there is a gradual increase in the dimensional stability of bamboo
through the application of cycles.
The results of water absorption and cross-sectional variation in-
dicate that the removal of starch from the bamboo increased the
amount of space available for water to occupy, which led to the
maintenance of water absorption but a reduction in dimensional var-
iation.
*Different letters (a, b, c, d) represent statistical difference in the
same immersion time (Tukey test, p-value < 0.05).
3.4. Density measured with a helium pycnometer
The density of bamboo samples before and after hornification was
assessed. During the testing of the prismatic specimens, it became
evident that a longer time interval was needed to stabilize the helium
pressure inside the chamber in comparison to tests with the bamboo
particles. To address this issue, each prismatic specimen density mea-
surement was taken after three minutes. All results are shown in
Table 3.
The prismatic specimens that had received the same level of treat-
ment showed high variability in their density. This can be related to the
inherent variability of bamboo, despite the specimens being cut from
the same internode. This was also observed for untreated bamboo
particles, when comparing to value that has been reported in the lit-
erature for the same bamboo species (Gauss et al., 2021b).
24 h 98 h 268 h
33.3a (4.7) 42.6a (5.7) 59.7 a (10.4)
38.3b (4.1) 50.2b (4.9) 58.1a (6.6)
36.9a, b (3.9) 46.8a, b (6.0) 54.0 a (8.2)
36.8a, b (4.7) 46.0 a,b (5.9) 53.8a (7.7)
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali Advances in Bamboo Science 2 (2023) 100014

Fig. 7. Dimensional analysis before and after treatment.

When the mean densities for prismatic specimens were compared, a
significant increase in the real density after the application of 10 cycles
of wetting and drying was observed. This can be related to the closure
of pores and shrinkage of the vascular bundles after hornification.
This pattern of change was not observed in bamboo particles. There
was no significant difference in the densities of treated and untreated
particles. This is likely because after grinding the material, the density
is no longer influenced by the shrinkage of the vascular bundles.
3.5. Tensile test
The mechanical properties of bamboo after hornification were
evaluated using a tensile test, where the tension strength parallel to the
fibres and the modulus of elasticity where obtained (Table 4).
The tensile strength of the bamboo decreased by approximately
20 % of after the treatment. Chemical treatments with citric acid also
induced a reduction in tensile strength. In contrast, treatments with

Table 3
Density results for bamboo samples using a helium pycnometer.

Type Treatment Specimen Density (g.cm−3)

Mean (SD) Mean/Cycle (SD)

Prismatic Specimens Untreated CP-01 1.26a (0.019) 1.20 a (0.069)

CP-02 1.14b (0.024)
10 cycles CP-11 1.57 c (0.037) 1.51b (0.070)
CP-12 1.45d (0.035)
Bamboo Particles Untreated - 1.55c (0.013) -
10 cycles - 1.57 c (0.010) -
Gauss et al. (2021b) 1.303 -

Different letters (a, b, c, d) represent statistical difference in the same column (Tukey test, p-value < 0.05, for mean; and t-test, p-value < 0.05, for mean/cycle).

6
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali
Table 4
Bamboo mechanical properties obtained using a tensile test.
Specimens ft,0 (MPa) Et,0 (GPa)
No treatment 258.6a ( ± 19.6) 23.0a (±3.79)
5 Cycles 217.9b ( ±22.7) 23.7a (±6.52)
10 Cycles 215.6b (± 13.5) 23.6a ( ± 6.55)
15 Cycles 207.5b (± 22.4) 25.2a ( ± 4.81)
Different letters (a, b) represent statistical difference in the same column (Tukey test, p-value < 0.05). Standard deviation between parentheses. ft,0 is the tension
capacity; Et,0 is modulus of elasticity; M.C. is moisture content.
boron compounds had no effect on the tensile strength (Gauss et al.,
2021a). The reduction in tensile strength following hornification may
be related to differences in the swelling rate and drying stress caused to
fibres and parenchymatic cells, which can lead to a weaker interface
between these components (Yuan et al., 2021).
For vegetable fibres treated with wetting and drying cycles, tensile
strength either increased or remained stable for up to ten cycles
(Amaral et al., 2021). The difference between the vegetable fibres and
bamboo may be because there is no significant reduction in the bamboo
cross section after hornification. In contrast, for vegetable fibres, the
closure of the lumens for the first ten cycles causes a reduction in their
cross-sectional areas, increasing their tensile strength.
After treatment, greater means were obtained for the modulus of
elasticity, with the greatest (ca. 10 % higher) occurring after 15 wetting
and drying cycles. However, this increase was not statistically sig-
nificant.
Cid et al. (2020) calculated the modulus of elasticity of Phyllostachys
pubescens specimens through four-point flexural tests and found in-
creases of at least 40 % after 10 cycles, and higher values were obtained
Fig. 8. Failure patterns (a) no treatment (b) 5 cycles (c) 10 cycles (d) 15 cycles.
7
Advances in Bamboo Science 2 (2023) 100014
M.C. ( %) Apparent density (g.cm−3)
3.8 % 0.78 (±0.02)
3.7 % 0.70 (±0.03)
4.0 % 0.69 (±0.03)
4.8 % 0.72 (±0.04)
after 5 cycles. They suggested that, due to the short length of the spe-
cimens, deflections were influenced by the elasticity and shear mod-
ulus. Nonetheless, the values obtained were higher than we found. For
vegetable fibres, hornification did not have a clear influence on the
modulus of elasticity until after 10 cycles (Amaral et al., 2021). After 20
cycles, a decline in this property was observed.
Most of the samples presented the same failure pattern, breaking in
the middle portion, which indicates a rupture between the fibre bundles
and the lignin matrix. Although a few specimens presented failures near
to the grip portion, their tensile strengths were similar to the others
(Fig. 8).
3.6. Scanning electron microscopy (SEM)
Fig. 9 presents some electron microscopy images of bamboo samples
without treatment (control) and after 10 cycles. In both images (‘a′ and
‘b′), the fibres and parenchyma tissue can be identified. No difference
could be observed through SEM analysis in the longitudinal direction.
On other images with different amplifications and at different locations
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali Advances in Bamboo Science 2 (2023) 100014

Fig. 9. Scanning electron microscope (SEM) analysis on longitudinal direction (a) untreated (b) 10 cycles.

hornification. Although the index is an indirect way to assess the

maintenance or alteration of mechanical properties, in the present re-
search, its increase did not result in an increase in either the modulus of
elasticity or the tensile strength after the application of wetting and
drying cycles. The results for modulus of elasticity had an increase of
approximately 10 % but was not statistically significant. The tensile
strength decreased by about 20 % after treatment.
For isolated sisal fibres (Agave sisalana Perrine), the same tendency
has been reported for both the crystallinity index (Cr.I) and the tensile
strength (Ferreira et al., 2015; Ferreira et al., 2017). Ferreira et al.
(2015) found an increase on Cr.I and tensile strength after 10 cycles.
Another study found an increase in both properties after 5 wetting and
drying cycles, and a decrease after 10 cycles (Ferreira et al., 2017).
For curaua (Ananas comosus var. erectifolius (L.B.Sm.) Coppens &
F.Leal (syn. Ananas erectifolius)) and jute (Corchorus capsularis L.) fibres,
an increase in tensile strength and Cr.I was found up to 5 cycles.
However, after 10 cycles, the results the tensile strength had increased
whereas there was a reduction in the crystallinity index (Ferreira et al.,
2017).
The relationship between the modulus of elasticity and the crystal-
linity index after wetting and drying cycles is unclear. With sisal fibers,
Fig. 10. Micropores in parenchymatic cells.
a decrease in the modulus of elasticity and an increase in the crystal-
linity index occurred after 10 cycles (Ferreira et al., 2015). For curaua
Table 5 fibres, both the elasticity modulus and the Cr.I increased after 5 cycles.
Crystallinity index for bamboo without treatment and after hornifi- A reduction in the Cr.I after 10 cycles was not accompanied by a re-
cation. duction in tensile strength. For jute fibres, a decrease in the modulus of
elasticity was observed after 5 and 10 cycles. In contrast, the Cr.I in-
Treatment Crystallinity Index - Cr.I ( %)
creased after 5 cycles and decreased after 10 cycles (Ferreira et al.,
No treatment 30.90 % 2017).
15 cycles 46.30 % In a study carried out with different types of cellulose, derived from
Variation 49.80 %
ramie (Boehmeria nivea Gaudich.) fibre, in addition to parameters re-
lated to the crystallinity of the material, the density of the amorphous
region also influenced the modulus of elasticity (Ishikawa et al., 1997).
of the specimen, the same was evident. In the literature, small cracks on This suggests that an analysis extending beyond the calculation of the
refugo fibres after 10 cycles (Lima et al., 2014) and roughened surfaces crystallinity index should be made when attempting to determine the
on hardwood and softwood fibres (Ballesteros et al., 2017) have been relationships between results obtained from x-ray diffraction and the
reported, but these were absent our bamboo samples. Micropores mechanical properties.
within the parenchymatic cells were observed (Fig. 10). These micro-
pores contribute to the flow of nutrients in bamboo (Pandoli et al., 3.8. Fourier-transform infrared spectroscopy (FT-IR) analysis
2019).
FT-IR analysis was used to assess the functional groups of bamboo
3.7. X-ray diffraction (XRD) and to verify if the hornification treatment caused any modifications to
the chemical composition. Common characteristic peaks from wood
The crystallinity indexes obtained through Eq. 6 for samples without could be identified graphically with the bamboo, either without treat-
treatment and after fifteen cycles of wetting and drying are shown in ment or after fifteen cycles (Fig. 11) (Huang et al., 2012). In general,
Table 5. The crystallinity index increased by almost 50 % following modifications could not be observed through graphical analysis.

8
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali
Fig. 11. Fourier-transform infrared spectroscopy (FT-IR) analysis. [2 column fitting].
Table 6
Ratios between peaks of interest from Fourier-transform infrared spectroscopy (FT-IR) results.
Treatment Ratios between absorbance intensities from different functional groups
I1723/3345 I1723/2900
No treatment 0.28 0.54
15 Cycles 0.29 0.55
896 cm−1 peak - cellulose and hemicellulose; 1317 cm−1 peak - high crystallinity cellulose; 1369 cm−1 peak - lignin; 1723 cm−1 peak - hemicellulose; 2900 cm−1
peak - hydrocarbon chains; 3400 cm−1 peak - hydroxyl groups. Source: (Huang et al., 2012).
To confirm this, the ratios between peaks of interest were calculated
(Table 6). The selected peaks were related to bamboo components
(cellulose, hemicellulose, lignin, hydroxyl group) and water absorption
capacity. The ratios between the peaks presented small or no variation,
indicating that there was no structural modification of these compo-
nents during the hornification treatment. For instance, Gauss et al.
(2021a) found an increase on the 1723 cm−1 peak, which is related to
the hydroxyl groups in bamboo, after a chemical treatment with citric
acid, which suggests a reduction in water absorption capacity.
For vegetable fibres, an increase in the hydrogen bonds was seen
after hornification, with an increase in the intensity of the 3400 cm−1
peak, and with curaua and jute fibres after 10 cycles (Ferreira et al.,
2015; Ferreira et al., 2017). However, for sisal residues, softwood and
hardwood pulps, there were no differences in the peaks related to the
absorption capacity of the fibres (Lima et al., 2014; Ballesteros et al.,
2017). This implies that either the changes in the chemical components
brought about by hornification are not consistent or they are too small
to be identified through only the FT-IR analysis.
The lack of influence of hornification on bamboo chemical com-
pounds may also be related to the maintenance of the water absorption
capacity in the samples after 10 cycles. We hypothesize that the physical
effects of the treatment, such as pore reduction and closure, and removal
of carbohydrates, are the main factors responsible for the variation in
water absorption capacity over the first 10 wet-and-dry cycles.
4. Conclusions
The effects of hornification, involving up to 15 cycles of wetting and
drying, were assessed on the physical, mechanical, and chemical
properties of Dendrocalamus asper. Water absorption uptake was not
reduced by the treatment, but an increase in dimensional stability was
seen. The maintenance of water absorption is attributed to pore size
reduction and closure up to the 10th cycle, which is a pronounced effect
9
Advances in Bamboo Science 2 (2023) 100014
I1723/1317 I1369/1317 I896/1317
0.72 1.02 0.88
0.76 1.00 0.90
on isolated vegetal fibres. This was compensated by a removal of
bamboo starch content during the first cycles.
Regarding the mechanical parameters, a reduction of 20 % of tensile
strength after treatment was identified. The observed effect contrasted
with the results for isolated vegetable fibers, in which the reduction in
the cross section was more pronounced. An increase in the modulus of
elasticity that has been reported in the literature for Phyllostachys
pubescens was not confirmed in our research. As a result, the expected
stiffening of the material did not occur.
The density results for prismatic samples indicated an increase in
density after 10 cycles of wetting and drying. Although the removal of
carbohydrates during the first five cycles increases the number of voids
in the vascular bundles, the gradual closure of pores that occurs up to
the 10th cycle is significant. For bamboo particles, treatment did not
result in a change in density.
As a suggestion for future research, the verification of the hypothesis
that water-soluble extractives are removed and the voids in the vascular
bundles increase during the first five cycles would open the possibility
to utilize the hornification effect as a pretreatment to increase the up-
take of treatment solutions. This could be combined with vacuum/
pressure treatments. However, it will be necessary to consider the ef-
fects of hornification on the mechanical properties of the bamboo.
Data Availability
Data will be made available on request.
Declaration of Competing Interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
L.M. do Amaral, C.d.S. Rodrigues and F.S.J. Poggiali Advances in Bamboo Science 2 (2023) 100014

Acknowledgments
The authors acknowledge the funding provided by the Federal
Centre for Technological Education of Minas Gerais (CEFET-MG),
Fundação de Amparo à Pesquisa do Estado de Minas Gerais (FAPEMIG)
and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior –
Brazil (CAPES) – Finance code 001 –, which supported the first author’s
work at CEFET-MG. Prof. Augusto C.S. Bezerra, doctoral students Laísa
R.S. Carneiro and Vitor A. Nunes, laboratory technicians Ivan Batista
Morais and Késsia Drumond (CEFET-MG) are also acknowledged for the
support they provided with the laboratory tests.

Appendix

Table A.1 presents all the statistical comparisons between each mean moisture content value obtained after each immersion cycle. Table A.2
shows the statistical comparisons of absorption variation, in which the influence of the moisture content after drying cycle is minimized.

Table A.1
Complete statistical analysis for moisture content measurements.

Moisture Content (%) Cycle Statistical comparison

Mean (SD) 1 2 3 4 5 6 7 8 9 10 11 12 13 14

55.7 (7.1) 1 - - - - - - - - - - - - - -
49.2 (5.3) 2 yes - - - - - - - - - - - - -
50.2 (4.6) 3 yes no - - - - - - - - - - - -
50.5 (5.1) 4 yes no no - - - - - - - - - - -
51.8 (5.1) 5 yes yes yes yes - - - - - - - - - -
51.5 (5.0) 6 yes yes yes yes no - - - - - - - - -
50.8 (5.0) 7 yes no no no yes yes - - - - - - - -
50.1 (4.8) 8 yes no no no yes yes yes - - - - - - -
50.4 (4.9) 9 yes no no no yes yes no no - - - - - -
50.1 (4.7) 10 yes no no no yes yes yes no no - - - - -
49.5 (4.7) 11 yes no no yes yes yes yes yes yes yes - - - -
49.8 (4.7) 12 yes no no no yes yes yes no yes no no - - -
50.2 (5.0) 13 yes no no no yes yes no no no no yes no - -
51.4 (4.4) 14 yes yes yes no no no no yes yes yes yes yes yes -
49.7 (4.3) 15 yes no no no yes yes yes no yes no no no no yes

Yes is statistical difference (repeated measures ANOVA and Bonferroni post hoc test, p-value < 0.05).

Table A.2
Complete statistical analysis for absorption variation measurements.

Absorption Variation (%) Cycle Statistical comparison

Mean (SD) 1 2 3 4 5 6 7 8 9 10 11 12 13 14

39.7 (6.7) 1 - - - - - - - - - - - - - -
44.7 (5.2) 2 yes - - - - - - - - - - - - -
45.8 (4.7) 3 yes no - - - - - - - - - - - -
46.8 (5.2) 4 yes yes yes - - - - - - - - - - -
49.0 (5.2) 5 yes yes yes no - - - - - - - - - -
49.6 (5.0) 6 yes yes yes no yes - - - - - - - - -
48.9 (4.9) 7 yes yes yes no no yes - - - - - - - -
47.7 (4.8) 8 yes yes yes no yes yes yes - - - - - - -
46.3 (5.0) 9 yes no no yes yes yes yes yes - - - - - -
46.7 (4.8) 10 yes yes no yes yes yes yes yes no - - - - -
46.9 (4.6) 11 yes yes no yes yes yes yes yes yes no - - - -
47.2 (4.7) 12 yes yes yes yes yes yes yes yes yes no no - - -
47.0 (4.9) 13 yes yes yes yes yes yes yes yes yes no no no - -
48.6 (4.4) 14 yes yes yes no no yes no yes yes yes yes yes yes -
46.7 (4.4) 15 yes yes no yes yes yes yes yes no no no no no yes

Yes is statistical difference (repeated measures ANOVA and Bonferroni post hoc test, p-value < 0.05).

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