Eur. J. Wood Prod.
(2018) 76:1021–1027
DOI 10.1007/s00107-017-1244-1
ORIGINAL
Isolation of cellulose nanocrystals from Gigantochloa scortechinii
ASAM pulp
Amin Moradbak1   · Paridah Md. Tahir1,2 · Ainun Zuriyati Mohamed1 ·
Mahnaz M. Abdi1,3 · Rawaida Liyana Razalli1 · Rasmina Halis1,2 
Received: 19 November 2016 / Published online: 23 October 2017
© Springer-Verlag GmbH Germany 2017
Abstract  This study aims to characterize the cellulose
nanocrystals (CNC) isolated from alkaline sulfite anthraqui-
none and methanol (ASAM) bamboo (Gigantochloa scorte‑
chinii) pulp. The hydrolysis was carried out using 64% (w/w)
sulfuric acid at 45 °C for 45 min. The CNC was subjected
to field emission scanning electronic microscopy (FESEM),
X-ray powder diffraction (XRD), Fourier transform infrared
spectroscopy (FTIR), and transmission electron microscopy
(TEM). The measurement of diameter for CNC was done
by FESEM and TEM, which was in the range of 10–20 nm.
The XRD and FTIR results exhibited that bamboo CNC has
higher crystallinity index, 78% compared to bleached ASAM
bamboo pulp, 60%.
1 Introduction
Cellulose is the most abundant polysaccharide, which consti-
tutes approximately one-third of annual plants and one-half
of perennial plants. It is a high molecular weight, stereo-
regular, and linear polymer of repeating β-D-glucopyranose
units. These units allow the chains of cellulose to remain in
* Amin Moradbak
aminmoradbak@gmail.com
* Ainun Zuriyati Mohamed
ainun.introp@gmail.com
1
Institute of Tropical Forestry and Forest Products (INTROP),
Universiti Putra Malaysia, UPM, 43400 Serdang, Selangor,
Malaysia
2 regions, and the product has a higher degree of crystallinity
Department of Forest Production, Faculty of Forestry,
Universiti Putra Malaysia, 43400 Serdang, Selangor,
Malaysia
3
Department of Chemistry, Faculty of Science, Universiti
Putra Malaysia, 43400 Serdang, Selangor, Malaysia
more or less extended form (Börjesson and Westman 2015;
Klemm et al. 2005; Missoum et al. 2013; Spence et al. 2010;
Zhang et al. 2012).
Cellulose molecules are completely linear and have a
strong tendency to form intra and intermolecular hydrogen
bonds. Bundles of cellulose molecules are thus aggregated
together in the form of microfibrils, in which highly struc-
tured (crystalline) regions alternate with less ordered (amor-
phous) regions. As a consequence of its fibrous structure and
strong hydrogen bonds, cellulose has a high tensile strength
and is insoluble in most solvents (Feldman 1985; Li 2004).
The unit cell of native cellulose (cellulose I) consists of
four d-glucose residues (Fig. 1) (Kontturi et al. 2006). In the
chain direction, the repeating unit is a cellobiose residue,
and each glucose residue is accordingly displaced 180° with
respect to its neighbours, giving cellulose a twofold screw
axis. It has now been established and largely accepted that
all chains in native cellulose microfibrils are oriented in the
same direction (Wada et al. 2008).
Molecules in crystalline regions are held by hydrogen
bonding, which makes the penetration of either solvent
or reagent molecules difficult. In contrast, the amorphous
regions are random, less dense, and much more suscepti-
ble to acid and enzyme hydrolysis than crystalline regions.
Hence, solvent and reagent molecules can penetrate the ran-
dom network and react more rapidly with the molecules (Xu
et al. 2013b).
When the cellulose is hydrolyzed with mineral acids,
which are not sufficiently concentrated to cause complete
solution, the attack occurs primarily in the amorphous
than the original cellulose (Beck-Candanedo et al. 2005).
Cellulose nanocrystals (CNC) in comparison with cel-
lulose have many advantages such as high specific strength,
high surface area, and high aspect ratio. CNC has a lot of
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Vol.:(0123456789)

1022
Fig. 1  Axial projections of the
structures of cellulose I and
regenerated cellulose II
hydroxyl groups (OH) on the surface. Effects of these groups
are amplified by the tiny size of the particles and their con-
sequently high surface area per unit mass. Thus, CNC can
be used in the microparticles retention system as organic
particles (Besbes et al. 2011; Eriksen et al. 2008; Missoum
et al. 2013; Xu et al. 2013b).
In recent decades, the isolation of CNC from natural and
renewable sources such as kenaf, cotton, pomelo, aspen,
and bamboo has increased. The origin of the cellulose raw
material and isolation process are the two main factors that
have effects on structure and geometric properties of CNC.
Differences in isolation process may affect the final CNC
properties (Ahola et al. 2008; Siqueira et al. 2009, 2010;
Tonoli et al. 2012).
The acid hydrolysis of polysaccharides attacks the
hemiacetal linkage by hydronium ion ­(H3O+). The rate of
hydrolysis in aqueous solution depends on the concentra-
tion of acid, temperature, nature of sugar unit, and mode of
linkage (Morelli et al. 2012; Rosli et al. 2013; Tonoli et al.
2012). The hydrolysis usually follows the kinetics of first
order reactions. The monosaccharides by hydrolysis are not
immune to further attack by acids and are partially converted
to furan-type compounds and other degradation products
(Zhou et al. 2012).
Hydrolysis of cellulose leads to a decrease in chain length
of polymer, then forming oligosaccharides and D-glucose
units. In initial stages of hydrolysis, the cellulose maintains
its original fibrous form and the progress of the hydrolysis is
evidenced by a decrease in physical strength of the fibers, a
decrease in viscosity [or Degree of Polymerization (DP)], an
increase in the content of reducing groups, and increments
solubility of aqueous alkaline solutions (Jonoobi et al. 2010;
Li et al. 2012; Morán et al. 2008).
A dependency of the length of crystallites on the angle
of the fibrils was deduced by Peter et al. (2003). According
to their findings, the average crystalline length becomes
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Eur. J. Wood Prod. (2018) 76:1021–1027
smaller with the increase in the angle of the fibrils. As the
acid hydrolysis proceeds, the DPs are expected to decrease
since the non-crystalline regions in the microfibril will be
removed. Due to the loss of non-crystalline regions, the
crystallinity will increase and also the insolubility against
water because the crystalline parts are less accessible
(Börjesson and Westman 2015).
The crystal structure of cellulose fibers is one of the
fundamental characteristics of fibers. X-ray diffraction
(XRD) has usually been applied to study the crystallinity
of fibers particularly. For example, cellulose I contains
fiber structure of highly structured crystalline domains
interposed among amorphous region (Ma et  al. 2015;
Monshi et al. 2012; Zhang et al. 2012).
This paper attempts to show the isolation of CNC from
ASAM pulping process of bamboo culms. The cellulose
fiber of ASAM bamboo pulp was transformed into CNC
for its future use as an organic particle for micro particles
retention system. Therefore, the characteristics of CNC
were obtained by XRD, FTIR, FESEM, and TEM.
2 Experimental
2.1 Materials
The ASAM pulping process was conducted in a 5-L
digester, which was heated electrically with liquor circu-
lation. The parameters selected included an 80/20 ratio of
­Na2SO3/NaOH, 15% methanol, 9/1 liquor-to-wood (L/W),
alkali charge 16%, 90 min cooking time, and 170 °C cook-
ing temperature. The pulp yield is 49.1% and the Kappa
number of unbleached bamboo ASAM pulp is 14.2
(Moradbak et al. 2016).
Eur. J. Wood Prod. (2018) 76:1021–1027 1023

2.2 Methodology empirical method (Segal et al. 1959), the crystallinity index

(CIr) of CNC ASAM bamboo pulp was measured.
2.2.1 Bleaching process {( ) }
CIr = I200 − Iam ∕ I200 × 100
The unbleached bamboo ASAM pulp was bleached by ele- I200 = the intensity value of crystalline cellulose (2𝜃 = 22.5◦ )
mental chlorine free (ECF) sequences, named D­ 1EpD2ED3P. Iam = the intensity value of amorphous cellulose (2𝜃 = 18◦ )
Table 1 shows the ECF bleaching conditions of ASAM bam-
boo pulp. 2.2.5 Morphological observation

2.2.2 Cellulose nanocrystals (CNC) production
The cellulose nanocrystals (CNC) of bleached bamboo
ASAM pulp were prepared using sulfuric acid hydrolysis.
The bleached pulp was hydrolyzed by sulfuric acid, 64% at
45 °C for 45 min with dynamic stirring, 400 rpm (IKA, RW
20, Digital, Malaysia). The ratio of acid-to-cellulose was
8.25:1. After acid hydrolysis had been accomplished, the
suspension was placed in an ice bath to stop the hydroly-
sis reaction. The acid-treated sample was washed with 5%
sodium bicarbonate and distillated water to pH of about
6. The suspension was washed six times by centrifuge at
6000 rpm for 30 min to remove the sulfur of sulfuric acid. To
obtain the CNC in powder form, the suspension was dried in
a vacuum freeze dryer.
2.2.3 Fourier transform infrared (FTIR) spectroscopy
Infrared spectra of bamboo meal, unbleached and bleached
ASAM pulp, and CNC were recorded by using a Spectrum
100, Perkin Elmer. The wavenumber of FTIR was within
the range 4000–280 cm−1 with 16 scans for each case at a
resolution of 4 cm−1.
2.2.4 X‑ray diffraction (XRD)
The X-ray diffraction analyses of CNC and bleached bam-
boo ASAM pulp were carried out using Philips PW 3040/60
X/pert Pro with wavelength 1.5405980. The scanning step
was done within the range 2θ = 10–30. According to Segal’s
The morphological observation of CNC was carried out
using Field Emission Scanning Electronic Microscopy
(FESEM) and Transmission Electron Microscope (TEM).
Using JEOL JSM-7600F at a voltage of 5 kV (FESEM) and
PHILIPS EM-208 at a voltage of 100 kV (TEM), the micro-
graphs of CNC of bamboo ASAM pulp were recorded.
3 Results and discussion
3.1 FESEM
The FESEM micrographs of CNC from bleached bamboo
ASAM pulp are shown in Fig. 2. The CNC produced by acid
hydrolysis was narrow and sharper. This may occur due to
the effect of acid on the fiber surface (Zhang et al. 2012).
3.2 TEM
The TEM micrographs of the diameter and the aspect ratio
of CNC are shown in Fig. 3. As can be seen in Fig. 3, the
needle-like structure of CNC from acid hydrolysis treat-
ment can be observed. The diameter and length of CNC
were within the range 5–20 and 170–500 nm, respectively.
The aspect ratio (L/d) of CNC was within the range 14–49.
This indicates that CNC from bleached ASAM bamboo pulp
can be used as a reinforcement agent in the manufacture of
nanocomposites (Razalli et al. 2017).
The dimension and morphology of CNC from bleached
ASAM bamboo pulp by acid hydrolysis are similar to CNC

Table 1  ECF bleaching Bleaching Chemical % Consist- Time (min) Temp (°C)

conditions of ASAM bamboo sequences ency (%)
pulp NaClO2 CH3COOH NaOH H2O2 Na2SiO3

D1 2 3 10 60 70
Ep 1.5 1 3 8.5 60
D2 1.25 3 0.1 120
E 0.7 90
D3 0.95 3 0.5 120
P 0.25 4 3 60

NaClO2 sodium chlorite, CH3COOH acetic acid, NaOH sodium hydroxide, H2O2 hydrogen peroxide,
Na2SiO3 sodium silicate, Temp temperature

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1024 Eur. J. Wood Prod. (2018) 76:1021–1027

Fig. 2  FESEM micrographs of CNC. a Magnification 50,000, 100 nm. b Magnification 25,000, 1 μm

Fig.  3  a TEM micrograph

of CNC. b and c Diameter
and aspect ratio of CNC from
bleached ASAM bamboo pulp

from other cellulosic materials. According to Zhang et al. The diameter, crystallinity index, and length of CNC from
(2012), the crystallinity index, diameter, and aspect ratio Eucalyptus kraft pulp using sulfuric acid 60 wt% at 45 °C for
of CNC from Moso bamboo by acid hydrolysis (60 wt% at 30 min were 10–50 nm, 76%, and 50–500 nm, respectively
45 °C for 60 min) were 78.8%, 14 nm, and 15, respectively. (Tonoli et al. 2012).

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Eur. J. Wood Prod. (2018) 76:1021–1027 1025
3.3 FTIR spectroscopy
During the ASAM cooking and bleaching, lignin and hemi-
cellulose are usually removed. In addition, during acid
hydrolysis, the amorphous part of cellulose was removed.
The crystalline parts of cellulose have a high resistance to
acid hydrolysis (Elazzouzi-Hafraoui et al. 2008; Ioelovich
2012; Khristova et al. 2002; Jahan et al. 2007; Vanhatalo and
Dahl 2014). The FTIR analysis of bamboo meal, unbleached
and bleached ASAM pulp and CNC are displayed in Fig. 4.
As noted by Rosli et al. (2013), the peaks at 1735 and
1247 cm−1 belonged to C=O and C–O of the acetyl, uronic
ester groups, and the aryl group in the hemicellulose and
lignin, respectively. During the bulk de-lignification phase
(pulping process), carbohydrates are very stable. In the final
cooking phase, enhancement of carbohydrate degradation
occurred when about 90% of the lignin had dissolved (Kord-
sachia et al. 1988; Zimmermann et al. 1992). According to
Patt et al. (1991) up to 80% of the pine glucomannan is dis-
solved in an ASAM cook, whereas the xylan is much more
stable. Cellulose is very stable in the ASAM system, with
only a small amount occurring in the final de-lignification
phase (total loss about 2% o.d. wood). These two peaks
had completely disappeared during pulping and bleaching
processes.
The peaks 3400–3300 cm−1 belonged to free O–H stretch-
ing of the hydroxyl group in the cellulose molecules. In
addition, the peak at 2900 cm−1 belongs to C–H stretching
(Cao and Tan 2004; Ivanova et al. 1989; Wang et al. 2007).
The peaks of the C–O and C–H bond in polysaccharide aro-
matic ring (cellulose and hemicellulose) were detected at
1360 cm−1 (Nacos et al. 2006).
The C–O–C bond of pyranose ring skeletal can be
observed at 1057  cm −1 increasing the intensity of this
bond due to increases in crystallinity of the samples
(Elanthikkal et al. 2010). The most significant absorption
Fig. 4  FTIR spectra of a bam-
boo meal, b unbleached pulp, c
bleached pulp, and d CNC
bond 896 cm −1 has been related to C-H bond of glyco-
sidic deformation and O-H bending. As noted by Alemdar
and Sain (2008), these properties are characteristic of the
β-glycosidic linkage between the anhydroglucose units in
cellulose. Table 2 shows the representative bands of lignin,
cellulose, and hemicellulose.
3.4 X‑ray diffraction analyses
The X-ray diffraction of CNC and bleached ASAM bam-
boo pulp are illustrated in Fig. 5. The intensity values of
amorphous and crystalline cellulose were shown around
2θ = 18 and 22.5, respectively (Li et al. 2011; Nishiyama
et al. 2002, 2003). The crystallinity of bleached bamboo
ASAM pulp was 60%. After acid hydrolysis had accom-
plished, the crystallinity increased to 78% of CNC.
The crystallinity of CNC was 78%, which was higher
than the bleached bamboo ASAM pulp, 60%. During the
bleaching, the structure of fiber is loosened, and swelling
of fiber is increased. In addition, the chemical composi-
tions of fiber such as hemicellulose, lignin, and pectin
were removed and caused an increment of the crystallin-
ity content of bleached fiber. Hydrogen peroxide affected
both crystalline and amorphous parts and more polysac-
charides aromatic rings and bending stretching vibration
were present on the fiber structure (Ioelovich 2012; Morán
et al. 2008; Rosli et al. 2013; Xing et al. 2010).
On the other hand, the addition of acid concentration to
bleached bamboo ASAM pulp increased the crystallinity
by up to 30%. This is due to the amorphous part of cellu-
lose, which was removed while the intensity of crystalline
part of cellulose was increased. Therefore, in Fig. 5 the
crystallinity of CNC from bleached ASAM bamboo pulp,
which was treated by sulfuric acid 64% (w/w) at 45 °C for
45 min, was obtained.
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1026 Eur. J. Wood Prod. (2018) 76:1021–1027

Table 2  Representative bands Chemical materials Wavenumber ­(cm−1) Functional groups Compounds

of cellulose, hemicellulose, and
lignin Lignin 4000–2995 OH Acid, alcohols
2890 H–C–H Alkyl, aliphatic
1730–1700 Aromatic
1632 C=C Benzene stretching ring
1613–1450 C=C Aromatic skeletal mode
1430 O–Ch3 Methoxyl–O–CH3
1270–1273 C–O–C Aryl–alkyl ether
1215 C–O Phenol
1108 OH C–OH
700–900 C–H Aromatic hydrogen
Cellulose 4000–2995 OH Acid, methanol
2890 H–C–H Alkyl, aliphatic
1640 Fiber–OH Adsorbed water
1170–1082 C–O–C Pyranose ring skeletal
1108 OH C–OH
896 C–H C–H deformation in cellulose
Hemicellulose 4000–2995 OH Acid, methanol
2890 H–C–H Alkyl, aliphatic
1765–1715 C=O Ketone and carbonyl
1270–1232 C–O–C Aryl–alkyl ether
1108 OH C–OH

Source: Morán et al. (2008) and Xu et al. (2013a)

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Fig. 5  XRD for a bleached bamboo ASAM pulp and b CNC
4 Conclusion
The results showed that the quality of CNC produced by
hydrolyzing bleached bamboo ASAM pulp is acceptable.
The diameter of CNC was obtained within the range of
10–20 nm. The crystallinity index of CNC was 78%, which
was higher than that of the bleached bamboo ASAM pulp
(60%).
Acknowledgements  The authors are grateful for the support of
the Institute of Tropical Forestry and Forest Products (INTROP) and
Research Management Center (RMC)—Universiti Putra Malaysia
(UPM), Grant no. PB 9413400.
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