Cellulose (2016) 23:1803–1812
DOI 10.1007/s10570-016-0904-3
ORIGINAL PAPER
Sago seed shell: determination of the composition
and isolation of microcrystalline cellulose (MCC)
Subair Naduparambath . E. Purushothaman
Received: 12 November 2015 / Accepted: 4 March 2016 / Published online: 23 March 2016
Ó Springer Science+Business Media Dordrecht 2016
Abstract Sago seed shells are agricultural wastes
that are discarded after taking the pith. The compo-
sition of sago seed shells has been determined by using
standard methods. Parameters such as extractives
(ASTM D1107-96), Klason lignin (ASTM D1106-
96), holocellulose (Wise et al. in Paper Trade J
122(2):35–42, 1946), a-cellulose (ASTM D 1103-60),
hemicellulose (by difference) and ash content (T 211
om 02) were determined. The components were
characterised using FTIR, TGA, XRD, SEM, TEM
and AFM. The detailed spectral, thermal, XRD and
SEM analyses show the presence Klason lignin,
holocellulose and a-cellulose. a-Cellulose has been
converted into microcrystalline cellulose (MCC) by
acid hydrolysis. MCC was also characterised by using
FTIR, TGA, XRD, SEM, TEM and AFM. Frequencies
of the FTIR spectrum are similar to those of a-
cellulose, and the TGA data reveal increased decom-
position temperatures for MCC and well as a well
defined TGA curve, indicating the increased structural
order or crystallinity. This is further supported by
XRD. SEM, TEM and AFM results, which reveal the
microstructural behavior of isolated MCC.
S. Naduparambath
E. Purushothaman (&)
Department of Chemistry, University of Calicut,
Malappuram, Kerala 673635, India
e-mail: purushotche@gmail.com
S. Naduparambath
e-mail: subairnp@gmail.com
Keywords Sago seed shells
Klason lignin

Holocellulose
a-Cellulose
MCC
Introduction
Cellulose is a versatile biopolymer, which is
biodegradable and renewable and is used in a wide
variety of industries (Klemm et al. 2005). It is a
linear polymer consisting of b (1 ? 4) glucopyra-
nose units. During biosynthesis, they are self-
assembled into microfibrils and are then packed into
macrofibrils containing amorphous and crystalline
regions (Nishiyama 2009). Cellulose is characterised
by hydrophilicity, low density and reinforcing abil-
ity, being amenable for modification. In addition, it
has environmental advantages and has attracted
many scientists to work on developing cellulose-
based composites (Eichhorn et al. 2010). Cellulose
can be hydrolysed using mineral acids so that the
amorphous regions are removed. Based on the extent
of removal of amorphous regions and on the
dimensions, microcrystalline and nanocelluloses can
be produced. Even though wood and cotton are the
principal sources for the commercial production of
MCC, other sources such as wheat and rice straw
(Jain et al. 1983), water hyacinth (Gaonkar and
Kulkarni 1987), sugar cane bagasse (Paralikar and
Bhatawdekar 1988), coconut shells (Gaonkar and
Kulkarni 1989), soybean husks (Nelson et al. 2000),
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flax fibres and flax straw (Bochek et al. 2003) and
jute (Sarwar Jahan et al. 2011) have been studied.
Microcrystalline cellulose is a white, odourless, fine
crystalline powder, used in a wide variety of
industries such as cosmetics, food and pharmaceu-
ticals as a suspension stabilisers, water retainers and
reinforcements in tablets, etc. Based on the origin,
the properties such as the crystallinity, moisture
content, surface area, porous structure, particle size
and molecular weight of MCC were found to vary
(El-Sakhawy and Hassan 2007). MCC can be added
as a reinforcing filler in the polymer matrix to give
biocomposites. In addition, it is one of the precursors
for obtaining nanocellulose.
Research on biocomposites has gained much
momentum in recent years because of environmental
concerns. The reinforcement can be natural fibres such
as sisal (Varghese et al. 1994), coconut (coir)
(Geethamma et al. 1995), bamboo (Mi et al. 1997),
wood (Coutinho et al. 1997), henequen (Herrera-
Franco and Valadez-González 2005), jute (John and
Thomas 2008) and palm (Haque et al. 2009). Several
fruit or seed shells have also been used to produce
biocomposites such as rice hulls (Yang et al. 2004),
ground nut shells (Raju and Kumarappa 2011), rattan
powder (Ismail et al. 2012) and coconut shell powder
(Sareena et al. 2012). Biocomposites find application
in areas such as the medical, cosmetic, electrical,
electronic, paper and packaging industries. Consider-
able progress has also been made in the development of
nanocomposites, which are designed to display the best
combination of the characteristics of the nano-dimen-
sional properties of constituents to give better proper-
ties, which are not exhibited by macrocomposites.
Sago (Cycas circinalis) is known to be an Indian
endemic, restricted to the Western Ghats, in the
states of Kerala, Karnataka, Tamil Nadu and the
south of Maharashtra. Research attention has been
mainly focussed on the edible part of the seed and
no systematic investigation has been carried out on
the shells of sago seeds. Therefore, the main
objective of this work is to determine the compo-
sition of sago seed shells, which are usually
discarded as agricultural waste after taking the pith,
and to isolate very useful MCC from this. Seed
shells are usually composed of lignin, hemicellulose,
cellulose, extractives and other minor components.
The analysis is carried out to determine the above
components.
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Cellulose (2016) 23:1803–1812
Experimental
Materials
The sago seed shells were collected locally and dried
in air for 2–3 days. The air-dried sago seed shells were
powdered and sieved through a 53-lm mesh.
Methods
Determination of the composition of sago seed shells
Since no literature is available on the composition of
sago seed shells, the first aim was to determine their
chemical composition. The powdered and meshed
sample was oven dried in a hot air oven maintained at
100–105 °C for 3–4 h till a constant weight was
obtained. The following analysis was carried out on an
oven dry sample. Extractives (ASTM D1107-96),
Klason lignin (ASTM D1106-96), holocellulose (Wise
et al. 1946), a-cellulose (ASTM D 1103-60), hemi-
cellulose (by difference) and ash content (T 211 om
02) were analysed.
Bleaching
The oven-dry sample was extracted in a Soxhlet
apparatus with and ethanol-toluene mixture (2:1) for
5 h. The extracted residue was oven dried at
100–105 °C for 3–4 h till a constant weight was
obtained (ASTM D1107-96). The residue (1 g) was
treated with 0.7 % NaClO2 (20 ml) in a water bath
kept at 80 °C, maintaining the pH at 5 by stirring with
acetic acid, for 5 h. The residue was filtered, washed
several times with distilled water till the washings
became neutral, and finally oven dried at 100–105 °C
for 3–4 h till a constant weight was obtained (Wise
et al. 1946). This process was carried out in order to
delignify the material and to obtain holocellulose.
Isolation of microcrystalline cellulose (MCC)
Preparation of MCC was carried out by using the
method adopted by Ohwoavworhua et al. (2004) with
a slight modification. In a typical procedure holocel-
lulose, obtained after bleaching from an oven dry
sample (2 g), was treated with 17.5 % NaOH (25 ml),
making three additions for about 45 min. The solution
was kept for 1 h and a sufficient quantity of distilled
Cellulose (2016) 23:1803–1812 1805

water was added to make the concentration of NaOH
8.3 %. The solution was filtered and washed with
distilled water and with 10 % acetic acid. The residue
was again washed several times with distilled water till
the washings were neutral and oven dried by main-
taining the temperature at 100–105 °C for 3–4 h till a
constant weight was obtained (ASTM D 1103-60).
The a-cellulose (1 g) obtained was hydrolysed with
2.5 N HCl (17 ml) into a glass vessel at boiling
temperature for 15 min. The hot acid mixture was
poured into 50 ml cold water followed by vigorous
stirring and allowed to stand overnight. The MCC
obtained was filtered, washed with distilled water till it
became neutral and dried in a hot air oven at 60 °C for
half an hour (Achor et al. 2014). The complete process
is schematically represented as shown below.
with CuK? (k = 1.54 Å). The samples were scanned
at the 2h range of 10°–50°, and a step size of 0.02° was
used for the analysis. Degree of crystallinity (DC) was
calculated by using the equation DC = (I200 - Iam)/
I200, where I200 is the intensity of the 200 peak at
2h = 22.8° and the Iam is the minimum intensity at the
amorphous region of 2h = 18° (Segal et al. 1959).
The morphology at the different stages of the
process was studied using SEM, TEM and AFM. The
surface morphology was studied using JEOL Model
JSM-6390LV SEM, with magnification of X100. The
SEM micrograph was taken at a voltage of 20 kV.
Transmission electron microscope (TEM) observa-
tions were performed using JEOL model JEM 2100. A
very diluted MCC aqueous suspension was ultrason-
icated in a water bath sonicator, and then a drop of the

Oven dried sago seed shells

Extracted with ethanol, toluene mixture (2:1) for five hours

Bleached with 0.7% NaClO2 -holocellulose

Treated with 17.5% NaOH -α -Cellulose

Hydrolysed with 2.5N HCl -Microcrystalline cellulose

Characterisation solution was deposited on a carbon-coated copper

The different isolated components and MCC were
characterised using various spectral and analytical
techniques.
FTIR spectra were recorded in the range of
4000–400 cm-1 with a JASCO FTIR-4100 spectrom-
eter using a KBr pellet. Thermogravimetric analysis
was carried out using a TA Q50 instrument. The
decomposition was studied from room temperature to
750 °C with a heating rate of 10° per minute under
nitrogen atmosphere to determine the thermal stability
and decomposition temperature of the different com-
ponents extracted.
The X-ray diffraction of the materials was carried
out using the RIGAKU MINIFLEX-600 diffractometer
grid, which was dried and used for imaging. Atomic
force microscopy was taken on a WI Tec Alpha
300RA (Germany) in non-contact mode. Drops of
dilute aqueous suspensions of MCC were deposited on
glass and left to dry at room temperature prior to
analysis.
Results and discussion
Weight percentages of different components isolated
from sago seed shells were determined and are listed in
Table 1.
The analysis shows that it has reasonably good
lignin contents and high cellulose levels compared to

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Table 1 Weight % (w/w) of different components isolated from sago seed shells
Name Extractives Klason lignin Holo cellulose a-Cellulose Hemicellulose Ash content

Weight % 8.2 ± 1 23.6 ± 0.8 59.0 ± 1.2 36.5 ± 1 22.5 ± 1 9.2 ± 0.2

Table 2 Cellulose content Agricultural Lignin Holocellulose Hemicellulose Cellulose Others

and % composition in (w/w)
Bagasse 20 67 23 44 13
Corn cob 12.8 76.6 42.5 34.1 10.6
Peanut shell 35.2 34.2 12.1 22.1 30.6
Rice hull 12.9 58.7 9.6 49.1 28.4
Rice straw 7 59 26 33 34
Sugar cane leaf and stalk 13 69 29 40 18
Sorghum leaf and stalk 11 61 30 31 28
Sago seed shells 23.6 59 22.5 36.5 17.4

corn cob, peanut shell, rice straw and sorghum leaf and
stalk. (Table 2; Atcha Boonmee 2012). Therefore,
sago seed shells can be used as a potential source for
the extraction of cellulose; moreover, the seed shell
powder can be effectively utilised as a filler for the
preparation of composites.
FTIR analysis
Figure 1a shows the FTIR spectrum of lignin, other-
wise called Klason lignin, which is composed of
phenyl propane derivatives and has a complex three-
dimensional structure. It is found together with
polysaccharide in the biomass. It has a perfect
amorphous structure and acts as glue between cellu-
lose fibres by virtue of the interaction or linkage
between the cellulose and matrix. The spectrum
obtained shows typical phenyl propane (lignin skele-
ton) vibrations due to methyl and methylene groups
and the aromatic ring. The most significant bands in
the lignin spectrum are due to structural subunits such
as guaiacyl propane, syringyl propane and parahy-
droxyphenyl propane. The frequency at 3426 cm-1 is
due to O–H stretching; 2920 and 2837 cm-1 are due to
C–H stretching in the methyl and methylene groups;
1614 and 1513 cm-1 are due to C=C (Kline et al.
2010) stretching of the aromatic ring in lignin. The
stretching frequency at 1435 cm-1 is due to O–CH3
(Yang et al. 2007) vibrations and 1268 cm-1 is due to
C–O stretching of aryl groups. The frequency at
1021 cm-1 has to be attributed to C–O stretching in
primary alcohols (Kline et al. 2010).
Figure 1b shows the FTIR spectrum of holocellu-
lose. Cellulose together with hemicellulose is holo-
cellulose. Holocellulose acts as the compatibiliser
between cellulose and lignin. It forms an amorphous
matrix surrounding cellulose and is softer than cellu-
lose. Hemicellulose is composed of xylose, mannose,
glucose, galactose, arabinose and uronic acids. The
frequency at 3400 cm-1 is due to O–H stretching.
Frequencies at 2920 and 2843 cm-1 is due to C–H
stretching in methyl and methylene groups;
1737 cm-1 is the carbonyl stretching in conjugated
carboxylic groups (C–O stretching of the acetyl and
uronic ester groups of hemicelluloses or the ester
linkage of carboxylic groups of ferulic and p-coumaric
acids of hemicelluloses); 1634 cm-1 may be due to
absorbed water and 1424 cm-1 corresponds to the C–
O stretching and CH or OH bending in hemicelluloses
(Sun et al. 1998). The frequencies at 1382 and
1169 cm-1 are attributed to C–H deformation and
C–O–C vibration in hemicelluloses, respectively. The
frequency at 1323 cm-1 is due to OH bending and
1021 cm-1 is due to C–O–H bending, which are
typical of xylans (Fang et al. 2000). By comparing the
FTIR of Fig. 1a and b, it can be concluded that the
stretching frequencies at 1614 and 1516 cm-1, which
are assigned to the aromatic skeleton and the

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Cellulose (2016) 23:1803–1812
Fig. 1 FTIR spectra of (a) lignin and (b) holocellulose
characteristic feature of lignin, are absent in Fig. 1b.
Moreover, the frequency at 1737 cm-1 is present in
Fig. 1b, indicating that the carbonyl group is absent in
Fig. 1a.
Figure 2a shows the FTIR spectrum of a-cellulose;
the broad band at 3419 cm-1 is due to O–H stretching
having strong inter- and intra-molecular H-bonding.
Frequencies at 2921 cm-1, 2846 cm-1 are due to C–H
stretching in the methyl and methylene groups. The
frequency at 1643 cm-1 is due to absorbed water.
Frequencies at 1437, 1383 and 1318 cm-1 are due to
the bending of CH, CH2 and OH, respectively, which
are typical for polysaccharides, and 1036 cm-1 is due
to C–O stretching.
Figure 2b shows the FTIR spectrum of isolated
MCC. The FTIR spectrum reveals that a-cellulose and
MCC show almost similar absorption frequencies at
2911, 2846, 1437, 1373, 1318 and 1036 cm-1. The O–
H stretching frequency in a-cellulose is found at 3419
and for MCC it is at 3409 cm-1. The decrease in
Fig. 2 FTIR spectra of (a) a-cellulose and (b) MCC
1807
vibrational frequency and band broadening is attrib-
uted to the extent of hydrogen bonding.
TG and DTG analysis
Figure 3a–d show the TGA of sago seed shell,
holocellulose, a-cellulose and MCC. Each shows
starting decomposition around 100 °C due to evapo-
ration of water. The wide range of 230–600 °C for sago
shells is attributed to the decomposition of lignin,
holocellulose and other components present in the seed
shell. For holocellulose (Fig. 3b), the main decompo-
sition is in the range 200–340 °C (Joseph et al. 2003;
Poletto et al. 2014). From the DTG curve Fig. 4b,
Fig. 3 TGA of (a) sago seed shell, (b) holocellulose, (c) a-
cellulose and (d) MCC
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Fig. 4 DTG of (a) sago seed shell, (b) holocellulose, (c) a-
cellulose and (d) MCC
Table 3 TGA results of Sago seed shells, holocellulose, a-
cellulose and MCC. Onset temperature (Tonset) and degradation
temperature on maximum weight-loss rate (T max) in °C
Name Tonset (°C) Tmax (°C)
Sago seed shells 230 600
Holocellulose 200 340
a-Cellulose 250 340
MCC 250 340
which has a shoulder at 250 °C, this is due to
hemicellulose and the peak at 340 °C is assigned to
cellulose (Sebio-Puñal et al. 2012), indicating the
presence of the crystalline, amorphous nature and also
to the heterogeneity in structure. a-Cellulose and MCC
have almost the same decomposition temperatures in
the range of 250–340 °C, which is due to degradation
processes of cellulose such as the decarboxylation,
depolymeristion and decomposition of glycosyl units.
The decomposition temperature is found to be higher
than for holocellulose and, moreover, there is no
shoulder around 250 °C indicating the removal of
hemicellulose portions. This can be clearly identified
from their DTG curves in Fig. 4c and d. The TGA
results of the different isolated components are
presented in Table 3. The pattern of the thermogram
for MCC is well defined, indicating a well-ordered
structure, which is further supported by XRD analysis.
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Cellulose (2016) 23:1803–1812
Fig. 5 XRD pattern of (a) sago seed shell, (b) a-cellulose and
(c) MCC
The TGA results show that the thermal stability of the
MCC is significantly lower than that of the shell
powder; this is because more heat-stable non-cellulosic
materials in the shell powder have been removed
during treatment (Carrier et al. 2011).
X-ray analysis
It has been well established that cellulose contains
both crystalline and amorphous regions. Figure 5a
shows the X-ray patterns of the sago seed shells. The
peaks are not defined, but in Fig. 5b, those of isolated
a-cellulose the peaks are defined and can be observed
for 2h at 21.2°, 34.6° and the shoulder in the 2h range
of 14°–17°, representing a typical cellulose I structure
(Bondeson et al. 2006). The DC is found to be 44 %.
The crystallinity index is high for cellulose because of
the removal of lignin and hemicellulose, which existed
as amorphous regions that reoriented the cellulose
chains (Li et al. 2009). Figure 5c shows the X-ray
pattern of MCC, which has a pattern similar to that of
a-cellulose, but the peaks are more defined and
intensified, with sharp peaks at 2h, 15.1°, 16.8°,
22.8° and 34.6° corresponding to the (110), (110),
(200), and (004) crystallographic planes (Sèbe et al.
2012). The X-ray diffraction pattern of MCC also
shows the possibility of a small amount of cellulose II
(Sèbe et al. 2012). The DC is found to be increased
from 44 to 67 %, exhibiting higher crystallinity
because of the efficient removal of the amorphous
parts by the cleavage of glycosidic linkages releasing
crystallites. When there is efficient removal of the
amorphous region, the rigidity increases, which is
Cellulose (2016) 23:1803–1812
Fig. 6 SEM images of a sago seed shell, b a-cellulose and c MCC
further supported by thermal analysis. Using more
crystalline cellulose materials such as MCC or
nanocellulose, the mechanical property of composite
will be increased.
SEM, TEM and AFM analysis
SEM analysis was carried out to study the morphology
and textural properties of the different extracted
components. Figure 6a–c reveals the morphological
change occurred during the isolation process. Fig-
ure 6a shows that there is a randomly oriented
distribution of morphologies in the structures of seed
shells due to the presence of lignin, hemicellulose and
other components. Hemicellulose, which acts as a
compatibiliser between celluloses and lignin, and
lignin, which acts as a binder, are gradually removed
to help the isolation of MCC. The isolated MCC
1809
consists of a mixture of aggregated and non-aggre-
gated fibres and showed an aggregated structure
composed of small fibres with coalesced boundaries.
Its morphology is similar to that of commercial MCC
(Kumar et al. 2002).
The transmission electron micrograph results are
shown in Fig. 7a. TEM analysis clearly shows that
small MCC particles are agglomerated to form large
particles on the micron scale having random orienta-
tions along with some non-agglomerated structures
(Mohamad Haafiz et al. 2014). The TEM results
corroborate with the surface morphology obtained by
SEM. The surface morphology has also been inves-
tigated by AFM. The results of the two-dimensional
AFM image (Fig. 7b) show the larger extent of
agglomeration or aggregated structure. Figure 7c
shows the 3D image and reveals that the isolated
MCC consists of some spherical particles with non-
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Fig. 7 a TEM images of MCC, b AFM image of MCC, height view, and c 3D view
uniform and rough surfaces (Mohamad Haafiz et al.
2013). Both the TEM and AFM results reveal the
microstructural behavior of isolated MCC.
Conclusions
The composition of sago seed shells has been estab-
lished by standard methods of determination and has
been found to be Klason lignin, holocellulose, a-
cellulose, hemicellulose (by difference) and ash
content. Separated components have been charac-
terised by using FTIR, TGA, XRD, SEM, TEM and
AFM. Sago seed shells have reasonably good lignin
content and high cellulose, therefore, they can be used
as a potential source for the extraction of cellulose;
moreover, the seed shell powder can be effectively
utilised as a filler for the preparation of biocomposites.
Isolated a-cellulose has been converted into MCC.
From FTIR, TGA and XRD, it has been established
that the isolated MCC has higher crystallinity than a-
cellulose because of the efficient removal of the
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Cellulose (2016) 23:1803–1812
amorphous regions. The SEM, TEM and AFM results
reveal the microstructural behavior of isolated MCC.
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