Asian Journal of Chemistry; Vol. 26, No.

4 (2014), 955-959

http://dx.doi.org/10.14233/ajchem.2014.15652

Physico-chemical and Thermal Properties of Starch

Derived from Sugar Palm Tree (Arenga pinnata)

J. SAHARI1, S.M. SAPUAN1,2,3,*, E.S. ZAINUDIN2,3 and M.A. MALEQUE4

1
Laboratory of Advanced Materials and Nanotechnology, Institute of Advanced Technology, 43400 UPM Serdang, Selangor, Malaysia
2
Department of Mechanical and Manufacturing Engineering, 43400 UPM Serdang, Selangor, Malaysia
3
Laboratory of Biocomposite Technology, Institute of Tropical Forestry and Forest Products, Universiti Putra Malaysia, 43400 UPM Serdang,
Selangor, Malaysia
4
Department of Manufacturing and Materials Engineering, International Islamic University Malaysia, 53100 Kuala Lumpur, Malaysia

*Corresponding author: E-mail: [email protected]; [email protected]

Received: 18 April 2013; Accepted: 27 August 2013; Published online: 15 February 2014; AJC-14677

Petroleum based polymers are extremely stable and commonly used in various industries include food packaging, furniture and automotive.
However, the waste that come from petroleum based polymer material has brought negative impact not only for human being, but also
create the serious environmental problems. Hence, biopolymers that come from natural source such as starches are now being considered
as an alternative to the existing petrochemical based polymers. This study was aimed to examine the potential of sugar palm starch
extracted from sugar palm tree (Arenga pinnata) as a new biopolymer. The important properties of sugar palm starch studied were the
chemical properties, thermal properties, particle size and morphological surface. The starches isolated from sugar palm tree contained
comparable amounts of amylose (37.60 %) which were higher than tapioca, sago, potato, wheat and maize. The results showed significant
differences in the chemical content as well as in the granule sizes of sugar palm starch. Thermal characteristic studies using thermogravimetry
analysis and differential scanning calorimetry showed that sugar palm starch was thermally stable than other starches. Study on morphological
surface indicated that sugar palm starch were rounded and oval-shaped.

Keywords: Sugar palm starch, Biopolymer, Chemical properties, Thermal properties.

INTRODUCTION product and the fruits can be cooked with sugary syrup for
desserts. The outer part of the stem consists of wood which is
Sugar palm tree is one of multipurpose trees grown in extremely hard and durable. It can be processed for flooring,
Malaysia. It is a member of the Palmae family and naturally a furniture and hand grips of tools. It is also reported that the
forest species. It belongs to the subfamily Arecoideae and tribe sugar palm’s roots are useful for medicine4,5. Nowadays,
Caryoteae. Haris1 reported that sugar palm have approximately researchers are more focusing on production of bioethanol
around 150 local names indicating its multiple uses by the that can be derived from neera sugar via fermentation process6,7.
villagers. The names includes, Arenga pinnata, Areng palm, Apart from that, sugar palm starch (SPS) also accumulates
Black fibre palm, Gomuti palm, Aren, Irok, Bagot and Kaong. in the core of the stem of the sugar palm. The common indus-
One of the most important products of the sugar palm tree is trial starches are typically derived from cereals (corn, wheat,
palm sugar locally known as neera sugar. Neera sugar usually rice, sorghum), tubers (potato, sweet potato), roots (cassava)
used as food sweeterner in traditional food. Palm sugar can be and legumes (mung bean, green pea). Sugar palm starch is the
consumed freshly or let it be fermented for a while to become example of starch derived from another source, the stem of
palm wine2. It has been reported that sugar palm was the first sugar palm same as commercial starch extracted from sago
sources of sugar, fermented drinks and syrup3. palm. It has been documented that one tree of sugar palm can
Besides yielding neera sugar, it also provides a great produce 50 to 100 kg of starch8.
variety of products such as ropes, filters, brooms and roof Due to unique behaviour of starch, many researchers have
materials. Sugar palm tree can also produce juices from its been using it as biopolymer9. Teixeira et al.10 used plasticized
fruits. The fruits are white in colours which are taken from its cassava starch as a biopolymer and combined it with cassava
fruit bunch. They can be preserved in heavy syrup for canned bagasse cellulose nanofibrils as reinforcing materials.
956 Sahari et al. Asian J. Chem.

Prachayawarakorn et al.11 prepared biodegradable polymer m

from thermoplastic rice starch (TPRS). Vallejos et al.12 applied ρ=
V
corn and cassava starchs plasticized with 30 wt % glycerin as where ρ is the density of fibre, m is the mass of fibre, V is the
biopolymer and using fibrous material obtained from ethanol- volume of water.
water fractionation of bagasse as reinforcement. However, up Determination of amylose: Amylose content of sugar
till today, there is no research been carried out to evaluate the palm starch was determined according to IRRI method13 using
potential of sugar palm starch as biopolymer. Hence, this study spectrophotometer.
was done in order to investigate the properties of sugar palm Determination of ash: An accurately sample (5 g) was
starch and to explore their potential to be used as a new alter- weighted and incinerated in a muffle oven at 600 ºC until a
native biopolymer. constant weight was achieved. Ash content was calculated as
the weight of the residue divided by the original weight of the
EXPERIMENTAL
sample, expressed as percentage.
Extraction of sugar palm starch: The sugar palm starch Determination of moisture content: Sugar palm starch
(SPS) was collected from sugar palm tree at Jempol, Negeri was weighted using a weighing balance and recorded as M1.
Sembilan, Malaysia. Fig. 1 shows the extraction method of The samples were dried in the oven at 105 ºC for 24 h and
sugar palm starch. Firstly, the matured sugar palm tree was reweighted (M2). The moisture content was calculated using
felled using chainsaw and the mixture (woody fibres and starch formula shown below:
powder) was obtained from the interior part of the stem. This M1 − M 2
mixture was then carried out for washing process to obtain Moisture content (%) = × 100
the starch. In washing process, water was added to the mixture M1
and then the mixture was kneaded by hand. The fibers remain where, M1 = weight of air dried sample (g), M2 = weight of
on the top of the sieve while the water carrying the starch oven dried sample (g).
granules in suspension passes through the sieve and was caught Fourier transform infrared (FT-IR) spectroscopy: The
in container. The starch settles on the bottom and the excess spectra were obtained using an IR spectrometer (100 Series
water flows over the sides. After washing process, the fibrous type, Perkin-Elmer). About 2 mg of sample which is in powder
remnants were discarded and the wet starch was taken out form was mixed with potassium bromide (KBr) and pressed
from the container. Then starch was kept in an open air for a into a disc of ca. 1 mm thick. The FT-IR spectra of the sample
moment and dried in an air circulating oven at 120 ºC for 24 h. were collected in range of 4000-200 cm-1. FTIR allows the
measurements of variations on samples because of the chemical
treatments. FTIR of the samples were recorded in the trans-
Sugar palm trunk
mittance mode.
Thermogravimetric analysis (TGA): Sugar palm starch
Collection the was prepared for TG analysis. The thermogravimetric analysis
mixture Outer part of trunk (TGA) conditions were: a nitrogen atmosphere, a flow rate of
20 mL min-1, a heating rate of 10 ºC min-1 and a temperature
range from ambient to 800 ºC.
Washing process Differential scanning calorimetry (DSC): DSC measu-
rements were carried out in a Shimadzu TA-50WSI Thermal
Fibres Analyzer equipped with DSC-50 modules. The scans were
Sieving
carried out from room temperature to 500 ºC at a heating rate
of 10 ºC min-1, using a nitrogen atmosphere with a flow of 20
Settling & washing mL min-1.
of starch Particle size analysis: Particle size and distribution was
analysed by using Mastersizer 2000 E (Malvern Instruments,
Malvern, UK) fitted with the Qspec Dry powder Feeder.
Drying Scanning electron microscopy (SEM): Scanning electron
microscopy (SEM) Hitachi S-3400N operating at an accele-
ration voltage of 0.3-30 kV was performed to study the surfaces
Sugar palm starch morphology of the native sugar palm starch.
(SPS)
RESULTS AND DISCUSSION
Fig. 1. Extraction of sugar palm starch
Chemical properties: It is known that sugar palm starch
Measurement of density: The density (ρ) of sugar palm and other commercial native starches contain 10-20 % moisture
starch was determined using specific gravity bottle and water under normal atmospheric conditions. Since starch is very
as liquid. Initially, sugar palm starch was weighted (m) and sensitive to water, the amount of water absorbed by starch
than immersed into water. The amount of water before and granules is dependent on the relative humidity (RH) and the
after immersion was recorded as the volume (V) and was used temperature of the atmosphere in which they have been stored.
in the determination of the density of sugar palm starch. The starches isolated from sugar palm starch contained
Vol. 26, No. 4 (2014) Physico-chemical and Thermal Properties of Starch Derived from Sugar Palm Tree 957

comparable amounts of amylose (37.60 %) which were higher of phosphate groups. As metals, the ash of native starches
than that of tapioca (17 %), sago (24-27 %), potato (20-25 %), contains mainly calcium, potassium, magnesium and sodium18.
wheat (26-27 %) and maize (26-28 %). All kinds of starch FTIR analysis: The FTIR technique detects the absorption
contain two types of glucose polymers i.e., an essentially linear of different bond vibrations in starch molecules and it is sensi-
molecule termed amylose and a highly branched polymer tive to changes in molecular structure such as starch chain
termed amylopectin. Amylose molecules consist of 200- conformation, helicity, crystallinity and moisture content. FTIR
20,000 glucose units which form a helix as a result of the was used in order to detect the presence of the functional groups
bond angles between the glucose units. Amylopectin is a highly existed in sugar palm starch. Fig. 3 shows the FT-IR spectrum
branched polymer containing short side chains of 30 glucose of sugar palm starch. The intense peaks at 3500-3200 cm-1
units attached to every 20-30 glucose units along the chain. shown in figure indicated the presence of O-H groups in sugar
Amylopectin molecules may contain up to two million glucose palm starch. This prove that starches are very sensitive to water
units (Fig. 2). The amylopectin content is calculated from: molecule due to the present of hydroxyl groups. Meanwhile,
amylose content + amylopectin content = 100 %. the strong peaks at 3000-2850 cm-1 assigned to the C-H stretching
and peaks at 1030-990 cm-1 was characteristic of the anhydro-
glucose ring O-C stretch19. The peaks at around 1450 and 1200
cm-1 were characteristic of C-O-H. While, peaks at 1600-1500
cm-1 attributed to the bending of water in starch20.

120

100

80
Intensity (%)

60

40

20

0
4000
3804
3608
3412
3216
3020
2824
2628
2432
2236
2040
1844
1648
1452
1256
1060
864
868
472
Wavenumber (cm–1)
Fig. 3. FT-IR spectrum of sugar palm starch

Fig. 2. Unit structure of amylose and amylopectin31 Thermal properties: Thermogravimetric analysis is one
of the thermal analysis techniques used to measure the mass
Proportion of the polysaccharides amylose and amylo- change, thermal decomposition and thermal stability of mate-
pectin become the most critical criteria that determine starch rial. Figs. 4 and 5 demonstrate the TG and DTG curve of sugar
behaviour14,15. Most amylose molecules (molecular weight palm starch. The molecular structure of sugar palm starch will
~ 105-106 Da) are consisted of (1→4) linked α-D-gluco- be degraded when heated. The mass loss below 100 ºC may
pyranosyl units and formed in linear chain. But, few molecules be attributed to evaporation of absorbed moisture21. The large
are branched to some extent by (1→6) α-linkages16,17. Amylose degradation at 310 ºC appears to involve further elimination
molecules can vary in their molecular weight distribution and of the polyhyroxyl groups, accompanied by depolymerization
in their degree of polymerization (DP) which will affect to and decomposition22. It has been documented earlier that at
their solution viscosity during processing and their retrogra- higher temperatures, depolymerization of the macromolecules
dation/recrystallization behaviour, which is important for takes place with the formation of b-(1,6) anhydro D-gluco-
product performance. Meanwhile, amylopectin is the highly pyranose (levoglucosan), 2-furaldehyde (furfural) and a range
branched polysaccharide component of starch that consists of of lower molecular-weight volatile and gaseous fragmentation
hundreds of short chains formed of α-D-glucopyranosyl products. A carbonaceous (substance rich in carbon) residue
residues with (1→4) linkages. These are interlinked by (1→6)- remains after all the volatile products have been driven off23.
α-linkages, from 5-6 % of which occur at the branch points. DSC is a thermal analysis technique that measures the
As a result, the amylopectin shows the high molecular weight temperature and heat flow associated with transition in mate-
(107-109 Da) and its intrinsic viscosity is very low because of rials as a function of temperature and time. One of the most
its extensively branched molecular structure. widely used applications of DSC is the determination of glass
For ash contents, sugar palm starch shows 0.2 % ash transition (Tg), melting point (Tm) and energy of fusion24-27.
content same as tapioca, sago and wheat starches. The ash From the curves in Fig. 6, Tg and Tm of sugar palm starch was
content can be determined as the residue after ignition of the around 242.14 and 279.84 ºC, respectively. These value were
starch at 600 ºC. From the table, it is found that potato starch has higher than Indica rice starch where Tg values was 237 ºC and
a relatively high ash-content compared because of the presence Tm was 276 ºC28. Luiz et al.29 have been reported that melting
958 Sahari et al. Asian J. Chem.
120 11
10
9 (a)
100 8

Volume (%)
7
6
80 5
4
Mass (%)

3
60 2
1
0
0.1 1 10 100 1000
40 Particle size (µm)

20 9
8 (b)
7

Volume (%)
0 6
0 100 200 300 400 500 600 5
Temperature (°C) 4
3
Fig. 4. TG curve of sugar palm starch
2
1
Temperature (°C) 0
0 0.1 1 10 100 1000
Particle size (µm)
0 100 200 300 400 500 600
Fig. 7. Particle size distribution of (a) sugar palm starch and (b) tapioca
-0.0005

The particle size of starch is one of the most important charac-

Derivative mass (%)

-0.0010
teristics, which may influence other physicochemical properties
such as swelling power and water-binding capacity30.
-0.0015

-0.0020

-0.0025

-0.0030
Fig. 5. DTG curve of sugar palm starch

-5

-10

Fig. 8. Scanning electron microscopy of sugar palm starch

-15

Scanning electron micrographs: The scanning electron

-20 micrographs of sugar palm starch granules was shown in Fig. 8.
The starch granules of sugar palm starch when viewed by SEM
-25 were rounded and oval-shaped granules with smooth surfaces.
50 100 150 200 250 300 350 400 450 500 550 From the micrographs, it is estimated that the granule size
Temperature (°C) ranges from approximately 10-100 µm, which is in agreement
Fig. 6. DSC curve of sugar palm starch with the study on particle size.
Conclusion
point of cassava starch occurred at 169.2 ºC. Thermal charac-
teristic studies using thermogravimetry analysis and differential The sugar palm starch was successfully extracted from
scanning calorimetry showed that sugar palm starch was thermally sugar palm tree. The important properties of sugar palm starch
stable than other starches. studied were the chemical properties, thermal properties,
Particle size: Starches from various sources are chemically particle size and morphological surface. The starches isolated
similar and their granules are heterogeneous with respect to from sugar palm tree contained comparable amounts of amylose
their size, shape and molecular constituents. Fig. 7a shows (37.60 %) which were higher than tapioca, sago, potato, wheat
the particle size analysis of sugar palm starch. It was revealed and maize. The results showed significant differences in the
that the sugar palm starch had the highest mean diameter chemical content as well as in the granule sizes of sugar palm
(36.308 µm) with a particle size distribution ranging from starch. Thermal characteristic studies using thermogravimetry
0.020-1000 µm. The results observed for the sugar palm starch analysis and differential scanning calorimetry showed that
peak are comparable to the tapioca starch as shown in Fig. 7b. sugar palm starch was thermally stable than other starches.
Vol. 26, No. 4 (2014) Physico-chemical and Thermal Properties of Starch Derived from Sugar Palm Tree 959

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