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To cite this article: Javier Chavarro Gomez, Mohd Noriznan Mokhtar, Alawi Sulaiman, Azhari Samsu Baharuddin & Zainuri Busu
(2015): Recovery of residual crude palm oil from the empty fruit bunch spikelets using environmentally friendly processes,
Separation Science and Technology, DOI: 10.1080/01496395.2014.994781
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Recovery of residual crude palm oil from the empty
fruit bunch spikelets using environmentally friendly
processes
Authors: Javier Chavarro Gomeza, Mohd Noriznan Mokhtar*a, Alawi Sulaimanb, Azhari Samsu
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Baharuddina and Zainuri Busuc.
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*Corresponding author:
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Mohd Noriznan Mokhtar (PhD)
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Faculty of Engineering, Universiti Putra Malaysia
MALAYSIA
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Phone no.: +603-89466367
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Fax no.: +603-8946 4440
Email: noriznan@upm.edu.my
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Details of co-authors:
a
Department of Process and Food Engineering, Faculty of Engineering, Universiti Putra
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Selangor, Malaysia
c
Felda Global Ventures Plantation Malaysia Trolak Region, 35600, Sungkai, Perak, Malaysia
Ac
Abstract
The development of new, low-cost technology to increase the oil recovery in the palm oil mill
especially from the palm oil wastes has been an important goal for the industry to increase OER.
According to preliminary oil detection, the residual oil is mainly located on the surface of
1
spikelet, about 73.73 0.05 % from total residual oil. The combined water-steam shows the best
oil extraction process, indicating 82 0.13 % of oil may be removed from the EFB spikelet.
Thus, this method is chemical free and environmentally friendly residual CPO recovery process
using EFB.
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Keywords: empty fruit bunches (EFB), spikelet, crude palm oil (CPO), hydro solvent assisted
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steam extraction (HYSASE), oil recovery
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1. Introduction
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The palm oil industry is one of the most significant growing industries with huge annual
production of crude palm oil (CPO) estimated on some 19 million tons in 2012 [1]. Despite that,
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there is still the need to improve the recovery process to minimize CPO losses. The total CPO
content inside fresh fruit bunches (FFB) from oil palm (Elaeis guineensis) reaches 23 25% [2].
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Yet in Malaysia, the oil extraction rate (OER) was only 20.25% in 2013 [3], which means that
around 2.7 4.7% of oil is lost in forms including biomass such as empty fruit bunches (EFB),
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mesocarp fiber, palm oil mill effluents (POME) and decanter cake.
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The EFB is the major component of the solid waste generated by palm oil mill. It constitutes
23% of the FFB wastes [4] in which 1.13 tons of EFB was generated from each ton of CPO
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produced. Due to the mechanical processes such as loading of OPEFB into the sterilizer cage,
sterilization and stripping, certain parts of the oil are impregnated in the EFB from the fruitlet.
This results in 3 - 4% (wet basis) of the residual oil in the EFB [5], indicating that a high amount
2
To minimize oil loss, some developments have been made to improve the CPO recovery mainly
from mesocarp fibers [6, 7], but there has been insufficient work on EFB. Few research projects
have been carried out regarding recovering [8], utilizing, and integrating [9] residual oil in the
EFB. In Malaysia, the extraction of residual oil from mesocarp fibre with hexane has been
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implemented with a monthly production of 1500 to 2000 tons of recovered oil. Nonetheless, it
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has shown not to be technically viable due to the bulkiness of EFB and the high potential to
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produce volatile organic compounds which leads to solvent loss and health problems [10]. Other
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technologies such as mulching and composting [11], EFB pelletizing, extraction of short and
long fibers, and etc. [12], have been explored in order to exploit the EFB and to minimize old
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practices such as combustion, in which residual oil in EFB can contribute to higher heat capacity
that suitable for the process. Nevertheless, the high water content (~ 60%) of EFB will decrease
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the efficiency of the combustion process as well as generate a high amount of carbon monoxide
and toxic gases. Thus, it has been forbidden by the Department of Environment (DOE) [13].
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Nowadays, some mills have implemented the usage of shredding and pressing machines to
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recover residual oil in EFB. The implementation of shredding and pressing systems is not only to
recover residual oil from EFB, but also to remove moisture content and as a pre-treatment for the
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EFB before composting or mulching [12]. However, the oil recovery using this process is only
1.5 % from EFB [8], indicating low oil removal compared to the total amount of residual oil
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(about 0.5 2.5 % still remained in the fiber). Besides that, the extracted oil may contain high
amount of impurities and residues; one of them is the waxy layer from the outer layer of the EFB
[14]. In additions, due to high content of silica body on the EFB, the strength and abrasive
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properties of the fibers are high [15], requiring frequent shredding blade maintenance and
Currently, the petroleum oil industries use steam and water to enhance the recovery of oil from
deep pounds [16]. Therefore, using some information regarding the cyclic steam method in
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petroleum recovery process, it can be modified and applied to remove CPO from EFB based on
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its lower viscosity at higher temperature [17]. The advantage is the availability of water and
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steam in the current palm oil mill, which may reduce the cost of implementation in the mill. The
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use of water and steam is also environmentally safe. Therefore, the aim of this work is to study
different extraction processes using steam or/and water to recover residual oil from the EFB.
2. Experimental procedures
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2.1 Material
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The fresh EFB and CPO were collected from Besout Palm Oil Mill located in Perak, Malaysia.
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The chemical used for oil detection was Sudan Red G (Sigma, Germany), dissolved (0.7%) in
polypropylene glycol (R&M, Malaysia) [18]. For oil content analysis, hexane (Fisher Chemical,
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U.K) was used. The quality of CPO was analyzed by Metalab Palm Oil Tester (225001/0006,
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CDR, Italy) according to standard procedures for free fatty acids (FFA), deterioration of
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2.2 Methods
Sample preparation
The EFB were packed in plastic bags and stored at 5C. Prior to extraction, the spikelets were
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manually separated from the stalk. From our observation and analysis (data not shown) the
spikelet was chosen due to residual oil is mainly located on it rather than on stalk, which is also
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described by Ma [19]. Then, they were further cut into 5 0.5 cm lengths and 40 3 g was used
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in each process. Finally, for the purpose of comparing oil removal efficiency that affected by the
size of material, the HYSASE process was repeated (it was carried out only two cycles) using
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three different sizes of EFB spikelet (with its original form; 13 0.5 cm, manually cut; 1 0.2
cm, and grinded form using machine (Retsch, SM200, Germany); ~ 1 mm).
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Extraction chamber description
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The extraction processes were carried out in 500 ml insulated chamber, described as a cylinder
tank. This chamber consisted of two inlets and two outlets, and each stream was controlled using
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valves. The outlets were placed with one at the top of chamber and another at the bottom. The
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two inlets were placed at the bottom of the chamber. A thermometer was connected directly to
the chamber.
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Oil detection
The detection of oil on EFB spikelet was accomplished using Sudan Red. The use of this dye has
been studied before to identify lipids on animal tissue and vegetables [18]. Sudan Red solution
5
was applied directly on the surface and inner part by the vertical cut of spikelet before the
process. The identification of oil was done using Dyno-Lite digital microscope (AM-413ZT,
Taiwan) at 40x magnification under UV light. Analysis was repeated after completing the
extraction process to visualize the remaining oil. In order to understand the structure of EFB,
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observation of inner fibers and the surface of spikelet were carried out by Scanner Electron
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Microscopy (SEM) (d4300, Hitachi, Japan).
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Steam
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The EFB spikelet was loaded into the empty extraction chamber. Then, the saturated steam was
injected into the chamber from the top at a flow rate of 7 mL/min. The condensed water with
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removed oil was collected at the bottom of the chamber every 5 min (each cycle is 5 min and it
was repeated for 3 times), and approximately 40 ml was obtained from each cycle. Oil analysis
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from each sample was carried out using EPA gravimetric method 1664A with hexane, in which
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oil can be recovered from water. The top layer (hexane-oil) was taken and dried in the oven at
70oC for 12 h. The dried residual oil was weighed for oil recovery analysis (Eq. 1).
ce
()
(%) = 100% (Eq. 1)
()
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To analyze the oil removal from EFB spikelet, the oil content in spikelets was initially obtained
before the process. The spikelet was dried in oven at 105C for 24 h. Then, the outer layer
(surface of spikelet) and inner layer were manually separated for independent analysis. After
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that, the oil content was analyzed using soxhlet with hexane in the ratio of 9:1 (solvent: fiber) for
6 h at 70C (AOCS method AM 2-93). The extracted solvent was evaporated using rotary
vacuum evaporator (IKA RV10 Digital V, Germany) at 50C and 2.85 psi. The sample was
further dried to remove remaining hexane in an oven at 70 C for 12 h. Finally, the process was
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repeated using spikelets obtained after the extraction process, and the oil removal was calculated
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based on the difference weight of recovered oil from dried spikelet, before, and after the process
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(Eq. 2).
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() ()
(%) = 100%
()
(Eq. 2) an
Hot water
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The process was carried out by loading the spikelet into the same extraction chamber as
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previously described. The hot water (60C) from the water bath was introduced to the bottom of
the chamber using peristaltic pump (FH15, Thermo Fisher Scientific, USA) at a flow rate of 150
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ml/min. The sample was collected at the top of the chamber every 5 min until the 4th sample. The
oil analysis was carried out as previously described using the gravimetric method. Finally, the
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process was repeated using hot water at 90C under the same process conditions.
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Steam-water
The spikelet was placed in the extraction chamber as described previously. The saturated steam
was injected at a flow rate of 7 mL/min into the chamber from the top for 5 min. Then, 100 ml of
water (30C) was added into the chamber to rinse the hot oil, and the sample was collected from
7
the bottom of the chamber. This cycle was repeated for three times. Finally, using the same
method described previously, the oil recovery analysis was calculated. The process was repeated
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The spikelet was loaded into the chamber as previously described. The chamber was fed by
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water at 30C through the bottom of chamber, until the spikelet was submerged completely
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(approximately 200 ml of water was used). Then, the water was bubbled using saturated steam
that injected into the chamber from the bottom at a flow rate of 7 mL/min until the temperature
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inside reached at 100C. The injection of steam was continued for additional 5 minutes allowing
the heat to further penetrate within the spikelet. Finally, the water with oil was drained and
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collected for further analysis as previously described. The process was repeated for 3 cycles;
option for soaking process, the vent can be manipulated to increase the pressure inside the vessel.
This study was only carried out under atmospheric pressure by opening the vent.
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Sudan Red was used to identify the oil in the spikelet under microscope. The stained oil produce
an intensively glow under UV light and reduce its florescence in the presence of water, allowing
identification of the difference of oil-water on the spikelet [20]. Fig. 2.a shows the results
8
obtained from the stained oil on the cut by transversal of spikelet. On the other hand, Fig. 2.b
depicts the Sudan Red on the surface of spikelet with the outcome that more oil was detected
compared to the oil that detected inside based on color intensity (Fig. 2.b).
The structure of inner fiber of EFB spikelet was inspected under SEM (Fig. 3.a; Fig. 3.b). SEM
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showed that the inner spikelet fibers integrated among of them with high pore volume (Fig. 3.a),
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and surrounded by cylinder of silica bodies (Fig. 3.b) as discussed by Bahrin et al. [14] and Omar
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et al. [15]. The visual analysis on the surface of EFB spikelet shows as a dense, uniform and non-
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porous surface (Fig. 3.c). It indicates the waxy layer of spikelet as described by Benazir et al.
[21] for plant based material. Therefore, the residual oil diffuses into the inner part of spikelet
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can be partly prevented; this is why more oil is accumulated mainly on the surface. Therefore,
the invention of process was taken place in the removal of oil that mainly attached on the
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surface, by minimizing destruction of original surface structure of EFB spikelet. Once the
surface is destroyed, more oil will move into the fiber, resulting in more difficulty for oil
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From this reason, the use of mechanical treatment which destroys the surface of the spikelet has
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limitations for oil recovery during the aqueous process. Shredding and pressing machine
destroyed the surface of spikelet, allowing more oil to diffuse into the inner fibers that adsorb the
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oil strongly, which requires additional energy consumption for the pressing machine to release
more oil from the fiber. Subramaniam et al. [7], studied the usage of aqueous process to remove
oil from mesocarp. Initially, mesocarp with residual oil (11% dry basis) was washed with hot
water in the digester. Then, the mesocarp was pressed using screw press system to achieve up to
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83% oil removal. However, the use of pressing systems may contribute to increase the
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The analysis of oil was based on yield recovery by gravimetric method of different processes
using steam, hot water, combined steam-water and combined water-steam as shown in Fig. 4. It
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indicates that the first cycle shows the highest oil recovery for all processes, except the process
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with steam. When the process cycle was repeated, the oil recovery reduces. It reflects to low oil
removal due to reduction of residual oil on the surface and certain portion of oil might already
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move into the inner part of the spikelet. The use of gravimetric method with hexane could not
recover all of the oil suspended in water due to certain portion of oil formed emulsion in very
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small droplets (in micro order) that can be clearly seen under microscope (result not shown here).
Even so, at least the method can be used to evaluate the performance of each process.
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The use of saturated steam for oil extraction is not feasible due to very low oil recovery per the
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analysis (Fig. 4), indicating only around 2.02 % for total of 4 cycles. Even the viscosity of oil
was reduced, the oil that attached on the surface was not completely removed due to steam is not
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an appropriate media to bring out the oil. The extraction using hot water indicates that higher
temperature (90C) that applied on the process obtained higher oil recovery analysis (7.14%)
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compared to lower temperature (60C) as shown in the same figure. Thus, the use of hot water is
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The application of hot water as a media in this experiment could not remove much oil from the
surface due to energy that provided from water was not enough to decrease the dynamic
viscosity of oil. For example, at 60C, only 0.73% of oil was recovered and the oil viscosity was
estimated at 20 mPas [17], which is still too high compared to the viscosity of hot water at that
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temperature (0.47 mPas). Therefore, to reduce the oil attached to the surface, the process
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requires more energy to minimize the viscosity difference between oil and water. The effect of
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temperature on the viscosity of CPO at high temperature was studied before [17]. At room
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temperature (30C), the dynamic viscosity difference between CPO and water was 53 mPas.
After increasing temperature to 100C, the viscosity of CPO and water were 5 mPas and 0.3
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mPas, respectively, indicating the difference was reduced significantly to 4.7 mPas. The
decreasing the CPO viscosity by increasing temperature is the main strategy to remove CPO
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from the material.
The application of petroleum oil recovery using steam cycle may be modified and implemented
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for the recovery of residual palm oil from biomass. According to Alvarez and Han [16], three
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basic steps are required for oil recovery process. First step is the temperature of oil must be
elevated at certain point that allows the oil to flow easily due to low viscosity (injection; with
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heating element) as explained in previous paragraph. In second step, the heat has to be further
penetrated and release the oil from support material (soaking) and the final step is oil requires a
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From this study, the combination of steam and water was examined. The basic idea, based on
energy supply, mainly comes from steam and oil media carrier as water. In Fig. 4, the highest
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total oil recovery using this method was obtained when applying 3 min steam injection time
(18.29 %, total of 4 cycles). When the steam injection was extended to 5 min, oil recovery
analysis was reduced to 14.29 % due to the higher probability of oil being adsorbed into the
fiber. In the first cycle, the highest oil recovery was obtained when using shorter steam injection
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time (1.5 min), indicating 9.28 % of oil recovery was obtained compared to 3 min (5.14 %) and 5
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min (4.80 %). Therefore, the steam injection time is a critical factor that affects oil recovery. The
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process must be carried out as fast as possible to minimize the oil loss that simultaneously
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penetrates into the fiber. It is important to recover oil during the initial process, before the oil
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In order to improve the oil recovery, extraction process was carried out by combining water with
steam, in which the process was named as Hydro Solvent Assisted Steam Extraction (HYSASE),
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(Fig.1). The chamber was filled with water as a media for heat transfer and oil removal. Then,
the steam was introduced to the chamber by bubbling the water to supply the energy. HYSASE
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shows the highest oil recovery compared to among processes, indicating about 61 %. It is
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The qualitative comparison of oil distribution after the steam and HYSASE processes was
conducted using Sudan Red and the results are shown in Fig. 5. After the extraction process by
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steam, the surface of spikelet shows a decrease of oil content but there was an increase of oil
inside the fiber based on color intensity. Therefore, the steam process contributed the oil
diffusion to porous fibers and resulted in lower oil removal. In contrast, after the extraction
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process by HYSASE, the oil detected in the inner spikelet was lower and less oil was identified
The oil content analysis was carried out for surface and inner layer of EFB spikelet as shown in
Fig. 6. Initially, about 73.73 0.05% from total residual oil content located on the surface, and
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remaining residual oil was within the fiber. After the processes, the residual oil on the surface
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decreased to 5% and 48% through the HYSASE and steam process, respectively. Oil removal
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from the inner part of spikelet when using steam was slightly increased from 26.27% to 30.48%,
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confirming that oil diffusion into inner part occurred during the steam process. In contrary, using
HYSASE, it decreased drastically to 11.36 %. Overall, in terms of total oil removal, higher
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amount of oil could be removed using HYSASE (82 0.13 %) than using saturated steam (26
0.28%).
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In Fig. 7, the highest oil recovery was achieved with spikelet in its original form, indicating
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39.60 0.26% of oil recovery for only the 1st cycle. When the material size was reduced, it
affected the decreasing oil removal. Therefore, by reducing its size means that its structure was
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destroyed and it encouraged the oil diffusion into the fiber as discussed before. In this case, due
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to oil distribution mainly on the surface of spikelets protected by waxy layer, it does not require
discussed by Rosenthal et al. [22], grinding the material is an important step to increase the
contact area during the extraction of bearing seeds such as soybean, sunflower, and so on, as well
as to breakdown the cell walls that contain the oil, which deferent from this case.
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3.4 Crude palm oil quality analysis
The quality analysis of oil that obtained by shredded and pressed, HYSASE, and fresh CPO from
the mill was conducted by Metalab Palm Oil Tester and the results are shown in Table 1. The
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FFA, DOBI and carotene indicate almost similar value for the recovered oil by shredded and
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pressed, and HYSASE. However, according to Pocketbook of Palm Oil Uses (MPOB) [23],
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these values are out of acceptable quality range compared to the value obtained from fresh CPO.
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The PV obtained by HYSASE was the highest compared with the other analyzed samples. This
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may be due to the high temperature used during the process (100C) and the presence of oxygen;
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these conditions may enhance the oxidation of oil [24]. Unfortunately, this cannot be avoided
due to oil being mainly located on the surface of spikelet and easily effected with oxygen.
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In general, the oil that recovered shows low quality compared to the oil that obtained from the
palm mill and may not suitable to be used for edible purposes. Nevertheless, due to high oil
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removal that obtained by HYSASE process, it indicated a good potential to be further explored
and developed. The recovered oil can be used for non-edible purposes (i.e. oleo-chemistry),
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5. Conclusions
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Oil recovery from EFB was carried out by applying different water and steam processes. The
study of oil that attached on the surface and inner part of spikelet provides an insight for
developing an appropriate technology to remove the residual oil. As a result, the HYSASE
14
process was introduced in which the highest oil recovery was obtained compared to other
processes. The oil recovered from shredded-pressed EFB and HYSASE indicate similar quality
values, except for PV, with the advantage that more oil may be recovered by HYSASE.
Therefore, the HYSASE process serves as an efficient, environmentally friendly and novel
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process to remove the residual oil from the EFB spikelet. According to the quality analysis, the
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recovered residual oil probably is not suitable to be used as CPO that obtained from the main
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process at the palm oil mill. However, it has potential to be used as a feedstock for biodiesel, bio-
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lubricant production and so on.
Acknowledgement
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This study was supported by Long-Term Research Grant Scheme (600-RMI/LRGS 5/3) by
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Ministry of Education Malaysia.
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Fig. 1: The step and temperature variation of HYSASE consists of (a) water flooding, (b) steam
injection, (c) steam soaking and (d) product draining
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Fig. 2: Triglyceride detection on EFB spikelet (a) cut by a transversal (inner part) and (b) on the
surface layer. The intensive glow indicates the oil detection.
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Fig. 3: Structure and surface of EFB spikelet using SEM (5.0 Kv: 700x magnification) (a) end of
inner EFB spikelet fiber (b) inner EFB spikelet and (c) surface of the EFB spikelet
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Fig. 4: Oil analysis by gravimetric method to compare the performance of different oil removal
processes (1st, 2nd, 3rd, 4th and 5th bars represent for 1st, 2nd, 3rd, 4th cycle and total cycles,
respectively)
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Fig. 5: Oil detection on the EFB spikelet (a) surface layer after steam process (b) inner part after
steam process (c) surface layer after HYSASE and (d) inner part after HYSASE. The intensive
glow indicates the triglyceride detection.
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Fig. 6: Oil content of inner and outer layer of EFB spikelet before and after oil removal using
saturated steam and HYSASE
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Fig. 7: Comparison of oil removal using different size of EFB spikelet after two cycles of
HYSASE.
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Table 1: Analysis of oil quality and parameter that obtained by pressed and shredded EFB,
HYSASE, and fresh CPO from the mill.
Oil Samples
Parameter
Parameter
t
Range for CPOa Shredded and
ip
HYSASE Palm oil mill
pressed EFB
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palmitic acid) 5.0 max 11.02 0.96 10.51 0.48 4.56 0.09
DOBI (%)
an
2.20 min 1.63 0.03 1.48 0.06 2.26 0.07
M
Carotene Total as -
carotene (mg.kg-1) 474 689 397.28 4.59 427.90 0.60 482.71 51.77
ed
a
(Sue and Pantzari, 2009) [23]
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