Industrial Crops and Products 54 (2014) 291295

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Industrial Crops and Products

journal homepage: www.elsevier.com/locate/indcrop

Optimizing the parameters in durian skin ber reinforced

polypropylene composites by response surface methodology
N. Nur Aimi a , H. Anuar a, , M.R. Manshor a,b , W.B. Wan Nazri b , S.M. Sapuan c
a
Department of Manufacturing and Materials Engineering, Faculty of Engineering, International Islamic University Malaysia, Jalan Gombak, 53100 Kuala
Lumpur, Malaysia
b
Food Technology Research Center, Malaysian Agriculture Research and Development Institute (MARDI), 43400 Serdang, Malaysia
c
Department of Mechanical and Manufacturing Engineering, Universiti Putra Malaysia (UPM), 43400 Serdang, Selangor, Malaysia

a r t i c l e

i n f o

Article history:
Received 18 September 2013
Received in revised form 7 January 2014
Accepted 10 January 2014
Available online 20 February 2014
Keywords:
Durian skin ber
Impact property
Optimization
Response surface methodology (RSM)

a b s t r a c t
Awareness on the advantages of natural bers stimulates the interest of researchers to use them as
reinforcement in polymer composites for robust application. Therefore, investigation on optimizing the
impact property of durian skin ber (DSF) reinforced polypropylene (PP) composites was carried out
to determine the effect of DSF content, ber size and maleic anhydride polypropylene (MAPP) content.
Response surface methodology (RSM) was used in the design of experiments and in the analysis of results.
The optimized value for the maximum impact strength of PPDSF composite was found at 50 wt% DSF
content and ber size range of 250500 m with 0 wt% MAPP. The maximum impact property for PPDSF
composite was 10.66 kJ/m2 . From the analysis of variance (ANOVA), ber content signicantly affects the
strength of PPDSF composites, followed by the ber size and MAPP content. The P-value of the model
of experiment is less than 0.05 and the determination coefcient (R2 ) is nearly 1 which suggested that
the model is signicant and implies on the precision and processability in the production.
2014 Elsevier B.V. All rights reserved.

1. Introduction
Durio zibethinus Murray, or durian is the king of fruits and
one of the important economic crop for local farmers. Thailand,
Malaysia and Indonesia are the three main countries in ASEAN
region which commercially planted durians. The availability of
durian is inuenced by short harvested periods; within two to three
months. Durian skin ber (DSF) is a waste of durian fruit and in
one fruit about 6075% of DSF can be obtained. Fig. 1 illustrates
the thorny and tight characteristics of durian skin that makes the
skin worthless. Like other cellulose bers, durian skin consists of
lignin (15.45%), hemicelluloses (13.09%) and celluloses (60.45%)
(Charoenvai et al., 2005). Potential uses of DSF in particle board
production and bioabsorbant were progressively reported by few
researchers (Foo and Hameed, 2011; Khedari et al., 2003). These
byproducts can also be value-added into carboxyl methyl cellulose
(CMC), crystalline cellulose (CC), papers, animal feeds, charcoal and
many other benecial materials.
The advancement of composite materials by using durian skin
can be one of the most favourable methods for expanding and
value adding the usage of agricultural wastes since there is no specic utilization for durian wastes which include its skin and seed

Corresponding author. Tel.: +60361965752; fax: +60361964477.

E-mail address: hazleen@iium.edu.my (H. Anuar).
0926-6690/$ see front matter 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.indcrop.2014.01.016

(Manshor et al., 2012). Even though DSF is a new source of natural ber, it is however expected that DSF will be great potential in
future specically for one time used application such as packaging.
Like other natural bre, DSF is renewable, biodegradable and cheap
thus suitable for packaging such as in food packaging application.
This effort will subsequently reduce the environmental pollution
by decreasing the number of organic trashes.
Optimization properties for any industrial production using
classical method may lead to the change of independent variables,
simultaneously keeping the other variables constant (Raissi and
Farsani, 2009). It results in more time consuming and ineffective in
nding the optimum parameter particularly when it comes to the
interactions of each variable. This weakness can be solved by means
of response surface methodology (RSM). RSM has the ability to evaluate the relationship between the responses and the independent
variables as well as to dene the inuence of independent variables
on the responses either by each single variable or via combination
in the process (Zafari et al., 2013). Number of planned experiments
can also be reduced by using RSM as compared to the conventional
method.
To the best of authors knowledge, there is no paper reported on
the factors that determine the impact properties of bre reinforced
composites in open literature. Therefore, the objective of this paper
is to study the effect of factors that determine the impact property
of the PPDSF composites. The factors involved are ber content,
ber size and coupling agent, and their interactions in composite

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Table 1
Parameters for experimental design.
Factor

Fiber content (wt%)

Fiber size (m)
MAPP content (wt%)

Level
Low (1)

Medium (0)

High (+1)

10
50100
0

30
100250
2.5

50
250500
5

polypropylene (Garkhail et al., 2003; Biagotti et al., 2003; Yang et al.,

2004; Arbelaiz et al., 2005; Faisal Amri et al., 2013; El-Sabbagh et al.,
2014). After completion of the mixing process, PPDSF composites
were injection moulded via BATTENFIELD HM 600/850 injection
moulding machine with pressure of 800 bar, cooling time of 20 s
and speed of 170 mm/s.
Fig. 1. Cross-section showing parts of durian fruit.

fabrication process. This paper also investigates the optimization

using response surface methodology (RSM) to quantify the effect
of main parameters and their interactions on impact property of
PPDSF composites.
2. Experimental
2.1. Materials
Durian skin waste was obtained from a local market. Durian
skins were washed thoroughly with tap water to remove any adhering particles and dust. The skins were then chopped, ground into
smaller size using crusher (HITOP, SY 20), and dried in an oven at
80 C for 12 h. Finally, DSF was screened through a stack of siever
ranging from 50 to 500 m. Polypropylene (PP) grade 6331 was
supplied by Titan Pro Polymers (M) Sdn. Bhd. with melt index of
14 g/10 min at 230 C, and density of 0.9 g/cm3 . Maleic anhydride
polypropylene (MAPP) was supplied by SigmaAldrich. The maleic
anhydride (MA) graft (%) was 1.2 and average molecular weight
(Mw ) was 9100.
2.2. Composites preparation
PPDSF composite was extruded using Haake 600P twin screw
extruder at 190 C with screw speed of 250 rpm. The composition of composite prepared was varied from 10 wt%, 30 wt% and
50 wt% of DSF content. The ber size ranges were from 50100 m,
100250 m and 250500 m. The amount of MAPP added was
0 wt%, 2.5 wt% and 5.0 wt%. The ranges of values selected were
based on previous reported studies on natural bre reinforced

2.3. Response surface methodology (RSM)

PP-DSF composite was prepared according to the experimental design. It was designed, analyzed and calculated using design
expert software 6.0 via RSM with three variables; ber content,
ber size and MAPP content and the response is impact property.
As three factors and three level of face centred cubic designed were
chosen, there will be 3 similar runs which is considered as centred point. Table 1 illustrates the range of variables from low (1),
medium (0) and high (+1). The experiment consisted of 17 runs with
an average of ve replicates for each. Statistical analysis of the process was performed to evaluate the analysis of variance (ANOVA)
and P-test.
2.4. Characterization of composites
Charpy impact test was conducted according to ASTM D256
to characterize the impact property of PPDSF composites. The
specimens were notched and tested using Dynisco Polymer Test;
Sismatic OP7 machine. The velocity and weight of the hammer were
3.67 m/s and 0.898 kg, respectively. Scanning electron microscope
(SEM, JEOL, JSM-5600) was used to observe the fracture surface
after the impact test for 50 wt% PP-DSF composite. The fracture ends
of the samples were mounted on an aluminium stub and coated
with a thin layer of gold to avoid electrostatic charging during
examination.
3. Results and discussion
Scanning electron micrographs in Fig. 2 illustrate the uneven
surface morphology of durian skin bres at micron and submicron
level. From Fig. 2(ab), brils are clearly seen which associated in

Fig. 2. SEM micrographs of durian skin bre.

N.N. Aimi et al. / Industrial Crops and Products 54 (2014) 291295

293

Table 2
Actual and predicted values of impact strength of PP-DSF composites.
Run

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17

Fiber content
(wt%)

30
50
30
10
30
10
50
30
10
10
50
50
30
30
10
50
30

Fiber size
(m)

100250
250500
100250
50100
100250
100250
100250
50100
50100
250500
50100
250500
250500
100250
250500
50100
100250

MAPP
content

Impact strength
(kJ/m2 )

(wt%)

Actual

Predicted

2.5
5
5
5
2.5
2.5
2.5
2.5
0
0
0
0
2.5
0
5
5
2.5

4.45
4.98
5.07
6.00
4.56
2.56
5.52
3.17
0.64
2.04
3.18
10.29
4.53
5.05
1.61
3.68
4.60

4.49
4.97
5.10
5.99
4.49
2.59
5.55
3.20
0.63
2.03
3.17
10.28
4.56
5.07
1.59
3.66
4.49

bundles form and the surface of the bre was smooth. The complex
structure of durian skin bre was due to the existence of cellulose,
hemicellulose and lignin.
Table 2 tabulates the impact strength of response surface model
tting which indicates the actual and predicted values obtained
from the experimental design. It can be seen in Table 2 that the optimum strength obtained is 10.29 kJ/m2 at 50 wt% DSF, at ber range
size of 250500 m without any coupling agent. The minimum
impact strength is however recorded in composite with 10 wt%
DSF, at ber size range of 50100 m and without the presence
of coupling agent. Impact strength of unreinforced polypropylene
measured was 1.86 kJ/m2 . This shows that DSF effectively reinforced PP matrix by almost 453%.
Based on Table 2, PPDSF composites are signicantly affected
by ber content and ber size. Even though there would be incompatibility between DSF and PP, impact test is a suddenly applied
high speed pendulum that requires the composite to resist fracture or impact loading and must be capable of being damaged
without undergoing complete failure (Folkes, 1982). Therefore,
there must be energy absorbing mechanisms presence in the reinforced composite. Folkes (1982) explained there are four ways
to lead to energy absorbing mechanism and controlled impact
strength. First, through utilization of tough matrices or rubber
modied polymers; second coat the bre with a layer of soft
coating; third through debonding and pullout the bres from
the matrix and fourth through weak interface between bre and
matrix. The use of tough matrices was supported by Biagiotti
et al. (2003) on ax bre reinforced PPEPDM composites who
reported that the impact energy of materials depends more on
the matrix composition than the bre percentage in the composites. Similarly, in elastomer-toughened polymer, the presence of
elastomer produces stress redistribution in the composite, causing micro cracking or crazing at many sites thereby resulting in
a more efcient energy dissipation mechanism (Canche-Escamilla
et al., 2002). Biagiotti et al. (2003) also reported that bres can
absorb impact energy through mechanical friction due to bre
pull-out and bre debonding that tends to stop the crack propagation.
In contrast to strength and stiffness behaviour, a reinforced
composite will sustain the deformation if the interface and wettability between the elements are good. To obtain good interface,
the effect of coupling agent or surface modication is very important as widely reported in open literature (El-Sabbagh, 2014; Nadir
Ayrilmis et al., 2013; Faisal Amri et al., 2013).

Fig. 3. SEM micrographs of PPDSF composites at 500 magnication (a) without

MAPP and (b) with MAPP.

Scanning electron micrographs of PPDSF composite at 50 wt%

DSF are shown in Fig. 3(a) and (b). Fig. 3(a) is without MAPP and
Fig. 3(b) is with the presence of MAPP. In Fig. 3(a), bre pullout,
bre debonding and bre fracture are clearly seen in the micrograph. This conrmed that the energy required was utilized to
debond, to pullout and to fracture the bres and hence increased
the toughness of PPDSF composite in the absence of MAPP. Meanwhile in Fig. 3(b), even though there is interaction between bre
and matrix, the energy absorbing mechanisms due to bre pullout
and bre fracture are still evidenced. Durian skin bre, a type of
natural bre is known to be incapable in dissipating stress through
shear yielding prior to fracture. This reduced the ability of reinforced composites to absorb energy during fracture propagation
(Abu Bakar et al., 2005).
Table 2 also shows higher impact strength was recorded for all
the composite systems regardless of the bre content, bre size or
MAPP content. This nding is contradicted to previously reported
researches (Yang et al., 2004). This could be due to the complex
structure of durian skin bre itself which composed of cellulose
(60.7%), hemicelluloses (22.1%) and lignin (17.2%). High cellulose
and hollocellulose contents are capable in reducing brittleness of
the lignocellulosic material (Meysam Zahedi et al., 2013). Therefore the incorporation of DSF increased the impact strength of PP
composites as can be seen in Table 2.
Fig. 3 SEM micrographs of PPDSF composites (a) without MAPP
and (b) with MAPP.
From the statistical analysis, the determination coefcient, R2
that tted the model is 0.99963; i.e. about 99.9% of the variability in the response. The adjusted determination is 0.999299 which
implies that the model is signicant with an adequate precision
of 221.3719 due to the noise. The closer the R2 value to 1, the
more signicant the model to predict the response (Wang et al.,
2008). The polynomial regression model which relates the impact
strength (response, Y) with all the variables (ber content (A), ber

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N.N. Aimi et al. / Industrial Crops and Products 54 (2014) 291295

Fig. 4. The 2-D contour plot of the response surface showing the effect of ber size
(m) vs. ber content (wt%) on the impact strength of the PPDSF composites.

Fig. 5. The 2-D contour plot of the response surface showing the effect of MAPP
content (wt%) with ber content (wt%) on the impact strength of the composites.

size (B) and MAPP content (C)) was calculated using design expert
and represented as Eq. (1).
Impact strength (Y ) = 4.497042 + 14.8A + 0.678B + 0.014C
0.42732A2 0.61732B2 + 0.592676C 2 + 1.425AB
1.2175AC 1.45BC

(1)

The probability P-value obtained from ANOVA is relatively low

(P model > F = 0.05) indicates that the model is signicant. Additionally, the signicance of the model is indicated by the non-signicant
value of the lack of t (LOF) test of 0.8514. The relatively lower value
of standard deviation (0.05) indicates better precision and reliability of the experiment (Saban Tanyildizi et al., 2005; Bangphan et al.,
2013). Table 3 also reveals the F-test and corresponding P-value
along with the estimated parameter. Among the three independent variables, the effect of MAPP is not signicant on the impact
strength of PP-DSF composite. Since the interaction between linear
and quadratic effects of ber content, ber size and MAPP content
is signicant, little variation of MAPP slightly affects the impact
strength of the composites. The 2-D contour plots of the response
surface for this model are presented in Figs. 46. Additionally, run
1, 5 and 17 are considered as centred-point of the experiment as
face centred design was selected.
The optimum values of the variables are the main aim using
response surface method. The graphical representation obtained
from the method depicted an innitive interaction between two

Fig. 6. The 2-D contour plot of the response surface showing the effect of ber size
(m) with MAPP content (wt%) on the impact strength of the composites.

test parameters with one parameter at constant. It also shows

whether the variables are independent or dependent to each other
to yield optimum response or vice versa (Myers and Montgomery,
2002). Additionally, smallest region in contour diagram indicates
the maximum predicted value with perfect interaction between
the variables (Myers et al., 2004). Perfect interaction between the

Table 3
ANOVA of response surface quadratic model for impact strength.
Source

Sum of squares

Degree of freedom

Mean square

F value

P-value (P model > F)

Model
A
B
C
A2
B2
C2
AB
AC
BC
Residual
Lack of t
Pure error
Cor total

73.68876
21.904
4.59684
0.00196
0.489246
1.021031
0.941125
16.245
11.85845
16.82
0.022618
0.010551
0.012067
73.71138

9
1
1
1
1
1
1
1
1
1
7
5
2
16

8.18764
21.904
4.59684
0.00196
0.489246
1.021031
0.941125
16.245
11.85845
16.82
0.003231
0.00211
0.333033

2534.021
6779.144
1422.692
0.606607
151.4183
316.0022
291.2719
5027.721
3670.112
3205.679

< 0.0001
< 0.0001
< 0.0001
0.4616
< 0.0001
< 0.0001
< 0.0001
< 0.0001
< 0.0001
< 0.0001

0.349755

0.8514

Standard deviation: 0.056843; R2 : 0.999693; Adj (R2 ): 0.999299; Adequate precision: 221.3719

Signicant

Not signicant

N.N. Aimi et al. / Industrial Crops and Products 54 (2014) 291295

predicted value and variable shows that there are only small
changes or none can give maximum results (Bangphan et al., 2013).
Fig. 4 shows that as the ber content and ber size increase, the
predicted impact strength is 6.07 kJ/m2 with constant content of
MAPP at 2.5 wt%. On the other hand, there was an increment in
impact strength as ber content and ber size increases (Figs. 56).
Both occurred at lower content of MAPP (01.25 wt%). However, the
curves suggested that as the MAPP was added the response did not
vary much as the MAPP was added (Figs. 45). Figs. 46 depicted
that the optimal response occurred when the predicted values of
ber content is between 30 to 50 wt%, ber range size from 250 to
500 m and MAPP content is 01.25 wt%.
4. Conclusions
The use of response surface methodology via experimental
design allowed the determination of optimum parameters for
impact strength of PPDSF composites. The determined optimum
parameters are ber content at 50 wt%, 250500 m DSF size and
0 wt% MAPP content. It can be concluded that bre content and
mesh size without MAPP signicantly affect the ability of PPDSF
composites to yield highest impact strength. The optimization of
those variables results in reduced cost of production, and time and
material savings.
Acknowledgements
The authors wish to thank the Ministry of Education Malaysia for
nancial support by awarding research grant Exploratory Research
Grant Scheme (ERGS12-022-0022) for the nancial support and
International Islamic University Malaysia and Universiti Putra
Malaysia for the facilities and equipment provided in making these
studies a success.
References
Arbelaiz, A., Fernandez, G., Ramos, J.A., Retegi, A., Llano-Ponte, Mondragon, I., 2005.
Mechanical properties of short ax ber bundle/polypropylene composites:
inuence of matrix/ber modication, ber content, water uptake and recycling.
Compos. Sci. Technol. 65, 15821592.
Bangphan, S., Bangphan, P., Boonkang, T., 2013. Implementation of response surface
methodology using in small brown rice peeling machine: Part I. World Acad. Sci.
Eng. Technol. 74, 611615.

295

Biagiotti, J., Lopez-Manchado, M.A., Arroyo, M., Kenny, J.M., 2003. Ternary
composites based on PP-EPDM blends reinforced with ax bers. Part
II: mechanical properties/morphology relationship. Polym. Eng. Sci. 43 (5),
10311043.
Canche-Escamilla, G., Rodriguez-Laviada, J., Cauich-Cupul, J.I., Mendizabal, E., Puig,
J.E., Herrera-Franco, P.J., 2002. Flexural, impact and compressive properties of a
rigid-thermoplastic matrix/cellulose ber reinforced composites. Compos. Part
(A): Appl. Sci. Manuf. 33, 539549.
Charoenvai, S., Khedari, J., Hirunlabh, J., Daguenet, M., Quenard, M., 2005. Impact
of rice husk ash on the performance of durian berbased construction
materials. In: 10th DBMC International Conference on Durability of Building Materials and Components, Lyon, France, Retrieved from http://www.
cstb.fr/leadmin/documents/publicationsScientiques/DOC00003448.pdf.
El-Sabbagh, A., 2014. Effect of coupling agent on natural bre in natural
bre/polypropylene composites on mechanical and thermal behaviour. Compos.
Part B-Eng. 57, 126135.
Amri, F., Husseinsyah, S., Hussin, K., 2013. Mechanical, morphological and thermal properties of chitosan lled polypropylene composites: the effect of binary
modifying agents. Compos. Part A-Appl. Sci. Manuf. 46, 8995.
Folkes, M.J., 1982. Short Fiber Reinforced Thermoplastics. John Wiley & Sons, Britain.
Foo, K.Y., Hameed, B.H., 2011. Transformation of durian biomass into highly
valuable end commodity: trends and opportunities. Biomass Bioenergy 35,
24702478.
Khedari, J., Charoenvai, S., Hirunlabh, J., 2003. New insulating particleboards from
durian peel and coconut coir. Build. Environ. 38, 435441.
Manshor, R.M., Anuar, H., Wan Nazri, W.B., Ahmad Fitrie, M.I., 2012. Preparation and
characterization of physical properties of durian skin bers biocomposite. Adv.
Mater. Res. 576, 212215.
Zahedi, M., Pirayesh, H., Khanjanzadeh, H., Tabar, M.M., 2013. Organo-modied
montmorillonite reinforced walnut shell/polypropylene composites. Mater. Des.
51, 803809.
Myers, R.H., Montgomery, D.C., 2002. Response Surface Methodology. Wiley, New
York.
Myers, R.H., Montgomery, D.C., Vining, G.G., Borror, C.M., Kowalski, S.M., 2004.
Response surface methodology: a retrospective and literature survey. J. Qual.
Technol. 36, 5377.
Ayrilmis, N., Kaymakci, A., Ozdemir, F., 2013. Physical, mechanical and thermal properties of polypropylene composites lled with walnut shell our. J. Ind. Eng.
Chem. 19, 908914.
Raissi, S.R., Farsani, E., 2009. Statistical process optimization through multi-response
surface methodology. World Acad. Sci. Eng. Technol. 51, 267271.
Saban Tanyildizi, M., Ozer, D., Elibol, M., 2005. Optimization of a-amylase production by Bacillus sp. using response surface methodology. Process Biochem. 40,
22912296.
Wang, Y.H., Feng, J.T., Zhang, Q., Zhan, X., 2008. Optimization of fermentation condition for antibiotic production by Xenorhabdus nematophila with response surface
methodology. J. Appl. Microbiol. 104, 735744.
Yang, H.-S., Kim, H.-J., Jungil Son Park, H.-J., Lee, B.-J., Hwang, T.-S., 2004. Rice-husk
our lled polypropylene composites; mechanical and morphological study.
Compos. Struct. 63, 305312.
Zafari, A., Kianmehr, M.H., Abdolahzadeh, R., 2013. Modeling the effect of extrusion
parameters on density of biomass pellet using articial neural network. Int. J.
Recycling Org. Waste Agric. 2 (9), 111.