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Article history: The objective of this study was to investigate the effect of different extraction methods on the fiber
Received 6 September 2012 morphology, density, chemical composition and tensile strength of kenaf bast fiber. Kena fbast fibers
Received in revised form 5 December 2012 were extracted using different methods (crude, decorticated, water retted, 5% sodium hydroxide retted
Accepted 16 December 2012
and 5% benzoate retted) and their physicochemical characteristics were investigated. The morphological
characteristics showed a significantly reduced lumen diameter and increased cell wall thickness after
Keywords:
treated with NaOH at 5%. On the other hand, increased lumen diameter and a decreased cell wall thickness
Kenaf
were observed with the decorticated and water retted bast fibers. A slight increase in fiber density was
Decortications
Density
observed for NaOH and benzoate retted bast fibers indicating cell wall densification. Interestingly, the
Fiber morphology extraction methods used in this study produced bast fibers with high cellulose content and low sugar
Chemical constituent and starch due to the removal of wax, oil, pectin and hemicelluloses. Regarding the tensile strength, the
Tensile strength water retted bast fibers showed highest tensile strength (426.05 MPa), while there was one no difference
between decorticated and NaOH retted fibers (386.83 and 393.03 MPa, respectively).
© 2012 Elsevier B.V. All rights reserved.
0926-6690/$ – see front matter © 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.indcrop.2012.12.015
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118 B.A. Amel et al. / Industrial Crops and Products 46 (2013) 117–123
big quantity of fiber with high quality (Liu, 2005; Zhang, 2003;
Abdolreza et al., 1997). From SEM analysis it was also reported that
3% NaOH was ineffective concentration for removing the impuri-
ties from kenf bast fibers surface, while 6% NaOH was the optimum
concentration for the chemical treatment to remove the impurities
(Mwaikambo and Ansell, 2002; Edeerozey et al., 2007). Jinshu et al.
(2011), Keshk et al. (2006), Song and Obendorf (2006) have reported
that high cellulose content can be obtained from kenaf bast fiber
using water and NaOH retting processes. It was also reported that
the cross-sectional shape of the kenaf fiber varied widely from Fig. 1. Fiber bundle diameter.
noncircular shapes such as a kidney bean shape for cotton to the
reasonably circular one for wool (Goswani et al., 2004).
were measured by using 70 mm fiber bundles length. The densities
However, there have been many studies on kenaf and very
of kenaf bast fiber bundles were measured by using Archimedes
limited information is available on the effect of extraction meth-
Method (ASTM-D3800-99, 2005). Based on the standard, the
ods on the properties of kenaf bast fiber. Therefore, the purpose of
method involves immersion of a known weight of fibers into a liq-
the current research is to investigate the effect of different extrac-
uid of lower density than the fiber. Canola oil with a density of about
tion methods, i.e. water retting, chemical retting and mechanical
0.915 g/cm3 was used as a liquid. Prior to testing, the kenaf fibers
decortications on the characteristics of kenaf bast fibers. These
were conditioned in an oven at 60 ◦ C until the moisture content
characteristics include changes in fibers morphology such as fiber
was reduced to below 5%.
length, diameter, lumen diameter, and cell wall thickness, density,
chemical composition and tensile strength.
2.3. Chemical analyses
2. Materials and methods
From each extraction methods, about 2 kg of kenaf bast fibers
Kenaf, sp.V36, was collected from Taman Pertanian Universiti was used to investigate the chemical composition. Five samples
(TPU) Malaysia. Stalks were harvested at the age of 3.5 month. A from each extraction methods were used in the study. The chemical
total of five hundred kenaf stems were used in this study. The chem- composition (alcohol acetone solubility, holocellulose, ␣-cellulose
icals (methanol, ethyl alcohol, acetone, acetic acid, sodium chlorite, and lignin) of the kenaf bast fibers was determined according to
sodium hydroxide, sodium benzoate, sulfuric acid, barium hydrox- the standard Technical Association of the Pulp and Paper Indus-
ide, barium sulphate, anthrone, glucose, fructose, potato starch, try (TAPPI) T 204 os-76, Wise et al., 1946, T 203 os-76 and T 222
10% potassium iodide, 0.01 N potassium iodate and perchloric acid) os-76, respectively. The alcohol acetone solubility was determined
used in this study were of analytical grade and obtained from Fisher using alcohol acetone solution to extract the samples. The holo-
Scientific Malaysia. cellulose content (␣-cellulose + hemicelluloses) of the kenaf bast
The kenaf samples were divided into five groups and treated fibers was determined by treating the fibers with a mixture of acetic
with different extraction methods. Except the decorticated bast acid and sodium chlorite solutions. The ␣-cellulose content of the
fibers, all other samples were peeled manually to separate the bast fibers was then determined by further treating the holocellulose
and core. The samples were kept in ambient conditions in the room with 17.5% and 8.3% sodium hydroxide to remove the hemicellu-
temperature of 25 ◦ C and 50% relative humidity for 3 weeks before loses. The lignin content of the kenaf bast fibers was determined by
extraction process was carried out in Table 1. treating them with a sulfuric acid solution. The method developed
by Yemm and Willis (1954) was applied to determine the sugar
2.1. Analysis for fiber surface morphology content. Also total starch was investigated using Humphreys and
Kelly (1961) method.
About 30 g of kenaf bast fiber was sampled from each extraction
method used in the study. Hitachi H-7100 transmission electron 2.4. Tensile properties
microscope (TEM) was employed to examine the morphology of
kenaf bast fibers, i.e. fiber length, cell diameter, lumen diameter The tensile strength test was conducted according to ASTM
and cell wall thickness. The samples were cut into 1 mm thick- D885 (1995) using an Instron Universal Testing Machine (Instron:
ness and placed into beam capsules. Then the cross sections were Model 3365) with cell load capacity 5 kN, at a crosshead speed of
further cut into 1 m thickness using glass knife and ultra micro- 1 mm/min. The standard specifies that the gauge should be three
tome. Finally ultra-thin sections (0.1 m) were prepared using ultra times the fiber length (in this case 90 mm – 3 mm × 30 mm), but
microtome, stained with 2% uranyl acetate and viewed under TEM. after it is glued to a cardboard on each end for better gripping, the
A total of 200 individual fibers were taken from different extraction effective gauge length was 60 mm. In this study, 30 g of kenaf bast
methods. Forty individual fibers from each extraction method were fiber bundles in eight replicates was used as representatives for
examined and the results were expressed as a mean value for each each extraction methods. The fiber diameter was obtained using an
treatment. A Leo 1455 variable pressure scanning electron micro- optical microscope with camera (image analyzer) at 300× magni-
scope (SEM) was also used to examine the effect of the extraction fication. The fiber bundle diameter was calculated as an average of
methods on the surface morphology of kenaf bast fibers. The accel- three readings (Fig. 1). Using the calculated fiber bundle diameter,
eration voltage was set to 20 kV and all samples were cut into 2 mm the tensile strength was calculated.
length and 1 mm thickness, stacked onto an aluminum stub; sam-
ples were coated with gold, and finally they were viewed under the 2.5. Statistical analysis
SEM.
The data were statistically analyzed using Statistical Analysis
2.2. Fiber density System (SAS) software, Version 9. Analysis of Variance (ANOVA)
was used to examine the effects of extraction methods on some
In this study 40 g kenaf bast fibers and three replicates were used properties of kenaf bast fibers. Least Significant Difference (LSD)
from each extraction methods. The densities of kenaf bast fibers method was used for further evaluation of the effect of extraction
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B.A. Amel et al. / Industrial Crops and Products 46 (2013) 117–123 119
Table 1
Fiber extraction procedures of kenaf using different medium.a
Type Procedure
Crude bast fiber Peeling manually (control) – aggregates of fibers still intact in sheet form.
Decorticated bast fiber Separation of kenaf bast fibers was done using a decorticator machine.
Water retted bast fiber 8 kg kenaf bast fibers were soaked in 40 L water (1:5) for 24 days. The water was changed every 12 days after 24 days
the stalks were washed with water, air driedb and combed.
NaOH retted bast fiber For each chemical extraction methods about 8 kg of kenaf bast fibers were soaked in 40 L
Benzoate retted bast fiber solutionc (1:5) for 24 days, the stalks were washed with water, air driedb , and combed
Note:
a
Mode of fiber production.
b
12% moisture content.
c
5% (by weight) for each (NaOH and benzoate).
methods. LSD ranks the means and calculates the minimum value 3.1. Effect of extraction methods on the morphology of kenaf bast
to be significantly different with each other at p ≤ 0.05. Means fibers
followed by the same letter a, b, c, . . ., etc. are not significantly
different. Table 3 shows the effect of extraction method on the fiber mor-
phology. It was generally found that the fiber length, diameter
and lumen diameter decreased as more severe treatments were
3. Result and discussion used. Compared to fibers obtained from crude bast fiber, treatment
using 5% NaOH seemed to be the most severe with fiber length
The analysis of variance for the fiber morphology, density, chem- reduced from 3228 m to 1757 m similarly with diameter and
ical analyses and tensile strength of different extraction methods, lumen diameter. Nevertheless, the cell wall thickness increased
i.e. crude, decorticated, water-, NaOH- and benzoate retted from significantly. The reduction in both length and diameter may be
kenaf bast fibers are presented in Table 2. Based on the test results; attributed to the reduction in the number of elementary fibers in
it is obvious that the extraction methods were significantly (at the fiber bundles after being treated with 5% NaOH. A mild alkali
p ≤ 0.01) influenced the fiber morphology, i.e. fiber length, diam- hydrolysis may have degraded the middle lamella thus separating
eter, lumen diameter and cell wall thickness, density, chemical the elementary fibers from the bundles. Similar finding was pre-
analyses, i.e. alcohol acetone solubility, ␣-cellulose, lignin, starch viously reported by Bos (2004). The cell wall, on the other hand,
and sugar and tensile strength of the kenaf bast fiber. However the experienced swelling as a result of reduction in crystalline region
effect of extraction methods on the holocellulose was insignificant. (increase in amorphous region) after being treated with alkali. The
Fig. 2. TEM micrographs of the cross sections of kenaf bast fibers: (A) crude bast fiber; (B) decorticated bast fiber; (C) water retted bast fiber; (D) benzoate retted bast fiber
and (E) NaOH retted bast fiber (magnification at 4000×).
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Table 2
Summary of ANOVA for the effect of extraction methods on the morphology, density, chemical analyses and tensile strength of kenaf bast fiber bundle.
Parameters DF p value
Fiber Fiber Lumen Cell wall Alcohol Holo-cellulose Cellulose Lignin Sugar Starch
length diameter diameter thickness Acetone
Extraction 4 <0.0001*** <0.0001*** <0.0001*** <0.0001*** <0.0001*** 0.8752, ns <0.0001*** <0.0001*** <0.0001*** <0.0001*** <0.0001*** <0.0001***
methods
Table 3
Effect of extraction method on fiber length, diameter, lumen diameter and cell wall thickness of kenaf bast fibers.a
Crude bast fiber 3228 a (2) 24.1 a (1.3) 13.4 a (1.03) 5.8 c (0.3)
Decorticated bast fiber 2315 b (1.5) 18.2 c (1.9) 8.9 b (0.44) 4.0 c (1.98)
Water retted bast fiber 3389 a (2) 17.4 cd (0.58) 9.6 b (0.49) 5.3 d (0.8)
5%Benzoate retted bast fiber 2225 b (1.2) 21.7 b (1.12) 7.7 c (0.4) 6.7 b(0.1)
5% NaOH retted bast fiber 1757 c (1) 16.1 d (0.7) 3.6 d (0.54) 7.3 a (0.2)
a
Values are average of 20 specimens; ( ) standard deviation.
b
Means followed by the same letters (a, b, c, d) in each column are not significantly different at p ≤ 0.05 according to Least Significant Difference (LSD) method.
increase in cell wall thickness is due to the presence of swollen treatments performed on kenaf bast fibers have modified the fibers
cellulose in the cell wall. surface where fine structural changes of the fibers were observed
There is no significant difference in the fiber length between on SEM micrographs. On the other hand, for water retted samples
crude fiber (3228 m) and water retted (3389 m). This finding is the lumen became larger and more rounded compared to the oth-
expected since water acts as a medium to better degrade pectinees ers. Similar results were reported by Munawar et al. (2006); they
materials and carbohydrates that bind the fiber together; there are found that all the cross-sectional shapes of single fibers provided
mild chemical reaction initiated by the microbe. Thus, the fibers were polygonal to round. Generally, the bundle shape, single fiber
experienced little degradation therefore resembled those of origi- shape, and the lumen diameter observed are different based on the
nal crude bast fibers. Both decorticated and benzoate retted fibers extraction methods. Except for NaOH retted fiber, all other types
are of similar quality. These results are similar to findings by Abdul of fiber exhibited noncircular shapes on the cross section of fiber
Khalil et al. (2010), who reported that bast fibers length of 3600 m bundles, very small lumen and densified cells (Fig. 3).
for crude bast fiber whilst, Ashori et al. (2006) reported an average
of 2480 m. 3.2. Effect of extraction methods on the density of kenaf bast
The average fiber diameter, lumen diameter and cell wall thick- fibers
ness of the crude kenaf bast fibers was observed 24.1, 13.4 and
5.8 m, respectively. However, there was no significant difference The density generally represents all the solid material as well
in the diameter between decorticated (18.2 m) and water retted as the pores within the fibers. Table 4 depicts the densities of
(17.4 m) as well as between water and NaOH (16.1 m) retted but kenaf bast fiber produced from different methods of extraction,
they are significantly different from each other and from benzoate i.e. crude, decorticated, water, NaOH and benzoate retted bast
retted (21.7 m). It was interestingly found that decortications pro- fibers. There is no significant difference between all extraction
cess degraded most fiber properties in particular cell wall thickness. methods. However, a positive slight change in fiber densities
Figs. 2 and 3 show the cross section micrographs on different was observed in the order: NaOH-retted > benzoate-retted > water-
extraction methods of kenaf bast fibers viewing under TEM and retted > decorticated > crude bast fibers. A positive change in fiber
SEM. It can be clearly seen that, the whole cross sections of kenaf densities normally signifies cell wall densification as a result of
bast fiber bundles after extraction methods are polygonal to cir-
cular. For the crude fibers in their original state, surface is filled Table 4
with impurities and the fibers are intact while for the decorticated Effect of extraction methods on the density (g/cm3 ) of kenaf bast fibers.
and benzoate retted fibers the lumen shape is similar to that of the
Extraction methods Density (g/cm3 )a Change in density (%)b
crude fibers and their surfaces are clean, Fig. 2. The presence of sur-
face impurities on the surface of kenaf bast fibers was very clear; Crude bast fiber 1.191 a 0
Decorticated bast fiber 1.193 a 0.17
except for the 5% NaOH retted bast fibers which showed smooth
Water retted bast fiber 1.195 a 0.34
surface compared to other kenaf bast fibers. These results indi- Benzoate retted bast fiber 1.195 a 0.34
cate that the extraction methods improve surface characteristics NaOH retted bast fiber 1.198 a 0.59
of the kenaf bast fibers as a result of removing natural and artifi- Kenaf bast fiberc
cial impurities, hence producing a smooth surface topography. This A. Untreated 1.193 0
B. Treated with 6% NaOH 1.222 2.4
result is in accordance with that found by Mohanty et al. (2006) who
reported that treating fibers with NaOH removes lignin, pectin, wax Note:
a
Means followed by the same letter (a) are not significantly different with each
substances, and natural oils that cover surface of the fiber cell wall.
other at p < 0.01 according to Least Significant Difference (LSD) method.
Morphological examinations carried out by Aziz and Ansell b
Change over crude bast fiber.
(2004) and Edeerozey et al. (2007) exposed that alkalization c
Aziz and Ansell (2004).
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B.A. Amel et al. / Industrial Crops and Products 46 (2013) 117–123 121
Fig. 3. SEM micrographs of the cross sections of different kenaf bast fibers: (A) crude bast fiber; (B) decorticated bast fiber; (C) water retted bast fiber; (D) benzoate retted
bast fiber (E) and NaOH retted bast fiber (magnification at 1000×).
removal of impurities (less dense fats and waxes) by alkali. A posi- have low lignin content (9.3–13.2%). The higher ␣-cellulose at 5%
tive change would signify cell wall leading to polymerization of the NaOH and water retted is probably due to removed pectin, wax and
cellulose molecule. Aziz and Ansell (2004) observed a small posi- part of hemicellulose. These are in line to some findings by Jinshu
tive change in fiber density for both hemp and kenaf fibers after 6% et al. (2011) and Keshk et al. (2006); they reported that high cel-
NaOH treatment, indicating a cell wall densification of their fibers. lulose content from kenaf bast fiber can be obtained when using
Sawpan et al. (2011) and Mwaikambo and Ansell (2006) also found water and NaOH retting process.
that the density of hemp fibers increased upon alkali treatment. Moreover, the total sugar percentage for crude, decorticated,
water retted, NaOH retted and benzoate retted bast fibers were
3.3. Chemical analyses 0.0038, 0.0035, 0.0033, 0.0037, and 0.0050%, respectively. The total
starch percentage for the respective kenaf bast fibers were 1.4769,
As shown in Table 5 the chemical composition is greatly affected
by extraction methods. All extraction methods namely crude,
Table 5
decorticated, water, NaOH, and benzoate retted fibers decreased Chemical analyses of the kenaf bast fiber.
alcohol acetone solubility whereas increased both ␣-cellulose and
Chemical Extraction methods
lignin. NaOH retted produced higher ␣-cellulose (73.89%) followed
constituenta
by water retted (72.68%), decorticated (70.89%), benzoate ret-
ted (68.94%) and crude (66.94%). However, the lignin contents Crude Decorticated Water NaOH Benzoate
increased from 9.87% to 11.43%, 13.93%, 14.55% and 13.07%. These Alcohol 2.26 a 1.55 b 0.66 c 0.48 c 0.58 c
changes can be attributed to the effects of retting process as well acetone
as to those of extracted by hand (crude). The increase in lignin is solubility
Holocellulose 81.55 a 80.15 a 80.94 a 77.06 a 79.55 a
expected to decrease wax, pectin and part of hemicelluloses. In
␣-Cellulose 66.94 e 70.89 c 72.68 b 73.89 a 68.94 d
addition the increase in cellulose observed in this study could be Lignin 9.87 c 11.43 bc 13.93 a 14.55 a 13.07 ab
attributed to the increase in lignin present in the primary wall and Sugar 0.0038 b 0.0035 c 0.0033 c 0.0037 b 0.0050 a
secondary wall mainly S1 and S2 layers thus increase in the pack- Starch 1.4759 a 0.6532 d 0.6514 d 0.8789 c 1.3226 b
ing order of the crystalline material. Previous study by Villar et al. a
At the same rows, chemical constituent mean with the same lower case letters
(2009) and Thi Bach et al. (2003) showed that the kenaf bast fiber (a, b, c, d) were not significantly different from each other (p < 0.01).
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122 B.A. Amel et al. / Industrial Crops and Products 46 (2013) 117–123
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