Journal of Natural Fibers

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Extraction and Characterization of Natural Fibers

from Citrullus lanatus Climber

Anish Khan, R Vijay, D Lenin Singaravelu, M R Sanjay, Suchart Siengchin,

Mohammad Jawaid, Khalid A. Alamry & Abdullah M. Asiri

To cite this article: Anish Khan, R Vijay, D Lenin Singaravelu, M R Sanjay, Suchart
Siengchin, Mohammad Jawaid, Khalid A. Alamry & Abdullah M. Asiri (2020): Extraction and
Characterization of Natural Fibers from Citrullus�lanatus Climber, Journal of Natural Fibers, DOI:
10.1080/15440478.2020.1758281

To link to this article: https://doi.org/10.1080/15440478.2020.1758281

Published online: 05 May 2020.

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JOURNAL OF NATURAL FIBERS
https://doi.org/10.1080/15440478.2020.1758281

Extraction and Characterization of Natural Fibers from Citrullus

lanatus Climber
Anish Khan a,b, R Vijayc, D Lenin Singaraveluc, M R Sanjay d, Suchart Siengchin d
,
Mohammad Jawaide, Khalid A. Alamrya,b, and Abdullah M. Asiria,b
a
Chemistry Department, Faculty of Science, King Abdulaziz University, Jeddah, Saudi Arabia; bCenter of Excellence
for Advanced Materials Research, King Abdulaziz University, Jeddah, Saudi Arabia; cDepartment of Production
Engineering, National Institute of Technology, Tiruchirappalli, India; dNatural Composites Research Group Lab, King
Mongkut’s University of Technology North Bangkok, Bangsue, Bangkok, Thailand; eDepartment of Biocomposite
Technology, Institute of Tropical Forestry and Forest Products, Universiti Putra Malaysia, Serdang, Malaysia

ABSTRACT KEYWORDS
The growing environmental awareness toward the replacement of non- Citrullus lanatus climber
biodegradable materials with biodegradable materials has led many research- fibers; natural fiber; X-ray
diffraction (XRD); scanning
ers for looking at many bio-based materials to suit various applications. This Electron Microscope (SEM)
study objective to evaluate the morphology and properties of fibers extracted
from Citrullus lanatus climber. The physical-chemical, thermal, mechanical, 关键词
crystalline, morphological characteristics of Citrullus lanatus climber fibers 瓜蒌攀缘纤维; 天然纤维;
were examined by Fourier transform-infrared spectroscopy (FTIR), thermogra- X射线衍射(XRD); 扫描电子
vimetric analysis (TGA), single fiber tension test, X-ray diffraction (XRD), and 显微镜(SEM)
scanning electron microscope (SEM). The test results showed cellulose content
(53.7 wt. %), density (1227 kg/m3), crystallinity index (33.33%) which prove that
Citrullus lanatus climber fibers can be used as reinforcement for light-weight
medium load applications.

文摘
随着环境保护意识的增强，以生物可降解材料代替不可降解材料，许多研
究人员开始寻找适合各种应用的生物基材料. 摘要本研究旨在探讨攀枝花瓜
纤维的形态和性质. 摘要采用傅里叶变换红外光谱(FTIR)、热重分析(TGA)、
单纤维拉伸试验、x射线衍射(XRD)、扫描电镜(SEM)等手段，研究了瓜氨酸
攀缘纤维的物理化学、热、力学、结晶和形态特征. 试验结果表明，纤维含
量(53.7 wt. %)、密度 (1227 kg/m3), 结晶度指数(33.33%)均可作为轻质中载应
用的增强材料.

Introduction
The current growth in environmental awareness has generated a growing interest in the use of
natural fibers instead of synthetic fibers (especially glass) as alternative reinforcement materials for
polymer composites (Ridzuan et al. 2016; Sanjay et al. 2018). Natural fibers have been widely used in
several applications, including composites, paper and fiberboards, textiles, and others. The extraction
technique depends mainly on the plant-part where the fibers are located such as stem (alfa, flax,
hemp, jute, and kenaf), a fruit (cotton, oil palm empty fruit bunches, and coir), and leaf (agave,
abaca, henequen, banana, and sisal) (Madhu et al. 2018; Vijay et al. 2019). In recent times, many new
fiber sources like Acacia leucophloea (Arthanarieswaran, Kumaravel, and Saravanakumar 2015),
Schumannianthus dichotomus (Barbhuiya and Ismail 2016), LygeumspartumL. (Belouadah, Ati, and
Rokbi 2015), Musa paradisiaca (Cadena Ch et al. 2017), Napier grass (Kommula et al. 2013) were

CONTACT M R Sanjay mcemrs@gmail.com Natural Composites Research Group Lab, King Mongkut’s University of
Technology North Bangkok, Bangsue, Bangkok, Thailand
© 2020 Taylor & Francis
2 A. KHAN ET AL.

Table 1. Physical and chemical properties of Citrullus lanatusclimber fibers.

Diameter (µm) Density (kg/m3) Cellulose (%) Hemicellulose (%) Lignin (%) Wax (%) Moisture (%) Ash (%)
210 ± 4.85 1227 ± 3.71 53.7 12.5 10.1 3.2 14 2.17

identified and characterized. Results of the investigation validate that these fibers are capable of
presenting similar characteristics as of conventional natural fibers such as abaca, bamboo, coir, flax,
jute, sisal, etc. (Indran, Raj, and Sreenivasan 2014; Maache et al. 2017), Citrullus lanatus is a species
of the Cucurbitaceae family, a flowering plant similar to a vine (scrambler and trailer) native to West
Africa. It is cultivated for its fruit. The subdivision of this species into two varieties, watermelons and
citrus melons, originated with the erroneous synonymization of Citrullus lanatus (Adebayo et al.
2014; Deshmukh, Jain, and Tambe 2015). The climbers are abundant source in the Southern parts of
Asia. The climbers mostly get discarded as waste after harvesting of fruit or get dried, in that way it is
a real potential. The cultivation of this climber for its fruit is around 118.4 million tons in the World
in 2017 as per FAOSTAT of the United Nations.
The objective of this research is to introduce a new fiber extracted from Citrullus lanatusclimber
fibers for which the physical-chemical characterization works have been carried out, to lay the
foundations for future research related to the development of this fiber as potential reinforcement in
bio-composite materials. This natural fiber is proposed for the first time to be used as a potential
reinforcement in bio-composite materials. For this purpose, the morphological, thermal, mechanical,
crystalline, and physicochemical characteristics of the Citrullus lanatusclimber fibers were examined
by scanning electron microscope (SEM), thermogravimetric analysis (TGA), single fiber tension test,
X-ray Diffraction (XRD), and Fourier transform-infrared spectroscopy (FTIR).

Materials and methods

Extraction of fibers
The fibers were obtained from the stem of Citrullus lanatus climber. Initially, the stem was soaked in
the water for 24 hours. Then, the soaked stem was fed into the manually operated retting machine
were fibers are produced. These fibers were again cleaned with distilled water to remove the adhered
dirt. Then, the fibers were dried in the hot sun for 5 days to remove the moisture.

Physical and chemical analysis

The objective of this analysis was to determine the chemical composition of the Citrullus lanatu-
sclimber fibers in terms of cellulose, lignin, wax, moisture, and ash content and physical properties
such as the density and diameter of the Citrullus lanatusclimber fibers. The cellulose content was
measured according to the method of Kurschner and Hoffer. The lignin content was determined
according to the APPITA P11 s-78 method. The ash content was analyzed according to the ASTM
E1755-01 method and the moisture content was determined with the help of an electronic moisture
analyzer (Sartorious, model MA45). The wax content of the Citrullus lanatusclimber fibers was
determined using the method developed by Conrad method. The density of the Citrullus lanatu-
sclimber fibers was evaluated using the Mettler Toledo xsz05 balance method. The digital micro-
meter used to measure the diameter of the fiber (Sanjay et al. 2019).

Morphological analysis
The surface morphology and cross-section of the Citrullus lanatusclimber fibers were studied using
a scanning electron microscope (SEM). The images were captured using Tescan VEGA 3LMU of the
Czech Republic in a high vacuum and low-pressure environment.
 JOURNAL OF NATURAL FIBERS 3

Fourier transform-infrared spectroscopy (FTIR) analysis

The functional group components present in the Citrullus lanatusclimber fiber were identified using
FTIR analysis. The analysis was carried out using Perkin Elmer/Spectrum 2 (Diamond UTAR). The
powdered Citrullus lanatusclimber fiber samples were placed over potassium bromide pellets, and
the infrared spectrums were recorded from the range of 4000 to 400 cm−1 with a resolution of 2 cm−1
signal to noise ratio.

X-ray diffraction (XRD) analysis

The crystallinity index of the Citrullus lanatusclimber fiber was measured using X-Ray diffraction
test. The samples were tested in X-Pert Pro diffractometer. It produces monochromatic radiation of
CuKα with a wavelength of 0.154 nm. It was recorded for 2θ values ranging from 10º to 80º.
Crystallinity index is calculated using equation (1)
H21:52  H16:18
CI ¼ (1)
H21:52
The crystal size calculated using equation (2)
Kλ
CS ¼ (2)
βCosθ
where Scherrer’s constant is given by K = 0.89. Here wavelength is denoted by λ and β denotes the
peaks full width at half-maximum

Thermal analysis
The thermal stability of the Citrullus lanatusclimber fiber was measured using thermogravimetric
analysis (TGA) (Perkin Elmer/TGA4000). Six milligrams of powdered Citrullus lanatusclimber fiber
samples were placed over an alumina crucible in the furnace with a controlled environment of the
nitrogen flow rate of 20 ml/min. The temperature ranges from room temperature to 600°C. The
heating temperature rate was 10°C per minute.

Single fiber tension test

Instron universal testing machine was used to measure the ultimate tensile strength of Citrullus
lanatusclimber fiber as per ASTM D3379. Testing was performed at a crosshead speed of 1 mm/
min for 50 mm gauge length. Twenty samples were tested and more consistent results were
reported.

Results and discussions

Physical and chemical analysis
Table 1 provides physical and chemical properties of Citrullus lanatusclimber fibers. The chemical
composition of Citrullus lanatus climber fibers shows a cellulose content of 53.7% and 12.5% of hemi-
cellulose together with other non-cellulosic compounds such as lignin (10.1%) and wax up to 3.2%. As
cellulose is the key structural element to provide resistance to cell walls, a moderate concentration of
cellulose (53.7%) helps to improve fiber resistance. However, the lower composition of hemicellulose
(12.5%) disintegrates the fibers into fibrils by loosening the bond between the cellulose molecules. The
content of lignin (10.1) has a notable influence on the hydrophilic nature of the fiber. Similarly, the wax
content in the fiber (3.2%) governs the interfacial union of natural fibers and makes their surface smoother.
It has the highest moisture content (14%), which may be due to the planting condition. Citrullus lanatus
4 A. KHAN ET AL.

Figure 1. (a) Photograph showing Citrullus lanatus climber and the part from which fiber is extracted; (b) SEM image of Citrullus
lanatus climber fiber surface; (c) SEM image of Citrullus lanatus climber fiber cross-section.

Figure 2. FTIR spectrum of Citrullus lanatusclimber fiber.

 JOURNAL OF NATURAL FIBERS 5

climber fibers contain the lowest ash content (2.17%), which increases fire resistance characteristics. The
density of the Citrullus lanatus climber fibers was 1,227 ± 3.71 kg/m3, which is significantly lower compared
to the ramie, sisal, cotton, linen, and hemp fibers. Low density improves light material for engineering
applications (Madhu et al. 2018). The diameters of Citrullus lanatus climber fibers are 210 ± 4.85 µm, which
is almost the same as other natural fibers (Sanjay et al. 2019; Kathirselvam et al. 2019).

Morphological analysis
Figure 1a shows the photograph of the Citrullus lanatus climber and the part from which fiber is
extracted. The SEM micrograph in Figure 1b shows the morphology of Citrullus lanatusclimber fiber
(elemental fiber). It shows a suitable cellulosic fiber with rough surface for good bonding with the
matrix polymer. The micrograph also shows that the small impurities are found on the surface.
Figure 1c shows the cross-section of Citrullus lanatus climber fiber, in which the cell walls are clearly
visible due to the presence of amorphous constituents like hemicellulose, lignin, and wax that aids in
the formation of such hollow structure. This type of behavior was seen in the Tridax procumbens
(Vijay et al. 2019)

FTIR analysis
The FTIR analysis is carried out to validate the chemical structures of the Citrullus lanatus climber
fibers. The composition changes examined for Citrullus lanatus climber fibers by FTIR analysis are
shown in Figure 2. This analysis identifies that the various significant changes are related to the
maximum intensities in the region of 3424, 2928, 2825, 1743, 1621, and 1018 cm−1. The peak at
3424 cm−1 reached as a result of the O–H stretching vibrations of the hydroxyl groups bound by
hydrogen from the cellulose. The maximum concentration at 2928 cm−1 has resulted in
a C-H stretch vibration in cellulose and hemicelluloses. The band at 2825 cm−1 is reached due
to the symmetrical stretching of methylene (groups –CH2). The maximum concentration at
1743 cm−1 is assigned to the C=O group of the stretching group in hemicelluloses. A strong
water absorption peak of approximately 1621 cm−1 is attributed to the C–O carboxyl stretch and

Figure 3. X-ray diffractogram of Citrullus lanatusclimber fiber.

6 A. KHAN ET AL.

also indicates the appearance of acetyl group in hemicelluloses. The peak signals at 1018 cm−1
correspond to the symmetrical C–OH stretch of lignin. FTIR peaks confirm once again the
appearance of cellulose, hemicelluloses, and lignin in the climber fibers of Citrullus lanatus
climber fibers (Fiore, Valenza, and Di Bella 2011; Kumar et al. 2018; Porras, Maranon, and
Ashcroft 2015).

XRD analysis
The X-ray diffraction pattern of the Citrullus lanatus climber fibers is revealed in Figure 3. That
displays two diffraction peaks at 2θ = 16.18° (1 1 0) and 21.52° (2 0 0), which are outstandingly

Figure 4. TGA and DTG curves of Citrullus lanatusclimber fiber.

 JOURNAL OF NATURAL FIBERS 7

detected in most of the natural fibers (Madhu et al. 2018). The peak at 2θ = 15.46° indicates the
existence of amorphous constituents in Citrullus lanatus climber fibers. The peak at 2θ = 21.52°
denotes the crystalline nature of the fiber. The crystallinity index was estimated as 33.33%
(Hyness et al. 2018).

Thermal analysis
The thermal stability behavior of Citrullus lanatusclimber fibers was studied using TG and DTG
curves as demonstrated in Figure 4. Normally, two stages of degradation were detected during the
Citrullus lanatusclimber fibers thermal stability study. The initial degradation noticed at 82.2°C
between room temperature and 100°C could be due to the evaporation of moisture present in the
Citrullus lanatusclimber fibers. The second major degradation progressed from the temperature
region of 250–380°C in which a peak quite close to 300°C related to thermal depolymerization of
hemicellulose with 26.20% of mass loss was observed. A very prominent peak at 325°C showed
a major mass loss of about 48.52% due to the degradation of cellulose. However, the degradation of
the aromatic structure of lignin occurred slowly under the initial temperature up to 600°C
(Manimaran et al. 2016; Yao et al. 2008).

Single fiber tension properties

The tensile stress–strain curve for Citrullus lanatus climber fiber is given in Figure 5. The ultimate
tensile strength of Citrullus lanatus climber fiber is 38.1 ± 1.56 MPa. It is inferred from the graph
that there is a sudden failure which is due to the brittle nature of the fiber caused by the amorphous
constituents, namely, lignin in its composition. In general, these tensile strength are also dependent
on the morphological properties and the voids present that degrade the results. The obtained tensile
strength values are higher than Tridax procumbens (25.75 MPa), while it is lower than Cocos nucifera
(175 MPa) (Tomczak, Sydenstricker, and Satyanarayana 2007; Vijay et al. 2019).

Figure 5. Tensile stress–strain graph of Citrullus lanatus climber fiber.

8 A. KHAN ET AL.

Conclusions
In this study, the properties of a new natural fiber extracted from the Citrullus lanatus climber fibers
were examined and the following conclusions were obtained. The study of morphology by SEM
revealed that the cross-section of the fiber of the Citrullus lanatusclimber fibers had a hollow
structure while the surface showed rough nature, which would greatly improve the bonding
mechanism in the manufacture of biocomposites. The peaks of the FTIR spectrum obtained for
the Citrullus lanatusclimber fiber were analyzed. The XRD analysis showed the semi-crystalline
nature of Citrullus lanatusclimber fiber which has a crystallinity index of 33.33%. The thermogravi-
metric analysis of Citrullus lanatusclimber fibers showed a thermal stability of up to 325°C. The
ultimate tensile strength of Citrullus lanatus climber fiber was 38.1 ± 1.56 MPa confirming the
possibility of its use as a reinforcement for light-weight medium load applications.

Funding
This project was funded by the Deanship of Scientific Research (DSR) at King Abdulaziz University, Jeddah, under
grant no. KEP-8-130-40. The authors, therefore, acknowledge with thanks to DSR for technical and financial support.

ORCID
Anish Khan http://orcid.org/0000-0002-3806-5956
M R Sanjay http://orcid.org/0000-0001-8745-9532
Suchart Siengchin http://orcid.org/0000-0002-6635-5686

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