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Characterization of a new natural cellulosic fiber extracted from

Derris scandens stem

C. Ilaiya Perumal, R. Sarala

PII: S0141-8130(20)34718-8
DOI: https://doi.org/10.1016/j.ijbiomac.2020.10.086
Reference: BIOMAC 16976

To appear in: International Journal of Biological Macromolecules

Received date: 17 July 2020

Revised date: 10 October 2020
Accepted date: 12 October 2020

Please cite this article as: C.I. Perumal and R. Sarala, Characterization of a new natural
cellulosic fiber extracted from Derris scandens stem, International Journal of Biological
Macromolecules (2018), https://doi.org/10.1016/j.ijbiomac.2020.10.086

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© 2018 Published by Elsevier.

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Characterization of a new natural cellulosic fiber extracted from Derris scandens stem

C. Ilaiya Perumala,*, R. Saralab

a
Department of Mechanical Engineering, Alagappa Chettiar Government College of

Engineering and Technology, Karaikudi-630004,Sivaganga District, Tamil Nadu, India.

E-mail: ipdesign2012@gmail.com

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b
Department of Mechanical Engineering, Alagappa Chettiar Government College of

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Engineering and Technology, Karaikudi-630004,Sivaganga District, Tamil Nadu, India.
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E-mail: sarala.sutharson@gmail.com
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*Corresponding author: C. Ilaiya Perumal

E-mail: ipdesign2012@gmail.com
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Mobile No.: +91 9944837438

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Abstract

The present study aims to identify a potential substitute for the harmful synthetic fibers in the

field of polymer composites. With this objective, a comprehensive characterization of Derris

scandens stem fibers (DSSFs) were carried out. The presence of high strength gelatinous

fibers with a traditional hierarchical cell structure was found in the anatomical study. The

chemical compositional analysis estimated the cellulose, hemicellulose, and lignin contents of

63.3 wt. %, 11.6 wt. %, and 15.3 wt. %, respectively. Further analysis with XRD confirmed

the presence of crystalline cellulose having a size of 11.92 nm with a crystallinity index of

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58.15%. SEM and AFM studies show that these fibers are porous, and the average roughness

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is 105.95 nm. Single fiber tensile tests revealed that the DSSFs exhibited the mean Young’s
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modulus and tensile strength of 13.54 GPa and 633.87 MPa respectively. Furthermore, the
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extracted fibers were found to be thermally stable up to 230°C, as confirmed by

thermogravimetric analysis. The fibers extracted from the stem of medicinal plant Derris
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scandens have the properties comparable to that of existing natural fibers, thus, suggesting it
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to use as a highly promising reinforcing agent alternative to synthetic fibers in polymer

matrix composites.
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Keywords: Natural fiber; Fiber extraction; Mechanical properties.

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1. Introduction

Global warming, severe pollution and scarcity of natural resources are a great threat to the

future generation. One of the ways to curtail the destruction of our earth’s resources and the

atmosphere is to find an alternative bio-based material derived from a natural renewable

resource. In the recent decade, natural fiber reinforced polymer composites with high thermo-

mechanical properties are an attractive material thanks to their biodegradable nature,

lightweight, low cost, and ease of production [12, 9]. For the most engineering applications,

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polymers are toughened with high strength fibers, to form a composite material that typically

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consists of synthetic fibers like glass, aramid, kevlar & carbon, etc., [7,11,15]. The scope of
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composite materials in modern technology ranges from aircraft (fuel tanks, wings), naval
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(moderate load-bearing structures), automobiles (seat, dial and switch housing panels, clutch

plates, bumpers, headrests, fuel lines, door panel, upholstery, grills, and mats), sports
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equipment, liquid storage tanks, electronic, construction, food packaging and furniture
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industry [1,3,4,8,13,14]. Unprotected handling of synthetic fibers may instigate suffocation,

carcinogenic, pulmonary toxicity, lung cancer, cell mutagenicity, and oxidative DNA damage
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to plant workers [6,15,31,48]. To overcome the drawbacks of synthetic fibers, natural fibers
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offer promising alternative properties such as unharmful, low density, biodegradable, non-

pollutant, good thermo-mechanical property, abundant, renewable and economical [1, 2, 5,7,

8,14]. Natural fibers can be extracted from diverse vegetations like trees, climbers, vine, herb,

shrubs, and grasses, etc., and they are particularly extracted from the plant body parts like

root, stem, bark, flowers, seeds, leaves, fruits, stalks, petioles, fruit husks [7,8,11,46]. The

architecture of natural fibers is composed of lumen (core) along with its secondary wall,

primary wall, and middle lamella [1,25,36]. Chemically, the natural fibers consist of

cellulose, hemi-cellulose, lignin, wax, ash and traces of other soluble substances [3,12].
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Physical, chemical, and mechanical characteristics of the natural fibers differ from each other

due to various factors such as the chemical composition of constituents, matureness, parts of

the plant where the fiber is extracted, the region in which the vegetation cultivation,

micronutrients level of soil, environmental condition. [1,12,13]. The increasing disparity

between the current demand [5,12] and the cultivation rate of conventional fibers as Cotton,

Banana, Hemp, Jute, Flax, etc., [1,30] has provoked the spotting of new natural fibers. The

recent novel natural fibers are Aerial roots of banyan tree, Tridax procumbens, Calotropis

gigantea fruit bunch, Thespesia populnea barks, Kigelia africana, Root of ficus religiosa tree

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[32,6,8,36,48,45]. In this study, a new variety of natural fiber source extracted from Derris

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Scandens Stem (DSS) has been identified which may replace synthetic fibers in polymer
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reinforced composites. One of the main reasons that make DSSFs desirable is that the fiber
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handlers need not worry about the allergic problem because it is a non-toxic medicinal plant

and does not create any discomfort to humans [22]. So, there is no need to follow any safety
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precautions to handle the fibers. In this work, we aim to extract natural fibers from the stem
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of Derris scandens and investigate their properties to be used as reinforcement materials.

Various characteristics such as anatomy, morphology, physical, chemical, thermal, and

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mechanical properties of the extracted DSSFs were studied.

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2. Materials and methods

2.1 Derris scandens Plant

Derris scandens is a perennial woody twining climber (Fig. 1a) of the Fabaceae or

Leguminosae family, which flourishes in tropical regions of India and also available

abundantly in South Asian countries [20]. It is mostly climbing and supporting themselves by

twining into nearby trees found in forest area, futile lands, farming grounds, river basins, and

lakes and sometimes cultivated as an ornamental. Derris scandens plant is popularly known
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as Thekilan Kodi in the Tamil language. It has medicinal applications in Indian and Thai

traditional herbal medical field [20,21]. The matured DSS (Fig. 1a) were collected from

Amaravathiputhur village roadsides near Karaikudi, Sivaganga, Tamil Nadu, India during

December 2019.

2.2 Fiber Extraction

The Derris scandens stems were immersed in water for seven days for microbial degradation

(Fig. 1b) after the removal of dirt. This lesser immersion period preserves the water indirectly

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and reduces the expenditure for extraction. And then, the fibers were extracted from the stem

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by rough hands (Fig. 1c) without any special tool and dried under the hot sun for forty-eight
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hours to eliminate the moisture (Fig. 1d). The average length of the obtained dry fiber is more
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sufficient to make composites with different orientations and weaving (Unidirectional,

bidirectional, mated, random, etc.). DSS has rich fiber content and a worthy percentage of
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yield with lesser wastage. The resultant DSSFs extracted from the stems of Derris scandens is
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shown in Fig. 1e.

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Fig. 1. (a) Derris Scandens plant stem, insets - leaf and fruit (b) Water retting of DS chopped
stems (c) Peeling of fiber from stem (d) Drying by sunlight (e) Extracted DSSFs

2.3 Characterization of DSSFs

2.3.1. Anatomical study of DSS

The anatomical microstructure of DSS and its fibers were recorded with the aid of the Nikon

polarized microscope (Model: ECLIPSE LV100N POL). A fully-grown stem piece was

chopped and immersed in the Formaldehyde Alcohol Acetic Acid (FAA) solution (5 ml of

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CH2 (formaldehyde) + 5 ml of CH3COOH (glacial acetic acid) + 90 ml of 70% C2H5OH

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(ethyl alcohol)) for a day. The specimens were drained out with the C4H10O (tert-butyl
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alcohol) series and positioned in petroleum wax [44]. The samples were bifurcated using a
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rotary microtome of size up to 12 -10 µm. Then rooted to a glass slide and having tint with a

mixture of tolonium chloride, fast green, and aqueous iodine solution [23] for a high profile
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picture. The dimension of DSSFs cell geometry is measured by image processing software
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(ImageJ).

2.3.2. Physical Analysis

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Twenty-five single fibers were picked up for the trial and they were captured solitary to
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evaluate the diameter, the measurements were taken randomly in three distinct places of

every single fiber image with the aid of ImageJ software [23]. Pycnometer method for solids

was used to compute the density of DSSFs with toluene as an immersion liquid [17]. The

linear density (Denier) of DSSFs was calculated with ASTM D 1577-92 [24] by weight up to

100 single fibers with each length equal to 90 mm.

2.3.3. Single Fiber Tensile Test

DSSFs were selected in a random way for each gauge length (GL) groups (10, 20, 30, 40 &

50 mm), each group having 25 single fibers. Then each group was perused by A Zwick/Roell
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Z005 static tensile test machine to find out the mechanical capacity as per ASTM D 3822–07

standard [1]. The values have been statistically analyzed with two-parameter Weibull

distribution using the Minitab 16 software. The microfibril (α) angle of DSSFs was

deliberately using the following equation (1) [19].

∆𝐿
ε = 𝑙𝑛 (1 + 𝐿 ) = −ln⁡(𝑐𝑜𝑠𝛼) (1)
𝑂

Where ε - the global deformation (or) strain, α - the microfibril angle in degree, Lo - the

gauge length (mm), and ΔL - the elongation at break (mm).

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2.3.4. Chemical Composition

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The weight percentage of cellulose, hemicellulose, and lignin present in DSSFs was

determined [8] and the contribution of wax was estimated by typical practice [5]. The ash
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percentage was recorded as per the ASTME1755-61 procedures [8]. The DSSFs moisture
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content was predicted by moisture analyzer (MA45Sartorius) [26].
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2.3.5. X-Ray Diffraction studies

X-ray diffraction analysis was carried out on X’ Pert Pro–PAnalytic diffractometer (Mumbai
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India) with Cu Kα (λ = 1.54 Å) radiation. The crystallinity index (CI) was determined by
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using the following equation (2) [10].

Ph22.8239 −Ph15.3488
CI = ⁡x⁡100% (2)
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Ph22.8239

where Ph22.8239 (Crystalline Phase) and Ph15.3488 (Amorphous Phase) are the peak intensity at

2θ angle. The crystallite size (CS) was obtained by using the following equation (3)[26].

Kλ
CS = ⁡ βCOSθ (3)

where K is the Scherrer constant (0.84), λ is the X-ray wavelength (0.154 nm), θ is the Bragg

angle and β is the peaks full width at half maximum.

2.3.6. FTIR spectroscopy

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The chemical and free functional substituents available in the DSSFs was finalized by Bruker

TENSOR 27 FTIR spectroscopy (Optik GmbH, Germany) with spectral resolution 2 cm-1 and

over wave number range of 500 - 4000 cm-1 region with 32 scans per minute in each case at a

temperature of 30o C with 65% humidity [15].

2.3.7. Atomic Force Microscopy

The DSSFs surface roughness was estimated by high clarity Atomic Force Microscope

(model Agilent-5100, USA). The samples were prepared by dissolving the fiber powder

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(0.01g) in 15ml of acetone. Then the homogeneous dispersion was coated on the glass slide

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and desiccated at room temperature. -p
2.3.8. Scanning Electron Microscopy
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The DSSFs surface morphology was investigated by Field Emission -Scanning Electron

Microscope (Quanta FEG 250) at different magnifications with an electron beam accelerating
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potential of 3 kV.
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2.3.9. X-Ray Photoelectron spectroscopy

The chemical properties of DSSFs surface were evaluated through X-ray photoelectron
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spectroscopy (PHI versa probe III, Physical Electronics Chanhassen MN, USA) with
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monochromatic Al-Kα (1486.8 eV) and spot beam size of 400 nm diameter with the energy

of 4.5W Shirley X-ray source developed.

2.3.10. TGA/DTG studies

The thermal behavior of DSSFs was estimated by thermogravimetric analysis using

simultaneous thermal analyzer (SDT-Q600, USA) in the nitrogen gas atmosphere at the

heating rate of 1o C/min. The kinetic activation energy (Ea) of DSSFs was assessed by

Broido’s equation (4) [17].

1 𝐸 1
ln [ln (𝑦)] = − ( 𝑅𝑎 ) [(𝑇) + 𝐾] (4)
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where Ea is the kinetic activation energy, R is the universal gas constant (8.32 J/mol K), T is

the temperature (Kelvin), y is the normalized weight (wt/wi), wi symbolizes initial weight of

the sample, wt indicates the weight of the sample at any time t, and K is the reaction rate

constant.

2.3.11. Contact Angle Measurement

Contact angle measurement of DSSFs was done by Data physics (OCA 15EC) contact angle

apparatus. The single fiber was positioned above the measuring table and a liquid droplet of

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volume of 2 μL was dispensed over the fiber surface via micropipette along the longitudinal

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axis of the fiber. High resolution images were taken using a computer interface camera.
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3. Result and Discussion

3.1 Anatomical study of DS stem

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The DSS anatomical structural arrangement revealed the existence of an ordinary stem
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structure, where the peripheral epidermal layer is less definite followed by cortex having

unique phloem and xylem zones (Fig. 2a). It is correspondingly unveiled abnormal subsidiary
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growth, which incorporates different zones of secondary phloem and xylem cylinders in
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consecutive secondary layers. The secondary xylem zone is broad, thick, and a slight ovoidal

in shape and loaded with plenty of rough walled circular deep vessels (Dia. ~30 to ~110 µm

& 10 µm thickness) and sieve-tube members/cells like parenchyma. Each vessel is bounded

by the bulk number of vertical bundles of mucilaginous or gelatinous type fibers (G-fibers or

gFi) (Fig. 2b , c, d & e). Usually, G-fiber has an extra cell wall layer within the thick

secondary wall termed as a gelatinous layer or G-layer, which consists of a large amount of

cellulose with very little lignin[27].

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Fig. 2. (a) Transverse section of DSS showing secondary phloem, secondary xylem, vessels

and fibers (4X) (b) An enlarged DSS segment exhibiting vessel surrounded by sclerenchyma
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and gelatinous fibers (20X) (c) Magnified view of the single vessel covered by gelatinous
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fibers groups and sclerenchyma (40X) (d) Expanded view of fiber cell’s gelatinous wall,
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secondary wall, middle lamella, primary wall, and cell lumen (40X) (e) Longitudinal view of

single gelatinous fibers (f) Longitudinal section of DSS showing fiber bundles with phloem
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ray, procumbent cell, upright cell and sieve element (20X)

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The gFi are having very thick outer and inner tangential walls that are steadily bonded with

the vessels outer fence and have distinct cell lumen (~70 to ~80 µm wide) with well-defined

thick secondary (~25 µm thick) wall, primary wall (~15 µm thick) and middle lamella (~2

µm thick). The important task of the G-layer is to facilitate the coil alignment of stems, which

can produce large tensional stress inside the mature organs. Thus, it either equips the mobility

of these organs or strengthens their physique structure and solidity [28]. Flax, hemp, and

ramie fibers are well-known examples of gelatinous type fiber [29]. Fig. 2 a & f depicts the
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phloem rays and procumbent cells in stretched cross-section that traces in between the

vessels.

3.2 Chemical Analysis

3.2.1. Physio-Chemical Property

The DSSFs consist of ~ 63.3 wt.% of cellulose, ~ 11.6 wt.% of hemicellulose, ~ 15.3 wt.% of

lignin, and ~0.81 wt.% of wax, ~4.57 wt.% of ash & ~6.02 wt.% of moisture. The density of

DSSFs is 1.43 ± 0.018 g/cm3. The linear density (fineness) of DSSFs is around 1020 denier.

This minimal density is beneficial to a mass reduction in the particular case of applications

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such as automobiles, aerospace, and sports equipment. This high quantity of cellulose (63.3wt

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%) provides toughness, strength, rigidity, and structural constancy to the DSSFs [30].
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Conversely, the large amount of hemicellulose existence diminishes the strength of the fiber
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[17]. Luckily, the extract DSSFs has lower (11.6 wt%) hemicellulose. The lignin behaves as a

protecting guard against the fungal or bacterial attack and also influence on morphology,
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structural properties, bonding nature and moisture resistance of the fiber [26,31]. DSSFs
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holds15.3wt% of lignin which is desirable. Less quantity of wax (0.81 wt%) in DSSFs helps

to reduce the uncouple effect between reinforcement and matrices [24]. DSSFs contour is
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almost cylindrical and its average diameter is observed in the range of 158 to 169 µm. The
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assessed chemical quantity, density, and diameter of DSSFs are compared with that of the

natural fibers extracted from other bio-resources and listed in Tables 3 and 4. It reveals that

the DSSFs exhibit the properties that are necessary for potential reinforcement material.

3.2.2. XRD Analysis

The XRD pattern of the DSSFs is shown in fig. 3a. The pattern exhibits two peaks

corresponding to the amorphous and crystalline planes appear at 2θ = 15.348o and 2θ =

22.823o, related to type I cellulose [32]. The crystallinity index (CI) of DSSFs is found to be
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58.15 %. This higher CI value shows that the molecular arrangement in DSSF is highly

ordered in nature [15].

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Fig.3. (a) X-ray diffraction, (b) FTIR spectrum acquired from DSSFs
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The CS of DSSFs is found to be 11.92 nm. This larger CS diminishes hydrophilic behavior,

chemical responsiveness of DSSFs and boosts the mechanical strength of the fibers [18]. The
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DSSFs crystalline properties are compared with other lignocellulosic fibers in Table 4.
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3.2.3. FTIR Analysis

FTIR spectrum that gives the qualitative information on the chemical structure of the DSSFs
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is shown in Fig. 3b. A broad concentrated peak detected at 3423 cm-1 indicates the existence
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of O-H stretching and H-bond vibration in the hydroxyl clusters of cellulose [33]. The peak

at 2924 cm-1 corresponds to the CH (CH2 and CH3) stretching, bending, and periodic motion

of the functional alkyl group of cellulose and hemicellulose elements [8]. A weak minor

stretching peak attained at 2310 cm-1 represents C≡C band which attributes to alkyne groups

stretching of wax and also verifies wax gist present in DSSFs [3]. The high sharp peak

noticed at 1635 cm-1 corresponds to the stretching vibration of carbonyl acid (C=O) /acetyl

group linkage of lignin and hemicellulose in DSSFs [19,34]. The peak at wavenumber 1454

cm-1 that corresponds to asymmetric deformation and aromatic vibration of CH of lignin and

CH2 symmetric bending of cellulose [35]. The two peaks observed at 1375 cm-1 and 1321 cm-
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corresponds to the bending vibration of CO and CH groups in polysaccharides arenes ring,

respectively [6]. A slight bounce at 1246 cm-1 corresponds to the stretching vibration -C=O

of polyose with ethanoyl groups of lignin [36]. The tiny peak at 1155 cm-1 is owed -COH to

stretching in cellulose [18]. The broad peak at 1028 cm-1 corresponds to the -C=O stretching

state oscillation of ether and hydroxy groups, β -glycosidic associated to the lignin [1,34].

The little peak at 894 cm-1, was attributed to the C-O stretching of the cellulose presence of b-

glycosidic linkages between the monosaccharides [5,13]. The minor peak at 777 cm-1

signifies the occurrence of saline content [15]. The peak noticed at 661 cm-1 & 518 cm-1

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belongs to the C-OH molecule out of plane bending vibrations involving ring structure it

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almost diminishes with plant maturity [11]. -p
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3.3 Study of Surface Characteristics

3.3.1. XPS Analysis

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From the XPS analysis, the carbon and oxygen contribution on the DSSFs is found to be
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80.16% and 19.33%, respectively. Likewise, the slight quantity of Si (0.32%) and Al (0.19%)

is present with nitrogen, calcium, and chlorine on the surface of DSSFs and it is usually
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emerging out of the soil and natural impurities adhere on the exterior surface of the fiber. The
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high-resolution spectrum of C1s that arises from the carbon present in the carbohydrate

constituents of DSSFs is shown in Fig. 4.

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Fig. 4. XPS spectra of C1s peaks belong to the DSSFs
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In DSSFs, O/C ratio is computed as 0.24 which is lesser than luffa cylindrica (0.54), kenaf
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(0.45), jute (0.46), henequen (0.25), althaea (0.26) and hemp (0.27) fibers[37]. The low O/C

ratio of DSSFs shows that a less amount of wax and lignin present in the surface of DSSFs
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[38]. The saturated carbon (C1) peak at 283.2 eV corresponds to the (C-C) carbon atoms of
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aliphatic compounds (fatty acid/esters) and aromatic rings of lignin and hydrocarbon

extractives of DSSFs [39]. The peak (C2) at 284.4 eV, corresponds (C-C & C-H) from
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hemicellulose and lignin [37,40]. The peak (C3) carbon peak at 287.2 eV represents the
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(C=O/O–C–O) carbonyl groups [40]. The peak (C4) at 288.8 eV denotes the O-C=O

associated with the aliphatic and aromatic ethers, esters and carboxylic acids in lignin and

extractives of DSSFs [40].

3.3.2. AFM studies

The 2D and 3D topographical images of DSSFs surface are shown in Fig. 5 a & b. The

average surface roughness (Ra) value of DSSFs is 105.959 nm which is greater than that of
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Thespesia populnea barks (3.002 nm), Furcraea Foetida (18.005 nm) Dracaena

reflexa(22.769 nm) fiber [36,17,3].

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Fig. 5 Surface topography images (a) 2D and (b) 3D of DSSFs using Atomic force

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microscopy in non-contact mode. -p
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The larger Ra value indicates that the surface of the DSSFs is free from impurities [17]. The

Root mean square roughness (Rq) value is 138.866 nm. The proportion of Rq & Ra is 1.31,
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which shows that it falls under the Gaussian normal distribution and also agreement with
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tribological standards [41]. The Roughness kurtosis (Rku) value is 1.40. The Rku value less

than 3 denotes that the surface of DSSFs is rough [3]. The estimated Roughness skewness
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(Rsk) value of DSSFs is -0.251. This negative sign reveals its negative skewness and natural
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porosity [36]. The maximum peak to peak height (Rt) and ten-point average absolute height

roughness (Rz) values are found to be 1446.49 nm and 721.366 nm, respectively. These

higher roughness values are adequate to facilitate great coherence between reinforcement and

matrix.

3.3.3. FE-SEM studies

FE-SEM images of the inner and outer surface of DSSFs are shown in Fig. 6. Transverse

sectional images (Fig.6 a-c) exhibit the elemental factors like the secondary wall, primary
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wall, middle lamella and lumen. The longitudinal surface view of DSSFs (Fig.6 d-f) shows

that the outer layer is filled over with rough hexagonal and rectangular shape texture and also

have some usual irregularities like shallow pores, pits, slots, grooves and smooth as well as

rough surfaces. At higher magnifications, DSSFs SEM images display that the fiber bundle is

articulated by microfibrils with hollow sub-fibers and that is masked with a waxy layer.

Furthermore, the presence of irregular rough surface structure can promote good

penetration of resin into the fibers that improve the adhesion between fiber and matrix in a

composite. This improved adhesion, in turn, attributes to the strength of composite laminates

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[42]. Further, the FE-SEM results are consistent with anatomical and AFM studies.

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Fig. 6. FE-SEM images of DSSFs in cross sectional view (a-c) and top surface view (d-f).

3.3.4. Contact Angle

Fig.7. Contact angle measurement of DSSFs

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Fig. 7 is a high-resolution photograph of a water droplet on the surface of DSSFs. As shown

in the figure, the contact angle can be readily obtained as 54.61ᵒ [6]. It is worthy to mention

that the presence of lignin and wax on the surface of the DSSFs is very low. In other words,

the lower contact angle results in greater wettability that empowers the fiber to get attached

with the polymer matrix, thereby increasing the strength of composites.

3.4 Single Fiber Tensile Strength and Weibull Analysis

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The stress-strain curves of DSSFs (Fig. 8) illustrate that the fibers are brittle in nature as they

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undergo sudden failure with severe load fall. Such an attitude is on par with other

lignocellulosic fibers [6]. The tensile characteristics of DSSFs verified under five different
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gauge length (GL) is presented in Table 1.
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Table 1 Tensile characteristics of DSSFs
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Gauge Young's Strain to Cross Sectional

Tensile
Length Modulus Failure Area
Strength (MPa)
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(mm) (GPa) (%) (mm2)

10 437.21 ± 47.83 4.80 ± 2.02 9.11 ± 3.54 0.020142 ± 0.0034
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20 650.41 ± 65.98 9.91 ± 5.71 6.56 ± 2.86 0.020706 ± 0.0021

30 785.34 ± 86.14 15.17 ± 7.74 5.18 ± 2.63 0.020870 ± 0.0013
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40 737.15 ± 78.10 22.07 ± 9.42 3.34 ± 2.30 0.021337 ± 0.0043

50 559.26 ± 64.08 15.77 ± 8.66 3.55 ± 1.64 0.022069 ± 0.0014
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Fig.8 Stress-Strain curves of DSSFs

The average tensile strengths of DSSFs were found to be in the range of 437 - 785 MPa. For

gauge lengths up to 30 mm, the average tensile strength of DSSFs varied with increasing

tendency, and then drastically decreased to 559 MPa at GL 50 mm. Such variation is

expected as the tensile strength of natural fiber not only depends on the gauge length but also

on the flaw characteristics such as mean flaw size and number of flaws per volume

[23,24,36]. Once a crack is initiated at the bigger flaw, further propagation of the crack and

its interaction with other flaws may occur [18]. For instance, when a higher number of flaws

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exists per unit length, the linkage between the flaws may be quicker, thereby resulting in

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lower ductility [47]. In DSSFs, the increase in tensile strength with gauge length up to 30mm
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is, perhaps attributed to less number of flaws in the fiber. Several other natural fibers derived
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from the sources like the Kigelia Africana fruit [48], Ficus religiosa tree [45], Coccinia

grandis root [15], Indian Areca Fruit [44], to name a few, show similar behavior as DSSFs.
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Young’s modulus values were found to vary between 4 - 22 GPa with the gauge lengths of 10
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mm to 50 mm. It is probably related to the variability in microstructure and defects that occur

during the extraction of DSSFs [15]. The percentage of strain to failure diminished with the
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increase in GL due to the higher probability of the occurrence of flaws like cracks, voids and
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their size scattered on all portions of the fiber [18]. Using equation (1), the microfibril angle

(α) of DSSFs was estimated to be 17.65◦ ± 5.36, which is in comparable to that of other fibers

obtained from Kigelia africana (13.5), Tridax procumbens (13.41), Thespesia populnea

(13.94). The higher angle provides adequate flexibility to withstand the loads without tearing

up to a certain limit [33,6,36]. The variation in the tensile properties of the single fibers may

be attributed to several factors as listed below. (i) plant source: variation of fiber cell number,

cell wall structure, fiber dimension, climatic conditions of cultivation, chemical composition

and its age (ii) fiber extraction method: duration of the retting, and (iii) testing parameters
 Journal Pre-proof

[47,1,30]. To verify the variation of experimentally measured values are statistically

meaningful, two-parameter Weibull distribution has been used [35]. The Weibull distribution

brings a statistically sensible resemblance of the measured data to assess the geometrical and

tensile properties of DSSFs. Fig. 9 shows Weibull statistical distribution curves for

experimentally measured values of DSSFs, a-d represents the diameter, tensile strength,

Young's modulus, and strain at failure with shape and scale parameters, respectively. The

curvatures demonstrate that the measured data are very close to the line and well-positioned

within the confidence level. Also, it shows an excellent concurrence with the correlation

of
factor of all mechanical properties, and acquired experimental values are very near to the

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average values. Table 2 is a comparison of the mechanical properties of DSSFs with
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commonly known synthetic fibers, whereas Table 3 presents the chemical and mechanical
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properties of other natural fibers reported in the literature. Although the tensile strength

values of DSSFs are significantly lower than the synthetic fibers, the biodegradability and
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non-toxic nature of DSSFs are promising.

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Fig. 9. Weibull distributions for the probability of survival corresponding to (a) Diameter
(b)Tensile strength (c) Young’s modulus and (d) Strain at the break.

Table 2 Comparison of mechanical properties of DSSFs with popular synthetic fibers

Mechanical Properties
Tensile Young’s
Fiber Strain to References
strength modulus
failure (%)
(MPa) (GPa)
Current
DSSFs 437-785 4.80-22.07 3.34-9.11
Study

of
E-glass 2000 - 3500 70 2.5 [18]
S-glass 4570 86 2.8 [18]
Carbon 2400 - 4000 230 - 400 1.4 – 1.8 [18]

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Aramid 3000 - 3150 63 – 67 3.3 – 3.7 [18]
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3.5 Thermal Analysis
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The TGA, DTG & Broido’s plots (Fig. 10 a & b) represent the various segments of thermal
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breakdown which is associated with the decay of primary chemical constituents of DSSFs.

The early weight loss (~ 7.71 %) till 100◦C is due to the eviction of water molecules, wax and
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volatile solvents from the DSSFs, which is also noticeable in the beginning stage of the DTG

curve [8]. There is no notable weight drop till 230 oC, which specifies that DSSFs has
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acceptable thermal stability. This thermal stability prevents the thermal break down of the
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natural fiber during fabrication.

Fig. 10 (a) TGA and DTA thermogram of DSSFs and (b) Broido’s Plot of DSSFs.
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In DTG another slight dip is observed at ~230◦C where lignin pyrolysis is originated with

lesser degradation of hemicelluloses [33]. The utmost weight loss (~55.38 %) was recorded

between 230 oC to 356 oC due to the depolymerization of hemicelluloses and the complete

breakdown of glycosidic links in α-cellulose [36]. Further, a sudden fall (332 oC) in the DTG

curve in this temperature range witnessed the complete degradation of cellulose [36]. In the

DTG curve, two tiny peaks at 475 oC and 625 oC were observed due to pyrolysis of lignin and

oxidative degradation of charred residue, respectively [15]. Above 600◦C, the

macromolecules of fibers get decomposed into low molecular weight compounds such as CO,

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CO2, hydrocarbons, and H2O [23]. From the Broido’s plot (Fig. 10. (b)), the kinetic

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activation energy (Ea) for the DSSFs is found to 73.2 kJ. Additionally, this (Ea) value is
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located within the standard activation energy (60-170 kJ/mol) boundary of woods [25].
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Table 3 Comparison of the chemical and tensile properties of DSSFs with other natural fibers.

Chemical Properties Tensile Properties

at break (%)
Elongation
Cellulose

Cellulose

Reference
Moisture

Modulus
Young’s
strength
(Wt. %)

(Wt. %)

(Wt. %)

(Wt. %)

(Wt. %)

(Wt. %)
Sl.

Content

Tensile
Lignin

(MPa)

(GPa)
Hemi
Name of Fiber

Wax

Ash
No.

437.21 ± 47.83 4.80 ± 2.02 3.34 ± 2.30

1 DSSFs 63.3 11.6 15.3 0.81 4.57 6.02 -

o f
785.34 ± 86.14
-
22.07 ± 9.42
-
9.11 ± 3.54
Current
Study

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Aerial roots of banyan
2 67.32 13.46 15.62 0.89 3.96 10.21 19.37±7.72 1.8±0.4 1.8±0.4 [32]
tree
3 Areca fruit Husk
57.35- 13- 23.17-
0.12 -
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7.32 147-322 1.124-3.155 10.23-13.15 [44]

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58.21 15.42 24.16
26.515-
4 Coccinia Grandis Stem 63.22 - 24.42 0.32 - 9.14 424.24-774.64 5.6-16 [18]

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123.51
10.17 ± 2.703 ±
5 Coccinia Grandis.L 62.35 13.42 15.61 0.79 4.38 5.6 273 ± 27.74 [12]

a
1.261 0.2736

n
Cissus Quadranularis
6 77.17 11.02 10.45 0.14 7.3 - 1857-5330 68-203 3.57-8.37 [15]

7
Root
Cissus Quadranularis
82.73
u
7.96 r 11.27 0.18 6.6 - 2300-5479 56-234 3.75-11.14 [23]

8
9
stem
Dracaena reflexa
Furcraea Foetida
70.32
68.35 J o
11.02
11.46
11.35
12.32
0.23
0.24
6.23
6.53
5.19
5.43
829.6
590.45-623.52
46.37
5.99-6.52
2.95
10.32-10.82
[3]
[17]
Ficus Religiosa tree root
10 55.58 13.86 10.13 0.72 4.86 9.33 433.32 ± 44 5.42 ±2.6 8.74±1.8 [45]
fiber
11 Prosopis juliflora bark 61.65 16.14 17.11 0.61 5.2 9.48 558 ± 13.4 - 1.77 ± 0.04 [25]
Saharana Aloe Vera
12 60.2 14.2 13.7 1.5 3.4 7.6 621.8 40.03 2.47 [26]
Cactus Leaves
13 Tamarindus Indica 72.84 11 15.3 0.2 - 6.3 1137-1360 11.2 - 20.7 6.5 - 10.1 [31]
14 Thespesia populnea barks 70.12 12.64 16.34 0.76 1.80 10.83 557.82 ± 56.29 20.57± 4.46 2.80 ± 0.56 [32]
15 Areca palm leaf stalk 57.49 18.34 7.26 0.71 1.43 9.35 364.6 ± 21.4 9.39±1.1 3.47±1.1 [42]
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Table 4 Comparison of the physical, crystalline and thermal properties of DSSFs with other natural fibers.

Physical Properties Crystalline Properties Thermal Properties

Diameter (μm)

Reference
Temperature
Crystallinity

Crystallinity

Degradation

Energy (Ea)
Activation
Index (%)

Size (nm)

Stability

(kJ/mol)
Thermal
Density
Sl.

(g/cm3)

(⁰ C)
(⁰ C)

Max.
Name of Fiber
No.

Current
o

Study
1 DSSFs 158-169 1.43 ± 0.018 58.15 11.92 230 332 73.2

r o
p
2 Aerial roots of banyan tree 0.09- 0.14 1.234 72.47 6.28 230 358 72.65 [32]
3 Areca fruit Husk 396-476 0.7-0.8 55.5

e - 7.9 240 325.8 64.54 [44]

4
5
Coccinia Grandis Stem
Coccinia Grandis.L
543-621
27.33 ± 0.3789
1.5175
1.243 ±
P r
46.09
52.17
1.91
13.38
250
213.4
320
351.6
82.3
67.02
[18]
[12]
6 Cissus Quadranularis Root 610-725 l
0.022

a
1.51 56.6 7.04 230 328.9 74.18 [15]
7
8
Cissus Quadranularis stem
Dracaena reflexa
770-870
176.2
r n 1.22
0.79
47.15
57.32
31.55
19.01
270
232.32
342.1
348.7
65.23
68.78
[23]
[3]
9 Furcraea Foetida
Ficus Religiosa tree root
o
12.8
u 0.77 52.6 28.36 270 320.5 65.64 [17]
10
11
12
fiber
Prosopis juliflora bark
Saharana Aloe Vera
J 25.62
20
91.15
1.246
0.58
1.325
42.92
46
52.6
5.18
15
5.6
325
217
238
400
331
350
68.02
76.72
60.2
[45]
[25]
[26]
Cactus Leaves
13 Tamarindus Indica 564-789 1-1.2 55 5.68 238 360 61.3 [31]
59.85 -
14 Thespesia populnea barks - 1412 48.17 3.576 245.4 323.7 [32]
73.01
Areca palm leaf
15 285-330 1.09±0.02 - - 279 365 - [42]
stalk
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4. Conclusion
In this study, a new lignocellulosic natural fiber was extracted from Derris scandens stem

and comprehensive characterizations were carried to evaluate the feasibility of utilizing it as a

reinforcing material in polymer composites. The anatomical study reveals DSS structural

arrangements and fiber secondary wall (~25 µm) and primary wall (~15 µm) dimensions.

FTIR analysis ensured the DSSFs having similar chemical groups (O=H), (C=O), (C=H) and

(C≡C) like other lignocellulosic fibers. The existence of a sufficient amount of cellulose

(63.3 wt.%) with the crystallinity index (58.15%) and crystallite size (11.92 nm) assured a

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high mechanical strength to DSSFs as confirmed through the tensile test . Two parameter

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Weibull statistical distribution exposed a good fit inside the permitted confidence levels.
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From XPS investigation, it is evident that the oxygen, carbon, and hydrogen were the
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principal elements and established that the DSSFs is organic. The findings acquired through

TGA confirmed the DSSFs thermal steadiness (230ᵒC) to withstand the high temperature
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involved in the fabrication process. SEM images provide noteworthy details about surface
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irregularities of fiber and AFM revealed that the DSSFs average surface roughness (105.95

nm). This higher roughness favors their adhesion with polymer matrix during the fabrication
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of composites. Most importantly, the reinforcing capability of this DSSFs created economic
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value to this plant and it can be efficiently employed for various usages with benefits in costs,

society, and environment. The findings of anatomical, physicochemical, mechanical, surface

morphological, and thermal properties acquired for DSSFs are mostly comparable to that of

other natural fibers. This authenticates the potential of the fiber as an alternative to the

manmade non-eco-friendly synthetic fibers

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Conflict of Interest
The authors declare no conflict of interest.

Acknowledgements

The authors are sincerely thankful to Central Pulp & Paper Research Institute Saharanpur for the

estimation of the chemical composition of natural fiber, SITRA (South Indian Textile Research

Association) for Single fiber tensile test, PSG Institute of Advanced studies Coimbatore for AFM

studies, Central Electro Chemical Research Institute (CECRI) Karaikudi for FTIR/ TGA

measurements, University Science Instrumentation Centre (USIC), Alagappa University,

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Karaikudi for the XRD measurements, FE-SEM&XPS measurement, The authors are also grateful

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to Prof. Dr. P. Jayaraman, Plant Anatomy Research Centre (PARC), Chennai for Anatomical study
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of the plant.
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References

[1] R.S. M, S. Siengchin, J. Parameswaranpillai, M. Jawaid, C.I. Pruncu, A. Khan, A

comprehensive review of techniques for natural fibers as reinforcement in composites:

Preparation, processing and characterization, Carbohydr Polym 207 (2019) 108-121.

[2] P. Madhu, M.R. Sanjay, M. Jawaid, S. Siengchin, A. Khan, C.I. Pruncu, A new study on

effect of various chemical treatments on Agave Americana fiber for composite

reinforcement: Physico-chemical, thermal, mechanical and morphological properties,

Polymer Testing 85 (2020), https://doi.org/10.1016/j.polymertesting.2020.106437.

of
[3] P. Manimaran, S.P. Saravanan, M.R. Sanjay, S. Siengchin, M. Jawaid, A. Khan,

ro
Characterization of new cellulosic fiber: Dracaena reflexa as a reinforcement for polymer
-p
composite structures, Journal of Materials Research and Technology 8(2) (2019) 1952-1963.
re
[4] A. Khan, A.M. Asiri, M. Jawaid, N. Saba, Inamuddin, Effect of cellulose nano fibers and

nano clays on the mechanical, morphological, thermal and dynamic mechanical performance
lP

of kenaf/epoxy composites, Carbohydr Polym 239 (2020) 116248,

na

https://doi.org/10.1016/j.carbpol.2020.116248.

[5] A. Khan, R. Vijay, D.L. Singaravelu, M.R. Sanjay, S. Siengchin, F. Verpoort, K.A.
ur

Alamry, A.M. Asiri, Extraction and Characterization of Natural Fiber from Eleusine Indica
Jo

Grass as Reinforcement of Sustainable fiber-Reinforced Polymer Composites, Journal of

Natural Fibers (2019) 1-9, DOI: 10.1080/15440478.2019.1709110.

[6] R. Vijay, D. Lenin Singaravelu, A. Vinod, M.R. Sanjay, S. Siengchin, M. Jawaid, A.

Khan, J. Parameswaranpillai, Characterization of raw and alkali treated new natural cellulosic

fibers from Tridax procumbens, Int J Biol Macromol 125 (2019) 99-108,

https://doi.org/10.1016/j.ijbiomac .2018.12.056.

[7] A. Saravanakumaar, A. Senthilkumar, S. S. Saravanakumar, M. R. Sanjay, A.Khan,

Impact of alkali treatment on physico-chemical, thermal, structural and tensile properties of

 Journal Pre-proof

Carica papaya bark fibers, International Journal of Polymer Analysis and Characterization

23(6) (2018), DOI: 10.1080/1023666X.2018.1501931.

[8] P. Narayanasamy, P. Balasundar, S. Senthil, M.R. Sanjay, S. Siengchin, A. Khan, A.M.

Asiri, Characterization of a novel natural cellulosic fiber from Calotropis gigantea fruit bunch

for ecofriendly polymer composites, Int J Biol Macromol 150 (2020) 793-801,

https://doi.org/10.1016 /j.ijbiomac.2020.02.134.

[9] A. Khan, R. Vijay, D. Lenin Singaravelu, G.R. Arpitha, M.R. Sanjay, S. Siengchin, M.

Jawaid, K. Alamry, A.M. Asiri, Extraction and characterization of vetiver grass

of
(Chrysopogon zizanioides) and kenaf fiber (Hibiscus cannabinus) as reinforcement materials

ro
for epoxy based composite structures, Journal of Materials Research and Technology 9(1)
-p
(2020) 773-778, https://doi.org/10.1016/j.jmrt.2019.11.017.
re
[10] N. Premalatha, S.S. Saravanakumar, M.R. Sanjay, S. Siengchin, A. Khan, Structural and

Thermal Properties of Chemically Modified Luffa Cylindrica Fibers, Journal of Natural

lP

Fibers (2019) 1-7, DOI: 10.1080/15440478.2019.1678546.

na

[11] Anish Khan, R Vijay, D Lenin Singaravelu, M R Sanjay, Suchart Siengchin, Francis

Verpoort, Khalid A. Alamry & Abdullah M Asiri (2019): Extraction and Characterization of
ur

Natural Fiber from Eleusine Indica Grass as Reinforcement of Sustainable fiber-Reinforced

Jo

Polymer Composites, Journal of Natural Fibers, DOI: 10.1080/15440478.2019.1697993.

[12] P. Senthamaraikannan, M. Kathiresan, Characterization of raw and alkali treated new

natural cellulosic fiber from Coccinia grandis.L, Carbohydr Polym 186 (2018) 332-343.

[13] K.Nijandhan, R Muralikannan, S Venkatachalam Ricinus communis fiber as potential

reinforcement for lightweigh polymer composites,Materials Research Express 5 ( 095307)

(2018) 1-9.
 Journal Pre-proof

[14] N.Kulandaivel, R. Muralikannan, K.S, Extraction and Characterization of Novel Natural

Cellulosic Fibers from Pigeon Pea Plant, Journal of Natural Fibers 175(5) (2018) 769-779,

DOI: 10.1080/15440478.2018.1534184.

[15] S. Indran, R.E. Raj, V.S. Sreenivasan, Characterization of new natural cellulosic fiber

from Cissus quadrangularis root, Carbohydr Polym 110 (2014) 423-9.

[16] J. Tulinska, E. Jahnova, M. Dusinska, M. Kuricova, A. Liskova, S. Ilavska, M.

Horvathova, L. Wsolova, S.A. Kyrtopoulos, A. Collins, V. Harrington, L. Fuortes,

Immunomodulatory effects of mineral fibres in occupationally exposed workers, Mutat Res

of
553(1-2) (2004) 111-24.

ro
[17] P. Manimaran, P. Senthamaraikannan, M.R. Sanjay, M.K. Marichelvam, M. Jawaid,
-p
Study on characterization of Furcraea foetida new natural fiber as composite reinforcement
re
for lightweight applications, Carbohydr Polym 181 (2018) 650-658.

[18] S.G. Jebadurai, R.E. Raj, V.S. Sreenivasan, J.S. Binoj, Comprehensive characterization
lP

of natural cellulosic fiber from Coccinia grandis stem, Carbohydr Polym 207 (2019) 675-683.
na

[19] Z. Belouadah, A. Ati, M. Rokbi, Characterization of new natural cellulosic fiber from

Lygeum spartum L, Carbohydr Polym 134 (2015) 429-37.

ur

[20] D. Kuljittichanok, P. Diskul-Na-Ayudthaya, C. Weeraphan, D. Chokchaichamnankit, K.

Jo

Chiablaem, K. Lirdprapamongkol, J. Svasti, C. Srisomsap, Effect of Derris scandens extract

on a human hepatocellular carcinoma cell line, Oncol Lett 16(2) (2018) 1943-1952.

[21] P. Puttarak, R. Sawangjit, N. Chaiyakunapruk, Efficacy and safety of Derris scandens

(Roxb.) Benth. for musculoskeletal pain treatment: A systematic review and meta-analysis of

randomized controlled trials, J Ethnopharmacol 194 (2016) 316-323.

[22] T. Sreelatha, A. Hymavathi, V. Rama Subba Rao, P. Devanand, P. Usha Rani, J.

Madhusudana Rao, K. Suresh Babu, A new benzil derivative from Derris scandens:

Structure-insecticidal activity study, Bioorg Med Chem Lett 20(2) (2010) 549-53.
 Journal Pre-proof

[23] S. Indran, R.E. Raj, Characterization of new natural cellulosic fiber from Cissus

quadrangularis stem, Carbohydr Polym 117 (2015) 392-9.

[24] V.S. Sreenivasan, S. Somasundaram, D. Ravindran, V. Manikandan, R. Narayanasamy,

Microstructural, physico-chemical and mechanical characterisation of Sansevieria cylindrica

fibres – An exploratory investigation, Materials & Design 32(1) (2011) 453-461.

[25] S.S. Saravanakumar, A. Kumaravel, T. Nagarajan, P. Sudhakar, R. Baskaran,

Characterization of a novel natural cellulosic fiber from Prosopis juliflora bark, Carbohydr

Polym 92(2) (2013) 1928-33.

of
[26] A.N. Balaji, K.J. Nagarajan, Characterization of alkali treated and untreated new

ro
cellulosic fiber from Saharan aloe vera cactus leaves, Carbohydr Polym 174 (2017) 200-208.
-p
[27] J. Felten, J. Vahala, J. Love, A. Gorzsas, M. Ruggeberg, N. Delhomme, J. Lesniewska, J.
re
Kangasjarvi, T.R. Hvidsten, E.J. Mellerowicz, B. Sundberg, Ethylene signaling induces

gelatinous layers with typical features of tension wood in hybrid aspen, New Phytol 218(3)
lP

(2018) 999-1014.
na

[28] E.J. Mellerowicz, T.A. Gorshkova, Tensional stress generation in gelatinous fibres: a

review and possible mechanism based on cell-wall structure and composition, J Exp Bot
ur

63(2) (2012) 551-65.

Jo

[29] T. Gorshkova, N. Mokshina, T. Chernova, N. Ibragimova, V. Salnikov, P. Mikshina, T.

Tryfona, A. Banasiak, P. Immerzeel, P. Dupree, E.J. Mellerowicz, Aspen Tension Wood

Fibers Contain beta-(1→4)-Galactans and Acidic Arabinogalactans Retained by Cellulose

Microfibrils in Gelatinous Walls, Plant Physiol 169(3) (2015) 2048-63.

[30] V. Fiore, T. Scalici, A. Valenza, Characterization of a new natural fiber from Arundo

donax L. as potential reinforcement of polymer composites, Carbohydr Polym 106 (2014) 77-

83.
 Journal Pre-proof

[31] J.S. Binoj, R.E. Raj, S. Indran, Characterization of industrial discarded fruit wastes (

Tamarindus Indica L.) as potential alternate for man-made vitreous fiber in polymer

composites, Process Safety and Environmental Protection 116 (2018) 527-534.

[32] T. Ganapathy, R. Sathiskumar, P. Senthamaraikannan, S.S. Saravanakumar, A. Khan,

Characterization of raw and alkali treated new natural cellulosic fibres extracted from the

aerial roots of banyan tree, Int J Biol Macromol 138 (2019) 573-581.

[33] M. Ilangovan, V. Guna, B. Prajwal, Q. Jiang, N. Reddy, Extraction and characterisation

of natural cellulose fibers from Kigelia africana, Carbohydr Polym 236 (2020) 115996.

of
[34] P. Manimaran, S.P. Saravanan, M.R. Sanjay, M. Jawaid, S. Siengchin, V. Fiore, New

ro
Lignocellulosic Aristida adscensionis Fibers as Novel Reinforcement for Composite
-p
Materials: Extraction, Characterization and Weibull Distribution Analysis, Journal of
re
Polymers and the Environment 28(3) (2019) 803-811.

[35] H. Boumediri, A. Bezazi, G.G. Del Pino, A. Haddad, F. Scarpa, A. Dufresne, Extraction
lP

and characterization of vascular bundle and fiber strand from date palm rachis as potential
na

bio-reinforcement in composite, Carbohydr Polym 222 (2019) 114997.

[36] M. Kathirselvam, A. Kumaravel, V.P. Arthanarieswaran, S.S. Saravanakumar, Isolation

ur

and characterization of cellulose fibers from Thespesia populnea barks: A study on

Jo

physicochemical and structural properties, Int J Biol Macromol 129 (2019) 396-406.

[37] A.Ç. Kılınç, S. Köktaş, Y. Seki, M. Atagür, R. Dalmış, Ü.H. Erdoğan, A.A. Göktaş,

M.Ö. Seydibeyoğlu, Extraction and investigation of lightweight and porous natural fiber from

Conium maculatum as a potential reinforcement for composite materials in transportation,

Composites Part B: Engineering 140 (2018) 1-8.

[38] F.A.K. Milan Sernek, W.G. Glasser, Comparative analysis of inactivated wood surface,

Holzforschung Walter de Gruyter 58 (2004) 22-31.

 Journal Pre-proof

[39] B.N. Melo, V.M.D. Pasa, M.D. Martins, W.A.A. Macedo, E.P. Muniz, Strengthening of

a Polyurethane Matrix by Luffa Cylindrica Treated with TDI: Water Absorption and

Mechanical Properties, Journal of Polymers and the Environment 26(6) (2017) 2514-2521.

[40] L.Q.N. Tran, X.W. Yuan, D. Bhattacharyya, C. Fuentes, A.W. Van Vuure, I. Verpoest,

Fiber-matrix interfacial adhesion in natural fiber composites, International Journal of Modern

Physics B 29(10n11) (2015).

[41] V.P. Arthanarieswaran, A. Kumaravel, S.S. Saravanakumar, Physico-Chemical

Properties of Alkali-Treated Acacia leucophloea Fibers, International Journal of Polymer

of
Analysis and Characterization 20(8) (2015) 704-713.

ro
[42] S. N, R. I, R. T, Characterization of untreated and alkali treated new cellulosic fiber from
-p
an Areca palm leaf stalk as potential reinforcement in polymer composites, Carbohydr Polym
re
195 (2018) 566-575.

[43] M. Maache, A. Bezazi, S. Amroune, F. Scarpa, A. Dufresne, Characterization of a novel

lP

natural cellulosic fiber from Juncus effusus L, Carbohydr Polym 171 (2017) 163-172.
na

[44] J.S. Binoj, R. Edwin Raj, V.S. Sreenivasan, G. Rexin Thusnavis, Morphological,

physical, mechanical, chemical and thermal characterization of sustainable Indian Areca fruit
ur

husk fibers (Areca Catechu L.) as potential alternate for hazardous synthetic fibers, Journal of
Jo

Bionic Engineering 13(1) (2016) 156-165.

[45] A.A.M. Moshi, D. Ravindran, S.R.S. Bharathi, S. Indran, S.S. Saravanakumar, Y. Liu,

Characterization of a new cellulosic natural fiber extracted from the root of Ficus religiosa

tree, Int J Biol Macromol 142 (2020) 212-221.

[46] M.R.S. P. Manimaran, P. Senthamaraikannan, S. S. Saravanakumar, Suchart Siengchin,

G. Pitchayyapillai & Anish Khan, Physico-Chemical Properties of Fiber Extracted from the

Flower of Celosia Argentea Plant, Journal of Natural Fibers

(2019), DOI: 10.1080/15440478.2019.1629149

 Journal Pre-proof

[47] F.d.A. Silva, N. Chawla, R.D.d.T. Filho, Tensile behavior of high performance natural

(sisal) fibers, Composites Science and Technology 68(15-16) (2008) 3438-3443,

https://doi.org/10.1016/j.compscitech.2008.10.001.

[48] R. Siva, T.N. Valarmathi, K. Palanikumar, A.V. Samrot, Study on a Novel natural

cellulosic fiber from Kigelia africana fruit: Characterization and analysis, Carbohydr Polym

244 (2020) 116494, https://doi.org/10.1016/j.carbpol.2020.116494.

[49] M.E. Alves Fidelis, T.V.C. Pereira, O.d.F.M. Gomes, F. de Andrade Silva, R.D. Toledo

Filho, The effect of fiber morphology on the tensile strength of natural fibers, Journal of

of
Materials Research and Technology 2(2) (2013) 149-157,

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https://doi.org/10.1016/j.jmrt.2013.02.003. -p
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Author Statement:

C. Ilaiya Perumal : Conceptualization, Resources & Visualization, Data curation,

Resources &Validation, Investigation, Writing original draft and
review.

R. Sarala : Methodology & Supervision.

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Table 1 Tensile characteristics of DSSFs

Gauge Young's Strain to Cross Sectional

Tensile
Length Modulus Failure Area
Strength (MPa)
(mm) (GPa) (%) (mm2)

of
10 437.21 ± 47.83 4.80 ± 2.02 9.11 ± 3.54 0.020142 ± 0.0034
20 650.41 ± 65.98 9.91 ± 5.71 6.56 ± 2.86 0.020706 ± 0.0021

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30 785.34 ± 86.14 15.17 ± 7.74 5.18 ± 2.63 0.020870 ± 0.0013
40 737.15 ± 78.10 22.07 ± 9.42
-p 3.34 ± 2.30 0.021337 ± 0.0043
50 559.26 ± 64.08 15.77 ± 8.66 3.55 ± 1.64 0.022069 ± 0.0014
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Table 2 Comparison of mechanical properties of DSSFs with popular synthetic fibers

Mechanical Properties

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Tensile Young’s
Fiber Strain to References
strength modulus

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failure (%)
(MPa) (GPa)
Current
DSSFs 437-785 4.80-22.07 3.34-9.11
-p Study
E-glass 2000 - 3500 70 2.5 [18]
S-glass 4570 86 2.8 [18]
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Carbon 2400 - 4000 230 - 400 1.4 – 1.8 [18]
Aramid 3000 - 3150 63 – 67 3.3 – 3.7 [18]
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Table 3 Comparison of the chemical and tensile properties of DSSFs with other natural fibers.

Chemical Properties Tensile Properties

Lignin (Wt.

Content (Wt.
(Wt.

(Wt.

Elongation at
break (%)
Cellulose

Cellulose

Moisture

Modulus
Young’s

Reference
Sl.

strength
(Wt. %)

(Wt. %)

Tensile

(MPa)

(GPa)
Hemi
Name of Fiber

%)

%)

%)

%)
No.

Wax

Ash
o f
437.21 ± 47.83 - 4.80 ± 2.02 - 3.34 ± 2.30 - Current

o
1 DSSFs 63.3 11.6 15.3 0.81 4.57 6.02
785.34 ± 86.14 22.07 ± 9.42 9.11 ± 3.54 Study

p r
-
2 Aerial roots of banyan tree 67.32 13.46 15.62 0.89 3.96 10.21 19.37±7.72 1.8±0.4 1.8±0.4 [32]

3 Areca fruit Husk

57.35-
58.21
13-
15.42
23.17-
24.16
0.12
r e- 7.32 147-322 1.124-3.155 10.23-13.15 [44]

4 Coccinia Grandis Stem 63.22 - 24.42

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0.32 - 9.14 424.24-774.64
26.515-
123.51
5.6-16 [18]

5 Coccinia Grandis.L 62.35 13.42

a
15.61 0.79 4.38 5.6 273 ± 27.74 10.17 ± 1.261
2.703 ±
[12]

rn
0.2736
6 Cissus Quadranularis Root 77.17 11.02 10.45 0.14 7.3 - 1857-5330 68-203 3.57-8.37 [15]
7 Cissus Quadranularis stem 82.73

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7.96 11.27 0.18 6.6 - 2300-5479 56-234 3.75-11.14 [23]
8
9

10
Dracaena reflexa
Furcraea Foetida
Ficus Religiosa tree root
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70.32
68.35

55.58
11.02
11.46

13.86
11.35
12.32

10.13
0.23
0.24

0.72
6.23
6.53

4.86
5.19
5.43

9.33
829.6
590.45-623.52

433.32 ± 44
46.37
5.99-6.52

5.42 ±2.6
2.95
10.32-10.82

8.74±1.8
[3]
[17]

[45]
fiber
11 Prosopis juliflora bark 61.65 16.14 17.11 0.61 5.2 9.48 558 ± 13.4 - 1.77 ± 0.04 [25]
Saharana Aloe Vera Cactus
12 60.2 14.2 13.7 1.5 3.4 7.6 621.8 40.03 2.47 [26]
Leaves
13 Tamarindus Indica 72.84 11 15.3 0.2 - 6.3 1137-1360 11.2 - 20.7 6.5 - 10.1 [31]

14 Thespesia populnea barks 70.12 12.64 16.34 0.76 1.80 10.83 557.82 ± 56.29 20.57± 4.46 2.80 ± 0.56 [32]
15 Areca palm leaf stalk 57.49 18.34 7.26 0.71 1.43 9.35 364.6 ± 21.4 9.39±1.1 3.47±1.1 [42]
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Table 4 Comparison of the physical, crystalline and thermal properties of DSSFs with other natural fibers.

Physical Properties Crystalline Properties Thermal Properties

Diameter (μm)

Reference
Temperature
Crystallinity

Crystallinity

Degradation

Energy (Ea)
Activation
Index (%)

Size (nm)

Stability

(kJ/mol)
Thermal
Density
Sl.

(g/cm3)

(⁰ C)

(⁰ C)
Max.
Name of Fiber
No.

o f
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Current
Study
1 DSSFs 158-169 1.43 ± 0.018 58.15 11.92 230 332 73.2

2 Aerial roots of banyan tree 0.09- 0.14 1.234

- p
72.47 6.28 230 358 72.65 [32]
3 Areca fruit Husk 396-476 0.7-0.8
re 55.5 7.9 240 325.8 64.54 [44]
4 Coccinia Grandis Stem 543-621

l
1.5175
1.243 ± P 46.09 1.91 250 320 82.3 [18]
5 Coccinia Grandis.L 27.33 ± 0.3789
a 0.022
52.17 13.38 213.4 351.6 67.02 [12]
6
7
Cissus Quadranularis Root
Cissus Quadranularis stem
610-725

u
770-870 rn 1.51
1.22
56.6
47.15
7.04
31.55
230
270
328.9
342.1
74.18
65.23
[15]
[23]
8
9
10
Dracaena reflexa
Furcraea Foetida
Ficus Religiosa tree root
fiber
J o 176.2
12.8
25.62
0.79
0.77
1.246
57.32
52.6
42.92
19.01
28.36
5.18
232.32
270
325
348.7
320.5
400
68.78
65.64
68.02
[3]
[17]
[45]
11 Prosopis juliflora bark 20 0.58 46 15 217 331 76.72 [25]
Saharana Aloe Vera
12 91.15 1.325 52.6 5.6 238 350 60.2 [26]
Cactus Leaves
13 Tamarindus Indica 564-789 1-1.2 55 5.68 238 360 61.3 [31]
59.85 -
14 Thespesia populnea barks - 1412 48.17 3.576 245.4 323.7 [32]
73.01
Areca palm leaf
15 285-330 1.09±0.02 - - 279 365 - [42]
stalk
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Figure Captions:

Fig. 1. (a) Derris Scandens plant stem, insets - leaf and fruit (b) Water retting of DS chopped

stems (c) Peeling of fiber from stem (d) Drying by sunlight (e) Extracted DSSFs

Fig. 2. (a) Transverse section of DSS showing secondary phloem, secondary xylem, vessels

and fibers (4X) (b) An enlarged DSS segment exhibiting vessel surrounded by sclerenchyma

and gelatinous fibers (20X) (c) Magnified view of the single vessel covered by gelatinous

fibers groups and sclerenchyma (40X) (d) Expanded view of fiber cell’s gelatinous wall,

secondary wall, middle lamella, primary wall, and cell lumen (40X) (e) Longitudinal view of

of
single gelatinous fibers (f) Longitudinal section of DSS showing fiber bundles with phloem

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ray, procumbent cell, upright cell and sieve element (20X)
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Fig. 3. (a) X-ray diffraction, (b) FTIR spectrum acquired from DSSFs
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Fig. 4. XPS spectra of C1s peaks belong to the DSSFs

Fig. 5. Surface topography images (a) 2D and (b) 3D of DSSFs using Atomic force
lP

microscopy
in non-contact mode.
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Fig. 6. FE-SEM images of DSSFs in cross sectional view (a-c) and top surface view (d-f).

Fig. 7. Contact angle measurement of DSSFs

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Fig. 8. Stress-Strain curves of DSSFs

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Fig. 9. Weibull distributions for the probability of survival corresponding to (a) Diameter
(b)Tensile strength (c) Young’s modulus and (d) Strain at the break.

Fig. 10. (a) TGA and DTA thermogram of DSSFs and (b) Broido’s Plot of DSSFs.
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Journal: International Journal of Biological Macromolecules

Manuscript ID: IJBIOMAC-D-20-04058

Title: Characterization of a new natural cellulosic fiber extracted from Derris scandens stem

Authors: C. Ilaiya Perumal, R. Sarala

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Author Statement:

C. Ilaiya Perumal : Conceptualization, Resources & Visualization, Data curation,

Resources &Validation, Investigation, Writing original draft and review.

R. Sarala: Methodology & Supervision.

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Highlights:
 New natural cellulosic fiber extracted from Derris scandens stem.
 Anatomical, chemical, physical and thermal properties of DSSFs studied.
 XRD and FTIR analyses exhibit the presence of cellulose in DSSFs.
 The surface characteristics of DSSFs were studied by SEM, AFM and XPS
respectively.

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