International Journal of Biological Macromolecules 135 (2019) 69–76

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International Journal of Biological Macromolecules

journal homepage: http://www.elsevier.com/locate/ijbiomac

Characterization of natural fiber obtained from different parts of date

palm tree (Phoenix dactylifera L.)
Majed D. Alotaibi a, Basheer A. Alshammari b, N. Saba c, Othman Y. Alothman d, M.R. Sanjay e,
Zeyad Almutairi f, Mohammad Jawaid c,d,⁎
a
Life Science and Environment Research Institute, King Abdulaziz City for Science &Technology, P.O. Box 6086, Riyadh 11442, Saudi Arabia
b
Materials Science Institute, King Abdulaziz City for Science and Technology, P.O. Box 6086, Riyadh 11442, Saudi Arabia
c
Department of Biocomposite Technology, Institute of Tropical Forestry and Forest Products (INTROP), Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia
d
Department of Chemical Engineering, College of Engineering, King Saud University, P.O. Box 800, Riyadh 11421, Saudi Arabia
e
Department of Mechanical Engineering, Ramaiah Institute of Technology, Bengaluru, Karantaka, India
f
Department of Mechanical Engineering, College of Engineering, King Saud University, P.O. Box 800, Riyadh 11421, Saudi Arabia

a r t i c l e i n f o a b s t r a c t

Article history: The current study is motivated by the strict environmental regulations regarding the utilization and consumption
Received 21 February 2019 of ecofriendly materials. In this context, the aim of this study has been to prepare and characterize different date
Received in revised form 9 May 2019 palm tree (Phoenix dactylifera L.) fibers processed through the conventional water retting method. The chemical,
Available online 19 May 2019
elemental, crystallinity, thermal and morphological characterization of trunk (DPTRF), leaf stalk (DPLST), sheath
or leaf sheath (DPLSH) and fruit bunch stalk (DPFBS) fibers was carried out. Chemical analysis revealed that the
Keywords:
Data palm tree
four types of date palm fibers display noteworthy differences in the content of cellulose, hemicellulose and lignin.
Sheath fibers Also, the amount of calcium is relatively high in all the date palm fibers; besides this, DPTRF exhibited 69.2% crys-
Crystallinity index tallinity, which is lower than that of DPLSH with 72.4% crystallinity. Moreover, DPLST and DPFBS fibers are more
Particle size distribution thermally stable (higher thermal degradation temperature) than DPTRF and DPLSH samples. Morphological anal-
Morphological properties ysis revealed that the fracture surface of DPFBS was relatively rougher, which would probably lead to increased
Thermal stability bonding strength with polymers in composites. Overall, we conclude that DPFBS would be promising alternative
sustainable and biomass material for the isolation of respective cellulose nanofibers and cellulose nanocrystals as
potential reinforcement in polymer composites.
© 2019 Elsevier B.V. All rights reserved.

1. Introduction
The high global demand for natural wood and its limited resources
have driven researchers and industries towards the usage of non-
wood materials, such as non-timber materials, wood byproducts and
agricultural residues [1–4]. Interestingly, the global production of
wood-based products reached 263.7 million in 2011, with 1.25 million
and 33.08 million reported for Europe and North America, respectively
[5]. Research efforts in this area have focused on less used varieties of
wood to lessen the environmental impact. Also, widening the range of
raw materials encourages smaller producers to lean on naturally occur-
ring plant species in the respective countries, without affecting the tim-
ber supply and having a detrimental effect on the environment. Some of
the materials that have received increased research attention include
wheat straw and corn pith [6], kiwi stalks [7], almond shell [8], hazelnut
products [9], clipped waste grass [3], tomato stalk [2], peanut products
⁎ Corresponding author at: Biocomposite Technology Laboratory, INTROP, Universiti
Putra Malaysia, 43400 UPM, Serdang, Selangor, Malaysia.
E-mail address: jawaid@upm.edu.my (M. Jawaid).
[10], cotton products [11], flax shiv [12], castor [13], peanut hulls [14],
eggplant [15], bagasse [16], palm leaves [17,18], betel palm [19], date
palm branches [20] and wastes of oil palm fruit [21,22]. The findings in-
dicated that the use of these plant materials is sustainable for countries
with adequate supply. Likewise, harvesting from trees growing on farms
and along the streets may supplement direct timber harvesting.
The Kingdom of Saudi Arabia (KSA) has a little natural forest area, es-
timated to ~2.1 M hectares, representing 1.3% of the KSA's land area
[23], and the scarcity of forested areas has required the KSA to rely on
imported wood to meet wood demands [24]. The growing demand for
wood products, including particleboard, wood-based fibers and their
composite products, imposed on the Kingdom is substantial – of
$476.8 USD million [23,25]. Environmental initiatives have restricted
harvesting from now protected forests, further limiting supply [26].
Therefore, to decrease import costs and the deforestation impact, plant-
ing fast-growing tree species, which offers a renewable resource of raw
material and is overlooked in other production processes, greatly bene-
fits the Saudi timber supply [4]. About 1% of the Saudi forests found po-
tential for yearly harvesting, which would provide between 55 and 70
thousand tons of wood [27,28]. One of the naturally occurring forest

https://doi.org/10.1016/j.ijbiomac.2019.05.102
0141-8130/© 2019 Elsevier B.V. All rights reserved.
70 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76
trees in the KSA is Athel, or Tamarix aphylla, which is ideal for use in
wood composite production [29]. The raw material supply can be also
supplemented by the use of plant residues already available in the
Saudi forests [17,30]. Interestingly, several Saudi research initiatives
have focused on the use of renewable resources to fabricate particle
boards [17]. Additionally, research has also investigated employing
natural residues, such as the tree pruning wastes of date palm tree,
Acacia salicina, Conocarpus erectus, Ficus altissima, Leucaenaglauca,
Pithecellobium dulce and Tamarix aphylla, in the production of biomass
energy, multi-layer composite board and cement reinforced/bonded
particleboard [23,29,31,32].
Among them, the date palm (Phoenix dactylifera L.) benefits from
higher acceptance in the Arabian region. The date palm tree is a member
of the palm tree family (Arecaceae) [33] and is the most significant in-
digenous wild desert agricultural crop cultivated in native harsh envi-
ronment [34]. It is considered the third most important palm species
in the global agricultural industry, after coconut and oil palms [35].
Date palm is found abundantly in the dry and semi-arid regions of the
world, including Saudi Arabia, Northern Africa, Pakistan, India, and the
United States [36,37]. Moreover, it is also regarded as the dominant con-
stituent of the sustainable biophysical and socio-economic structures of
the oasis ecosystem [34]. It has been established by many researchers
that Egypt, Iran, Saudi Arabia United Arab Emirates, Pakistan, Algeria
and Sudan are the largest producers, as they have been the most highly
productive countries over the last years [38,39].
Different residues remain during date palm tree cultivation and fruit
harvesting around the globe, including leaf stalks, bunch stalks, rachis
and tree trunks [40]. Date palm trees bear fruit 4–8 years after planting
and require a further 7–12 years to produce commercially viable yields
[41]. Each year, the tree is pruned, including trimming of around 10–30
new leaves, which leads to substantial waste generation [41]. Notably,
Fig. 1. Visual of date palm leaf sheath.
huge amounts of N15,000 metric tons of date palm leaves and trunk
are generated as wastes in Saudi Arabia alone [36].
Besides the fibers originating from abundant natural resources, such
as those derived from leaf stalk, tree trunk and fruit stalk, the develop-
ment and utilization of date palm leaf sheath fiber have been increas-
ingly explored [39]. Nowadays, the date palm leaf sheath has become
a frequent raw material for extracting fibers [33]. The sheath is the
part of the tree that surrounds the trunk of the plant attached to its lat-
eral edges near the top of the trunk, as displayed in Fig. 1 [41]. Thus, the
date palm leaf sheaths originate from the stem and surround it layer by
layer. Currently, the fibers from the leaf sheaths are utilized for ropes
and baskets, but also for the reinforcement of composite materials
[41]. Other biomass residues generated from palm tree pruning are cur-
rently used in a variety of applications, such as the manufacture of par-
ticle board, low and medium density fiber board, and in pulp and paper
industries [33].
Until now, several studies on different Phoenix dactylifera L. tree
parts have been reported, some of the recent published research
works are tabulated in Table 1. From Table 1, it is evident that pruning
of trees along Saudi streets and on farms can also yield large amounts
of viable biomass palm material every year, which can be used for
wood, plastics composites and paper production to restrain both the en-
vironmental impact and the cost of importing.
The present study was conducted to investigate the utility of plant
residues and wood byproducts for supplementing the Saudi timber sup-
ply. The major objective of this research was to determine the standard
of the products obtained by date palm pruning and their potential for
industrial use, through systematic characterization and interpretation
of the data. This experimental work evaluated and compared the
results obtained by chemical analysis, particle size distribution analysis,
X-ray diffraction (XRD), scanning electron microscopy (SEM) and
 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76
Table 1
Recent published research studies on date palm tree fibers.
Parts of date palm tree (Phoenix dactylifera L)
Extraction and characterization of 3 different date palm water
insoluble fibers: Barhee, Sultana and Owadi
Twenty Pakistani date palm from nine different geographical regions
A comprehensive review on date palm fibers
Date palm seeds from the Regional Centre for Research in Oasis
Agriculture (Degach, Tunisia)
Chemical structure of anatomical parts of date palm, namely trunk,
frond base, frond midrib, leaflets, coir, fruit stem, date stone and
fruit empty bunches
Seeds of the fruit of the date palm
Date palm tree fruit
Date palm fresh mature leaflets
Date palm leaf sheath fibers
Date palm fruit stalks
Date palm leaf sheath fiber from Eastern Province of Saudi Arabia
Oman Date palm leaves (or leaflets)
Date palm leaf sheath (tree stem) fibers from Eastern Province of
Saudi Arabia
Date palm rachis from (Monastir) Tunisia
thermogravimetric analysis (TGA) of date palm trunk (DPTRF), leaf stalk
(DPLST), leaf sheath (DPLSH) and fruit bunch stalk (DPFBS) fibers to as-
sess their potential as renewable materials for industrial applications.
The obtained results will provide an insight into the suitability of
these fibers for extracting nanocellulose.
2. Materials and methods
2.1. Preparation of Samples
In this study, pruning residue materials were obtained from date
palm tree trunk, leaf stalk, leaf sheath and fruit bunch stalk. The date
palm pruning residues were collected from the streets in Riyadh,
Saudi Arabia. Primarily, the collected raw materials were cleaned with
tap water properly to remove any attached dust and impurities. After-
wards, the date palm materials were immersed in a vessel filled with
fresh water for 5 days at atmospheric temperature for retting. After
5 days, the fibers were dried in an oven at 70-80 °C for 3 days. The
dried fibers were then ground to fine powder using a coffee grinder
for experimentation [48].
2.2. Chemical composition analysis
The chemical composition of all the date palm fibers was analyzed
according to the standard methods of the Technical Association of
Pulp and Paper Industry (TAPPI). The analytical method used for deter-
mining the contents of cellulose and lignin involved crushing of the bio-
mass samples and extraction for 5–6 h in an ethanol–benzene solution
at a ratio of 1:2 (v/v of biomass to the solvent) in a soxhlet apparatus,
as per TAPPI standard (T264 om-97) [49] to remove resins, waxes, ste-
rols, fats, fatty acids, tannins, gums, sugars and other colored matter
[50,51]. This step was then followed by chemical analysis of the ex-
tracted residue. The hemicellulose and cellulose contents of the fibers
were determined by using a sodium chlorite (NaClO3) and sodium hy-
droxide (NaOH) mixture solution according to TAPPI Standard (T203
OS-74) [52,53]. The hemicellulose was calculated by the difference be-
tween the holocellulose and cellulose quantities, as shown below:
%Hemicellulose ¼ %Holocellulose−%Cellulose
The lignin (acid-insoluble) content of the fibers was determined by
extracting the residue in a sulphuric acid (H2SO4) solution of 72% as
per TAPPI Standard (T222 om-83) [54–56].
71
2.3. Thermo-gravimetric analysis (TGA)
References TGA is the thermal technique in which the heat flow and mass
[42]
losses of the sample are monitored against temperature or time,
while the temperature is programmed. TGA was carried out using a
[43] Q50-TA thermogravimetric analyzer to determine the thermal sta-
[36] bility of all the date palm fibers. For analysis, the samples were
[44]
heated from room temperature to 500 °C under nitrogen atmosphere
[45] at 10 °C/min [52].
2.4. X-ray fluorescence (XRF) spectroscopy
[35]
[38]
[46]
The chemical composition of all the date palm samples was investi-
[39] gated by X-ray Fluorescence Spectroscopy, using a JPS – 9200 (JGOL),
[40] with standard Mg-Kα radiation as the X-ray source.
[33]
[37]
2.5. X-ray diffraction (XRD)
[41]
[47] The crystallinity of all the date palm samples was studied using a D8-
Advance (Bruker) XRD, with CuKα radiation (=0.1541 nm) in the 2θ
range of 5°–40° at a scanning speed of 2 °C/min. The empirical method
was used to obtain the crystallinity index (CI) of the samples [57], as
shown in Eq. (1):
I200 −I am
CI ¼ ð1Þ
I200
where, I200 is the crystalline peak corresponding to the intensity of ap-
proximately 22.8° and Iam is the amorphous peak corresponding to the
intensity of approximately 19.0°.
2.6. Particle size analysis
A particle size analyzer uses a gas laser as a coherent light source
that traverses a sample. The particle size distribution (PSD) is calcu-
lated from the intensity variations within the diffraction pattern at
infinity [58]. The particle size distributions of date palm fibers
were determined by a dynamic light scattering (DLS) Zetasizer
Nano ZS. This instrument can detect the PSD in the range of
0.02–2000 μm.
2.7. Scanning electron microscopy (SEM)
The morphology of the dried date palm fiber samples was ob-
served using a Hitachi S-3400N scanning electron microscope at an
accelerating voltage of 15 kV. Prior to scanning, the samples were
sputter-coated with platinum in order to avoid any possible charging
effect.
3. Results and discussion
3.1. Chemical composition
The chemical composition of all four types of fibers obtained from
date palm tree prunings is summarized in Table 2. From Table 2, it
may be concluded that there is a noteworthy difference between the
fiber samples with regard to the amounts of cellulose, hemicellulose
and lignin. For the sake of comparison, the chemical compositions of
other wood and non-wood materials [33,39,41,47,55,59,60] are also
tabulated in Table 2.
However, it can be noted that the hemicellulose content in DPTRF is
relatively low, compared to the lignin contents in the other samples. In
addition, the lignin content in DPFBS is relatively low, compared to the
lignin contents in the other samples. Nasser et al. [45] has reported a
similar observation with regard to the chemical composition of date
palm timber. Also, these results are in partial agreement with the
72 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76

Table 2
Comparative chemical compositions of date palm fibers and biomass/natural fibers.

Date palm fibers/biomass Cellulose (%) Hemicellulose (%) Lignin (%) Moisture Volatile matter Ash (dry matter)

DPLST 35.00 15.40 20.13 15.6 73.05 12.6

DPFBS 44.00 26.00 11.45 9.6 84.11 1.85
DPLSH 43.50 24.00 18.00 6.8 78.13 7.73
DPTRF 40.00 9.75 29.48 5.7 79 3.67
Tunisia Phoenix dactylifera leaves [47] 33.5 59.5 27 – – 6.5
Posidonia oceanica sea grass [47] 40 61.8 29.8 – – 12
Brutia pine wood [47] 47 28.5 26.1 – – 0.4
Holm Oak wood [47] 43 28.3 16.3 – –
Olive wood [47] 41.5 24.33 15.64 – – 1.4
Retama monosperma (non wood) [47] 43 29.0 21.5 – – –
Banana pseudo-stems (non wood) [47] 40 25.2 12.7 – – 14
Arundo donax (non wood) [47] 29.2 32.1 20.9 – – 4.8
Softwood [55] 30–60 – 21–37 – – b1
Hardwood [55] 31–64 – 14–34 – – b1
Malaysian kenaf (bast +core) [55] 53.8 51.83 [59] 14.38–21.2 – – 4–4.69
Malaysian oil palm empty fruit bunch fibers [60] 43.70 29.02 13.33 – – 3.31
Saudi Arabia (Eastern Province) date palm Leaf sheath fiber [41] 45.1 ± 3.4 27.7 ± 1.5 16.9 ± 0.3 – – 1.7 ± 0.1
Eastern Province of Saudi Arabia Date palm fiber [33] 46 18 20 – – 10.54
Egypt raw date palm sheath fibers [39] 42.66 ± 1.63 – 20.74 ± 1.46 – 5.30 ± 0.30 1.37 ± 0.06

Note: Trunk fiber (L), leaf stalk (A), sheath or leaf sheath (G) and fruit bunch stalk (AA).

findings of some other previously published studies. Ghori et al. [36]
who examined date palm fibers and their polymer composites, reported
that the holocellulose content, comprising cellulose and hemicellulose,
in date palm fiber constituted 60–75%, while the lignin content was
~20%. In addition, similar elemental compositions were observed by
other researchers reporting rich amounts of potassium, calcium and
magnesium, but low sodium content in date palm fibers [42,45]. More-
over, the lignin contents of DPLSH, DPLST and DPTRF were also found to
be in the range of those of other wood species and non-wood plants. The
lignin % for DPLSH and DPTRF fibers ranged between 18 and 30, as also
reported by other researchers for Iraqi phoenix date palm pruning
woods (17.6 to 36) [61]. The ash content of the date palm biomass
was found to be relatively higher than that of bituminous coal, sawdust
and wood pellets. Comparable results were also observed for other date
palm biomass wastes, like seeds, leaves and leaf stems, by the TGA tech-
nique [45,62].
All the published studies displayed diverse results for different parts
of palm trees in terms of their lignocellulose contents, including cellu-
lose, hemicelluloses and lignin, which was primarily attributed to soil
differences and to the climatic conditions, in which the date palm
trees were cultivated.
3.2. Thermogravimetric analysis (TGA)
Thermal stability is commonly evaluated by determining the
onset temperature of thermal decomposition. Fig. 2 shows the rela-
tive thermal stabilities of the date samples fibers. From Fig. 2, it is
clear that there is no considerable weight loss up to ~250 °C in any
of the samples. As the temperature increases (N250 °C), the weight
loss also increased considerably over a small temperature range, as
seen by the sharp slopes. However, the onset temperature at which
weight loss begins is different for the fiber types under study. For in-
stance, the onset thermal degradation temperature of samples
DPTRF and DPLSH is about ~188 °C, while for samples DPFBS and
DPLST – of ~245 °C. It could be due to the different amounts of lignin
present in the samples (Table 3). Moreover, the thermal decomposi-
tion temperatures corresponding to 5% weight loss, of around 196 °C
for both DPTRF and DPLSH, while for both DPFBS and DPLST – of
about 254 °C, were close to the onset thermal degradation tempera-
tures of the samples, respectively. This indicated that the initial heat
tolerance of DPFBS and DPLST was relatively greater than that of
DPTRF and DPLSH. It has been reported that, when the temperatures
reach the range from 170 °C to 600 °C, the lignin and other inorganic
materials degrade after the thermal decomposition of hemicellu-
loses, cellulose and volatile materials [45]. Noticeably, Fig. 2 shows
that the first degradation occurred at a temperature lower than 250
°C, because of the evaporation of water/moisture and other volatiles
[62]. However, none of the samples shows a considerable weight

Table 3
TGA thermal analysis data of DPLSH, DPTRF, DPLST and DPFBS fibers.

Samples Tonset (°C)a T5 (°C)b Wloss (%)c Wresidue(%)d

DPLSH 188.4 196.1 67.4 25.1

DPTRF 187.6 195.8 69.2 23.9
DPLST 245.1 253.9 67.9 24.6
DPFBS 245.3 254.4 71.4 23.7

Notes:
a
Onset thermal decomposition temperature.
b
Thermal decomposition temperature at which 5% weight loss.
c
Maximum weight loss.
d
Fig. 2. TGA plots of DPLSH, DPTRF, DPLST and DPFBS samples. Char residue weight.
 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76
loss, which can be explained by their respective contents of moisture
and other volatiles. When the temperatures rose in the range of 250
°C–360 °C, the degradation observed corresponds to the decomposi-
tion of hemicelluloses. Interestingly, as the temperature was in-
creased to 360 °C–400 °C, the degradation occurred due to the
presence of cellulose. It can be explained by the release of non-
combustible gases, such as carbon dioxide and carbon monoxide,
present in the samples containing high cellulose content. However,
the decomposition processes of these three components are seen to
overlap, and these elements are regarded as pseudo-components,
similarly to the decomposition of other lignocellulosic materials
[45,62]. Additionally, the residual mass of the date palm fiber sam-
ples was found in the range from 20 to 30% at high temperature
(500 °C) (Table 3). This is could be attributed to the carbonaceous
residue in nitrogen atmosphere. A similar amount of residue has
been reported by other researchers [34].
In addition to this, a wide range of decomposition temperatures has
been reported by other researchers. Some researchers, who investigated
the combustion kinetics of UAE date palm tree materials [35], reported
that the lignocellulose materials and the glycosidic links of cellulose
decomposed between 300 °C and 350 °C. In another study, the re-
searchers revealed that the decomposition of lignin took place over a
wide range of temperatures up to 900 °C [45].
DPLST
DPTRF
Fig. 3. XRF spectra of DPLSH, DPTRF, DPLST and DPFBS samples.
73
Other researchers, who studied the chemical structure of differ-
ent parts of the date palm tree, also reported similar observations
[45]. They found that the hemicellulose, cellulose and lignin
decomposed in the temperature ranges of 260 °C–340 °C for hemi-
cellulose, 320 °C–380 °C for cellulose and 300 °C–580 °C for lignin,
showing their overlapping decomposition processes. Moreover, the
degree of crystallinity also influences the thermal stability of natural
fibers. Thus, when the crystallinity index of the materials increased,
the thermal degradation temperature also increased. Among the
samples, DPFBS and DPLST were found to be relatively more stable
(high thermal degradation temperature) than samples DPTRF and
DPLSH. This may be ascribed to the high crystalline region in the cel-
lulose and the intrinsic flame-retarding properties of cellulose, thus
contributing towards the high residue. Overall, the analysis results
revealed that DPFBS and DPLST fibers have good thermal stability
and might be applied in industrial manufacture of composites,
which require high resistance to elevated temperature.
3.3. X-ray fluorescence (XRF) spectroscopy
Fig. 3 shows the XRF spectra for samples DPLSH, DPTRF, DPLST and
DPFBS, while the elemental composition of all the samples was deter-
mined and summarized in Table 4. It is found from the data in Table 4
DPFBS
DPLSH
74 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76

Table 4 literature for comparing the elemental composition of date palm prun-
The elemental composition of different date palm fibers. ing, as determined in this study.
Elements (wt%) DPLST DPFBS DPTRF DPLSH

Silicon (Si) 15.64 1.04 9.56 6.49

3.4. Morphology and particle size analysis
Sulfur (S) 8.42 3.05 3.39 6.23
Chlorine (CL) 26.65 – – – SEM images of DPLSH, DPTRF, DPLST and DPFBS samples are pre-
Potassium (K) 6.02 24.25 3.778 20.544 sented in Fig. 4(a–d). The DPLSH sample shows a compactly packed
Calcium (Ca) 51.8 70.11 78.14 63.26
structure with less ruptured surface, DPTRF exhibits individualized fi-
Chromium (Cr) 0.12 – 0.21 0.32
Mn (Mn) 0.07 – 0.18 0.205 bers with irregular shape, as compared with other fibers. Among the fi-
Iron (Fe) 0.96 0.57 3.12 2.63 bers, the surface of DPLST was observed to be clearly smooth, with a few
Zinc (Zn) 0.13 – – – cracks, while a relatively rough surface was observed for the DPFBS fi-
Strontium (Sr) 0.03 – 0.1 0.08 bers. The particle size distribution of the fibers is illustrated in Fig. 5.
Zirconium (Zr) 0.04 – 0.01 –
Phosphorus (P) – 0.78 0.82 –
The volume weighted mean diameters of DPLSH, DPTRF, DPLST and
Titanium (Ti) – 0.17 0.42 – DPFBS are 331.17 μm, 175.21 μm, 252.48 μm and 294.56 μm, respec-
Nickel (Ni) – – 0.10 – tively. The DPLSH sample exhibits the highest particle size, possibly
Copper (Cu) – – 0.13 0.22 due to its apparently compacted stucture. Additionally, an asymmetrical
size distribution can be observed for the DPTRF sample, which is likely
attributed to its non-uniform shape. The sample of DPFBS presents a
larger particle size than that of DPLST. It may be explained by the
that the amount of calcium is relatively high in all the fiber samples, more cracked morphological structure associated with the DPLST sam-
compared with the other chemical elements present in them. This can ple. Nonetheless, the DPFBS fiber presents the most symmetrical parti-
be attributed to the chemical composition of the soil in which the date cle size distribution, with its well-resolved curve, as compared to that
palm trees were grown (Saudi Arabia in this study). Other elemental of the other fibers. This can impart great dispersion behaviour, which
constituents that are found in minor (trace) quantities include copper, is important in reinforcing composites.
nickel, titanium, phosphorous, zirconium, strontium, zinc, iron, magne-
sium and chromium. Researchers revealed that date fruit are good 3.5. X-ray diffraction analysis (XRD)
sources of iron and potassium, a fair source of microelements, such as
calcium, sodium, chlorine, copper, magnesium and sulfur, and a minor XRD analysis is most commonly used to determine the crystallinity
source of phosphorus [63]. Another study reported that dates contain percentage and the structure of the samples under investigation. Fig. 6
appreciable amounts of calcium, magnesium, phosphorous, potassium, exhibits the XRD patterns of DPLSH, DPTRF, DPLST and DPFBS fiber
iron and zirconium [64]. Accordingly, no results are available in the samples. Date palm fibers are basically composed of lignin,

Fig. 4. (a–d). SEM micrographs of (a) DPLSH, (b) DPTRF, (c) DPLST and (d) DPFBS at 1000× magnifications.
 M.D. Alotaibi et al. / International Journal of Biological Macromolecules 135 (2019) 69–76
Fig. 5. Particle size distribution of DPLSH, DPTRF, DPLST, and DPFBS samples.
hemicellulose and cellulose, of which cellulose is known as crystal-
line in nature, while lignin is amorphous having the benzene ring.
From Fig. 6, it is clear that all the fibers predominantly reveal their
reflections at 2θ = 16.1° and 22.8° in the diffraction spectra, indicat-
ing that the fibers are almost similar with regard to their crystalline
structure. However, DPTRF has a crystallinity of 69.2%, which is
lower than that of DPLSH – of 72.4%. This is probably caused by the
difference in lignin and hemicellulose contents in these samples.
Moreover, the main crystalline peak at about 22.8° appears as
sharp for both DPLST and DPFBS fibers. It may be attributed to the
large cellulose content in both of these fibers. The DPFBS fiber sample
possesses higher crystallinity, of 78.6%, compared to the DPLST sam-
ple, with 73.7% crystallinity. Meanwhile, DPFBS demonstrates a
slightly more intense peak at 16.1°, compared to the DPLST fibers.
Moreover, the presence of a small peak at 34.7° is only observed for
DPFBS, which is likely due to the highly exposed cellulose crystalline
structure. Thus, the highly crystalline nature of DPFBS contributes to
its rigid structure, which may favor the nanocomposite fabrication.
4. Conclusion
The current study presents the first phase in the research on date
palm fibers obtained from different tree parts, with the objective to
Fig. 6. XRD of DPLSH, DPTRF, DPLST and DPFBS samples.
75
explore and compare their chemical/elemental composition, thermal
properties and microstructure. The results of the analyses revealed
that the cellulose content was higher in DPFBS (44.00%), while the lig-
nin content was increased in DPTRF (29.48%). From XRF analysis, it
was noted that the amount of calcium was relatively high in all the
fiber samples. Also, DPTRF had a crystallinity of 69.2%, lower than that
of DPLSH with 72.4%, and the DPFBS fiber had a higher crystallinity –
of 78.6% – in comparison with DPLST, with 73.7% crystallinity. Overall,
the particle size evaluation and SEM analysis also supported the good
thermal stability of DPFBS and DPLST, compared to DPLSH and DPTRF,
and their suitability as promising sustainable materials for isolating
nanocellulose to be used as reinforcing agent in polymer composites.
Acknowledgements
The Authors would like to thank King Abdulaziz City for Science and
Technology (KACST), for characterization support and encouragement
in this work. The authors also extend their appreciation to the Interna-
tional Scientific Partnership Program ISPP at King Saud University for
funding this research work through ISPP-0011.
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