Comparative Study of Direct Red 81 Sorption using Date Pits Waste
FELLA-NAOUEL ALLOUCHE1,*, SONIA. SAADI2, SARAH. ROUMANE2, A.GHEZLOUN1
1Centre de Développement des Energies Renouvelables (CDER),
BP. 62, Route de l’Observatoire, Bouzaréah, 16340, Algiers,
ALGERIA
2Université Des Sciences et Technologie Houari Boumedienne,
Algiers,
ALGERIA
Abstract: - This study evaluates the ability of recycled date pit waste for dye sorption. The potential of natural
date pits waste (NDP) to remove direct red 81 from an aqueous solution was compared with activated date pits
(ADP) and commercial activated carbon (CAC). The effect of operating parameters such as initial pH, initial
dye concentration, and contact time were investigated in batch system. The maximum capacity of sorption
reaches 3.06 mg/g 1.29 mg/g and 19.23 mg/g for (NDP); (ADP) and (CAC), respectively, showing the
potential of natural date pits to direct red 81 removal. The pseudo-second-order kinetic model has proved
favorable for (RD81) sorption by (NDP), (ADP), and (CAC). The prepared materials were analyzed using FT-
IR spectroscopy before and after direct red 81 sorption, to detect the major functional groups related to the
sorption process.
Key-Words: - Date pit waste; dye removal; direct red 81; commercial activated carbon; sorption; kinetics;
modelling.
Received: May 15, 2023. Revised: November 18, 2023. Accepted: December 16, 2023. Published: December 31, 2023.
1 Introduction
Date palm, (Phoenix dactylifera) is a tree of the
palm family (Arecaceae) cultivated for its sweet
edible fruits called dates. The species is widely
cultivated in northern Africa, the Middle East, and
South Asia, and is naturalized in many tropical and
subtropical regions worldwide, [1]. However, from
a more industrial point of view, Algeria is one of
the world leaders in the field of date production.
This emerging sector enhances value to dates and
creates value-added products by transforming them
into a number of products, such as sugar, alcohol,
vinegar, forage, jam, drinks energy, cosmetics,
bread yeast, etc. The main by-products in date
production are date pits (DP) from date
consumption and the processing industry, which
represent about 10-15 % of the total mass of fruits,
[2]. The processing of date pits biomass has shown
its wide use for several applications such as
production of animal feed, [3], as activated carbon
for energy, [4], and much more in water treatment,
[5], [6]. Their use in human food remains very
poorly explored, with the single exception of a few
traditional applications which have been developed
in some countries, [7]. Natural materials based on
agricultural wastes have attracted more and more
interest for eco-friendly materials and
environmental care due to their renewable nature,
biodegradability, economic feasibility, and eco-
balance benefits. The method of synthesis of these
materials and their application as sorbents represent
a novelty in this field of science. For the water
treatment sector and in comparison to commercial
activated carbon for removing various toxic
pollutants, including metals and dyes, agricultural
waste is a valuable resource with a great potential
for reuse, [8]. Based on recent advances, dye
removal from wastewater and industrial aqueous
effluents is a much-explored area of research. In
general, the use of agricultural waste for dye
sorption is closely related for its chemical
composition and the availability of numerous
functional groups including hydroxyl, aldehyde,
carbonyl, carboxyl and phenolic, which allow them
to interact with pollutants present in wastewaters
through a variety of binding mechanisms and
interactions, [9]. According to the literature review,
azo dyes are commonly characterized by the
presence of the azo functional group (N=N) linking
two identical or non-identical alkyl groups
(symmetrical or dissymmetrical azo). They are
toxic, carcinogenic, and recalcitrant to biological
treatments. These dyes are the most widespread in
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terms of application, representing more than 50%
of the world's dye production, [10]. They are
widely used in the dyeing of textiles and in the
printing industry, plastics, surface treatment, and
other materials. The effluents from textile
industries are extremely concentrated in dyes. In
general, coloring waters present problems related to
color, temperature, high concentration of biological
oxygen demand (BOD5), chemical oxygen demand
(COD), and suspended solids (SS), as well as
toxicity and high conductivity. Increasing demands
for natural resources and environmental protection
(discharge standards, taxes, etc.) require
manufacturers to adopt appropriate pollution
control to reduce the impact of dyes on the
environment. The industrials have a choice of three
possibilities for treating aqueous effluents.
Depending on the case, discharges of azo dyes and
their byproducts into the natural environment after
treatment by an independent treatment plant
(internal to the industrial site). On the other hand,
after pretreatment on the industrial site, the
wastewater is discharged into a sewage plant via a
municipal or urban wastewater treatment plant
before being discharged into the natural
environment. Therefore, the treatment of industrial
dyeing wastewater can be performed by biological,
chemical, or physical methods, [11], [12]. Among
these methods for textile dyes removal, the one
selected method is often related to operating costs
and ease of design.
In this study, direct red 81 as a coloring agent,
is a most common azo dye in textile industry and
was used as one of the case studies to investigate
the potential application of date pits (DP) as a dye
sorbent. One of the main objectives of this study,
date pits were used as a sorbent to remove direct
red 81 from an aqueous solution via batch sorption
experiments under experimental conditions
including pH, initial dye concentration,
temperature, and contact time. Kinetic parameters
were determined.
2 Experimental
2.1 Materials
2.1.1 Dye
The azo dye direct red 81 (C29 H19 N5 Na2 O8 S2)
and M = 676 g mol−1 obtained from Sigma-
Aldrich company (Figure 1). The stock solution
(1000 ppm) of direct red 81 (DR81) was prepared
by dissolving the dye in 1000 mL of demineralized
water (Milli-Q). Standard solutions of the selected
concentrations were prepared by appropriate
dilution. Dye concentration was measured using a
spectrophotometer (UV–visible Thermo
ELECTRON CORPORATION) at a wavelength of
510 nm.
Fig. 1: Chemical structure of Direct red 81
2.1.2 Reagents
All chemicals and reagents used in this work are of
analytical grade purity. The solutions were
prepared using demineralized water (Milli-Q). The
following reagents were used without further
purification: Phosphoric acid (H3PO4, 85%) from
Sigma-Aldrich. The solution pH was adjusted using
appropriate amounts of 0.1 M (HCl/NaOH)
purchased from Fluka.
2.1.3 Sorbents
2.1.3.1 Date Pits Waste
The date pits waste were collected from Daglet
nour of Ouled Djallal region (Southwest of
Algeria). The collected material was first washed
with tap water to remove particles, before being
dried in sunlight for a week. The dried material was
then crushed into powder. The date pits (DP) were
sieved to form different particle sizes from small to
large as : G1 (<125 μm), G2 (125–250 μm), G3
(250–500 μm), G4 (500–710 μm), and G5 (710–
1000 μm). In this study, the G2 fraction was used
as the reference size material.
2.1.3.2 Preparation of Activated Carbon
Activated carbon was synthesized by chemical
activation of date pits. H3PO4 (20%) during 90
minutes. The impregnated material (PO/H, H3PO4)
was carbonized under airflow for 3 h at 600 °C and
the final product was filtered after several washings
with distilled water and drying at the ambient
temperature. The obtained activated date pits are
treated with HCl (0.1 N) and placed at room
temperature for 90 minutes. The collected material
is first washed several times with tap water and
then with distilled water until neutral pH. Once
washed, the samples are drained and dried in an
oven at a temperature of 105°C about 24 h.
Activated date pits (ADP) were conserved in closed
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bottles until use. For comparison, a commercial
activated carbon (CAC) was used in this study as
granular, (12-20 mesh) purchased from Sigma
Aldrich with surface area. of 650 m2.g-1
2.2 Sorption Experiments
The effect of some parameters: pH, contact time,
and initial concentration of dye was examined on
the prepared sorbent by varying parameters and
carried out in batch sorption. The sorption
experiment was obtained using experimental set up
as previously described, [13], [14].
To investigate the effect of pH on direct red 81
sorption, the pH was ranged from 2.0 to 7.0 with
an initial dye concentration of 10 mgL−1 and a
sorbent concentration of 1 g L−1. The solutions are
stirred at 150 rpm for 24 h. The pH solution was
measured using the pH-meter OHAUS (STARTER
3100) and adjusted during the experiments to the
desired value using a molar solution of HCl or
NaOH. The equilibrium time for maximum
sorption was studied in conical flasks (250 mL) of
dye solutions (5, 10, and 25 mg.L−1) at different
time intervals by adjusting the pH to a value of 2-3
with either molar solution at a constant speed of
150 rpm at 25 °C. At each time, samples are
filtrated and the absorbance data of the filtrates
were analyzed using UV–visible spectrophotometer
of the Thermo ELECTRON CORPORATION to
evaluate residual dye concentration (Ceq). For the
sorption isotherm experiments, the sorption
efficiency of direct red 81 and the sorption capacity
of different sorbents (NDP, ADP, and CAC), were
studied using 100 mL conical flasks containing 50
mL of dye solutions at the desired initial dye
concentration and pH. The sorption capacity (q, mg
DR81 g−1) was calculated by using a mass balance
with the following equations:
qeq = (C0 − Ceq) × V/m (1)
(2)
C0: initial dye concentration in mg/L.
Ce: final dye concentration at equilibrium mg/L.
m: mass of biomass in g.
V: volume of dye solution in L.
3 Results and Discussions
Figure 2, shows the UV absorption spectra profile
of direct red 81 used in this work. By examining
Figure 2, UV–Vis absorption spectroscopy was
used to determine the maximum absorbance
(maximal wavelength λmax), of direct red 81,
represented by λmax = 510 nm.
Fig. 2: Sorption spectra of Direct Red 81
3.1 pH Effect on Direct Red 81 Sorption
pH solution is an important parameter in the
sorption process as it acts directly on the surface
charge, the degree of ionization of dye as well as
the dissociation of functional groups of the
available active sites on material surfaces. Figure 3
shows the effect of pH on sorption capacity of
direct red (DR81) by natural date pits (NDP),
activated date pits (ADP) and commercial activated
carbon (CAC): the variation of pH on the
adsorption of (DR81) (a), adsorption capacity (b)
and sorption yield (c), studied under similar
operating conditions, temperature T: (25 °C), C0:10
mg DR81 L-1. As depicted in Figure 3, the removal
of direct red (DR81) decreased, with increasing pH
solution. It can be seen, that natural date pits (NDP)
have approximately the same sorption capacity as
the prepared activated date pits (ADP) from pH 2
up to pH 7. In short, comparing the sorption
capacity, it was noted that the acidic condition in
the range (pH = 2 and 3) was most suitable for
(DR81) sorption by (NDP, ADP, and CAC)
respectively. However, the removal efficiency of
direct red 81 (DR81) at pH 2 is 91.42% for natural
date pits (NDP) while for activated date pits (ADP)
the efficiency decreases significantly and reaches
17.73% for an optimum pH equal to 3. The removal
of (DR81) by (CAC) is optimal at pH 3 with
removal efficiency equal to 84.33%. According to
the literature research, date pits have an acidic
character (the pH zero charge point pHpzc is equal
to pH=5.9 and 4.01 for natural date pits and
activated carbon, respectively), [15]. Meanwhile, if
the pH is higher than pHpzc, the surface of the date
pits is negatively charged which favors the
attraction of cations and the opposite occurs when
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the pH value is lower than pHpzc. Therefore, for
this study, the optimum adsorbate solution at pH
condition was established at pH 2.0 for natural date
pits (NDP) and pH 3.0 for (ADP) and (CAC).
3.2 Isotherm
To describe the adsorption process of DR81 dye on
the studied materials for our experimental results,
the sorption isotherm was analyzed by both
empirical Langmuir and Freundlich models
respectively, [16], [17]. The batch isothermal data
relating to the equilibrium concentrations of the dye
adsorbed onto the materials are shown in Figure 4.
The relevant fitting parameters and correlation
coefficients obtained for the adsorption of DR81
are summarized in Table 1. It is clear that (CAC)
had the highest sorption capacity for direct red 81
solution. The maximum adsorption capacity qm, as
obtained by (CAC) was about 19.23 mg g–1 and
decreased from 3.06 mg g–1 in (NDP) to 1.29 mg g–1
for (ADP).
The following equation was used for
Langmuir isotherm model :
qe = KfCen (3)
where qe (mg/g) and Ce (mg/L) represent solid-
phase and liquid-phase concentrations of solute at
sorption equilibrium condition, respectively; Kf
((mg/g)/(mg/L)n) is sorption coefficient; n is
linearity index. Values where n >1 represent
favorable adsorption conditions. In most cases the
exponent between 1 < n < 10 shows beneficial
adsorption. A linearized expression of the
Langmuir model [14] follows as equation (4) :
(4)
where q0 is a constant related to the area occupied
by a monolayer of sorbate, reflecting the maximum
sorption capacity (mg g−1), Ce is the equilibrium
liquid-phase concentration (mg L−1), KL is a direct
measure of the intensity of sorption (L mg−1) and
qm is the amount sorbed at equilibrium (mg g−1). A
linearized form of the Freundlich model, [15], is
represented by equation (4):
(5)
where KF ((mg/g) (L/mg)1/n) and n are Freundlich
constants integrating all factors affecting the
adsorption process such as adsorption capacity and
intensity, respectively. The dependence of the
direct red 81 uptake (qe) on the equilibrium
concentration (Ce) in aqueous solution and the
Langmuir and Freundlich isotherm plots of direct
red 81 sorption onto natural date pits (NDP),
activated date pits (ADP) and commercial activated
carbon (CAC) at 25 °C and pH 2-3 are shown in
Figure 4 (a, b).
Under our experimental conditions, we
conclude that activation of material has no
significant impact on the prepared adsorbent. As a
result, we can say that the prepared adsorbent is
still sufficient for low dye concentrations,
particularly if we compare our results with a
commercial activated carbon, which has an average
qm. From the values of R2, it can be seen from the
fitting results that the sorption behavior of dye
(DR81) on the different date pits samples is highly
consistent with a higher R2 value (R2 > 0.99). In the
present work, sorption data is well fitted by
Freundlich isotherm equations, suggesting that the
surface of the materials is energetically
heterogeneous and multi-layer sorption. This
model considers that there are different types of
adsorption sites with different energies but with the
same entropy, distributed according to an
exponential distribution as a function of adsorption
heat. The adsorption of direct red (DR81) dye
using the natural date pits (NDP), activated date
pits (ADP), and commercial activated carbon
(CAC) is compared with other
reported materials in Table 2.
Table 1. Isotherm parameters for direct red 81 sorption
Sorbent
Langmuir
Freundlich
KL (L.mg-1)
R2
nf
kF (mg.g-1)
R2
Natural date pits (NDP)
3,067
2,99
0,745
3,52
1,455
0,952
Activated date pits (ADP)
1.29
0.525
0.890
1.4
0.99
0,898
Commercial Activated Carbon (CAC)
19,23
0,426
0.962
1,845
6,924
0,64
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The sorption capacity of direct red 81 found to
be 120.48 mg.g-1 using soy meal hull, [18]. Besides
that, a significant results on the direct red 81
sorption was 23.83 mg.g−1 obtained by Cross-
linked chitosan bead, [19]. Sorption of direct red
81 on Xanthuim strumarium demonstrated a
sorption capacity of 14.67 mg.g−1 at pH 3, [20].
The maximum sorption capacity under optimal
conditions was found to be 13.83 mg.g−1 and 6.43
mg.g−1 for both treated bamboo dust and natural
bamboo dust respectively, [21]. On the other hand,
the waste from banana pith were inspected and the
maximal direct red 81 sorption capacity was 5.92
mg.g−1, [22]. The lowest sorption capacity of 1.83
mg.g−1 at pH 3 was obtained with Pumice stone,
[23]. For sorption properties using Argemone
mexicana, sorption capacity was 16.21 mg.g−1,
[24].
3.3 Sorption Kinetics
The effect of contact time on the prepared material
compared to commercial activated carbon is shown
in Figure 5. The adsorption kinetics profile is
marked by the presence of two phases. Red direct
81 sorption by (NDP), (ADP) and (CAC)
respectively is rapid in the first 60 min, and the
adsorption capacity increase progressively during
the next 360 min with a slow rate to equilibrium.
The first phase is rapid and due to the presence of
several active sites on the surface of adsorbent. A
second, slower phase is also observed when the
adsorption sites are saturated, which requires
diffusion of the adsorbate within the pores of the
adsorbent and achieves equilibrium. The values of
the rate constants of the pseudo second order model
k2 for the Direct Red 81 dye (DR81), decrease from
0.0065 to 0.0017 mg g-1min-1 for activated date pits
(ADP), and from 0.006 to 0.00038 mg.g-1 min-1 for
commercial activated carbon (CAC). The activated
date pits (ADP) and commercial activated carbon
(CAC) show that the pseudo-second-order kinetic
model has a better correlation coefficient R2. As a
result, the model, [25], is the most suitable for
expressing the order of dye (DR81) adsorption
kinetics at various initial concentrations (Table 3).
Fig. 4: The plots of the experimental data for direct red 81 sorption onto prepared sorbent using (a) Langmuir,
and (b) Freundlich isotherm models
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Table 2. Comparison of direct red 81 (DR81) for different sorbents
Table. 3 Sorption Kinetic constant parameters at various dye concentrations
Fig. 5: Effect of contact time on direct red 81
(RD81) removal efficiency by prepared materials at
pH 2-3 for an initial concentration of 25 mg/L
3.4 FTIR Studies
Fourier transform infrared spectroscopy (FT-IR) is
an analytical method used to determine the amount
of light absorbed by the material as a function of
wavelength. In this study, FT-IR measurements
were performed before and after dye sorption, to
identify a number of absorption bands
corresponding to different functional groups
(Figure 6). The FT-IR spectroscopy of the
synthesized materials are shown in Figure 6. The
absorption bands show the presence of alkane,
aldehyde, aliphatic, ketone, aromatic, alkyle, nitro,
and ester groups in the prepared adsorbents. The
peak obtained at 2964 cm-1 and 2970 cm-1 indicates
the symmetric and asymmetric C-H stretching
vibration with high intensity belonging to the
alkane groups (CH3). In the range 2880 cm-1, we
notice the presence of a weak intensity attributed to
aliphatic -C-H groups with a C-H bond. On the
other hand, we observe an absorption of variable
intensity at the region 1696 cm-1, which confirms
the existence of the band C=O attributed to
aromatic ketone groups. Additionally, we also note
the presence of four bands of average intensity
located at 1575 cm-1 attributed to a C=C band
Sorbent
Sorption Capacity
q (mg.g-1)
pH
References
Natural date pit
Activated date pit
3.06
1.29
2
3
In this study
Commercial activated carbon
19.23
3
In this study
Soy meal hull
120.48
3
[18]
Cross-linked chitosan bead
23.83
4
[19]
Xanthuim strumarium
14.67
3
[20]
Treated bamboo dust
Natural Bamboo dust
13.83
6.43
2
2
[21]
Banana pith
5.92
2
[22]
Pumice stone
1.83
3
[23]
Argemone mexicana
16.21
2
[24]
Sorbent
C0
(mg.L-1)
Pseudo-Second-Order (PSO)
qe
(mg.g-1)
qm
(mg.g-1)
k2
(mg.g-1min-1)
h
(mg.g-1min-1)
R2
Activated date
pits
5
2,28
2,18
0,0065
0,034
0,96
10
3,73
3,53
0,003
0,044
0,988
25
5,376
5,00
0,0017
0,0497
0,921
Commercial
Activated
Carbon
5
5,15
5,26
0,006
0,166
0,995
10
9,9
9,58
0,002
0,2118
0,991
25
22,22
20,55
0,00038
0,19
0,935
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related to aromatic groups. The appearance of a C-
O bands with strong intensity located at 1212 cm-1,
suggests the existence of an acid group and the
presence of primary alcohol groups of variable
intensity. Analysis of the spectra of activated date
pits (ADP) and commercial activated carbon
(CAC) after adsorption of Direct Red 81 (DR81)
shows an almost similar profile as it does not show
any distinct peaks / absorption changes in the
spectrum. According to [26], this type of profile
explains that there were no substantial changes on
the adsorbent surface before and after dye sorption.
Based on the above results, several possibilities can
be generated between materials and dye, involving
hydrogen bonding and electrostatic interaction.
Fig. 6: FT-IR Spectra of the selected material
before and after direct red 81 (DR81) sorption
4 Conclusion
Solid waste of date pits from date palm have been
tested as a resource to obtain renewable sorbents
for the removal of textile dyes from aqueous
solutions. The experimental study showed the role
of the main parameters controlling the sorption
process including pH, contact time, and dye
concentration. For direct red 81 sorption, we noted
that increasing pH induces a decrease in the
sorption capacity by natural date pits (NDA);
activated date pits (ADP); and commercial
activated carbon (CAC) respectively which
indicates that the sorption system involves
electrostatic interactions which is the most
important mechanism. From the kinetic profiles, we
can conclude that the process is relatively fast from
the very first instants for the selected material and
follows the pseudo second-order reaction. This
work opens up several possibilities for research and
development of new sorbents from natural and
renewable origin. However, a new conditioning and
design in perspective should make it possible to
treat effluents from the textile industry with low
dye concentration compared with a commercial
activated carbon (CAC).
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WSEAS TRANSACTIONS on ENVIRONMENT and DEVELOPMENT
DOI: 10.37394/232015.2023.19.118
Fella-Naouel Allouche,
Sonia. Saadi, Sarah. Roumane, A. Ghezloun
E-ISSN: 2224-3496
1311
Volume 19, 2023
uranium (VI) uptake and extraction in
aqueous solutions. Journal of Molecular
Liquids, Vol, 273, pp. 192-202,
10.1016/j.molliq.2018.10.018.
Contribution of Individual Authors to the
Creation of a Scientific Article (Ghostwriting
Policy)
- F-N Allouche: Conceptualization-Methodology–
Investigation-Writing-Original draft-Visualization.
-S. Ait Saadi : Investigation.
- S. Roumane : Investigation.
- A. Guezloun: Visualization.
Sources of Funding for Research Presented in a
Scientific Article or Scientific Article Itself
No funding was received for conducting this study.
Conflict of Interest
The authors have no conflicts of interest to declare.
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This article is published under the terms of the
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WSEAS TRANSACTIONS on ENVIRONMENT and DEVELOPMENT
DOI: 10.37394/232015.2023.19.118
Fella-Naouel Allouche,
Sonia. Saadi, Sarah. Roumane, A. Ghezloun
E-ISSN: 2224-3496
1312
Volume 19, 2023