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Removal of nitrate ions by adsorption onto micro-particles of shrimp- shells

waste: Application to wastewater of infiltration-percolation process of the
city of Agadir (Morocco)

Article  in  Materials Today: Proceedings · September 2020

DOI: 10.1016/j.matpr.2020.08.603

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[CIDEEV_2019]

Removal of nitrate ions by adsorption onto micro-particles of

shrimp-shells waste: Application to wastewater of infiltration-
percolation process of the city of Agadir (Morocco)

M’hamed Abali1*, Abdeljalil Ait ichou1, Ahmed Zaghloul1, Fouad Sinan1, Mohamed
Zerbet1
1
Department of Chemistry, Faculty of Science, University Ibn Zohr, BP. 8106, Agadir, Morocco

Abstract

The infiltration-percolation process adopted at the M'zar wastewater treatment plant (WWTP) is a widely used
treatment process capable of depolluting and decontaminating the effluent.
The first objective of this study was to evaluate the purification performance of this treatment process with
regard to the elimination of carbonaceous pollution and nitrate ions. The obtained results confirmed that
infiltration-percolation is an advanced treatment technique for the treatment of organic pollution parameters such
as: chemical oxygen demand (COD), biochemical oxygen demand measured after five days (BOD 5) and total
suspended solids (TSS).
Nevertheless, this process contributes to the increase of nitrate ions by oxidation of nitrogen pollution at the sand
filter level; consequently, this pollutant causes serious ecological problems, such as the eutrophication
phenomenon.
Therefore, it is therefore essential to reasonably control nitrates before they are released into the environment.
The second objective of this work was to develop and valorize new low-cost, widely available and
environmentally friendly adsorbents of animal origin.
Raw shrimp shell (RSS), a biomaterial of animal origin, is abundant, available, renewable and non-toxic. It has
physicochemical properties that can induce a significant adsorptive activity. The surface micro-morphology of
the biomaterial was investigated using scanning electron microscope; while the qualitative element composition
was analyzed using energy dispersive X-ray and infrared spectroscopies.
For this reason, our research team proceeded to evaluate the effectiveness of crushed shrimp shell particles in
order to remove nitrate ions from municipal wastewater effluents.
The founded results of raw wastewater decanted (RWWD) and purified wastewater (PWW) are encouraging and
show significant purification yields: 68 % (RWWD) and 79 % (PWW) for nitrate ions.
Keywords: Domestic wastewater; Infiltration-percolation process; Adsorption; Shrimp-shells waste; Nitrate ions

1. Introduction

Nitrates are common in the environment and have caused serious ecological problems, such as lake
eutrophication [1]. This phenomenon produces aquatic environment degradation, either by changes in species
composition, harmful algal blooms or bottom anoxia [2]. It poses a serious problem for the different affected
environments. High concentration of nitrates in drinking water is harmful to human health [3].
Moreover, the nitrate ions, poses a serious threat because the presence of elevated NO 3- levels in drinking water
can induce methemoglobinemia and blue baby syndrome [4,5]. Meanwhile, the nitrates would be transformed
into toxic nitrite iron in human bodies which is the precursor of the carcinogenic nitrosoamine [6].
The high concentration of nitrogen as nitrates in the environment provokes the eutrophication of water bodies,
and results in negative consequences for public health [7].
Furthermore, nitrates are common in the environment and have caused serious ecological problems, such as lake
eutrophication and red tides [8,9]. Hence, eutrophication of aquatic environment frequently causes fish kills,
phytoplankton blooms, and deteriorates water quality [10].

* Corresponding author. Tel.:+212 662034622 ; fax: +212 05 28 22 01 00

E-mail address: mhamed.abali@edu.uiz.ac.ma

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On the other hand, competitive interactions between natural anions and dissolved organic matter can inhibit the
removal of nitrate ions [11]. However, the residual concentration of nitrate in secondary effluents is too low to
be removed through traditional biodegradation and chemical precipitation methods.
High levels of nitrate ions were produced by the oxidation of nitrogen pollution in the percolation infiltration
process adopted at the WWTP under study. Accordingly, it is imperative to develop a feasible and effective
technique to contribute to remove nitrate ions prior to discharge into aquatic ecosystems.
The implemented regulations to limit the concentration of nitrate in wastewater has triggered the introduction of
various nitrate removal technologies including adsorption [12].
In recent years, considerable attentions have been devoted to the study of different types of low-cost materials
and other waste for the adsorption of certain toxic substances to the environment. The adsorption using
biomaterials is an attractive and promising option for wastewater decontamination because of several advantages
such as convenient operation, economical practices, eco-friendly characteristic and fast adsorption rate [13,14].
A wide range of adsorbents has been developed for nitrate adsorption through various synthesis and modification
approaches. Nevertheless, insufficient removal and low regeneration ability of the existing adsorbents have
limited their practical applications. Hence, the design of effective adsorbent for nitrate-containing wastewater
treatment is still highly desired in this field [15].
Therefore, it is imperative to develop a cheap and easy-to-obtain, highly efficient and easy-to-regenerate
adsorbent. Consequently, a substantial increase in the amount of waste produced during manual and industrial
processing of seafood becoming environmental problem. Also, shrimp shells wastes are biowastes that could be
responsible for pollution of coastal areas. However, according to a previous study, this biological waste could be
valorized in order to be used as an adsorbent for the removal of mineral pollutants [16].
The study of the chemical composition of shrimp shell particles in previous work has shown that this biomaterial
is rich in proteins, polypeptides and other biomolecules such as chitin and its derivatives which are involved in
ion retention [17,18]. However, few studies have explored the selectivity of adsorption of nitrate ions from real
wastewater using residual solid waste [16].
The main purpose of this work is to improve the station's purification performance by using shrimp-shells inert
biomaterials in adsorption separation technology, which is today one of the most important separation
technologies, in order to attenuate the nitrate ions.

2. Materials and methods

2.1 Description of the wastewater treatment plant (WWTP) of M’zar

The M’zar treatment plant (30°20′28.1″N, 9°35′35.0″W) is located in the south of Agadir, Morocco; it was
founded in 2002 inside the Souss Massa national park (Fig.1).

Fig.1. Schema of M’zar WWTP

The purification mode, includes three successive treatment stages (Table 1), carried out as follows: a first stage
in which the raw water is sedimented for 3 days in the settling bassins, with a treatment capacity of 75000
m3/day, which have the role of decanting the suspended matter and the degradation of the carbonaceous organic

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matter. Secondary treatment, in which decanted water is percolated in the sand basins, which provides a
treatment capacity of 30000 m3/day, which have large dimensions.
Finally, the infiltrated water disinfected by ultraviolet radiation exposure. Their size and number depends on the
required bacteriological quality of the final effluent.
Table 1
Geometrical characteristics of the wastewater treatment process of the M’zar WWTP

Primary treatment: Secondary treatment: Tertiary treatment :

Anaerobic decantation Infiltration percolation UV disinfection
Flow 75000 m3/day Flow 30000 m3/day Flow 30000 m3/day

Number of decanters 13 Number of filters 64 Number of pumps 6

Length of decanter 115 m Filter surface 5000 m2 Number of reactors 6

Number of UV lamps per
Width of decanter 35 m Sand thickness 2m 14
reactor
Depth of the decanter 4.24 m Gravel thickness 0.5 m Exposure dose 50 mJ/cm2
Total volume of
210000 m3 Infiltration speed 1 m/day Contact time 4s
decanter

2.2 Sampling

The sampling method adopted is composite type in 24 hours in order to obtain a representative sample. Sampling
points were taken at the inlet and outlet of the treatment plant. The samples were collected in polyethylene
bottles [19]. The characterization was focused on the determination of in situ physicochemical parameters (water
temperature, pH, dissolved oxygen, electrical conductivity) which were measured on site, while the mineral
parameters and the major parameters of pollution (Five-day biochemical oxygen demand (BOD5), chemical
oxygen demand (COD) and total suspended solids (TTS) were analyzed in the laboratory using accredited
techniques and methods.
The sampling lasted from January 2014 to June 2016. During this period, we collected the wastewater at the inlet
and outlet of the WWTP in order to get an idea of the purification efficiency of the wastewater treatment plants.

2.3 Physico-chemical parameters studied

The parameters that were evaluated of this study are those on site namely: Air temperature (Alla France-type
thermometer); Water temperature and pH (portable pH-meter type WTW pH 3310 SET) [19]; Electrical
conductivity (conductivity meter type WTW Cond 3310 SET) [19]; Dissolved oxygen (portable oximeter type
WTW Oxi 3310 SET) [19]; In addition to the major pollution parameters, namely: Chemical oxygen demand
COD (colorimetric method) [20]; Biochemical oxygen demand measured after five days BOD5 (electrometric
method) [21]; Total suspended solids TSS (gravimetric method) [22]; Nitrate NO3--N (Cadmium Reduction
Method) [19].

2.4 Preparation of the adsorbent based on shrimp-shells particles

Shrimp-shells wastes were recovered at the port of Agadir (south-west Morocco). Before using it in this
exeperiment, collected wastes rinsed several times with tap water, and they were air-dried for 2-3 days and then
ground and sieved with a grain size of less than or equal to 500 μm. The study of the adsorption of NO3- ions on
shrimp-shells wastes was carried out under static conditions. This system makes it possible to have a better
contact between the adsorbent and the adsorbate, avoiding any decantation of the adsorbent. The agitation speed
was kept constant for each run to ensure equal mixing.
The ratio R = mass biomaterial /Volume of the solution (R = m/V) used in our study corresponds to the smallest
mass of biomaterial which leads to a maximum adsorption rate. In the batch adsorption experiments, 40 mL of
wastewater solution with a given ions concentration, Ci0, was mixed with 1g of micro-particles of shrimp-shells

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without any pre-treatment. The mixture being vigorously stirred with the use of a magnetic stirrer, and was
maintained in water bath thermostat at a constant temperature of 25 °C.
To find the adsorption equilibrium time, a 6 h kinetic adsorption experiment was conducted, and the nitrate
concentration was measured at different time intervals (1-360 min). The time required to reach the adsorption
equilibrium for a given initial ion concentration was determined by sampling aliquots of analyzed solution for
different times. Before analyzing the requested parameters, the resulting solutions were centrifuged at 5000 rpm
for 10 min and the supernatant was filtered through on Whatman paper of 1.2 µm porosity and the filtrate was
analyzed. The corresponding experimental and analytical tests were carried out more than 3 times to obtain
repeatable results and the average results are presented in this study. The concentrations retained Cr (mg/L) by
the equilibrium biomaterial and the quantities of adsorption Q ads (mg/g) are given by the following relationships:
C r mg / L   Ci  C eq
V
Qads (mg / g)  (Ci  Ceq ) 
m
Where m: mass of biomaterial in g; V: total volume in (L); Ci: initial concentration (mg/L);
Ceq: equilibrium concentration in (mg/L); Qads: amount adsorbed per 1 gram of biomaterial (mg/g).
The percentage of nitrate removal (%) was calculated as follows:
% Removal  (Ci  Ceq ) / Ci   100

2.5 Adsorbent characterization

The surface morphology of the shrimp shell particles was studied by Scanning Electron Microscopy (SEM,
HITACHI S-4500). The elemental analysis was analyzed by SEM coupled with energy dispersive X-ray analysis
(SEM/EDX, LEICA-S-260). The surface functional groups were detected by Fourier transforms infra-red (FT-
IR) spectrometer (Spectrum 100 Perkin Elmer). A KBr pellet containing the sample was used for the FT-IR
spectroscopic measurements and the spectra were collected in the scan range between 400 and 4000 cm -1.

3. Results and discussion

3.1 Scanning electron microscopy of the shrimp shell particles

According to the figure (Fig.2), the biomaterial is made up of large grains of different size and morphologies,
which confirms the heterogeneity of the surface of this raw biomaterial. The images also show the pore nature of
the crude ground with a diversity in the size and texture of the pores, which proves the existence of very large
internal specific surfaces. The morphology of this biomaterial can facilitate the adsorption of anions, due to the
irregular surface.

Fig.2. SEM images of shrimp shell particles [16]

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3.2 Energy dispersive X-ray spectroscopy

The figure (Fig.3), illustrates the energy dispersive X-ray spectroscopy (EDX) of biomaterial being studied, This
spectrum presents the chemical elements that make up the structure of this substance as well as their mass and
atomic percentages.
It shows that the shrimp shell particles, in addition to carbon, oxygen, the major constituents of proteins, chitin,
and bicarbonates, the main components of the shrimp shell, is also composed largely of calcium. This confirms
that the majority of bicarbonates are composed of calcium bicarbonates.

Fig.3. EDX spectrum of shrimp shell particles [16]

3.3 Infrared spectroscopy

Infrared spectroscopy provides information on the chemical structure of the adsorbent material. The FT-IR
spectra of shrimp shell particles (Fig. 4).
The figure (Fig.4), presents typical absorption bands of the biomolecules. Hydroxyl groups (OH) and amine
(NH) are represented by a broad band at 3300 cm-1 and absorption of these groups indicates an attribution to the
hydrogen bonds.
Stretching vibration corresponds to C-H are also common to both spectra. They are characterized by absorption
in the region of 2800 cm-1 and 3030 cm-1. The absorption bands in the region of 1500 and 1650 cm-1 corresponds
to carbonyl groups stretching vibrations.
The absorption bands in the region of 1030 cm-1 and 1450 cm-1 corresponds to RC-H, R-OH and amines
vibration. The broad band at 1420 cm-1 is due to mineral salts, especially bicarbonates, characterized by CC, CO
and CN groups.
The adsorption by raw shrimp shells might be attributed mainly to their surface, which contains anion binding
functional groups as carboxyl, hydroxyl and amino groups.

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Fig.4. Infrared spectrum of the raw shrimp shells in KBr

3.4 Characterization of RWWD and PWW of the WWTP of M’zar

In order to evaluate the purifying performances of the infiltration-percolation process adopted at the M'zar
WWTP. A study of the polluting load of wastewater used was carried out from January 2014 to June 2016, the
table below (Table 2) presents the physico-chemical parameters of the raw wastewater decanted (RWWD) and
purified wastewater (PWW) of the WWTP M’zar.

Table 2
Pollution load of wastewater used from WWTP M’zar

Sampling date Standard

Parameters Water type
24/01/2014 22/04/2015 17/10/2015 21/06/2016 Deviation
RWWD 21.5 22.6 22.5 26.5 35
Temperature (°C)
PWW 19.5 21 20.5 22.8 [23]
RWWD 7.85 7.67 7.75 7.84
pH 6.5-8.6 [23]
PWW 7.57 7.37 7.45 7.40
Electrical RWWD 4284 3975 4035 4125
conductivity -
(µs/cm) at 20°C PWW 3235 3145 3265 3465

Dissolved oxygen RWWD 0 0 0 0

(mg O2/L) -
PWW 4.8 4.4 4.7 4.7
RWWD 865 783 812 765
150
TSS (mg/L) PWW 8.5 9 12 13
[24]
% Elimination 99 99 99 98
RWWD 810 840 835 760
BOD5 120
PWW 35 12 15 23
(mg O2/L) [24]
% Elimination 96 99 98 97
RWWD 1767 1715 1724 1654
COD 250
PWW 98 43 59 28
(mg O2/L) [24]
% Elimination 94 97 97 98
NO3- RWWD 2.6 1.5 1.3 2.2 30
(mg-N/L) PWW 385 412 434 424 [23]

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3.5 Evaluation of the purification performance of the WWTP

Temperature is an important biologically significant factor for purified wastewater, which plays important role in
the metabolic activities of the organism. The temperature ranged from 19.5 °C to 22.8 °C during the study
period. Lowest water temperature (19.5 °C) was observed in the winter period and highest temperature (22.8 °C)
value was observed in the summer period.
The pH values of the purified wastewater varied between 7.37 and 7.57 and were within the limit prescribed by
the standard for the quality of water intended for irrigation [23].
On the other hand, the electrical conductivity, reflects the overall degree of mineralization, and provides
information on the salinity level.
The results obtained show that the electrical conductivity values of PWW vary between 3145 and 3465 µs/cm
with an average of 3277 µs/cm. While at the entrance to the WWTP they vary between 3975 and 4284 µs/cm
with an average of 4105 µs/cm (Table 2).
The qualitative analysis of the raw wastewater decanted (RWWD) shows that it has a higher concentration than
the typology of urban wastewater in Morocco in terms of BOD 5 (200-400 mg O2/L), COD (500-800 mg O2/L)
and TSS (250-500 mg/L) parameters [25].
The qualitative analysis of purified wastewater at the outlet of tertiary treatment shows that the carbon loading in
terms of COD, BOD5 and TSS complies with the specific limit values for domestic discharges [24], with
purification efficiencies of the order of 98 % for TSS, 98 % for COD and 97 % for BOD5.
Concerning nitrate ions NO3-, it can be seen that NO3- concentrations in RWWD vary from 1.3 mg/L to 2.6 mg/L
with an average of 1.9 mg/L. Previous studies have shown that nitrates are typically absent in untreated domestic
effluent [26].
On the other hand, the purified wastewater (PWW) has very high concentrations of nitrate ions, which greatly
exceed the limit value set by the Moroccan standard for water intended for irrigation, which is around 30 mg N/L
[23].
The treatment of wastewater by percolation infiltration on sand promotes bacterial transformation of organic
nitrogen and mineral nitrogen into nitrate, which leads to an increase in nitrate ions at the outlet of the WWTP.
This high concentration could present a risk leading to the phenomenon of eutrophication and disables the
recovery and use of these discharges in irrigation [27].
However, nitrate ions contribute to the excessive development of algae in the storage tanks of treated water after
UV treatment. This leads to clogging of the pipes intended for the reuse of the treated water. Eutrophication also
contributes to the reduction of oxygen levels in the water and disrupts the natural balance of the ecosystem [28].
In order to solve these problems, it is desirable to develop a lowcost and simple treatment alternative. Our study
is part of a sustainable development approach, aiming at improving the purification performance of WWTP by
introducing adsorbent biomaterials, abundant and inexpensive, hence the valorisation of the biomaterials of the
region.
To begin this study, we selected the sampling campaign of 21/06/2016 to study the adsorption of NO3- ions in
raw wastewater decanted and purified wastewater. Its results are reproducible and verifiable.

3.6 Study of adsorption of NO3- by shrimp shell particles

3.6.1 Adsorption of NO3- ions contained in the RWWD and PWW

The curves below (Fig.5 and Fig.6), show the variation of the retained concentration and the removal efficiency
of the nitrate ions contained in RWWD and PWW as a function of the contact time (R = 25 g /L, T = 25 ° C).
The adsorption equilibrium time of the shrimp shell particles was determined by performing 6-hour nitrate
adsorption tests with an initial nitrate concentration of 2.2 mg-N/L for RWWD and 424 mg-N/L for PWW.

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100
2,0 100
RWWD (Ci = 2.2 mg/L) PWW (Ci = 424 mg/L)
1,8 90
400 90
Removal efficiency (%) Removal efficiency (%)

Concentration removed (mg/L)

Concentration removed (mg/L)

1,6 80 350 80

Removal efficiency (%)

Removal efficiency (%)
1,4 70 70
300
1,2 60 60
250
1,0 50 50
200
0,8 40 40
150
0,6 30 30

0,4 20
100 20

0,2 10 50 10

0,0 0 0 0
0 30 60 90 120 150 180 210 240 270 300 330 360 390 0 30 60 90 120 150 180 210 240 270 300 330 360 390
Contact time (min) Contact time (min)
Fig.5. Effect of contact time and efficiency of nitrate ion removal by Fig.6. Effect of contact time and efficiency of nitrate ion removal by
shrimp shell particles for RWWD shrimp shell particles for PWW

The results of the adsorption study of NO3- ions contained in the RWWD and PWW are the average of three
successive reproducible and verifiable tests. The analysis of the figures (Fig.5 and Fig.6) reveals that the retained
concentration Cr of nitrate ions contained in the RWWD and PWW of the M'zar WWTP, increases with the
contact time and equilibrium is quickly reached. The time to equilibrium is around 30 min.
Moreover, the shape of the curves does not make it possible to distinguish two distinct stages of adsorption,
everything happens as if the adsorption takes place in a single very rapid step from the very first minutes of
contact. This step corresponds to the retention of ions located near the surface of the mill particles, and
consequently to a rapid diffusion of the nitrate anions to the external sites of the adsorbent surface.
Concerning removal efficiency of nitrate ions in the wastewater studied. The figures (Fig.5 and Fig.6) show that
the removal efficiency of nitrate ions in raw wastewater decanted and purified wastewater is of the order of 68 %
for RWWD and 79 % for PWW. This difference in treatment efficiency could be explained by the initial
concentration of each type of wastewater studied.

3.6.2 Purification performance of shrimp shell particles in the removal of nitrate ions contained in RWWD and
PWW.

The Percentage removal of NO3- ions at adsorption equilibrium in raw wastewater decanted (RWWD) and
purified wastewater (PWW) are presented below (Table 3).

Table 3
Percentage removal of NO3- ions at adsorption equilibrium in RWWD and PWW

Values
Initial concentration Ci (mg /L) 2.2
Concentrations retained Cr (mg /L) 1,5
RWWD
Quantities of adsorption Qads (mg/g) 0.1
Removal percentage (%) 68
Initial concentration Ci (mg /L) 424
Concentrations retained Cr (mg /L) 339
PWW
Quantities of adsorption Qads (mg/g) 14
Removal percentage (%) 79

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These results show that shrimp shell particles present high purification efficiencies with regard to the removal of
NO3- ions. These purification yields are of the order of 68 % and 79 %, respectively, for RWWD and PWW.
Analysis of these results shows that the quantity of nitrate ions retained increases with the initial concentration of
each type of wastewater studied. The efficiency of nitrate ion removal correlates with a recent study applied to
domestic wastewater with agro-food discharges like the M'zar WWTP
This study shows a nitrate ions removal rate of about 52 % with an adsorbed quantity of nitrate ions removed of
the order of 14.4 mg/g [29].

4. Conclusion

The pollutant load of the raw wastewater from the M'zar WWTP presents very high concentrations compared to
the Moroccan urban wastewater typology for the main parameters of organic pollution. This increase in
concentration is due to the connection of the industrial units of agro-food type.
For the purified wastewater of the M'zar WWTP, the purification yields recorded by the percolation infiltration
system for BOD5, COD and TSS parameters are high.
For nitrate ions, there is an increase in nitrate ions levels from the inlet to the outlet of the WWTP. This increase
is due to the oxidation of the nitrogen pollution within the sand filters. Therefore, adequate denitrification
treatment of the treated wastewater must be provided. The residual concentrations remain very high in the treated
effluent and could constitute a great risk of eutrophication for these discharges for irrigation purposes.
For that reason, the search for new unconventional cleaning processes based on biomaterials which would be
inexpensive and easy to implement is strongly recommended in order to improve the quality of purified water
according to the required standards. Moreover, the purification efficiency of NO 3- ions by shrimp shell particles
is important. Shrimp shell particles could then constitute a potential adsorbent for NO3- pollutants, given their
low cost and high retention rate. Such a process can be used in the purification of wastewater and could integrate
in the purification system of the WWTP of M'zar in order to improve the purification yield and to comply with
the Moroccan regulations in force.
This experimental study using a real wastewater showed that the removal of nitrate ions by adsorption onto
micro-particles of shrimp-shells particles is a viable and effective alternative to the use of more expensive or less
environmentally friendly treatments.

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