Materials Today: Proceedings xxx (xxxx) xxx

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Materials Today: Proceedings

journal homepage: www.elsevier.com/locate/matpr

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 Abali ⇑, Abdeljalil Ait ichou, Ahmed Zaghloul, Fouad Sinan, Mohamed Zerbet
Department of Chemistry, Faculty of Science, University Ibn Zohr, BP. 8106 Agadir, Morocco

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

Article history: The infiltration-percolation process adopted at the M’zar wastewater treatment plant (WWTP) is a widely
Received 29 June 2020 used treatment process capable of depolluting and decontaminating the effluent.
Received in revised form 20 August 2020 The first objective of this study was to evaluate the purification performance of this treatment process
Accepted 25 August 2020
with regard to the elimination of carbonaceous pollution and nitrate ions. The obtained results confirmed
Available online xxxx
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
Keywords:
days (BOD5) and total suspended solids (TSS).
Domestic wastewater
Infiltration-percolation process
Nevertheless, this process contributes to the increase of nitrate ions by oxidation of nitrogen pollution
Adsorption at the sand filter level; consequently, this pollutant causes serious ecological problems, such as the
Shrimp-shells waste eutrophication phenomenon.
Nitrate ions Therefore, it is therefore essential to reasonably control nitrates before they are released into the envi-
ronment.
The second objective of this work was to develop and valorize new low-cost, widely available and envi-
ronmentally 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 qualita-
tive 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 par-
ticles in order to remove nitrate ions from municipal wastewater effluents.
The founded results of raw wastewater decanted (RWWD) and purified wastewater (PWW) are encour-
aging and show significant purification yields: 68% (RWWD) and 79% (PWW) for nitrate ions.
Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of The International Confer-
ence on Water Depollution and Green Energy 2019.

1. Introduction environments. High concentration of nitrates in drinking water is

harmful to human health [3].
Nitrates are common in the environment and have caused seri- Moreover, the nitrate ions, poses a serious threat because the
ous ecological problems, such as lake eutrophication [1]. This phe- presence of elevated NO
3 levels in drinking water can induce
nomenon produces aquatic environment degradation, either by methemoglobinemia and blue baby syndrome [4,5]. Meanwhile,
changes in species composition, harmful algal blooms or bottom the nitrates would be transformed into toxic nitrite iron in human
anoxia [2]. It poses a serious problem for the different affected bodies which is the precursor of the carcinogenic nitrosoamine [6].
The high concentration of nitrogen as nitrates in the environ-
ment provokes the eutrophication of water bodies, and results in
⇑ Corresponding author. negative consequences for public health [7].
E-mail address: [email protected] (M. Abali).

https://doi.org/10.1016/j.matpr.2020.08.603
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of The International Conference on Water Depollution and Green Energy 2019.

Please cite this article as: M. Abali, A. Ait ichou, A. Zaghloul et al., Removal of nitrate ions by adsorption onto micro-particles of shrimp-shells waste: Appli-
cation to wastewater of infiltration-percolation process of the city of Agadir (Morocco), Materials Today: Proceedings, https://doi.org/10.1016/j.
matpr.2020.08.603
M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

Furthermore, nitrates are common in the environment and have anted water is percolated in the sand basins, which provides a
caused serious ecological problems, such as lake eutrophication treatment capacity of 30000 m3/day, which have large dimensions.
and red tides [8,9]. Hence, eutrophication of aquatic environment Finally, the infiltrated water disinfected by ultraviolet radiation
frequently causes fish kills, phytoplankton blooms, and deterio- exposure. Their size and number depends on the required bacteri-
rates water quality [10]. ological quality of the final effluent.
On the other hand, competitive interactions between natural
anions and dissolved organic matter can inhibit the removal of 2.2. Sampling
nitrate ions [11]. However, the residual concentration of nitrate
in secondary effluents is too low to be removed through traditional The sampling method adopted is composite type in 24 h in
biodegradation and chemical precipitation methods. order to obtain a representative sample. Sampling points were
High levels of nitrate ions were produced by the oxidation of taken at the inlet and outlet of the treatment plant. The samples
nitrogen pollution in the percolation infiltration process adopted were collected in polyethylene bottles [19]. The characterization
at the WWTP under study. Accordingly, it is imperative to develop was focused on the determination of in situ physicochemical
a feasible and effective technique to contribute to remove nitrate parameters (water temperature, pH, dissolved oxygen, electrical
ions prior to discharge into aquatic ecosystems. conductivity) which were measured on site, while the mineral
The implemented regulations to limit the concentration of parameters and the major parameters of pollution (Five-day bio-
nitrate in wastewater has triggered the introduction of various chemical oxygen demand (BOD5), chemical oxygen demand
nitrate removal technologies including adsorption [12]. (COD) and total suspended solids (TTS) were analyzed in the labo-
In recent years, considerable attentions have been devoted to ratory using accredited techniques and methods.
the study of different types of low-cost materials and other waste The sampling lasted from January 2014 to June 2016. During
for the adsorption of certain toxic substances to the environment. this period, we collected the wastewater at the inlet and outlet
The adsorption using biomaterials is an attractive and promising of the WWTP in order to get an idea of the purification efficiency
option for wastewater decontamination because of several advan- of the wastewater treatment plants.
tages such as convenient operation, economical practices, eco-
friendly characteristic and fast adsorption rate [13,14]. 2.3. Physico-chemical parameters studied
A wide range of adsorbents has been developed for nitrate
adsorption through various synthesis and modification approaches. The parameters that were evaluated of this study are those on
Nevertheless, insufficient removal and low regeneration ability of site namely: Air temperature (Alla France-type thermometer);
the existing adsorbents have limited their practical applications. Water temperature and pH (portable pH-meter type WTW pH
Hence, the design of effective adsorbent for nitrate-containing 3310 SET) [19]; Electrical conductivity (conductivity meter type
wastewater treatment is still highly desired in this field [15]. WTW Cond 3310 SET) [19]; Dissolved oxygen (portable oximeter
Therefore, it is imperative to develop a cheap and easy-to- type WTW Oxi 3310 SET) [19]; In addition to the major pollution
obtain, highly efficient and easy-to-regenerate adsorbent. Conse- parameters, namely: Chemical oxygen demand COD (colorimetric
quently, a substantial increase in the amount of waste produced method) [20]; Biochemical oxygen demand measured after five
during manual and industrial processing of seafood becoming days BOD5 (electrometric method) [21]; Total suspended solids
environmental problem. Also, shrimp shells wastes are biowastes TSS (gravimetric method) [22]; Nitrate NO
3 -N (Cadmium Reduc-
that could be responsible for pollution of coastal areas. However, tion Method) [19].
according to a previous study, this biological waste could be val-
orized in order to be used as an adsorbent for the removal of min- 2.4. Preparation of the adsorbent based on shrimp-shells particles
eral pollutants [16].
The study of the chemical composition of shrimp shell particles Shrimp-shells wastes were recovered at the port of Agadir
in previous work has shown that this biomaterial is rich in pro- (south-west Morocco). Before using it in this exeperiment, col-
teins, polypeptides and other biomolecules such as chitin and its lected wastes rinsed several times with tap water, and they were
derivatives which are involved in ion retention [17,18]. However, air-dried for 2–3 days and then ground and sieved with a grain size
few studies have explored the selectivity of adsorption of nitrate of less than or equal to 500 lm. The study of the adsorption of NO
3
ions from real wastewater using residual solid waste [16]. ions on shrimp-shells wastes was carried out under static condi-
The main purpose of this work is to improve the station’s purifi- tions. This system makes it possible to have a better contact
cation performance by using shrimp-shells inert biomaterials in between the adsorbent and the adsorbate, avoiding any decanta-
adsorption separation technology, which is today one of the most tion of the adsorbent. The agitation speed was kept constant for
important separation technologies, in order to attenuate the each run to ensure equal mixing.
nitrate ions. The ratio R = mass biomaterial /Volume of the solution (R = m/
V) used in our study corresponds to the smallest mass of biomate-
rial which leads to a maximum adsorption rate. In the batch
2. Materials and methods adsorption experiments, 40 mL of wastewater solution with a
given ions concentration, Ci0, was mixed with 1 g of micro-
2.1. Description of the wastewater treatment plant (WWTP) of M’zar particles of shrimp-shells without any pre-treatment. The mixture
being vigorously stirred with the use of a magnetic stirrer, and was
The M’zar treatment plant (30°200 28.100 N, 9°350 35.000 W) is maintained in water bath thermostat at a constant temperature of
located in the south of Agadir, Morocco; it was founded in 2002 25 °C.
inside the Souss Massa national park (Fig. 1). To find the adsorption equilibrium time, a 6 h kinetic adsorp-
The purification mode, includes three successive treatment tion experiment was conducted, and the nitrate concentration
stages (Table 1), carried out as follows: a first stage in which the was measured at different time intervals (1–360 min). The time
raw water is sedimented for 3 days in the settling bassins, with a required to reach the adsorption equilibrium for a given initial
treatment capacity of 75000 m3/day, which have the role of ion concentration was determined by sampling aliquots of ana-
decanting the suspended matter and the degradation of the car- lyzed solution for different times. Before analyzing the requested
bonaceous organic matter. Secondary treatment, in which dec- parameters, the resulting solutions were centrifuged at 5000 rpm
2
M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

Fig. 1. Schema of M’zar WWTP.

Table 1
Geometrical characteristics of the wastewater treatment process of the M’zar WWTP.

Primary treatment: Anaerobic decantation Secondary treatment: infiltration Tertiary treatment : UV disinfection
percolation
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
Width of decanter 35 m Sand thickness 2m Number ofUV lamps per reactor 14
Depth of the decanter 4.24 m Gravel thickness 0.5 m Exposure dose 50 mJ/cm2
Total volume of decanter 210000m3 Infiltration speed 1 m/day Contact time 4s

for 10 min and the supernatant was filtered through on Whatman 3. Results and discussion
paper of 1.2 mm porosity and the filtrate was analyzed. The corre-
sponding experimental and analytical tests were carried out more 3.1. Scanning electron microscopy of the shrimp shell particles
than 3 times to obtain repeatable results and the average results
are presented in this study. The concentrations retained Cr (mg/ According to the figure (Fig. 2), the biomaterial is made up of
L) by the equilibrium biomaterial and the quantities of adsorption large grains of different size and morphologies, which confirms
Qads (mg/g) are given by the following relationships: the heterogeneity of the surface of this raw biomaterial. The
images also show the pore nature of the crude ground with a diver-
C r ðmg=LÞ ¼ Ci
C eq
sity in the size and texture of the pores, which proves the existence
of very large internal specific surfaces. The morphology of this bio-
V
Q ads ðmg=gÞ ¼ ðC i
C eq Þ  material can facilitate the adsorption of anions, due to the irregular
m
surface.
where m: mass of biomaterial in g; V: total volume in (L); Ci: initial
concentration (mg/L);
3.2. Energy dispersive X-ray spectroscopy

Ceq: equilibrium concentration in (mg/L); Qads: amount

The figure (Fig. 3), illustrates the energy dispersive X-ray spec-
adsorbed per 1 g of biomaterial (mg/g).
troscopy (EDX) of biomaterial being studied, this spectrum pre-
The percentage of nitrate removal (%) was calculated as follows: sents the chemical elements that make up the structure of this
  substance as well as their mass and atomic percentages.
%Remov al ¼ ðC i
C eq Þ=C i  100 It shows that the shrimp shell particles, in addition to carbon,
oxygen, the major constituents of proteins, chitin, and bicarbon-
2.5. Adsorbent characterization ates, the main components of the shrimp shell, is also composed
largely of calcium. This confirms that the majority of bicarbonates
The surface morphology of the shrimp shell particles was stud- are composed of calcium bicarbonates.
ied by Scanning Electron Microscopy (SEM, HITACHI S-4500). The
elemental analysis was analyzed by SEM coupled with energy 3.3. Infrared spectroscopy
dispersive X-ray analysis (SEM/EDX, LEICA-S-260). The surface
functional groups were detected by Fourier transforms infra-red Infrared spectroscopy provides information on the chemical
(FT-IR) spectrometer (Spectrum 100 Perkin Elmer). A KBr pellet structure of the adsorbent material. The FT-IR spectra of shrimp
containing the sample was used for the FT-IR spectroscopic mea- shell particles (Fig. 4).
surements and the spectra were collected in the scan range The figure (Fig. 4), presents typical absorption bands of the bio-
between 400 and 4000 cm
1. molecules. Hydroxyl groups (OH) and amine (NH) are represented
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M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

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

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

by a broad band at 3300 cm
1 and absorption of these groups indi- 3.4. Characterization of RWWD and PWW of the WWTP of M’zar
cates an attribution to the hydrogen bonds.
Stretching vibration corresponds to CAH are also common to In order to evaluate the purifying performances of the
both spectra. They are characterized by absorption in the region infiltration-percolation process adopted at the M’zar WWTP. A
of 2800 cm
1 and 3030 cm
1. The absorption bands in the region study of the polluting load of wastewater used was carried out
of 1500 and 1650 cm
1 corresponds to carbonyl groups stretching from January 2014 to June 2016, the table below (Table 2) presents
vibrations. the physico-chemical parameters of the raw wastewater decanted
The absorption bands in the region of 1030 cm
1 and (RWWD) and purified wastewater (PWW) of the WWTP M’zar.
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 bicar- 3.5. Evaluation of the purification performance of the WWTP
bonates, characterized by CC, CO and CN groups.
The adsorption by raw shrimp shells might be attributed mainly Temperature is an important biologically significant factor for
to their surface, which contains anion binding functional groups as purified wastewater, which plays important role in the metabolic
carboxyl, hydroxyl and amino groups. activities of the organism. The temperature ranged from 19.5 °C
4
M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

Concerning nitrate ions NO

3 , it can be seen that NO3 concentra-
tions 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 irriga-
tion, 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 phe-
nomenon of eutrophication and disables the recovery and use of
these discharges in irrigation [27].
However, nitrate ions contribute to the excessive development
Fig. 4. Infrared spectrum of the raw shrimp shells in KBr. 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
to 22.8 °C during the study period. Lowest water temperature oxygen levels in the water and disrupts the natural balance of
(19.5 °C) was observed in the winter period and highest tempera- the ecosystem [28].
ture (22.8 °C) value was observed in the summer period. In order to solve these problems, it is desirable to develop a
The pH values of the purified wastewater varied between 7.37 lowcost and simple treatment alternative. Our study is part of a
and 7.57 and were within the limit prescribed by the standard sustainable development approach, aiming at improving the purifi-
for the quality of water intended for irrigation [23]. cation performance of WWTP by introducing adsorbent biomateri-
On the other hand, the electrical conductivity, reflects the over- als, abundant and inexpensive, hence the valorisation of the
all degree of mineralization, and provides information on the salin- biomaterials of the region.
ity level. To begin this study, we selected the sampling campaign of
The results obtained show that the electrical conductivity val- 21/06/2016 to study the adsorption of NO
3 ions in raw wastewater
ues of PWW vary between 3145 and 3465 ms/cm with an average decanted and purified wastewater. Its results are reproducible and
of 3277 ms/cm. While at the entrance to the WWTP they vary verifiable.
between 3975 and 4284 ms/cm with an average of 4105 ms/cm
(Table 2). 3.6. Study of adsorption of NO

3 by shrimp shell particles
The qualitative analysis of the raw wastewater decanted
(RWWD) shows that it has a higher concentration than the typol- 3.6.1. Adsorption of NO
3 ions contained in the RWWD and PWW
ogy of urban wastewater in Morocco in terms of BOD5 (200– The curves below (Figs. 5 and 6), show the variation of the
400 mg O2/L), COD (500–800 mg O2/L) and TSS (250–500 mg/L) retained concentration and the removal efficiency of the nitrate
parameters [25]. ions contained in RWWD and PWW as a function of the contact
The qualitative analysis of purified wastewater at the outlet of time (R = 25 g /L, T = 25° C).
tertiary treatment shows that the carbon loading in terms of The adsorption equilibrium time of the shrimp shell particles
COD, BOD5 and TSS complies with the specific limit values for was determined by performing 6-hour nitrate adsorption tests
domestic discharges [24], with purification efficiencies of the order with an initial nitrate concentration of 2.2 mg-N/L for RWWD
of 98% for TSS, 98% for COD and 97% for BOD5. and 424 mg-N/L for PWW.

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

Parameters Water type Sampling date Standard Deviation

24/01/2014 22/04/2015 17/10/2015 21/06/2016
Temperature (°C) RWWD 21.5 22.6 22.5 26.5 35 [23]
PWW 19.5 21 20.5 22.8
pH RWWD 7.85 7.67 7.75 7.84 6.5-8.6 [23]
PWW 7.57 7.37 7.45 7.40
Electrical conductivity (ms/cm) at 20°C RWWD 4284 3975 4035 4125 -
PWW 3235 3145 3265 3465
Dissolved oxygen (mg O2/L) RWWD 0 0 0 0
PWW 4.8 4.4 4.7 4.7
TSS (mg/L) RWWD 865 783 812 765 150 [24]
PWW 8.5 9 12 13
% Elimination 99 99 99 98
BOD5 (mg O2/L) RWWD 810 840 835 760 120 [24]
PWW 35 12 15 23
% Elimination 96 99 98 97
COD (mg O2/L) RWWD 1767 1715 1724 1654 250 [24]
PWW 98 43 59 28
% Elimination 94 97 97 98
NO

3 (mg-N/L) RWWD 2.6 1.5 1.3 2.2 30 [23]

5
M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

Table 3
Percentage removal of NO

3 ions at adsorption equilibrium in RWWD and PWW.

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

Fig. 5. Effect of contact time and efficiency of nitrate ion removal by shrimp shell 3.6.2. Purification performance of shrimp shell particles in the removal
particles for RWWD. of nitrate ions contained in RWWD and PWW.
The Percentage removal of NO
3 ions at adsorption equilibrium
in raw wastewater decanted (RWWD) and purified wastewater
(PWW) are presented below (Table 3).
These results show that shrimp shell particles present high
purification efficiencies with regard to the removal of NO
3 ions.
These purification yields are of the order of 68% and 79%, respec-
tively, 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 corre-
lates 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 purifica-
Fig. 6. Effect of contact time and efficiency of nitrate ion removal by shrimp shell tion yields recorded by the percolation infiltration system for
particles for PWW. 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 oxi-
dation of the nitrogen pollution within the sand filters. Therefore,
The results of the adsorption study of NO
3 ions contained in the adequate denitrification treatment of the treated wastewater must
RWWD and PWW are the average of three successive reproducible be provided. The residual concentrations remain very high in the
and verifiable tests. The analysis of the figures (Figs. 5 and 6) treated effluent and could constitute a great risk of eutrophication
reveals that the retained concentration Cr of nitrate ions contained for these discharges for irrigation purposes.
in the RWWD and PWW of the M’zar WWTP, increases with the For that reason, the search for new unconventional cleaning
contact time and equilibrium is quickly reached. The time to equi- processes based on biomaterials which would be inexpensive and
librium is around 30 min. easy to implement is strongly recommended in order to improve
Moreover, the shape of the curves does not make it possible to the quality of purified water according to the required standards.
distinguish two distinct stages of adsorption, everything happens Moreover, the purification efficiency of NO
3 ions by shrimp shell
as if the adsorption takes place in a single very rapid step from particles is important. Shrimp shell particles could then constitute
the very first minutes of contact. This step corresponds to the a potential adsorbent for NO
3 pollutants, given their low cost and
retention of ions located near the surface of the mill particles, high retention rate. Such a process can be used in the purification
and consequently to a rapid diffusion of the nitrate anions to the of wastewater and could integrate in the purification system of the
external sites of the adsorbent surface. WWTP of M’zar in order to improve the purification yield and to
Concerning removal efficiency of nitrate ions in the wastewater comply with the Moroccan regulations in force.
studied. The figures (Figs. 5 and 6) show that the removal efficiency This experimental study using a real wastewater showed
of nitrate ions in raw wastewater decanted and purified wastewa- that the removal of nitrate ions by adsorption onto micro-
ter is of the order of 68% for RWWD and 79% for PWW. This differ- particles of shrimp-shells particles is a viable and effective alterna-
ence in treatment efficiency could be explained by the initial tive to the use of more expensive or less environmentally friendly
concentration of each type of wastewater studied. treatments.
6
M. Abali et al. Materials Today: Proceedings xxx (xxxx) xxx

Author contributions [10] X. Song, Y. Pan, Q. Wu, Z. Cheng, W. Ma, Phosphate removal from aqueous
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Declaration of Competing Interest https://doi.org/10.1016/j.jece:2019.103235.
[16] M. Abali, A. Ait Ichou, A. Dabagh, M. Chiban, M. Zerbet, F. Sinan, Improvement
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The authors declare that they have no known competing finan- stabilization ponds type: removal of sulfate and nitrate ions by adsorption
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