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Progress of Cryogenics and Isotopes Separation Volume 20, issue 2/2017

AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS

FROM WATER AND WASTEWATER

Violeta Niculescu*, Claudia Sandru, Nadia Paun, Marius Miricioiu

National Research and Development Institute for Cryogenics and Isotopic Technologies –
ICSI Rm. Valcea, 240050, Rm. Valcea, Uzinei Street no. 4, P.O. Box Râureni 7, Valcea,
Romania

ABSTRACT

Excess nitrogen compounds can cause environment pollutions and healthy problems. The
commonly encountered nitrogen compounds in wastewater are the nitrate ions, due to human
activities (agriculture and human wastes). The removal of nitrate from groundwater, surface water
and wastewater is of prime importance, the most common methods including biological and
physicochemical technologies. However, these methods have shortcomings and limitations (high
costs and complex operations). The adsorption process has been found successful in nitrate removal
by using various materials as adsorbents due to the simple design, easy and economical operation
as well as allowing nitrate recovery. For example, ammonium-functionalized SBA-16 mesoporous
silica was used as an efficient potential adsorbent for nitrate removal, due to the large specific
surface area, the ordered mesostructure and the functionalization ability with various surface
functional groups. In view of the above facts and in a continuous quest for high capacity, selective,
effective and regenerable adsorbents, the present work is aimed to highlight the use of mesoporous
materials for the removal of nitrate from water and wastewater.

Keywords: nitrogen, removal, silica, waste.

1. INTRODUCTION

Nitrogen compounds are considered extremely important in wastewater

management, due to the effects that nitrogenous material can have on the
environment. Nitrogen can deplete oxygen by nitrification, fertilize aquatic plant
growth, exhibit toxicity toward aquatic life, affect chlorine disinfection efficiency
and present a public health hazard (Huang et al., 2017). Before the final selection
of the appropriate removal technology, some questions must be answered:
1. What are the forms and concentration of the pollutants in the focused
ecosystem?
2. Are these forms and concentrations changing over time? If “yes”, what
are the processes involved?
3. From what sources the pollutants came?

*Corresponding author: Violeta Niculescu, phone: 0250732744; Fax: 0250732746, E-mail:

violeta.niculescu@icsi.ro
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AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS FROM WATER
AND WASTEWATER

4. The problems are local, regional or global?

Figure 1 presents a route from emission of mass and energy to a solution of
the related environmental problems. Emission is translated into imission and
concentration. The effect and impact of a concentration of a compound or energy
involve all the chemical, physical and biological processes that take place in the
ecosystem, requiring the application of ecological models as a management tool,
due to the fact that the processes are interactive.

Figure 1. Diagram of the route from emission to the solution of the problem

The procedure presented in Figure 1 concerned with ecosystems is the

most complex one, requiring a very comprehensive ecological and environmental
scientific knowledge, which often must be synthesized in a model in order to
give applicable answers to the crucial environmental problems.
In the last years, different parts of the world have been facing the problem of
nitrogen pollution in the environment. The main forms of nitrogen are ammonia (NH3),
nitrate (NO3-) and nitrite (NO2-). Nitrate is the most stable form in water, almost all
sources of aqueous nitrogen tending to be converted to nitrate. Nitrate (NO3-) is an
inorganic compound that dissolves easily in water and can be used in agricultural fields
as fertilizer. Also, nitrate anions are applied as plant nutrients but become an important
problem when their amounts exceed. High concentrations of nitrate and phosphorus in
ground and surface water can accelerate the eutrophication, stimulating the growth of
algae and rooted aquatic plants. As a consequence, the entire aquatic ecosystem
32
 Violeta Niculescu, Claudia Sandru, Nadia Paun, Marius Miricioiu

can be changed, reducing light penetration into the water and leading to decreases
in the plants living in the deeper water. Once the concentrations of nitrate and
phosphorus in water increase, the dissolved oxygen tends to decrease, affecting
negatively t he life of aquatic organisms that need oxygen (Abe et al., 2002).
Excessive levels of nitrate ions in drinking water may cause health problems,
especially for infants under six months of age and pregnant women (Abe et al.,
2002). In 1990, environmental protection agency (EPA) indicated that 250,000 water
supply sources had maximum contaminant levels (MCL) for nitrate (Archna et al.,
2012). In 2004, the World Health Organization (WHO) found that 30% of the 2,000
sources in the world had more than 24 mg N- NO3-/L (Archna et al., 2012). When
nitrate is converted to nitrite in the body system, it reduces the oxygen-carrying
capacity of the blood, resulting in a condition called "methaemoglobinaemia", also
known as "blue baby syndrome". The reaction between nitrite and secondary or tertiary
amine from acidic media can lead to the formation of nitroso compounds (NOC),
which are known carcinogenic, teratogenic and mutagenic (Shams, 2010). Due to all
the mentioned reasons, the removal of nitrate and nitrite from water is of significant
importance in environment and the health.
Many traditional methods have been applied to the removal of nitrogen
compounds from wastewater, including physical processes (Elmidaoui et al.,
2001), chemical processes (Cengeloglu et al., 2006) o r biological de-nitrification
processes (Abe et al., 2002). The disadvantages of these techniques include high
costs, increased volumes of sludge and complex and strict control of the operating
conditions (Chatterjee et al., 2009).
Recently, adsorption has been used for the removal of nitrogen
compounds, this technique being easy and economical and generates little sludge,
allowing nitrate recovery (Bhatnagar et al., 2008). Various materials were been
used as adsorbents for removal of nitrogen compounds from water and
wastewater: active red mud (Cengeloglu et al., 2006), C-cloth (Afkhami et al.,
2007), chitosan hydrogel beads (Chatterjee et al., 2009) or surfactant-modified
zeolite (Schick et al., 2010). These adsorbents have the disadvantage o f low
adsorption capacity due to limited surface area. Mesostructured materials with
uniform mesopores and high surface area were found to be efficient for the
adsorptive removal of nitrogen compounds from water (Saad et al., 2007).
Taking into account all the above aspects and the continuous need for high
capacity, selective, effective and regenerable adsorbents, this study highlights the
use of mesoporous materials for the removal of nitrate from water and wastewater.

2. THE NITROGEN CYCLE

The biogeochemical cycles include the nitrogen cycle, in which atmospheric

nitrogen is converted to many chemical forms (ammonium-NH4+, nitrite-NO2-, or
nitrate-NO3-, through different processes: nitrogen fixation, ammonification
(mineralization), nitrification and denitrification (Figure 2) (Archna et al., 2012).
Nitrate is a stable form and highly soluble and migrates easily to the water through the
soil, accelerating the eutrophication and leading to health problems.

33
AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS FROM WATER
AND WASTEWATER

Figure 2. The nitrogen cycle

As it was mentioned before, the nitrate is the most important nitrogen pollutant
occurring from natural sources and anthropogenic activities (e.g. agriculture, chemical
industry, domestic waste). The contribution of natural is usually low because natural
systems have balance between the production and the consumption of nutrients. On the
contrary, human sources occur from agricultural (a major source of nitrate) or
industrial activities (Shao et al., 2009). Nitrogen transformation in soils is due to
excessive use of fertilizers, animal manures, or compost. The nitrogen compounds in
the water and wastewater also comes from many other sources including urban
wastewater, urban storm- water runoff, industrial processes, fossil fuel combustion,
aquaculture, or septic tanks (Schick et al., 2010).
The effects of nitrogen discharge are: fertilization (eutrophication) of aquatic
ecosystems; oxygen depletion in aquatic ecosystems; toxicity to aquatic life and
contamination of ground water by nitrate and its effect on the public health. The word
eutrophic generally means "nutrient rich". The eutrophication of lakes in Europe and
North America has grown rapidly during the last few decades due to the increased
urbanization and the increased discharge of nutrients per capita (Schick et al., 2010).
The production of fertilizers has grown exponentially in this century and the
concentration of nutrients in many lakes reflects the same exponential growth. The
word eutrophication is usually used in the sense of the artificial addition of nutrients,
mainly nitrogen and phosphorus, to water. Eutrophication is generally considered to be
undesirable, although it is not always so. For example, the green colour of eutrophic
lakes makes swimming and boating less safe due to increased turbidity. Eutrophic
lakes might exhibit high oxygen concentrations at the surface during the summer, but
low oxygen concentrations in the hypolimnion, which may cause fish death. On the
other hand, an increased nutrient concentration may be beneficial for shallow ponds
used for commercial fishing, as the algae directly or indirectly form food for the fish
population.

34
 Violeta Niculescu, Claudia Sandru, Nadia Paun, Marius Miricioiu

The main concern about eutrophication is correlated with the rapidly

increasing amounts of phosphorus and nitrogen, normally present at relatively low
concentrations. Phosphorus is often considered the major cause of eutrophication.
Nitrogen accumulates in lakes to a lesser extent than phosphorus and a considerable
amount of nitrogen is lost by denitrification. In oligotrophic waters, the N:P ratio is
more than or equal to 10, which means that phosphorus is less abundant relative to
the needs of phytoplankton than nitrogen. If the sewage is discharged into a lake,
this ratio will decrease, due to the N:P ratio of about 3:1 of municipal wastewater.
This is reason why it is necessary to set up a mass balance for the nutrients,
explaining the input of nitrogen from nitrogen-fixing blue green algae, dry and wet
deposition. These considerations have result in the conclusion that the
eutrophication process can be controlled by a reduction in the nutrient budget
(Archna et al., 2012).

3. METHODS OF NITROGEN COMPOUNDS REMOVAL

Different processes have been applied to the removal of nitrogen

compounds. Traditional methods include biological de-nitrification processes, ion
exchange (IX), reverse osmosis (RO), or electrodialysis (ED). Each of these
technologies has its own advantages and disadvantages and their feasibility
depends on different factors: cost, water quality improvement, residuals handling,
and post-treatment requirements.

3.1. Biological denitrification method

The biological denitrification has been used intensively for the reduction
of nitrate ions from wastewater (Shao et al., 2009; Naik et al., 2011). By this
method, nitrate is converted to nitrogen gas by denitrifying bacteria in the
absence of oxygen:

ܱܰଷ → ܱܰଶ → ܱܰ → ܰଶ ܱ → ܰଶ (1)

Denitrification can be achieved using both heterotrophic and autotrophic

bacteria. In order to achieve heterotrophic denitrification, an organic compound is used
as the carbon and energy source (ex: methanol, glucose, acetate, ethanol or acetic acid).
Recently, some studies reported the use of different materials such as cotton, wheat
straw, wood shavings, sawdust and biodegradable plastic as the organic carbon source
(Zhao et al., 1998). For the autotrophic denitrification, an inorganic energy source is
necessary: sulphur, reduced sulphur species (e.g. thiosulphate) or hydrogen gas; the
carbon dioxide or bicarbonate were used as carbon sources (Shams, 2010).
It was reported the nitrate removal from wastewater by using immobilized
Psuedomonas Stutzeri bacteria in a fluidized bed bio reactor with different initial
nitrate concentrations (150, 180 and 200 ppm), t h e highest removal efficiency
(96%) b e i n g a c h i e v e d with methanol as carbon source, followed by
ethanol (77%) and methane (70%) during the period 6-8 hours (Naik et al. 2011).

35
AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS FROM WATER
AND WASTEWATER

3.2. Ion exchange method

Ion exchange involves the removal of dissolved nitrate ions from water
and wastewater by exchanging them with chloride ions on anion exchange
resin. When the capacity of the resins is exhausted, it can be regenerated by using
a sodium chloride solution with high concentration, in order to displace the nitrate
on the resin. Ion exchange is a method with high efficiency, simple operation and
relatively low cost. Several resins have been tested: Purolite A 520E (Samatya et
al., 2006); Amberlite IRN 9766 resin (Dron et al., 2011); Amberlite IRA 400 resin
(Chabani et al., 2006); etc.
For example, it was studied the equilibrium and kinetic parameters for the
removal of nitrate ions from aqueous solutions on Amberlite IRA 400 resin and
reported the maximum adsorption capacity of Amberlite IRA 400 resin was 769.2
mg NO3-/g at 25°C (Chabani et al., 2006).

3.3. Reverse osmosis (RO)

Reverse osmosis (RO) is a pressure-driven membrane separation method, in

which a feed stream under pressure is separated into a purified permeate and a
concentrated stream by selective permeation of water through a semi-permeable
membrane. Membranes generally contain cellulose acetate, polyamides and
composite materials (Archane et al., 2011). In practice, this method is applied for
water desalination and for treatment of diverse wastewaters (Schoeman et al.,
2003). They showed that nitrogen was reduced from 42.5 mg/L in the RO feed to
only 0.9 mg/L in the RO product water (98% removal).

3.4. Electrodialysis

Electrodialysis involves the passing of cation and anion from aqueous

solutions through ion exchange selective membranes using the driving force of an
electric field.
It was reported the removal of nitrate in the presence of organic matter and the
percentage of removal was about 94.1% with 100 mg/L of initial concentration of
nitrate (Schoeman et al., 2003).

3.5. Adsorption method

Adsorption method involves collecting soluble in solution on a suitable

interface. Adsorption process has many advantages: ease of operation, generates little
sludge, simplicity of design, and allows nitrate recover. Also, the adsorbents can be
recycled easily and do not contain harmful pollutants in component. Furthermore, this
process can eliminate or minimize different types of organic and inorganic pollutants
from wastewater and therefore, it has a wider applicability in water pollution control.
Sorption can be classified upon the type of bonding involved:

36
 Violeta Niculescu, Claudia Sandru, Nadia Paun, Marius Miricioiu

a) Physical sorption (or physisorption): no exchange of electrons take place;

the adsorbate is held to the surface by the relatively weak Van der Waals forces, the
process of physical adsorption being easily reversed.
b) Chemical sorption (or chemisorption): the chemical bonds involve an
exchange between specific surface sites and solute molecules; it is characterized by
interaction energies between the surface and adsorbate comparable to the strength of
chemical bonds, chemisorption being much stronger and much more stable.
The use of activated carbon is a traditional method to treat wastewater.
However, activated carbon is expensive. Several studies presented the removal of
nitrate from water by carbon based adsorbents as powdered activated carbon
(PAC) and commercial granular activated carbon (GAC) (Demiral et al., 2010)
or carbon nanotubes (CNTs) (Tofighy et al., 2012).
Also, many other materials have been used for the removal of nitrogen
compounds from water and wastewater: zeolite and modified zeolite (Schick et al.,
2010; Zhan et al., 2011), chitosan (Chatteerjee et al., 2009), or miscellaneous
adsorbents as nano – alumina (Bhatnagar et al., 2010). For example, the chitosan
hydro-beads have been found to be an effective biosorbent for the removal of nitrate
from an aqueous solution (Chatterjee et al. 2009). The maximum adsorption capacity
was 92.1 mg/g at 30°C and the adsorption data fitted well to Langmuir–Freundlich
isotherm model and negative value of enthalpy ΔH0 (−2.302 kJ/mol) confirmed that
exothermic process on adsorbent (Chatterjee et al., 2009).
Recently, it was reported the elimination of nitrate from water on surfactant-
modified zeolite. The adsorbent was obtained by the treatment of a clinoptilolite
sample with hexadecyltrimethylammonium bromide surfactant (Schick et al., 2010).
The removal process occurred quickly and efficiently, the final removal rate
being higher than 80%. The adsorption equilibrium data were in good agreement
with the Langmuir isotherm model (Schick et al., 2010).
Selection of a suitable adsorbent for nitrogen compounds removal depends
on several factors, including: the initial NO3- concentrations; competitive ions and
their concentration in water; optimization of adsorbent loading; adjustment of pH in
water; temperature. Almost all studies showed that the pseudo-second-order kinetic
model was found to fit well with the data. The isotherm models of nitrate
sorption by various adsorbents are characterized by Freundlich and Langmuir
models. However, during chemical treatment of adsorbent, it should not be ignored
the cost factor. Low production cost with higher removal efficiency would make
the process economical and efficient.
Most of the studied adsorbents had insufficient adsorption capacity and they
could not be regenerated; also, they had poor selectivity and limited surface area.

4. MESOPOROUS SILICA MATERIALS

To undertake the mentioned drawbacks, mesostructures with uniform

mesopores and high surface area were found to be good assets for nitrate removal.
Recently, ammonium- functionalized mesoporous silica MCM-41, MCM-48, SBA-15
were synthesized via post- synthesis grafting and co-condensation method (Niculescu
et al., 2011).
37
AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS FROM WATER
AND WASTEWATER

The ordered mesoporous materials with pore size between 2 to 50 nm were

discovered in 1992 by Mobil Corporation and they can exhibit high specific surface
area, large pore diameter, increased adsorption capacity and enhanced diffusion rate,
leading fast adsorption. In addition, mesoporous silica with surface hydroxyl groups
can be functionalized with specific organic groups which represent alternative
adsorbents for the removal of nutrient species from aqueous solutions.
Various mesoporous silica oxide with ordered structure in the form of
hexagonal (denoted as MCM-41, SBA-15), cubic (denoted as MCM-48, SBA- 16) and
the lamellar (denoted ad MCM-50) can be obtained, depending on the starting
materials and varying synthesis condition (Figure 3).

Figure 3. The classification of mesoporous materials silica

SBA-15 materials have larger pore size, thicker wall and higher thermal and
hydrothermal stability, comparing to MCM-41. BothMCM-41and SBA-15 have
two-dimensional mesoporous structures, limiting the accessibility of the pores.
Recently, a novel and attractive mesoporous silica SBA-16 with 3-dimensional
porous structure was reported (Kim et al., 2005). SBA-16 has large cage-like
mesopores (5-15 nm) arranged in a three-dimensional cubic ordered. The structure of
SBA-16 can be depicted by a triply periodic minimal surface of I-WP (body centred,
wrapped package), each mesopore being connected to eight neighbouring mesopores
(Figure 4) (Rivera-Muñoz et al., 2010).

Figure 4. 3D structure of SBA-16 (Rivera-Muñoz E. et al., 2010)

This adsorbent can be synthesized under acidic conditions using a non-ionic

Pluronic surfactant F127 as structure-directing agent, obtaining SBA-16 mesoporous
silica with thicker pore walls than SBA-15 mesopores. SBA-16 facilitates mass
transfer and is less susceptible to pore blockage, making SBA-16 more attractive for
applications as adsorption and catalysis.
38
 Violeta Niculescu, Claudia Sandru, Nadia Paun, Marius Miricioiu

Ordered mesoporous silicas were used as supports due to their uniform and
large pores, high porosity and high surface areas as well as a large number of the
hydroxyl groups on surface. These groups were used for surface modification,
anchoring organic molecules to the silica surface to form the functional groups.
Different organic functionalities were used for modifying the surface properties of
mesoporous silica materials (ex: thiols, sulfonic, carboxylic acids and amines)
(Hoffmann et al., 2006). Normally, the functionalization can be achieved by two
methods: post synthesis grafting and co-condensation method.
Post-synthesis grafting method involves stirring the mesoporous silica (after
surfactant removal) and silane- or polymer-containing functional groups in a solvent
(e.g. toluene), under reflux conditions (Figure 5). This method may be considered
when the purpose is to maximize the number of functional groups on the surface but
distribution of the organic moiety on the surface is uncontrollable.

Figure 5. Post synthesis grafting method (Hoffmann F. et al., 2006)

Co-condensation method can be performed by stirring a mixture solution of

the organo-silane, surfactant and silica source to form functionalized mesoporous
silica. Co-condensation involves the hydrolytic condensation of an organosilane
together with conventional silica sources as TEOS (tetraethylorthosilicate) (Figure
6) (Athens et al., 2009).

Figure 6. Co-condensation method (Athens G. L. et al., 2009)

Many recent investigations present functionalized mesoporous with various
amines groups for various environmental applications. For instance, it was reported
nitrate and phosphate removal on MCM-48 functionalized with amino groups by
post-synthesis grafting (Hamoudi et al., 2007).
39
AN OVERVIEW ON THE REMOVAL OF NITROGEN COMPOUNDS FROM WATER
AND WASTEWATER

Also, functionalized SBA-16 mesoporous silica was synthesized by post-

synthesis grafting and co-condensation method using different silane-groups
(mono-, di- and tri-amine groups). The characterization results confirmed the cubic
structure of functionalized materials with uniform and ordered channels. By using
the functionalized silica in the nitrogen removal from wastewater, the percentage of
nitrogen incorporation decreased with increasing molar ratio organoalkoxysilane:
silica in the synthesis, suggesting that the molar ratio organoalkoxysilane: silica of
10% is a good compromise for functionalized SBA-16 silica. The adsorption rate
increased rapidly at early stages of the treatment and the time required for
equilibrium was 5 minutes. The reported maximum percentage of nitrate removal
was about 40% at equilibrium adsorption on functionalized SBA-16. The adsorption
equilibrium data were in good agreement with the Langmuir and Temkin isotherm
models. The amount of adsorbed nitrate increased with changing the amine type
from mono-, di-amine to tri-amine (Huang et al., 2017).

5. CONCLUSIONS

Water is vital for life on earth. High levels of nitrogen compounds in aquatic
environments constitute serious environmental worldwide problem, due to the fact
that nitrate anion is involved in the eutrophication of receiving surface waters.
Agricultural and urban wastewater, improper disposal of municipal and industrial
wastes, leakage in septic systems, landfill leachate, and animal manure are sources
of nitrate anion contamination. While nitrate is relatively nontoxic to adults, because
of nitrate excretion from the kidneys, concentrations above 10 mg/L N–NO3- are
fatal for children under 6 months. This study presented an overview of several
processes for the removal of nitrogen compounds in water and wastewaters. Current
available technologies for water treatment of nitrate are found to be expensive,
inefficient and generate additional by-products. Among them, adsorption systems
are favourable, because they allow straightforward and economical operation,
bringing about less sludge generation and disposal issues. Among the absorbent
materials, mesoporous silica has gotten extensive consideration due to the high
specific surface area, well-defined pore size and pore shape. Furthermore,
functionalized mesoporous silica can be considered promising materials for future
use as adsorbent for the removal of nitrogen from water and wastewater.

Acknowledgements: The work has been funded by the Romanian Ministry

of Scientific Research and Innovation, 34N/2016 NUCLEU Program, under Project
PN 16 36 04 03 „Research on the development of new porous materials with high
selective and catalytic properties for the reduction and stabilization of the pollutant
concentrations in gaseous and liquid backgrounds”.

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