Biomass and Bioenergy 152 (2021) 106198

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Biomass and Bioenergy

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

Effect of the ozonation pretreatment on biogas production from waste

activated sludge of tehran wastewater treatment plant
Mahdi Hodaei a, Shahnaz Ghasemi b, *, Arash Khosravi c, d, Manouchehr Vossoughi e
a
Department of Civil Engineering, Sharif University of Technology, Tehran, Iran
b
Sharif Energy, Water and Environment Institute, Sharif University of Technology, Azadi Avenue, Tehran, P.O.Box 11365-8639, Tehran, Iran
c
Sustainable Membrane Technology Research Group, Department of Chemical Engineering, Persian Gulf University, P.O.Box 75169-13817, Bushehr, Iran
d
Sustainable Energy Research Group, Persian Gulf University, P.O.Box 75169-13817, Bushehr, Iran
e
Department of Chemical and Petroleum Engineering, Sharif University of Technology, Tehran, Iran

A R T I C L E I N F O 1 . A B S T R A C T

Keywords: In this study, the ozonation impact on anaerobic digestion of wasted thickened activated sludge of Tehran
Anaerobic digestion wastewater treatment plant has been investigated. Regarding that, the thickened activated sludge, a final solid
Biogas production waste of treatment plants, was subjected to ozonation pretreatment to evaluate its characteristics. Three major
Dewatering
sludge characteristics were considered for investigating ozonation effects on anaerobic digestion. A comparison
Ozonation pretreatment
of two different ozone doses, i.e., 0.05 and 0.1 gO3 g− 1TS was performed for short-term (10 days) and long-term
Thickened activated sludge
(30 days) sludge retention times. Furthermore, biogas production, sludge composition, dewaterability, and en­
ergy balancing, were studied during the periods mentioned above. The results show that the lower ozone dose
has an acceptable performance in a short-term operation for all parameters except energy balance which was
negative in all the scenarios. Higher ozone dosage not only decreased biogas production and volatile solids
reduction but also significantly increased the energy demand of the system. In addition, a longer retention time
reduced the effectiveness of the ozone pretreatment during that time. Eventually, the feasibility of ozone pre­
treatment capacity for sustainable management of different sludge from economic and technological perspectives
can be evaluated by further assessing this case study.

1. Introduction
Industrial development and ongoing urbanization in recent years,
along with expansions of the sewage and refining networks, have led to a
significant enhancement in sludge production. Stringent regulations for
sludge reuse or disposal have forced both public and private sludge
generators to administer their own sludge management strategies [1].
There are currently three main ways for sludge disposal, including
incineration, landfilling, and ocean disposal. However, in most cases,
strict landfilling criteria and a ban on dumping sludge in the oceans
made reusing sludge more attractive [2]. In addition, anaerobic diges­
tion of waste-activated sludge has been widely considered as an envi­
ronmentally friendly wastewater treatment due to the sludge
stabilization as well as a reliable source of renewable energy for
wastewater treatment plants [2,3].
Besides, anaerobic digestion is considered the most effective and
accessible energy recovery from sludge [4]. Applying this method,
organic solids of sludge have been transformed into biogas containing
CH4, CO2, and a trace amount of other gases [5]. In particular, biogas
includes 60–70 % methane, 30–40 % carbon dioxide, and a trace amount
of nitrogen, hydrogen sulfide, and water [3,6]. Methane gas generated
by anaerobic digestion is used to produce electrical energy and reduce
the operating cost of treatment plants [6]. Furthermore, this approach
decreases methane leakage through natural routes from landfills and
reduces CO2 production by utilizing methane instead of using fossil fuels
as a treatment plant’s energy source [3]. However, the production of a
considerable amount of digested materials, and the high content of the
degradable organic compounds in the digested matter, can result in a
significant increase in soil microbial activity. Recycled materials in
sludge technically and economically can be divided into two categories,
materials for nutrients (i.e., Nitrogen & Phosphorus) and materials for
energy (Carbon) [7]. The presence of non-biodegradable components
that are relatively resistant to decomposition as well as complicated
organic matter (i.e., proteins and lipids) leads to a decrease in anaerobic

* Corresponding author. ,
E-mail addresses: shodaeie@buffalo.edu (M. Hodaei), sh.ghasemi@sharif.edu (S. Ghasemi).

https://doi.org/10.1016/j.biombioe.2021.106198
Received 4 February 2021; Received in revised form 24 June 2021; Accepted 18 July 2021
Available online 23 July 2021
0961-9534/© 2021 Elsevier Ltd. All rights reserved.
M. Hodaei et al.
digestion’s efficiency [8]. In this regard, simultaneous hydrolysis of
organic substances and bacterial cells inhibit anaerobic digestion per­
formance [9]. Sludge pretreatment is one of the practical approaches to
enhance anaerobic digestion efficiency, helps destroy bacteria’s cell
wall. Furthermore, pretreatment techniques accelerate the decomposi­
tion of complex organic components into smaller and simpler ones
which in turn can increase the sludge hydrolysis rate [10].
Accelerating the whole digestion process, reducing sludge retention
time, and increasing biogas production rates are mentioned as other
benefits of sludge pretreatment [11,12]. All pretreatment methods aim
to speed up the digestion process and increase sludge dewaterability.
However, the research results demonstrated that pretreatments signifi­
cantly affect active sludge digestion rather than primary sludge [13].
Pretreatment methods are categorized into three main categories,
physical, chemical, biological, or a combination of these categories [14].
Chemical pretreatment techniques utilizing acids, bases, and strong
oxidation agents such as ozone are considered more popular due to their
simple operation and high efficiency. However, chemical oxidation
pretreatment with ozone is more effective than acids or bases because
ozone does not change sludge salt concentration. Besides, ozone can
decompose a wide range of organic and inorganic materials [15]. As a
powerful oxidizing agent, ozone reacts with the bacteria’s cell walls
rapidly, killing microorganisms in the sludge and oxidizing complex
organic matter to a simpler compound [16–18]. In a closer look, it reacts
with polysaccharides, proteins, and lipid membranes of the cell, con­
verting them into simpler molecules that have a higher biodegradation
rate. As a result, it could enhance biogas production in the anaerobic
digestion process compared with raw sludge [19–21]. On the other
hand, if the ozone concentration would be high enough, it can convert
cell components into minerals like H2O and CO2 and consequently
reduce biogas production [22]. For the balance of cost and efficiency,
the amount of ozone should be optimized gO3 per gTS. The optimum
amount of ozone depends on the sludge characteristics and the test
condition [23,24]. Ozone dose varies according to its application in
wastewater treatment because ozone is being used in a broad range of
applications in wastewater treatment processes like disinfection as
advanced treatment or pretreatment for increasing the degradability of
organic substances [24–26]. Therefore, the ozone dose depends on the
purpose of the ozonation and waste type and varies from few micro­
grams to several milligrams per carbon content of the sludge, as dis­
cussed in the previous studies [27,28]. Most of the earlier researches on
the ozonation pretreatment mainly focused on ozone dose and its effects
on sludge composition and biogas production [29–31]. However, a
comprehensive study that evaluates all aspects of ozonation pretreat­
ment, including retention time, dewatering, and energy balance in
addition to conventional parameters, is missing from the literature.
In this study, the ozonation pretreatment impact on experimental
parameters of anaerobic digestion and sludge deposal was thoroughly
investigated. Regarding that, three categories of experimental parame­
ters that are very useful in an actual wastewater treatment plant for
sludge management have been investigated. The first category of pa­
rameters consisted of the chemical composition of the sludge, particu­
larly volatile solids and total solids concentration. The second category
is the dewaterability of sludge, which is very important for sludge
disposal management according to the high cost of sludge transmission
to the landfill. Finally, the third category is referred to energy balance,
including biogas production and ozonation energy demand, which is
essential for assessing the sustainability of the ozonation pretreatment.
Considering these parameters, sludge pretreatment has been performed
using two ozone doses of 0.05 and 0.1 g of O3 per total solid (TS) (g O3
g− 1 TS). The effect of ozonation on the performance of anaerobic
digestion, including biogas production, sludge chemical composition
(particularly total solids (TS) and volatile solids (VS) concentration),
and digested sludge dewatering (which causes high sludge transition
cost), was evaluated in a short and long time sludge retention time.
Eventually, the energy balance of the ozonation approach was
2
Biomass and Bioenergy 152 (2021) 106198
calculated in order to assess the ozonation efficiency and sustainability.
2. Materials and methods
2.1. Sludge composition and dewatering capacity measurement
Three different sludges, including raw primary sludge, activated
thickened sludge, and digested sludge, were provided from the South
Tehran wastewater treatment plant as the largest and most advanced
wastewater treatment plant in Iran. These sludge types are typical in
conventional wastewater treatment plants, and their analysis could
show the performance of the anaerobic digestion facility. Volatile solids
(VS) and total solids (TS) content of the different types of sludges were
measured by standard methods [32].
Sludge dewatering capability as the most critical parameter of sludge
quality was determined using centrifugation with 3000 rpm for 5 min
after solids were settled. Remained solid volume was considered as
dewatered sludge, followed by measuring the dry solid content; Volu­
metric Dewatering Percentage (VDP) was calculated volumetrically by
the following equation [33]:
V0 − VSludge
VDP = × 100 (1)
V0
where V0 is the initial sludge volume (30 ml for each test), and VSludge is
the dewatered sludge volume after centrifuge.
2.2. Ozonation and anaerobic digestion systems
The experimental setup consisted of two ozonation and anaerobic
digester reactors. The ozonation reactor was constructed from two cy­
lindrical glass chambers with a volume of 2 L. The first chamber was
utilized for sludge ozonation, while the second cylindrical glass chamber
containing water was used to neutralize the residual ozone coming out
from the first cylindrical chamber. A flow controller was installed on the
first chamber to control the ozone generator flow (PCM5 model, made in
Iran, the production rate of 5 g h-1, the discharge rate of 5 L min− 1, 100
W). An anaerobic digester reactor (ADR), as a batch-type reactor, was
constructed from a 5-Liter cylindrical glass container equipped with a
heater and thermometer to adjust the temperature. A scheme of the
experimental set-up has been presented in Fig. 1.
The sludge inlet was on the top of the reactor, and the sludge outlet
was on the bottom, which was used for sampling without any gas
leakage from the digester. The gas outlet of ADR was connected to the
pressure gauge and flow meter to measure biogas pressure and volume.
The ozonation process was carried out in four steps. The first to third
steps were performed with the volume of 0.5 L sludge, while the final
step was fulfilled by 0.3 L sludge. Overall, 1.8 L ozonated sludge was
prepared for the ADR. Through all these steps, the ozone dose and
contact time were carefully controlled. The short-term sludge retention
time was considered ten days because of the similarity to the actual
sludge retention time of digesters in the South Tehran wastewater
treatment plant, while the long-term retention time was determined to
be 30 days. The temperature of the digestion process was set at meso­
philic conditions (35 ◦ C). Therefore, all experiments were carried out in
the same qualitative and quantitative conditions, and the only variable
was the ozone dose and sludge retention time. For the first experiment as
a control test, ADR was fed with untreated waste thickened activated
sludge (WTAS). For the rest of the experiments, ADR was supplied by
ozone-pretreated WTAS. The operating conditions of each test have been
summarized in Table A1 in supporting information.
2.3. Biogas production
The biogas production rate was measured through both pressure
measurement using a gauge and volume measurement using a flow
M. Hodaei et al.
Fig. 1. A scheme of the experimental setup.
meter connected to the ADR gas outlet. It should be noted that the sol­
ubility of CO2 and CH4 in the sludge was neglected due to insignificancy.
In the current research, the maximum degradation rate (L biogas. kg− 1
VS. d− 1) and cumulative biogas production (L biogas. kg− 1 VS) were
considered as two main factors for comparison. The maximum degra­
dation rate was derived from the slope of the curve during the meth­
anogenesis stage of the anaerobic digestion process. The cumulative
biogas production (CBP) was determined using equation (2) [34]:
∑
Vt,biogas
CBP = (2)
VSin
where Vt, biogas is the volume of produced biogas in time of t (day), and
VSin is the initial volatile solids concentration in ADR. The impact of
ozonation on the conversion of volatile solids to biogas was evaluated by
calculation of the biogas production yield by the following equation:
(Bioassay for monitoring biochemical methane potential and anaerobic
toxicity)
PB
BPY = (3)
VSreduced
where BPY is the biogas production yield [L biogas. kg− 1 VSreduced], PB
stands for the produced biogas [L], and VSreduced is the amount of vol­
atile solids that are converted to biogas [kg].
2.4. Energy balance measurement
The energy consumed to produce ozone for each test was calculated
using the following equations:
Eozonation = W × t (4)
where W is the ozone generator power (100 W), t is the ozonation period
in seconds. Since the energy consumption of the heater was the same for
all tests, therefore it was ignored in this estimation. Therefore, only
ozonation energy was considered as consumed energy. The produced
energy through the anaerobic digestion process was calculated using the
ideal gas law. For this reason, at first, methane density was calculated at
the pressure and temperature of each test conditions [35] as follow:
Pact Tstd
ρ act
=ρstd
× × (5)
CH4 CH4
Pstd Tact
whereρact
CH4 is the methane density at standard temperature and pressure
(0.72 kg m− 3), Tstd is the standard temperature (273 K), Pstd is the
standard pressure (101.325 kPa), the Tact is the gas temperature (303 K),
and Pact is the total pressure equal to the gauge pressure plus air
3
Biomass and Bioenergy 152 (2021) 106198
pressure. Generated biogas energy was calculated considering the
composition of 65 % methane and 35 % carbon dioxide identified using
gas chromatography analysis, which has the same composition as the
previous studies [36]. The total produced biogas energy was derived
from the following equations:
VCH4
Hu.act = × ρact
CH4 × Hu,n (6)
VTotal
Ebiogas = Hu.act × Vbiogas (7)
where Hu,n is the normal calorific value of biogas equal to 50,000 kJ
kg− 1, Hu,act is the actual calorific value of given biogas ( kJ
kg ), and Vbiogas is
the biogas volume (L). Eventually, energy balance was measured by the
following equation.
Energy balance = Eozonation − Ebiogas (8)
3. Results and discussion
Three types of sludges, such as waste thickened activated sludge,
primary sludge, and digested sludge, were considered in this study. The
moisture and the volatile solid concentration of these sludge types have
been shown in Fig. A1 in supporting information. Therefore, comparing
the chemical characteristics of these sludge types helps us estimate the
performance of the anaerobic digestion process of the treatment plant.
As the results in Fig. A1 demonstrated, the removal of volatile solids
in the anaerobic digester of the treatment plant is not sufficient. The
reason for this problem is that the ten days retention time for sludge in
the digester is not enough time to complete the hydrolysis process due to
its complexity. Besides, pretreatment of waste thickened activated
sludge is more efficient than primary sludge due to less degradable
substances in this sludge than primary sludge [37]. Therefore, the
ozonation impact on the anaerobic digestion of waste-thickened acti­
vated sludge was investigated in this study. The characteristics of the
waste thickened activated sludge has been shown in Table A2 in sup­
porting information.
3.1. Effect of ozonation dosage on biogas production
The pretreatment of the waste-thickened activated sludge was car­
ried out using two doses of 0.05 and 0.1 g of O3 per total solid (g O3 g− 1
TS). The impact of ozonation on cumulative biogas production for
retention times of 10 and 30 days has been depicted in Figs. 2 and 3,
respectively. As Fig. 2 shows, the produced biogas was significantly
increased for ozone-treated sludges compared to untreated sludge for
M. Hodaei et al.
Fig. 2. Variation of cumulative biogas production in the retention time of
10 days.
Fig. 3. Daily cumulative biogas production in 30 days.
the retention time of 10 days. In particular, cumulative biogas produc­
tion (CBP) increased to 169 % for 0.05 g O3 g− 1 TS and 140 % for 0.1 gO3
g− 1 TS ozonized sludge.
Maximum daily biogas production (MDBP) increased from 2.08 L
biogas. kg− 1 VSin.d− 1 for untreated sludge to 6.26 L biogas. kg− 1 VSin.
d− 1 for ozone-treated sludges, indicating the ozonation pretreatment
accelerated methanogenesis mechanism. The biogas production volume
reached its maximum (which can be considered as the main methano­
genesis period) on the 6th and 7th days for 0.05 gO3. g− 1TS and 0.1
gO3g− 1TS ozonated sludges, respectively. The main methanogenesis
stage begins when the biogas production curve reaches the upward
linear zone. Considering Fig. 2, the linear zone started on the 6th and 7th
days for 0.05 gO3g− 1TS and 0.1 gO3g− 1TS, respectively. It can be
concluded that a higher amount of the ozone concentration not only
decreases the CBP at the end of the 10th day but also delayed the
beginning of the main methanogenesis stage while triggering the CBP for
the first day. The obtained results are consistent with the findings of the
previous study, which indicated higher ozone doses (0.08 and 0.10
gO3g− 1TSS) adversely affected biogas production [38]. The CBP rate is
increasing linearly after the 3rd day for 0.05 gO3. g− 1TS ozonated sludge
till the end of 10 days, while the CPB of the higher ozone dosage was
decreased between 5th and 7th. The reason for that is the effects of
higher ozone dose on the sludge composition parameters, especially pH,
which led to the formation of by-products less biodegradable than un­
treated substrate [39]. This fact was elaborated in the sludge
4
Biomass and Bioenergy 152 (2021) 106198
composition section and Fig. 3.
As indicated in Fig. 3, different behavior was observed for the effect
of varying ozone dose in biogas production in the long-term retention
time of 30 days. Furthermore, it was demonstrated that ozonation made
not only CBP curves stepper (MDBP of untreated sludge increased from
5.01 biogas. kg− 1 VSin.d− 1 to around 6.26 biogas. kg− 1 VSin.d− 1 using
ozonation) but also decreasing main methanogenesis phase starting
point, which means ozonation successfully could accelerate AD process
both in shortening hydrolysis phase and providing more degraded
organic matter for methanogenic bacteria. However, the maximum daily
biogas production was equal for both ozone doses, which means the
higher ozone dose forms non-biodegradable by-products that cannot be
destroyed by anaerobic bacteria, suggesting that longer time or higher
ozone doses could be unnecessary.
Despite these promising consequences, some quantitative compari­
sons deserving of increasing sludge retention time need to be investi­
gated. First, the difference between the CBP ratio of untreated sludge
and the average of the ozonized sludge decreased from 22.86 L biogas.
kg− 1 VSin to 14.626 L biogas. kg− 1 VSin over time, which means the
difference between cumulatively produced biogas of the untreated
sludge and ozonized sludge decreased at the end of the 30 days. Besides,
the CBP difference increased from − 3.57 L biogas. kg− 1 VSin to 1.67 L
biogas. kg− 1 VSin at the end of the 10th compared to the end of the 30th
day for ozonized sludges with different ozone doses that indicate higher
ozone dose has a negligible effect on the final produced biogas amount
in a long time.
Secondly, the main methanogens phase for untreated sludge started
on the 12th day, and CBP gradually increased till the 14th day, which
reached its maximum value. It continuously increased till the 24th day.
All the CBP variations were smooth, corresponding to the typical
exponential growth of the anaerobic bacteria [40]. On the other hand,
the methanogenesis phase for ozonized sludge started earlier. It ceased
on the 21st day, which means no more degradable organic matter was
left in the sludge for methanogenic bacteria on that day. It might be due
to the fact that ozonation pretreatment significantly affected the accel­
eration of degrading organic matter and overall anaerobic digestion
process rather than exceeding degradable organic matters or even
higher ozone dose caused mineralization of organic matters [41].
In conclusion, investigating biogas production in the long term vs.
short term can indicate the importance of the sludge retention time in
biogas production. According to acquired data from the experiment,
ozonation pretreatment positively affected biogas production in the
short-term retention time of sludge in the anaerobic digestion process.
However, its effectiveness faded away in higher retention time. As a
result, higher sludge retention time not only has a limited influence on
biogas enhancement but also drastically increases the operational cost of
the wastewater treatment plant when ozonation is used as sludge pre-
treatment. Therefore, optimization of the sludge retention time (SRT)
should be performed to maximize biogas production and minimize
operation costs when ozonation pretreatment is implemented for the
anaerobic digestion process. Determining optimum SRT depends on the
factors such as the ozonation method (i.e., micro bubbling, macro
bubbling, etc.) and anaerobic digestion operational parameters (i.e.,
temperature, pH, CperN ratio, etc.). It may vary from sludge types and
treatment plants as well. Besides biogas production, other ozone con­
sequences, particularly in sludge composition, dewaterability, and en­
ergy balance, need to be considered in determining the most appropriate
SRT and ozone dose.
3.2. Effect of ozonation pretreatment on sludge composition
3.2.1. Impact of ozonation pretreatment on TS and VS reduction
Fig. 4 shows the concentration of TS and VS of each test after the
retention time of 10 and 30 days.
As shown in Fig. 4 (a), at the end of the 10th day, the total solids
concentration decreased from 38.8 gl-1 to 32.8 gl-1 and 34.2 gl-1 for 0.05
M. Hodaei et al. Biomass and Bioenergy 152 (2021) 106198

Fig. 4. The effect of the ozonation pretreatment on TS and VS reduction. (a) Total solids, (b) Volatile solids.

g O3g− 1 TS and 0.1 g O3g− 1 TS ozonized sludges, respectively.

Comparing these values with the initial TS concentration of 49.3 gl-1, the
calculated TS reduction rate increased from 21.3 % for untreated sludge
to 33.4 % and 30.6 % for 0.05 g O3g− 1 TS and 0.1 g O3g− 1 TS, respec­
tively. Obtained results from the long-term operation of the anaerobic
digestion revealed that the effectiveness of the ozonation on TS reduc­
tion is decreasing over time. For instance, the TS reduction rate at the
end of the 30th day for untreated sludge was 59.6 %, which increased to
62.2 % and 62.6 % for ozonized sludge, respectively. As demonstrated in
Fig. 4 (b), the same trend was observed for VS reduction because the
main reason for the TS removal was VS degradation and conversion to
biogas. Since mineral concentration was approximately constant during
the experiment (around 10 gl-1); therefore, the only parameters that can
alter total solids are the amount of the volatile solid.
As Fig. 4(b) elucidated, the volatile solids concentration at the end of
the 10th day decreased from 29.4 gl-1 for untreated sludge to 22.6 gl-1
for 0.05 g O3g− 1 TS and 23.5 gl-1 for 0.1 g O3g− 1 TS ozonized sludge. It
should be noticed that the higher ozone dose slightly decreased VS
reduction, which is in line with the decrease in biogas production in
higher ozone dose in 10 days of AD operation. The evaluation of the
ozonation effect on VS reduction shows the same variations as the last
part. The final VS concentration in both untreated and ozonized sludges
was close at the end of the 30th day.
Reduction in volatile solids degradation rate in higher ozone dose is
similar to previous research that volatile solids reduction by 0.063 g O3
g− 1 TS ozonation increased to 65 % while increasing the amount of
ozone to 0.083 g O3 g− 1 TS and 0.1 g O3 g− 1 TS, the amount of volatile
solid reduction dropped to 55 % and 57 %, respectively [38]. This
phenomenon occurred for two reasons. The first possibility is that the
organic materials were converted to minerals due to high ozone con­
centration [41–44]. Since the mineral concentration was approximately
constant with increasing ozone dose during all tests (about 10 gl-1), this
reason is not acceptable. The second reason could be acidic pH, which
inhibited the methanogenesis process. The acidity of the anaerobic
digestion process will be evaluated by the biochemical activity of bac­
teria. The methanogenic bacteria converted volatile fatty acids to
methane and carbon dioxide and stabilized the pH of the anaerobic Fig. 5. (a) The effect of ozonation pretreatment on pH variation (b) the impact
digestion process is which can effectively balance anaerobic digestion of ozone dose and pH variation on biogas production during the AD process in
acidity [45]. It is evident that ozonation accelerates the hydrolysis rate 10 days.
of organic matter, and higher ozone doses would increase it.
Consequently, 0.1 g O3 g− 1 TSozonation dose, speeding up hydro­ 7.2 to 6.45 for 0.05 g O3 g− 1 TS ozonized sludge. Increasing ozone dose
lysis, increases the concentration of volatile fatty acids while meth­ to 0.1 g O3g− 1 TS, the pH dropped to 6.45 on the 5th day, which, as
anogenic bacteria do not be able to convert them to biogas. Therefore, demonstrated in Fig. 5(b), biogas production was at the minimum rate,
system acidity will be increased, and pH will drop below the optimum and then it rose again along with the enhancement of biogas production.
pH of methanogenesis bacteria, which is between 6.5 and 7.2 [46–49]. Hence, this evidence proved that higher ozone dosage speeds up the
In particular, a pH lower than 6.7 will reduce methanogenic activity hydrolysis process with the rate that methanogenesis bacteria cannot
[50]. To prove this hypothesis, pH variation during the first 10 days was cope with that in a short time; therefore, biogas production would be
measured, and the results were demonstrated in Fig. 5(a). The effect of decreased.
ozone dose and pH variation on biogas production has been depicted in Despite the different ozone effects on sludge composition in the short
Fig. 5(b). Considering Fig. 5(a), pH varies from 7.2 to 7 untreated sludge retention time, it has a constant impact in a long time. In particular, TS
and 7.2 to 6.9 for 0.05 g O3 g− 1 TS ozonized sludge, while it ranges from and VS decreased as the ozone dose increased. However, the difference

5
M. Hodaei et al.
between the final TS and VS concentration after 30 days was the same
for each test. It shows that ozonation efficiency will be decreased over a
long time, as observed in the previous part.
3.2.2. Effect of ozonation pretreatment on biogas production yield (BPY)
BPY is an essential factor that implies converting the rate of organic
matters into biogas. Table 1 shows the BPY values for each test. As ob­
tained results show, the ozonation pretreatment significantly increased
sludge BPY by 62.23 % for 0.05 g O3g− 1 TS and 53.12 % for 0.1 g O3g− 1
TS in the retention time of 10 days, which is correlated to previous
studies that proved ozonation pretreatment successfully enhance biogas
yield [51,52]. Otherwise, these values drastically dropped to 7.760 %
and 6.940 % for ozonized sludge after 30 days of the AD operation,
which is not directly pointed in the previous studies. In fact, ozonation
enhances the degradation rate of complex organic matters, which aided
biogas production as well as VS reduction. However, no significant ef­
ficiency has been observed for ozonation in long sludge retention time,
resulting from the sludge type and characteristics.
3.3. Effect of ozonation on sludge dewaterability
As one of the essential parts of the wastewater treatment plant, the
digested sludge dewatering process has the highest operational costs. It
is critical decreasing sludge volume to minimize the cost of transporting
sludge to the landfill, especially for the South Tehran wastewater plant
due to the high production of sludge volume and lack of available
landfills. The dewatering process has been carried out by various
physical methods such as vacuum filter, centrifuge, belt press, etc. In the
filtration approach as a typical technique for dewatering, capillary
suction time (CST) and sludge resistance to filtration (SRF) are consid­
ered as quantitative indexes for the evaluation of the dewatering per­
formance [53]. In the current study, the centrifuge was utilized for
dewatering, and VDP (Volumetric Dewatering Percentage) and dry
solids (DS) were considered as evaluation factors of dewaterability
performance. Three samples were performed for each experiment. The
obtained results for VDP and dry solids for different retention times were
demonstrated in Fig. 6.
As the results of Fig. 6 depicted, the ozonation pretreatment with
different dosages increases the sludge dewaterability and obtained dry
solids in short and long retention times compared to untreated sludge;
therefore, it has a great impact on the reduction of residual sludge
volume as well as its water content. In particular, VDP increased from
50 % for untreated sludge to 58 % and 61 % for 0.05 g O3 g− 1 TS and 0.1
g O3g− 1 TS ozonized sludges respectively in 10 days (Fig. 6(a)). More­
over, the conversion of organic substances to biogas decreases sludge
content [23]; therefore, VDP has increased over time, and consequently,
sludge dewatering has become easier. However, Fig. 6(b) revealed that
the differences between the dewaterability of various ozone doses
decreased in the long retention time due to changes in sludge texture.
Moreover, the sludge residue will become very thick in the higher
dewatering process, and the DS increased above 50 % for ozonized
sludge after 30 days. Besides, it indicates that sludge dewaterability
increased in higher ozone dosage because ozonation in low doses causes
particle size reduction, which deteriorates sludge dewaterability [54].
Dry solids for untreated sludge was 20 % and increased up to 28 %,
Table 1
Effect of ozonation pretreatment on Biogas Production Yield.
Short-Retention time (10 days)
− 1
Ozone dosage (g O3g TS)
Untreated 0.05
Biogas Volume(L) 1.050 2.820
Reduced VS(kgl− 1) 0.0104 0.0172
BPY 100.6 163.15
Difference (%) – +62002E23
6
Biomass and Bioenergy 152 (2021) 106198
and 36 % for 0.05 g O3 g− 1 TS and 0.1 g O3 g− 1 TS ozonized sludge,
respectively in 10 days (Fig. 6(a)), which is higher than the average dry
solids concentration of filtered sludge (20–25 % dry solids). These re­
sults are along with previous studies in which ozonation effectively
enhanced sludge amount after dewatering [55,56]. However, after 30
days of digestion, dry solids reached 48 % for untreated sludge and up to
50 % for ozonized sludges indicating that ozonation has less influence on
dewaterability in long-term digestion (Fig. 6(a)).
These results are conflicts with previous researches about ozone
pretreatment effect on sludge dewaterability, indicated low ozone dose
(<400 mgO3g− 1 TS) decreases sludge dewaterability [57,58] due to
enhancement of SRF (sludge resistance to filtration) and CST (capillary
suction time) by producing more fine particles [36]. Ozonation can
significantly affect the physicochemical properties of the sludge, which
is directly related to sludge dewaterability. Many researchers utilized
belt filter press or similar methods for sludge dewatering. The perfor­
mance of these methods can be quantified by optimizing variables like
CST, hydrophobicity, etc. However, these parameters depend on some
specific sludge properties, including available particle surface area to
contact with water-bound, protein content, EPS concentration, and
dissolved matter that ozonation pretreatment can efficiently improve
them in a higher dose [53]. The centrifuge method, independent of
available particle surface area and more effective for separating water
from a residual part of sludge in low ozone dosage, was implemented for
dewatering in the current research. It may be because ozone first dis­
rupts the aggregated flocs, destroys the bacteria cell’s wall, emits
intercellular water, and destroys complex matter into simple structures
[53]. In other points of view, fine particles could retard filtration by
clogging filter porous media while the centrifuge process is not influ­
enced by fine particles [59–61].
3.4. Energy balance of ozonation pretreatment
The significant factors affecting the total cost of the scaling up
ozonation pretreatment for treatment plants are energy production and
consumption. Therefore, the produced and consumed energy for ozone
pretreatment as well as energy balance have been calculated here. The
results were summarized in Table 2. It should be noted that because of
the ideal condition assumption, energy loss is supposed to be negligible
during ozonation and sludge digestion; consequently, it was not entered
into the calculation. On the other hand, energy balance measurement is
a comparative analysis between ozonation energy demand and final
produced energy to reveal the sustainability of ozonation pretreatment.
As indicated, values of consumed energy in comparison with pro­
duced energy for ozonized sludge are very high. In particular, 0.05 g O3
g− 1 TS and 0.1 g O3 g− 1 TS ozonized sludges could provide only 37.8 %
and 28.5 % of their consumed energy for ozonation in 10 days. These
values were increased over time because of more biogas production
during the anaerobic digestion process. Besides, the energy balance for
all ozone pretreatment tests is negative in the short and long retention
time, which indicates ozonation has high energy demand as a pre­
treatment method. Still, it should be considered that ozonation has other
benefits, including reducing organic carbons, increasing sludge dew­
atering, and also reducing methane leakage through landfills. Therefore,
rather than energy demand, other comprehensive economic analyses are
Long-Retention time (30 days)
1
Ozone dosage (g O3g− TS)
0.1 Untreated 0.05 0.1
2.520 6.450 7.440 7.560
0.0163 0.0293 0.0314 0.0322
153.98 219.5 236.5 234.6
+53.12 – +7.760 +6.940
M. Hodaei et al.
Fig. 6. Ozonation pretreatment effects on sludge dewaterability and obtained Dry Solids for the retention times of (a) 10 days (b) 30 days.
Table 2
Effect of ozonation on energy balance.
Short-term (10 days) Long-term (30 days)
Ozone dose [g O3g− 1 0 0.05 0.1 0 0.05
TS]
Ozonation Energy [kJ] 0 324 388.8 0 324
Produced Energy [kJ] 44.4 122.7 110.9 272.7 323.7
Energy Balance [kJ] 44.4 − 201.3 − 277.9 272.7 − 0.3
needed to evaluate whole aspects of ozone pretreatment, which is out of
the scope of this research, and it is strongly recommended for further
investigation. Nevertheless, we believed that the obtained results could
provide useful information about the feasibility of ozone pretreatment
capacity for sustainable management of different sludge from economic
and technological perspectives. All obtained results in this study are
summarized in Table A3 in supporting information.
4. Conclusion
The influence of ozone as a strong oxidizing agent on improving the
performance of anaerobic sludge digestion at a particular rate and
biogas production, sludge chemical composition, and dewaterability in
short and long retention times has been investigated. Obtained results
demonstrated that the ozone effect on the biogas production and other
anaerobic digestion parameters of waste-activated sludge highly de­
pends on the ozone dosage and sludge retention time. Biogas produc­
tion, volatile solids reduction, sludge dewatering, and energy efficiency
were measured for two ozone dosages of 0.05 and 0.1 g O3g− 1 TS. The
results were compared to the untreated sludge values after 10 and 30
days of sludge retention time. MDBP increased from 2.08 to 6.26 L
biogas. kg− 1 VSin.d− 1 by ozonation. At the end of the 10th day, the total
solids concentration decreased from 38.8 gl-1 to 32.8 gl-1, and 34.2 gl-1
for 0.05 g O3 g− 1 TS and 0.1 g O3g− 1 TS ozonized sludges, respectively.
The obtained results after 10 days showed that ozonation increased
digested sludge quality by reducing volatile and total solids concentra­
tion as well as increasing sludge dewaterability. However, higher ozone
dose increased energy consumption and reduced anaerobic sludge
digestion performance, including biogas production rate and volatile
solids reduction. It was because the higher ozone dose accelerated the
hydrolysis phase rapidly, which increased the volatile fatty acid con­
centration in the acidogenesis phase, which caused methanogenic bac­
teria performance reduction due to their sensitivity to acidic pH. After
30 days of digestion, the results of both ozonated sludge and untreated
sludge showed approximately the same performances in biogas pro­
duction and sludge physic-chemical properties, which indicates the
importance of the sludge retention time along with ozone dose in
ozonation pretreatment for anaerobic digestion.
As conclusion, lower ozone dose (0.05 g O3g− 1 TS) for ozonation
pretreatment of anaerobic digestion was more effective in short-term
sludge retention time (10 days), and its effectiveness faded away by
time in compared to untreated sludge.
Biomass and Bioenergy 152 (2021) 106198
Acknowledgments
The authors are grateful to the Sharif University of Technology. This
research did not receive any specific grant from funding agencies in the
0.1 public, commercial, or not-for-profit sectors.
388.8
Appendix A. Supplementary data
332.7
− 56.1
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.biombioe.2021.106198.
Data availability
The raw data will be available based on request.
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