Journal of Ecological Engineering

Journal of Ecological Engineering 2023, 24(10), 351–359 Received: 2023.07.24

https://doi.org/10.12911/22998993/170897 Accepted: 2023.08.09
ISSN 2299–8993, License CC-BY 4.0 Published: 2023.08.24

Removal of Organic Pollutants from Wastewater Using

Different Oxidation Strategies

Nibras Raad Fajri1, Rusul Naseer Mohammed1*

1
Department of Chemical Engineering, College of Engineering, University of Basrah , Basra City, Iraq
* Corresponding author’s e-mail: [email protected]

ABSTRACT
Many countries use nontraditional methods to treat wastewater, especially those with water lacks. Among these
methods, heterogeneous photocatalysis is more commonly widely used since it converts organic molecules into
carbon dioxide and water. In this study, the photocatalytic degradation process of total organic carbon was inves-
tigated by TIO2/UV technique (TUT). This treatment is carried out in a batch recycle reactor using a UV light and
catalyst TIO2. The optimum operating parameters were investigated regarding the best organic removal including,
total organic carbon concentration, flow rate, pH, irradiation time, and photocatalysis dosage. The result showed
that the TUT is affected by reducing total organic carbon (TOC) from synthetic wastewater (SW) by 61% at 50 ml/
min of flow rate, 250 mg of catalyst concentration TIO2, and a concentration of TOC of 25 mg/l. Then the result
of TUT was compared with a process of combining TIO2/UV and an oxidizing agent (Hydrogen peroxide H2O2).
It was found that 73% of organic removal was obtained which is best than TUT when using an H2O2 dosage of
100 mg/l. Experimentally, Ozone was also added to the process of TUT and the result showed that the removal
percentage increased to 80%.

Keywords: catalysis, wastewater, oxidation, UV, organic matter removal.

INTRODUCTION wastes, and by-products generated to treat waste-

water (Ren et al., 2021). also, these techniques
A natural resource that is vital to human sur- might not be very successful. Due to the costly
vival is water. However, the lack of this priceless equipment required for these processes (Moham-
resource has emerged as a significant issue for the med et al., 2022). An efficient substitute for the
majority of nations worldwide. This is typically treatment of wastewater has been created called
caused by effluent from human activities, primar- the advanced oxidation process (AOPs), This pro-
ily industry and agriculture, contaminating its cess is highly efficient and can be used to treat
sources (Preisner, 2020). due to the presence of a wide range of pollutants, including persistent
organic matter and biological and, raw water is organic pollutants (POPs). furthermore, the ad-
invalid for human consumption (Ali et al., 2012). vanced oxidation process AOPs are cost-effec-
There are many different technologies applied in tive and can be used in large-scale applications
wastewater decontamination, primarily including (Zhang and Sun, 2021). AOPs are additionally
electrodialysis (Zazouli et al., 2017), membrane non-destructive and do not create any harmful by-
filtration (Zularisam et al., 2006), precipitation products. Although hydrogen peroxide frequently
(Azimi et al., 2017), adsorption (Yagub et al., supplies (Teh and Mohamed, 2011) the active hy-
2014), electrochemical reduction (Mousset et droxyl radicals, utilizing it increases the process’s
al., 2020), and electro deionization (Arar, 2014). operating costs. Highly active hydroxyl radi-
These processes usually consume large amounts cals (Ledezam Estrada, et al., 2012), which are
of energy and may be more complicated by trans- produced by a number of sources, are involved
ferring pollutants between different fluids, various in the oxidation process (Ledezam Estrada,

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Journal of Ecological Engineering 2023, 24(10), 351–359

et al., 2012). The combination of photocatalyst carbonate, sodium hydrogen carbonate, Bacterial
with the ozone method has been successfully peptone, Glucose anhydrous, and Beef extract
used for the degradation of organic substances in broth) as shown in Table 1. A typical biodegrad-
an aqueous solution, such as formic acids (Wang, able and nontoxic wastewater has been utilized
et al., 2002), dibutyl phthalate (Kercet et. al, as a substrate to measure its effect of treatment
2003), and mono chloroacetic acid and pyridine methods (Wilson et al., 1997; Doskaliyev et al.,
(Li et al., 2005) . This paper aimed at three differ- 2018). Under various operational conditions,
ent parts: the first part is the study of the removal TUT was used in a photo reactor to analyze syn-
of total organic carbon (TOC) from (SW) using thetic wastewater with different concentrations of
combined of TIO2/UV technique (TUT) under total organic carbon. Distilled water was used to
various operating settings, including TOC con- dilute the stock solution in order to obtain various
centration, flow rate, irradiation time, and TIO2 concentrations.
dosage. The second part investigates the impact
of TiO2 and H2O2 together on organic deteriora- Experimental setup
tion. The third part is the impact of TiO2 and O3
together on organic deterioration. Also, study the In this study, three different configurations
kinetics of organic decomposition using (Pseudo- were performed as shown in Figures 1a and 1b,
first-order model). a set-up of two schematics for an experiment. In
configurations (I) and (II), an annular photo reac-
tor is used for batch recycling with TUT while
MATERIALS AND METHODS H2O2 is added in configuration (II) named TiO2-
UV, H2O2 technology (TUHT). (A clear glass
Materials tube with a UV wavelength of 254 nm, 42 v, 6
W, measuring 1.6 cm in diameter and 2.12 cm in
Materials that are used in this study is tita- length (TUV 6 W 4P-treated wastewater included
nium dioxide nanopowder as a catalyst, with par- in 500 ml). The irradiation volume was 57 ml, in
ticle sizes of 10±30 nm, a specific surface area contrast. The peristaltic pump was used to control
of 50±100 m2/g, and a weight ratio of 70 anatase the flow rate (Drive model BT300M, Drive size
to 30 rutile. The stock solution is prepared for 234×154×143 mm), and max flow (250 ml/min).
each experiment including (potassium hydrogen A pH meter (INOLAB 72 WTW CO., Weilheim,
Germany) was used to measure the solution’s pH.
Table 1. Stock wastewater’s composition In configuration III, the ozone generator is used
Constituents Concentration, g/l* with the same schematic as configuration I and II.
Beef extract broth 0.3
Bacterial peptone 0.42 Process analysis
Glucose (C6H12O6) 0.165
Sodiumhydrogen carbonate
Samples were taken out of each experiment
0.04 at intervals of two hours for analysis. then, it was
(CHNAO3)
Potassium hydrogen filtered using Chromophile Xtra (0.2 MN) to de-
0.04
carbonate (CHKO3) termine the total organic carbon (TOC) content of
Note: * The concentration of total carbon was 0.9 g/l. the sample. The TOC-LCSH standalone method

Figure 1. Diagram depiction of the experimental unit: (a) TUT, (b) TUOT

352
 Ct
% Removal = �1 − � × 100
Ci
Journal of Ecological Engineering 2023, 24(10), 351–359
dC Ct
% Removal
R = = �1 =−−kC� × 100
Table 2. Experimental conditions dt (2): Ci
By integrating equation
Parameter Range CtdC −kt
Flow rate (ml/min) 50±250 R= == e −kC (3)
Cidt
TOC (mg/l) 25±500
The following CtCt −kt
TiO2 (mg) 50±500 ln relationship
==e −kt can be found by
Total volume treated (ml) 500 CiCo
taking the natural logarithm of equation (3):
UV lamp (w/nm): 6/245 Ct
ln = −kt (4)
Temperature (C): room temperature 21–25 Co
Time (hours) 2
In equation (4), the plot ln (Ct) as a function
of time for a first-order reaction is linear.
Table 3. The TOC analysis details
Carrier gas Nitrogen (99.999%)
High-temperature
Technique of digestion
combustion
RESULTS AND DISCUSSION
The heat required for
combustion
680 °C Process configuration by TUT
Catalyst Regular
In the first part of this study, the process con-
Sample volume (ml) 50 µl
figuration that is shown in Figure 1a is occupied
Rinse volume (ml) 2000 µl
by photocatalytic and TiO2. The reaction occu-
Repeats for the TOC 3 pied by TiO2 photocatalysts is activated by light
radiation, specifically photons, as reported by
was used to measure TOC concentrations. Table (Baran et al., 2008). Excitation of electrons oc-
2 shows the experimental conditions used in this curs when the energy of solar radiation surpasses
work and Table 3 provides further information on the bandgap of TiO2, leading to the transition
the TOC analysis. of electrons from the valence band (VB) to the
conduction band (CB). The aforementioned pro-
cess generates electron-hole pairs, whereby the
Removal finding valence band (VB) holes exhibit notable oxida-
Equation (1) was used to calculate the per- tion reaction activity within the range of 1.0 to
centage of TOC removal. 3.5 volts, while the conduction band (CB) elec-
trons demonstrate favorable reducibility within
Ct
% Removal = �1 − � × 100 (1) the range of 0.5 to 1.5 volts. Upon exposure to
Ci light, TiO2 generates positive holes and electrons
where: Ci is the totaldC
organic carbon concentration in its valence band (hv + vb) and conduction band
R= = −kC (e-cb), as reported by (Poulopoulos et al. 2004).
at the start ofdtthe treatment procedure;
Ct is the total The formation of hydroxyl radicals (Equation 3)
Ct organic carbon concentra-
tion at a certain −kt
= epoint in time. or direct reaction with organic molecules can
Ci result in the oxidation of organic molecules as
Ct posited by Ahmad et al. (2016). Reduction prod-
Kinetic rate modelln = −kt
Co ucts can be generated by a sequence of reactions
The correlation between the experimental re- (Equations 5-11) in which electrons engage with
sults and the response deterioration may be mea- organic compounds. The involvement of oxygen
sured using typical kinetic rate expressions. Pseu- in these reactions is significant, as it undergoes a
do-first-order reactions are used in the majority reaction with the electrons generated by the pho-
of degradation processes. Ct tochemical process. Organic compounds have
% Removal = �1 −(Hameed and Mousa,
� × 100
Ci
2019) expressed used in equation (2) : the potential to undergo oxidative degradation
dC via their interactions with hydroxyl and peroxide
R= = −kC (2) radicals, valence band holes, and reductive cleav-
dt
age through electron reactions. This process leads
Ctconstant
where: K is the rate for the pseudo-first- to the formation of diverse byproducts and ulti-
= e−kt
order, min Ci.
-1
mately mineral end-products.
Ct
ln = −kt 353
Co
Journal of Ecological Engineering 2023, 24(10), 351–359

hv + TiO2 → hv+vb + e-cb (5) restricted at high flow rates. Elevating the flow
rate resulted in a reduction of the residence time
OH-surface + hv+vb → OH• (6) and an increase in the thickness of the water layer.
(7)
This, in turn, impeded photon penetration to the
H2O absorbed + hv+vb → H+ + OH•
liquid/solid interface (Kane et al., 2022).
e-cb + O2 absorbed → O-2 (8)

Organic + hv+vb → Oxidation products (9) Effect of catalytic dosage

Organic + OH• → Degradation products (10) Figure 3a shows the effect of a catalytic dosage
ranging between (50±500) mg in 500 ml on total
Organic + e-cb → Reduction products (11)
organic carbon (TOC) removal. The experimental
results depicted that a 24% removal rate in TOC
Effect of initial TOC concentrations was achieved when using 50 mg TiO2/500 ml. The
increase of catalysis dosage to 250 mg TIO2/500 ml
Figure 2a shows the change of concentration
resulted in a 61% removal of total organic carbon
over time for various initial total organic carbon
(TOC), which exhibited negligible variation when
(TOC) concentrations that were studied (20±500)
the titanium dioxide dosage was increased to 500
mg/l at pH 7, 250 mg of TIO2, 50 ml/min of flow,
mg TIO2/500 ml. According to Chakrabarti et al.
and UV light. It is obvious that the removal of
TOC is reduced generally by the rise in concen- (2004), beyond a certain time, the process is not ac-
tration. The explanation for this reality, there are celerated by an increase in the amount of catalyst as
more molecules available in the solution at low the treated solution becomes impenetrable to UV ir-
concentrations which makes it easier for UV light radiation. It is obvious that TUT played a critical role
to reach the catalyst surface and increases the pho- in attaining significant total organic carbon (TOC)
tocatalytic removal rate. However, at greater con- removals. As a result, the dosage of 250 mg TIO2
centrations, the initial organic carbon content had per 500 milliliters was subsequently employed.
a negative impact on the photocatalytic treatment
because there were fewer reactive species present Effect of irradiation time
as present previously by (Sharma et al., 2010).
The effect of reaction time on the photocata-
lytic degradation efficiency of TIO2 on TOC re-
Effect of flow rate
moval was investigated, as depicted in Figure 3b.
Different flow rates are used in this study at It was noticed that the overall TOC removal was
an initial concentration of 20 mg/l, and TIO2 of increased from 7% to 61% as the oxidation time in-
250 mg as shown in Figure 2b. The result shows creased from 30 to 120 minutes. However, the re-
that the TOC removal was increased when the moval rate remained constant as the oxidation time
flow rate decreased due to the prolonged duration was further extended. According to that, the most
of the residence period. A high flow rate condi- favorable parameters for achieving the highest lev-
tion, results in an increased opportunity for the els of total organic carbon (TOC) removal efficien-
TOC to participate with the radicals present at the cies were found to be 120 min of irradiation time,
interface of the solution and the catalytic surface. 20 mg/l of initial TOC concentration, 250 mg/500
However, the removal efficiency was found to be ml of TIO2 and 50 ml/min of a flow rate.

a) b)

Figure 2. Removal efficiencies of TOC (a) at different concentrations for TIO2 = 250 mg,
Q = 50 ml/min. (b) at different flow rates for TIO2 = 250 mg, TOC = 20 mg/l

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 Journal of Ecological Engineering 2023, 24(10), 351–359

a) b)

Figure 3. Removal efficiencies of TOC: (a) at various catalysis dosages for TOC = 20 mg/l,
UV, Q = 50 l/min, (b) effect of oxidation time on the removal efficiencies of TOC

Process configuration by TUHT The highest rate of degradation was found for H2O2
(100) mg/l. but over-dosing of H2O2 (more than
The effect of the addition of hydrogen perox- 100) may lead to concurrent reactions that might
ide to TUT as oxidant on TOC removal, Optimized consume H2O2 or lead to H2O2 self-decomposing
catalyst concentration, and optimized initial TOC into oxygen and water, reducing the production of
concentration was studied by varying amounts OH radicals and decreasing the effectiveness of
of H2O2 (50, 100, 150) mg/l shown in Figure 4 TOC removal (Kruithof et al., 2007).
which shows the variation in the photo-degrada-
tion rate of TOC for a different amount of H2O2. Process configuration by TUOT

For the treatment of organic compounds that

are barely degradable, a combination of photo-
catalysts and ozone is a feasible option since the
organic compounds are anticipated to degrade
more quickly and accomplish complete miner-
alization to water and carbon dioxide. Adsorbed
ozone can clearly operate as a very powerful
electrophilic agent to form OH radicals through
O3. reaction pathways (Equation 12) by trapping
photoproduced electrons in the heterogeneous
photocatalytic process with ozone (Sanchez et
al., 1998). Ozone input dosage of 200 mg/h with
Figure 4. at different H2O2 dosage for TOC = 25 250 mg of TIO2 to obtain the removal efficiencies
mg/l, UV, Q = 50 l/min, and TIO2 = 250 mg of TOC 80%.

Figure 5. Removal efficiencies of TOC at different process TUT, TUHT, TUOT

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Journal of Ecological Engineering 2023, 24(10), 351–359

O3 + e-→ O3ℴ- (12) Table 5 shows that the rate of TOC removal k
increases as the initial concentrations of TOC de-
O3ℴ- + H+ → HO3 (13) crease 0.0083, 0.0042, and 0.0020 min-1 for TOC
initial 20, 150, and 500 mg/l respectively. The K
HO3ℴ → O2 + OHℴ (14)
values using different TIO2 dosages were 0.0024,
0.0083, and 0.0076 min-1 For 50/500, 250/500,
Kinetic results and 500/500 mg/l respectively. The rate constant
increases at a TIO2 concentration of 250 mg/500
Equation (4) was applied to all of the experi- ml. Also, the k values increase as the flow rate de-
mental results to find the rate of reaction (removal crease 0.0083, 0.0063, and 0.0049 min-1 for flow
of TOC by TUT). In pseudo-first order; a plot of rate 50, 150, and 250 ml/min.
(-ln Ct/Ci) vs. time is shown in Figure 6. The slope For K values increase when using TUOT to
of the line in this plot is equal to the pseudo-first- 0.013 min-1 which is higher than the k value of
order rate constant k (min-1) and the intercept is 0.0083 min-1 using TUT for the removal of 20
equal to ln (Ci). The calculated value of k for the mg/l TOC concentration. Also, k values are high
different operating conditions listed in Table 4. when using TUHT to 0.011 min-1.

Figure 6. First-order rate constant of TOC removal by TUT at 20 mg/l concentration, 250 g TIO2

Table 4. First-order rate constant k (min-1) under various conditions of operation

Exp. Toc conc., mg/l TIO2, mg/l Flow rate, ml/min K, min-1 R2
1 20 250/500 50 0.0083 0.956
2 150 250/500 50 0.0042 0.9704
3 500 250/500 50 0.002 0.6636
4 20 50/500 50 0.0024 0.9107
5 20 250/500 50 0.0083 0.956
6 20 500/500 50 0.0076 0.9316
7 20 250/500 50 0.0083 0.956
8 20 250/500 150 0.0063 0.9556
9 20 250/500 250 0.0049 0.9427

Table 5. First-order rate constant k (min-1) under various conditions of process

Process Toc conc., mg/l TIO2, mg/L Flow rate, ml/min H2O2, mg/l O3, mg/h K, min-1 R
TUT 20 250/500 50 0 0 0.0083 0.956
TUHT 20 250/500 50 100 0 0.011 0.975
TUOT 20 250/500 50 0 200 0.013 0.880

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Table 6. Comparison between TIO2, TUT, TUHT, TUOT for different times
Time (min) LSD0.05
Type
0 30 60 90 120 p-value
0 1.34% 3.90% 4.53% 6.64% 3.743
TIO2
d c b ab a 0.0049 HS
0 7.42% 23.18% 49.83% 61.15% 4.357
TUT
e d c b a 0.0051 HS
4.632
0 35% 54.50% 69.30% 73.20%
TUHT 0.0017 HS
d c b a a

0 51.50% 74.56% 77.90% 80% 3.666

TUOT
d c b ab a 0.023S
LSD0.05 4.249 3.489 5.341 3.440
NS
p-value 0.0032S 0.0026S 0.0013HS 0.0143S
Note: NS – non-significant difference at 0.05 level S: significant difference at 0.05 level, HS – high significant
difference at 0.01 level . Different letters are significant difference between groups.

Figure 7. Comparison between TIO2, TUT, TUHT, and TUOT for different times

Statistical analysis method is a good method for TOC where 61%

of TOC removal is achieved under 25 mg/l of
The statistical program SPSS (Statistical Pack- TOC initial, 250/500 mg/l of TIO2. Also, the re-
age for Social Science) version 26 is used to analyze sult concluded that adding 100 mg/l H2O2 to the
the dataset used throughout this study. the analysis TUT system called the TUHT process was 73%
of variance (ANOVA) is used to compare between successful for TOC removal. As a result, the ad-
the groups. lest square difference (LSD) test was dition of a zone significantly increased the TOC
used to check the multiple comparisons between removal to (80%). It was concluded that the re-
groups with a significant level of 5% (p-value < moval of total organic carbon is decreased as its
0.05) and 1% (p-value < 0.01) (Table 6). The result initial concentration increase, reaching 61% at 20
of the statistical analysis is shown in Figure 7. mg/l TOC concentration at 2 hours. but was not
exceeded 3% at 500 mg/l. Also, effect of flow rate
and catalytic TIO2 dosage on the TUT methods
CONCLUSIONS were systematically evaluated, and the most fa-
vorable conditions were found to be at the flow
The photocatalytic method was used to clean rate of 50 l/min, and TIO2 dosage of 250 mg/500
synthetic wastewater that was primarily made ml. Increasing the concentration of H2O2 from 50
up of organic carbon in this study. Total organic to 100 mg/l increased TOC removal from 56% to
carbon removal was measured using different 73%. The kinetic study concluded that the TOC
combinations of titanium dioxide, UV, hydro- removal increases when using TUOT to 0.013
gen peroxide, and ozone. It was concluded, TUT min-1 of K values which is higher than the 0.0083

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Journal of Ecological Engineering 2023, 24(10), 351–359

min-1 k value when using TUT for the removal Hazardous Materials, 112(3), 269–278.
of 20 mg/l TOC concentration. Also, it was in- 11. Dhaka S., Kumar R., Lee S Hun, Kurade M.B., Jeon
creased to 0.011 min-1 k when using TUHT. As a B.H. 2018. Degradation of ethyl paraben in aque-
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12. Doskaliyev, D., Poulopoulos, S.G., Yeshmuratov,
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