Global J. Environ. Sci. Manage.

10(1): 13-26, Winter 2024, Serial #37

Global Journal of Environmental Science and Management

(GJESM)

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ORIGINAL RESEARCH PAPER

Green synthesis of titanium dioxide photocatalyst using Lactobacillus bulgaricus for

processing palm oil mill effluent
L. Agustina1, M. Romli2, P. Suryadarma2, S. Suprihatin2,*
1
Agroindustrial Engineering Study Program of Graduate School, IPB University, PO Box 220, Bogor, West Java, Indonesia
2
Department of Agroindustrial Technology, Faculty of Agricultural Engineering and Technology, IPB University, PO Box 220,
Bogor, West Java, Indonesia

ARTICLE INFO A B ST R AC T
BACKGROUND AND OBJECTIVES: To improve photocatalytic degradation perfomance,
Article History: photocatalyst particles with a larger surface area preferred. The effectiveness of titanium dioxide
Received 16 January 2023 as a photocatalyst depends on the synthesis method used. The method affect the particle size,
Revised 02 June 2023 crystallinity and phase composition of the produced catalyst. This study aims to develop a green
Accepted 11 July 2023 synthesis process of nano- titanium dioxide photocatalysts for the advanced treatment of palm oil
mill effluent.
METHODS: The green synthesis of titanium dioxide nanoparticles used de Man-Rogosa-Sharpe
Keywords: broth media containing Lactobacillus bulgaricus culture and titanium oxyhydroxide metal oxide.
Advanced wastewater treatment The factors investigated were the molarity of titanium oxyhydroxide (0.025 molar; 0.035 molar
and 0.045 molar) and temperature (40; 50 and 60 degrees Celsius). The synthesized photocatalyst
Green synthesis was characterized using a particle size analyzer to determine the particle size. The produced
Palm oil mill effluent photocatalyst with a nanoparticle size range of 1-100 nanometer was further characterized using
Nano titanium dioxide scanning electron microscopy-energy dispersive X-ray and X-ray diffraction. The photocatalyst
Photocatalytic process was tested for advanced treatment of palm oil mill secondary effluent. The factors investigated in
this test included the irradiation time and titanium dioxide photocatalyst dosage. The treatment
performance was evaluated in terms of effluent quality and pollutant elimination efficiency.
FINDINGS: Nano titanium dioxide photocatalysts have been synthesized through titanium oxyhydroxide
metal oxide biologically using Lactobacillus bulgaricus. The synthesis process at a temperature of 60
degrees Celsius and a 0.025 molar metal oxide solution produced a titanium dioxide photocatalyst
with a size of 33.28 nanometer. The content of titanium and oxygen constituents in the photocatalyst
was confirmed to be 39.06 percent and 47.95 percent respectively, with 67.6 percent titanium
dioxide crystallinity in a theta degree of 25.4. This indicates that the green synthesis has produced an
anatase diffraction nano titanium dioxide photocatalyst. Testing the titanium dioxide photocatalyst
to treat palm oil mill secondary effluent yielded in elimination efficiency of 16.16-27.27 percent for
chemical oxygen demand and 11.05-21.95 percent for biological oxygen demand. Phenol, which is
toxic and difficult to degrade biologically, could eliminated significantly (up to 81.12 percent) using a
photocatalyst dose of 1 gram per liter at a time irradiation of 2.5 hour.
CONCLUSION: The biological synthesis of nano titanium dioxide photocatalysts is affected by
temperatures and metal oxide concentrations. The photocatalytic process for advanced treatment
of palm oil mill secondary effluent shows that this synthesis process effectively eliminates phenols.
Some compounds such as lignin, amino acids, and pectin are not significantly mineralized using this
DOI: 10.22034/gjesm.2024.01.02 process.

This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).

NUMBER OF REFERENCES NUMBER OF FIGURES NUMBER OF TABLES

42 6 3
*Corresponding Author:
Email: [email protected]
Phone: +62813 1089 5109
ORCID: 0000-0001-9641-8820
Note: Discussion period for this manuscript open until April 1, 2024 on GJESM website at the “Show Article”.
 L. Agustina et al.

INTRODUCTION TiO2 photocatalyst is combined with feroxalate and

The increase in crude palm oil (CPO) production exposed to a stream of ozone, yielding a 54 percent (%)
increases in the amount of liquid waste (Palm Oil Mill decrease in organic compound content (as measured
Effluent/POME) produced (Agustina et al., 2021). by the decrease in chemical oxygen demand (COD)
Biological treatment (anaeraobic and aerobic) has value). A decolorization effect of 90% on congo red
been widely applied to treat POME because the with the use of TiO2 combined with gadolinium has also
processing costs are low. However, the resulting been achieved in previous research (Khademalrasool
effluent still contains contaminants in the form of et al., 2016). This research used a TiO2 nanoparticle as
suspended and dissolved materials difficult to degrade the photocatalyst to provide an improved effect on
biologically (recalcitrant), such as pectin, lignin, degradation of palm oil mill wastewater. Efforts were
tannins, and other phenolic compounds (Zainuri et al., made in this research to improve the characteristics
2018; Samimi and Shahriari-Moghadam, 2020). These of TiO2 through green synthesis. Method for creating
materials can cause the effluent to be colored, causing nanoparticles, include physical, chemical, and
water pollution problems and ecosystem disturbances. biological processes. However the biological method
The remaining pollutants in the effluent need to be is the simplest and uses no chemicals (Agustina et al.,
removed using appropriate methods to produce clean 2020). This method can improve the properties of TiO2
water to support palm oil mill activities, where the photocatalysts thus, the biological approach is thought
need for clean water at factory sites is now becoming a to be more ecologically friendly (Mukherjee and Nethi,
problem. Therefore, the development of a wastewater 2019) and efficient. TiO2 nanoparticles with a size of
recycling process in palm oil mills can be a win-win 30 nanometer (nm) with a tetragonal structure and
solution for environmental and economic interests. anatase phase (which has the best ability to degrade
Considering that pollutants in the effluent of biological organic compounds because it has the highest
processes are generally difficult to degrade biologically bandgap) have been proven in research (Jha et al.,
(recalcitrant), non-biological process is suitable for 2009) using Lactobacillus on nutrient-broth media. To
eliminating these pollutants. To achieve this goal, the increase the adsorption ability of a TiO2 photocatalyst
research plan is intended to develop a photocatalytic (Azhar et al., 2011) performed synthesis with the help
degradation process for eliminating dissolved organic of Lactobacillus on de Man-Rogosa-Sharp (MRS) broth
pollutants difficult to degrade biologically. A review of media, however the size of the TiO2 photocatalyst
the results of previous research shows that this method produced was still large (150 nm). Based on the results
has various advantages for advanced wastewater obtained from their research, green synthesis of TiO2
treatment (Wang et al., 2022), such as being effective was performed in this research to improve its physical
for recalcitrant pollutants, and the process is fast, does and chemical characteristics so that it can be used as a
not depend on microbial activity, and can utilize local photocatalyst in the processing of palm oil liquid waste
resources (Li Puma, 2003; Fathinia and Khataee, 2013; using the photocatalytic method. The green synthesis
Ng and Cheng, 2015; Ng et al., 2019). The performance method is expected to provide advantages that are not
of the photocatalytic process is mainly determined by obtained in physical and chemical synthesis (Bandeira
the photocatalyst used (Nguyen et al., 2021; Hidayah et al., 2020). Polysaccharides from MRS broth media,
et al., 2022). One of the prospective metal oxides is which promote the stability of synthesis, are the
titanium dioxide (TiO2) because it is inert, harmless, medium to be used in green synthesis (Makarov et
cheap, chemical corrosion resistant, and has good al., 2014). According to Jha et al. (2009), Lactobacillus
optical characteristics (Khan et al., 2015; Fares et al., is a non-pathogenic, partially oxygen-tolerant, gram-
2022). The requirement for a good catalyst is to have a positive, prokaryotic, anaerobic-mesophilic bacterium
large surface area (Supriyanto et al., 2014) to increase with adaptability and high metabolism. It can be
the adsorption capacity so that a larger photocurrent is used to enhance the synthesis condition by assisting
produced (Sucahya et al., 2016). Therefore, the particle in the formation of nanoparticles from TiO2. The
size of a good catalyst needs to be reduced/reduced to green synthesized TiO2 photocatalyst also has other
nano size. Several studies in this field have used TiO2 potential applications besides POME treatment. For
photocatalysts doped with other metal oxides in a example, it can be used for air purification (removal of
photocatalytic system (Fadzil et al., 2013), where the air pollutants, including volatile organic compounds,

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 Global J. Environ. Sci. Manage., 10(1): 13-26, Winter 2024

nitrogen oxides, and sulfur oxides (Prasetya et al. Furthermore, the specific aims of this research are as
2021); coating self-cleaning surfaces such as glass, follows: 1) To produce TiO2 photocatalysts through a
ceramics, and metals; solar energy conversion; green synthesis process using L. bulgaricus as a bio-
environmental remediation, which is related to this reductor; 2) To obtain the performance value of the
study (degradation of organic recalcitrant in case of photocatalytic process (using the main parameter:
a water purification process). Table 1 shows some COD, biological oxygen demand (BOD5) and phenol
important research conducted related to the synthesis degradation). This study was conducted from 2021 to
of nanoparticles for photocatalysts. 2022, using samples of palm oil liquid waste from a
To date, no specific information about the successful factory located in South Kalimantan, Indonesia.
implementation of green synthesis using Lactobacillus
bulgaricus (L. bulgaricus) for palm oil mill secondary MATERIALS AND METHODS
effluent (POMSE) treatment on an industrial scale Material
has been found. This study was conducted to solve The materials used were metal oxide titanium
the following problems; 1) How to determine the oxyhydroxide: TiO(OH)2, MRS broth, MRS agar, L.
best conditions for performing green synthesis of bulgaricus culture, POME, POMSE, TiO2 photocatalyst
TiO2 photocatalysts with superior characteristics to from green synthesis, polyaluminium chloride (PAC),
degrade recalcitrant pollutants in advanced processing filter paper, distilled water and other materials for
of palm oil mill wastewater; 2) How to determine analysis. The tools used are photoreactors, hot plates
the performance of the photocatalytic process using (with stirrers), water bath, incubators and glassware
green synthesized TiO2 photocatalysts for advanced for synthesis and analysis.
treatment of POMSE. The main objective of this study
is to develop a photocatalytic process with a focus on Green synthesis of TiO2 photocatalyst
green synthesis of TiO2 photocatalysts so that the Synthesis using specific media (MRS broth
produced photocatalyst can be used for advanced containing L. bulgaricus and metal oxide TiO(OH)2) was
processing of liquid waste, as an effort to apply the performed in the following steps (work procedures
concept of recycled wastewater in palm oil mills. adjusted from the study of (Jha et al., 2009):
Table 1: Research on photocatalyst synthesis
Table 1: Research on photocatalyst synthesis
No. Results Sources
1. Nano TiO2 films have significantly better climatic resistance than blank polyethylene films. Xing et al. (2012)
TiO2 nanoparticles were added, which increased in water vapor transmission from 18.1 to
24.6 g/m2 in 24 h. Results showed that TiO2 nanoparticles incorporated into polyethilen‐
based films have a good potential application as an active food packaging solution.
2. TiO2 nanoparticles made from Planomicrobium sp., a microbial species isolated from Chelladurai et al. (2013)
melting ice, were resistant to the growth of Bacillus subtilis, Klebsiella planticola, and
Aspergillus niger bacteria. This nanoparticle synthesis used an eco‐friendly, cost‐effective
process.
3. Nanobiotechnology procedures involving biological synthesis have a tremendous potential Shah et al. (2015)
to increase the production of nanoparticles without the use of harsh, expensive, and toxic
chemicals typically used in conventional physical and chemical processes.
4. Catalytic activity during the photodegradation of dyes significantly diminished when TiO2 Amini and Ashrafi (2016)
was substituted with zinc oxide (ZnO) because ZnO is unstable and results in inconsistent
dissolution processes to form zinc hydroxide (Zn(OH)2) on the ZnO particle surfaces, leading
to catalyst deactivation.
5. Analyses of the experimental conditions, nanoparticle properties, and possible uses of Ghosh et al. (2017)
nanoparticles in pharmaceuticals and biomedical applications were presented for the
production of high‐value nanoparticles from food waste (in aquaculture and horticulture).
6. The reduction of aromatic aldehydes was facilitated using produced metal oxide Muthuvinothini and Stella
nanoparticles. Ammonium formate was used as a green hydrogen donor during the (2019)
reduction, and the corresponding alcohols were produced in excellent yields in 2–24 h.
7. Current analysis of various biological substrate sources, green synthesis processes, and Bandeira et al. (2020)
effects on the characteristics of zinc oxide nanoparticles.

15
 Green synthesis of TiO2 photocatalyst

the main culture with various dilutions was added Jha et al. (2009) that used a minimum molarity level
to MRS broth (culture: MRS broth; 25 millilitre (mL): of 0.025 M. It was then expected that the higher
75 mL) and incubated for 24 h at 27 degrees Celsius concentrations would help the synthesis process to
(oC). Then a 20 mL TiO(OH)2 solution was added produce the desired nanocatalyst characteristics. The
with the molarity according to the factor applied to synthesized photocatalyst was tested for size using a
the treatment combination. Heat the solution in a particle size analyzer (PSA) in Laboratory of Materials
water bath (temperature adjusted according to the Physics, Institut Teknologi Sepuluh Nopember,
treatment combination) for 20-25 min until a white Surabaya, Indonesia, if the size of the produced
precipitate forms at the bottom of the Erlenmeyer photocatalyst is within the nanoparticle size range,
flask. The solution was then incubated at room proceed with another characterization using scanning
temperature (25oC) for 48 h until a stable white electron microscopy-energy dispersive X-ray (SEM
precipitate formed on the Erlenmeyer flask bottom. EDX) spectroscopy at Integrated Laboratory and
The goal of the synthesis is to obtain the appropriate Technology Innovation Center, University of Lampung
size (1-100 nm) in the size range of nanoparticles and X-ray diffraction (XRD) Institut Teknologi Bandung
(Carvalho et al., 2018); thus the initial design applied Nanoscience and Nanotechnology Research Center.
was a-completely randomized (two replications)
at different temperatures of 40oC, 50oC, and 60oC Photocatalytic process
and molarity levels of 0.025, 0.035, and 0.045 M. The performance of the photocatalyst obtained
The Determination of the levels was based on the through the green synthesis process was tested by
research results of Jha et al. (2009). The molarity level applying the photocatalytic process to POMSE in a
and temperature chosen to synthesize Lactobacillus suspended photoreactor, as shown in Fig. 1. In this
sp. in this study were 0.025 M TiO(OH)2 and 50oC, study stage, the POMSE sample was first coagulated
respectively. The mesophilic Lactobacillus bacterium and filtered using filter paper to homogenize the
can thrive between 35oC and 45oC. The ideal growth solution, and then, it was tested for the COD, BOD5
temperature for L. bulgaricus is between 45oC and and phenol. The analysis was performed in South
47oC. According to previous research findings, green Kalimantan Province Health Laboratory. The factors
synthesis of TiO2 nanoparticles was conducted studied were catalyst dose and irradiation time
over a temperature range of 37oC–60oC; thus, for the photocatalytic process using a completely
the temperature was set at 40oC, 50oC, and 60oC. randomized trial design with two replications. The
Determination of the ​​molarity levels of 0.025, 0.035, photocatalytic process was performed under the
and 0.045 M considered the research results of following conditions: (a) the photocatalyst used

Mercury
lamp

suspended
sample and
photocatalyst

Fig. 1: Scheme of photoreactor

Fig. 1: Scheme of photoreactor

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 Global J. Environ. Sci. Manage., 10(1): 13-26, Winter 2024

was TiO2 resulting from green synthesis; (b) the shade is one of the early signs of the production of
photocatalyst dosages used were 1 gram (g), 1.5 g, high-quality nanoparticles (Ridhawati and Fajar,
and 2 g (Thota et al., 2014; Lestari, 2017); 2017). Based on the self-defense mechanisms of
(c) irradiation times (contact time) in the microbes, microorganisms are used in the fabrication
photocatalytic process were 1.5, 2, and 2.5 h; (d) the of nanoparticles (Ghosh et al., 2017). The biological
light source used was a 350-W Philips mercury lamp. mechanism converts reactive ions into stable atoms
because high ion concentrations are typically lethal
RESULTS AND DISCUSSION to bacterial cells. In this investigation, L. bulgaricus
Green synthesis of TiO2 photocatalyst cells were cultivated for 36 h in sterile distilled water
The research phase begins with the preparation containing carbon and nitrogen sources. A white
of the microorganism culture (L. bulgaricus) used precipitate appeared at the bottom of the Erlenmeyer
for experiments. Furthermore, the main culture of flask after 20 mL of TiO(OH)2 was heated in a water
L. bulgaricus was made on MRS broth media with bath at 500C for 20–25 min to create the metal
four times dilution. In this synthesis, atoms and oxide. This precipitate appearance is proof that TiO2
molecules mix to create precursor blocks, which nanoparticles have formed. The solution was then
are later self-assembled into nanoparticles (Ealia incubated at room temperature (25oC) for 48 h until
and Saravanakumar, 2017). This method is known a stable white precipitate formed on the Erlenmeyer
as a bottom-up technique. The primary biological flask base. Fig. 2 depicts the green synthesis process
factor affecting the synthesis of a substance is of TiO2.
the cell membrane, which is composed of lipids
and membranes. In the cell membrane, synthetic Measurement using PSA
biochemical conversion occurs following the oxidation The results of particle size analysis using the
and reduction mechanisms. Because the composition PSA showed a different pattern. From Fig. 3a, at
of the membrane is dynamic and flexible, the effect of a constant treatment temperature of 40oC but
the composition is not always constant and facilitates increasing concentrations (0.025, 0.035, and 0.045
the synthesis (Capeness et al., 2019). It is anticipated M), the size of the particles formed increases. From
that green synthesis of TiO2 nanoparticles will be able Fig. 3b, using the same concentration of 0.025 M but
to use extracellular and intracellular microorganisms at different temperatures of 40oC, 50oC, and 60oC
under suitable environmental conditions. produced better synthesis results, with the particle
Electrostatic interaction between the membranes size decreasing. At 60oC and 0.025 M the results were
of microorganisms containing negatively charged significant, with the obtained particle size within
phospholipids and the combination of metal oxides the size range of nanoparticles (33.28 nm). TiO2
used can also result in the extracellular creation of nanoparticles have high protein affinity for binding
nanoparticles (Anandgaonker et al., 2019). Eq. 1 is metals, which prevents particle aggregation. Proteins
the chemical reaction that probably occurs (Makarov and polysaccharides are produced when L. bulgaricus
et al., 2014). is used as a bio-reductor during the synthesis of
TiO2 nanoparticles, which is not the case when the
C6H12O6 → CH3 − CO – COOH (Pyruvate) ⇔ CH3 · synthesis is performed using physical or chemical
CH(OH) · COOH (Lactate)  methods. This aids in the process of synthesizing
NaHCO3 ⇔ Na+ + HCO−3 (1) metal oxide bonds so that they do not cause protein
HCO−3⇔ OH− + CO2 agglomeration. (Makarov et al., 2014). Regulation of
TiO·(OH)2 → TiO2 ↓ +H2O. the synthesis media is necessary to create an optimal
synthesis environment.
According to Malik et al. (2014), additional research Factors affecting the synthesis include pH, metal
into other metal oxides and culture variables oxide concentration, and temperature. Generally,
is necessary to produce certain nanoparticles. glucose-containing media support the growth of
However, the types of nanoparticles produced microorganisms, particularly Lactobacillus grown
also depend on the temperature used during the on MRS media. As glucose is a reducing agent, it
synthesis. The color change of the media to a lighter tends to reduce the value of the oxidation reduction

17
 L. Agustina et al.

Fig. 2: Green synthesis of TiO2 photocatalyst using L. bulgaricus

Fig. 2: Green synthesis of TiO2 photocatalyst using L. bulgaricus
Experimental unit
Experimental unit

P3 33.28

P2 1677.33
KS3 2376.00
KS2 1937.67 P1 2038.67
KS1 1749.00
-500.00 500.00 1500.00 2500.00 3500.00 -1000.00 0.00 1000.00 2000.00 3000.00
Particle size (nm) Particle size (nm)
(a) (b)
Experimental unit:
KS1 : 40o C; 0.025 M; P1 = 40o C; 0.025 M;
KS2 : 40o C; 0.035 M; P2 = 50o C; 0.025 M;
KS3 : 40o C; 0.045 M; P3 = 60o C; 0.025 M;

Fig. 3: Graph of particle measurement results a) fixed temperature with increasing concentration,
b) increasing temperature with fixed concentration
Fig. 3: Graph of particle measurement results a) fixed temperature with increasing concentration,
b) increasing temperature with fixed concentration
potential. The degree of aerobiosis is quantified by pH of the medium and the overall r-H2, both of which
the oxidation-reduction potential, which is written as are partially controlled by bicarbonate, have an impact
the oxidation reduction potential (r-H2); the negative on the synthesis conditions of TiO2 nanoparticles
logarithm of the partial pressure of hydrogen gas. The in addition to the use of glucose, an energy-

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 Global J. Environ. Sci. Manage., 10(1): 13-26, Winter 2024

cps/eV
50

40

30

Ti
Ag Zn
C O Na Ag Ti Zn
20

10

0
1 2 3 4 5 6 7 8 9 10
keV

Fig. 4: Spectrum of TiO2 based on SEM EDX analysis

Fig. 4: Spectrum of TiO2 based on SEM EDX analysis

generating substance (in the synthesis medium). product was determined at 60oC with a molarity level
The membrane-bound oxidoreductase is activated of 0.025 M which was further characterized using SEM
by the anticipated slightly acidic pH and decreased EDX. The characterization results were also used to
r-H2. The temperature also plays a significant role in determine whether the product can be synthesized
the synthesis process. The mesophilic Lactobacillus in larger quantities so that it can be used as a
bacterium can thrive between 35oC and 45oC. The photocatalyst in processing palm oil mill wastewater
ideal growth temperature for L. bulgaricus is 45oC using the photocatalytic technique. Confirmation
and 47oC. According to earlier research findings, of the content of the synthesized TiO2 elements was
green synthesis of TiO2 nanoparticles was conducted performed using SEM EDX. As shown in the spectrum
over a temperature range of 37oC–60oC (Jha et al., in Fig. 4, the amounts of the titanium (Ti) and oxygen
2009). However, the present study’s findings indicate (O) elements are 39.06% and 47.95%, respectively.
that the best green synthesis conditions occurred at Table 2 shows the overall results of the constituent
60oC. This suggests that for nanoparticle synthesis elements in the TiO2 nanocatalyst synthesis process
to occur, the temperature must be raised above the (in atomic and weight percentages). Through SEM
range for growth. The concentration of metal oxides EDX it is possible to identify the constituent elements
used during catalyst synthesis may have effects on in the synthesis in detail. In addition, to Ti and O, the
the process. Higher concentrations may lead to other elements were carbon (C), zinc (Zn), silver (Ag)
agglomeration of metal oxide particles, resulting in and sodium (Na).
decreased surface areas and reduced accessibility The peak area formed (Fig. 5) shows that the
of active sites. Conversely, lower concentrations can crystallinity of TiO2 is 67.6%, which also indicates
promote better dispersion and higher surface areas, the amount of TiO2 in the mixture is 67.6%, with the
which can enhance catalytic activity. In this study the remaining 32.4% being an amorphous component.
main factors studied were the process temperature The highest peak is in the range of 25.4 degrees
and concentration of the metal oxide used. theta, indicating anatase diffraction formed by TiO2.

Nanoparticle characterization (using SEM EDX and XRD) Photocatalyst performance

Based on the results of particle measurements Through photocatalysis, the TiO2 photocatalyst is
resulting from the green synthesis, the treatment crucial in the treatment of POMSE, which is a waste

19
 Green synthesis of TiO2 photocatalyst

Table 2:
Table 2: Elements
Elements in
in TiO
TiO2 nanocatalyst
nanocatalyst synthesis
synthesisprocess
process
2

Formula Mass (%) Atom (%)

C 0.41 0.13
O 47.95 59.98
Zn 8.62 1.98
Ag 2.63 0.37
Na 1.33 0.87
Ti 39.06 36.68
Total 100 100

Fig. 5: Peak area of TiO2 based on XRD analysis

Fig. 5: Peak area of TiO2 based on XRD analysis

product of the extraction of palm oil that contains TiO2 (hVB+) + H2O → TiO2 + H+ + OH•  (3)
significant concentrations of organic contaminants,
suspended particles, and nutrients making it TiO2 (hVB+) + OH−→ TiO2 + OH•  (4)
hazardous to the environment if released into the
environment untreated. When exposed to light TiO2 (eCB−) + O2 → TiO2 +O2•−  (5)
energy, especially in the ultraviolet spectrum, the
TiO2 photocatalyst can start and accelerate chemical O2•− + H+ → HO2•  (6)
reactions through the photocatalytic process. When
TiO2 is exposed to ultraviolet light, electron hole pairs HO2• + HO2• → H2O2 + O2  (7)
are produced, where electrons and holes develop
into highly reactive species. The TiO2 photocatalyst TiO2 (eCB−) + H2O2 → OH• + OH− 
(8)
can assist with the overall remediation process in
the context of treating POMSE in organic pollutant H2O2 +O2•− → OH• + OH− +O2  (9)
degradation. The reactive species generated by TiO2,
such as hydroxyl radicals (•OH), can oxidize and break H2O2 + hν → 2OH•  (10)
down complex organic compounds in POMSE. These
radicals react with organic pollutants, converting Organic compound + OH• → degradation products (11)
them into simpler and less harmful substances, such
as carbon dioxide and water. The general mechanism Organic compound + TiO2 (hVB+) → oxidation products (12)
is described in Eqs. 2 to 13 (Claes et al. 2019).
TiO2 + hν → TiO2 (eCB− + hVB+)  (2) Organic compound + TiO2 (eCB−) → reduction products (13)

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 Global J. Environ. Sci. Manage., 10(1): 13-26, Winter 2024

Increasing the amount of O2 in the liquid waste by research conducted by (Chang and Wu, 2010) who
affects the BOD5 and COD values, because the reported that under the same pH conditions (7-8), it
availability of sufficient O2 in the liquid waste helps the takes 960 min of degradation time, to degrade lignin
degradation process of organic components, thereby up to 88% with a TiO2 photocatalyst concentration
reducing the BOD5 and COD values ​​in the liquid waste. of 10 gram per liter (g/L) without the addition of air.
The reduction and percentage of the elimination Concerning the degradation of amino acids, some
parameters COD, BOD5 and phenol are presented researchers have stated that the degradation of
in Table 3. According to Table 3, the measurement amino acids is affected by the molecular structure of
results of the waste quality parameters after the its constituents (especially the side chains) and the
photocatalytic process was applied did not meet the interactions between the amino acid side chains and
specified quality standards. the catalyst surface which vary with pH (Tran et al.,
The percentage reductions of COD (Table 3 and 2006). Thus, not all amino acids can be degraded at
Fig. 6) ranged from 16.16% to 27.27%. This shows similar pH values.
that the ability of the TiO2 catalyst to degrade organic Research related to the application of the
pollutants ranges from 16.16% to 27.27% for 2.3 h. photocatalytic process to POMSE has been
The assumption that can be given from these results conducted, but the TiO2 photocatalyst used is a result
is that in 150 min, organic pollutants which account for of chemical synthesis. The TiO2 photocatalyst can
approximately 16-27% of the total organic pollutants degrade organic compounds (COD) and effectively
have been mineralized. Meanwhile, the rest, which are eliminate phenolic pollutants in POMSE (31.36%
complex compounds (lignin, amino acids, pectin) and COD degradation performance and up to 96.66%
some phenols remain in the depolymerization stage to phenol elimination by TiO2 loading of 1.5 g/L; air flow
form molecules with smaller molecular weights (micro- rate of 10 cc/min) at 120 min (Lestari et al. 2017).
molecules) as intermediate compounds, which require Another research by Nawaz et al. (2023) investigated
a longer total mineralization time. This is based on the effectiveness of photocatalytic remediation of
visual observations of the color of POMSE (presumably treated POME-containing phenolic compounds using
from lignin) before and after 150 min of photocatalysis, TiO2 nanomaterials. Chemical precipitation was used
which did not exhibit a significant color change. The to prepare the TiO2 nanomaterial. Under visible light
presence of sufficient dissolved oxygen in the reactor, illumination, 78.32% of 224.85 milligram per liter
which enables microorganisms to break down (mg/L) phenolic compounds were broken down in 180
polluting substances, is one environmental aspect min at the optimal TiO2 dosage (0.9 g/L). The reaction
that contributes to the high COD value (Elystia et al., of hydroxyl free radicals is non-selective, thus, some
2022). Palm liquid waste contains high protein (in the free radicals attack phenols, whereas others attack
form of amino acids); thus, it also contains high organic other organic pollutants; when almost all phenols
matter and causes pollutant concentrations to remain are mineralized, the hydroxyl radicals formed oxidize
high (Alhaji et al., 2016). This statement is reinforced other organic pollutants in POMSE. Based on this, the

Table
Table 3:
3: Measurement
Measurement results
results and
and percentage
percentage of
of elimination
elimination parameters
parameters COD,
COD, BOD and phenol
BOD55 and phenol

Measurement results (mg/L) Elimination percentage (%)

Variables
BOD5 COD phenol BOD5 COD phenol
Quality standard 50 100 0.5 ‐ ‐ ‐
POMSE 2061.50 4852.50 4.28 ‐ ‐ ‐
F1 (1 g/L TiO2; 1.5 h of irradiation) 1790.5 3940.4 3.37 13.21 18.86 21.25
F2 (1,5 g/L TiO2; 1.5 h of irradiation) 1740 3700.6 3.45 15.66 23.79 19.48
F3 (2 g/L TiO2; 1.5 h of irradiation) 1609 3529.1 1.86 22.01 27.32 56.57
F4 (1 g/L TiO2; 2 h of irradiation) 1801 3949.3 1.93 12.70 18.67 54.85
F5 (1,5 g/L TiO2; 2 h of irradiation) 1786.5 3918.1 1.83 13.40 19.31 57.20
F6 (2 g/L TiO2; 2 h of irradiation) 1833.75 3856.9 1.09 11.11 20.57 74.62
F7 (1 g/L TiO2; 2.5 h of irradiation) 1746.1 3828.65 0.81 15.36 21.16 81.12
F8 (1,5 g/L TiO2; 2.5 h of irradiation) 1814.95 3930.3 1.55 12.02 19.06 63.73
F9 (2 g/L TiO2; 2.5 h of irradiation) 1813.5 4067.8 1.65 12.09 16.23 61.54

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 L. Agustina et al.

F1 (1 g/L TiO2; 1,5 h) F4 (1 g/L TiO2; 2 h) F7 (1 g/L TiO2; 2,5 h)

F2 (1,5 g/L TiO2; 1,5 h) F5 (1,5 g/L TiO2; 2 h) F8 (1,5 g/L TiO2; 2,5 h)
F3 (2 g/L TiO2; 1,5 h) F6 (2 g/L TiO2; 2 h) F9 (2 g/L TiO2; 2,5 h)
Fig. 6: Effect of irradiation time and TiO2 photocatalyst dosage on elimination percentage of COD, BOD5 and Phenol

Fig. 6: Effect of irradiation time and TiO2 photocatalyst dosage on elimination percentage
assumption that can be given is that approximatelyof COD, environmental
70%BOD5 and Phenol benefits compared with conventional
of the pollutants not been mineralized are intermediate methods. Here are some key advantages,
compounds resulting from the degradation of lignin, ● Reduced energy consumption: green synthesis
amino acids, phenols, pectin, oils and greases, as methods typically employ milder reaction conditions,
well as macromolecules, which are constituent of such as lower temperatures and pressures, resulting in
organic pollutants in POMSE. However, COD could reduced energy requirements. This decrease in energy
only be reduced by 16.16%-27.27%. Phenol, which is a consumption contributes to lower greenhouse gas
hazardous substance, toxic, and difficult to degrade by emissions and overall environmental impact.
decomposer organisms, can be reduced significantly ● Decreased chemical waste: green synthesis
to close to environmental quality standards (0.5 part approaches typically emphasize the use of
per million). The experimental unit F7 (dose of 1 g/L; environmentally friendly solvents and reagents,
irradiation of 2.5 h) resulted in phenol elimination of up minimizing the generation of hazardous byproducts
to 81.12%, producing an effluent phenol concentration and chemical waste. This aspect reduces the risk of
of 0.81 mg/L. water and soil contamination and helps preserve
ecosystem health.
Benefits of using a green synthesis approach for TiO2 ● Lower toxicity and pollution potential: conventional
photocatalyst production synthesis methods may involve the use of toxic
Utilizing a green synthesis approach for TiO2 chemicals and hazardous reagents, which can pose
photocatalyst production can offer several risks to human health and the environment. Green

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 Global J. Environ. Sci. Manage., 10(1): 13-26, Winter 2024

synthesis techniques prioritize the use of nontoxic (in this case TiO2) functions to absorb photon energy
or low-toxicity substances, thereby minimizing the and produce holes (h+). h+ oxidizes organic molecules
potential for pollution and associated adverse effects. and reacts with hydroxide (OH-) or hydrogen dioxide
● Renewable feedstock: green synthesis approaches (H2O). Increasing the amount of oxygen (O2) in the liquid
typically utilize renewable feedstock or bio-based waste affects the BOD5 and COD values, because the
materials as starting materials, reducing reliance on availability of sufficient O2 in the liquid waste helps the
non-renewable resources. By utilizing sustainable degradation process of organic components, thereby
sources, such as biomass or agricultural waste, the reducing the BOD5 and COD values ​​in the liquid waste.
environmental impact of the synthesis process is The synthesized TiO2 photocatalyst seems to specifically
reduced, and the overall sustainability is improved. degrade phenol. Phenol experienced a significant
● Water and energy conservation: certain reduction of up to 81.12% at a photocatalyst dose of 1 g/L
green synthesis methods emphasize water-based and time irradiation of 2.5 h. Overall, adopting a green
reactions or solvent-free approaches, reducing water synthesis approach for TiO2 photocatalyst production
consumption and minimizing the need for organic offers significant environmental benefits, including
solvents. Furthermore, by optimizing the synthesis reduced energy consumption, decreased chemical
process, green approaches can reduce the overall waste, lower toxicity and pollution potential, renewable
reaction time, thereby saving energy. feedstock utilization, water and energy conservation,
● Enhanced product performance: green synthesis and improved product performance. These advantages
methods can prepare TiO2 photocatalysts with contribute to a more sustainable and environmentally
improved performance characteristics, such as higher friendly production process for TiO2 photocatalysts.
surface areas, better crystallinity, or narrower particle Notably, while there are challenges associated with
size distributions. Enhanced product performance the green synthesis of TiO2 photocatalysts using L.
can lead to more efficient photocatalytic reactions, bulgaricus, these limitations can be addressed through
reducing the amount of catalyst required and thus further research in terms of process optimization and
minimizing the overall environmental impact. technological advancements. Green synthesis methods
hold great potential for sustainable and eco-friendly
CONCLUSION production of TiO2 nanoparticles, and ongoing efforts
Green synthesis of TiO2 photocatalysts was aim to overcome these challenges to make them viable
performed using TiO(OH)2 metal oxide, yielding a TiO2 alternatives to conventional synthesis methods.
photocatalyst with a particle size of 33.28 nm at 60oC
and a 0.025 M metal oxide solution. The content of AUTHOR CONTRIBUTIONS
Ti and O constituents in the TiO2 photocatalyst was L. Agustina contributed to the process of sampling
confirmed to be 39.06% and 47.95%, respectively, and experimental research on laboratory (green
with TiO2 crystallinity of 67.6% in the range of 25.4 synthesize and photocatalytic process), manuscript
degrees theta, indicating that the results of the green preparation and revision. M. Romli sharpened the
synthesis have formed anatase diffraction. The process background, supervised the experimental research on
temperature and metal oxide concentration are the laboratory related to photocatalytic process, extended
factors influencing the formation of nanoparticles. By the discussion, and improvement recommendations.
applying a photocatalytic to POMSE using synthesized P. Suryadarma sharpened the implemented
TiO2 photocatalyst, the following results were obtained; methodology, supervised the experimental research
COD can be reduced by 16.16%-27.27%, BOD5 by on laboratory related to green synthesize, extended
11.05%-21.95%, and phenol by 19.49% up to 81.12%. the discussion, and improvement recommendations.
The concentration of dissolved carbon dioxide (CO2) S. Suprihatin, the corresponding author, supervised
in water influences the increase in the amount of the experimental research on laboratory, organized
oxygen (O2). Generally, this is because CO2 triggers the discussion, and proofread the manuscript.
an increase in the concentration of hydrogen (H) ions
which decreases the pH of water to neutral, from 8.39 ACKNOWLEDGEMENT
to a neutral pH value of 6.83-6.91. In the mechanism This study was financially supported by the Ministry
of the photocatalytic process, the photocatalyst used of Research, Technology and Higher Education of the

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 L. Agustina et al.

Republic of Indonesia through a BPPDN (Beasiswa 1.5 g/L dosage of TiO2; 1.5 hour
Pendidikan Pascasarjana Dalam Negeri, [Grant F2
irradiation time
Number: 190031088303]. 2 g/L dosage of TiO2; 1.5 hour
F3
irradiation time
CONFLICT OF INTEREST 1 g/L dosage of TiO2; 2 hour irradiation
The authors declare that there is no conflict of F4
time
interests regarding the publication of this manuscript. 1.5 g/L dosage of TiO2; 2 hour
In addition, the ethical issues, including plagiarism, F5
irradiation time
informed consent, misconduct, data fabrication and/ 2 g/L dosage of TiO2; 2 hour
or falsification, double publication and/or submission, F6
irradiation time
and redundancy, have been completely observed by 1 g/L dosage of TiO2; 2.5 hour
the authors. F7
irradiation time
1.5 g/L dosage of TiO2; 2.5 hour
OPEN ACCESS F8
irradiation time
©2024 The author(s). This article is licensed under 2 g/L dosage of TiO2; 2.5 hour
a Creative Commons Attribution 4.0 International F9
irradiation time
License, which permits use, sharing, adaptation, g Gram
distribution and reproduction in any medium or g/L Gram per liter
format, as long as you give appropriate credit to the H Hydrogen
original author(s) and the source, provide a link to the
h+ Holes
Creative Commons license, and indicate if changes
were made. The images or other third-party material H2O Hydrogen dioxide
in this article are included in the article’s Creative ITB Institut Teknologi Bandung
Commons license, unless indicated otherwise in a KS1 40o C; 0.025 M
credit line to the material. If material is not included KS2 40o C; 0.035 M
in the article’s Creative Commons license and your KS3 40o C; 0.045 M
intended use is not permitted by statutory regulation L Liter
or exceeds the permitted use, you will need to obtain L.
permission directly from the copyright holder. To view Lactobacillus bulgaricus
bulgaricus
a copy of this license, visit: http://creativecommons. M Molarity
org/licenses/by/4.0/. mg Milligram

PUBLISHER’S NOTE mL Milliliter

GJESM Publisher remains neutral with regard to MRS de Man Rogosa and Sharpe
jurisdictional claims in published maps and institutional Na Natrium
afflictions.
nm Nanometer
ABBREVIATIONS O Oxygen
% Per cent O2 Oxygen
Ag Argentum OH- Hydroxide
BOD5 Biochemical oxygen demand
o
C Celcius degrees
C Carbon P1 40o C; 0.025 M
CO2 Carbon dioxide P2 50o C; 0.025 M
COD Chemical oxygen demand P3 60o C; 0.025 M
CPO Crude palm oil PAC Poly aluminium chloride
Eq. Equation pH Potential hydrogen
1 g/L dosage of TiO2; 1.5 hour POME Palm oil mill effluent
F1 POMSE Palm oil mill secondary effluent
irradiation time

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photocatalytic reactors. Chem. Eng. J., 361: 725-735 (10 pages).

ppm Part per million
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AUTHOR (S) BIOSKETCHES

Agustina, L., Ph.D. Candidate, Agroindustrial Engineering Study Program of Graduate School, IPB University, PO Box 220, Bogor, West
Java, Indonesia.
▪ Email: [email protected]
▪ ORCID: 0000-0001-6780-0158
▪ Web of Science Researcher ID: GOG-9829-2022
▪ Scopus Author ID: 57210411885
▪ Homepage: http://tip.ulm.ac.id/id/dosen/
Romli, M., Ph.D., Professor, Department of Agroindustrial Technology, Faculty of Agricultural Engineering and Technology, IPB Univer-
sity, PO Box 220, Bogor, West Java, Indonesia.
▪ Email: [email protected]
▪ ORCID: 0000-0002-1533-325X
▪ Web of Science ResearcherID: GPW-9612-2022
▪ Scopus Author ID: 55574122275
▪ Homepage: https://tin.ipb.ac.id/
Suryadarma, P., Ph.D., Associate Professor, Department of Agroindustrial Technology, Faculty of Agricultural Engineering and Technol-
ogy, IPB University, PO Box 220, Bogor, West Java, Indonesia.
▪ Email: [email protected]
▪ ORCID: 0000-0002-1655-3035
▪ Web of Science ResearcherID: AAW-3282-2021
▪ Scopus Author ID: 54879446100
▪ Homepage: https://tin.ipb.ac.id/
Suprihatin, S., Ph.D., Professor, Department of Agroindustrial Technology, Faculty of Agricultural Engineering and Technology, IPB
University, PO Box 220, Bogor, West Java, Indonesia.
▪ Email: [email protected]
▪ ORCID: 0000-0001-9641-8820
▪ Web of Science Researcher ID: GNH-5658-2022
▪ Scopus Author ID: 56085767200
▪ Homepage: https://tin.ipb.ac.id/

HOW TO CITE THIS ARTICLE

Agustina, L.; Romli, M.; Suryadarma, P.; Suprihatin, S., (2024). Green synthesis of titanium dioxide
photocatalyst using Lactobacillus bulgaricus for processing palm oil mill effluent. Global J. Environ. Sci.
Manage., 10(1): 13-26.
DOI: 10.22034/gjesm.2024.01.02
URL: https://www.gjesm.net/article_706081.html

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