Synthesis of Iron (II, III) Oxide Nanoparticles (IONs) -

derived (Fe3O4) Ferrofluid with “Lato” (Caulerpa

Lentillifera) for Microplastic Reduction in Water
Zaira Pamela L. Arida, Carl Joshua P. Portugal, Wilfredo A. Rivera III, Erin Jaycee D. Salazar, Jeric
Ronnel P. Ylagan

Researchers, Batangas State University - The National Engineering University - Alangilan

[email protected], [email protected], [email protected],
[email protected], [email protected]

Abstract: Water is a very abundant resource on the planet, as such, it is faced with the challenge of being clean. Due to its
abundance, it is apparent that most living organisms depend on the nutrients, and value it provides. Water is in an endless
circulation around the world, meaning it brings about different things essential to an organism’s survival, but it also
encounters materials which are either neutrally or negatively affecting its significant purpose – which is to provide for lives.
One of the most found materials which are dispersed within different bodies of water are plastics. Plastics are materials which
degrade slowly, which then turns to micro plastic particles, and have qualities which can adsorb other contaminants like
heavy metals and other organic pollutants. As plastic-based materials are integrated with the flow of the water, the organisms
that wander through it may be affected followed by its consumers. With this, the proponents of this study synthesized Iron
(II, III) Oxide Nanoparticles using+- Lato (C. lentillifera) forming a ferromagnetic fluid to extract microplastic in water. The
characteristics of the magnetite presented through SEM, FTIR Transmittance, and UV-Vis Absorbance results prove its
magnetic properties. Moreover, the behavior of the nanoparticles in fluids were tested thru checking their oxidation,
suspension, and rate of magnetism. Furthermore, the ferrofluid treatment of microplastics shows that as the volume of the
ferrofluid increase the percent microplastic removal also increases. Thus, yielding successful treatment results with the use
of the synthesized iron oxide nanoparticle-derived ferrofluid.

Keywords: Water Bodies, Microplastics, IONs, Lato, Microplastic Reduction, Ferrofluid.

1. Introduction according to National Geographic, the amount of plastic in

the Atlantic Ocean alone has tripled since the last record
Water is the most abundant natural resource on Earth as
during the 1960s [3]. A garbage patch covering almost
it makes up approximately 71% of this blue planet. Under
620,000 square miles is floating in the Pacific Ocean, and the
this percentage lies different bodies of water such as ground
major contributor to such is plastics of single use [5].
water, seawater, lakes, and rivers [1]. As water travels
through these different bodies of water, it carries nutrients According to the International Journal of Environmental
that are broken down through the water cycle and the Research and Public Health, humans have aided an
circulations through these channels. Water in circulation is exponential development in global plastic manufacturing
also abundant with the concentration of different pollutants over the last 70 years, which has seeped into the environment
from organic, natural, and artificial pollutants that directly [6]. These synthetic polymers are environmental
affect the living organisms on and under it and those who contaminants in and of themselves, acting as carriers of
feed off it, including humans [2]. In addition, these pollutants various chemicals. However, they are also considered as
likely float off from a far distance in these watery habitats or valid markers of the recent and present periods, mainly after
sink to the depths of these bodies of water. They are then the mid-20th century [6]. Microplastics may provide dangers
consumed by the organisms and introduced to the global in three forms: physical particles, chemicals, and
food chain [3]. microbiological diseases found in biofilms. Particles can
have a variety of physicochemical qualities, including size,
One of the most rampant materials found in waterway
surface area, and shape, which can result in effects on the
systems and other bodies of water are plastics. They vary in
body. While most plastic polymers are non-toxic, plastics
properties, structure, and characteristics, but the effect is
and microplastics may include loose monomers and
virtually identical to all living things. Plastics of different
additives.
sizes have become the most dominant marine litter, and an
estimated 5.25 trillion plastic particles weighing above In this study, the researchers were inspired to remove
268,000 tons are discarded into oceans [4]. Moreover, microplastics from a simulated solution using magnetic
nanoparticles with ferrofluid. Microplastic in water bodies For the preparation of ferrofluids, coconut oil and iron
may pose environmental and health issues. These, in general, oxide NPs were utilized, along with magnets for testing.
cause disarray in the quality of life within the ecosystem - Characterization of ferrofluid was also conducted.
and its nutritional, and life value - those benefits from these Equipment such as scanning electron microscope (SEM) and
affected water bodies. As specifically stated by Alfaro- centrifuge was used. Coconut Oil was bought in local
Nunez et. al., 2021, that there are approximately 5.25 trillion convenience stores, the centrifuge, Electron Microscope, and
plastic particles dominating the marine litter, this in turn UV-VIS was provided in the laboratory.
needs urgent attention, and resolution [4]. For its effectiveness or adsorption experiments, the
ferrofluid was used in water samples. Microplastic solutions
To make this happen, Iron (II, III) Oxide Nanoparticles
were prepared from PET. The plastic materials were obtained
are synthesized from Caulerpa Lentillifera extract. They are
from common household materials and were cut 5 x 5 mm.
formed into ferrofluid so that the magnetite is suspended in
the oil used for the ferrofluid production, which will control
the dispersion of the Iron Oxide to the environment. This will 2.2. Methodology
likely reduce the amount of microplastic pollutants present 2.2.1. Preparation of “lato” (C. lentillifera) Extract
in the water solution subject to the study. As the experiment The seaweeds were collected and bought from public
will be done in a laboratory simulation, the proponents hope markets of Lipa and Batangas City, wherein they are sold
to apply the success of the results in contaminated waterways mostly and were stored in a cooler with a block of ice during
which may increase the lifetime value of these water bodies. transportation, and immediately transferred to a freezer. The
As for the raw material to be used, lato or Caulerpa collected seaweed samples were then washed with seawater
Lentillifera is a highly abundant seaweed in the Philippines. to remove the epiphytic and extraneous matters. After that,
Thus, the procurement of the main component of the they were washed with distilled water to free the seaweeds
magnetic extractor, namely Iron and this Lato as a reducing from potential contaminants. Then, rinse the seaweeds and
agent, was easy. The acquisition and utilization of this freeze dry them. Ground the dried seaweeds into powder or
resource are also sustainable as it grows in Coron and the introduce them to a food processor to produce a more
Northern parts of Palawan. Iron, a widely known delicate powder.
ferromagnetic element, is highly reactive due to its large And then, in a reflux setup, using a condenser and two
surface area. Thus, lessening the presence of various neck flask, put 10 grams of the Lato powder, and 100 mL of
microplastics within the waters inhabited by living Distilled water and heated to boil in a magnetic stirrer at
organisms and are used by human beings. 80 °C at a 700 rpm rate. Start the timer for 1 hour if the
temperature reaches 80 °C. Utilize the cheese cloth to
initially squeeze out the extract to speed. Press it until there
2. Materials and Methodology is no extract. The samples were then filtered using the
conventional qualitative filter which is 150 mm. Finally, this
2.1. Materials extract was then subjected to Total Phenolics Concentration
In this study, iron oxide nanoparticles (IONs) were Analysis (TPCA) using UV-VIS equipment.
synthesized via green route from Lato (C. lentillifera) or
seaweeds. The materials used in this process are seaweed, 2.2.2. Preparation of Simulated Wastewater with
deionized and distilled water, food processor or mortar and Microplastics
pestle, Fe3+ and Fe2+ solutions, stirring plate, N52-grade Microplastics are prepared by grinding PET bottles. A
neodymium magnet, ammonium hydroxide and (anhydrous) coarse sandpaper (grit 60-80) and fine sandpaper (grit 1500)
ethanol. Furthermore, solutions of ammonia utilized for pH were used to mill the PET bottles. To make microplastic
adjustment along with pH meter and centrifuge were then solution, the powder residue of the PET is collected in a
used to allow settling. separate beaker and is distributed in DI water. The
The seaweeds were gathered/bought from Lipa City and proponents prepared 0.025 grams of 8 μm microplastics
Batangas City public markets. Deionized water was bought mixed to 500 mL distilled water that was further blended
in DKL Laboratory Supply and Belman while Distilled using a home-use blender equipment until it was dissolved
Water was acquired in nearby convenience stores. Items like well. For the treatment process, prepare 50 mL of this
the Food Processor/Mortar and Pestle were ordered in the microplastic solution readily available when the magnetite is
online shop (Shopee). synthesized.
Depending on what would be used, Fe3+ / Fe2+
solutions were bought in DKL Laboratory Supply or in 2.2.3. Synthesis of Iron (II, III) Oxide Nanoparticle-
Belman. The Magnetic Stir Bar, pH meter, Sonicator, and Derived (Fe3O4)
Centrifuge is provided by the ChEFE laboratory. N52-grade
Through co-precipitation, the prepared 27.201 g of
neodymium magnet was be ordered in Shopee. Ethanol, and
Ammonia, was provided by the ChEFE Laboratory or Ferrous Sulfate (FeSO4) and 54.06 g of Ferric Chloride
purchased in DKL Laboratory Supply or Belman. Lastly, (FeCl3) were dissolved in 1000 mL distilled water stirred for
Agitator (Digital) was provided by the laboratory as well.
10 to 15 minutes with constant rpm of about 700 rpm in determined as follows:
magnetic stirrer. When settled, prepare 100 mL FeSO4 and • The ferrofluid is submerged in clear water from a
specific distance from the magnet.
100 mL FeCl3 of each of this iron solution and then mix in a
• The magnet is attached to the far-right area of the
1000 mL beaker that were put in the nitrogen environment container.
setup inside a glass casing agitated for 500 rpm. All the • The speed with which the ferrofluid reaches the
possible holes should be patched up to avoid the N2 gas from magnet is recorded.
escaping. The induction was set at a temperature of 90- 2.2.6. Design of Experiment
100 °C and when it reaches this desired condition, the timer To prepare the experiment’s design variation
started for 45 mins. This is followed by the addition of 0.8 M procedure, the researchers determined the effect of ferrofluid
Ammonium hydroxide to the solution. This reaction was on the degradation of microplastics. The first step for this
done within 30 minutes under constant stirring and bubbling phase is to prepare a microplastic solution by adding 0.025 g
of Nitrogen Gas. of microplastic to 50 mL of hot water, which is then reheated
Continue stirring the solution for one hour (or longer if for 10 minutes. Next, 3 drops of base or 1 drop of acid is
needed) until the pH level of 11 was obtained to homogenize added to the solution based on the indication from the DOE
the solution and complete the reaction. Afterwards, add 50 table, with the solution remaining unchanged if it is neutral.
mL Lato extract stabilizer in the solution and wait for 40 The acid/base solution is then remixed to evenly distribute
minutes after all the extract was subjected to the magnetite. the solution. The next step is to add the required amount of
Cool the extract for a minimum of 2 hours and after ageing, Ferrofluid, with either 1, 3 or 5 drops of FF equivalent to
wash it until it reaches neutral condition. After the solution 0.021 g or 21 mg. After the solution has been prepared, it is
has settled, separate the magnetite via N-52 Grade placed on the water bath shaker, with the rpm adjusted to
Neodymium magnet, then wash it with deionized water, then 140. The solution is then timed for the required number of
with ethanol. They were then subjected to 15 minutes of minutes (2, 4 or 6 minutes), after which the turbidity is
sonification. checked and recorded. The experiment is then repeated with
the variation of the amount of Ferrofluid, with the turbidity
2.2.4. Characterization of Magnetite values recorded for each condition. Finally, the paper
The magnetite obtained were washed with distilled
concludes with a discussion of the results and its significance
water while separating them again using a magnet. Prepare
in the study of microplastic degradation, along with any
three different magnets for a three-part division of the
limitations and future research directions.
magnetite through isopropanol washing. Then dry them with
the container upside down and the magnet with it. With this, 2.2.7. Isotherm
the powdered Fe3O4 Magnetite is obtained, allowing the Isotherm relates microplastic concentration with the
proponents to characterize the magnetite. adsorption potential of Ferrofluid. Ten samples (labeled I1-
I9) of 50 mL distilled water doped with microplastic at
2.2.5. Preparation and Characterization of the Ferrofluid
varying amounts in mg at 300, 500, 700, 1000, 1500, 2000,
Prepare a ratio of 1:5 Fe3O4 NPs and coconut oil. Mix
2500, 3000, and 3500 ppm were prepared. Each regulated to
them thoroughly until the Fe3O4 NPs are suspended in the
assume neutral pH levels and dosed with 105 mg of
solution. Utilize the magnets to test and characterize the
Ferrofluid before subjecting to a constant 6-minute water
ferrofluid in terms of time and behavior. A Viscometer was
bath shaker. Turbidity is then measured through a
used to determine the viscosity of the ferrofluid. To
turbidimeter.
determine the turbidity of the ferrofluid, it was centrifuged at
2000 rpm for varying times, up to five minutes, and then
2.2.8. Kinetics
submitted to the digital turbidity meter. Scanning Electron
Evaluation of kinetics requires preparation of ten
Microscope (SEM) was used to determine the particle size of
samples of 50 mL distilled water doped with 25 mg of
the magnetite after it has been combined with the oil to
microplastic which results in a 500-ppm solution. Each
generate the ferrofluid. Finally, the rate of magnetism is
sample (labeled K1-K10) is subjected to 21 mg of magnetite is a Transmittance Electron Microscope or TEM.
synthesized Ferrofluid before fixing in a water bath shaker at
2.3.3. Characterization of the Ferrofluid
varying extents of time at a range of 1 to 10 minutes in
For the characterization of the ferrofluid produced in
intervals of 1. Turbidity is then measured through a
the experiment, the following characteristics are taken into
turbidimeter. Adsorption capacity is evaluated against time.
account - viscosity, turbidity, particle size, and rate of
magnetism.
2.2.9. Reusability
Reusability tests the limits at which Ferrofluid Viscosity is initially identified by using a viscometer in
adsorption remains within acceptable parameters of the ferrofluid. As for the turbidity of the ferrofluid, it was
microplastic removal. Two samples (labeled PA and PB) and agitated at 2000 rpm rotating under different periods of time,
a third, serving as a control (PC), were prepared. five minutes being the maximum, and is then subjected to the
Concentration is set constant at 500 ppm, dosage at 105 mg turbidity meter. For the particle size, SEM was used to
of Ferrofluid, water bath shaker at 6 minutes, and at neutral determine the particle size after the magnetite has been
pH levels. Samples PA and PB ran five cycles of testing, mixed with the oil which formed the ferrofluid.
percent removal per cycle is measured in a turbidimeter. And finally, the rate of magnetism is tested as follows;
the ferrofluid was submerged in a clear water container from
2.3. Analytical Testing a specific distance away from the magnet, the magnet
2.3.1 Synthesis of Iron Nanoparticles
attached at the far-right area of the container, and the speed
Prepare the sea grape (C. lentillifera), initially it must
at which the ferrofluid has reached the magnet was recorded
be washed, then rinsed and freeze dried using the freeze
as the rate of magnetism. The reusability of the magnetite
dryer equipment. After it has been dried it should be
was also tested by repetitively subjecting it into the simulated
grounded into powder then further processed in a food
wastewater by five (5) times, and each submersion to the
processor for a finer powder. Next, in a reflux setup, using a
solution it was viewed under the microscope.
condenser and two neck flask, put 10 grams of the Lato
powder, and 100 mL of Distilled water and heat to boil in a
magnetic stirrer at 80 C at a 700 rpm rate. 3. Results and Discussion
The samples were then filtered using the conventional 3.1. Total Phenolic Content of Different Extraction
qualitative filter which is 150 mm wherein the extract that Methods
were collected further used for synthesizing the magnetite. A
ratio of 100:100 mL 1 Fe3+ and Fe2+ solutions were added
together. Gradually stir the solution with 500 rpm while 0.8
M of NH4OH are being added per drop to reach the pH level
of 11. To homogenize the solution, stir for 30 minutes or
longer if needed. Let the solution settle completely and cool
at room temperature. Afterwards, add 50 mL Lato extract
stabilizer in the solution and wait for 40 minutes after all the
extract was subjected to the magnetite. The magnetite was
Figure 1. Total Phenolic Content of Different Extraction Methods
visible by this time, and it was separated with the use of N52-
grade neodymium magnet, and washed simultaneously with The above figure shows the trend analysis of the
distilled water, and repeated. presented TPC values for each extraction process. The
outcomes of this experiment also revealed that reflux extract,
2.3.2. Characterization of Iron Nanoparticles
which was preceded by boiling and MAE extraction, had the
In characterizing the Iron Nanoparticles to be extracted,
highest phenolic contents. A comparable trend was
Scanning Electron Microscope SEM is necessary. Another
evidenced in all antioxidant assays as that of TPC, revealing
equipment that provided further characterization of the
phenolics to be the significant component in the antioxidant
capability of the Lato seaweed. In summary, it can be made 3 acquired 1.5 cm/s and 1 cm/s, respectively.
Figure 4. Relationship Between UV-Visible Absorption Fe3O4
a point of saying that factors like the extraction technique
and C. lentillifera Extract
influence the yield of phenolic compounds.
The UV - Visible Absorption was used to characterize
3.2. Total Phenolic Content of Different C. Lentillifera the structure of the synthesized Fe3O4 using NH3 as its base,
Powder Weight through Reflux Extraction and Lato (C. lentillifera) as its stabilizer. Figure 4.4 presents
the absorption peaks of the synthesized Fe3O4 nanoparticles
within the range of the average absorption region. The
Fe3O4 - Extract 1 shows that within 300 to 500 nm the
average highest peak was recorded at 347 nm with 2.42; and
average lowest peak is at 800 nm with 2.163. All Fe3O4 -
Extract Samples show that the same highest and lowest
average peaks were observed at the same area.

Figure 2. Total Phenolic Content (ppm) of Different C. lentillifera

powder weight through Reflux Extraction

The figure above shows the trend analysis of the total

phenolic content extracted using different lato powder
weight through reflux extraction. The bar graph clearly
indicates a significant difference between three trial ratios of Figure 5. FTIR Spectra Result of Fe3O4 Nanoparticles
lato to water. It can be concluded that, greater amount of lato
powder have the highest value of total phenolic content. According to a Merck KGaA (2022) IR Spectrum Table
& Chart, the bond assignment for the FTIR result of the
magnetite has been observed and read [8]. Another study
published last 2014 by F. Hosseini entitled Fe3O4
nanoparticles modified with APTES as the carrier for (+) -
(S)-2-(6-methoxynaphthalen-2-yl) propanoic acid
(Naproxen) and (RS) 2-(3-benzoylphenyl)-propionic acid
(Ketoprofen) drug helped interpret the data [9]. The Fe3O4
value of 3432.11 and 2927.56 was observed to be assigned
as (O-H) stretching bond, 1724.41 value for (C-H) bending,
1627.43 value assigned as (C=C) stretching, 1384.64 for
Figure 3. Rate of Magnetism of 1g of Magnetite from different bond assignment (C-H) bending and lastly (Fe-O) bond for
Volume Lato Extracted Magnetite 577.64. This means that the FTIR spectra of the Fe3O4
nanoparticles particularly showed the bonds in the magnetite
Figure 3 shows how weak or strong the attraction of along with their corresponding values.
one gram of magnetite from a different volume of lato
extracted magnetite. It can be seen that under three trials, trial
1 with 25 mL of lato extract obtained the strongest magnetic
attraction having a 3 cm/s magnetic rate. Hence, trials 2 and

Figure 6. Morphology of Fe3O4, Iron Oxide Nanoparticles

 The Figure above (a), (b), (c), (d), and (e) each shows ongoing research exploring their potential uses and
morphological condition of the iron oxide nanoparticle or optimizing their properties.
magnetite at 2 𝜇m, 3 𝜇m, 5 𝜇m, 10 𝜇m and 50 𝜇m
respectively. With the use of SE and HV detector 10 kV it
can be seen that the condition regarding the morphology
appeared slightly agglomerated forming tiny particles with
scours. It is also observed that most of them are cubic in
nature and have an irregular shape. The data above shows the
formation of a cubic shape of ferrous nanoparticles.

Figure 7. General Map Sum Spectrum, Iron Oxide Nanoparticle

Figure 9 : (a) XRD diffraction pattern of Magnetite with
Shown in the above figure is the general map sum Caulerpa Lentillifera (b) XRD diffraction pattern of
spectrum for the sample which provides information about Magnetite from Du et al. (2020)
the chemical composition and molecular structure of iron
oxide nanoparticles. In this technique, the spectrum is The figure above shows near proximity relation signifies
obtained by adding together the individual spectra of all a favorable synthesis as obtained data matches with literature
points with the respective peaks of the high ratio of elemental from [10] and referenced values for pure magnetite from
components in a given map. [11]. Minute differences in peak intensities and overall
distribution of data in XRD pattern of (a) and (b) is
speculated to be due to the presence of an amorphous organic
compound which in this case is the bio-stabilizer caulerpa
lentillifera.

Figure 8. (a) Scanning Electron Microscopy (SEM) image

of iron oxide nanoparticles, (b) Iron (Fe) element, (c) Oxygen (O)
element, (d) Chlorine (Cl) element, (e) Carbon (C) element, (f)
Sulfur (S) element

The elemental composition and morphology of iron oxide

nanoparticles (NPs) were studied using scanning electron Figure 4.12. Box-Cox Plot for Power Transforms
microscopy (SEM). The NPs were found to be composed of
iron (Fe) and oxygen (O), with a size of 25 micrometers and This figure shows the range of power transformations on
irregularly shaped particles due to reactant concentration. the x-axis and the corresponding transformed response
The SEM analysis showed strong dispersion, enhancing the variable on the y-axis. The plot also shows a confidence
nanoparticles' characteristics. Iron oxide nanoparticles have interval for the optimal transformation which is 3.78694. The
unique magnetic, optical, and electronic properties due to highest point in this plot (the green line) corresponds to the
their small size and high surface area-to-volume ratio, optimal power transformation which maximizes the
making them potential for a wide range of applications, with normality and constant variance of the residuals. We can see
that it is close to zero which signifies that the log
transformation is appropriate. This is based on the 2018 Box-
Cox plot reading of reactive red degradation through a dye-
tolerant marine Acinetobacter baumannii-mediated process
[12] which mentioned that the lambda is the most appropriate
power transformation to apply the response data and the RSS
is the minimum residual sum of squares. Hence, this box-cox
plot is an essential diagnostic tool that was utilized in this
study in conjunction with other diagnostic plots and
statistical tests to assess the adequacy of the statistical model
in this DOE.

Figure 4.29. Average Reusability Graph of the

Ferrofluid and Its Percent Microplastic Removal

The data above represents the average of P1A and P1B as

seen in Table 4.13 and are now labeled as Cycles. In each
cycle, the average percent microplastic removal of P1A and
P1B is also represented. As the data suggests, the more
cycles there are, the less effective the ferrofluid is in
removing microplastic from water. The data was also
stopped in cycle 5 since it already shows a downward trend,
therefore the proponents conclude that it will continue to
decrease as the cycles increase. The F-critical value is also
provided in the table, which is the value that the F-statistic
Figure 4.25. Freundlich Isotherm Model must exceed in order to decline the null hypothesis. In this
case, the F-critical value is 5.3177.
This shows that the Freundlich Model is suitable in
describing the adsorption mechanism of microplastics onto Table 4.13. Summary of Coded and Actual Factors
the ferrofluid. This is in agreement with the study [13] which affecting the MP Removal
fitted Freundlich isotherm model in the adsorption of three
pesticides on polyethylene microplastics. Additionally, this
is further supported [14], wherein their experiment was well
suited under the adsorption isotherm model of Freundlich
Model.

The table also shows the relationships between the

different factors. The data in the table indicates that the
negative value of A or the pH of the solution, once increased,
affects the microplastic removal. Moreover, the ferrofluid
dose and the concat time which shows positive figures
indicates that they propose a positive effect on the MP
removal, suggesting that an increase in the dosage, and that
the increase in time, directly affects the removal as it also
increases. The A-C relationship has significantly affected the
Figure 4.28. Pseudo-Second Order Model removal of Microplastics in the wastewaters, and that the
correlation of the three factors have positively affected the
These findings demonstrate the suitability of using removal of microplastics. This is supported by the obtained
pseudo-second order to investigate the adsorption process of results from Hamzah., S. et. al, (2021), which showed that
MP removal in wastewater. This result can be compared with the removal efficiency was the lowest (99.11%) when using
[15]. which is based on the microscopic investigation on the 0.25 g/L of iron oxide and increasing the iron oxide dosage
adsorption of lubrication oil on microplastics. improved the efficiency up to 99.72%.
Table 4.14. Conditions for Removal, with its Predicted
 and Actual Mean, and %Error Table 53 Analysis of Variance

The table provides information on the prediction of mean

and median responses for a variable called "MP Removal".
The predicted mean value for MP Removal is 99.6575,
which means that, on average, the response variable is
expected to be around this value. The predicted median value
for MP Removal is also 99.6575, indicating that the median
response variable is also expected to be around this Based on the table, A-pH, B-FF Dose, C-Time, and their
value.The predicted mean value for some variable (which is interactions are all significant predictors of the response
not explicitly stated) under these conditions was calculated variable (p < 0.0001). The interaction term AB is not
to be 99.6575+1.05409. The actual data mean value (again, significant (p = 0.3392), whereas the interaction terms AC
for the same variable) was 99.4. The percent error between and BC are significant (p = 0.0013 and p < 0.0001,
the predicted and actual values was calculated to be respectively). The Lack of Fit test suggests that the model is
0.25915493, which means that the predicted value was off not a good fit for the data (p = 0.0522), but this is not
by about a quarter of a percent. statistically significant, meaning that there is no strong
evidence to reject the model. Overall, the ANOVA table
provides important information on the significance of each
4. Statistical Treatment of Data predictor variable and interaction and can help in identifying
the most important factors that affect the response variable.
Table 1. Fit Summary of the Design of Experiment

5. Summary
From the interpretation and analysis of results obtained
in the study, the following were drawn:

Table 4 presents that the Quadratic model has the 1. Extraction Method. The focal point of this research
highest Adjusted R² and Predicted R² values, indicating that derives from the formulation of a ferrofluid through
it provides the best fit to the data among the models tested. reacting Fe (II) and Fe (III) salts, producing
The Sequential p-value and Lack of Fit p-value for all models ferromagnetic nanoparticles. This study aims to
are less than 0.0001, indicating that all models are utilize the properties of non-polar substances to aid
significant. The Cubic model has a higher Adjusted R² value in a microfiltration process by extraction using the
than the Quadratic model, but it is considered aliased, ferrofluids magnetism to guide the material through
indicating that some of the model terms are linearly the solution. Through optimization, relative to three
dependent on each other. lato extraction methods, reflux proved to be the best
Table 2. Fit Statistics, Signal to Noise Ratio in terms of total phenolic content averaging at
50.89.

2. Total Phenolic Content.. Resulting lato-water ratio

at average TPC of 52.66, settled at 10g:100 mL. The
ferromagnetic iron oxide particles stabilized
relative to the amount of lato extract introduced
which was at 50 mL and 75 mL as lower
The Predicted R² of 0.9813 is in reasonable agreement concentrations proved to be undesirable. Final
with the Adjusted R² of 0.9852; i.e. the difference is less than concentration with respect to suspension in carrier
0.2. fluid, results suggest 50 mL lato extract.
Adeq Precision measures the signal to noise ratio. A ratio
greater than 4 is desirable. As the table presents the ratio of 3. Characterization of Magnetite. For UV-VIs, within
64.143, this indicates an adequate signal. This model can be 300 to 500 nm wavelengths of Lato-synthesized
used to navigate the design space. Magnetite, data peaks high at 347 nm with 2.42.
Lowest peak observed at 800 nm with 2.16. Data is
supported by previous research. (O-H) stretching
 bond is assigned by a Fe3O4 value of 3432.11 and sample affected the removal rate.
2927.56, (C-H) bending at 1724.41, as (C=C)
stretching at 1627.43, (C-H) bending at 1384.64, 5. Kinetics and Isotherm. Full saturation of 25 mg
and finally (Fe-O) bond for 577.64. The findings ferrofluid in 50 mL water to 500 ppm microplastic
discuss the use of SEM-EDS to provide information observed at 6 minutes of treatment. Turbidity of k6
on the composition, purity, and morphology. By sample at 6 NTU, percent of microplastic removed
analyzing the elemental spectra, researchers at its highest of 97.60%, adsorption in mg/g peaked
identify the different chemical species present on at 244. Further increase in minutes past 6 led to a
the nanoparticle surface and their relative decrease in percent efficacy. The results are
abundance. By utilizing a SE and HV detector at 10 presented in a graph, showing that the removal rate
kV, it is apparent that the morphology of the iron varies between 75% and 99% depending on the
oxide nanoparticles or magnetite is slightly experimental parameters. Moreover, for the
agglomerated, resulting in the formation of small isotherm test, the trend shows that the further
particles with scours. The majority of these increase in the concentration of the microplastic in
particles exhibit a cubic nature, although their shape the simulated wastewater decreases the % MP
is also irregular. The data supports the formation of Removal. Furthermore, Freundlich has the highest
ferrous nanoparticles with a cubic shape. FT-IR value of 0.9737. However, the Langmuir model had
results showed bonds in the magnetite. Iron, the lowest RMSE value (54.11) among the two
moreover, is the most abundant element in the models. This shows that the Freundlich Model is
samples having 70.16% in all spectrum regions, suitable in describing the adsorption mechanism of
with oxygen, carbon, manganese, and chromium microplastics onto the ferrofluid. And the kinetics
also present in smaller quantities. It notes the order tests demonstrated the suitability of using
presence of minor peaks for other elements, which pseudo-second order to investigate the adsorption
may be impurities in the precursor iron oxide process of MP removal in wastewater.
material. Analysis of XRD data result in four
compound matches within the sample: Magnetite 6. Reusability. The data for reusability indicates that
[Fe2+Fe3+2O4], Zincochromite [Zn2+Fe3+2O], as the ferrofluid is used repeatedly, its effectiveness
Franklinite [Zn2+Fe3+2O], and Magnesioferrite in removing microplastics decreases. The results
[MgFe3+2O] with a nearness rating of 89, 90, 91, suggest that as the number of cycles increases, the
and 91 respectively. Peak geometry and distribution ferrofluid becomes less effective in removing
of data suggests a crystalline structure, based on microplastics from water. The data was stopped at
calculated lattice constants; the sample is cycle 5 since it already displays a downward trend,
speculated to adapt a cubic lattice system. XRD indicating that it will continue to decrease as the
data regarding magnetite’s lattice constant has a cycles increase.
99.67% similarity to literature. Presence of Zn, Cr,
and Mg metals are suspected to be originating from
lato as the elemental composition thereof contains 6. Conclusions
aforementioned metals in mg/kg concentrations of
After each procedure from synthesis of Iron Oxide
15.2 ± 0.3, 3.3 ± 0.5, and 10,663 ± 52 respectively.
Nanoparticles and the production of ferrofluid to treatment
Through the modified Scherrer equation, a
of microplastic in simulated solution, the following
computed average crystallite size of 11.98 nm was
conclusions were drawn:
obtained. 1. The effects of the varying metal to extract ratio to
the Fe3O4 and its characteristics are the oxidation is
4. Optimization of Factors. For the results obtained in dependent on the extract’s increase; the suspension
the Design of Experiment (DOE) conducted to is dependent on the sufficient volume; and, the rate
determine the optimal conditions for the removal of is dependent on the decrease of extract.
microplastics using ferrofluids, the response 2. As the rate of stirring increases in the synthesis, and
variable is the percentage of microplastic removal, the volume of stabilizing -coating extract is
which varies based on different experimental average, the particle size generated is in nanoscale.
parameters such as pH level, ferrofluid amount, and 3. As the contact time and the ferrofluid dose for the
contact time. The optimum conditions were found treatment increases, the microplastic removal
to be a pH level of 5.28, FF dosage of 4.88, a contact increases. In contrast to the two factors, as the pH
time of 5.85. This yielded a percentage removal of of the solution decreases, the microplastic removal
99.50% with a desirability of 1. In contrast, the increases in parallel.
lowest mean value from all the standard run 4. As the magnetite was reused for cycles, the
samples was 76.0%. The study also found that ferrofluid is still able to reduce microplastics in the
alkalinity and the amount of ferrofluid used in the solution.
 5. The suitable Adsorption Isotherm Model for the fit recyclable catalyst for the preparation of pyrrolo[3,4-c]
is Fleundrich, as for the Kinetic Order, the suitable quinoline-1,3-dione derivatives. RSC Advances (RSC
model was the Pseudo-second order. Publishing).
6. The null hypothesis which suggests that Iron Oxide https://pubs.rsc.org/en/content/articlelanding/2014/ra/c4ra1
Nanoparticle-derived (Fe3O4) Ferrofluid with 1623b
Caulerpa Lentillifera have no significant effects on
the microplastics in water, was declined. [8] IR Spectrum Table & Chart. (2022). MERCK.
https://www.sigmaaldrich.com/NL/en/technical-
documents/technical-article/analytical-
7. Recommendations chemistry/photometry-and-reflectometry/ir-spectrum-table
As this study is limited to microplastic recovery of PET, [9] Hosseini, F. (2014). Table 1 from Fe3O4 nanoparticles
it is recommended to further this through inclusion of modified with APTES as the carrier for (+) -(S)-2-(6-
varying types of plastics and correlate each recovery in methoxynaphthalen-2-yl) propanoic acid (Naproxen) and
relation to plastic type. Improvement on recovery data and (RS) 2-(3-benzoylphenyl)-propionic acid (Ketoprofen) drug
variables through comprehensive tests is advised. In line of | Semantic Scholar.
similar studies, categorization by type of plastic and size of https://www.semanticscholar.org/paper/Fe3O4-
plastic particulates in benefit of a more thorough result. nanoparticles-modified-with-APTES-as-the-for-Hosseini-
As the microplastic solution is merely simulated, it is Seyedsadjadi/df2702b1b7eedc95c3cf4efc7fcff322de7abefa
suggested to explore the synthesized ferrofluid’s capabilities /figure/0
in real world settings such as extraction of microplastics in
seawater.
[10] Du, X., Yan, P., Shen, Y., & Junkai, C. (2020).
Microwave Absorption Properties of Magnetite Particles
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