CHAPTER III

RESEARCH METHODS AND PROCEDURES

The main objective of this chapter is to provide an outline of the various steps involved in

conducting the research in the production and characterization of magnetic activated carbon

derived from taro leaves. It also presents the data gathering, optimization, and isotherm and

kinetic studies executed during the course of the study.

CONCEPTUAL FRAMEWORK

The conceptual framework is a graphical representation of the method by which the

researchers came up with the study's concept and formulation.

Input includes raw materials, reagents used in the synthesis of activated carbon,

preparation of the magnetic activated carbon and as well as experimentation. The parameters and

other data required for the experiment were gathered through related literature and studies.

Process involves the synthesis of the activated carbon, the experiments to identify the

suitable parameter ranges, the determination of oil percent concentration and statistical

evaluation of the results.

Output comprises the magnetic activated carbon made using taro leaves and its

properties, the magnetic activated carbon and the graphical analysis of the oil concentration in

varying parameters.
 PROCESS

INPUT  Synthesis of the

Activated Carbon
from taro leaves
OUTPUT
 Raw Materials  Production of the
(Taro Leaves) magnetic
 Activating activated carbon
 Magnetic
reagents and other  Treatment of the
Activated Carbon
reagents used simulated oil spill
 Statistical results
 Related  Determination of
Literatures and the oil percent
Studies concentration
 Statistical
Evaluation of the
Results

Figure 1. Conceptual Paradigm of the Study

Research Design

Experimental design will be utilized in the study to determine the diesel oil adsorption

capacity of magnetic activated carbon derived from Taro leaves. The study will use an

experimental approach to investigate the effects of the amount of dosage and contact time to the

adsorptive capacity of the activated carbon in adsorbing diesel oil from water.
 Collection of the Taro Leaves

Washing and Drying of the Taro Leaves

Size Reduction and Drying of the Taro Leaves

Impregnation with 80% KOH

Vacuum Filtration

Oven Drying at 120 °C for 12 hours

Activation of the Taro Leaves

Magnetization of the Activated Taro Leaves

Batch Adsorption Experiment

Statistical Treatment

Figure 2. Schematic Diagram of the Study

Figure 2 presents the experimental setup for the evaluation of the diesel oil adsorptive

capacity of Taro leaves derived oval tablets activated carbon. The Taro leaves will be collected

from a vacant lot in Lipa City, Batangas. The preparation for the Taro leaves will start. Then, it

will be followed by the activation and synthesis of the taro leaves. It will discuss the effects of
contact time and amount of the magnetic activated carbon to the adsorption of diesel oil from the

simulated oil spill. The experimental setup will include preparation of 3 sets of simulated oil spill

for the three varying amount of magnetic activated carbon and another 3 sets of simulated oil

spill for the assigned contact time. The study will also provide a graphical analysis of the

relationship between the number of oval tablets activated carbon applied, contact time, and the

adsorptive capacity of the oval tablet activated carbon.

Materials and Equipment

1. Taro Leaves

The Taro leaves will be acquired from a vacant lot Lipa City, Batangas. These will be

manually cut to reduce its size and will then be washed with distilled water. Then it will be sun

dried for 3 days and powdered to 150 mesh.

Figure X. Taro leaves

Source: Research Matters

 2. Bentonite

Calcium bentonite will be purchased from FCG Trading Inc., Carsadang Bago, Imus

City, Cavite.

Figure X. Calcium bentonite

Source: Livestrong

3. Potassium Hydroxide

The potassium hydroxide will be purchased Terran Supply Depot, Marcos Highway,

2600 Baguio City.

Figure X. Potassium hydroxide

Source: Noah Chemicals

 4. Ferric Chloride

The anhydrous Ferric Chloride will be purchased from Jinan Future Chemical Co., Ltd.

Figure X. Ferric chloride

Source: IndiaMart

5. Simulated Oil Spill

Diesel oil will be mixed with sea water at a concentration of 1% diesel oil by volume.

Diesel oil will be purchased from Sh Kumintang Llaya Bats, Shell petrol station.

6. Iron (ii) Sulfate Heptahydrate

The pure iron (ii) sulfate heptahydrate will be purchased from ChemPur.
 Figure X. Iron (ii) sulfate heptahydrate

Source: Science Photo Library

7. Muriatic acid

This will be used to adjust the pH of the samples. It will be purchased at Ace hardware,

SM Lipa City, Batangas.

Figure X. Muriatic acid

Source: Tesoro en Maderas

8. Sodium Hydroxide

This will be used to adjust the pH of the samples. It will be purchased at Binondo, Metro

Manila.
 Figure X. Sodium hydroxide

Source: WoodFinishing Enterprises

9. Analytical Balance

This will be used for a precise weight measurement of the activated carbon. It will be

used to measure mass in a sub-milligram range.

Figure X. Analytical balance

Source: Adam Equipment

10. Desiccator

The activated carbon will be stored in a desiccator to preserved it and preventing it

from having a chemical reaction with the moisture in the air.

 Figure X. Desiccator

Source: IndiaMart

11. Mechanical Sieve Shaker

This will be used to test the particle size distribution of the sample.

Figure X. Mechanical sieve shaker

Source: Gilson Company

12. Convection Oven

This will be utilized to dry the Taro leaves for 12 hours at a temperature of 120

degree Celsius. It will also be used in oven-drying the mixture of activated carbon for 12

hours at a temperature of 120 degree Celsius.

 Figure X. Convection oven

Source: EPDC - DOST

13. Squat form glass

This will be used in the production of magnetic activated carbon derived from taro

leaves.

Figure X. 2-liter squat form glass

Source: Capital Analytical

14. pH meter

The pH meter will be used to monitor and control the pH value of the synthetic water.
 Figure X. pH meter

Source: Shop Milwaukee Instruments

15. Hot Plate Magnetic Stirrer

The magnetic stirrer will be used to stir the powdered taro leaves, KOH and distilled

water to impregnate the powdered Taro leaves. The magnetic stirrer will run at 240 rpm for 6

hours at 80 °C temperature.

Figure X. Hot plate magnetic stirrer

Source: MMS Medical and Laboratory Supplies

PREPARATION OF THE MAGNETIC ACTIVATED CARBON

Synthesis of the Activated Carbon

1. 5 kg of the taro leaves will be acquired from a vacant lot Lipa City, Batangas.

2. These will be manually cut to reduce its size and will then be washed with distilled

water.

3. Then it will be sun dried for 3 days and powdered to 150 mesh.
 4. Taro leaves powder will be impregnated by mixing with KOH and adequate amount

of distilled water at impregnation ratio of 4:1 (KOH: taro leaves) with continuous

stirring for 6 hours at 80 °C using magnetic stirrer hot plate.

5. The mixture will be vacuum-filtered and oven-dried for 12 hours at 120 °C.

6. Then a 500 g of the dried powder will be sent to DOST for activation.

7. After the carbonization and activation of the taro leaves powder, it will then be

washed with a 3 N hot HCl solution to achieve a pH of 6.5 – 7.

8. Following vacuum filtration of the neutral activated carbon, residues will be removed

by repeated washing with 80 °C distilled water.

9. The prepared activated carbon will then be dried in an oven at 120 °C for 12 hours.

10. The activated carbon will be cooled and stored in a desiccator for further analysis as

the final step.

Magnetic Activated Carbon Preparation

1. In 500 mL of distilled water, 50 g of activated carbon from taro leaves will be

suspended.

2. A ferric chloride solution (FeCl3·6H2O) will be made by dissolving 135 g ferric

chloride in 1300 mL of distilled water, while a ferrous sulfate solution

(FeSO4·7H2O) will be made by dissolving 65 g ferrous sulfate in 150 mL of distilled

water.

3. In a 2-L beaker, both solutions will be mixed and heated to between 60 and 70 °C

before vigorous stirring with a magnetic stirrer. To ensure proper mixing, the ferric

chloride/ferrous sulfate solution suspension will be added to the previous aqueous

 suspension of taro leaves activated carbon and stirred slowly at room temperature for

30 minutes.

4. After mixing, 10 M NaOH solution will be added dropwise into the suspension until

it reaches a pH of 10 to 11 and will be left for 60 minutes. The activated carbon

suspension will be aged at room temperature for 24 hours without stirring, and the

suspended materials obtained from the reaction of taro leaves activated carbon and

iron suspension will be washed repeatedly with distilled water and ethanol until the

pH of the filtrate is around 7. The produced magnetic activated carbon will be

vacuum filtered and oven dried overnight at 50 °C.

Characterization of the Activated Carbon

A batch of the made activated carbon will be sent to Advanced Device and

Materials Testing Laboratory located at Bicutan, Taguig City and the powder will be

subjected to Fourier transform infrared spectroscopy (FTIR) analysis to know the

composition and the functional groups present on the surface of the activated carbon.

EXPERIMENTAL SET-UP

Experiments will be conducted to determine the effect of the amount of magnetic

activated carbon and contact time.

1. Three set ups will be required to determine the effects of the amount of sorbent

applied.

2. The simulated oil-water mixture will be prepared by mixing 15 mL of diesel oil with

1.5L water in a 20 cm x 15 cm x 20 cm container.

3. The pH of the mixture will be measured afterwards.

 4. The oil adsorption experiment will be performed with amount of magnetic activated

carbon (10g, 15g, 20g) and a controlled contact time (60 minutes).

5. After the specified contact time, the setups will be filtered, and the filtrate will be

sent to LLDA Labs to determine their oil and grease concentrations.

Table 2. Experimental Set-ups on the Varying Number of Tablets

Source: Catorce, J., et al (2022)

Run Number pH Amount of Contact Time % Removal of

magnetic (Minutes) Diesel Oil

activated carbon

(grams)

1 6 10 60

2 6 15 60

3 6 20 60

1. Three set ups will be required to determine the effects of contact time (30 minutes,

60 minutes and 90 minutes).

2. The simulated oil-water mixture will be prepared by mixing 15 mL of diesel oil

with 1.5L water in a 20 cm x 15 cm x 20 cm container.

3. The pH of the mixture will be measured afterwards.

4. The oil adsorption experiment will be performed with varying contact time (30

minutes, 60 minutes and 90 minutes) and a controlled amount of magnetic activated

carbon (15g).
 5. After the specified time of contacts, the setups will be filtered, and the filtrate will

be sent to LLDA Labs to determine their oil and grease concentrations.

Table 3. Experimental Set-ups on the Varying Contact Time

Source: Catorce, J., et al (2022)

Run Number pH Sorbent Dosage Contact Time % Removal of

Number of tablets) (Minutes) Diesel Oil

1 6 15 30

2 6 15 60

3 6 15 90

ANALYTICAL METHODS

Analysis of Activated Carbon

Activated carbon is used to purify liquids and gases in a variety of applications. This

includes municipal drinking water, food, beverage processing, odor removal and industrial

pollution control. The following are the different test methods that will be applied to determine

the properties of activated carbon:

1. Apparent bulk density test method

 This method is easy to do. It also has a low equipment cost with low maintenance.

The result is determined by a controlled free fall of the particles into a 100-milliliter

graduated cylinder.

2. Particle Size Sieving test method

This is a practical and cost-effective test to know the particle size. It functions by

providing mechanical separation with standard sieves

3. Scanning Electron Microscopy (SEM) Analysis

This is a strong analytical technique for performing examination on a wide range

of materials at high magnifications and producing high resolution images. Information

concerning properties such as pore size, surface area, and surface morphology can be

obtained through this test analysis.

4. ASTM D4607-94

It is intended to quantitatively measure the adsorption capacity of activated

carbons with a high adsorption capacity using the Standard Test Method for

Determination of Iodine Number of Activated Carbon. The test provides a reliable

indication of the carbon's microporosity.

Oil Concentration Determination

After the specified time of contacts, the setups will be filtered, and the filtrate will be sent

to Laguna Lake Development Authority (LLDA) Labs to determine their oil and grease

concentrations.

The amount of oil absorbed, q in mg/g, in each set-up will be calculated using the

formula:
 q= [ Ci−Cf
m ]V

Where:

 Ci is the initial oil concentration in mg/L

 Cf is the final oil concentration in mg/L

 V is the volume of solution in L

 m is the mass of the activated carbon in g

The percentage of removal of oil, Rem%, in solution will be calculated using the

following equation:

Rem %= ( Ci−Cf
Ci )
x 100 %

Adsorption Isotherm

The relationship between the solid phase concentration of the adsorbate and the solution

phase concentration of the adsorbent at the equilibrium condition under constant temperature will

be examined by conducting isotherm experiments. Mass ratio of the adsorbate to adsorbent will

be plotted against the oil concentration.

Statistical Treatment

Analysis of Variance (ANOVA) will be utilized in order to test the significant effect of

varying amount of magnetic activated carbon and contact time on the adsorption capacity.

The t-test will be used to determine if there is a significant difference in the percentage of

oil concentration before and after the treatment under optimal conditions.
Budget Requirements

The table below summarizes the budget requirements and allocation for this research.

The budget for this study will include the cost of raw materials, equipment, and testing

procedures to be performed in various laboratories.

Table 6. Cost Estimate

COST ESTIMATION

Product/Services Raw Price Quantity Price

Diesel Oil ₱ 80 1 liter ₱ 80

Collection of Taro leaves ₱0 5 kg ₱0

Distilled water ₱ 25 1 jug ₱ 25

Potassium hydroxide ₱ 75 3 packets ₱ 225

Muriatic acid ₱ 200 1 liter ₱ 200

Sodium Hydroxide ₱ 70 3 packets ₱ 210

Iron (ii) Sulfate Heptahydrate ₱ 780 1 packet ₱ 780

Ferric Chloride ₱ 700 1 kg ₱ 700

8 Liter container ₱ 150 8 pieces ₱ 1, 200

2-Liter Beaker

Glass Desiccator FREE OF USE FROM BSU MAIN II LABORATORY

 pH meter

Preparation of Activated ₱ 1, 466 1 test ₱ 1, 466

Carbon

SEM Analysis ₱ 8800 1 test ₱ 8, 800

FTIR Analysis ₱ 4000 1 test ₱ 4, 000

Oil and Grease Content ₱ 900 7 tests ₱ 6, 300

Sieve Analysis ₱ 400 1 test ₱ 400

TOTAL ₱ 24, 386

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