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Research Plan

Mae Anrielle O. Geniza


Doroteo S. Mendoza Sr. MNHS
Division of Oriental Mindoro

Production of Calamansi Peels Activated Carbon


for Biological Wastewater Treatment

General Objective :

The study aim to determine the effectiveness of Calamansi peel activated carbon (

Citrofortunella microcarpa) in treating biological wastewater.

Specific Objectives:

1. To produce an activated carbon out of calamansi peels.

2. To determine the properties of calamansi peel that can be used in production of activated

carbon.

3. To determine the effectiveness of different components of calamansi peel activated

carbon in treating wastewater in terms of:

a. pΗ

b. odor

c. color

d. time of removing impurities from wastewater

e. microbial properties

4. To determine the significant difference in the effectiveness between the different

components of calamansi peel activated carbon used in treating wastewater in terms of :

a. pΗ

b. odor
c. color

d. time of removing impurities of water

e. microbial properties

5. To determine the significant difference in the effectiveness between the experimental and

control group in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. microbial properties

Main Problem:

This study will find out the effectiveness of calamansi peel activated carbon in treating

biological wastewater.

Specific Problem:

The researcher will answer the following specific problem:

1. What properties are present in calamansi peel that can be used in the production of

activated carbon?

2. How effective are the different components of calamansi peel activated carbon in treating

biological wastewater in terms of:

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater


e. removing microbial properties

3. Is there significant difference in the effectiveness between the different components of

calamansi peel activated carbon in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties

4. Is there significant difference in the effectiveness between the experimental and control

group in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties

Statement of the Hypothesis

1. There is no significant difference in the effectiveness between the different components

of calamansi peels activated carbon in treating biological wastewater in terms of:

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties


2. There is no significant difference in the effectiveness between the experimental and

control group in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties

METHODOLOGY

The quantification of materials to be used in the study will be shown in the table below.

Quantity Materials
50 grams Medium size young calamansi peels
100 mḶ Hydrochloric acid
100 mḶ Sodium hydroxide
900 mḶ Storm Flood water
900 mḶ Sewage water
1 pc. Weighing scale
1 pc. Mortar and pestle
2 pcs. Old casserole
9 pcs. Beaker
1 pc. Stirrer
1 pc. Pot holder
1pc. Electric furnace
Methods to be used in the study will be shown in the flowchart below.

Collection Of Raw Materials ( Calamansi Peels)

Washing – SunDrying

Soaking with Hydrochloric acid and Sodium


Hydroxide

Filtering - Heating/ Cooking – Cooling - Pounding

Testing

Evaluating the Effectiveness of Calamansi Peels


Activated Carbon in Treating Biological Wastewater
Methodology

A. Collection Of Raw Materials

Fifty grams (50) of calamansi peel will be collected, while 100 mḶ of hydrocholoric acid

and sodium hydroxide will be purchased in laboratory.

Three hundred mḶ of rainwater and drainage water will be collected in the school

compound, that will be treated with calamansi activated carbon.

B. Washing – Sundrying

Obtained calamansi peel will be washed thoroughly with clean water to remove dirt. It

will be sundried for at least 6 – 7 days until the desired dryness achieved and the moisture

totally remove.

C. Soaking

One hundred (100) mḶ of hydrochloric acid and sodium hydroxide will be measured,

prepared, and label correctly. 4.5 grams of calamansi peels will be soaked in hydrochloric

and sodium hydroxide separately in 20 minutes.

D. Filtering - Cooking – Cooling – Measuring - Pounding

After soaking was done, calamansi will be filtered, then it will be transferred in casserole

for cooking using electrical furnace in temperature range from 100 – 150 ºC, in 15 minutes,

separately ( calamansi peels treated with hydrochloric acid and sodium hydroxide)

Obtained calamansi activated carbon will be cooled in a room temperature and pounded,

then it will be measured and transferred in a clean container labeled correctly according to its

treatment.
E. Testing

Experimental set-up and control setup will be used in the study to determine the

effectiveness of calamansi peel activated carbon in treating biological wastewater, in three

treatments; T1 Calamansi activated carbon ( activated with hydrochloric acid - acid), T2

Calamansi activated carbon ( activated with sodium hydroxide- basic solution), T3 with

commercialized activated carbon in three trials.

The initial pΗ level of the wastewater sample, (100 mḶ storm flood water and sewage

water), will be measured and noted as well as the color and the odor of the water sample.

100 mḶ of wastewater sample will be treated with 1.5 grams of calamansi activated

carbon, mixed directly on the water sample and filtered in three trials. The time of filtration

will be observed and noted, as well as the changes in the samples color and odor. The pΗ

level of the water samples will also be measured in each treatment and trials.

Sensory evaluation technique will be used in evaluating the rate of changes in color and

odor of the water samples, using the given rating scale.

Color Description Rate Interpretation

Color less/ Clear - absence of Very Effective

any suspended particles 4

Clear, little amount of Effective

suspended particles can be 3

seen in the light

Slightly clear – there are Partially Effective

some suspended particles that 2

can be observed in the water


Dark Color- Suspended

Particles are observable in 1 Not Effective

the water

Odor Description Rate Interpretation

Odorless – No odor came

from the water 4 Very Effective

Slightly Odorless– Far from

the nose trill no odor can be 3 Effective

detected, near the nose trill a

slight foul odor detected

Somewhat Odorless- a foul

odor can easily detected 2 Partially Effective

A foul odor detected 1 Not Effective

Same set-up will be used in the control group.

F. Data Analysis
Weighted average mean will be used to determine the effectiveness of different

components of calamansi peel activated carbon in treating biological wastewater in terms of

pΗ, color, odor, time of filtration/removing impurities of wastewater and removing microbial

properties. Meanwhile t-test will be used to determine the significant difference in the

effectiveness between the different components of calamansi activated carbon in treating

biological wastewater. On the other hand to determine the significant difference in the

effectiveness between the experimental and control group in treating biological wastewater

Anova will be used, both in terms of pΗ, color, odor, time of removing impurities of water

and the rate of removing microbial properties.

1. What properties are present in calamansi peel that can be used in the production of

activated carbon?

Table 1

Calamansi Peel Properties that can be used in Production of Activated Carbon

Calamansi Peels Properties that can be used Description

in Production of Activated Carbon

2. How effective are the different components of calamansi peel activated carbon in treating

biological wastewater in terms of:

a. pΗ

b. odor

c. color
d. time of removing impurities of wastewater

e. removing microbial properties

Table 2

Effect of Different Components of Calamansi Peel Activated Carbon in Treating Biological

Wastewater (Storm Flood Water) in terms of pΗ Level

Trial Trial Trial Average

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon ( activated with

hydrocholoric acid – acidic solution)

T2- Calamansi Peel Activated Carbon ( activated with sodium

hydroxide – basic solution)

T3- Commercialized Activated Carbon ( Control)

Table 3

Effect of Different Components of Calamansi Peel Activated Carbon in Treating Biological

Wastewater (Sewage Wastewater) in terms of pΗ Level

Trial Trial Trial Average

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon ( activated with

hydrocholoric acid – acidic solution)

T2- Calamansi Peel Activated Carbon ( activated with sodium

hydroxide – basic solution)

T3- Commercialized Activated Carbon (Control)


Table 4

Rate in changes in Odor of Wastewater (Storm flood Water) treated with Calamansi Peels

Activated Carbon

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Control)

Table 5

Rate in changes in Odor of Wastewater (Sewage Wastewater) treated with Calamansi Peels

Activated Carbon

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic


solution)

T3- Commercialized Activated Carbon (

Control)

Table 6

Rate in changes in Color of Wastewater (Storm Flood Water) treated with Calamansi Peels

Activated Carbon

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Control)

Table 7

Rate in changes in Color of Wastewater (Sewage Wastewater) treated with Calamansi Peels

Activated Carbon

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic


solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Control)

Table 8

Time of Removing Impurities of Wastewater ( Storm flood water), using Calamansi Peels

Activated Carbon in Seconds

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Control)

Table 9

Time of Removing Impurities of Wastewater ( Sewage Wastewater), using Calamansi Peels

Activated Carbon in Seconds


Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Control)

Table 10

Rate of Removing Microbial of Wastewater ( Storm flood water), using Calamansi Peels

Activated Carbon in Seconds

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (


Control)

Table 11

Rate of Removing Microbial of Wastewater ( Sewage), using Calamansi Peels Activated Carbon

in Seconds

Trial Trial Trial Average Interpretation

Treatment 1 2 3

T1-Calamansi Peel Activated Carbon (

activated with hydrocholoric acid – acidic

solution)

T2- Calamansi Peel Activated Carbon (

activated with sodium hydroxide – basic

solution)

T3- Commercialized Activated Carbon (

Conrol)

3. Is there significant difference in the effectiveness between the different components of

calamansi peel activated carbon in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties


Table 12

Summary of Differences in pΗ between the Different Components of Calamansi Peel Activated

Carbon in Treating Biological Wastewaster ( Storm Flood Water).

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 13

Summary of Differences in pΗ between the Different Components of Calamansi Peel Activated

Carbon in Treating Biological Wastewaster ( Sewage Waste Water).

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 14

Summary of Differences in the Time of Removing Impurities of Wastewater ( Storm Flood

Water) between the Different Components of Calamansi Peel Activated Carbon in Seconds

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon


Table 15

Summary of Differences in the Time of Removing Impurities of Wastewater ( Sewage Water)

between the Different Components of Calamansi Peel Activated Carbon in Seconds

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 15

Summary of Differences in the Rate of Changes in Color of Wastewater ( Storm Flood

Wastewater) between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 16

Summary of Differences in the Rate of Changes in Color of Wastewater ( Sewage Wastewater)

between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon


Table 17

Summary of Differences in the Rate of Changes in Odor of Wastewater ( Storm Flood

Wastewater) between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 17

Summary of Differences in the Rate of Changes in Odor of Wastewater ( Sewage Wastewater)

between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 18

Summary of Differences in the Rate of Removing Microbial Properties ( Storm Flood

Wastewater) between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

Table 19
Summary of Differences in the Rate of Removing Microbial Properties ( Sewage Wastewater)

between the Different Components of Calamansi Peel Activated Carbon.

Experimental Set-ups df Computed Critical f Interpretation

f value value

Different Components of

Calamansi Peel Activated Carbon

4. Is there significant difference in the effectiveness between the experimental and control

group in treating biological wastewater in terms of :

a. pΗ

b. odor

c. color

d. time of removing impurities of wastewater

e. removing microbial properties

Table 20

Summary of Differences in the pΗ Level of Wastewater ( Storm Flood Wastewater) between

the Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 21
Summary of Differences in the pΗ Level of Wastewater ( Sewage Wastewater) between the

Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 22

Summary of Differences in the Rate of Changes in the Color of Wastewater ( Storm Flood

Wastewater) between the Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 23

Summary of Differences in the Rate of Changes in the Color of Wastewater ( Sewage

Wastewater) between the Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 24
Summary of Differences in the Rate of Changes in the Odor of Wastewater ( Storm Flood

Wastewater) between the Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 25

Summary of Differences in the Rate of Changes in the Odor of Wastewater ( Sewage

Wastewater) between the Experimental and Control Groups

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 26

Summary of Differences in the Time of Removing Impurities of Wastewater ( Storm Flood

Wastewater) between the Experimental and Control Groups in Seconds.

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 27
Summary of Differences in the Time of Removing Impurities of Wastewater ( Sewage

Wastewater) between the Experimental and Control Groups in Seconds.

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 28

Summary of Differences in the Rate of Removing Microbial Properties of Wastewater ( Storm

Flood Wastewater) between the Experimental and Control Groups.

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups

Table 29

Summary of Differences in the Rate of Removing Microbial Properties of Wastewater ( Storm

Flood Wastewater) between the Experimental and Control Groups.

Groups df Computed Critical f Interpretation

f value value

Experimental and Control Groups


Introduction

In the Philippines, agriculture is one of the major source of income, due to its suitable

location for agricultural activities, having a tropical climate and gifted natural and aquatic

resources. One of the countries product from agricultural industry is calamansi. It has been

transported in different parts of the country for industrial uses like food and beverages, cosmetics

etc, but it’s peels has been neglected and consider as waste.
In the province of Oriental Mindoro, Calamansi plantation is also dominant in the

municipality of Victoria and due to its dominance, researcher think about the way on how to

utilize calamansi peels into an activated carbon, converting it from waste to useful one, that can

be used in treating wastewater.

Wastewater contain physical, chemical and biological pollutants, contributed to the

problem in water pollution. It came from domestic waste water from households, municipal

wastewater from communities or industrial wastewater from industrial activities, however it can

be treated to purify and reuse again, since water is one of the most significant necessities of the

living organisms; and all plants, animals and humans are reliant on water to survive.

Wastewater treatment is a process use to remove the pollutants from the wastewater.

These can be done through distillation, electro coagulation, dehumidification process and

adsorption process. It can also be done with the use of activated carbon.

Activated carbon also called activated charcoal or activated coal, is a form of carbon

processed to have small, low-volume pores that increase the surface area available for adsorption

or chemical reactions. Activated is sometimes substituted with active. Due to its high degree of

micro porosity, just one gram of activated carbon has a surface area in excess of 500 m2 (5,400

sq ft), as determined by gas adsorption. An activation level sufficient for useful application may

be attained solely from high surface area; however, further chemical treatment often enhances

adsorption properties. Activated carbon is usually derived from charcoal and, increasingly, high-

porosity bio char. Activated carbon is used in gas purification, decaffeination, gold purification,

metal extraction, water purification, medicine, sewage treatment, air filters in gas masks and

respirators, filters in compressed air and many other applications (Engineers Edge, 2017).
Biological activated carbon (BAC) has great advantages in low concentration and

refractory organic wastewater degradation. There are several advantages of BAC that includes

several aspects.(1)The adsorption function of active carbon: organic matter is enriched in carbon

particles, increasing contact time of organic matter and microorganisms and providing favorable

conditions for microbial acclimation, so that the refractory material can be removed.

(2)Adsorption of active carbon increases organic matter concentration around carbon particles,

which is favorable to biological degradation. (3)The rough surface with cracks and honeycomb

pits provides residential area for dominant bacteria to evade fluid shear stress. (4) The active

carbon with strong adsorption capacity can absorb dissolved organic matters (DOMs). These

DOMs provide food for the dominant bacteria. (5)Intense microbial activity accelerated the

removal of organic matter. Even in the condition of low organic content, microorganisms still

grow actively and decompose organic matter constantly due to the accumulation of carbon

surface. And then the concentration of organics in the effluent decreased. (6)Active carbon

reduces the effect of harmful substances to microorganism in water. (7)This is mainly because

the adherent microorganism can resist poison of biodegradable organic compounds (Xie, Guan,

Ji, Song, and Zhao, 2014).

Calamansi peel with porous structure possesses hydrophilic surface group is a cheap

adsorbent, that can be used in production of activated carbon. Absorption can be enhanced by

carbonization and activation. During the activation process, activator get into the interface due to

the natural pore of calamansi peel.Thus, the activation reaction can be in progress under a mild

condition. The as-prepared active carbon with loose pore structure and large specific surface area
and massive surface functional groups possesses favorable biophile characteristic and adsorption

performance (Xie, Guan, Ji, Song, and Zhao, 2014).

According to Roopa (2016), bitter orange, seville orange, sour orange, bigarade orange,

or marmalade orange refers to a citrus tree the botanical name for bitter orange is Citrus

aurantium. It was employed in herbal medicine as a stimulant and appetite suppressant, due to its

active ingredient, synephrine, that explores the feasibility of bitter orange, a biomass as an

alternative precursor for preparation of activated carbon with sulphuric acid activation (H2SO4)

as activating agent at relatively low temperatures such as 90, 120, 150 were used to produce

different activated Carbons. Therefore calamansi peels, can also be used in production of

activated carbon with the used of any activating agent, that can be used in removing heavy metal

in water.

According to Fernandez et al. (2014), activated carbon from orange (Citrus sinensis) peel

was developed through H3PO4 acid activation. The orange peel-based activated carbon presented

a high specific surface area (1090 m2/g), predominance of mesopores and acidic character. It also

showed a high adsorption capacity for both dyes in batch and dynamic modes. Experimental

equilibrium isotherms obtained from single-dye solutions fitted the Langmuir–Freundlich model,

and those obtained from binary solutions were properly described by single and multi-component

models. Breakthrough curves obtained from single-dye solutions exhibited a better removal

The treatment of wastewater is needed due to the absence of water resources all over the

world, and after treatment the wastewater may be used again for different purposes likes

chemical processes in the manufacturing works and irrigation of grasses in parks. Activated
carbon is used in water station, waste water station, fuel storage, gas purification and chemical

purification.

From this scenario, researcher came up with this study which aims to determine the

effectiveness of calamansi ( C. microcarpa )peels activated carbon in treating biological

wastewater.

Significance of the Study

This study will be beneficial to all, they can used calamansi peels activated carbon in
treating wastewater, to lessen water pollutants and increase the possible source of clean water.

For the community, it will help in decreasing the environmental pollutions caused by the
contaminated wastewater as well as providing a healthier community.

For the food processor industry, this could help in lessening the allotted budget for the

treatment facility since we are using waste peel from Calamansi.

For the farmers, they can utilize the used of calamansi peel activated carbon in treating

wastewater, to be used in irrigation or supply of water.


For the school, this study will provide understanding about wastewater treatment that can

lead for more researches regarding the alternative ways of providing wastewater treatment.

For the present researchers, this study will give background on future researches about

Actived Carbon for biological wastewater treatment.

Scope and Limitation

The study will focus only in producing an activated carbon out of calamansi peels and
determining its effectiveness in treating biological wastewater.

Hydrochloric acid and Sodium hydroxide will be used in the production of activated
carbon out of calamansi peels. It will be tested in two different types of biological wastewater;
storm flood water and the sewage water. The pΗ level of the wastewater samples will be
measured, while the changes in color, odor and the time of purification will be observed and
noted.

The study will be conducted from June 4- July 30, 2018 at Doroteo S. Mendoza Sr.
MNHS, Pagkakaisa, Naujan Oriental Mindoro.
Wastewater emitted from Domestic and industries contain impurities that are destructive for our

health as well as the Environment. Therefore, it must be treated even before discharging it out. In

this study, knowledge regarding the production of activated carbon from Calamansi peel for

biological wastewater treatment was gathered which could help in many industries.

For the community, this study could help in decreasing the environmental pollutions

caused by the contaminated wastewater as well as providing healthier community.

For the food processor, this could help in lessening the allotted budget for the treatment

facility since we are using waste peel from Calamansi.

For the fishing industry, sport fishing enthusiasts, and future generations, it is important

to produce activated carbon from the Calamansi peel by using it in eco-friendly method to

decrease the pollution and increase economy.

For the academe, the Batangas State University, this study will provide understanding

about wastewater treatment that can lead for more researches regarding the alternative ways of

providing wastewater treatment.

For the present researchers, this study will give background on future researches about

Actived Carbon for biological wastewater treatment.


Review of Related Studies

According to Roopa (2016), bitter orange, seville orange, sour orange, bigarade orange,

or marmalade orange refers to a citrus tree the botanical name for bitter orange is Citrus

aurantium. It is a hybrid between Citrus maxima (pomelo) and Citrus reticulata (mandarin).

Many varieties of bitter orange are used for their essential oil, and are found in perfume, used as

flavouring or as a solvent. The Seville orange variety is used in the production of marmalade.

Bitter orange is also employed in herbal medicine as a stimulant and appetite suppressant, due to

its active ingredient, synephrine. This work explores the feasibility of bitter orange, a biomass as

an alternative precursor for preparation of activated carbon with sulphuric acid activation

(H2SO4) as activating agent at relatively low temperatures such as 90, 120, 150 were used to

produce different activated Carbons and finally 150C for 30min were used for the study

purposes. The effects of the operation al parameters were investigated with reference to the CAC

value. In addition to this, physical characterization of the same was done to determine its bulk

density, ash content, moisture content, ion exchange capacity, matter soluble in water and matter

soluble in acid. Further this activated carbon is used to remove the heavy metal that is present in

water.

According to Fernandez et al. (2014), activated carbon from orange (Citrus sinensis) peel

was developed through H3PO4 acid activation. Its ability as an adsorbent for the removal of two

representative basic dyes (methylene blue and rhodamine B) from single and binary dyes
solutions in batch and continuous modes was examined. The orange peel-based activated carbon

presented a high specific surface area (1090 m2/g), predominance of mesopores and acidic

character. It also showed a high adsorption capacity for both dyes in batch and dynamic modes.

Experimental equilibrium isotherms obtained from single-dye solutions fitted the Langmuir–

Freundlich model, and those obtained from binary solutions were properly described by single

and multi-component models. Breakthrough curves obtained from single-dye solutions exhibited

a better removal performance for rhodamine B. Adsorption capacity at exhaustion time for this

dye was 11% higher than for methylene blue. Additional experiments in dynamic conditions with

a binary solution of both dyes pointed to adsorption competition for the active sites of the

developed carbon. Breakthrough curves were adequately represented by a modified two-

parameter model.

According to Mohammad et al. (2015), this study was conducted to investigate the

removal of cadmium (II) from aqueous solution by using low cost, natural and eco-friendly

biosorbent of Banana peels Activated Carbon (BPAC) through batch experiments. The Activated

Carbon was characterized by FTIR, SEM, TEM with EDX. Various adsorption parameters such

as effect of pH, amount of the biomass, initial concentration of Cadmium ion and contact time on

the adsorption capacity of the biosorbent were studied. Biosorption experiments were carried out

at the temperature of 25ºC. The percent removal of Cadmium ions was 98.35% from synthetic

wastewater. These results were observed at the optimum dose of 0.8 g at pH 4.0. The removal of

Cadmium ions from wastewater is mainly influenced by pH of the synthetic wastewater and the

amount of biosorbent dose. The equilibrium adsorption data were fitted to Langmuir adsorption

isotherm model and the model parameters were evaluated. The kinetic study showed that the

pseudo-second order kinetic model better described the biosorption process. These results
demonstrated that the Banana peels could be used as a natural biosorbent for removal of

Cadmium from aqueous solution

According to Mahanim et al. (2010), this study was conducted to produce activated

carbon from bamboo residues using carbonization and steam activation in a high temperature

reactor. Tests were carried out to study the effects of two processing parameters, namely,

activation time (30, 60, 90, 120 and 150 min) and activation temperature (650, 700, 750 and

800°C) on the properties of activated carbon produced. Activated carbon properties were

analysed based on iodine number and Brunauer-Emmett Teller (BET) surface area. Increasing

activation temperature gave higher iodine values. Optimum conditions for producing activated

carbon from bamboo wastes were at activation temperature 800°C and activation time 120 min

that resulted in bamboo activated carbon with the highest iodine number of 823 mg g -1 and BET

surface area of 719 m 2 g -1. With these parameters, waste bamboo has the potential to be a

promising precursor for the production of activated carbon. The characteristics of the activated

carbon in this study were comparable with commercial ones.

According to Panyathanmaporn et al. (2008), the production of activated carbon from

coconut shell treated with phosphoric acid (H3PO4) was optimized using the response surface

methodology (RSM). Fifteen combinations of the three variables namely; impregnation ratio (1,

1.5, and 2); activation time (10, 20, and 30 min); and activation temperature (400, 450, and

500 °C) were optimized based on the responses evaluated (yield, bulk density, average pore

diameter, small pore diameter, and number of pores in a unit area). Pore diameters were directly

measured from scanning electron microscope (SEM) images. Individual second-order response

surface models were developed and contour plots were generated for the optimization analysis.

The optimum range identified for impregnation ratio was from 1.345 to 2, while for the
activation time was from 14.9 to 23.9 min. For the activation temperature it was from 394 to

416 °C. The optimum points are 1.725, 19.5 min, and 416 °C, respectively. The models were

able to predict well the values of the responses when the optimum variable parameters were

validated as proven by the generally acceptable values of the residual percentages. Direct

characterization of the pores using the SEM was found to be a good technique to actually see the

pores and get actual measurements. Additionally, RSM has also proven to be a good tool in

optimization analysis to get not only optimum production condition points but ranges, which are

crucial for the flexibility of the production process, as well.

According to Villarante, Bautista and Sumalapao (2017), heavy metals are emitted to the

environment via different processes and pathways leading to environmental pollution.

Bioremediation, the utilization of naturally occurring microorganisms to break down

environmental pollutants, has been an emerging field of study. Currently, several processes are

employed in the removal of toxic metal ions such as ion exchange, membrane processes,

precipitation, and adsorption. Adsorption is recognized as an efficient and economic method for

the removal of pollutants from wastewater. However, innovations have been developed

involving this process such as the utility of low-cost bio sorbents as these can reduce the cost of

an adsorption system significantly. Batch adsorption of toxic Cr (VI) ion from an aqueous

solution using lumbang (Aleurites moluccana) activated carbon-chitosan composite cross-linked

with epichlorohydrin as an adsorbent was investigated. The adsorption experiments were

performed at varying pH, agitation time, initial Cr(VI) ion concentration, temperature, and

adsorbent dose. At an initial concentration of 60 ppm Cr(VI), the maximum adsorption was

observed at pH 3, adsorbent dose of 3 g/L, contact time of 75 min, and temperature of 30oC.
Analysis of the experimental data using different kinetic models revealed that the bio sorption

phenomenon behaved under a pseudo second-order rate mechanism.

Last 2007, Lizardo conducted a study entitled “Activated Carbon from Various

Agricultural Wastes and their Efficacy for the Removal of Dyes and Metal Ions from Aqueous

Solutions”. Maize cob, coconut sawdust, and dalandan peels were carbonized and treated with

H3PO4 (85%w) as activating agent. The activating carbon was used in batch mode studies using

aqueous solutions of methylene blue, Rhodamine–B, Congo red, methyl violet and Mercury

(Hg2+) as adsorbates. Fifty – milliliter dyes or metal ion solution (25 mg/L) and 250 mg

adsorbent (particle size < 250 m) were taken in a 100mL Erlenmeyer flask and agitated at 160

rpm. The flasks were withdrawn at 1, 3, 24 h interval, centrifuged and subjected to

spectrophotometric analysis. Experimental results showed that carbon was effective in the

removal of pollutants from water. Activated carbon prepared from coconut sawdust exhibited

94.4% removal of methyl violet, 93.4% removal of methylene blue, 91.54% removal of Hg

solute, 78.76% removal of Congo red and 63.48% removal of Rhodamine-B. . Activated carbon

prepared from corncob exhibited 94.77% removal of Hg solute, 89.25% removal of methyl

violet, 75.25% removal of Rhodamine–B, 72.285% removal of methylene blue and 51.71%

removal.

According to Cruz, Mirilä, Huuhtanen, Marrión, Alvarenga, and Keiski (2012), activated

carbons were obtained from cocoa pod husk using two different initial particle sizes (ranges 0.25

– 0.50mm and 0.50 – 1.00mm), three chemical activation agents (K2CO3, KOH and ZnCl2) and

carbonization under nitrogen atmosphere during two hours at three different temperatures

(500°C, 650°C and 800°C). The prepared activated carbons were characterized using Brunauer–

Emmett–Teller (BET) and Langmuir surface areas, pore volume, average pore size, bulk density,
moisture, ash content, and yield. The five best activated carbons were selected for further

experiments according to the chemical activation agent used, high BET surface area, high pore

volume and low ash content. Additionally, content of impurities, carbon content and FE-SEM

micrographs were determined for these five best activated carbons. As adsorption tests were also

carried out with these samples. Results of the experiments show that cocoa pod husk is a material

that can be used to produce activated carbon by chemical activation and ZnCl2 showed to be the

best chemical activation agent based on the highest BET surface area (780 m2/g in the best case)

and pore volume (0.58 m3/g in the best case), the lowest ash content (6.14% in the best case),

and the highest carbon content (86.1% in the best case), compared with others chemicals.

Carbons activated by ZnCl2 are capable to adsorb As(V), getting As(V) removal levels up to

80% in less than 1 hour in the experimental conditions applied (initial pH 6-7, activated carbon

concentration 0.1 g/l and 0.5 g/l, initial As concentration 100 ppb).

Gallardo and Tanala (2012) conducted a study that describes a method to decrease the

incidence of diseases caused by pesticides, heavy metals, and bacteria through a simple, low-

cost, and sustainable personal water purification solution for the citizens of Nagcarlan, Laguna in

the Philippines. Activated carbon (AC) adsorption was the primary treatment used in the removal

of methomyl, a carbamate pesticide, and hexavalent chromium (Cr(VI)), a heavy metal. Also,

citricidal was used to disinfect water from coliforms. Surface hydroxyl with aliphatic and

aromatic groups from the AC, were confirmed using Fourier transform infrared (FTIR)

spectroscopy. The activated carbon used in this study was produced from coconut shell through

the process developed by the Industrial Technology Development Institute (ITDI) under the

Department of Science and Technology (DOST) in the Philippines.


According to Demafelis and Matibag (2001), technologies are currently being developed to treat

wastewater so that the water can be used again. Production of activated carbon (AC) from

agricultural by-products is a good example of this technology. AC is a very fine form of carbon

used in various industrial processes such as the removal of unwanted colors and odors, recovery

of solvent vapors, purification of water, and removal of obnoxious, toxic, or unwanted gases and

vapors. The problem is how to produce activated carbon efficiently and cheaply, hence, the

studies on the coconut shell, as waste product in copra making. AC was produced by pulverizing

the coconut shell and treating the powder with ammonium chloride (NH4Cl) from one hour at

different temperature settings (400, 600, and 800 degrees C) and at different NH4Cl-shell ratios

(1:4, 1:6, 1:8). For activation, a device called pyrolyzer was used. The device was a local

prototype adapted from a Japanese design. Based on the amount of carbon produced and the

capability of the activated carbon to decolorize wastewater, the best treatment combination for

producing activated carbon from coconut shell is at a temperature setting of 800 degrees C and a

NH4Cl-shell ratio of 1:4.


Review of Related Literature

Related Studies

Foreign Studies

According to Roopa (2016), bitter orange, seville orange, sour orange, bigarade orange,

or marmalade orange refers to a citrus tree the botanical name for bitter orange is Citrus

aurantium. It is a hybrid between Citrus maxima (pomelo) and Citrus reticulata (mandarin).

Many varieties of bitter orange are used for their essential oil, and are found in perfume, used as

flavouring or as a solvent. The Seville orange variety is used in the production of marmalade.

Bitter orange is also employed in herbal medicine as a stimulant and appetite suppressant, due to

its active ingredient, synephrine. This work explores the feasibility of bitter orange, a biomass as

an alternative precursor for preparation of activated carbon with sulphuric acid activation

(H2SO4) as activating agent at relatively low temperatures such as 90, 120, 150 were used to

produce different activated Carbons and finally 150C for 30min were used for the study

purposes. The effects of the operation al parameters were investigated with reference to the CAC

value. In addition to this, physical characterization of the same was done to determine its bulk

density, ash content, moisture content, ion exchange capacity, matter soluble in water and matter

soluble in acid. Further this activated carbon is used to remove the heavy metal that is present in

water.

According to Fernandez et al. (2014), activated carbon from orange (Citrus sinensis) peel

was developed through H3PO4 acid activation. Its ability as an adsorbent for the removal of two

representative basic dyes (methylene blue and rhodamine B) from single and binary dyes

solutions in batch and continuous modes was examined. The orange peel-based activated carbon

presented a high specific surface area (1090 m2/g), predominance of mesopores and acidic
character. It also showed a high adsorption capacity for both dyes in batch and dynamic modes.

Experimental equilibrium isotherms obtained from single-dye solutions fitted the Langmuir–

Freundlich model, and those obtained from binary solutions were properly described by single

and multi-component models. Breakthrough curves obtained from single-dye solutions exhibited

a better removal performance for rhodamine B. Adsorption capacity at exhaustion time for this

dye was 11% higher than for methylene blue. Additional experiments in dynamic conditions with

a binary solution of both dyes pointed to adsorption competition for the active sites of the

developed carbon. Breakthrough curves were adequately represented by a modified two-

parameter model.

According to Mohammad et al. (2015), this study was conducted to investigate the

removal of cadmium (II) from aqueous solution by using low cost, natural and eco-friendly

biosorbent of Banana peels Activated Carbon (BPAC) through batch experiments. The Activated

Carbon was characterized by FTIR, SEM, TEM with EDX. Various adsorption parameters such

as effect of pH, amount of the biomass, initial concentration of Cadmium ion and contact time on

the adsorption capacity of the biosorbent were studied. Biosorption experiments were carried out

at the temperature of 25ºC. The percent removal of Cadmium ions was 98.35% from synthetic

wastewater. These results were observed at the optimum dose of 0.8 g at pH 4.0. The removal of

Cadmium ions from wastewater is mainly influenced by pH of the synthetic wastewater and the

amount of biosorbent dose. The equilibrium adsorption data were fitted to Langmuir adsorption

isotherm model and the model parameters were evaluated. The kinetic study showed that the

pseudo-second order kinetic model better described the biosorption process. These results

demonstrated that the Banana peels could be used as a natural biosorbent for removal of

Cadmium from aqueous solution


According to Mahanim et al. (2010), this study was conducted to produce activated

carbon from bamboo residues using carbonization and steam activation in a high temperature

reactor. Tests were carried out to study the effects of two processing parameters, namely,

activation time (30, 60, 90, 120 and 150 min) and activation temperature (650, 700, 750 and

800°C) on the properties of activated carbon produced. Activated carbon properties were

analysed based on iodine number and Brunauer-Emmett Teller (BET) surface area. Increasing

activation temperature gave higher iodine values. Optimum conditions for producing activated

carbon from bamboo wastes were at activation temperature 800°C and activation time 120 min

that resulted in bamboo activated carbon with the highest iodine number of 823 mg g -1 and BET

surface area of 719 m 2 g -1. With these parameters, waste bamboo has the potential to be a

promising precursor for the production of activated carbon. The characteristics of the activated

carbon in this study were comparable with commercial ones.

According to Panyathanmaporn et al. (2008), the production of activated carbon from

coconut shell treated with phosphoric acid (H3PO4) was optimized using the response surface

methodology (RSM). Fifteen combinations of the three variables namely; impregnation ratio (1,

1.5, and 2); activation time (10, 20, and 30 min); and activation temperature (400, 450, and

500 °C) were optimized based on the responses evaluated (yield, bulk density, average pore

diameter, small pore diameter, and number of pores in a unit area). Pore diameters were directly

measured from scanning electron microscope (SEM) images. Individual second-order response

surface models were developed and contour plots were generated for the optimization analysis.

The optimum range identified for impregnation ratio was from 1.345 to 2, while for the

activation time was from 14.9 to 23.9 min. For the activation temperature it was from 394 to

416 °C. The optimum points are 1.725, 19.5 min, and 416 °C, respectively. The models were
able to predict well the values of the responses when the optimum variable parameters were

validated as proven by the generally acceptable values of the residual percentages. Direct

characterization of the pores using the SEM was found to be a good technique to actually see the

pores and get actual measurements. Additionally, RSM has also proven to be a good tool in

optimization analysis to get not only optimum production condition points but ranges, which are

crucial for the flexibility of the production process, as well.

Local Studies

According to Villarante, Bautista and Sumalapao (2017), heavy metals are emitted to the

environment via different processes and pathways leading to environmental pollution.

Bioremediation, the utilization of naturally occurring microorganisms to break down

environmental pollutants, has been an emerging field of study. Currently, several processes are

employed in the removal of toxic metal ions such as ion exchange, membrane processes,

precipitation, and adsorption. Adsorption is recognized as an efficient and economic method for

the removal of pollutants from wastewater. However, innovations have been developed

involving this process such as the utility of low-cost bio sorbents as these can reduce the cost of

an adsorption system significantly. Batch adsorption of toxic Cr (VI) ion from an aqueous

solution using lumbang (Aleurites moluccana) activated carbon-chitosan composite cross-linked

with epichlorohydrin as an adsorbent was investigated. The adsorption experiments were

performed at varying pH, agitation time, initial Cr(VI) ion concentration, temperature, and

adsorbent dose. At an initial concentration of 60 ppm Cr(VI), the maximum adsorption was

observed at pH 3, adsorbent dose of 3 g/L, contact time of 75 min, and temperature of 30oC.

Analysis of the experimental data using different kinetic models revealed that the bio sorption

phenomenon behaved under a pseudo second-order rate mechanism.


Last 2007, Lizardo conducted a study entitled “Activated Carbon from Various

Agricultural Wastes and their Efficacy for the Removal of Dyes and Metal Ions from Aqueous

Solutions”. Maize cob, coconut sawdust, and dalandan peels were carbonized and treated with

H3PO4 (85%w) as activating agent. The activating carbon was used in batch mode studies using

aqueous solutions of methylene blue, Rhodamine–B, Congo red, methyl violet and Mercury

(Hg2+) as adsorbates. Fifty – milliliter dyes or metal ion solution (25 mg/L) and 250 mg

adsorbent (particle size < 250 m) were taken in a 100mL Erlenmeyer flask and agitated at 160

rpm. The flasks were withdrawn at 1, 3, 24 h interval, centrifuged and subjected to

spectrophotometric analysis. Experimental results showed that carbon was effective in the

removal of pollutants from water. Activated carbon prepared from coconut sawdust exhibited

94.4% removal of methyl violet, 93.4% removal of methylene blue, 91.54% removal of Hg

solute, 78.76% removal of Congo red and 63.48% removal of Rhodamine-B. . Activated carbon

prepared from corncob exhibited 94.77% removal of Hg solute, 89.25% removal of methyl

violet, 75.25% removal of Rhodamine–B, 72.285% removal of methylene blue and 51.71%

removal.

According to Cruz, Mirilä, Huuhtanen, Marrión, Alvarenga, and Keiski (2012), activated

carbons were obtained from cocoa pod husk using two different initial particle sizes (ranges 0.25

– 0.50mm and 0.50 – 1.00mm), three chemical activation agents (K2CO3, KOH and ZnCl2) and

carbonization under nitrogen atmosphere during two hours at three different temperatures

(500°C, 650°C and 800°C). The prepared activated carbons were characterized using Brunauer–

Emmett–Teller (BET) and Langmuir surface areas, pore volume, average pore size, bulk density,

moisture, ash content, and yield. The five best activated carbons were selected for further

experiments according to the chemical activation agent used, high BET surface area, high pore
volume and low ash content. Additionally, content of impurities, carbon content and FE-SEM

micrographs were determined for these five best activated carbons. As adsorption tests were also

carried out with these samples. Results of the experiments show that cocoa pod husk is a material

that can be used to produce activated carbon by chemical activation and ZnCl2 showed to be the

best chemical activation agent based on the highest BET surface area (780 m2/g in the best case)

and pore volume (0.58 m3/g in the best case), the lowest ash content (6.14% in the best case),

and the highest carbon content (86.1% in the best case), compared with others chemicals.

Carbons activated by ZnCl2 are capable to adsorb As(V), getting As(V) removal levels up to

80% in less than 1 hour in the experimental conditions applied (initial pH 6-7, activated carbon

concentration 0.1 g/l and 0.5 g/l, initial As concentration 100 ppb).

Gallardo and Tanala (2012) conducted a study that describes a method to decrease the

incidence of diseases caused by pesticides, heavy metals, and bacteria through a simple, low-

cost, and sustainable personal water purification solution for the citizens of Nagcarlan, Laguna in

the Philippines. Activated carbon (AC) adsorption was the primary treatment used in the removal

of methomyl, a carbamate pesticide, and hexavalent chromium (Cr(VI)), a heavy metal. Also,

citricidal was used to disinfect water from coliforms. Surface hydroxyl with aliphatic and

aromatic groups from the AC, were confirmed using Fourier transform infrared (FTIR)

spectroscopy. The activated carbon used in this study was produced from coconut shell through

the process developed by the Industrial Technology Development Institute (ITDI) under the

Department of Science and Technology (DOST) in the Philippines.

According to Demafelis and Matibag (2001), technologies are currently being developed

to treat wastewater so that the water can be used again. Production of activated carbon (AC)

from agricultural by-products is a good example of this technology. AC is a very fine form of
carbon used in various industrial processes such as the removal of unwanted colors and odors,

recovery of solvent vapors, purification of water, and removal of obnoxious, toxic, or unwanted

gases and vapors. The problem is how to produce activated carbon efficiently and cheaply,

hence, the studies on the coconut shell, as waste product in copra making. AC was produced by

pulverizing the coconut shell and treating the powder with ammonium chloride (NH4Cl) from

one hour at different temperature settings (400, 600, and 800 degrees C) and at different NH4Cl-

shell ratios (1:4, 1:6, 1:8). For activation, a device called pyrolyzer was used. The device was a

local prototype adapted from a Japanese design. Based on the amount of carbon produced and

the capability of the activated carbon to decolorize wastewater, the best treatment combination

for producing activated carbon from coconut shell is at a temperature setting of 800 degrees C

and a NH4Cl-shell ratio of 1:4.

Synthesis

The study made by Roopa D. (2016) produced activated carbon to treat waste water. The

difference is that orange peel is used as the raw materials. This work explores the feasibility of

bitter orange, a biomass as an alternative precursor for preparation of activated carbon with

sulphuric acid activation (H2SO4) as activating agent at relatively low temperatures such as 90,

120, and 150 were used to produce different activated Carbons and finally 150C for 30min were

used for the study purposes.

Another study by Fernandez et al. (2014) produced activated carbon for waste water

treatment. The difference is activated carbon from orange (Citrus sinensis) peel was developed

through H3PO4 acid activation. Its ability as an adsorbent for the removal of two representative

basic dyes (methylene blue and rhodamine B) from single and binary dyes solutions in batch and

continuous modes was examined.


Findings made by Mohammad et al. (2015) produce activated carbon to treat waste water.

The difference is that this study was conducted to investigate the removal of cadmium (II) from

aqueous solution by using low cost, natural and eco-friendly biosorbent of Banana peels

Activated Carbon (BPAC) through batch experiments. The study made by Mahanim et al. (2010)

also produced activated carbon for waste water treatment. The difference is that the instead of

using calamansi peel, the researchers used bamboo residues using carbonization and steam

activation in a high temperature reactor.

On the other hand, the study by Panyathanmaporn et al. (2008) difference is the

production of activated carbon from coconut shell treated with phosphoric acid (H3PO4) was

optimized using the response surface methodology (RSM). Fifteen combinations of the three

variables namely; impregnation ratio (1, 1.5, and 2); activation time (10, 20, and 30 min); and

activation temperature (400, 450, and 500 °C) were optimized based on the responses evaluated

(yield, bulk density, average pore diameter, small pore diameter, and number of pores in a unit

area).

For the local setting, study conducted by Villarante et al. (2017) shows the production of

bio absorbent for waste water treatment. The difference is that the raw materials that are used is

Lumbang. Same goes with the study made by Lizardo (2007), the difference is the use of maize

cob, coconut sawdust, and dalandan peels as raw materials while carbonized and treated with

H3PO4 (85%w) as activating agent instead of using calamansi peel treated in sulfuric acid. The

study made by Cruz (2012) is producing activated carbon to treat waste water. The difference is

that cocoa pod husk was used and treated in three chemical activation agents (K2CO3, KOH and

ZnCl2) as activating agent instead of using calamansi peel treated in sulfuric acid.
Gallardo et al. (2012) conducted a study with the same goal of this study, and that is to

produce activated carbon for waste water treatment. The only difference is that the activated

carbon used in this study was produced from coconut shell through the process developed by the

Industrial Technology Development Institute.

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