Preliminary Study on the Use of Activated Corn

Husk on Simulated Nitrate and Phosphate Waters

by

Laurence Clair O. Alaban

Jerrold M. Belandres
Jerzy Rhein A. Custodio

A Research Paper Submitted to the Mapúa Senior High School Office

in Partial Fulfillment of the Requirements for

Research Project (RES04)

Mapúa University
May 2020
 APPROVAL SHEET

This is to certify that we have supervised the preparation of and read the research paper
prepared by Laurence Clair O. Alaban, Jerrold M. Belandres, and Jerzy Rhein A.
Custodio entitled Preliminary Study on the Use of Activated Corn Husk on Simulated
Nitrates and Phosphate Waters and that the said research paper has been submitted for
final approval by the Oral Examination Committee.

Kathleen Faye A. Lagasca Irah Nathanne D. Tiburcio

Thesis Coordinator Thesis Adviser

As members of the Oral Examination Committee, we certify that we have examined this
research paper and hereby recommend that it be accepted as fulfillment of the research
requirement for the Senior High School – Science, Technology, Engineering, and
Mathematics (STEM).

Kris Andrew D. Borero Charlene L. Jadia

Panel Member Panel Member

Ardvin Kester S. Ong

Committee Chairman

This research paper is hereby approved and accepted by the Mapúa Senior High School as
fulfillment of the research requirement for the Senior High School – Science, Technology,
Engineering, and Mathematics (STEM).

Dr. Lilibeth D. Sabino

Principal

ii
 ACKNOWLEDGEMENT

My deepest ‘thank you’ LORD for all the gifts You have given me and for directing my path
to the following persons who have been instrumental in the completion of my thesis /
practicum or research report.

To our family, for giving endless support, for being considerate while we do our research
and for giving financial support to the group.

To IS223, our classmates, for showing support and encouragement.

To Kathleen Faye Lagasca, our RES02 and RES04 professor, for giving guidance and for
showing support and consideration. For giving guidance, providing opportunities to improve,
and for always being patient with us.

To Mr. Irah Nathanne Tiburcio, the center source of all our knowledge poured into this
research, our research adviser, for guiding us and helping us through each and every hardship
we encountered. he is a good mentor who motivates and pursues us to finish and give our
best shot in every part of our research study. On top of everything else, he stood out from all
the course advisers by always making sure that we are clearly heard and understood in all
circumstances, despite the circumstances.

To the Lord Almighty, for providing us the strength and knowledge to be able to do this
research project. For giving us patience and leading us to the right direction. All Glory and
Honor in Your Name.

Laurence Clair O. Alaban

Jerrold M. Belandres
Jerzy Rhein A. Custodio
 TABLE OF CONTENTS

TITLE PAGE i

APPROVAL PAGE ii

ACKNOWLEDGEMENT iii

TABLE OF CONTENTS iv

LIST OF TABLES vi

LIST OF FIGURES vii

ABSTRACT viii

Chapter 1: INTRODUCTION 1

Chapter 2: REVIEW OF LITERATURE 4

Eutrophication 4
Phosphates 4
Nitrates 5
Adsorption 6
Corn 7
Corn Husk Adsorbents 7
Wastewater 8

Chapter 3: PRELIMINARY STUDY ON THE USE OF ACTIVATED CORN HUSK

ON SIMULATED NITRATE AND PHOSPHATE WATERS 9

Abstract 　　

Introduction 9

Methodology 12

Gathering and Preparation of Corn husk 13

Adsorbent Activation 13
Simulated Water Preparation 13

iv
 Results and Discussion 14

Nitrate and Phosphate Testing before and after Adsorption 15

Statistical Analysis 15

Conclusion 16

References 17

Chapter 4: CONCLUSION 19

Chapter 5: RECOMMENDATION 20

REFERENCES 21

APPENDICES 22

v
 LIST OF TABLES

Chapter 3
TABLE 1. NITRATE AND PHOSPHATE CONCENTRATIONS BEFORE AND
AFTER ADSORPTION 12

Appendices
TABLE 2. t-TEST: TWO-SAMPLE ASSUMING EQUAL VARIANCES 27

vi
 LIST OF FIGURES

Chapter 3
FIGURE 1. FLOW DIAGRAM 12

Appendices
FIGURE 1. WASHING AND PREPARATION OF MATERIALS FOR EXPERIMENT 23
FIGURE 2. PULVERIZATION OF ACTIVATED CORN HUSKS 23
FIGURE 3. SODIUM NITRATE (LEFT) AND SODIUM PHOSPHATE (RIGHT)
SALTS 24
FIGURE 4. PREPARATION OF SIMULATED NITRATE AND PHOSPHATE
WATERS 24
FIGURE 5. BATCH ADSORPTION USING AN ORBITAL SHAKER FOR 1 HOUR 25
FIGURE 6. FILTRATION OF THE ADSORBED SIMULATED WATERS 25
FIGURE 7. TEST KIT INSTRUCTIONS FOR PHOSPHATE (LEFT) AND
NITRATE (RIGHT) CONCENTRATIONS 25
FIGURE 8. PHOSPHATE CONCENTRATION (LEFT) AND NITRATE
CONCENTRATION (RIGHT) BEFORE ADSORPTION 26
FIGURE 9. PHOSPHATE CONCENTRATION (LEFT) AND NITRATE
CONCENTRATION (RIGHT) AFTER ADSORPTION 26

vii
 ABSTRACT

Eutrophication has devastating effects on marine life and is main cause of algal
blooms in water bodies. Its prevention is highly attributed to a low nutritional value for the
algae. These nutrients, which are most commonly phosphates and nitrates, need to be
removed and many processes are available such as adsorption, absorption, filtration, and
many more. For this research, the determination of the effect on the concentrations of nitrate
and phosphate on simulated waters using activated corn husks was done via adsorption
process. The husks were thermally activated in an oven and then powdered until fine.
Simulated nitrate and phosphate waters were prepared using sodium nitrate and sodium
phosphate, respectively. The range of the concentrations of nitrates and phosphates were
analyzed using respective test kits and the before and after concentrations were compared
after using 1 gram of the corn husk adsorbent in each sample of the simulated waters. Due to
the CoVid-19 crisis, the experimentation was halted and only preliminary results were
obtained. It was found that using only 1 gram of adsorbent may not give any noticeable
change in the concentrations of the nitrates and phosphates and thus, it is recommended for
future researchers to have increased adsorbent dose.

Keywords: Phosphate, Nitrate, Adsorption, Corn Husk

viii
 Chapter 1

INTRODUCTION

Phosphates and nitrates are two of the most important nutrients plants need in order to

grow and survive. The two chemicals are limiting factors for some plants especially in

freshwater ecosystems (Nur, 2014). Many industrial plants also need phosphates as a main

component in their manufacturing and its excessive use can become a source of phosphate

contamination in their wastewaters. Households, mining activities, industrial and agricultural

plants, and even municipal wastewaters have also released phosphates into bodies of water

(Hussain et al., 2011; Paleka & Deliyanni, 2009; Xu et al., 2010). On the same trend in recent

years, according to Ward et al. (2018), the levels of nitrate in the water resources have also

grown in many areas because of the use of inorganic fertilizers and animal manure in

agricultural areas. Excess phosphates and nitrates can help in a water phenomenon known as

eutrophication. Eutrophication occurs when high levels of nutrients such as phosphates,

nitrates, and others help in the growth of algae and other microorganisms. These growths will

constitute to a huge roof on top of the water body, shielding sunlight from the organisms

below. Insufficient sunlight may cause plants and some animals dependent on it to wither and

die. Thus, a need to remove these nutrients from bodies of water is a must (Nur, 2014).

In a study by Bakshi, Verma, and Dash (2019), phosphate is a food source of algae,

bacteria, and other microorganisms that can lead to fish kill because they compete with

oxygen and may be the cause of eutrophication. The two major sources of phosphates in

bodies of waters are human wastes and industrial wastes that lead to increased phosphate

concentrations. Thus, Bakshi, Verma, and Dash used a successful way for removing these

1
phosphates: electrocoagulation and modeled the results. On the research of Kalaruban

(2017), elevated nitrate concentrations in surface and groundwater can pose a threat to human

health especially to infants by causing “blue baby syndrome” when the water was drunk. He

thus used an anion exchange resin labelled Dowex 21K XLT in near neutral pH in order to

adsorb nitrate.

Corn husks have been known to be potential antecedents for preparing activated

carbons because of their high carbon and low ash contents. Activated carbon is a common

adsorbent for many applications, including wastewater adsorption. Corn husks are also

examples of large-scale agricultural waste produced annually which can be converted into

activated carbon with the capacity to remove different kinds of pollutants (Guan, Latif, &

Yap, 2013). Due to the success in using activated corn husk, an easily accessible agricultural

waste material, there may be a possible use of the adsorptive capability of corn husk in the

cleansing of wastewaters. There are still no studies conducted when it comes to determining

its effect on phosphate and nitrate concentrations which is why a preliminary study done on

simulated waters is essential.

This preliminary study would try to determine the possible effect of adsorption via

activated corn husks when subjected in simulated water samples containing both nitrates and

phosphates. The resulting activated corn husks shall be used in order to determine the effect

on the two pollutants. Solutions containing phosphate concentrations prepared from sodium

phosphate and nitrate concentrations prepared from sodium nitrate shall be analyzed. Simple

phosphate and nitrate test kits shall be used for the analysis, both of which may be purchased

from aquarium and fish shops.

2
 Removal of phosphates and nitrates from water may help reduce the instances of

eutrophication. For nitrates, the effects at high concentrations were colorectal cancer,

bladder, and breast cancer, and thyroid diseases (Ward et al., 2018) . On the other hand, an

enormous quantity of phosphorus is present in wastewater in the form of phosphates may be

recycled. If this phosphorus content is recovered, it can be used to meet the phosphorus needs

of industries and agriculture, to compensate for the global exhaustion of high-grade

phosphate ores which are used in many agricultural and industrial applications.

The research only focuses on the adsorptive capability of corn husks on only two

contaminants namely phosphate and nitrate. Adsorption is the only process that will be

executed, and the activation shall be done using a simple furnace at a certain temperature.

The study will not employ natural wastewater from agricultural and industrial plants rather a

simulation of these waters shall be done using sodium phosphate and sodium nitrate. No

other pollutants shall be analyzed and no other adsorbents shall be used. Only three trials

shall be done for the adsorption process and the concentration determination as adapted from

Ko, Phyo, & Ni, (2018) and the results of the trials were compared via t-Test statistical

analysis. No other parameters were varied such as temperature, humidity, pressure, etc. and

the experiment shall only be accomplished under ambient conditions.

3
 Chapter 2

REVIEW OF LITERATURE

Eutrophication

Bakshi, Verma, and Dash (2019) stated that phosphate is a good food source of algae,

bacteria, and many other microorganisms. However, these microorganisms, when in large

population, may compete with the oxygen in the water in phenomenon known as

Eutrophication, and may lead to plant and fish kill.

Kobeti & Robert (2019) stated that in the increased biomass, physico-chemical

properties of the surrounding environment may change and thus can result in hypoxia and

death of the biota. There are two types of eutrophication: natural eutrophication and artificial

eutrophication. Natural eutrophication comes from soils and dead animals when surface run-

off occurs. Artificial eutrophication, on the other hand, is man-made. The two main sources

of artificial phosphates in bodies of waters are human and industrial wastes. Kalaruban

(2017) on the other hand said that elevated nitrate concentrations in surface and groundwater

may cause also eutrophication in natural water bodies. This can become a danger to human

health, especially to infants by causing “blue baby syndrome”.

Eutrophication is thus a major concern for all ecosystems. Anthropogenic sources of

these dangerous components, together with heavy metals, may be resolved by many means

such as electroplating, adsorption, and filtration (Gallagher et al. 1990; Reed et al. 1994).

Phosphates

The major component of phosphates as a nutrient for plants is the Phosphorus. It is an

element in food production and was introduced during the mid-20 th century for agricultural

4
uses. Phosphate fertilizers were the mined from phosphate rocks and both are decreasing in

terms of quantity and quality at an alarming rate. The China and US are recently controlling

the remaining phosphate rocks in order to properly regulate the crisis. Tervahauta (2014)

proposed a solution: sanitation. Here, the energy and the fertilizer are both successfully

recovered in black water that was collected in vacuum in order to be reused again.

As of now, there are no alternative sources of phosphorus in the market that could replace the

recent global manufacture of 20 million 15 tons (Mt) of phosphorus from phosphate rock.

While phosphorus shortage is likely to be one of the greatest challenges of the 21 st century, it

is possible to prevent this crisis with the help of government and societal action (Cordell et

al., 2011).

Nitrates

Poon (2013) stated that nitrates are the primary component of some fertilizers in

farms, but the pollution of nitrate in aquatic environment and surface water has become a

serious concern. Although nitrate has known harmful effects, it was used before as medicine.

It was used to cure some ailments such as lack of appetite, kidney stones, and as prophylactic

against smallpox and even the bubonic plague, and treatment for angina (chest pain).

Adsorption

Adsorption is one simple and effective way in removing different pollutants in soils,

wastewater, and even air. Fan & Zhang (2018) created adsorbents from raw corn stalks. It

was modified and characterized in terms of thermogravimetric analysis, elemental analysis,

surface analysis using scanning electron microscopy–energy dispersive spectrometry (SEM-

EDS) and chemical analysis using the Fourier transform infrared spectroscopy (FT-IR)

spectra. Another research by Kalaruban (2017) used an anion exchange resin known as

5
Dowex 21K XLT as its adsorbent media and was surface modified by incorporating Fe

(Dowex-Fe) to increase the surface positive charges and tested for removing nitrates in water

at neutral pH. According to Battas et al. (2019), their study is about the removal of nitrate

ions through adsorption by using local clay. They conducted a series of batch experiments to

test the effects of contact time, adsorbent characteristics, initial concentration of nitrate, pH

of the solution, concentration, and granulometry of adsorbent. The results of their experiment

claimed that the local clay was effective.

Corn

Corn comes from the same family as sugarcane and is a genus Zea vegetable. The

skin of the corn which are light, thin, and hairy that protects the kernel is known as its husk.

Corn husks are one of the large amounts of agricultural wastes and are sometimes reused for

multiple applications. Corn husks are potential precursors for preparing activated carbons

because of their high carbon and low ash content (Guan, Latif, & Yap, 2013).

Corn Husk Adsorbents

Ko, Phyo, & Ni (2018) fish sauce is an important product in most southeast Asian

countries. High sodium content chloride of fish sauce was reduced by a corn husk. The

activated Corn Husk has a potential economic on reducing the environmental impact. Corn

husk activated carbon was prepared by chemical activation method using zinc chloride

(ZnCl2) as activating agent. The effect of various preparation parameters such as

concentration of activating agent, carbonization temperature and carbonization time that

depend on characteristics of activated carbon. The result of the studies were the activated

carbon prepared by impregnation the precursor with 20% ZnCl 2, followed by carbonization at

250°C for 40 min., was selected as the appropriate condition due to the following good

6
characteristics of activated carbon: high surface area, high iodine sorption capacity, and the

results of the SEM analysis.

In the study by Tsai et al., (2001), activated carbons derived from corn husks were

prepared by using potassium salts and gasification of carbon dioxide. In their study, the main

factor that has an effect on an adsorbent’s total effective surface area is the exposition of its

carbon content, the component that has good adsorbing capacity. These agricultural wastes,

corn cobs, were activated by means of two processes: Chemical and Thermal activation. The

chemical activation was done using potassium hydroxide and potassium carbonate while

thermal activation was done by means of a furnace at a maximum of 800OC with increments

of 10 OC per minute for 4 hours. The experiment showed a higher adsorptive capacity when

activated. According to the study of Loh, Kai, & Li (2018), carbonization temperatures using

a furnace range from 600-900°C which causes formation of chart that is usually done on

nitrogenous atmosphere. Carbonization done is to eliminate large amounts of internal carbons

and volatile content so that the material obtained will have higher fixed carbon content for

activation.

Wastewaters

Phosphate Contamination

In a study of Nur (2014), phosphate contamination in water just like nitrate,

phosphate is a necessary nutrient for plants to survive and is a limiting factor in plant growth.

Phosphate is also an important chemical element for many industries and because of its

excessive use the wastes produced by these industries can be a major phosphate contaminant

in wastewaters. Domestic usage, mining companies, industrial and agricultural plants, and

municipal discharges may release phosphate into water bodies in the form of organic and

7
inorganic phosphates (Hussain et al., 2011; Paleka and Deliyanni, 2009; Xu et al., 2010a).

Like nitrate, the excess phosphate in water should be removed in order to control

eutrophication and maintain a sustainable green environment for future generations. To

control eutrophication, environmental protection agencies in many countries have

recommended that total phosphorus (P) should not exceed 0.005-0.1 mg P/L in natural water

bodies and must be regulated in its use.

Nitrate Contamination

Nitrates and nitrites from water can result in the creation of N-nitroso compounds in

the presence of nitrosatable precursors that are contained in meats, fish and some common

drugs when drank. These are carcinogenic and may be a precursor to other diseases. As

stated by Poon (2013), in terms of toxic elements, nitrate has a weaker effect compared to

other toxic elements. Nitrate warrants our attention because it may affect our health and well-

being when ingested in higher concentrations. Removing these nitrates from water to avoid

any contamination that may cause harm to humans and ecosystems are of primary

importance.

8
 Chapter 3

PRELIMINARY STUDY ON THE USE OF ACTIVATED CORN HUSK ON

SIMULATED NITRATE AND PHOSPHATE WATERS

Abstract

Eutrophication has devastating effects on marine life and is main cause of algal
blooms in water bodies. Its prevention is highly attributed to a low nutritional value for the
algae. These nutrients, which are most commonly phosphates and nitrates, need to be
removed and many processes are available such as adsorption, absorption, filtration, and
many more. For this research, the determination of the effect on the concentrations of nitrate
and phosphate on simulated waters using activated corn husks was done via adsorption
process. The husks were thermally activated in an oven and then powdered until fine.
Simulated nitrate and phosphate waters were prepared using sodium nitrate and sodium
phosphate, respectively. The range of the concentrations of nitrates and phosphates were
analyzed using respective test kits and the before and after concentrations were compared
after using 1 gram of the corn husk adsorbent in each sample of the simulated waters. Due to
the CoVid-19 crisis, the experimentation was halted and only preliminary results were
obtained. It was found that using only 1 gram of adsorbent may not give any noticeable
change in the concentrations of the nitrates and phosphates and thus, it is recommended for
future researchers to have increased adsorbent dose.

Keywords: Phosphate, Nitrate, Adsorption, Corn Husk

Introduction

Phosphates and nitrates are two of the most important nutrients plants need in order to

grow and survive. The two chemicals are limiting factors for some plants especially in

freshwater ecosystems (Nur, 2014). Many industrial plants also need phosphates as a main

component in their manufacturing and its excessive use can become a source of phosphate

contamination in their wastewaters. Households, mining activities, industrial and agricultural

plants, and even municipal wastewaters have also released phosphates into bodies of water

(Hussain et al., 2011; Paleka & Deliyanni, 2009; Xu et al., 2010). On the same trend in recent

years, according to Ward et al. (2018), the levels of nitrate in the water resources have also

grown in many areas because of the use of inorganic fertilizers and animal manure in

9
agricultural areas. Excess phosphates and nitrates can help in a water phenomenon known as

eutrophication. Eutrophication occurs when high levels of nutrients such as phosphates,

nitrates, and others help in the growth of algae and other microorganisms. These growths will

constitute to a huge roof on top of the water body, shielding sunlight from the organisms

below. Insufficient sunlight may cause plants and some animals dependent on it to wither and

die. Thus, a need to remove these nutrients from bodies of water is a must (Nur, 2014).

In a study by Bakshi, Verma, and Dash (2019), phosphate is a food source of algae,

bacteria, and other microorganisms that can lead to fish kill because they compete with

oxygen and may be the cause of eutrophication. The two major sources of phosphates in

bodies of waters are human wastes and industrial wastes that lead to increased phosphate

concentrations. Thus, Bakshi, Verma, and Dash used a successful way for removing these

phosphates: electrocoagulation and modeled the results. On the research of Kalaruban

(2017), elevated nitrate concentrations in surface and groundwater can pose a threat to human

health especially to infants by causing “blue baby syndrome” when the water was drunk. He

thus used an anion exchange resin labelled Dowex 21K XLT in near neutral pH in order to

adsorb nitrate.

Corn husks have been known to be potential antecedents for preparing activated

carbons because of their high carbon and low ash contents. Activated carbon is a common

adsorbent for many applications, including wastewater adsorption. Corn husks are also

examples of large-scale agricultural waste produced annually which can be converted into

activated carbon with the capacity to remove different kinds of pollutants (Guan, Latif, &

Yap, 2013). Due to the success in using activated corn husk, an easily accessible agricultural

waste material, there may be a possible use of the adsorptive capability of corn husk in the

10
cleansing of wastewaters. There are still no studies conducted when it comes to determining

its effect on phosphate and nitrate concentrations which is why a preliminary study done on

simulated waters is essential.

This preliminary study would try to determine the possible effect of adsorption via

activated corn husks when subjected in simulated water samples containing both nitrates and

phosphates. The resulting activated corn husks shall be used in order to determine the effect

on the two pollutants. Solutions containing phosphate concentrations prepared from sodium

phosphate and nitrate concentrations prepared from sodium nitrate shall be analyzed. Simple

phosphate and nitrate test kits shall be used for the analysis, both of which may be purchased

from aquarium and fish shops.

Removal of phosphates and nitrates from water may help reduce the instances of

eutrophication. For nitrates, the effects at high concentrations were colorectal cancer,

bladder, and breast cancer, and thyroid diseases (Ward et al., 2018) . On the other hand, an

enormous quantity of phosphorus is present in wastewater in the form of phosphates may be

recycled. If this phosphorus content is recovered, it can be used to meet the phosphorus needs

of industries and agriculture, to compensate for the global exhaustion of high-grade

phosphate ores which are used in many agricultural and industrial applications.

The research only focuses on the adsorptive capability of corn husks on only two

contaminants namely phosphate and nitrate. Adsorption is the only process that will be

executed, and the activation shall be done using a simple furnace at a certain temperature.

The study will not employ natural wastewater from agricultural and industrial plants rather a

simulation of these waters shall be done using sodium phosphate and sodium nitrate. No

other pollutants shall be analyzed and no other adsorbents shall be used. Only three trials

11
shall be done for the adsorption process and the concentration determination as adapted from

Ko, Phyo, & Ni, (2018) and the results of the trials were compared via t-Test statistical

analysis. No other parameters were varied such as temperature, humidity, pressure, etc. and

the experiment shall only be accomplished under ambient conditions.

Methodology

Experimental Process

Gathering Corn Husk

↓
Drying Corn Husk for 24 hours in an oven
↓
Pulverization of Corn Husk
↓
Thermal Activation
↓
Making of simulated nitrate and phosphate water
↓
Nitrate and Phosphate Content before Adsorption
↓
Adsorption Process
↓
Nitrate and Phosphate Content after Adsorption
↓
Statistical Analysis and Interpretation
Figure 1. Experimental Process

Gathering and Preparation of Corn Husks

Figure 1 shows the nine steps that this research adapted from the study of Sengupta

and Balomajunder, (2014). A sack of corn husks was gathered from corn suppliers from

Cainta, Rizal. The corn husks were washed with distilled water to remove impurities. The

12
husks were then oven dried at 50oC for 24 hours (Ko, Phyo, & Ni, 2018). The dry husks were

cut into small pieces using scissors and then blended using a small personal blender in order

to pulverize the corn husks.

Adsorbent Activation

The powdered corn husks were activated at a temperature of 600 oC for two hours and

then cooled to room temperature overnight. The now activated corn husks were then weighed

using a digital weighing scale to determine the amount of activated adsorbent produced (Loh

& Li, 2018).

Simulated Water Preparation

In order to create the simulated water containing the Nitrate and Phosphate pollutants,

one liter of 40ppm (parts per million) Nitrate simulated water and one liter of 10ppm

Phosphate simulated water solutions were prepared from sodium nitrate (NaNO 3) and sodium

phosphate (Na3PO4) on separate 1 L volumetric flasks respectively.

Nitrate and Phosphate Testing before Adsorption

Two test kits were purchased from nearby aquarium shops: Nitrate Test Kit and

Phosphate Test Kit. The initial nitrate concentration of the simulated nitrate water was tested

using a nitrate test kit. The initial phosphate concentration was also tested, however, using

the phosphate test kit this time. The instructions in the manual for the given test kits were

strictly followed and then recorded in Table 1.

Adsorption Process

The adsorption process was done by having multiple adsorbent to simulated water

mass ratios. This process was adapted from Banu, Karthikeyan, and Meenakshi (2019).

50mL of the respective phosphate and nitrate solutions were placed in separate 50mL

13
Erlenmeyer flasks using a pipette. 0.1g of the activated corn husk adsorbents were placed

inside the two flasks and were placed in an orbital shaker at 125 rpm for 1 hour (De & Maiti,

2012). The resulting adsorbed solutions were filtered out using a Whatman filter paper to

remove the adsorbents and then transferred to another 50 mL Erlenmeyer flask for later

testing. The same process was done two more times for the three-trial requirement and

recorded in Table 1.

Nitrate and Phosphate Testing after Adsorption

The same process for the phosphate and nitrate testing was done for the adsorbed

mixtures in order to test the after-adsorption nitrate and phosphate concentrations. The

concentrations were recorded in Table 1. The percentage reduction for both concentrations

was calculated using Equation 1.

Initial Concentration-Final Concentration

% Reduction= x 100% (Eq. 1)
Initial Concentration

Statistical Analysis – Independent t-Test for Two Samples

Essentially, a t-test is a hypothesis testing statistic which allows us to compare the

average values of the two data sets and test whether the two values are related. In this study,

an Independent t-Test for Two Samples was utilized in order to determine the relationship

between the acquired percentage reductions in the concentrations of nitrates and phosphates.

For this statistic, the null hypothesis (H o) predicts that the mean of the percentage reduction

in nitrate concentration is the same as the mean of the percentage reduction in phosphate

concentration while the alternative hypothesis (HA) predicts that the means of the

aforementioned percentage reduction in concentrations have different means:

14
 H o : μnitrate = μ phosphate

H A : μnitrate ≠ μphosphate

Results and Discussion

In this preliminary study, a single initial concentration of the pollutants was

tested. Although further tests were planned at lesser concentrations, the CoVid-19

crisis ended these future experiment plans. In Figure 8 (Appendix A), the actual

picture of the initial color range concentration of both the nitrate and phosphate

simulated waters is shown. Figure 9, on the other hand, shows the final color range

concentration after adsorption. By analyzing the closeness of the colors to the color

palette of the test kits, the initial and final concentrations for the simulated and

adsorbed phosphate water stayed at 10.0ppm while for the nitrate water, it stayed at

40.0ppm. Table 1 presents the results for the three trials adsorption at 40.0ppm

initial concentration of simulated nitrate solution and 10.0ppm initial concentration

of simulated phosphate solution.

Table 1. Nitrate and Phosphate Concentrations Before and After Adsorption

Nitrate Concentrations
Treatment: Before After % Reduction
Trial 1 40.0 ppm 40.0 ppm 0%
Trial 2 40.0 ppm 40.0 ppm 0%
Trial 3 40.0 ppm 40.0 ppm 0%
Average % Reduction: 0%
Phosphate Concentrations
Treatment: Before After % Reduction
Trial 1 10.0 ppm 10.0 ppm 0%
Trial 2 10.0 ppm 10.0 ppm 0%
Trial 3 10.0 ppm 10.0 ppm 0%

15
 Average % Reduction: 0%
After a batch adsorption for 1 hour, the final concentrations of both nitrates

and phosphates stayed the same for all three trials, giving out a 0% reduction in

concentration, thus showing that there was no change in the initial and final

concentrations in both nitrate and phosphate simulated water samples. For further

analysis, Table 2 in Appendix B shows the t-Test Statistical Analysis to compare

the means between the percentage reductions in the concentrations of nitrates and

phosphates. From the resulting t-Test Statistic, the p-value calculated was

undefined. This happened since the formula contained a fraction with a

denominator of zero. The comparison using t-Test cannot be defined in this case

since both the percentage reduction in concentration of both the nitrate and the

phosphate simulated waters were zero.

There are multiple possible reasons as to why there were no change in the

concentrations of the nitrates and phosphates in the simulated waters. One possible

reason would be the activation temperature which was limited to a maximum of

600oC using the available furnace in the laboratory. In the study conducted by

Guan, Latif, and Yap (2013), their activation temperature was 800 oC. This higher

temperature may have exposed a carbon surface that could have better affinity in

adsorbing the nitrates and the phosphates. In the same study of Guan, Latif, and

Yap (2013), they also carbonized their sample corn husk under a nitrogen

atmosphere, ensuring inert conditions. Since the corn husk in this study was

carbonized at ambient atmosphere, there may have been chemical reactions to

compounds present in the air that could have affected the adsorption capabilities of

the corn husk. Another possible reason for the unchanging phosphate and nitrate

16
 concentrations could be the amount of the adsorbent used. In this study, the amount

of adsorbent used was only 0.1g in 50mL of simulated water as adapted from Banu,

Karthikeyan, and Meenakshi (2019). This gives an adsorbent to adsorbate weight

ratio of 1:500 (%wt/wt). However, it is possible that this amount may not have been

enough in the experimental set-up to make noticeable changes in the concentrations

after adsorption. A study by Ko, Phyo, and Ni (2018) has optimized their adsorbent

to adsorbate weight ratio at 1:50 (%wt/wt) in their adsorption set-up. This would

entail the use of 1g instead of 0.1g to 50mL of simulated nitrate and phosphate

waters. Lastly, the contact time for the adsorbent in the simulated waters may also

be an important factor that may have affected the results. This study, the contact

time of De and Maiti (2012) at 1 hour and 125 rpm was adapted. In the study of

Sengupta and Balomajumder (2014), they actually optimized the contact time of

their corn husk adsorbent between 30 to 50 hours at the same rpm for phenol and

cyanide. Future studies may adapt the increased adsorption time in order to possible

show more noticeable changes in the concentrations of nitrate and phosphate.

Conclusion

The result from the preliminary study showed that the activated corn husk adsorbent

was not effective in reducing the concentrations of nitrate and phosphate in simulated waters.

Due to this, the t-Test Statistical Analysis gave an undefined p-value, making the resulting

data impossible to statistically compare. The possible factors that may have affected the

results could have been the low activation temperature, the activation atmosphere, the low

adsorbent dosage of 0.1g, and the small contact time of just 1 hour. An increase in the

activation temperature from 600oC to 800oC at inert nitrogen atmosphere may help improve

17
its adsorption capacity. Furthermore, an increase in the adsorbent dose from 0.1g to 1g and

contact time from 1 hour to time exceeding 30 hours may also help improve the adsorption

data for this study.

References

Bakshi, A., Verma, A. K., & Dash, A. K. (2019). Optimization using Response Surface
Behavior Techno-economic. Journal of Cleaner Production. Retrieved from:
https://doi.org/ 10.1016/j.jclepro.2019.118988

Banu, H. A. T., Karthikeyan, P., & Meenakshi, S., (2019). Comparative studies on revival of
nitrate and phosphate ions using quaternized corn husk and jackfruit peel.
https://doi.org/10.1016/j.biteb.2019.100331

De, S., and Maiti, A., (2012) Arsenic removal from Contaminated Groundwater. New Delhi:
The Energy and Resources Institute (TERI). 19

Fan, C., & Zhang, Y. (2018). Adsorption isotherms , kinetics and thermodynamics of nitrate
and phosphate in binary systems on a novel adsorbent derived from corn stalks. Journal
of Geochemical Exploration, 188(September 2017), 95–100. https://doi.org/10.1016/
j.gexplo.2018.01.020

Guan, B., Latif, P., & Yap, T., (2013) Physical Preparation of Activated Carbon from
Sugarcane Bagasse and Corn Husk and its Physical and Chemical characteristics Int. J.
Engg. Res. And sci and tech. Vol. 02, No. 3 pp. 1-4

Guin, J. P., Bhardwaj, Y. K., & Varshney, L. (2017). Radiation grafting: A voyage from bio-
waste corn husk to an efficient thermostable adsorbent.

Kalaruban, M., Loganathan, P., Kandasamy, J., Vigneswaran, S., (2017). Submerged
Membrane Adsorption Hybrid System using four Adsorbents in removing Nitrate from
Water. Environmental Science and Pollution Research, 1-8.

Ko, T. L., Phyo, S. W., & Ni, K. T. (2018). Effectiveness of prepared corn husk activated
carbon on the abatement of sodium chloride content in fish sauce. Universal Journal of
Agricultural Research, 6(2), 91–97. https://doi.org/10.13189/ujar.2018.060206

Loh, X. J., Kai, D., & Li, Z. (2018). Functional materials from lignin: methods and advances.
London: World Scientific.

Nur, T. (2014). Nitrate, Phosphate and Fluoride removal from Water using Adsorption
process. , 65–71.

18
Paska, O., Pacurario, C., Muntean, S., (2011). Kinetic and Thermodynamic studies on
Methylene Blue Biosorption using Corn Husk. DOI:101039/c0xx00000x

Sengupta, P., & Balomajumder, C., (2014) Potential of Corn Husk leaves for the Coremoval
of Phenol and Cynide from Waste Water using Simultaneous Adsorption and
Biodegration N23191163 Vol. 03, Issue 02 pp. 700-706

Chapter 4

CONCLUSION

The result from the preliminary study showed that the activated corn husk adsorbent

was not effective in reducing the concentrations of nitrate and phosphate in simulated waters.

Due to this, the t-Test Statistical Analysis gave an undefined p-value, making the resulting

data impossible to statistically compare. The possible factors that may have affected the

results could have been the low activation temperature, the activation atmosphere, the low

adsorbent dosage of 0.1g, and the small contact time of just 1 hour. An increase in the

activation temperature from 600oC to 800oC at inert nitrogen atmosphere may help improve

its adsorption capacity. Furthermore, an increase in the adsorbent dose from 0.1g to 1g and

contact time from 1 hour to time exceeding 30 hours may also help improve the adsorption

data for this study.

19
 Chapter 5

RECOMMENDATION

In order to help future researchers find better results, the following adjustments in

their experimentation could be made: (a) an activation temperature of 800oC; (b) a nitrogen

atmosphere during the activation process; (c) an adsorbent dose of 1 gram or possibly higher;

and (d) a longer adsorption contact time at 30 hours or higher. These, based on adaptations in

previous studies, may help ensure that the adsorption process becomes noticeable and the

results become statistically comparable.

If the results become positive, the activated corn husks may be used on different

pollutants such as heavy metals for removal. If the adsorption parameters and conditions

have been optimized, the corn husk adsorbents may be also be used in aquarium set-ups in

order to help reduce the formation of algae for small scale applications. The wide prevention

of eutrophication in bodies of water with the help of these adsorbents may also be possible

for large scale application.

20
 REFERENCES

Bakshi, A., Verma, A. K., & Dash, A. K. (2019). Optimization using Response Surface
Behavior Techno-economic. Journal of Cleaner Production. Retrieved from:
https://doi.org/ 10.1016/j.jclepro.2019.118988

Banu, H. A. T., Karthikeyan, P., & Meenakshi, S., (2019). Comparative studies on revival of
nitrate and phosphate ions using quaternized corn husk and jackfruit peel.
https://doi.org/10.1016/j.biteb.2019.100331

De, S., and Maiti, A., (2012) Arsenic removal from Contaminated Groundwater. New Delhi:
The Energy and Resources Institute (TERI). 19

Fan, C., & Zhang, Y. (2018). Adsorption isotherms , kinetics and thermodynamics of nitrate
and phosphate in binary systems on a novel adsorbent derived from corn stalks. Journal
of Geochemical Exploration, 188(September 2017), 95–100. https://doi.org/10.1016/
j.gexplo.2018.01.020

Guan, B., Latif, P., & Yap, T., (2013) Physical Preparation of Activated Carbon from
Sugarcane Bagasse and Corn Husk and its Physical and Chemical characteristics Int. J.
Engg. Res. And sci and tech. Vol. 02, No. 3 pp. 1-4

Guin, J. P., Bhardwaj, Y. K., & Varshney, L. (2017). Radiation grafting: A voyage from bio-
waste corn husk to an efficient thermostable adsorbent.

Kalaruban, M., Loganathan, P., Kandasamy, J., Vigneswaran, S., (2017). Submerged
Membrane Adsorption Hybrid System using four Adsorbents in removing Nitrate from
Water. Environmental Science and Pollution Research, 1-8.

Ko, T. L., Phyo, S. W., & Ni, K. T. (2018). Effectiveness of prepared corn husk activated
carbon on the abatement of sodium chloride content in fish sauce. Universal Journal of
Agricultural Research, 6(2), 91–97. https://doi.org/10.13189/ujar.2018.060206

Loh, X. J., Kai, D., & Li, Z. (2018). Functional materials from lignin: methods and advances.
London: World Scientific.

Nur, T. (2014). Nitrate, Phosphate and Fluoride removal from Water using Adsorption
process. , 65–71.

Paska, O., Pacurario, C., Muntean, S., (2011). Kinetic and Thermodynamic studies on
Methylene Blue Biosorption using Corn Husk. DOI:101039/c0xx00000x

Sengupta, P., & Balomajumder, C., (2014) Potential of Corn Husk leaves for the Coremoval
of Phenol and Cynide from Waste Water using Simultaneous Adsorption and
Biodegration N23191163 Vol. 03, Issue 02 pp. 700-706

21
APPENDICES

22
 APPENDIX A
Experiment Pictures

Figure 1. Washing and preparation of materials for experiment

Figure 2. Pulverization of Activated Corn Husks

23
Figure 3. Sodium Nitrate (left) and Sodium Phosphate (right) salts

Figure 4. Preparation of Simulated Nitrate and Phosphate Waters

24
 Figure 5. Batch adsorption using an Orbital Shaker for 1 hour.

Figure 6. Filtration of the adsorbed simulated waters

Figure 7. Test kit instructions for Phosphate (left) and Nitrate (right) concentrations

25
Figure 8. Phosphate Concentration (left) and Nitrate Concentration (right) before adsorption.

Figure 9. Phosphate Concentration (left) and Nitrate Concentration (right) after adsorption.

Appendix B

26
 Independent t-Test Results

Table 2. t-Test: Two-Sample Assuming Equal Variances

  Variable 1 Variable 2
Mean 0 0

Variance 0 0

Observations 3 3

Pooled Variance 0

Hypothesized Mean Difference 0

df 4

t Stat 65535

P(T<=t) one-tail Undefined

t Critical one-tail 2.131846786

P(T<=t) two-tail Undefined

t Critical two-tail 2.776445105

27