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ABSTRACT

This research was carried out to improve the application of activated carbon which is one of the
fastest growing areas in environmental applications such as wastewater treatment due to the
increase in contamination of wastewater by heavy metals. The activated carbon was produced
from Apple of Sodom plant stem for the removal of heavy metal ions (Pb +2 and Ni+2) in the
hospital waste water sample. The precursor material was collected, washed, sundried and oven
dried at105° for 24 hours. The activated carbon produced was prepared by chemical activation
using nitric acid (HNO3) as activating agent. Proximate composition analysis (bulk density,
moisture content, ash content) of the activated carbon produced were determined and recorded
as 2.06g/ml, 26.5%, and 0.85% respectively. The initial concentrations of the heavy metal ions
(Pb+2 and Ni+2) present were determined and recorded as 2.915mg/L and 1.87mg/L respectively.
The final concentrations of the heavy metal ions (Pb +2 and Ni+2) present were determined and
recorded as 1.92mg/L and 1.02mg/L respectively. The amount of Pb +2 and Ni+2 absorbed is 7.08
and 11.625 respectively. The surface morphology as well as the surface functional groups
present were determined using the Scanning Electron Microscope (SEM) and Fourier Transform
Infrared (FTIR) spectroscopy equipment respectively.
Table of Contents

Title Page i

Declaration ii

Certification iii

Acknowledgement iv

Abstract v

CHAPTER ONE

1.0 INTRODUCTION - - - - - - - - 1

1.1 Aim of the Research - - - - - - - - 6

1.2 Objectives of the Research6

1.3 Scope of the Research7

CHAPTER TWO

2.0 LITERATURE REVIEW8

2.1 Heavy Metals8

2.1.1 The Occurrence of Heavy Metals in Nature9

2.1.2 Behavior of Heavy Metals in the Environment9

2.1.3 Uses of Heavy Metals10

2.1.4 Human Exposure & Health Hazards Associated with Heavy Metals10

2.2 Review of Instrumental Techniques for Metal Analysis12

2.2.1 Atomic Spectroscopy (AAS)12

2.2.2 Inductively Coupled Plasma (ICP)14


ii
2.2.3 Fourier Transform Infrared (FTIR)Spectroscopy14

2.2.4 Scanning Electron Microscopy (SEM)17

2.3 Activated Carbon20

2.4 Preparation of Activated Carbon21

2.4.1 Pyrolysis/Carbonization21

2.4.2 Activation22

2.5 Forms of Activated Carbon24

2.6 Application of Activated Carbon25

2.6.1 Gas-Phase Applications25

2.6.2 Liquid-Phase Applications26

2.7 Hospital wastewater27

CHAPTER THREE

3.0 MATERIALS AND METHOD28

3.1 Sample Collection and Pretreatment28

3.2 Carbonization and Chemical Activation28

3.3 Sample Characterization29

3.4Determination of Bulk Density30

3.5 Determination of Moisture Content30

3.6 Determination of Ash Content31

3.7 FTIR Analysis31

3.8 Determination of Heavy Metals31


iii
CHAPTER FOUR

4.0 RESULTS AND DISCUSSION33

4.1 Results33

4.2 Discussions43

CHAPTER FIVE

5.0 SUMMARY, CONCLUSION AND RECOMMENDATION46

5.1 Summary46

5.2 Conclusion46

5.3 Recommendation47

References48

iv
LIST OF TABLES

Table 4.1 Proximate composition results.

Table 4.2 Initial and Final Concentrations of the Metal ions present.

Table 4.3 Amount of Pb+2 and Ni+2 absorbed and percentage removed.

Table 4.4 FT-IR analysis wave numbers and corresponding functional groups present.

v
CHAPTER ONE

INTRODUCTION

Recently, carbon has been one of the magnificent elements which have revolutionized material

science. From carbon we obtain the best porous absorber (activated carbon) with excellent

properties for large spectrum of industrial applications (Gupta and Nayak,2012).

Activated Carbon (AC) is the common term used for a group of absorbing substances of

crystalline form, having a large internal pore structures that make the carbon a good absorbent.

These properties are obtained when a char is subjected to controlled gasification by oxidizing

gases, or when a raw material impregnated with dehydrating agents is subjected to carbonization

(Guo, J. and Lau, A.,2002).

Activated carbon, a widely used adsorbent in industrial processes, is composed of a microporous,

homogenous structure with high surface arca and shows radiation stability (Ahmad, I., 2005).

The process for producing efficient activated carbon is not completely investigated in developing

countries. Furthermore, there are many problems with the generation of used activated carbon

(Gupta and Nayak, 2012).

In this research, the local agricultural product used is Apple of Sodom (Calotropis procera) plant

stem to produce an activated carbon due to the availability and inexpensive material with high

carbon and low inorganic content.

By now, a lot of research has been done on to improve the application of activated carbon. One

of the fastest growing areas is in environmental applications such as wastewater treatment. In the

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treatment of wastewater, it is used for purification, decolorization and the removal of toxic

organics and heavy metal ions (B. Rao, and D. Singh,2007).

Waste materials that have been successfully used to manufacture activated carbon in the recent

past include sago waste (K. Kadirvelu, and C. Karthika, 2005), coir pith (C.Namasivayam, and S.

Kumar, 2001), orange peel (Khaled et al., 2009), coffee husk(Ahmad and Rahman, 2011), pine

sawdust (Gecgel and Kolancilar, 2012), rice husk(Yahaya et al., 2011), oil palm fruit fibre

(Bello, 2013), sugarcane dust (S. Khattri, and M.Singh, 1999), rubber wood sawdust (K.

Vasanth, and S. Sivanesan, 2007), moss peat (D.JohnWase et al., 1995) tea waste(E. Malkoc,and

Y. Nuhoglu,2006) and Coconut husk(Foo and Hameed,2012).

The importance of activated carbon cannot be over emphasized, thus leading to the search of

means for its production other than the known traditional methods, due to its applicability in all

or almost all of life's endeavors. The production of activated carbon from agricultural byproducts

has both economic and environmental effects, as it converts unwanted, low-value agricultural

waste to useful high-value adsorbent (Jankowska, H. et al,1991).

Since the second part of 20th century, there has been growing concern over the diverse effects of

heavy metals on humans and aquatic ecosystems. Environmental impact of heavy metals was

earlier mostly attributed to industrial sources. In recent years, metal production emissions have

decreased in many countries due to strict legislation, improved cleaning/purification technology

and altered industrial activities. Today and in the future, dissipate losses from consumption of

various metal containing goods are of most concern. Therefore, regulations for heavy metal

containing waste disposal have been tightened (European Commission,2002).

2
A significant part of the anthropogenic emissions of heavy metals ends up in wastewater. Major

industrial sources include surface treatment processes with elements such as Cd, Pb, Mn, Cu, Zn,

Cr, Hg, As, Fe and Ni, as well as industrial products that, at the end of their life are discharged in

wastes. For some applications which during the last decade have been phased out in some

countries, there may, however, today be significant differences in uses (Hui, K. et al.,2005).

Most common sources of heavy metals to waste and/or waste water are;

i. Minning and extraction; a significant part of the four heavy metals with mining waste

actually concerns the presence of the heavy metals in waste from extraction of other

metals like zinc, copper and nickel. It should however be kept in mind that mining

waste is generated independent of the subsequent application of the heavy metal.

ii. Primary smelting and processing; a minor part of the heavy metals will end up in

waste from the further processing of the metals.

iii. Use phase; a small part of the heavy metals may be lost from the products during use

by corrosion and wear. The lost material may be discharged to the environment or

end up in solid waste either as dust or indirectly via sewage sludge.

iv. Waste disposal; the main part of the heavy metals will still be present when the

discarded products are disposed off. The heavy metals will either be collected for

recycling or disposed off to municipal solid waste incinerators (MSWI) or landfills or

liquid waste. A minor part will be disposed of as chemical waste and recycled or land

filled via chemical waste treatment.

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v. Metallurgical industries. Actually, metal pollutants are neither generated nor

completely eliminated; they are only transferred from one source to another. Their

chemical forms may be changed or they are collected and immobilized not to reach

the human, animals or plants (European Commission, 2002).

The term bioavailability is more appropriate to define the potential toxicity of metallic elements

and their compounds. Bioavailability depends on biological parameters as well as the

physicochemical properties of metallic elements, their ions, and compounds. These in turn

depend upon the atomic structure of the metallic elements. Thus, any classification of the

metallic elements to be used in scientifically based legislation must itself be based on the

periodic table or some subdivision of it. In conclusion, heavy metals commonly used in industry

and generically toxic to animals and to aerobic and anaerobic processes, but all of them are not

dense or entirely metallic. Includes As, Cd, Cr, Cu, Pb, Hg, Ni, Se, Zn. All of them pose a

number of undesired properties that affect humans and the environment (Duffus, J.,2002).

Effluents from textile, leather, tannery, electroplating, galvanizing, pigment and dyes,

metallurgical and paint industries and other metal processing and refining operations at small and

large-scale sector contain considerable amounts of toxic metal ions (Ahluwalia, S. and Goyal, D.,

2007). The toxic metals and their ions are not only potential human health hazards but also to

other life forms. Toxic metal ions cause physical discomfort and sometimes life-threatening

illness including irreversible damage to vital body system (Malik, A., 2004). From the eco-

toxicological point of view, the most dangerous metals are mercury, lead, cadmium and

chromium (VI). Metal ions in the environment bioaccumulate and are biomagnified along the

food chain. Therefore, their toxic effect is more pronounced in animals at higher tropic levels.

4
Among commonly used heavy metals (III), Cu, Zn, Ni and V are comparatively less toxic than

Fe and Al. An effluent treatment facility within the industry discharging heavy metals

contaminated effluent will be more efficient than treating large volumes of mixed wastewater in

a general sewage treatment plant. Thus, it is beneficial to devise separate treatment procedures

for scavenging heavy metals from the industrial wastewater (K. Kadirvelu et al.,2001).

The analysis of wastewater for trace and heavy metal contamination is an important step in

ensuring human and environmental health. A variety of inorganic techniques can be used to

measure trace elements in waste water including flame atomic absorption spectrometry (FAAS)

and graphite furnace (or electrothermal) atomic absorption spectrometry (GFAAS) or ETAAS),

inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled

plasma mass spectrometry (ICP-MS).Depending upon the number of elements to be determined,

expected concentration range of analytes and the number of samples to be run, the most suitable

technique for business requirements can be chosen (Goyal, D.et al.2007).

In recent years, some new processes such as biosorption, neutralization, precipitation, ion

exchange, adsorption etc. Have been developed and extensively used for the heavy metal

removal from wastewater (K. Selvi, et al., 2001).

1.1 Aim of the Research

The aim of this research is to produce activated carbon from the local agricultural waste which is

Apple of Sodom (Calotropis procera) plant stem impregnated with 1M HNO3 for removal of

heavy Pb+2 and Ni+2 in hospital waste water.

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1.2 Objectives of the Research

This study was carried out with the following objectives:

i. To study the effect of chemical activation on the development of pore structure on

the activated carbon produced.

ii. To examine the characteristic of powdered activated carbon produced (i.e., proximate

analysis, adsorption capacity, surface morphology of activated carbon produced).

iii. To evaluate the potential application of locally produced activated carbon in removal

of Pb+2 and Ni+2 from wastewater.

1.3 Scope of the Research

This work focuses on the production and characterization of activated carbon produced from

Apple of Sodom. The raw material activated will be carbonized under certain temperature(0-

400°c) with control time (1hr).

In this research, the production and characterization of the activated carbon produced were

performed by using several analyses such as the elemental analysis, proximate analysis, pore size

analysis, surface functional groups analysis and adsorption capacity (Mohan, D.,2007).

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CHAPTER TWO

LITERATURE REVIEW

2.1 Heavy Metals

A metal of relatively high density (specific gravity greater than 5) or of high relative atomic

weight is defined as a heavy metal. The term "Heavy metals" is used to describe more than a

dozen elements that are metals or metalloids (Karvelas, M., 2003); e.g., chromium, arsenic,

cadmium, lead, mercury, manganese, etc. Because they cannot be degraded or destroyed, heavy

metals are persistent in all parts of the environment. Living organisms require varying amounts

of "heavy metals". Iron, cobalt, copper, manganese, molybdenum, and zinc are required by

humans. Excessive levels can be damaging to the organisms (Vogel's, 1989). Therefore, heavy

metals can be described as any metallic element that has a relatively high density and is toxic or

poisonous at low concentrations. Humans are also responsible for altering the chemical forms of

heavy metals released to the environment. Such alterations often affect a heavy metal's toxicity

by allowing it to bioaccumulate in plants and animals, bioconcentrate in the food chain, or attack

specific organs of the body. Bioaccumulation refers to an increase in the concentration of a metal

in a biological organism over time, compared to the normal concentration in the environment. In

small quantities, 289 certain heavy metals are nutritionally essential for a healthy life (e.g., iron,

copper, manganese, and zinc). Some of these are referred to as the trace elements (Demirbas, A.,

2008).

2.1.1 The Occurrence of Heavy Metals in Nature

Metals may be present as individual elements, and as organic and inorganic compounds. The

geosphere is the original source of all metals (except those that enter the atmosphere from space
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in the form of meteorites and cosmic dust). In the hydrosphere, metals occur as dissolved ions

and complexes, colloids, and suspended solids. In the atmosphere, metals may be present as

gaseous elements and compounds and as particulates and aerosols (Sag, Y., 2001). Gaseous and

particulate metals may be inhaled and solid and liquid (aqueous-phase) metals may be ingested

or absorbed, thereby entering the biosphere (Adrienne et al., 2008). In addition to being the

original source of all terrestrial metals, the geosphere may represent a sink for metals. A

reservoir may act as a catalyst for changes of state of metals and metal compounds, without

actually having incorporated those metals, as in the case of some biologically mediated reactions

(Volesky, B.,2007).

2.1.2 Behavior of heavy metals in the Environment

A number of biogeochemical processes take place at the heterogeneous interface between the

rock, soil, water, air and living organisms (Spark, 2005). These processes or interactions in turn

control the solubility, mobility, bioavailability and toxicity of metals (Sparks, 2005).

Microorganisms can transform metals such as Hg, Se, Sn, As and Cr by means of oxidation-

reduction and methylation (the process of replacing an atom, usually a H atom, with a methyl

group) mechanisms and demethylation reactions. These processes affect transport or mobility

and solubility or toxicity of metals (Adriano, 2001).

For example, methylated (organic) forms of Hg are more toxic than inorganic forms of the

clement and they bioaccumulate in organisms (Sparks, 2005).

2.1.3 Uses of Heavy Metals

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i. Cadmium is mainly used in batteries, plastics and it is also found in cigarette smoke,

in shellfish and vegetables (ATSDR, 1999).

ii. Mercury is found in batteries, dental amalgam, vacuum pumps and valves, jet fuel

and heating oil.

iii. Arsenic is present in wood preservatives, herbicides, corrosion inhibitors, in lead and

copper alloys.

iv. Chromium is found in fresh foods, copy machine toner and nickel in coins, kitchen

utensils and milk (ATSDR, 1997).

i. V. Copper is essential to all living organisms and has a wide range of effects

depending on concentration and chemical formulation.

v. Lead has been used in batteries, electronic equipment’s, in petrol, toys, paint, etc.

2.1.4 Human Exposure and Health Hazards associated with Heavy Metals

Metals and their compounds can accumulate in the body tissues, such as bones or nerves. They

can cross the placenta and harm an unborn child in pregnant women. The health hazards

presented by heavy metals depend on the level and the length of exposure (Thomson,2005). In

some cases, the health effects are immediately apparent while in others, the effects are delayed.

i. Aluminum (Al): Alzheimer's disease, osteodystrophy (adverse neurological

conditions affecting speech and memory, eventually leading to dementia).

ii. Arsenic (As): skin, liver, kidney, and lymphatic cancer (Shi H. et al.,2004).

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iii. Cobalt (Co): sterility, hair loss, vomiting, bleeding, and diarrhea.

iv. Copper (Cu): anemia, liver and kidney damage, gastrointestinal problems (Nuhoglu

and Oguz, 2003), and lung cancer (Yu et.al., 2000).

v. Iron (Fe): hemosiderosis or hemochromatosis.

vi. Mercury (Hg): acrodynia or pink disease, rashes, deafness, brain damage, digestive

problems, kidney damage, and mental retardation (ASTDR,1999).

vii. Nickel (Ni): damage to lungs, the nervous system, and mucous membranes (Nicholas

et al., 2003).

viii. Lead (Pb): headache, hypertension, abdominal pain, renal dysfunction, arthritis,

intellectual disability, birth defects, autism, psychosis, etc. and even death

(Papanikolaou, N.,2005).

ix. Tin (Sn): breathlessness, urination problems, liver damage, malfunctioning of

immune systems, chromosomal damage, shortage of red blood cells, and brain

damage.

x. Vanadium(V): bronchitis, pneumonia, cardiae and vascular disease inflammation of

stomach and intestines, damage to the nervous system. bleeding of livers and kidneys,

paralyses.

xi. Zinc (Zn): retarded growth, chromosomal abnormalities, dwarfism, poor appetite,

mental lethargy, stomach cramps, nausea, vomiting, and central nervous system

disorder.

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2.2 Review of Instrumental Techniques for Metal Analysis

2.2.1 Atomic Spectroscopy

Atomic spectroscopy is the determination of elemental composition by its electromagnetic or

mass spectrum (Skoog D., 1998). In the atomic absorption process, if light of just the right

wavelength impinges on a free, ground state atom, the atom may absorb the light as it enters an

excited state. Atomic absorption measures the amount of light at the resonant wavelength which

is absorbed as it passes through a cloud of atoms. As the number of atoms in the light path

increases, the amount of light absorbed increases in a predictable way. By measuring the amount

of light absorbed, a quantitative determination of the amount of analyte element present can be

made. In atomic emission, a sample is subjected to a high energy, thermal environment in order

to produce excited state atoms, capable of emitting light. The energy source can be an electrical

arc, a flame, or plasma. The emission spectrum of an element exposed to such an energy source

consists of a collection of the allowable emission wavelengths, commonly called emission lines,

because of the discrete nature of the emitted wavelengths. This emission spectrum can be used

both for qualitative and quantitative identification of the element. The technique of flame

photometry is an application of atomic emission for quantitative analysis.

Atomic fluorescence technique incorporates aspects of both atomic absorption and atomic

emission. The intensity of this "fluorescence" increases with increasing atom concentration,

providing the basis for quantitative determination. The source lamp for atomic fluorescence is

mounted at an angle to the rest of the optical system. So that the light detector sees only the

fluorescence in the flame and not the light from the lamp itself. It is advantageous to maximize

12
lamp intensity since sensitivity is directly related to the number of excited atoms which in turn is

a function of the intensity of the exciting radiation.

The ease and speed at which precise and accurate determinations can be made have made atomic

absorption one of the most popular methods for the determination of metals among the three

techniques (Skoog, D.,1998).

Figure 2.1 Schematic Diagram of Atomic Absorption Spectrometer (AAS)

2.2 Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

An ICP-MS combines a high-temperature ICP (Inductively Coupled Plasma) source with a mass

spectrometer. The ICP source converts the atoms of the elements in the sample to ions. These

ions are then separated and detected by the mass spectrometer. ICP technology was built upon

the same principles used in atomic emission spectrometry. Samples are decomposed to neutral

elements in high temperature argon plasma and analyzed based on their mass to charge ratios. An
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ICP-MS can be thought of as consisting of four main processes, including sample introduction

and aerosol generation, ionization by an argon plasma source, mass discrimination, and the

detection stem (Chen Z., 2007).

Figure 2.2 Schematic diagram of (ICP-MS)

2.23 Fourier Transform Infrared (FTIR)Spectroscopy

Infrared absorption spectroscopy is the study of interaction of infrared radiation with matter as a

function of photon frequency. Fourier Transform Infrared Spectroscopy (FTIR) provides

specific information about the vibration and rotation of the chemical bonding and molecular

structures, making it useful for analyzing organic materials and certain inorganic materials. An

infrared spectrum represents a fingerprint of a sample with absorption peaks which correspond to

the frequencies of vibrations between the bonds of the atoms making up the material. Therefore,

infrared spectroscopy can result in a positive identification (qualitative analysis) of every

different kind of material. In addition, the size of the peaks in the spectrum is a direct indication

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of the amount of material present. With modern software algorithms, infrared is an excellent tool

for quantitative analysis (K. Kadirvelu et al., 2005).

The IR region is commonly divided into three smaller areas: near - IR (400 - 10 cm-1), mid - IR

(4000 - 400 cm-1), and far - IR (14000 - 4000 cm-1). Chemical bonds vibrate at characteristic

frequencies, and when exposed to infrared radiation, they absorb the radiation at frequencies that

match their vibration modes. Measuring the radiation frequency produces a spectrum that can be

used to identify functional groups and compounds (Yahaya et al., 2010). There are three basic

spectrometer components in an FTIR interferometer; a moving mirror, a fixed mirror, and a

beam splitter.

Figure 2.3a Schematic Diagram of FTIR Spectrometer Components

The beam splitter is a semi-reflecting device and is often made by depositing a thin film of

germanium onto a flat KBr substrate. Radiation from the broadband IR source is collimated and

directed into the interferometer, and impinges on the beam splitter. The basic instrument design

is quite simple. The normal instrumental process is as follows:

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i. The Source: Infrared energy is emitted from a glowing black-body source. This beam

passes through an aperture which controls the amount of energy presented to the

sample and ultimately, to the detector.

ii. The Interferometer: The beam enters the interferometer where the 'spectral encoding'
takes place. The resulting interferogram signal then exits the interferometer.

iii. The Sample: The beam enters the sample compartment where it is transmitted

through or reflected off of the surface of the sample, depending on the type of

analysis being accomplished. This is where specific frequencies of energy, which are

uniquely characteristic of the sample, are absorbed.

iv. The Detector: The beam finally passes to the detector for final measurement. The

detectors used are specially designed to measure the special interferogram signal.

v. The computer: The measured signal is digitized and sent to the computer where the

Fourier transformation takes place. The final infrared spectrum is then presented to

the user for interpretation and any further manipulation (Shen,2008).

Figure 2.3b Schematic Diagram of FTIR Spectrometer

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2.2.4 Scanning Electron Microscopy (SEM)

Accelerated electrons in an SEM carry significant amounts of kinetic energy, and this energy is

dissipated as a variety of signals produced by electron-sample interactions when the incident

electrons are decelerated in the solid sample. These signals include secondary electrons (that

produce SEM images), backscattered electrons (BSE), diffracted backscattered ‘electrons

(DBSE, that are used to determine crystal structures and orientations of minerals), photons

(characteristic X-rays that are used for elemental analysis and continuum X-rays), visible light

(cathodoluminescence--Cl), and heat.

Secondary electrons and backscattered electrons are commonly used for imaging samples:

secondary electrons arc most valuable for showing morphology and topography on samples and

back scattered electrons are most valuable for illustrating contrasts in composition in multiphase

samples (i.e., For rapid phase discrimination). X-ray generation is produced by inelastic

collisions of the incident electrons with electrons in discrete orbitals (shells) of atoms in the

sample. As the excited electrons return to lower energy states, they yield X-rays that are of a

fixed wavelength (that is related to the difference in energy levels of electrons in different shells

for a given element). SEM analysis is considered to be "non-destructive"; that is, x-rays

generated by electron interactions do not lead to volume loss of the sample, so it is possible to

analyze the same materials repeatedly (J. Goldstein, and H. Yakowitz,1977).

Essential components of all SEMs include the following:

i. Electron Source ("Gun")

ii. Electron Lenses

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iii. Sample Stage

iv. Detectors for all signals of interest

v. Display/Data output devices

Infrastructure Requirements:

i. Power Supply

ii. Vacuum System

iii. Cooling system

iv. Vibration-free floor

v. Room free of ambient magnetic fields

Figure 2.4 Schematic Diagram of Scanning Electron Microscopy (SEM) Instrument

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The SEM is routinely used to generate high-resolution images of shapes of objects (SEI) and to

show spatial variations in chemical compositions:

i. Acquiring elemental maps or spot chemical analyses using EDS.

ii. Discrimination of phases based on mean atomic number (commonly related to

relative density) using BSE.

iii. Compositional maps based on differences in trace element (typically transition metal

and rare Earth elements) using Cl.

The SEM is also widely used to identify phases based on qualitative chemical analysis and/or

crystalline structure. Precise measurement of very small features and objects down to 50 nm in

size is also accomplished using the SEM (Springer, 2007).

2.3 Activated Carbon

Activated carbon also called activated charcoal, is a form of carbon that has been processed with

oxygen to create millions of tiny pores between the carbon atoms. Commercial activated carbons

have internal surface area ranging from 500 to 1500 m 2/g. The most common feed stocks used

for the production of activated carbon are wood, coconut shell, bituminous coal, peat etc. The

chars obtained from them could be activated easily to produce reasonably high-quality activated

carbons. During the activation process, the unique internal pore structure is created, which

provides the activated carbon its outstanding adsorptive properties. Activated carbons have a

number of unique characteristics such as large internal surface area, well-developed internal

micro porosity, and wide spectrum of surface functional groups. According to IUPAC definitions

three groups of pores can be identified (Guo and Lau, 2003), which includes;
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i. Macropores (above 50nm diameter)

ii. Mesopores (2-50nm diameter)

iii. Micropores (Under 2nm diameter)

Micropores generally contribute to a major part of the internal surface area. Macro and

micropores can generally be regarded as the highways into the carbon particle, and are crucial for

kinetics. The desired pore structure of an activated carbon product is attained by combining the

right raw material and suitable activation procedure.

Figure 2.5a Diagram of Activated Carbon Pores Structure

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2.4 Preparation of Activated Carbon

2.4.1 Pyrolysis/Carbonization.

Pyrolysis/Carbonization involves heating the source materials to temperatures ranging between

600 to 900°℃ in the absence of air (Cooney, 1999).

This process is to eliminate most of the non-carbon elements such as hydrogen, nitrogen, oxygen

and Sulphur as volatile gaseous products. Low molecular weight volatiles are first released,

followed by light aromatics and finally the hydrogen gas, the resultant product being a fixed

carbonaceous char. The residual carbon atoms are grouped into condensed sheets of aromatic

ring with a cross-linked structure in a random manner. The mutual arrangement of these aromatic

sheets is irregular and leaves free interstices between the sheets, which may be filled with the

tarry materials.

To remove these tarry materials, activation process is carried out. It also enlarges the diameters

of the pores, which were created during the carbonization process and creating new porosity

(Smisek &Cerny,1970).

2.4.2 Activation

The basic characteristics of a carbon are established during the pyrolysis, and the ensuing

oxidation step must be designed to complement the pyrolysis step. During this step, the oxidizing

agent increasingly erodes the internal surfaces of the carbon, develops an extensive and fine

network of pores in the carbon, and changes the atoms lying on the surface to specific chemical

forms which may have selective adsorption capabilities. This activation step is done by two

methods physical activation or chemical activation.


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i. Physical activation

Physical activation or partial gasification is generally carried out at elevated temperatures

between 750 and 1100°℃ using oxidants such as steam, carbon dioxide, air or mixture of these

gases. Chlorine, Sulphur vapors, Sulphur dioxide, ammonia and a number of other substances

having activation effects are rarely used. Gasification of the carbonized material with steam and

carbon dioxide occurs by the following endothermic reactions:

C + H2O → H2 + CO + 117kJ/ (g.mol)


(2.1)

C + CO2 → 2CO + 159 kJ/ (g.mol)


(2.2)

The reaction of steam with carbon is accompanied by the water gas formation reaction. Which is

catalyzed by the carbon surface as,

CO + H2O → CO2 + H2 + 42 kJ/(g.mol)


(2.3)

Since the reaction of carbon with steam and with carbon dioxide is both endothermic. External

heating is required to drive the reactions and to maintain the reaction temperature. The activation

process can be manipulated to produce products of desired characteristics. Activation

temperature, steam and CO2 flow rates control the pore development, which in turn affect pore

size distributions and the level of activity of the activated carbon (Guo and Lau,2003).

ii. Chemical activation

Chemical activation is usually carried out by impregnating the raw or pre-carbonized material

with an activating agent and pyrolyzed between 400 and 800° ℃ in the absence of oxygen. The
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most commonly used activating agents are phosphoric acid, hydrochloric acid, Sulphuric acid,

alkalis namely KOH and NaOH, zinc chloride and alkaline metal compounds. Phosphoric acid

and zinc chloride are used for the activation of lignocellulosic materials. Phosphoric acid is the

most preferred activating agent because of its low environmental impact when compared to zinc

chloride. The resultant activated carbon is washed, dried till constant weight is obtained and

ground to required size. Activated carbons produced by chemical activation generally exhibit a

very open structure and bottle shaped, ideal for the adsorption of large molecules (O.Ekpele et

al,2011).

iii. Combination of physical and chemical activation

A combination of activated Carbons with a Very high surface area and porosity adequate for

certain specific physical and chemical activation can be tested to Prepare granular applications

such as gasoline vapor, control, gas storage, etc. Activated carbons of this type have reported

using lignocellulosic precursors chemically activated with been phosphoric acid and zinc

chloride and later activated under a flow of carbon dioxide. Uniform, medium-size microporosity

and surface areas above 3600 ㎡/g are obtained with this mixed procedure (Bansal,1988).

2.5 Forms of Activated Carbon

There are three main forms of activated carbon (activated charcoal).

i. Granular Activated Carbon (GAC) - are irregular shaped particles with sizes ranging

from 0.2 to 5mm. This type is used in both liquid and gas phase applications.

23
ii. Powdered Activated Carbon (PAC) - are pulverized carbon with a size

predominantly less than 0.18mm (US Mesh 80). These are mainly used in liquid

phase applications and for flue gas treatment.

iii. Extruded Activated Carbon (EAC) - are extruded and cylindrical shaped with

diameters from 0.8 to 5mm. These are mainly used for gas phase applications because

of their low pressure drop, high mechanical strength and low dust content.

2.6 Application of Activated Carbon

Activated carbon is a unique and effective agent for purification and isolation and recovery of

trace material. The various applications can be broadly divided into two categories,

i. Liquid-phase applications.

ii. Gas-phase applications.

2.6.1 Gas-Phase Applications

i. This includes separation, gas storage and catalysis. These products are generally more

expensive than liquid phase carbons (Allen et al., 1998).

ii. Natural gas purification; removal of H2S and BTX Flue gas cleaning at waste

incineration plants for the removal of dioxins and heavy metals.

iii. Exhaust air treatment following production processes for the removal of organic

impurities. Purification of process gases, e.g., CO2; scrubbing and separation of oil

from compressed air. Removal of pollutants in air conditioning, ventilation and

exhaust systems.
24
iv. Emission control, e.g., at filling stations and during tank ventilation for motor vehicle

and industrial applications.

v. Pollutant removal in car interior ventilation systems in gas masks, and as a carrier

medium for special impregnating agents or catalysts.

2.6.2 Liquid-Phase Applications

In the water treatment sector, activated carbon is used cither in powdered (suspension process) or

granular (fixed bed process) form, depending upon the specific application and process.

Increasingly exacting quality requirements for drinking water, coupled with increasing pollution

levels in untreated water (groundwater and surface water), have led10 the optimization of

activated carbon as a means of guaranteeing acceptable drinking water quality (O. Ekpete et

al,2011).

In recent years, the use of activated carbon processes has become widely established in drinking

water treatment, groundwater rehabilitation and the treatment of service water. Likewise,

activated carbon is being used to an increasing extent in waste water treatment, whether it be in

the systematic treatment of individual effluent streams (e.g., in the chemicals industry), in the

removal of substances toxic to bacteria in biological wastewater treatment or in tertiary waste

water treatment, where effluent restrictions are particularly severe (P. Sugumaran, et al., 2012).

The use of activated carbon is especially advisable in cases requiring the removal of toxic

substances or pollutants that are not easily biodegradable. Activated carbon is almost always

employed in the treatment of waste water in the paper, textile and petrochemical industries

(Santhy and Selvapathy, 2006).

25
2.7 Hospital Wastewater

Wastewater can be defined as any water, whose quality has been adversely being abused by

anthropogenic influence which includes liquid waste discharged from domestic home, industries,

agricultural and commercial sectors (Ekhaise and Omavwoya,2008).

Previous study had shown that the volume of water generally generated from hospitals varies

from 400 to 1200L/day/bed. This volume of water produces by the hospital contain micro-

organisms, heavy metals, toxic chemicals and radioactive elements which results in the

production hybrid wastewater as the combination of domestic, industrial and effluents of care

and medical research. The hospital wastewater is also found to contain chlorinated molecules in

high concentrations and heavy metal such as mercury and silver. The occurrence of

pharmaceuticals in wastewater also being reported which is including antibiotics, hormones,

strong painkillers, tranquilizers and chemotherapy chemicals given to cancer patients excreted by

humans and domestic animals are distributed into the environment by flushing toilets and

spreading manure and sewage sludge onto and into soil (Emmanuel et al., 2002). From WHO

report,85% of hospital waste is non-hazardous, 10% infective and 5% not infective but

hazardous (Ekhaise and Omavwoya,2008).

Waste water from hospital may come from few categories of hospital facility which are clinical

and research laboratories, medical waste incinerators and hospital laundries (Niumpang,2006).

26
CHAPTER THREE
MATERIALS AND METHOD
3.1 Sample Collection and Pretreatment

3.1 The Apple of Sodom (Calotropis procera) plant stems were collected from trees located at

kamazou and janruwa roadside, new road, Kaduna North, Kaduna. The stems collected were

then washed with Tap water to wash of all dirt and dusts and sun dried for 3days. Afterward

washed with distilled/deionized water and then oven dried at 105°for 24hours.The hospital

wastewater was collected from the maternity ward at Barau Dikko Teaching hospital Kaduna

state, Kaduna. The listed procedures below were then carefully carried out.

3.2 Carbonization and Chemical Activation

The Apple of Sodom (Calotropis procera) plant collected was dried and pounded then, sieved

with a 2mm mesh size sieve.

Open Carbonization was done using the hot plate for 15min and afterward carbonization using

the muffle furnace at a temperature of (0 - 400° C) for 1hr. The sieved product was allowed to

cool down in the desiccator and activated using prepared 1M HNO3 as activating agents. The

activated carbon was produced with a slight modification using standard methods of Ekpete (O.

Ekpete, et al., 2011) and Sugumaran (P.Sugumaran, et al., 2012).In a beaker,15g of the

carbonized Pride of Barbados was impregnated with 60mL 1M HNO 3. The beaker contents (15g

of the carbonized sample and 60mL 1M HNO 3) were thoroughly mixed using a heating mantle at

a constant temperature of 80° C until it formed a paste (the activating agent was fully absorbed

by the raw material). The paste was then transferred into a crucible. The carbonized sample was

allowed to cool to room temperature and was washed using hot water and was further washed
27
with distilled water to remove residual acid until a neutral pH of 6.1 was obtained. It was then

oven-dried at 105° C for 6hrs, and then kept in air tight pack for further analysis and labelled as

CAHAC (Carbonized Apple of Sodom HNO3 Activated Carbon), and UAC (Untreated Apple of

Sodom Carbon).

3.3Surface Morphology-Scanning Electron Microscopy (SEM)

The activated carbon sample was dried to avoid relatively high surface tension and micro-ripping

of the surface upon leaving. The surface dusts were removed using acetone. Hexamethyldisilane

(HMDS) was used in cell preparation and after a short (3 minutes) incubation, it was removed

and excess was left to evaporate. The sample was mounted on a metal stub using a sticky carbon

disc which increases conductivity. The sputter was coated with a conductive material (gold) to

prevent charge buildup on sample surface. The metal was applied in a controlled manner in the

sputter coater. The coating thickness was around 10nm to prevent charging and to ensure clarity

of the sample surface details. The sample was completely dried before loading into SEM

chamber (Haitao Z, 2008).

A Zeiss EVO-50 Scanning Electron Microscope (SEM) was used to determine the surface

morphology of the activated carbon produced at magnifications of 255, 350, 500, 1000, 1500 and

2000 times with virtually unlimited depth of field.

3.4 Determination of Bulk Density

A glass cylinder(25mL) was filled to a specified volume with 1.0g 2mm powder carbon sample

of each of CAHAC, and dried in an oven at 105°C for 6hr.The cylinder was tapped for 1-2

28
minutes to compact the carbon (P.Sugumaran, et al., 2012).The bulk density calculated and

presented as g/mL following the formula:

Bulk density = Mass of Sample (dry) ÷ Volume of measuring cylinder x 100

(3.1)

3.5 Determination of Moisture Content

Thermal drying method was used in the determination of moisture content of the samples.1.0g

carbonized sample was weighed in triplicate and placed in clean, dried, and weighed crucible.

The crucible was placed in an oven at 105°C to constant weight for 4hrs according to the method

of Rengaraj (S. Rengaraj, et al., 2002). The difference between the initial and final mass of the

carbon represents the moisture content. The percentage moisture content (%) was computed as

follows:

Moisture (%) = Loss in weight on drying (g) ÷ Initial weight x100 (3.2)

3.6 Determination of Ash Content

For ash content determination, crucibles were preheated to about 105°C for 45min,then cooled in

a desiccator for 15min, and weighed. 1.0g of each sample was transferred into the crucibles and

reweighed. The crucibles containing the samples were then placed in the oven and the

temperature was allowed to rise to 105℃ for about 3hr and allowed to cool in a desiccator to

room temperature (30°C) and reweighed (S.Rengaraj, et al., 2002). The ash content was

calculated using the equation;

Ash (%) dry = Ash weight (wet) (g) ÷ Oven dried weight (g) x 100 (3.3)

29
3.7 The Fourier Transform Infrared (FTIR) Analysis

For sample analysis, 0.5g of activated carbon was mixed with about the same amount of

potassium bromide KBr. The mixture thus obtained was crushed in a mortar to obtain a

homogeneous powder which was then introduced into a mould to obtain very fine plates. The

plates were then introduced into the spectrophotometer for analysis. The wave number was found

to vary between 4000 and 650cm-1. The Fourier Transform Infrared (FTIR)analysis of the

samples was carried out using FTIR equipment of Happ-Genzel for the examination of the

spectra (Transmittance Method).

3.8 Determination of Heavy Metal ions (Pb+2 and Ni+2)

2g of the activated carbon was mixed with 100mL of the hospital wastewater in a 100mLconical

flask and stirred at room temperature of 32°C for 15 min and allowed to stand for 50 min to

ensure equilibrium. It was then filtered using the filter paper. The concentration of Pb +2 and Ni+2

in the hospital wastewater was determined before and after interaction with the activated carbon

using Hanna Instrument Multi-Parameter Photometric with COD (Apiprecya, et al., 2006), The

amount of metal ions adsorbed by the adsorbent was determined using the equation;

Q = (Initial concentration - Final concentration) x Volume of wastewater used

Mass of Adsorbent used

The percentage of metal ions removed was obtained from the equation;

R(%) = (initial concentration - Final concentration) x 100 (3.4)


30
Initial contentration

31
CHAPTER FOUR

RESULTS AND DISCUSSION

4.1 Results

4.1.1 Proximate Composition Analysis

The proximate composition analysis (bulk density, moisture content and ash content)

results are shown in table 4.1.

4.1.2 The Atomic Absorption Spectroscopy (AAS) Analysis

The heavy metal ions present in the wastewater sample were analyzed using the Hanna

Instrument Multi-Parameter Photometric with COD. It detected the concentrations of Pb +2 and

Ni+2 present. The initial and final concentrations of Pb +2 and Ni+2 present in the wastewater is

shown in table 4.2 and the quantity of metal ions removed and percentage removed are shown in

table 4.3.

32
Table 4.1 Proximate composition of activated carbon from apple of Sodom plant stem.

Parameters Values

Bulk density (g/mL) 2.06

Carbon content (%) 20.13

Moisture content (%) 4.03

Ash content (%) 7.03

Table 4.2 Quantity of Pb+2 and Ni+2 in waste water before and after treatment with activated
carbon.

Metal ions Before treatment After treatment


(wastewater)

Pb+2 2.915 1.92

Ni+2 1.87 1.02

Table 4.3 The quantity of metal ions (Pb+2 and Ni+2) and percentage removed after treatment
with activated carbon.

Metal ions Quantity removed Percentage removed

Pb+2 7.08 45.45

Ni+2 11.625 47.86

33
Percentage (%) yield = weight of final activated carbon x 100
(3.5)

Mass of the original raw sample

% yield = 2.06 x 100 (3.6)

15g

% yield = 13.733% (3.7)

4.1.3 The Fourier Transform Infrared (FTIR) spectroscopy analysis

The FTIR spectroscopy analysis results show these Infrared Spectra which are generally

informative about what functional group are present. The result is shown in figure 4.1.

Fig 4.1 The FTIR spectroscopy analysis of activated carbon produced from apple of Sodom
plant stem.

34
4.1.4 Sample surface morphology: - The scanning electron microscopy (SEM)

The scanning electron microscope images of activated carbon produced from apple of Sodom

plant stem activated using nitric acid (HNO 3) are shown in plates 4.1(a-f) at 255, 350, 500, 1000,

1500 and 2000 magnifications.

35
Plate 4.1a

36
Plate 4.1b

37
Plate 4.1c

38
Plate 4.1d

39
Plate 4.1e

40
Plate 4.1f

41
4.2 Discussion

4.2.1 The proximate composition analysis of activated carbon from Apple of Sodom Plant

Stem

The proximate analysis of activated carbon from apple of Sodom plant stem (Table 4.1) was

carried out to determine the percentage by mass of the moisture content, carbon content, ash

content and bulk density which was gotten as 4.03%, 20.13%, 7.03% and 2.06g respectively. The

above result goes in agreement with other research work when compared (Kalpana Patidar and

Manish vashishtha, 2019, characterization and isotherm study of activated carbon production

from mustard stalk by Zncl2 activation) results where; moisture content 9.58%, carbon content

12.65%, ash content 0.01%. (Mohd Iqbaldin MN, Khudzir I, Mohd Azlan MI, Zaidi AG, surani

B and Zubri Z, 2013, properties of coconut shell activated carbon), results where; ash content

0.8% and carbon content 21.38%. (Noor Shawal Nasri et al,2020, synthesis and characterization

of green porous carbon with large surface area by two steps chemical activation with KOH),

results where; moisture content 8.21%, ash content 0.01%, carbon content 18.6%. So therefore,

from the above results compared to this investigation, it shows one thing in common, i.e., they

all have a high carbon content and a low ash content, proving that basically researches on

activated carbon has a high carbon content and low ash content. The significance of ash content

and carbon content in activated carbon is that, the ash content is an actual property of activated

carbon, it decreases the effectiveness of the activated carbon, you will find low ash content in all

activated carbon products, while the carbon content on the other hand gives an indication of the

amount of carbon bound during pyrolysis.

42
4.2.3 The FTIR spectroscopy analysis of activated carbon produced from apple of Sodom

plant stem (fig 4.1)

The FTIR absorption bands of the apple of Sodom plant stem activated carbon revealed that the

carbon contains the following functional groups; alkene(C-H), amine salt (N-H), alkane (C-H),

thiocyanate (SC≡N), conjugate alkene (C=C), nitro compounds (N-O), sulfoxide (S=O), halo

compound (C-Cl), halo compound (C-Br) and halo compound (C-I). The assignment of the

specific wavelength to some functional group was not possible because the adsorption bands of

various functional groups overlap and shift depending on their molecular structure and

environment.

43
Table 4.4 FTIR analysis wave length and standard IR wave number and corresponding

functional groups of Apple of Sodom plant stem activated carbon present.

Standard IR Activated carbon Functional vibration Intensity


wave no. (cm-1) wave length (cm- groups
1
)

3100 – 3000 2919.71 Alkene C-H Stretching Medium

3000 – 2800 2919.71 Amine salt N-H Stretching Strong broad


300 – 2840 2851.13 Alkane C-H Stretching Medium

2175 – 2140 2166.66 Thiocyanate Stretching Strong


SC≡N

1650 – 1600 1600.16 Conjugate Stretching Medium


alkene C=C

1550 – 1500 1492.10 Nitro compound Stretching Strong


N-O

1450 1451.32 Alkane C-H Bending Medium

1070 – 1030 1027.51 Sulfoxide S=O Stretching Strong

915 – 905 905.39 - - -

850 – 550 752.94 Halo compounds Stretching Strong


C-CL

700 ± 20 694.80 - - -

690 – 515 539.59 Halo compounds Stretching Strong


C-Br

600 – 500 506.11 Halo compounds Stretching Strong


C-I

44
These results are in agreement with the findings of other research work on activated carbon.

Researches on activated carbon used to compare (N. mirghaffari, M. Soleimani, H.

shariatmadari, C. beiver and J. bedia, 2019, phenol adsorption on high microporous activated

carbons from oily sludge) results were; 3422, 1455, 1090, 800 which are amine, alkene, alkane,

secondary alcohol and halo compound c-cl. (Yufeng zhao, chul-woong cho, longzhe cui, wei

wei, 2019, adsorption removal of endocrine disruption compounds and a pharmaceutical using

activated charcoal from aqueous solution) results were; 3422, 2924, 2854, 2346, 2086, 1622,

1444, 1118,874 which are amine, alkane, carbon dioxide, isothiocyanate, alkene, secondary

alcohol. (Cafer saka, 2012, iodine number analysis and preparation of activated carbon from a

corn shell by chemical activation with ZnCl2) results where; 2919, 2853, 2325, 1743, 1544,

1145, which are alkane, carbon dioxide, ester, nitro compound and sulfone.

From the above different works on activated carbon compared to this investigation, the results

gotten where similar, the little differences may result from the solvent that was used for the

chemical activation. For the work of (N. mirghaffari, M. Soleimani, H. shariatmadari, C. beiver

and J. bedia, 2019) the research uses phenol as the solvent for chemical activation and the only

different functional groups from this research are secondary alcohol and carbon dioxide. For the

work of (Yufeng zhao, chul-woong cho, longzhe cui, wei wei, 2019) the research uses KOH as

activating agent and the only different functional group for this research is secondary alcohol.

For the work of (Cafer saka, 2012) the research uses ZnCl 2 as solvent for chemical activation and

the only different functional group sulfone, esters and carbon dioxide.

The slight reason for the differences observed in these researches compared to this investigation

was because nitric acid (HNO3) was used as solvent for chemical activation. Comparing with the

45
standard and the above works on activated carbon, it falls with the normal recommended

functional groups as shown above.

4.2.3 Assessment of the activated carbon produce from the apple of Sodom plant stem for

the removal of Pb+2 and Ni+2

Based on equilibrium studies, the activated carbon produced from the apple of Sodom plant stem

removal capacity for the two heavy metal ions (Pb +2 and Ni+2) studied, appears to be greatest for

Pb+2 followed by Ni+2 due to the percentage removal value determined and recorded as 47.86%

and 45.45% respectively.

Comparing the metal ions percentage removed of this investigation which are (Pb +2 45.45% and

Ni+2 47.86%) with (Hala Ahmed Hegazi, 2013, removal of heavy metals from wastewater using

agricultural and industrial waste as adsorbents) the percentage of metal ions of Fe 2+, Pb2+, Cd2+,

Cu2+, and Ni2+ are 68.59%, 22.22%, 26.04%, 24.49% and 94.885% respectively. The difference

occurs in the usage of adsorbents, in this investigation agricultural waste was used and the results

gotten were (Pb+2 45.45% and Ni+2 47.86%) but in the above research work, agricultural and

industrial waste was used as adsorbents and the percentage of the metal ions was high. From the

work of (Benard E, Jimoth A. and Odigure J.O, 2013, heavy metal removal from industrial

wastewater by activated carbon prepared from coconut shell). The percentage of the metal ions

Cu2+, Fe2+, Zn2+ and Pb2+ are 43.50%, 16.60%, 17.40 and 0.005% respectively. From the above

research the adsorbent was industrial waste and metal ion percentage were Cu 2+, Fe2+, Zn2+ and

Pb2+ are 43.50%, 16.60%, 17.40 and 0.005% respectively. Compared to these investigation,

agricultural waste was the adsorbent and the metal ion percentages (Pb +2 45.45% and Ni+2

46
47.86%). So therefore, it was observed that different wastewater has numerous percentages of

metal ion depending on where it was gotten from.

4.2.4 The surface morphology images of activated carbon from the apple of Sodom plant

stem

The scanning electron microscopy images of activated carbon produced from the apple of Sodom

plant stem using nitric acid (HNO3) are shown in fig 4.1(a-f) at 255, 350, 500, 1000, 1500 and

2000 magnifications. The SEM photograph showed that wide varieties of pores are present in the

activated carbon which revealed that it is porous in nature and thereby, a good adsorbent.

Compared to the research of (Benard E, Jimoth A. and Odigure J.O, 2013, heavy metal removal

from industrial wastewater by activated carbon prepared from coconut shell). Which shows in

plate 1 and 2 the image of activated carbon with the pores on them proving that they are good

adsorbent.

47
CHAPTER FIVE
SUMMARY AND RECOMMENDATION
5.1 Summary of Results

As the activated carbon produced is highly dependent on the raw materials used, Apple of

Sodom was used due to its high carbon content. The activating agent used HNO3 was used

because acid activated carbon performs better in the low concentration range. The activation

process is also essential for production of a good adsorbent; the activated carbon was prepared

by chemical activation because it gives higher yield of carbon as well as larger pore size in the

activated carbon produced.

The activated carbon produced was analyzed for the following; bulk density, moisture content,

ash content, percentage adsorption/removal capacity of Pb+2 and Ni+2 and recorded as

2.06g/ml,4.03%,7.03%,45.45% and 47.86% respectively. The surface functional groups present

includes; alkene(C-H), amine salt (N-H), alkane (C-H), thiocyanate (SC≡N), conjugate alkene

(C=C), nitro compounds (N-O), sulfoxide (S=O), halo compound (C-Cl), halo compound (C-Br)

and halo compound (C-I). The surface morphology determined is shown in Plate 4.1a-f.

In conclusion, the production of activated carbon from agricultural waste materials using

chemical activation process for use as adsorbent provides an environmentally friendly source of

alternative energy. The HNO3 activation develops good porous structure; HNO 3 etches the

carbon surface through vigorous reaction while acting as a dehydrating agent to force all

hydrogen and oxygen out of the carbon structure.

48
5.2 Recommendations

Due to the duration and cost implication of this research work, only few analysis were carried

out on the activated carbon produced. However, it is recommended that;

1.Research on the production and characterization of activated carbon from Apple of Sodom by

varying the absorbent dosage activation time and temperature respectively should be carry out.

2. More in-depth analysis on production of activated carbon from pride of Apple of Sodom using

other activating agents such as; phosphoric acid (H3PO4) and sulphuric acid(H2SO4) should be

carried out.

3. Similar research using different precursor material with additional analysis such as; adsorption

isotherms, pore volume estimates, kinetic studies and gravimetric analysis to estimate porosity

should be carry out.

49
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