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PRE-LIMINARY STUDY ON TREATMENT OF TEXTILE

WASTEWATER BY PINEAPPLE LEAVES BIOSORBENTS

MUHAMMAD NAJJIB B HAZLAN

A project report submitted in fulfilment of the requirement for the award of the
Degree Bachelor of Chemical Engineering Technology (Biotechnology) with
Honours

Faculty of Engineering Technology


Universiti Tun Hussein Onn Malaysia

JANUARY 2019
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I hereby declare that the work in this project report is my own except for quotations
and summaries which have been duly acknowledged,

Student : ……………………………………………………
MUHAMMAD NAJJIB B HAZLAN
Date : ……………………………………………………

Supervisor : ……………………………………………………
DR MAS RAHAYU BINTI JALIL
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This thesis is dedicated to whom that I love especially my parents.


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ACKNOWLEDGEMENT

I would like to express my utmost gratitude to my supervisor Dr. Mas Rahayu bt Jalil
for her kind guidance and supervision during the preparation of this report. Her
encouragement, guidance, and support enabled me to develop a very detailed
understanding of the subject thus ensured the smoothness and success of all the
works involved. In addition, I would also like to take this opportunity to thank those
who made this report possible. Special thanks to my parents for their endless support
and pray given to me. I’m also very grateful to the helpful lab officers, En Redzuan,
Pn Mas Ayu and Pn Aziah, and En Sidek for their willingness to assist me in lab and
guide me in the way to use all the valuable equipment. Last but not least, million
thanks to my peers who were doing this project with me and shared ideas. The
process of completing this report wouldn’t be so smooth and inspiring without their
cooperation and encouragement.
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ABSTRACT

This research was conducted to study the use of pineapple (Ananas comosus L.
Merryl) leaves as bio sorbent for reducing pollutant from textile wastewater.
Pineapple is mainly produced as canned fruits and consumed worldwide. During
harvesting, pineapple leaves is usually discharged and left abundantly. From the
points of the view of multipurpose utilization and environmental protection,
utilization of pineapple leaves is of important significance. Therefore, this study
could help in converting these wastes into useful product by investigating its
feasibility as bio sorbent. Pineapple leaves was first treated with Sodium Hydroxide
(NaOH) in order to increase adsorption efficiency. Following that, batch adsorption
by using treated bio sorbent was conducted to investigate the effects of different
adsorbent dosage on adsorption performance. The parameter that is being studied in
this research were chemical oxygen demand (COD), dissolved oxygen (DO).
turbidity, conductivity and colour. The treatment process was conducted by using
different dose of bio sorbent (0.2g, 0.4g, 0.6g, 0.8g and 1.0g) and agitated at 150 rpm
shaking speed, 30oC temperature for 2 hours. From the results obtained, the
biosorption test revealed that the removal pollutant depending on adsorbent dosage.
The results proved that agricultural wastes are good option for the reduction of
pollutant from textile effluents. Somehow, the optimum dosage was not identified
due to some error such as insufficient dosage, low contact time, low reaction
temperature and low initial concentration. Thus, further investigations in order to
analyse optimum dosage need to be conducted.
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ABSTRAK

Kajian ini dijalankan adalah untuk mengkaji kebolehan menggunakan daun nenas
(Ananas comosus L. Merryl) sebagai biosorben untuk mengurangkan pencemaran di
dalam air sisa industri tekstil. Nenas biasanya ditinkan dan digunakan sebagai bahan
makanan dengan meluas. Semasa penuaian, daun nenas sering dibuang dan dibiarkan
dengan begitu sahaja. Dari sudut pandangan penggunaan serbaguna dan
perlindungan alam sekitar, penggunaan daun nenas adalah penting. Oleh itu, kajian
ini membantu menjadikan hasil buang pertanian ini ke suatu hasil yang bermanfaat
dengan mengkaji kebolehan daun nenas sebagai biosorben. Daun nenas pada
mulanya dirawat dengan natrium hidroksida (NaOH) untuk meningkatkan
keberhasilan penyerapan dan prestasi. Dengan itu, air sisa industri tekstil dirawat
secara berperingkat dengan menggunakan biosorben yang telah dirawat dan
dijalankan untuk mengkaji kesan dos yang berbeza kepada keberhasilan penyerapan.
Parameter yang dikaji dalam kajian ini adalah Keperluan Oksigen Kimia, Oksigen
Larut, kekeruhan, pengaliran elektrik dan warna. Hasil kajian membuktikan
modifikasi kimia pada daun nenas dengan natrium hidroksida meningkatkan prestasi
penyerapan pencemaran dari air sisa industri tekstil. Proses bioserap dijalankan
dengan menggunakan dos biosorben yang berbeza iaitu (0.2g, 0.4g, 0.6g, 0.8g and
1.0g) dan digoncang pada 150rpm kelajuan goncangan, pada suhu 30oC, untuk 2 jam.
Dari hasil kajian yang didapati, ujian biserap menunjukkan keberhasilan penyerapan
bergantung kepada dos biosorben. Hasil kajian membuktikan sisa buang pertanian
adalah pilihan yang baik untuk mengurangkan pencemaran dari sisa air industri
tekstil. Walau bagaimanapun, dos optima tidak dapat dikenal pasti disebabkan oleh
beberapa faktor seperti kekurangan dos, masa reaksi rendah, suhu reaksi rendah dan
kepekatan awal rendah. Oleh itu, kajian seterusnya harus dilakukan pada masa
depan.
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CONTENTS

TITLE i
DECLARATION ii
DEDICATION iii
ACKNOWLEDGEMENT iv
ABSTRACT v
ABSTRAK vi
CONTENTS vii
LIST OF TABLES ix
LIST OF FIGURES x
LIST OF SYMBOLS AND ABBREVIATIONS xi
LIST OF APPENDICES xii

CHAPTER 1 INTRODUCTION 1

1.1 Project Background 1


1.2 Problem Statement 3
1.3 Project Objectives 3
1.4 Project Scopes 3

CHAPTER 2 LITERATURE REVIEW 5

2.1 Introduction of bio sorbent from pineapple leaves 5


2.2 Properties of pineapple leaves 6
2.2.1 Physical properties of pineapple leaves 6
2.2.2 Chemical properties of pineapple leaves 6
2.3 Textile wastewater 8
2.4 2.4 Parameters used for characterization of textile 9
Waste wastewater
2.4.1 Chemical Oxygen Demand (COD) 9
2.4.2 Electric Conductivity 10
2.4.3 Colour 10
2.4.4 Turbidity 11
2.5 Effluent discharge standards 11
2.6 Textile effluent treatment process 12
2.6.1 Physical method 12
2.6.2 Chemical method 14
2.6.3 Biological method 15
2.6.4 Biosorption 16
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CHAPTER 3 METHODOLOGY 18

3.1 Introduction 18
3.2 Material and apparatus 20
3.3 Sample wastewater 20
3.4 Experimental procedure 21
3.4.1 Preparation of bio sorbents 21
3.4.2 Characterisation of bio sorbents 23
3.4.3 Adsorption of textile wastewater by bio 24
sorbents
3.5 Analysis of textile wastewater 25
3.5.1 Analysis of COD 25
3.5.2 Analysis of DO 26
3.5.3 Analysis of turbidity 27
3.5.4 Analysis of conductivity 28
3.5.5 Analysis of colour 28

CHAPTER 4 RESULTS AND DISCUSSION 29

4.1 Introduction 29
4.2 Characterisation of bio sorbents 30
4.3 FTIR spectra after adsorption process 33
4.4 Blank sample analysis 34
4.5 Analysis of textile wastewater 34
4.5.1 Effect of bio sorbent dosage on COD. 35
4.5.2 Effect of bio sorbent dosage on DO 37
4.5.3 Effect of bio sorbent dosage on 37
conductivity
4.5.4 Effect of bio sorbent dosage on turbidity 39
4.5.5 Effect of bio sorbent dosage on colour 40
4.6 Problems related to experimental procedure 41

CHAPTER 5 CONCLUSION 43

5.1 Conclusion 43
5.2 Recommendation for future work 44

REFERENCES 45
APPENDICES 50
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LIST OF TABLES

2.1 Properties of pineapple leaves fibre 6


2.2 Parameters of effluent compared with DOE 12
4.1 FTIR of the bio sorbent before and after adsorption process 31
4.2 Readings of blank sample 34
4.3 Results of raw wastewater 35
4.4 Conductivity Limits in National Quality Standards for Malaysia 38
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LIST OF FIGURES

2.1 Chemical structure of cellulose 7


2.2 Structural unit of lignin 7
2.3 Structural unit of hemi cellulose 8
3.1 Flow chart of the experimental procedure 19
3.2 Raw wastewater collected from textile industry 20
3.3 Water bath used to boil pineapple leaves 21
3.4 Mature pineapple leaves (left);the air dried leaves (right) 22
3.5 NaOH treated leaves (left);treated bio sorbent (right) 22
3.6 Oven used during drying process of NaOH treated 23
pineapple leaves
3.7 FTIR used for bio sorbent characterization 24
3.8 Rotary incubator shaker used during adsorption process 25
3.9 DR200 thermostat used to reflux the COD reagent 26
3.10 DO meter used to measured DO in treated water 27
3.11 Turbidity meter to measure turbidity to measure turbidity 28
of treated wastewater
3.12 DR6000 uv vis spectrophotometer 29
4.1 Pineapple leaves bio sorbent 31
4.2 FTIR spectra of pineapple leaves bio sorbent before 33
adsorption process
4.3 FTIR spectra of pineapple leaves bio sorbent after 34
adsorption process
4.4 COD vs dosage 36
4.5 DO vs dosage 37
4.6 Conductivity vs dosage 39
4.7 Turbidity vs dosage 40
4.8 Appearance of water sample 40
4.9 Colour vs dosage 41
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LIST OF SYMBOLS AND ABBREVIATIONS

COD - Chemical Oxygen Demand


DO - Dissolved Oxygen
TDS - Total Dissolved Solid
H2O - Water
O3 - Ozone
H2O2 - Hydrogen peroxide
K2Cr2O7 - Potassium dichromate
Fe(NH4)2(SO4)2 - Ferrous ammonium sulphate
NaOH - Sodium hydroxide
AOP - Advanced Oxidation Process
UV - Ultra violet
FTIR - Fourier Transform InfraRed Spectroscopy
HPLC - High Performance Liquid Chromatography
ADMI - American Dyes Manufacturer’s Institute
DOE - Department of Environment
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LIST OF APPENDICES

Appendix A Raw data of COD, DO, Turbidity, Conductivity 50


and Colour
Appendix B Gantt Chart 55
CHAPTER 1

INTRODUCTION

1.1 Project background

In textile industries various processes are carried out starting from fibre production to
the final finishing of product (Ahmad and Hameed, 2009). The textile industry is a
substantial consumer of water (Solis et al., 2012), dyes, surfactants and various other
chemicals. Hence the amount of wastewater generated from all these processes is
very high and highly contaminated (Lin and Chen, 1997). The textile wastewater
contributes to high biochemical oxygen demand (BOD), suspended solids (SS),
dissolved solids, color, chemical oxygen demand (COD), heat, acidity, basicity and
other soluble substances (Ahn et al., 1999). This highly contaminated water has a
high environmental impact and therefore needs to be treated before being discharged
to the environment (Kumar et al., 2008).
A wide variety of biological, physical and chemical methods for the treatment
of colored wastewater include photocatalytic degradation (Mahmoodi et al., 2005),
coagulation (Sabur, 2012), membrane filtration (Wu et al., 1998) and microbiological
degradation (Pearce et al., 2003). All these methods have different color removal
abilities, capital costs and operating rates (Amin et al., 2009). The adsorption process
is preferred over other processes due its low cost, easy operation, flexibility and
simplicity. Adsorption processes using activated carbons are widely used to remove
color and other pollutants from wastewaters but the high cost of activated carbon
makes its use limited (Yangui, 2013). Recently scientists are giving considerable
attention on the use of biological-based materials and their by-products as
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the biosorbent for the removal of pollutants from different wastewaters because of
presence of carboxyl, hydroxyl and amino groups over their surfaces (Ay et al.,
2012). These groups are responsible for the biosorption process. Biological-based
materials such as agricultural-based biomasses are cheap and easily obtainable in
considerably substantial quantities. Many researchers have used agricultural-based
biomasses such as cocoa shells (Meunier et al., 2003), grape stalks (Martinez et al.,
2006), hazelnut and almond shells (Pehlivan et al., 2009), Capsicuum annuum seeds,
(Ozcan et al., 2007), citrus wastes (Asgher and Bhatti, 2010), rice husk (Safa and
Bhatti, 2011) and barely husk (Haq et al., 2011) for the removal of dyes from
aqueous solution. Agricultural by products are easily available in Malaysia so the
present study was designed to exploit the abundantly available agricultural wastes for
the treatment of textile effluents.

1.2 Problem statement

With the production of pineapple fruits, tons of pineapple waste are produced
annually. Most of the excess pineapple wastes such as leaves, peels and stems are
discarded or composted as they have no commercial purpose, resulting in
environmental pollution. Hence, the utilization of pineapple leaves as an adsorbent to
treat contaminant from industrial effluent can greatly reduce the amount of waste
produced. This adsorbent is easy to obtain and inexpensive as well. Therefore, this
study was conducted to investigate the utilization of pineapple leaf as low-cost
adsorbent to treat contaminant from industrial textile wastewater. This is because,
textile wastewater needed to be treated so that the effluent can be released to
environment. The textile industry consumes high volume of water for its different
wet processing operations. These effluent contains chemicals like acids, alkalis, dyes,
hydrogen peroxide, starch, surfactants dispersing agents and soaps of metals (Paul et
al., 2012). So, in terms of its environmental impact, the textile industry is estimated
to use more water than any other industry, globally and almost all wastewater
discharged is highly polluted (Haasan, 2017). Average sized textiles mills consume
water about 200 L per kg of fabric processed per day (Wang et al., 2011; Kant,
2012). This highly colored textile wastewater severely affects photosynthetic
function in plant. It also has an impact on aquatic life due to low light penetration
and oxygen consumption (Neelu, 2017). It may also be lethal to certain forms of
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marine life due to the occurrence of component metals and chlorine present in the
synthetic dyes (Holkar et al, 2016).
Recently scientists are giving considerable attention on the use of biological-
based materials and their by-products as the biosorbent for the removal of pollutants
from different wastewaters because of presence of carboxyl, hydroxyl and amino
groups over their surfaces (Ay et al., 2012). These groups are responsible for the
biosorption process. Biological-based materials such as agricultural-based biomasses
are cheap and easily obtainable in considerably substantial quantities. Many
researchers have used agricultural-based biomasses such as cocoa shells (Meunier et
al., 2003), grape stalks (Martinez et al., 2006), hazelnut and almond shells (Pehlivan
et al., 2009), Capsicuum annuum seeds, (Ozcan et al., 2007), citrus wastes (Asgher
and Bhatti, 2010), rice husk (Safa and Bhatti, 2011) and barely husk (Haq et al.,
2011) .Agricultural by products are easily available in Malaysia so the present study
was designed to exploit the abundantly available agricultural wastes for the treatment
of textile effluents to remove color, COD, dissolved, turbidity and conductivity.

1.3 Project Objective

The objectives of this study are:


1. To treat textile industrial wastewater by NaOH treated pineapple leaves bio
sorbents.
2. To study the effects of bio sorbent dosage on reducing chemical oxygen
demand (COD), turbidity, electric conductivity and colour.
3. To study the functional groups that involve in adsorption process.

1.4 Project Scopes

The scopes of this research are:


1. Treat textile wastewater that contain dye by using treated pineapple leaves
bio sorbents. The pineapple leaves undergo chemical modification with
NaOH in order to increase the adsorption efficiency.
2. Study the effect of different amount of bio sorbent dosage (0.2g, 0.4g, 0.6g,
0.8g and 1.0g) on the adsorption efficiency of contaminant removal from
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textile wastewater and analyze the values of COD, DO, turbidity, colour and
conductivity in treated water.
3. Evaluate the characteristic of the bio sorbents in term of functional groups
that involved in adsorption process before and after bio sorption experiment
by using FTIR.
CHAPTER 2

LITERATURE REVIEW

2.1 Introduction of bio-sorbent from pineapple leaves

Pineapple is a tropical fruit also known botanically as Ananas comosus is


produced in large quantities in tropical country such as Malaysia. Pineapple leaf is a
by product of the extraction of pineapple fruit. These natural raw materials are not
only low cost, but also save the disposal cost and prevent the on-site burning.
Normally, leaves on farmland are used as a natural compost material or burned on
site after the harvest, creating a point source of air pollution (Weng et al, 2009).
Utilization of this waste for the treatment of wastewater is a win–win strategy
because it is also converts the waste into a useful material. Thus, the use of pineapple
wastes as bio-sorbent is an attractive alternative from both economical and
environmental point of view. Adsorbents processed from agriculture byproducts are
strongly recommended because of their local availability, cost effectiveness, and
reduced environmental effects (Li et al., 2008).
Pineapple leaves contains insoluble cell walls, on which some certain
functional groups such as carboxylate, aromatic carboxylate, phenolic hydroxyl, and
hydroxyl groups are able to adsorb contaminants (Conrad and Hansen, 2007). As
such, the leaves are potentially pollutant scavengers from aqueous solutions. Conrad
and Hansen (2007) stated that dye from textile wastewater are subject to being
adsorbed by carboxylic, phenolic, hydroxylic, and carbonyl groups in plant fiber
molecules through bio sorption
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2.2 Properties of pineapple leaves

Pineapple leaves is a versatile material and possesses some unique properties.


Pineapple leaves properties include physical and chemical properties.

2.2.1 Physical properties of pineapple leaves

The cellulosic fiber of pineapple leaves has carboxylic, phenolic, hydroxylic, and
carbonyl groups that have several favorable properties including shrinkage
capability, high sorption capacity good modifiability and recoverability and
insensitivity to toxic substances (Mopoung and Amornsakchai, 2016).
Those properties are used widely in various application. The physical
properties of pineapple leave are summarized in Table 2.1.

Table 2.1: Properties of pineapple leaves fiber by Asim et al., (2015)


Physical properties Pineapple leaf fibre
Length (mm) 3-9
Breadth (10-3 mm) 4-8
L/B ratio 450
Tenacity (gm/tex) 50
Young’s Modulus 60-82
Extension at break (%) 2-6
Density (Gm/cc) 1.48
Relative Humidity 11.8
Transverse swelling in water (%) 18-20

2.2.2 Chemical properties of pineapple leaves

The major constituents of pineapple leaf are cellulose (70–80%), lignin (5–12%),
and hemicellulose (Saha et al. 1991). Cellulose is a semi crystalline polysaccharide
consisting of D-glucopyranosyl units linked together by beta-(1-4)-glucosidic bond
(Bledzki & Gassan, 1999). The figure of cellulose is shown in Figure 2.1. Three
hydroxyl groups at the C2 and C3 positions of secondary hydroxyl groups and the C6
position of primary hydroxyl group can form intra and inter molecular hydrogen
bonds. These hydrogen bonds allow the creation of highly ordered, three dimensional
crystal structure. (Khalil et al., 2011).
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Figure 2.1: Chemical structure of cellulose (Yan et al., 2008)

Whereas lignin is a polymer of phenylpropane units which are highly complex


mainly aromatic and amorphous, but have less water sorption than other natural
components (Rowell et al., 1997). Figure 2.2 shows the structural unit in lignin.

Figure 2.2: Structural unit of lignin (Ralph, 2010)

Hemicellulose is branched, fully amorphous and has a lower molecular weight than
cellulose. It is partly soluble in water. Hemicellulose is hygroscopic due to its open
structure containing hydroxyl and acetyl groups (Frederick & Norman, 2004). Figure
2.3 shows the structural unit of hemicellulose.
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Figure 2.3: Structural unit of hemi cellulose (Wang, 2009)

2.3 Textile wastewater

Textile industry consumes huge amount of dyes and chemicals as well as large
amount of water and also produces large volumes of textile wastewater effluents. The
textile effluents contains different type of dyes, organic acid and salts, inorganic acid
and salts, bleaching agent, trace metals in variable concentration (Mostafa, 2015).
These untreated industrial effluents not only deteriorate surface water quality, ground
water, soil and vegetation, but also cause many diseases like haemorrhage, ulceration
of skin, nausea, severe irritation of skin and dermatitis (Nese et al., 2007). As the
textile wastewater is harmful to the environment and people, some environmental
protection agencies worldwide have imposed rules entrusted with the protection of
human health and guarding the environment from pollution caused by the textile
industry. These agencies imposed certain limits on the disposal of effluents into the
environment. Some of the regulations imposed by several countries. However, due to
the difference in the raw materials, products, dyes, technology and equipment, the
standards of the wastewater emission have too much items. It is developed by the
national environmental protection department according to the local conditions and
environmental protection requirements which is not fixed. It varies according to the
situation in different regions (Mostafa, 2015).
The characteristics of textile effluents vary and depend on the type of textile
manufactured and the chemicals used. Dyes in water give out a bad colour and can
cause diseases like haemorrhage, ulceration of skin, nausea, severe irritation of skin
and dermatitis (Nese et al., 2007). They can block the penetration of sunlight from
water surface preventing photosynthesis. Dyes also increase the biochemical oxygen
demand of the receiving water and in turn reduce the reoxygenation process and
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hence hamper the growth of photoautotrophic organisms (Nese et al., 2007). The
suspended solid concentrations in the effluents play an important role in affecting the
environment as they combine with oily scum and interfere with oxygen transfer
mechanism in the air water interface (Laxman, 2009). Inorganic substances in the
textile effluents make the water unsuitable for use due to the presence of excess
concentration of soluble salts. These substances even in a lower quantity are found to
be toxic to aquatic life (Tholoana, 2007). Some of the inorganic chemicals like
hydrochloric acid, sodium hypochlorite, sodium hydroxide, sodium sulphide and
reactive dyes are poisonous to marine life. The organic components are found to
undergo chemical and biological changes that result in the removal of oxygen from
water (Martha, 2014). There are strict requirements for the discharge of the waste
water as the wastewater is harmful to the environment and the human being by the
textile industry.

2.4 Parameters used for characterization of textile wastewater

In order to choose the best method to treat textile wastewater, the characteristic of
some parameters need to be analysed.

2.4.1 Chemical Oxygen Demand (COD)

The chemical oxygen demand or COD is the most widely used parameter for
wastewater characterization. It measures the oxygen equivalent of the organic matter
content that is susceptible to oxidation by a strong chemical oxidant. The methods to
analyse COD is described in the Standard Methods Handbook by the APHA (Alam,
2015). 'Standard methods' lists three methods; the open reflux method, the titrimetric
closed reflux method and the colorimetric closed reflux method. All three methods
use dichromate as an oxidant, which makes the description standard dichromate
method. Other methods for COD analysis, including the use of test kits or reagent
sets.
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2.4.2 Conductivity

Conductivity is used as a measure of the salt content of the wastewater, and serves
as an alternative for TDS. Factors influencing the conductivity are the presence,
concentration, mobility and valence of ions and the temperature (Zimmerman, 2017).
It is measured using a conductivity cell with a platinum or nonplatinum electrode
(Bischops et al, 2003). In textile processing, salts are mainly used to improve the
exhaustion of direct and reactive dyebaths. Additionally, salts can be formed as by-
product in other processes, for instance neutralisation (Spanjers, 2003) It is measured
using a conductivity cell with a platinum or nonplatinum electrode (Clesceri et al,
1998).

2.4.3 Colour

A major contribution to colour in textile wastewater is usually the dyeing and the
washing operation after dyeing which as much as 50% of the dye might be released
into the effluents (Joshi et al., 2004). Textile dyes are mainly cationic, anionic and
non-ionic dyes. The chromophores in anionic and non-ionic dyes are mostly azo
group or anthraquinone types. The reactive cleavage of azo linkage is responsible for
the formation of toxic amines in the effluents. Presence of colour in the waste water
is one of the main problems in textile industry. Anthraquinone based dyes are most
resistance to degradation due to their fused aromatic structure and therefore remain
coloured for long time in the textile wastewater. These colours are easily visible to
human eyes even at very low concentration. Hence, colour from textile wastes carries
significant aesthetic importance. Most of the dyes are stable and has no effect of light
or oxidizing agents (Joshi, 2003)
Quantitative analysis of dyes can be done by HPLC, DR6000 and high-
performance capillary electrophoresis, measuring concentrations of specific dyes
(Hao et al, 2000). Dye solutions have a very high variability in tinctorial
characteristics (Koh, 2011). Therefore, no generalizations can be made about the
specific 'amount' of colour (in units) produced by a certain amount of dye (Robert
1996). A complex dye solution can show light absorption in a UV-VIS spectrum
range from 250 - 600 nm (Hao et al, 2000). In many countries legal limits have been
developed, defining the maximum absorbance at three fixed wavelengths (Bechtold
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et al, 2001). When comparing different methods for colour measurement, a high
correlation between the ADMI, dilution ratio and Lovibond methods was discovered.
Quantitative conversion between the units is possible. The transparency method
however, showed no correlation with the other three methods (Kang et al, 1999). In
the literature colour is often specified as absorbance at a single wavelength (usually
465 nm) (Hongve & Akesson, 1996). As all colours are related to absorption of light
at different wavelengths, this method can not represent the colour of wastewaters as
complex as a mixed textile effluent (Hao et al 2000). Furthermore, many factors for
example suspended solids can disturb spectrophotometric measurements. A lightly
coloured stream with a high suspended solids content would result in too high colour
values when the solids are not removed (Branigan, 2013). He stated that, removal of
the solids can lead to a value that is much lower than the colour that is actually
experienced by the human eye. Single dyeing streams with low turbidity however,
should pose no problems (Branigan, 2013).

2.4.4 Turbidity

Turbidity is a measure of the light-scattering properties of the wastewater. Therefore,


turbidity is of importance when measuring wastewater colour (Grobbelaar, 2009). It
is calculated by comparing the intensity of light scattered by a sample, compared
with a reference suspension under the same conditions (Smith, 1996). Suspended
matter, soluble coloured organic compounds and microorganisms all contribute to the
turbidity. The higher the intensity of light scattered by the sample, the higher the
value (Perlman, 2016). For measurements a turbidimeter is used, consisting of a
nephelometer with a light source and detector(s) for indication of the intensity of the
light scattered at 90° (Clesceri et al, 1998). Turbidity is usually given in FTU
(Formazin Turbidity Unit) or NTU (Nephelometric Turbidity Unit) values. Both
units give the same value (Anderson, 2005).

2.5 Effluent discharge standards

Wet processing of textiles involves, in addition to extensive amounts of water and


dyes, a number of inorganic and organic chemicals, detergents, soaps and finishing
chemicals to aid in the dyeing process to impart the desired properties to dyed textile
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products (Mahfuz, 2009). He reported that residual chemicals often remain in the
effluent from these processes. In addition, natural impurities such as waxes, proteins
and pigment, and other impurities used in processing such as spinning oils, sizing
chemicals and oil stains present in cotton textiles, are removed during scouring and
bleaching operations. He also reported that, this results in an effluent of poor quality,
which is high in BOD and COD load. Table 2.2 lists typical values of various water
quality parameters in untreated effluent from the processing of fabric and compares
these to the DOE effluent standards for discharge into an inland surface water body.
As demonstrated, the effluent from textile industries is heavily polluted (Laursen et
al, 1997)

Table 2.2: Parameters of effluent compared with DOE (Law of Malaysia, 1994).
Parameters DOE Standards for wastes from industrial
units
Appearance -
pH 6-9
Color -
Heavy metal Depends on type of metal
Suspended solids 150
Total Dissolved Solids 2100
Chemical Oxygen Demand 200
Biochemical Oxygen Demand 50
Oil and grease 10
Surfactants -
Sulphide 1

2.6 Textile effluent treatment processes

Many pollutant removal technological processes have been developed in the past
decades to treat the textile wastewater. The treatment processes is being chosen on
the basis of composition, characteristics and concentration of material present in the
effluents.

2.6.1 Physical method

Physical methods are useful for the decolorization of wastewater containing disperse
dyes. They also have low decolorization efficiency for the wastewater having
reactive and vat dyes (Oliver et., 2000). These techniques also limit their use due to
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the low decolorization efficiency and large generation of resultant sludge (Liang et
al., 2014). Adsorption approaches have attracted significant attention due to their
greater decolorization efficiency for wastewater containing a variety of dyes (Holkar
et al., 2016). High affinity, capability for the compounds and adsorbent regeneration
ability are the main characteristics which need to be considered during the selection
of an adsorbent for color removal (Jadhav and Srivastava, 2013). Activated carbon is
an effective adsorbent for a wide range of dyes. But, its high price and difficulty in
its regeneration limits the application for decolorisation (Galan et al., 2013). For
economically practicable application of the adsorption method, some researchers
used a low costs adsorbent material such as peat, bentonite clay, fly ash and
polymeric resins (Kyzas, 2014). Some scientists also tried many biotic resources like
wheat residue, treated ginger waster, ground nut shell charcoal, date stones and
potato plant waste for the decolorisation of textile wastewater (Sundaram and
Sivakumar, 2012). However, applications of these adsorbents have been restricted by
the several problems such as its regeneration and/or dumping, sludge generation and
high price of the adsorbent (Gupta et al., 2011). According to Gupta et al., (2011),
stated that adsorbents should be applied to processes that have low concentrations of
pollutants or when the adsorbent has a low cost or can be easily regenerated.
Filtration techniques like ultrafiltration (UF), nanofiltration (NF) and reverse
osmosis (RO) have been used to recover and reuse a water. For the choice of the
filter and its permeability, it is necessary to consider the content and the temperature
of textile wastewater essential for the separation method (Le and Nunes, 2016). In
textile industry, an application of membranes delivers exciting potential for the
recycle of hydrolysed reactive dyes and auxiliaries used during dyeing which
concurrently decrease the biological oxygen demand (BOD), chemical oxygen
demand (COD) and color from the textile wastewater (Chollom et al., 2015). But,
membranes also have a significant disadvantages such as its cost of initial
investment, possible fouling of membrane and the generation of another wastes
containing water insoluble dyes (e.g. indigo dye) and starch which need further
treatment (Koyuncu and Güney, 2013).
14

2.6.2 Chemical method

One of chemical method of textile wastewater treatment is oxidation. These are the
most usually used methods of degradation of dyes by chemical means due to its
easiness of application (Farhad et al., 2009). According to Farhad et al., (2009),
these oxidation technologies can be categorized as advanced oxidation processes
(AOP) and chemical oxidation. These processes have the ability to degrade the toxic
initial and their by product chemicals, dyes, pesticides, etc. either partly or
completely under ambient conditions. Farhad et al., (2009) also reported that these
oxidation technologies can be used individually as well as in synergism with each
other. This synergism is termed as the hybrid advanced oxidation process (AOP)
technologies Advanced oxidation processes (AOP) are the processes in which
hydroxyl radicals are produced in adequate amounts. These hydroxyl radicals are
powerful oxidizing agents. Hydroxyl radicals react with most dyes with high rate
reaction constants (Asghar et al., 2015). These hydroxyl radicals are also be able to
oxidize majority of the complex organic and inorganic chemicals present in the
textile effluent water. These AOP processes contain cavitation, generated either by
means of ultrasonic irradiation termed as acoustic cavitation (Jadhav et al., 2015) or
via constrictions like orifice, venturi, etc. in the hydraulic devices termed as
hydrodynamic cavitation Gogate et al., 2015). Based on Gogate et al., (2015), these
AOP processes also involve photocatalytic oxidation and Fenton chemistry. Fentons
reagent is an appropriate chemical (mostly an iron salt) which promote oxidation of
complex organic pollutant (by promoting H2O2 decomposition), which are resistant
to biological degradation. It has also been shown to be operative in degrading both
soluble and insoluble dyes. One main drawback of Fenton method is the iron sludge
generation due to combined flocculation of the reagent and the dye molecules
(Babuponnusami and Muthukumar 2014). Chemical oxidation methods use
oxidizing agents like O3 and H2O2 (Brienza and Katsoyiannis, 2017). Brienza and
Katsoyiannis, (2017) stated that ozone and H2O2 forms strong non-selective
hydroxyl radicals at high pH values. Brienza and Katsoyiannis, (2017) also stated
that these radicles due to this high oxidation potential can effectively break down the
conjugated double bonds of dye chromophores as well as other functional groups
such as the complex aromatic rings of dyes. Subsequent formation of smaller non-
15

chromophoric molecules decreases the colour of the effluents (Tehrani-Bagha et al.,


2010)
Degradation of the dye is also possible by the combined treatment of UV
light and the H2O2 due to the production of high concentrations of hydroxyl radicals
(Holkar et al., 2016). According to Holkar et al., (2016), this combined method of
UV light and the H2O2 is advantageous for dye-containing textile effluent due to no
sludge production and reduction in foul odors. Here, UV light is used to activate the
decomposition of H2O2 into hydroxyl radicals. Holkar et al., (2016) stated that these
hydroxyl radicals cause the chemical oxidation of dye or organic material,
mineralizing the same to CO2 and H2O. The parameters such as UV radiation
intensity, pH, structure of dye molecule and the dye bath composition need to be
optimized to get a more rate of dye removal (Soares et al., 2013; Yen, 2015). Thus,
free radicals can be generated by the combination of ozone with hydrogen peroxide
(Muhammad et al., 2008). In other way, free radicals can also be produced by the
action of ozone or hydrogen peroxide in presence of the energy dissipating
components (Gogate and Pandit, 2003). Here, UV, sun light or ultrasound are the
energy dissipating components (Saharan et al., 2014). These hybrid techniques have
lesser treatment times as related to any one of the individual methods but are also
associated with higher energy cost (Bagal and Gogate, 2014).

2.6.3 Biological method

The biological process removes only the dissolved matter such as sulfides,
chromates, and color
in textile wastewater (Mostafa, 2016). The removal efficiency is influenced by the
ratio of organic load/dye and the microorganism load, its temperature, and oxygen
concentration in the system. On the basis of oxygen requirement (Pramnik et al,
2009).Biological methods can be classified into aerobic, anaerobic and anoxic or
facultative or a combination of these. An aerobic method use microbes for the
treatment of the textile wastewater in presence of oxygen while an anaerobic
methods use microbes to treat it in absence of oxygen (Kulkarni et al., 2009). The
combination of anaerobic and aerobic method is typically implemented in real
practice which use an anaerobic process to treat textile wastewater of chemical
oxygen demand (COD), followed by the use of aerobic polishing treatment to treat
16

the resulting textile wastewater of low COD (Wang et al., 2011). Generation of
“methanogenic biogas” by anaerobic process is possible only if the wastewater has a
rather high COD, higher than 3 g/L, which is the case for desizing wastewater
containing more biodegradable organic compounds such as polyvinyl alcohol (PVA)
or starch (Rongrong et al., 2011).
In biological methods, microorganisms adapt themselves to textile dyes and
new resilient strains grow naturally out of survival requirement, which then convert
several dyes into less hazardous forms. In this system, the biodegradation mechanism
for recalcitrant dyes is based on the stroke of the enzymes such as laccase, lignin
peroxidase, NADH-DCIP reductase, tyrosinase, hexane oxidase and aminopyrine N-
demethylase (Solís et al., 2012). The biological methods for the complete
degradation of textile wastewater have benefits such as: (a) eco-friendly, (b)
costcompetitive, (c) less sludge production, (d) giving non-hazardous metabolites or
full mineralization (e) less consumption of water (higher concentration or less
dilution requirement) compared with physical/oxidation methods (Hayat et al.,
2015).
The efficiency of biological methods for degradation depends on the
adaptability of the selected microbes and the activity of enzymes (Joutey et al.,
2010). According to Joutey et al., (2010), a large number of microorganisms and
enzymes have been isolated and tried for the degradation of several dyes. The
isolation of potent microbes and its use for degradation is an interesting biological
aspect of textile wastewater treatment. Joutey et al., (2010) reported that a wide
range of microorganisms such as bacteria, fungi and algae are able to degrade a wide
variety of dyes present in the textile

2.6.4 Biosorption

Biosorption is defined as a property of certain molecules (or types of biomass) to


bind and concentrate selected ions or molecules from aqueous solutions (Volesky,
2007). It is an alternative technology to remove heavy metals from dilute aqueous
solutions using inactive and dead biomasses (various kinds of microorganisms,
agricultural and fermentation wastes) to bind and accumulate these pollutants by
different mechanisms such as physical adsorption, complexation, ion exchange, and
surface microprecipitation (Aksu et al, 1991). Biosorption process has received great
17

attention in recent years as a more economical alternative method in place of current


adsorption processes since it utilizes not only plant materials but also a wide variety
of microorganisms in dead, pretreated and immobilized forms as adsorbing agents.
These materials are cheap to produce and carry wide range of binding sites for dye
molecules.
Adsorption of the dye molecules on the surface of absorbents are typically
highly heterogeneous by its nature and a complicated process, in which various
mechanisms may be involved (Muraleedharan et al, 1991). Due to the ionic nature of
the dye species in wastewater, electrostatic forces between the dye species and
ionized active groups on the absorbent surface plays an important role (Aksu and
Isoglu, 2005). Chemisorption as well as ion-exchange and other physical phenomena
will participate in the dyes absorption process, but their proportions and significance
may differ for different dyes and different kinds of absorbents (Volesky, 2007).
Carboxylic and hydroxylic functional groups are commonly present in the structure
of most natural absorbents (Aksu and Isoglu, 2005). These groups undergo
dissociation at suitable pH values, forming negatively charged sites on the absorbent
surface, which facilitates the retention of cationic dyes (Aksu and Isoglu, 2005).
Biosorption involves integration both of active and passive transport
mechanisms starting with the diffusion of the adsorbed component to the surface of
the cell (Arnold, 2009). Once the component has diffused to the cell surface, it will
bind to sites on the cell surface, which exhibit some chemical affinity for the
component (Dogar et al., 2010). The interactions between absorbents and dyes
depend on the chemical properties of all the reaction partners (Jimenez et al, 2015).
Each dye has certain affinity to various absorbents and on the other side one
absorbent is able to bind to more than one type of dyes (Dogar et al., 2010). In order
to prepare the absorbents for biosorption, all the biomasses both living and dead are
heat killed, dried, acid and/or otherwise chemically treated first (Azizian, 2004).
CHAPTER 3

METHODLOGY

3.1 Introduction

This chapter discussed the material, equipment and experimental procedure about
this research. In this study, five main parts of the methodology is proposed which are
the preparation of bio sorbent, the pre-treatment of bio sorbent, collection of
wastewater, adsorption of pollutant from textile wastewater and analysis of treated
water. The overview of methodology for this research is summarize in Figure 3.1.
In order to enhance the pore size and increase the surface area of the bio
sorbent, it was treated with NaOH. This study also aims to analyse the effect of bio
sorbent dose (0.2g,0.4g,0.6g,0.8g,1.0g) on the adsorption efficiency of COD,
conductivity, turbidity and colour removal from textile wastewater.
19

Figure 3.1: The flow chart of the experimental procedure


20

3.2 Material and apparatus

The material and apparatus that being used in the experiment were cloth bag,
measuring cylinder, beakers, volumetric flask, burette, dropper, conical flask, pH
meter, DO meter, DR200 thermostat, DR 6000 uv-vis spectrophotometer, turbidity
meter, conductivity meter, water bath, magnetic stirrer, grinder, oven, analytical
balance, plastic container, aluminium foil, tongs and evaporating dish.

3.3 Sample wastewater

The sample was collected from the textile wastewater treatment plant located at Batu
Pahat, Johor as shown in figure 3.2. The sample then was stored in chiller room at
4oC for 7 days period to avoid the physico-chemical characteristics loss (Aksu and
Isoglu, 2005). The initial readings of COD, DO, turbidity, conductivity and color was
taken.

Figure 3.2: Raw wastewater collected from textile industry


21

3.4 Experimental Procedure

In this research, there are three parts of the experimental procedures that has been
conducted. The three parts are preparation of bio sorbents, analysation of functional
groups that involve in biosorption process on the NaOH treated bio sorbents,
adsorption of wastewater by bio sorbent and analysis of colour, turbidity,
conductivity, dissolved oxygen and COD.

3.4.1 Preparation of bio sorbents

The raw materials were obtained from the local plantation in Semerah, Batu Pahat,
Johor, Malaysia. Fresh leaves were taken from plants at harvesting time. The
pineapple leaves were cleaned and washed for several times with tap water in order
to remove dirt and impurities. The leaves then were cut into small pieces. The leaves
were boiled in water bath at 95ºC to remove colour of the leaves (Mopoung et al,
2016).

Figure 3.3: Water bath used to boil pineapple leaves

It was then treated with 1 M NaOH using a 1:10 ratio of weight/volume (1g
of leaves/10ml of NaOH solution) (Mopoung et al, 2016). The treatment was
conducted in three batch. 25 g of dried leaves were treated with 250 mL of NaOH
22

solution for each batch. The slurry mixtures were boiled for 2 h with stirring at 700
rpm (Mopoung et al, 2016). Figure 3.4 on the left shows the mature pineapple leaves
meanwhile Figure 3.4 on the right shows the air dried pineapple leaves. Figure 3.5 on
the left shows the pineapple leaves being treated with NaOH solution at 150oC and
700 rpm for 2 hours meanwhile figure 3.5 on the right shows the treated bio sorbents
after being washed for several times until pH 7 and oven dried for 24 hours.

Figure 3.4: Mature pineapple leaves (left) ; the air dried leaves (right)

Figure 3.5: NaOH treated leaves (left) ; treated bio sorbents(right)

After that, boiled slurry mixtures were washed for several times with distilled
water until pH 7-7.5. The washed slurry mixtures oven dried at 100 ºC for 24 h
(Mopoung et al, 2016). Figure 3.6 shows the oven used during the drying process of
NaOH treated pineapple leaves.
23

Figure 3.6: Oven used during the drying process of NaOH treated pineapple leaves

The dried leaves were blended to become bio sorbent. It was stored in
dessicator for further use to prevent the exposure from air and humidity as it can wet
the bio sorbents (Mopoung and Kengkhetkit, 2016). .

3.4.2 Characterization of the bio sorbent

The functional groups that involve in biosorption process on the NaOH


treated bio sorbents were analyzed by Fourier-transform infrared spectrophotometer
(FTIR) model Cary 660 FTIR, Agilent Technologies. FTIR analysis was carried out
in order to identify the different functional groups present in pineapple leaves which
were responsible for adsorption process. Characterization analysis was conducted for
both bio sorbents before and after the bio sorption process. Fourier-transform
infrared of the pineapple leaves were recorded in the range of (400-6000 cm-1) with
scanning resolution of 8 cm-1 and 16 scans in open beam air background in the mid
IR region (NJoki et al., 2016).
24

Figure 3.7: FTIR used for bio sorbent characterization

3.4.3 Adsorption of textile wastewater by bio sorbent.

The adsorption of pollutant on pineapple leaves bio sorbent was studied by


batch technique. Batch adsorption studies were carried out using 250 ml conical
flasks containing 100 mL of dye wastewater with different dosage of dry NaOH
treated adsorbents. Bio sorbents was packed in cloth bag (Mopoung and Kengkhetkit,
2016). According to Mopoung and Kengkhetkit (2016), bio sorbent was packed in
cloth bag to ease the separation process of bio sorbent and wastewater. Six different
conical flasks prepared containing 100 ml effluent and bio sorbents were prepared on
the basis of dosage values as 0.2g, 0.4g, 0.6g, 0.8g, 1.0g and blank. The conical flask
were covered with aluminum foils. The conical flasks were agitated at 150 rpm in
incubator rotary shaker, model Thermostable 1S- 10RL, Daihan Scientific. The
adsorption process was incubated at 30oC for 2 h (Mopoung and Kengkhetkit, 2016).
25

Figure 3.8: Incubator rotary shaker used during adsorption process

3.5 Analysis of textile wastewater

The values COD, DO, turbidity, conductivity and colour in textile wastewater were
analysed before and after adsorption process. The procedure described below.

3.5.1 Analysis of COD

Reagent of COD was prepared by adding 1.5ml K2Cr2O7, 3.5 ml of sulfuric acid
reagent and 2.5 ml of wastewater into vial. The solution was shaken well. Blank
solution was prepared without addition of wastewater sample. The solution being
heated at 150oC for 2 hours with DR200 thermostat (Westwood, 2006).
26

Figure 3.9: DR200 thermostat used to reflux the COD reagent

The solution was cooled down to room temperature after the refluxing period.
The reagent was poured into 250 ml conical flask and added with 3 drops of Ferroin
indicator solution. The solution was titrated with 0.1 N of Ferrous ammonium
sulphate (FAS) Fe(NH4)2(SO4)2 and the volume of FAS used was recorded (John
Stone, 2010). According to Toprak (2017), the value of COD is calculated by using
the following formula:

COD mg/L = (a-b) (N) x 8000/ sample size, mL (1)

Where: a = volume of FAS used for blank, mL


b = volume of FAS used for sample, mL
N = normality of FAS, N

3.5.2 Analysis of DO

The quality of treated water has been analysed by using analytical method. Dissolved
Oxygen in textile wastewater before and after adsorption process was measured by
using Hanna Series benchtop meters. The readings were recorded and the average
27

values was calculated. The figure of DO meter used to measured DO in treated water
is shown in Figure 3.10.

Figure 3.10: DO meter used to measured DO in treated water

3.5.3 Analysis of turbidity

The turbidity in textile wastewater before and after adsorption process was measured
by using turbidity meter, model TN 100, Eutech Instruments. 10ml of wastewater
was filled into the vial and put into the turbidity meter. The readings of turbidity was
measured by pressing ‘Measure’ button. Figure 3.11 shows the turbidity meter used
to measure turbidity of treated wastewater.
28

Figure 3.11: turbidity meter used to measure turbidity of treated wastewater

3.5.4 Analysis of conductivity

The initial and final conductivity value in textile wastewater was measured by using
conductivity meter. The probe dipped into the wastewater and readings were
recorded for triplicate in order to calculate the average readings.

3.5.5 Analysis of color

Concentration of color in untreated and treated wastewater has been examined by


using the analytical method. Concentration of color was determined by DR6000 uv-
vis spectrophometer as shown in figure 3.12 (Camargo et al, 2017). The wavelength
measured was at 500 nm. The program was started by selecting 97 Color ADMI 1
inch. Sample cell was filled with 10 mL of distilled water act as blank. Press ZERO
button to display the scan status, then 0 ADMI Value. Sample cell then filled with 10
mL of sample and take measurement by pressing READ button (Hach DR6000 User
Manual, 4th Edition, 2018).
29

.
Figure 3.12: DR6000 uv vis spectrophotometer
CHAPTER 4

RESULT AND DISCUSSION

4.1 Introduction

This chapter discussed the results that have been obtained from the experimental
works that has been conducted according to the procedures in chapter 3. The
experiments were conducted to check out the effect of bio sorbent dose on the
removal of COD, turbidity, conductivity and colour by varying the mass of bio
sorbent (0.2g, 0.4g, 0.6g, 0.8g and 1.0 g) and results are presented in form of graph.
The readings of blank sample for COD, DO, conductivity, turbidity and colour of
textile effluent were collected and tabulated in table 4.2. The data collected were
analysed and recorded in the form of table and graph. Furthermore, the results
collected were discussed. The raw data collected was tabulated in appendix A.
However, optimum dosage of bio sorbent for reduction of COD, conductivity,
turbidity and colour were undetermined due to some experimental error. Section 4.7
will discuss the possible error that occurred during the experiment.

4.2 Characterisation of bio sorbent

FTIR spectroscopy characterisation of bio sorbent was conducted as preliminary


qualitative analysis of chemical groups presents on the surface of the sample and to
determine the functional groups that commonly involve in adsorption process such as
carboxylic and hydroxyl group. The FTIR spectra is shown in Table 4.1. As shown in
figure 4.1, the physical appearance of pineapple leaves after treated with NaOH was
31

white in colour, having no impurities and dirts. The green colour and the lignin
components of pineapple leaves was completely removed.

Figure 4.1: Pineapple leaves bio sorbent

Table 4.1: FTIR of the bio sorbent before and after the adsorption process
IR peak Before adsorption After adsorption Functional group

1 3334 cm-1 3330 cm-1. Bonded –OH


groups,
Krishni et al, 2014
2 1315 cm-1 1315 cm-1 Bonded –OH
groups,
Krishni et al, 2014
3 2904 cm-1 2362 cm-1 Two bands for -
CH2 groups,
Esmaieli, 2014
4 1645 cm-1 - C=O stretching of
COOH groups,
Monanty et al.
2000
5 1,159 cm-1 1159 cm-1 C–O–C bridge
Maniruzzaman et
al, 2012
6 426 cm-1 426cm-1 C-H groups.
Krishni et al, 2014
7 897 cm−1 - –C–H bending
Krishni et al, 2014
8 - 503 cm-1 C-H groups
Krishni et al, 2014
9 - 667cm-1 C–O–H twist broad
Krishni et al, 2014
.
32

As shown in figure 4.2, the broad and intense band at 3334 cm-1 indicate the
vibration of hydroxyl group (OH-) on the cellulose and lignin of pineapple leaves
(Krishni et al, 2014). According to Krishni et al., (2014), the broad and intense band
ranging from 3,333 to 3,345 cm−1 was due to –OH vibration in cellulose and lignin.
The existence of OH group on the bio sorbent enhance by the chemical treatment of
pineapple leaves with NaOH (Aweed, 2008). Krishni (2014) also stated that the
peaks at 1315 cm-1 also indicate the presence of OH group. Krishni (2014) reported
that the peaks between 1314 to 1,318 cm-1, corresponded to the presence of –OH.
The peak at 2904 cm-1 is attributed to the C-H stretching vibration from the CH2
group of cellulose and hemi cellulose.(Esmaieli,2014). According to Esmaieli
(2014), the peak at between 2900 to 2,920cm−1 is due to –CH stretching vibration.
The peaks which appeared around 1645 cm-1 was due to the C-O bond of carboxylic
group (> C-O) in the hemicelluloses (Monanty et al. 2000). Monantry et al., (2000)
reported that the peaks between 1643 to 1645 cm-1 due to C-O bond of carboxylic
group. The prominent peaks at 1,159 cm-1 can be ascribed to the antisymmetric C–
O–C bridge in the pyranose ring of cellulose (Maniruzzaman et al, 2012). As
reported by Maniruzzaman et al., (2012), the peaks between the prominent peaks at
1,158 to 1,159 cm−1 can be ascribed to the antisymmetric C–O–C bridge in the
pyranose ring of cellulose. The existence of weak band in the region of 426 cm-1 and
897 cm−1 indicates the C-H bending vibration of cellulose (Krishni et al, 2014).
Krishni et al., (2014) reported in their studies that the peaks at 400 to 900 cm-1
represent vibrations, spectra due to C–H bonds.
33

Figure 4.2: FTIR spectra of pineapple leaves bio sorbent before adsorption process

4.3 FTIR spectra after adsorption process

As shown in figure 4.3, after adsorption process, the adsorbent detected some shift,
disappear and new peaks, elucidating possible involvement of the functional groups
during the adsorption process. The spectra of bio sorbent after the treatment of textile
wastewater is shown in figure 4.3. As we can see in the figure 4.3, -OH stretching
was shifted from 3334 cm-1 to 3330 cm-1. The peaks of C-H stretching also shifted
from 2904 cm-1 to 2362 cm-1. This was due to substitution of hydrogen atom by the
dye atoms (Macharia et al, 2016). Macharia and others (2016) stated that the
functional groups that have a hydrogen atom, for example O-H and C-H can possibly
have the atom replaced by the dye atom. In the figure 4.2, there was disappearance of
peaks which is at 1645cm-1 of C-O bond. These results implies the presence of
unfilled orbitals in the pollutant allow bonding with lone pair of functional groups in
C-O bond (Macharia et al, 2016). This is likely to take place in the functional groups
containing elements that have lone pairs of electrons. These include C-O which
presence of unfilled orbitals in the dye allow bonding with the lone pairs of electrons
found in the functional groups present. The peak at 1315 cm-1 and 1159 cm-1 of O-H
and C-O-C bond were remains unchanged. The dominant peaks observed at 426cm-1
and 503 cm-1 suggest the presence of C–H vibrations of cellulose. Presence of peaks
at 667cm-1 indicated the C–O–H twist broad. These differences could be related to a
34

possible involvement of specific functional groups on the pineapple leaves bio


sorbent surface during the adsorption process (Ramesh et al, 2014).

Figure 4.3: FTIR spectra of pineapple leaves bio sorbent after adsorption process

4.4 Blank sample analysis

The blank sample was prepared by pouring exactly 100 ml of effluent into a conical
flask and agitated in rotary incubator shaker with 150 rpm agitation speed, at 30oC
for 2 hours without bio sorbent addition. The readings of COD, DO, conductivity,
turbidity and colour were taken for triplicate and the average was calculated.
Readings of blank sample were recorded in order to determine the potential of
pineapple leaves bio sorbents in reducing pollutant from textile effluents.
Table 4.2: Readings of blank sample
Parameters Readings
COD (mg/l) 174.3
DO (mg/l) 4.54
Conductivity (µS/cm) 1585.2
Turbidity (NTU) 34.5
Colour (ADMI) 518.6

4.5 Analysis of textile wastewater

Table 4.3 showed the results of the raw wastewater before treatment of COD, DO,
conductivity, turbidity and colour. From the table, we can observe that textile
35

effluent can be characterized with having orange brownish colour, high COD, high
turbidity and conductivity which is higher than the values of COD, DO, conductivity,
turbidity and colour after adsorption process. Thus, it is needed to be treated before
being discharged into water body such as rivers and lakes. From the experimental
findings, one of the methods that can reduce COD, conductivity, turbidity and colour
from textile effluent is adsorption by pineapple leaves bio sorbents.

Table 4.3: Results of the raw wastewater before treatment


Dosage CODi DOi ECi Turbidityi Colori
(g) (mg/L) (mg/L) (µS/cm) (NTU) (ADMI)
0.2 176.2 4.48 1655.5 36.4 521.3

0.4 173.1 4.12 1637.4 34.5 524.0

0.6 169.2 4.4 1640.0 35.6 524.1

0.8 171.3 4.32 1652.4 33.5 522.2

1.0 173.0 4.44 1634.8 34.2 519.8

Where CODi = initial COD readings


DOi = initial DO reading,
ECi = initial electric conductivity,
Turbidityi = initial turbidity reading
Colori = initial color reading

4.5.1 Effect of bio sorbent dosage on COD

During the biosorption process, the amount of bio sorbent plays a very significant
role. As shown in the figure 4.4, the COD removal was reduced as the dosage of bio
sorbent increased. The readings of COD decreased gradually with increased of bio
sorbent dose from 176.2 mg/l to 76.mg/l.The value of COD obtained were 142.3
mg/l, 128.1 mg/l, 109.33 mg/l, 97.4 and 76.8 mg/l for 0.2g, 0.4g, 0.6g, 0.8g and 1.0g
of bio sorbent dosage. The lowest value of COD recorded was 76.8 mg/l by using 1g
of pineapple leaves bio sorbent. Patel and Vashi (2010) also worked on the treatment
of real textile effluents through adsorption and while investigating the effect of bio
36

sorbent dose, they found similar trend of increasing COD reduction by increasing
corncobs biomass adsorbent dose. The percentage removal of COD was found from
57.3 to 87.6% for 1 to 11g of adsorbent respectively. However, Patel and Vashi
(2010) found the optimum dosage and observed at 8g. The optimum dosage was not
successfully identified due to some error during experimental procedure.
The value of COD decreased as the bio sorbent dosage increased due to
increased adsorbent surface area and availability of more adsorption sites. This is
because, as the bio sorbent immersed in the textile wastewater, this may be attributed
to the existence of the functional groups and the surface area of the prepared bio
sorbent, and therefore, there were active sites available for the adsorption of
chemical toxic, less organic compounds can be chemically oxidised thus reduced the
COD value from the aqueous solution (Zhang et al. 2012).

Figure 4.4: COD vs dosage


37

4.5.2 Effect of bio sorbent dosage on DO

Based on figure 4.5, the graphs show the increment of dissolve oxygen (DO) versus
dosage of bio sorbent used during adsorption process. According to figure 4.5, as
expected, the readings of DO in treated wastewater is increased as the bio sorbent
dosage increased. The values of DO increased rapidly as the dosage increased from
4.92 mg/l to 7.22 mg/l for 0.2 to 1.0g. COD and DO in treated wastewater are
depending on each other. Based on the theory, when COD is reduced, DO will
increase (Ravzy, 2017). As studied by Kulkarni, Patil and Bhalerao (2011), they
found that, as the bio sorbent dosage increased, the DO value in treated wastewater
also increased. They reported that the DO of the diluted effluent (1% concentration)
increased from 3 mg/l to 8.5 mg/l for 1g to 6g of dosage.

Figure 4.5: DO vs dosage

4.5.3 Effect of bio sorbent dosage on conductivity

Other parameter that shows significant improvement after treatment process is


conductivity. Before treatment, the value of conductivity in the range of 1634.8-
1655.5 µS/cm, which is very high than the permissible limits which is 1000μS/cm
according to National Water Quality Standards for Malaysia as shown in table 4.4
which indicates the highest degree of pollution.
38

Table 4.4: Conductivity Limits in National Water Quality Standards for Malaysia
Parameter Unit Class
I IIA IIB III IV V
Conductivity µS/cm 1000 1000 - - 6000 -

From the figure 4.6, adsorption process by bio sorbent really helps in
reducing value of conductivity in wastewater. After adsorption process, the value
decreased up to more than 50% than the initial value of untreated wastewater. The
maximum decrease in conductivity was observed at bio sorbent dosage of 1.0g and
the least was observed at that dosage of 0.4g. From the figure 4.4.1, the conductivity
reduction were 823.7µS/cm, 976.1µS/cm, 896.8µS/cm, 653.3 µS/cm and 641.9
µS/cm at dosage of 0.2g,0.4g,0.6g,0.8 and 1.0g respectively. The maximum decrease
in conductivity was observed at bio sorbent dosage of 1.0g for 641.9 µS/cm and the
of adsorption efficiency can be reached until 60.8%. The existence of anion groups
such as carbonyl and alcohol on the surface of pineapple leaves increase the
possibilities to adsorb cation groups from textile wastewater (Banerjee et al, 2017).
Bhatti et al (2015) also reported that increasing sugarcane bagasse bio sorbent
dosage, the reduction of conductivity also increased. He reported that the
conductivity was reduced from 2299 µS/cm, 2027 µS/cm, 2005 µS/cm, 1568 µS/cm
and 1302 µS/cm for 0.05, 0.1, 0.15, 0.2 and 0.3 g 50 mL-1 of sugarcane bagasse bio
sorbent dosage.
39

Figure 4.6: Conductivity vs dosage

4.5.4 Effect of bio sorbent dosage on turbidity

The turbidity of textile wastewater was found to be in the range of 33.5 – 36.4 NTU
before treatment. According to figure 4.7, the turbidity of bio sorbent dosage at 0.2g
was found to be highest and that of dosage at 1.0 g was lowest. From the figure, the
treatment decreased the turbidity of textile wastewater to 25.8 NTU for 0.2g bio
sorbent dosage, 23.3 NTU for 0.4g bio sorbent dosage, 21.7 NTU for 0.6g bio
sorbent dosage, 20.2 NTU for 0.8g bio sorbent dosage and 19.5 NTU for 1.0g bio
sorbent dosage. The treatment of textile wastewater by bio sorbent from pineapple
leaves decreased the turbidity up to percentage of 42.9% for 1.0g amount of dosage
used during adsorption process. Removal of dye after adsorption treatment caused
the total suspended solids and turbidity of the textile wastewater to decrease. Daniel
(2015) reported the same trend in his study on turbidity removal by maize cobs
adsorbent. He stated that the percentage removal of turbidity from water increases
with increase in adsorbent dose because as the adsorbent dose is increased more
surfaces are available for adsorption. He reported that percentage removal was
increased from 15%, 52%, 55%,58% and 60% for 0.1g, 0.2g,0.3, 0.4g, 0.5g of
dosage.
40

Figure 4.7: Turbidity vs dosage

4.5.5 Effect of bio sorbent dosage on colour

Figure 4.8 shows the treated textile effluent after adsorption process. As shown in the
figure, the colour of wastewater after adsorption process slightly turned to clear. As
the dosage of bio sorbent increased, the general appearance of effluent became less
turbid. The peach colour of the effluent moderately the peach colour turned lesser.

1.0g 0.8g 0.6g 0.8g 0.2g

Figure 4.8: Appearance of water sample


41

Adsorbent dosage is one of the important parameters studied while


conducting batch mode studies. The effect of adsorbent dosage on the removal of dye
from wastewater was studied by varying dosage from 0.2 g to 1.0 g. From the results
it was found that adsorption was highly dependent on adsorbent concentration and it
increased with increase in adsorbent dosage. From the figure 4.9, it indicates that the
readings of color were 297.5 ADMI, 272.8 ADMI, 224.2 ADMI, 243.4 ADMI and
218.5 ADMI for 0.2g,0.4g,0.6,0.8g and 1.0g of dosage respectively.

Figure 4.9: Colour vs dosage

The increase in biosorption of dyes by increase in bio sorbent dose can be


attributed due to the fact that at higher bio sorbent doses, the surface area and hence
the binding sites available for the attachment of dye molecules increased which
results in the more efficient biosorption process (Mane and Babu, 2011). Similar
results have been reported for the removal of colour and COD from the real effluent
of textile mills (Ahmad and Hameed, 2009).

4.6 Problems related to experimental procedure

From the results obtained, although the COD, turbidity, conductivity and colour were
reduced as the bio sorbent dosage increased, however the optimum dosage of bio
sorbent was unsuccessfully to determine. The graph of the removal of COD,
turbidity, conductivity and color supposedly gradually achieved equilibrium as the
42

optimum dosage of bio sorbent reached. This is due to some experimental error. One
of the errors that possibly happened was the dosage of bio sorbent was insufficient to
reduce COD, turbidity, conductivity and colour until it reaches equilibrium. This
cause the active site for the adsorption of the pollutant in textile effluent was not
sufficient. Next, is the contact time. Contact time also plays an important role in
adsorption process, because it is necessary to estimate the equlibrium contact time,
may be adsorption capacity can increase with increase in contact time until it reaches
equilibrium. Besides, reaction temperature can also can be the source of error. As
mostly the adsorption phenomenon is exothermic in nature and at some points
temperature can play important role in increasing the adsorption capacity. Finally,
initial concentration also plays an important role.
CHAPTER 5

CONCLUSIONS AND RECOMMENDATIONS

5.1 Conclusion

The treatment of textile wastewater before disposal into the environment is important
and ensures safety to the environment without affecting the quality of lakes, rivers
and other water body. Thus, pineapple leaves bio sorbent shows a good potential to
reduce COD, turbidity, conductivity and colour in textile waste water. The results
from FTIR spectroscopy revealed that the functional groups and chemical
characteristics of pineapple leaves changed after adsorption process. As shown in
FTIR spectra, Hydroxyl (-OH) and carboxyl group (C-O) on the cellulose of
pineapple leaves played a major role for sorption of dye ions from the textile
wastewater. The adsorption process depends on dosage of bio sorbent. The findings
of the experiments indicate that as the dosage of bio sorbent increased, the removal
of COD, conductivity, turbidity, color increased. The reduction of COD, turbidity,
conductivity and colour values were increased as the dosage increased for 0.2g, 0.4g,
0.6g, 0.8g and 1.0g. Furthermore, the readings of DO in treated wastewater also
increased. The potential of bio sorbent to treat effluent from textile wastewater shows
significant results before it is being released to environment. From the result
obtained, conclusion can be drawn that the removal of COD, conductivity, turbidity
and colour gradually increased with enhancing bio sorbent dosage. Somehow, the
optimum dosage was not identified due to some error such as insufficient dosage,
low contact time, low reaction temperature and low initial concentration. Thus,
further investigations need to be conducted.
44

5.2 Recommendation for future work

As regards to future work, the following recommendations are suggested:


i. Further research and study should be conducted to obtain the optimum dosage
of bio sorbent as this experiment failed to identified optimum amount of
pineapple leaves due to some experimental error such as insufficient dosage,
low contact time and low reaction temperature and high initial concentration.
ii. The application of this environmentally friendly and efficient bio sorbent for
the removal of pollutants from real industrial effluents, continuous flow
system studies need to be performed.
iii. The adsorption kinetics, thermodynamics and mechanism of bio sorbent in
textile wastewater treatment need to be studied to have deep understanding on
how the bio sorbent work.
45

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50

APPENDIX A

Raw data of COD, DO, Turbidity, Conductivity and


Colour
Readings of blank sample

Parameters
COD (mg/l) DO (mg/l) Conductivity Turbidity Color
(µS/cm) (NTU) (ADMI)
Initial 174.4 4.54 1585.1 34.5 518.5
174.2 4.55 1585.2 34.6 518.6
174.4 4.54 1585.2 34.5 518.5
Final 174.3 4.55 1585.2 34.4 518.4
174.3 4.54 1585.3 34.5 518.5
174.4 4.54 1585.2 34.5 518.5

Initial Colour Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0

Colour reading of first set of 525.2 527.1 525.5 521.5 515.9


experiment, (ADMI)

Colour reading of second set of 518.5 517.0 519.1 520.4 522.7


experiment, (ADMI)

Colour reading of third set of 520.4 528.0 520 524.8 520.8


experiment, (ADMI)

Average reading, (ADMI) 521.3 524.0 524.1 522.2 519.8


51

Initial Turbidity Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
Turbidity reading of first set of experiment, 35.9 34.4 35.4 36.2 33.2
NTU
Turbidity reading of second set of 33.6 33.4 36.9 32.1 33.0
experiment, NTU
Turbidity reading of third set of experiment, 39.7 35.7 34.1 32.4 36.4
NTU
Average reading, NTU 36.4 34.5 35.6 33.5 34.2

Initial Conductivity Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
Conductivity reading of first set 1652.3 1635.6 1635.0 1651.1 1630.2
of experiment, µS/cm

Conductivity reading of second 1656.1 1638.5 1644.8 1653.2 1636.2


set of experiment, µS/cm

Conductivity reading of third set 1658.2 1638.1 1640.2 1653.0 1638.1


of experiment, µS/cm

Average reading, µS/cm 1655.5 1637.4 1640 1652.4 1634.8

Initial COD Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
COD reading of first set of experiment, 175.1 171.1 167.6 169.3 171.1
mg/l
COD reading of second set of 176.4 174.1 169.7 172.1 172.7
experiment, mg/l
52

COD reading of third set of experiment, 177.2 174.2 170.3 172.4 175.2
mg/l
Average reading, mg/l 176.2 173.1 169.2 171.3 173.0

Initial DO Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
DO reading of first set of experiment, mg/l 4.46 4.11 4.39 4.33 4.46

DO reading of second set of experiment, mg/l 4.50 4.12 4.42 4.34 4.43

DO reading of third set of experiment, mg/l 4.47 4.14 4.40 4.30 4.42

Average reading, mg/l 4.48 4.12 4.4 4.32 4.44

Final Colour Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
Colour reading of first set of experiment, 314.8 271.5 223.4 240.2 222.5
(ADMI)
Colour reading of second set of 292.8 274.2 238.3 254.0 209.8
experiment, (ADMI)
Colour reading of third set of experiment, 284.9 272.8 211.0 236.2 223.1
(ADMI)
Average reading, (ADMI) 297.5 272.8 224.2 243.4 218.5
53

Final Turbidity Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0

Turbidity of first set of experiment, (NTU) 26.2 23.3 21.8 18.5 19.6
Turbidity of second set of experiment, (NTU) 27.2 24.2 22.6 22.0 18.7

Turbidity of third set of experiment, (NTU) 23.9 22.1 20.7 20.3 20.1
Average reading, (NTU) 25.8 23.3 21.7 20.2 19.5

Final Conductivity Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0

Conductivity of first set of experiment, 821.5 971.4 894.9 651.2 640.1


(µS/cm)

Conductivity of second set of 825.1 976.1 896.1 655.4 642.4


experiment, (µS/cm)

Conductivity of third set of experiment, 824.6 977.9 899.4 653.2 643.1


(µS/cm)

Average reading (µS/cm) 823.7 975.1 896.8 653.3 641.9

Final COD Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
COD of first set of experiment, (mg/L) 143.5 127.6 109.1 96.4 74.8
COD of second set of experiment, (mg/L) 141.3 129.3 107.2 99.2 78.9
54

COD of third set of experiment, (mg/L) 141.9 127.4 107.2 96.5 76.8
Average reading, (mg/L) 142.3 128.1 109.3 97.4 76.8

Final DO Test Readings

Biosorbent Dosage, (g)


0.2 0.4 0.6 0.8 1.0
DO of first set of experiment, (mg/L) 143.5 127.6 109.1 96.4 74.8
DO of second set of experiment, (mg/L) 141.3 129.3 107.2 99.2 78.9
DO of third set of experiment, (mg/L) 141.9 127.4 107.2 96.5 76.8
Average reading, (mg/L) 142.3 128.1 109.3 97.4 76.8
55

APPENDIX B

GANTT CHART