OPTIMIZATION OF RHODAMINE B DYE REMOVAL FROM fileOPTIMIZATION OF RHODAMINE B DYE REMOVAL FROM AQUEOUS SOLUTIONS BY LIQUID-LIQUID EXTRACTION by WANG JIAO Thesis submitted in fulfilment

OPTIMIZATION OF RHODAMINE B DYE

REMOVAL FROM AQUEOUS SOLUTIONS BY

LIQUID-LIQUID EXTRACTION

WANG JIAO

UNIVERSITI SAINS MALAYSIA

2017

OPTIMIZATION OF RHODAMINE B DYE

REMOVAL FROM AQUEOUS SOLUTIONS BY

LIQUID-LIQUID EXTRACTION

by

WANG JIAO

Thesis submitted in fulfilment of the requirements

For the degree of

Master of Science

July 2017

ii

ACKNOWLEDGEMENT

It is a pleasure to thank those people who gave me help and encourage for my

work. I would like to acknowledge my main supervisor, Dr. Mohd Rafatullah, and

co-supervisor, Prof. Dr. Norhashimah Morad, School of Industrial Technology,

Universiti Sains Malaysia, for the professional guidance, kindness and patience. I

would like to thank my senior, Dr. Amir Talebi, and my friends with their efforts in

helping me with my research. I would also like to express my sincere gratitude to all

the Lecturers and Laboratory staffs in School of Industrial Technology. Thanks for

Soon Soon Oil Mill Sdn. Bhd. supplying the vegetable oils in my research. Lastly,

my deeply appreciate to my dear parents who are kind, generous and gave me

support in all my pursuits, and most importantly, my loving boyfriend Yuan Tianlong,

for his patience, encourage and faithful support. Thank you.

Wang Jiao

July 2017

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TABLE OF CONTENTS

ACKNOWLEDGEMENT ………………………………………………… ii

TABLE OF CONTENTS ………………………………………………….. iii

LIST OF TABLES …………………………………………………………. vii

LIST OF FIGURES ………………………………………………………... viii

LIST OF SYMBOLS……………………………………………………….. x

LIST OF ABBREVIATION ……………………………………………….. xii

ABSTRAK ………………………………………………………………….. xiii

ABSTRACT ………………………………………………………………… xvi

CHPTER 1: INTRODUCTION 1.0 Overview ………………………………………………………………….. 1

1.1 Dye Wastewater …………………………………………………………… 1

1.2 Treatment Techniques for Dye Wastewater Treatment ……………………. 2

1.2.1 Adsorption …………………………………………………………... 3

1.2.2 Irradiation …………………………………………………………… 3

1.2.3 Ozonation …………………………………………………………… 3

1.2.4 Advanced Oxidation Processes …………………………………….. 4

1.2.5 Biological Treatment ……………………………………………….. 4

1.2.6 Electrochemical Treatment …………………………………………. 4

1.3 Liquid Membrane …………………………………………………………. 5

1.3.1 Bulk Liquid Membrane …………………………………………….. 5

1.3.2 Supported Liquid Membrane ………………………………………. 6

1.3.3 Emulsion Liquid Membrane ……………………………………….. 6

1.4 Problem Statement ………………………………………………….......... 7

1.4.1 Rhodamine B ………………………………………………………. 7

1.4.2 Conventional Organic Solvents and Extractants …………………… 7

1.5 Objectives of Research ……………………………………………………. 8

1.6 Thesis Organization ………………………………………………………. 8

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CHAPTER 2: LITERATURE REVIEW 2.0 Introduction ……………………………………………………………… 10

2.1 Classification of Dyes …………………………………………………… 10

2.2 Characteristics of Rhodamine B ……………………..………………….. 11

2.3 Liquid-Liquid Extraction ………………………………………………... 12

2.4 Transport Mechanism of Liquid Membrane …………………………….. 13

2.5 Bulk Liquid Membrane ………...……………………………………...... 14

2.6 Factors Affect Rhodamine B Extraction ………………………………… 15

2.7 Distribution Coefficient ………………………………………………….. 16

2.8 Vegetable Oils …………………………………………………………… 17

2.8.1 Composition of Vegetable Oils …………………………………….. 18

2.8.2 Viscosities of Vegetable oils ………………………………………. 19

2.9 Response Surface Methodology …………………………………………. 20

2.9.1Design of Experiments ……………………………………………... 20

2.9.1(a) Two-level Full Factorial Design ………………………….. 21

2.9.1(b) Two-level Factional Factorial Design …………………….. 22

2.9.1(c) Central Composite Design ……………………………….. 23

2.9.2 Regression Analysis ……………………………………………….. 24

2.9.3Model Adequacy Checking ………………………………………... 25

2.6.3(a) Analysis of Variance………………………………………. 26

2.6.3(b) Coefficient of Determination …...………………………… 27

2.6.3(c) Residual Analysis………………………………..………… 27

CHAPTER 3: MATERIALS AND METHODS 3.0 Introduction ………………………………………………………………. 29

3.1 Materials ………………………………………………………………….. 29

3.2 Equipment ………………………………………………………………… 29

3.3 Experimental Procedure …………………………………………………... 32

3.3.1 Extraction and Stripping of RB by LLE System ………………..….. 33

3.3.1(a) Extraction Procedure ……………………………………….. 34

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3.3.1(b) Stripping Procedure ………………………………………… 35

3.3.2 Selection of Vegetable Oil as the Organic Solvent for RB Extraction from Aqueous Solutions…………………………………………….

36

3.3.3 Optimization of Factors Affecting RB Extraction from Aqueous Solutions Using Vegetable oil as Organic Phase by using RSM ……. …………………………………………………………

36 3.3.3(a) Screening Experiments ……………………………………. 37

3.3.3(b) Optimization Experiments ……………………………….... 38

3.3.4 Investigation of RB Extraction Under Optimum Condition .……… 39

3.5 Selection of Stripping Agent ………………………………………….. 39

3.6 Investigation of Viscosity Affecting RB Extraction by using BLM System and Procedures ………………………………………………..

40

CHAPTER 4: RESULTS AND DISCUSSION 4.0 Introduction ……………………………………………………………… 41

4.1 Selection of Vegetable Oil-Based Organic Solvent for RB Extraction from Aqueous Solutions ………………………………………………...

41

4.1.1 pH-extraction Isotherms……………………………………………. 41

4.1.2 Determination of Viscosities of Vegetable Oils …………..……….. 42

4.1.3 Investigation of Different Factors Affecting RB Extraction by using Soybean Oil as Organic Solvent ……………………………

44

4.1.3(a) O/A Ratio …………………………………………………. 44

4.1.3(b) Shaking Speed ……………………………………………. 45

4.1.3(c) Shaking Time……………………………………………… 46

4.2 Optimization of Factors Affecting RB Extraction from Aqueous Solutions using Soybean Oil as Organic Solvent by RSM …....................................

47

4.2.1 Screening of Factors Affecting RB Extraction …………………….. 47

4.2.2 Optimization of Significant Factors Affecting RB Extraction …...... 50

4.2.3 Regression Model for RB Extraction ……………………………… 51

4.2.4 Model Adequacy Checking ………………………………………... 52

4.2.5 Response Contour and Determination of Optimum Conditions…… 55

4.3 Selection of Stripping Agent for RB Stripping from Loaded Soybean Oil Organic Solvent …………………………………………………………..

56

4.4 Investigation of the Effect of Viscosity …………………………..……… 57

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CHAPTER 5: CONCLUSIONS AND RECOMMENDATIONS

5.0 Conclusions …………………………………………………………….... 60

5.1 Recommendations ……………………………………………………….. 61

REFERENCES……………