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NICKEL REMOVAL FROM ELECTROLESS WASTEWATER USING COAGULATION FLOCCULATION AND ION EXCHANGE NOR AZIMAH BINTI AHMAD UNIVERSITI TEKNOLOGI MALAYSIA

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Page 1: NICKEL REMOVAL FROM ELECTROLESS WASTEWATER USING ...eprints.utm.my/id/eprint/78307/1/NorazimahAhmadMFKK20131.pdf · NOR AZIMAH BINTI AHMAD UNIVERSITI TEKNOLOGI MALAYSIA . i NICKEL

NICKEL REMOVAL FROM ELECTROLESS WASTEWATER USING

COAGULATION FLOCCULATION AND ION EXCHANGE

NOR AZIMAH BINTI AHMAD

UNIVERSITI TEKNOLOGI MALAYSIA

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NICKEL REMOVAL FROM ELECTROLESS WASTEWATER BY USING

COAGULATION FLOCCULATION AND ION EXCHANGE

NOR AZIMAH BINTI AHMAD

A thesis submitted in fulfilment of the

requirements for the award of the degree of

Master of Engineering (Environmental)

Faculty of Chemical Engineering

Universiti Teknologi Malaysia

AUGUST 2013

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Dedicated to my husband, daughter, siblings, nieces, mother in-law and

beloved parents for their support, spirit, prayer and throughout any time of

need.

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ACKNOWLEDGEMENT

In the name of Allah the Most Beneficent and the Most Merciful,

alhamdulillah and praise be to Allah the Almighty that I am able to complete my

studies here in UTM.

Working on this thesis is a challenging task. Therefore I would like to

express my utmost appreciation to my supervisors, Associate Prof. Dr Ariffin b.

Abu Hassan and Dr Zainura for their endless guidance, inspiration, encouragement

and mentorship to complete this thesis. Also, many thanks to my supportive superior

En Raja Ahmad Tajuddin bin Dato Ridzuan. I thank you for your support and

understanding.

Last but not least, I would like to thank my family and friends who have

directly or indirectly given me support during the completion of this thesis.

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ABSTRACT

A massive growth in the industry of electroplating is associated with an

increase in the quantity of nickel found in surface water and groundwater. This

study focused on the removal of nickel concentration from organic solid waste

stream of electroplating industry by using coagulation flocculation and ion exchange

methods. In this study, various types of coagulants such as chitosan, WPC 6001,

ferric chloride and polyacrylamide were tested to determine the best coagulant for

removal of nickel, total suspended solid, chemical oxygen demand and turbidity.

The effects of process variables such as pH and coagulant dosage on the

performance of these coagulants were also investigated. Polyacrylamide (PAA) was

found to be the best coagulant with percentage of 96.6%, 47.2%, 99.6% and 99.6%

for removals of nickel, chemical oxygen demand, total suspended solid and turbidity

respectively at the pH value of 10 and 1.6 mL/L dosage. From Response Surface

Methodology (RSM), the optimal conditions for removal of nickel were found to be

at pH 10.46 and 1.64 ml/L PAA dosage. Chelating resin was found to be the best

resin with 99.6% nickel removal at pH value of 4. The treated wastewater’s nickel

content meets Standard A of the Malaysian Environmental Standard.

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ABSTRAK

Pertumbuhan pesat dalam industri penyaduran dikaitkan dengan peningkatan

dalam kuantiti nikel yang terdapat di permukaan dan air bawah tanah. Kajian ini

memberi tumpuan kepada penyingkiran kepekatan nikel dari aliran sisa pepejal

organik industri penyaduran dengan menggunakan kaedah pengentalan

pengelompokan dan pertukaran ion. Dalam kajian ini, pelbagai ejen pengental

seperti kitosan, WPC 6001, ferrik klorida dan poliakrilamida telah diuji untuk

menentukan ejen pengental yang terbaik untuk penyingkiran nikel, permintaan

oksigen kimia (COD), pepejal terampai dan kekeruhan. Kesan pembolehubah

seperti pH dan dos pengental terhadap keberkesanan ejen pengental juga dikaji.

Poliakrilamida (PAM) didapati merupakan ejen pengental yang terbaik dengan

peratus penyingkiran 96.6%, 47.2% , 99.6% dan 99.6% bagi nikel, permintaan

oksigen kimia, pepejal terampai dan kekeruhan pada nilai pH 10 dan 1.6 mL/L dos

pengental. Dari Response Surface Methodology (RSM), keadaan optimum bagi

penyingkiran nikel didapati pada pH 10.46 dan 1.64 mL/L dos pengental

poliakrilamida. Resin pengkelatan merupakan resin yang terbaik dengan peratusan

penyingkiran nikel 99.6% pada nilai pH 4. Air sisa yang dirawat kandungan

nikelnya memenuhi piawaian A menurut Sistem Piawaian Alam Sekitar Malaysia.

.

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TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENTS iv

ABSTRACT v

ABSTRAK vi

TABLE OF CONTENTS vii

LIST OF TABLES xii

LIST OF FIGURES xiv

LIST OF ABBREVIATIONS xviii

LIST OF APPENDICES xx

1 INTRODUCTION 1

1.1 Research Background 1

1.2 Problem Statement 3

1.3 Research Objectives 6

1.4 Research Scope 7

1.5 Significance of the Study 7

1.6 Organization of Thesis 8

2 LITERATURE REVIEW 9

2.1 Nickel Waste 9

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2.2 Electroless Plating Industry Wastewater 10

2.2.1 Wastewater Characteristics and Source 10

2.2.2 Process of Nickel Electroless Plating

At the Seagate 14

2.2.3 Source of Wastewater at Seagate 15

2.3 Coagulation and Flocculation 16

2.3.1 Charge Neutralization 19

2.3.2 Bridging Flocculation 20

2.3.3 The Effect of Operation Condition in

Flocculant 22

2.3.3.1 Effect of Coagulant Dosage 23

2.3.3.2 Effect of pH 23

2.3.3.3 Effect of Mixing Time 24

2.4 Chitosan 25

2.4.1 Chitin 25

2.4.2 Mechanism of Chitosan 27

2.4.3 Cation on Chitosan Interaction 28

2.4.4 Application of Chitosan 29

2.5 Polyacrylamide 30

2.5.1 Anionic Polyacrilamide 31

2.5.2 Cationic Polyacrylamide 32

2.5.3 Non-ionic Polyacrylamide 32

2.5.4 Application of Polyacrylamide in Nickel

Removal from Wastewater 32

2.5.4.1 Effect of PAA Dosage 33

2.5.4.2 Effect of pH 34

2.5.4.3 Effect of Temperature 35

2.5.4.4 Effect of Contact Time 35

2.6 Ferric Chloride 36

2.7 Ion Exchange 37

2.7.1 Classes of Ion Exchange 42

2.7.1.1 Strong Acid Cation Exchange

Resin (SAC) 42

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2.7.1.2 Weak Acid Cation Exchange

Resin (WAC) 43

2.7.1.3 Strong Base Anion Resin (SBA) 44

2.7.1.4 Weak Base Anion Resin (WBA) 45

2.7.1.5 Chelating Resin 46

2.7.2 Application of Ion Exchange in Nickel

Removal from Wastewater 47

2.7.2.1 Nickel Ion Concentration 47

2.7.2.2 Effect of pH 48

2.7.2.3 Effect of Contact Time 49

2.7.2.4 Effect of Resin Dosage 50

2.7.2.5 Effect of Degree of Stirring 51

2.7.2.6 Effect of Temperature 52

2.8 Response Surface Methodology (RSM) 53

2.8.1 Two Level Factorial Design 54

2.8.2 Three Level Factorial Design 55

2.8.3 Central Composite Design 57

3 METHODOLOGY 60

3.1 Introduction 60

3.2 Material and Apparatus 61

3.3 Experimental Procedure 63

3.3.1 Sample Collection 63

3.3.2 Sample Characterization 63

3.3.2.1 Determination of Total Nickel 63

3.3.2.2 Determination of COD, pH, TSS

and Turbidity 64

3.3.3 Sample and Coagulant Preparation 64

3.3.3.1 Chitosan 65

3.3.3.2 Ferric Chloride 66

3.3.3.3 WPC 6001 66

3.3.4 Jar Test 67

3.3.4.1 Jar Test – Effect of Coagulant Dosage 68

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3.3.4.2 Jar Test – Effect of pH 69

3.3.5 Ion Exchange 70

3.3.5.1 Sample and Experimental Preparation 71

3.3.5.2 Ion Exchange – Effects of pH

Adjustment 72

3.3.5.3 Ion exchange Effect of Contact

Time from Flow rate 73

3.4 Procedure for RSM Experimental Design 74

4 RESULTS AND DISCUSSION 77

4.1 Introduction 77

4.2 Characteristic Study on Wastewater 78

4.3 Chitosan 79

4.3.1 Effect on Chitosan Dosage 79

4.3.2 Effect of pH 80

4.4 Organic Coagulant (WPC 6001) 83

4.4.1 Effect of Dosage on WPC 601

Performance 83

4.4.2 Effect of pH 84

4.5 Ferric Chloride (FeCl3) 85

4.5.1 Effect of FeCl3 Dosage 85

4.5.2 Effect of pH 86

4.6 Polyacrylamide (PAA) 88

4.6.1 Effect of PAA Dosage 88

4.6.2 Effect of pH 90

4.7 Optimization of PAA Coagulant 91

4.7.1 Response Surface Methodology 91

4.7.2 Statistical Analysis 91

4.7.3 Variable Effect on the Responses 99

4.7.4 Optimization 101

4.8 Ion Exchange 102

4.8.1 Strong Acid Cation Resin – Purolite

D5041 103

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xi 4.8.2 Chelating Resin – Purolite D5047 106

4.9 Effect of Operating Variable on the

Performance of the Chelating Resin 107

4.9.1 Effect of pH 107

4.9.2 Evaluation of Contact Time

from Flow rate 108

5.0 CONCLUSION AND RECOMMENDATION 110

5.1 Conclusion 110

5.2 Recommendation 111

REFERENCES 112

Appendices A-C 125 - 134

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LIST OF TABLES

TABLE NO. TITLE PAGE

1.1 Nickel content at subsequent sampling point 4

2.1 Waste characteristics of metal finishing (USEPA, 1992) 11

2.2 Electroless nickel solution constituents and operation

parameter (Henny et al., 2000) 12

2.3 Types of waste stream from production process

(Seagate, 2007) 15

2.4 Few application of ion exchange materials including both

well developed and experimental techniques (Andrie, 2007) 41

2.5 Functional groups of standard ion-exchange resin

(IAEA, 2000, Helfferich, 1962) 42

2.6 Strong acid cation selectivity of ion-exchange resin

(Paul Chen et al., 2006) 43

2.7 The effect of stirring on the adsorption of nickel 52

2.8 The effect of temperature on the adsorption of nickel 53

3.1 List of experimental material 62

3.2 List of apparatus 62

3.3 Method of analysis 64

3.4 Independent variables process and their

corresponding levels 75

3.5 Experimental design base on central composite design

in coded factor 76

4.1 Waste characteristic of OS waste stream 78

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xiii 4.2 Experimental design and predicted responses 92

4.3 Analysis of variance (ANOVA) 96

4.4 Predict analysis on removal of nickel at optimum

conditions 102

4.5 Predict and observed values of the removal of nickel at

optimal conditions 102

4.6 Typical chemical and physical resin characteristics 103

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LIST OF FIGURES

FIGURE NO. TITLE PAGE

2.1 Electroless reaction 12

2.2 Charge neutralization model (Moudgil and 19

Somasundaran, 1985)

2.3 Schematic of reactions between particles and

polymers by bridging flocculation (Weber, 1972) 22

2.4 Structure of chitosan (Bough et al., 1976) 25

2.5 Structure of chitin (Lima and Airoldi, 2004) 26

2.6 Preparation of chitin and chitosan (Vishnu et al., 2005) 27

2.7 Polymerization of acrylamide (Yang, 2008) 31

2.8 Effect of dosage on nickel removal (Mousavi et al., 2012) 34

2.9 Effect of temperature on the absorption of Cr (III) and

Ni onto PAA 35

2.10 Ion exchange resin 40

2.11 Exchange capacity of ( ) weak acid cation and (---)

weak base anion resin with solution pH (Ramco, 1981) 44

2.12 Effect of initial concentration (Kumar et al., 2010) 48

2.13 Effect of pH (Kumar et al., 2010) 49

2.14 Effect of time (Kumar et al., 2010) 50

2.15 Effect of resin dosage (Kumar et al., 2010) 51

2.16 Adsorption profile at different speeds (Theo, 1998) 51

2.17 Adsorption profile at different temperature (Theo, 1998) 53

2.18 Two-level factorial design (a) two fraction and (b) three

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xv factors (Anderson and Whitcomb, 2007) 54

2.19 Three level factorial design (a) two factors (b) three

factors (Marco et al., 2008) 56

2.20 General quadratic response surface type (a) peak

(b) hillside (c) rising ridge (d) saddle 57

2.21 Layout of CCD (a) factorial design (b) star design

(c) central composite design 58

3.1 Overall work plan 61

3.2 Atomic absorption spectrometer 64

3.3 Sequence of chitosan coagulant preparation 65

3.4 Sequence of WPC 6001 coagulant preparation 67

3.5 Jar test 68

3.6 Sequence of experiment for studying effect of

coagulant dosage 69

3.7 Sequence of experiment for studying the effect of pH 70

3.8 Ion exchange resin column test 71

3.9 Ion exchange column 72

3.10 Ion exchange experimental process on pH Effect 73

3.11 Ion exchange experimental process on contact time

of flow rate 74

4.1 Effect of chitosan dosage on Ni, COD, TSS and

turbidity removal at pH 6 80

4.2 Effect of pH on Ni, CODm TSS and turbidity removal

at chitosan dosage 700 mg/L 81

4.3 Metal soluability versus pH (Hoffland, 2006) 82

4.4 Effect of WPC 6001 dosage on Ni, COD, TSS and

turbidity removal at pH 4 84

4.5 Effect of pH on Ni, COD, TSS and turbidity removal

at WPC 6001 dosage at 270 mg//L 85

4.6 Effect of FeCl3 dosage on Ni, COD, TSS and turbidity

removal at pH 4 86

4.7 Effect of pH on Ni, COD, TSS and turbidity removal

at FeCl3 dosage 26.6 mg/L 87

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xvi 4.8 Effect of PAA dosage on Ni, COD, TSS and turbidity

removal at pH 6 89

4.9 Effect of pH on Ni, COD, TSS and turbidity removal

at PAA dosage 1.6 mg/L 90

4.10 Graph predicted value versus observed values for

nickel removal 93

4.11 Graph predicted values versus observed values for

COD removal 94

4.12 Graph predicted values versus observed values for

TSS removal 94

4.13 Graph predicted values versus observed values for

Turbidity removal 95

4.14 Pareto chart of nickel removal 97

4.15 Pareto chart of COD removal 97

4.16 Pareto chart TSS removal 98

4.17 Pareto chart of turbidity removal 98

4.18 3D response surface plots of nickel removal

versus coagulant dosage and pH 99

4.19 3D response surface plots of COD removal

versus coagulant dosage and pH 100

4.20 3D response surface plots of TSS removal versus

coagulant dosage and pH 100

4.21 3D response surface plots of Turbidity removal

versus coagulant dosage and pH 101

4.22 Percentage of nickel removal (%) with strong acid

cation resin at pH 4 105

4.23 Nickel content (mg/L) with strong acid cation resin

at pH 4 105

4.24 Percentage of nickel removal with chelating resin at

pH 4 106

4.25 Nickel content (mg/L) with chelating resin 107

4.26 Effect of pH on chelating ion-exchange resin 108

4.27 Effect of contact time on 1st column chelating resin

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xvii at different flow rate 109

4.28 Effect of contact time on 2nd column chelating resin

at different flow rate 109

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xviii

LIST OF ABBREVIATIONS

Al+3 - Aluminum ion

ANOVA - Analysis of variance

Β - Beta

Cd - Cadmium

COD - Chemical oxygen demand

-COOH - Carboxylic acid

Cu - Copper

Cr(III) - Trivalent chromium

Co+2 - Cobalt

DBPs - Disenfection by products

EDTA - Ethylenediaminetetraacetic

EN - Electroless nickel

EPA - Environmental protection agency

Fe2+ - Ferrous

FeCl3 - Ferric chloride

HCl - Hydrochloric Acid

Hg+2 - Mercury

HPO2- - Hypo

H+ - Hydrogen ion

MW - Molecular weight

Na+ - Sodium ion

NaCl - Sodium cloride

NaOH - Sodium hydroxide

Ni - Nickel

Ni-P - Nickel phosphorus

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-NH2 - amino groups

NOM - Natural organic matter

NTU - Nephelometric turbidity units

NH3+ - Ammonia ion

OH- _ Hydroxide ion

OS - Organic solid

OMG - Object Management Group

P - Phosphorus

PAA - Polyacrylamide

Pb - Lead

R-NH2 - Primary weak base resin

R-NHR1 - Secondary weak base resin

R-NR12 - Tertiary weak base resin

RSM - Response surface methodology

R2 - Coefficient of determination

SAC - Strong acid cation

SBA - Strong base anion

SD - Standard deviation

SRWTP - Sacramento Regional Wastewater Treatment

Plant

SO3- - Sulfite

S2- - Sulfide

THM - Trihalomethane

TSS - Total suspended solid

WAC - Weak acid cation

WBA - Weak base anion

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LIST OF APPENDICES

APPENDIX TITLE PAGE

A Standard Methods 125

B Coagulation Flocculation 127

C Ion Exchange 132

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CHAPTER 1

INTRODUCTION

1.1 Research Background

The global latent demand for nickel, nickel-alloy wire, insulated wire and

cable is estimated to be $0.6 billion in 2006. The distribution of world latent demand

(potential industry earning) is not even across regions. The largest market is Asia,

with $0.2 billion (31.86 percent), followed by North America and the Caribbean with

$0.2 billion (25.67 percent) and Europe with $0.2 billion (25.16 percent) of the world

market (Philip, 2005).

Ruelle (2010) reported that the mining firm Nickel Asia Corporation

projected that nickel price will increase from the current $10.75-$10.85 to $11.90 per

pound by the year 2012. Nickel is mainly used to produce rust-resistant stainless

steel. Also, the demand of stainless steel rose to 9.1 million tons per year in the year

2012; hence the demand of raw nickel is growing by 8.5% annually in the same

period. This figure can stipulate the quantities of nickel discharge to the aquatic

environment. Thus, nickel contributes to the major surface water and groundwater

contaminants.

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Nickel pollution is invariably hazardous as the effluent contaminates the air,

water and soil. Nickel pollution has deleterious effects on human health. According

to the Environmental Quality (Industrial Effluent) Regulation of 2009, the effluent

discharge under Standard A specification shall not exceed 0.2 mg/L (EQA, 2009).

As a result, decreasing nickel concentration is necessary to reach permissible limits

before it is discharged to the environment and to ensure that the effluent is within

permissible levels.

The most commonly used methods of chemical treatment are precipitation

and coagulation flocculation. The precipitation method can reduce soluble metal

ions from a solution by producing metal hydroxides. The process is controlled by a

simple pH adjustment. The pH is raised using an alkaline substance such as sodium

hydroxide or lime. Then, the solution is converted into an insoluble form and it

precipitates. Metcalf and Eddy (2003) reported that the general precipitation

methods use hydroxides (OH-) and sulfides (S2-).

Beside chemical precipitation, Zhen Liang et al. (2009) reported that

coagulation and flocculation are important processes in waste and wastewater

treatment. Most commonly used as coagulant are aluminum based salts and iron

based salts. Whereby in the removal of dissolved organic carbons, iron salts have

been reported to be more effective than alum salts. This is followed by the

flocculation process, where ferric chloride is added to wastewater which causes the

colloidal material to destabilize and small particles to agglomerate by forming a

large flock to settle (Amudaa and Amoob, 2007).

One well-known chemical coagulation and flocculation method uses chitosan.

Chitosan is a biodegradable polymer, which is a non-toxic linear cationic polymer of

high molecular weight and is more environment-friendly (Tan et al., 2007). Chitin, a

cellulose material similar to biopolymer, is widely distributed in nature, found

mainlyin marine invertebrates, fungi, insects and yeasts. Chitosan is a good choice

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3 as a coagulant because it is readily soluble in acid solutions (Mohd Ariffin et al.,

2008). Pan et al. (1999) reported that in various food wastes processing, chitosan is

an effective coagulating agent for suspended solids. The high molecular weight

(MW) of chitosan enhances the generation of bridging mechanisms (Roussy et al.,

2005).

There is a growing interest in the development of natural low-cost materials

as an alternative to synthetic polyelectrolytes (Vijayaraghavan and Yun, 2008,

Sharma et al., 2006, Crini 2005). Numerous studies have proposed a biological

product as an effective coagulation and flocculation agent (Maximova and Dahl,

2006, Deng et al., 2005). Wang et al. (2007) reported types of bioflocculants to

include biopolymers such as starches, chitosan, alginates and microbial materials

produced by microorganisms including bacteria, fungi and yeast. Bioflocculants are

safe and biodegradable polymers and generate no secondary pollution; they are

applicable in food, fermentation, and water and wastewater treatment. Due to public

concerns of polyelectrolyte toxicity, it is believed that bioflocculants will be used

more extensively (Bratby, 2007, Sharma and Dhuldhova, 2006, Crini, 2005).

1.2 Problem Statement

There is a steady increase in nickel-laden wastewater generated worldwide as

a result of rapid industrialization. In the year 2000, 158,000 tons of nickel was used

in the US, 13 % of which was consumed by the galvanic industry (Spoor, 2002). The

annual growth of stainless steel demand has been estimated to increase by 9.1 million

tons from the year 2009 to 2012. The result shows a growing demand for raw nickel

to a tone of 8.5% annually for the same period (Ruelle, 2010). The contaminations

that release into the water bodies can cause potential hazardous to aquatic, human

health as well as the environment. Nickel has been identified to cause serious

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4 problems in humans such as allergy, dermatitis, sensitization and lung-nervous

system damage; in fact, it has been placed on a list of thirteen hazardous metals by

the US Environmental Protection Agency (Malkoc, 2006). Thus, it must be treated

appropriately before being released into the environment.

At Seagate International (J) Sdn. Bhd, one of the heavy metals that are found

to contaminate the wastewater is nickel. The current coagulation flocculation method

is uneconomic, due to the in efficient removal of nickel despite using a high dosage

of coagulants. The in efficient nickel removal from coagulation flocculation

necessitates a subsequent treatment called ion exchange, and constant regeneration is

needed. The level of nickel from exhausted ion exchange exceeds Malaysia’s

industrial effluent specification limit of Standard A (≤ 0.2 mg/L). This scenario may

create an excursion condition to Seagate International (J) Sdn. Bhd. Therefore, the

wastewater must be treated appropriately before it is discharged into municipal

drains. The mean reading for nickel found in the wastewater are shown in Table 1.1.

Table 1.1 : Nickel content at subsequent sampling points

Parameter OS

Influence

(mg/L)

OS

Effluent

(mg/L)

Final

Discharge

(mg/L)

Standard A

Specification

(mg/L)

Nickel

94.3

6.94

0.12 – 0.29

0.2

Note:

OS – Organic Solid

Chemical precipitation by coagulation and flocculation is an important

process in waste and wastewater treatment. It is used to remove heavy metals such

as nickel, suspended solids (SS), reduce chemical oxygen demand COD and turbidity

(Amudaa and Amoob, 2007). Common coagulants include aluminum-based and

iron-based salts. Other coagulants include commercial organic coagulants,

polyacrylamide and chitosan, which is a biodegradable, non-toxic linear cationic

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5 polymer with a high molecular weight (Assaad et al., 2007; Ashoka et al., 2007;

Mohd Ariffin et al., 2008). At neutral to alkaline pH, ferric salts will precipitate as

an amorphous hydrated oxide or oxy-hydroxide, which has relatively stable and

reproducible surface properties. The ability of the ferric hydroxide precipitate to

absorb ions of heavy metals is characterized in single- and multi-adsorbate systems.

Heavy metals could be absorbed as cations (Cr+³, Pb+, Cu+², Zn+², Ni+², Cd+²) in a

neutral to high pH environment, and are absorbed as anions (SeO2-2, CrO4

-2,

VO3(OH)-2, AsO4-3) in a neutral to mildly acidic pH environment (Patoczka et al.,

1998). Studies agree that ferric chloride is more effective than alum for capturing

metals from wastewater. It is reported that the efficiency of ferric chloride

outperformed alum in arsenic removal, with 96% of arsenic remove dusing ferric

chloride compared to 81% when using alum salts (Johnson et al., 2008).

Studies have also shown that the effectiveness of coagulants is affected by

dosage, pH and temperature. These factors need to be tweaked to obtain a high

efficiency of treatment. The conventional method to seek optimal conditions is by

trial and error approach, using jar tests. This involves changing the levels of one

factor and at the same time, keeping the others constant, the running the experiment,

observing the results and moving on to the next factor (Mohd Ariffin et al., 2008).

This is indeed time and energy consuming. It is also usually incapable of revealing

the optimal combination of factors, because it ignores the interaction among them (El

Karamany, 2010; Trinh and Kang, 2011; Zheng et al., 2012). Moreover, a majority

of wastewater treatment processes are contains multiple variables and optimization

through the classical method is inflexible, unreliable and time-consuming (Bashir et

al., 2012). A better alternative is the used of Respond Surface Methodology (RSM)

because it includes the influences of individual factors as well as the influences of

their interaction. RSM is a technique for designing experiments and building models

which evaluates the effects of several factors to achieve optimum conditions for

desirable responses with a limited number of planned experiments (Cristian et al.,

2010; Raissi et al., 2009; Zheng et al., 2012). There are published RSM studies that

focuses on the usability of RSM for optimization of various types of wastewater

treatment processes (Bashir et al., 2012; Trinh and Kang, 2011; Zheng et al., 2012).

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6 However, it is observed that works concerning the optimization of nickel removal

using chitosan are not readily available.

1.3 Research Objective

The main objectives of this research are outlined below.

To determine the performance of coagulants (chitosan, WPC6001, ferric

chloride and polyacrylamide) in the removal of nickel from wastewater.

To determine the effects of coagulant dosage and pH on the performance of

these coagulants.

To optimize performance of the best coagulant by using RSM.

To determine the performance of ion exchange (strong acid cation and

chelating resin) on the nickel removal process.

1.4 Research Scope

The scope of this research includes:

The study is carried out in a lab-scale operation which utilized the actual

electroless wastewater by analyse the characterization as the influent.

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7 Study the nickel, COD, TSS and turbidity removal efficiency of the various

coagulants (chitosan, WPC6001, ferric chloride and polyacrylamide (PAA))

at different pH levels(4 – 11) and coagulant dosages.

Evaluating the optimum pH and coagulant dosage for PAA using response

surface methodology (RSM).

Study the performance of different ion exchange (strong acid cation and

chelating resin) on nickel removal at pH 4.

Evaluate the operation condition for chelating resin at different pH and

contact time.

1.5 Significance of The Study

Large quantities of trace metals such as nickel are discharged from various

industrial processes into the environment; endanger humans as well as flora and

fauna. Growing public concern about environmental protection/sustainability and

public health has led to the enactment of environmental laws and environmental

standards being set up. Therefore, to meet these standards, there is an urgent need

for manufacturers to minimize release of these metallic pollutants into bodies of

water by treating the wastewater prior to discharging it into the environment.

This has prompted more researches to be conducted to find more efficient

ways to remove these nickels from the wastewater before being released into the

environment. Therefore, the result from this research will serve as a guide to treat

wastewater for electroless industries, regulatory bodies and policymakers.

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8 1.6 Organization of the Thesis

This thesis consists of five chapters. Each chapter gives information about a

specific research area.

Chapter 1 details the research background, research aim and objectives as

well as the scope of the study.

Chapter 2 reviews literature on general information on nickel, electroless

plating industry wastewater, coagulation-flocculation method and ion

exchange.

Chapter 3 covers a general description of the experimental setup and the

procedures in carrying out the research work. It includes: sample collection

and characterization, assessment of nickel removal efficiency by different

coagulants, assessment of nickel removal efficiency by different ion

exchange resins and determination of optimum operating conditions for

chemical precipitation using response surface methodology (RSM).

Chapter 4 presents and discusses the results of the research. It includes the

effect of pH and coagulant dosage on the efficiency of nickel removal. The

performances of various ion exchange resins are discussed. Finally, the

results of the optimization process using RSM is presented.

Chapter 5 deals with conclusions and recommendations. It presents the

conclusions derived from this research study and recommendations for future

studies.

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