REMOVAL OF COPPER AND CADMIUM IONS FROM SYNTHETIC INDUSTRIAL WASTEWATER USING CONTINUOUS ION EXCHANGE COLUMN SYSTEM SALEM OMAR SALEM BAMATRAF A dissertation submitted in partial fulfillment of the requirements for the award of the degree of Bachelor of Engineering (Chemical) Faculty of Chemical Engineering Universiti Teknologi Malaysia JANUARY 2013 DECLARATION ii ABSTRACT Removal of copper and cadmium ions from synthetic industrial wastewater using commercial cation exchange resin (Ambrlite 200) was investigated. The experimental investigations were conducted in a fixed bed column system. Where the experiments studied the effect of three essential parameters: 1) bed height (3-5cm), 2) initial concentration (5-20 mg/l), 3) flow rate (15-25 ml/min) in three different solutions: 1) Cu(II) solution, 2) Cd(II) solution 3) and a mixture solutions of metals ( Cu(II), Cd(II), Cr(III) and Cr(VI)). The experimental investigations were undertaken based in the response surface area (RSM). The inductively coupled plasma mass spectrometry (ICM-Ms) technique was used to determine the concentration of heavy metals in the treated water. Minitab 15 software was used to analyse the data. In addition, space velocity and distribution coefficient were used to determine the effectiveness of the ion exchange resin to remove Cu (II) and Cd (II). The obtained results from the response surface plots and breakthrough curves indicates that the ion exchange resin efficiency increases at lower initial concentration, lower value of flow rate and higher resin bed heights. The Distribution Coefficient ( Kd) values for Cu (II) and Cd (II) at different concentration values indicates that the commercial cation exchange resin (Ambrlite 200) has a high selectivity in removing Cu (II). In a brief, the results indicated that the removal percentage of Cu (II) was in the range of 98-99.99% while the removal percentage of Cd (II) was in the range of 90-99%.in a nutshell, Ambrlite 200 resins can be used efficiently to remove Cu (II) and Cd (II) from synthetic industrial wastewater using a continuous ion exchange column system. iii ABSTRAK Penyingkiran tembaga dan ion kadmium daripada air sisa sintetik industri yang menggunakan resin pertukaran kation komersial (Ambrlite 200) telah dikaji. Ujikaji eksperimen telah dijalankan ketinggian tetap lajur sistem. Jika eksperimen mengkaji kesan tiga parameter penting: 1) ketinggian katil (3-5cm), 2) kepekatan awal (5-20 mg / l), 3) kadar aliran (15-25 ml / min) dalam tiga penyelesaian yang berbeza : 1) Cu (II) penyelesaian, 2) Cd (II) penyelesaian 3) dan penyelesaian campuran logam (Cu (II), Cd (II), Cr (III) dan Cr (VI)). Siasatan eksperimen telah dijalankan berdasarkan kawasan permukaan respons (RSM). The induktif ditambah plasma spektrometri jisim (ICM-Cik) teknik telah digunakan untuk menentukan kepekatan bahan logam berat di dalam air yang dirawat. Minitab 15 perisian telah digunakan untuk menganalisis data. Di samping itu, halaju ruang dan pekali agihan telah digunakan untuk menentukan keberkesanan resin pertukaran ion untuk membuang Cu (II) dan Cd (II). Keputusan yang diperolehi dari plot permukaan tindak balas dan “breakthrough curves” menunjukkan bahawa pertukaran ion kecekapan kenaikan resin pada kepekatan yang lebih rendah awal, nilai yang lebih rendah daripada kadar aliran dan tinggi ketinggian katil damar. Pengagihan Pekali (Kd) nilai pada nilai berbeza kepekatan Cu (II) dan Cd (II) menunjukkan bahawa resin pertukaran kation komersial (Ambrlite 200) mempunyai kepilihan yang tinggi dalam membuang Cu (II). Dalam ringkas, keputusan menunjukkan bahawa peratusan penyingkiran Cu (II) adalah dalam julat 98-99,99% manakala peratusan penyingkiran Cd (II) adalah dalam lingkungan 90-99%. Secara ringkas, Ambrlite 200 resin yang boleh digunakan dengan cekap untuk membuang Cu (II) dan Cd (II) daripada air sisa sintetik industri menggunakan pertukaran ion yang berterusan lajur sistem. iv TABLE OF CONTENTS CHAPTER TITLE PAGE DECLARATION OF THESIS SUPERVISOR’S DECLARATION 1 2 TITLE PAGE i STUDENT’S DECALARATION ii DEDICATION iii ACKNOWLEDGEMENT iv ABSTRACT v ABSTRAK vi TABLE OF CONTENTS vii LIST OF TABLES x LIST OF FIGURES xii LIST OF SYMBOLS xv LIST OF ABBREVIATIONS xvi INTRODUCTION 1 1.1 Background 1 1.2 Problem Statement 3 1.3 Objectives of the Study 4 1.4 Scope of the Study 4 1.5 Dissertation Outline 6 LITERATURE REVIEW 7 2.1 Heavy Metals 7 2.1.1 Copper (Cu) 8 2.1.1.1 Applications 9 v 2.1.1.2 Health Effects of Copper 10 2.1.1.3 Environmental Effects of Copper 11 2.1.2 Cadmium (Cd) 2.2 2.3 2.1.2.1 Applications 13 2.1.2.2 Health Effects of Cadmium 14 2.1.2.3 Environmental Effects of Cadmium 15 Ion Exchange Process Principles 17 2.2.1 Mechanism of Ion Exchange 17 Ion Exchange Resins 20 2.3.1 Classification of Ion Exchange Resins 20 2.3.2 Anion Exchange Resins 21 2.3.3 21 Cation Exchange Resins 2.4 Amberlite 200C Na Resin 22 2.5 Fundamentals of Ion Exchange Fixed-Bed Operations 23 2.5.1 Ion Exchange, Adsorption and Sorption 23 2.5.2 Fixed-Bed Operations 24 2.6 Ion Exchange Capacity 26 2.7 Breakthrough Capacity 27 2.8 Response Surface Methodology (RSM) 28 2.8.1 Central Composite Rotatable Designs (CCRD) 29 2.9 Inductively Coupled Plasma – Mass Spectrometry (ICP-MS) 29 2.10 Effects of Operating Temperature 31 2.11 Effects of Operating pH 31 2.12 Selective Removal of Copper (II) 32 2.13 Selective Removal of Cadmium (II) 34 2.14 Previous Studies Related To Removal of Cu (II) and Cd (II) with Ion Exchange System 3 12 35 METHODOLOGY 37 3.1 Chemicals, Reagents and Equipment 37 3.2 Pre-treatment of Resins 38 3.3 Preparation of Synthetic Solutions 39 3.4 Batch System Study 39 vi 4 3.5 Ion Exchange Column Study 39 3.6 Procedure 40 3.7 Experimental Design 41 3.8 Breakthrough Data analysis 42 3.9 Distribution Coefficient 43 3.10 Space Velocity 44 3.11 Spectrometer Analysis ICP-MS 44 RESULTS AND DISCUSSION 46 4.1 Introduction 46 4.2 pH Determination 47 4.3 Optimization of Column Performance using Minitab 47 4.3.1 Regression Analysis 48 4.3.2 Plots of the Main Effect 49 4.4 4.5 Effects of Operating Parameters in Removing Heavy Metals 51 Determination of the Breakthrough Curves 53 4.5.1 Effect of Initial Concentration on Breakthrough Curves 54 4.5.2 Effect of Bed heights on Breakthrough Curve 60 4.5.3 Effect of Feed Flow Rate on Breakthrough Curves 65 4.6 4.7 5 Equilibrium Distribution Coefficient (Kd) Determination of Space Velocity 70 -1 (SV h ) 72 CONCLUSIONS AND RECOMMENDATIONS 74 5.1 Conclusion 74 5.2 Recommendations for Future Research 75 REFERENCES 77 APPENDICES 82 REFERENCES Abo-Farha, S. 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