ABSTRACT COPPER REMOVAL BY CELLULOSE XANTHOGENATE DERIVED FROM IMPERATA CYLINDRICA L. LEAF POWDER

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1 ABSTRACT COPPER REMOVAL BY CELLULOSE XANTHOGENATE DERIVED FROM IMPERATA CYLINDRICA L. LEAF POWDER The efficiency of cellulose xanthogenate derived from Imperata cylindrica L. leaf powder (CXIC) for removing Cu(II) from aqueous solutions has been investigated. The effects of physicochemical parameters on biosorption capacities such as biosorbent dosage, ph, initial concentration of Cu(II) and contact time were studied. The biosorption capacities of CXIC increased with the rise in ph and Cu(II) concentration but decreased with the increase in biosorbent dose. Biosorption of Cu(II) was considered fast as the time to reach equilibrium was 60 min. Two kinetic models; pseudo-first order and pseudo-second order were applied to analyse the Cu(II) biosorption process, and it was found that the pseudo-second order fitted well with the biosorption data with correlation coefficients (R 2 ) greater than In order to understand the mechanism of biosorption, spectroscopic analyses involving Fourier Transform Infrared (FTIR) and Scanning Electron Microscope (SEM) coupled with Energy Dispersive Spectroscopy (EDS) were carried out on the CXIC. FTIR analyses revealed that -OH, -NH, C=C, COO-, -CS 2 and C-O-C as the major functional groups involved in the binding of Cu(II) and complexation was one of the main mechanisms for the removal of Cu(II) as indicated by FTIR spectra. Ion exchange was another possible mechanism involved as indicated by EDS spectra since there was a release of light metal ions during the biosorption of Cu(II). The isotherm study indicated that the CXIC fitted well with the Langmuir model compared to the Freundlich model. Based on the Langmuir model, the maximum biosorption capacity was mg.g -1. ii

2 ABSTRAK PENYINGKIRAN KUPRUM OLEH XANTHOGENATE SELULOSA DARI SERBUK DAUN IMPERATA CYLINDRICA L. Keberkesanan selulosa xanthogenate terhasil daripada serbuk daun lalang (Imperata cylindrica L.) untuk menyingkirkan Cu(II) daripada larutan akueus telah dikaji. Kesankesan beberapa parameter fizikokimia ke atas biopenjerapan seperti dos biopenjerap, ph, kepekatan Cu(II) dan masa sentuhan turut dikaji. Kapasiti biopenjerapanan oleh CXIC meningkat dengan peningkatan ph dan kepekatan Cu(II) tetapi menurun dengan peningkatan dos biopenjerap. Tempoh biopenjerapan oleh CXIC dianggap singkat iaitu hanya mengambil 60 min untuk mencapai keseimbangan. Dua model kinetik; tertib pseudo pertama dan tertib pseudo kedua telah digunakan untuk menganalisis proses biopenjerapan bagi Cu(II) dan didapati bahawa tertib pseudo kedua adalah sepadan dengan data biopenjerapan di mana R 2 adalah melebihi Bagi memahami mekanisma biopenjerapan, analisis spektroskopi melibatkan Fourier Transform Infrared (FTIR) dan Scanning Electron Microscope (SEM) digabung bersama Energy Dispersive Spectra (EDS) telah dijalankan ke atas CXIC. Analisis FTIR menunjukkan bahawa -OH, -NH, C=C, COO-, -CS 2 and C-O-C adalah kumpulan berfungsi utama yang terlibat di dalam pengikatan Cu (II) dan pengkompleksan adalah salah satu mekanisma utama terhadap penyingkiran Cu (II) seperti yang ditunjukkan oleh spektra FTIR. Pertukaran ion merupakan satu lagi mekanisma yang mungkin terlibat seperti yang ditunjukkan oleh spektra EDS kerana terdapat penyingkiran ion-ion logam ringan sepanjang biopenjerapan Cu (II). Kajian isoterma menunjukkan CXIC menepati model Langmuir berbanding model Freundlich. Berdasarkan model Langmuir, kapasiti maksimum biopenjerapan adalah mg.g -1. iii

3 ACKNOWLEDGEMENTS First of all, I am grateful to Allah Almighty for his Blessing and Guidance. I would like to complete this dissertation entitled Copper Removal by Cellulose Xanthogenate Derived from Imperata cylindrica L. Leaf Powder. I would like to acknowledge and express my deepest, sincere gratitude and appreciation to my supervisors Dr. Ghufran bin Redzwan (UM) and Prof Madya Dr. Megat Ahmad Kamal bin Megat Hanafiah (UiTM) for their supervision, guidance, advice, understanding, encouragement, faith and constructive critics that led to the successful completion of this project. Their understanding and patience in the project were most comforting and necessary. I would also like to acknowledge all the lab staff at the Environmental Laboratory for their assistance throughout the course of this study. My special thanks goes to my fellow friends, Tn. Hj Hayub bin Ta and Tn. Hj. Rahimi bin Mat Noor in helping me to handle the spectroscopy devices and providing guidance in the process of data analysis. Also thanks to the rest of my friends for their help, meaningful discussion, memories shared and constructive suggestion throughout this study. Lastly, I would like to extend my deepest appreciation to my family members especially to my wife Siti Noorezrin binti Mahmod for her support, understanding, inspiration and ecouragement during the course of the study. Zubir bin Othman iv

4 TABLE OF CONTENTS Page CHAPTER 1 INTRODUCTION 1.1 Background Problem statement Significance of study Aim and objectives of study Scope of work 5 CHAPTER 2 LITERATURE REVIEW 2.1 Introduction Heavy metal pollution Copper polution Removal of heavy metal Removal of copper Biosorption study on heavy metal removal Kinetic of biosorption Inexpensive and effective biosorbents The use of non living plant materials as biosorbent Modification of biosorbent Cellulose xanthogenate as a modified biosorbent 25 CHAPTER 3 METHODOLOGY 3.1 Characterisation of CXIC Sample collection Preparation of CXIC Fourier transform infrared (FTIR) analysis 28 v

5 3.1.4 SEM and EDS analysis Experimental design to determine the effects of various physicochemical parameters on biosorption of Cu(II) Cu(II) aqueous solution preparation Batch biosorption studies Effect of biosorbent dose Effect of ph Equations used Effect of initial Cu(II) concentration, contact time and kinetics Equations used Experimental design to determine the maximum biosorption capacity of CXIC by isotherm of Cu(II) Equations used Analysis of Cu(II) 35 CHAPTER 4 RESULTS AND DISCUSSION 4.1 Characterisation of CXIC Fourier transform infrared (FTIR) analysis SEM and EDS analysis The effect of various physicochemical parameters on biosorption of Cu(II) Effect of biosorbent dose Effect of ph Effect of initial Cu(II) concentration and contact time Biosorption kinetic studies Maximum biosorption capacity of CXIC by isotherm of Cu(II) 54 vi

6 CHAPTER 5 CONCLUSION AND RECOMMENDATIONS 61 APPENDIX 63 REFERENCES 82 vii

7 LIST OF FIGURES Figure Caption Page 1.1 Flow chart of the batch biosorption study FTIR spectra of UIC, CXIC before and after Cu(II) biosorption SEM images at 500X magnification and EDS spectra of UIC SEM images at 500X magnification and EDS spectra of CXIC before biosorption 4.4 SEM images at 500X magnification and EDS spectra of CXIC after biosorption 4.5 Effect of biosorbent dose on Cu(II) biosorption onto CXIC (initial Cu(II) concentration = 10mg.L -1 ; shaking rate = 150rpm; ph = 4) 4.6 Effect of ph on the Cu (II) biosorption by CXIC (initial Cu(II) concentration = 10mg.L -1 ; shaking rate = 150rpm; biosorbent weight = 0.05g) 4.7 Effect of initial Cu(II) concentration and contact time of Cu(II) biosorption by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) 4.8 Pseudo-first order of Cu(II) biosorption by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) 4.9 Pseudo-second order of Cu(II) biosorption by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) 4.10 General biosorption isotherm plot of Cu(II) by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) Linearized Langmuir isotherm plot of Cu(II) biosorption by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) 4.12 Linearized Freundlich isotherm plot of Cu(II) biosorption by CXIC (biosorbent weight = 0.05g; ph = 4; volume = 50ml; shaking rate = 150rpm) viii

8 LIST OF TABLES Table Caption Page 2.1 Anthropogenic sources of heavy metals in the environment Permissible limit and health effects of various toxic heavy metals Conventional treatment technologies for the removal of heavy metals from the wastewaters and associated advantages and disadvantages Major functional groups for biosorption Proposed models used in the study of biosorption Summary of modified biosorbents for the removal of copper from aqueous solution ICP-OES setting parameters for analysis of copper Amount of Cu(II) removed (%) and adsorbed (mg.g -1 ) at different biosorbent dosage 4.2 The pseudo-first order and pseudo-second order at different concentration of Cu(II) 4.3 Langmuir and Freundlich isotherm constants and correlation coefficients 4.4 Comparison of biosorption capacity of CXIC for Cu(II) with other biosorbents ix

9 LIST OF SYMBOLS AND ABBREVIATIONS SEM EDS FTIR : Scanning Electron Microscope : Energy Dispersive Spectroscopy : Fourier Transform Infra-red CXIC : Cellulose Xanthogenate of Imperata cylindrica L. ICP-OES mg.l -1 mg.g -1 COD BOD TOC M : Inductively Coupled Plasma Optical Emission Spectroscopy : Milligram per litre : Miligram per gram : Chemical Oxygen Demand : Biological Oxygen Demand : Total Organic Carbon : Molar UIC : Untreated Imperata cylindrica L. KBr HCl NaOH Cu Cd Cr Mn U V Zn Ni : Potassium bromide : Hydrochloric acid : Sodium hydroxide : Copper : Cadmium : Chromium : Manganese : Uranium : Vanadium : Zinc : Nickel x

10 Pb Hg As Ti Ba Mg Na Cu(II) g : Lead : Mercury : Arsenic :Titanium : Barium : Magnesium : Sodium : Copper (II) ion : gram % : percentage k ev H + min sec Neb Aux ml rpm min -1 R 2 q e,cal q e,exp q max nm : kilo : electron volt : hydrogen ion : minute : second : nebulizer : auxillary : mililitre : rotation per minute : per minute : regression coefficient : calculated value of biosorption capacity : experimental value of biosorption capacity : maximum value of biosorption capacity : nanometre xi

11 LIST OF APPENDICES Appendix Caption Page A Plausible mechanisms of biosorption 64 B Abbreviated table of group frequencies for organic functional groups 65 C Group frequency region and fingerprint region 65 D Analytical sequence of ICP-OES 66 E Calibration graph 67 F Examples of ICP spectra 68 G Examples of ICP data 70 H Results for effect of biosorbent dose 74 I Results for effect of ph 74 J Kinetic study (Concentration & Contact Time) 75 K Isotherm Study 76 L Examples of calculation 77 xii

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