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Stable Isotopes Analyses of Carbon-13 and Nitrogen-15 in Kelantan River Sediments

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Stable Isotopes Analyses of Carbon-13 and Nitrogen-15 in Kelantan River Sediments STABLE ISOTOPES ANALYSES OF CARBON-13 AND NITROGEN-15 IN KELANTAN RIVER SEDIMENTS NUR ZAFIRAH BINTI ZULKIFLI UNIVERSITI SAINS MALAYSIA 2019 STABLE ISOTOPES ANALYSES OF CARBON-13 AND NITROGEN-15 IN KELANTAN RIVER SEDIMENTS by NUR ZAFIRAH BINTI ZULKIFLI Thesis submitted is fulfillment of the requirements for the degree of Master of Science March 2019 ACKNOWLEDGEMENT Alhamdulillah, thanks to the grace of Allah, the Most Compassionate and Merciful because His consent gives me the guidance to complete this thesis. A very invaluable appreciation and thanks to my supervisor, Dr. Muhammad Izzuddin Syakir Bin Ishak for giving me much support and guidance throughout my research project. His guidance had helped me from the research stage until the phase of writing this thesis. I felt very overwhelmed by having a very good supervisor and mentor who gave a lot of inspiration in this research. In addition, I would like to thank Dr. Syahidah Akmal Binti Mohammad for helping me analysed the isotope data. Next, I would also like to thank the laboratory assistants in the Industrial Technology School, who taught me ways to use the equipment and machines in the lab because without their help I might fail to carry out this experiment. I am also grateful for having friends who were always on my side during the up and down times in completing this thesis. Many thanks to all of them and may God reward all of their good deeds. Finally, my endless gratitude is extended to my parents and lovely family for all the supports and prayers throughout my study period. Thanks to all of your prayers, this thesis is perfectly completed. Thank you. ii TABLE OF CONTENT Acknowledgement ii Table of Contents iii List of Tables vii List of Figures viii List of Abbreviations and Symbols x Abstrak xii Abstract xiv CHAPTER 1- INTRODUCTION 1.1 Background of Study 1 1.2 Problem Statement 3 1.3 Objectives of the Study 4 1.4 Hypothesis 5 1.5 Scope of Study 6 CHAPTER 2- LITERATURE REVIEW 2.1 Challenges Faced by Kelantan Watersheds 7 2.2 Soil Erosion and Sedimentation 7 2.2.1 The Processes of Erosion and Sedimentation 8 2.3 The Implication of Anthropogenic Activities on Watersheds 10 2.4 Hydrology and environment impact studies of Kelantan watershed 11 2.5 Sediment Tracing within Watersheds 14 2.6 The Source of Tracing Techniques in Sediments 15 iii 2.6.1 Tracing Techniques in Sediments 16 2.6.2 Stable Isotopes 18 2.6.2(a) Case Studies 20 2.6.2(b) Limitation 21 2.6.3 C/N ratio 22 2.6.3(a) Case Studies 23 2.6.3(b) Limitation 24 2.6.4 Radioisotopes 25 2.6.4(a) Case Studies 27 2.6.4(b) Limitation 28 2.6.5 Heavy Metal 28 2.6.5(a) Case Studies 30 2.6.5(b) Limitation 31 2.6.6 Magnetic Properties 34 2.6.6(a) Case Studies 33 2.6.6(b) Limitation 34 CHAPTER 3- METHODOLOGY 3.1 Study Area 36 3.1.1 Kelantan Basin 36 3.1.2 Climate and Hydrology of Kelantan Basin 40 3.2 Methodology 41 3.2.1 Experimental design 41 3.2.2 Sample Collection of River Sediments 42 iv 3.2.3 Sample Preparation 43 3.2.4 Stable Isotope Analysis 43 3.2.5 Carbon Nitrogen Ration (C/N Ratio) Analysis 47 3.2.6 Sediement Yield and WaterQuality Data 48 3.3 Statistical Analysis 49 3.3.1 Isotope Analysis 49 3.3.2 Sediment Yield Data 50 3.3.3 Water Quality Data 50 CHAPTER 4- RESULTS AND DISCUSSIONS 4.0 Introduction 51 4.1 Stable Isotope Carbon (13C) 51 4.1.1 The Temporal Distribution of Stable Carbon Isotopes (13C) in 51 Kelantan Rivers 4.1.2 The Spatial Distribution of Stable Carbon Isotopes (13C) in Kelantan 52 Rivers 4.2 Stable Isotope Nitrogen (15N) 56 4.2.1 The Temporal Distribution of Stable Nitrogen Isotopes (15N) in 56 …Kelantan Rivers 4.2.2 The Spatial Distribution of Stable Nitrogen Isotopes (15N) in 59 …Kelantan Rivers 4.3 Carbon to Nitrogen Ratio (C/N Ratio) 61 4.4 Sediment Yield in Kelantan River Networks 63 4.5 Water Quality Analysis 65 4.6 Summary 67 v CHAPTER 5- CONCLUSION AND RECOMMENDATIONS 5.1 Conclusion 68 5.2 Recommendations for Future Study 69 REFERENCES 70 APPENDICES 93 vi LIST OF TABLES Page Table 2.1 The consequences within watershed caused by natural processes 11 and anthropogenic activities. Table 2.2 Summaries of different sediment tracing techniques according to 16 their timeframe, scales, advantages and limitations. Table 3.1 Point for sampling 40 Table 3.2 Experimental design 49 Table 4.1 Spatial isotopic composition of stable isotope 13C in sediment 54 Table 4.2 Spatial isotopic composition of stable isotope 15N in sediments 60 Table 4.3 Proposed factor of sediment yields in Kelantan watershed 64 Table 4.4 Factor loadings of sediment yields over two principal components 64 F1. F1 represent 99% of cumulative loading indicate significant sedimentation in Kelantan watershed for all year round. F2 showed significant role of NEM in intensifying sediment yield of Kelantan watershed. Table 4.5 Proposed factor of water parameter in Kelantan catchment. Factor 65 loading 1, (F1) represents the anthropogenic factors & Factor loading 2, (F2) represents the key indicator of the river health. vii LIST OF FIGURES Page Figure 1.1 The cross section of sediment mechanism (in terms of isotope 5 perspective) in a river Figure 2.1 The erosion process is driven by water (rain) agents. Water 9 droplets will cause detachment, transport and translocation of soil particles thus deposition of sediment (Hairsine & Rose, 1991). Figure 3.1 Peninsular Malaysia map 38 Figure 3.2 Map of the Kelantan River and study sites 39 Figure 3.3 Kelantan rainfall data since 2013 to 2016 40 Figure 3.4 Ekman Grab Sampler 42 Figure 3.5 Tools used for sample preparation into tin capsule 44 Figure 3.6 Isotope-ratio mass spectrometry (IRMS) 44 Figure 3.7 Perkin Elmer 2400 Series II CHN Elemental Analyser 47 Figure 3.8 The process of experimental design for sediment analysis 41 Figure 3.9 Process of crimpling sample in tin capsule 45 Figure 4.1 Bar frequency 13C [‰] sediments from two different seasons; 51 the Southwest Monsoon (July) and Northeast monsoon (January) Figure 4.2 Spatial variation in 13C in sediments in the Kelantan rivers. 53 Depletion trend towards the ocean characterized by spatial variations of 13C in sediment describe the metabolism of the watershed (Photosynthesis: enrich versus respiration: deplete) – Carbon cycle. Figure 4.3 Bar frequency 15N [‰] sediments on two different seasons; the 56 Southwest Monsoon (July) and Northeast monsoon (January) Figure 4.4 Nitrogen conversion and processes affecting 15N values in forest 57 ecosystem which result in enrich and deplete of the product (Source Nadelhoffer & Fry 1994; Kendall, 1998). viii Figure 4.5 The average value of 15N in July and January. Organic nitrogen 58 signatures are more pronounced during January. Figure 4.6 Spatial variation in 15N in sediments in the Kelantan rivers. No 59 trend of 15N is observed across the river networks, suggesting complex nitrogen cycle superimposed by the anthropogenic activities in the watershed. Figure 4.7 The 13C and C/N ratio of various types of terrestrial and aquatic 62 organic matters overlapping by the sediment range of Kelantan catchments ix LIST OF ABBREVIATIONS AND SYMBOLS % Percentage Delta Plus minus Approximately 13C Delta carbon 13 15N Delta nitrogen 15 < Less than > Greater than ‰ Parts per mill ANOVA Analysis of variance BOD Biochemical oxygen demand C/N ratio Ratio of the mass of carbon to the mass of nitrogen in a substance C3 The plants exhibiting C3 pathway C4 The plants exhibiting C4 pathway CAM Crassulacean acid metabolism CHN Used to measure Carbon (C), Hydrogen (H) and Nitrogen (N) COD Chemical oxygen demand DID Department of Irrigation and Drainage DO Dissolved oxygen DOE Department of Environment IRMS Isotopic Ratio Mass Spectrometer MEA Millennium ecosystem assessment mg/l Milligram per liter N Nitrogen NH3-N Ammoniacal nitrogen + Ammonium NH4 - Ammonia NO3 PCA Principal component analysis x pH pH meter POM Particulate organic matter SPSS Statistical Package for the Social Sciences SS Suspended solid xi ANALISIS ISOTOP STABIL KARBON-13 DAN NITROGEN-15 DALAM SEDIMEN DI SUNGAI KELANTAN ABSTRAK Peningkatan proses pemendapan telah meningkatkan ancaman bencana alam di Sungai Kelantan (cth: banjir). Memandangkan kesan hakisan tanah kepada pemendapan, pengenalpastian sumber hakisan adalah penting bagi pengurusan tadahan air di Kelantan. Isotop stabil karbon dan nitrogen, bersama-sama dengan analisis nisbah C/N telah dijalankan untuk mengenal pasti sumber pendapan di sungai Kelantan. Pensampelan telah dilakukan pada bulan Julai 2015 (Monsun Barat Daya, SWM) yang mewakili musim kering dan Januari 2016 untuk musim hujan (Northeast Monsun, NEM). Sampel dianalisis dengan menggunakan Spectrometer Mass Ratio Isotopic Analysis Elementary (EA-IRMS) dan Perkin Elmer 2400 Series II CHN Elemental Analyzer. Isotop stabil 13C menunjukkan bahawa tumbuhan jenis C3 dominan di tadahan air Sungai Kelantan dengan tidak mempunyai perbezaan statistik yang ketara antara bulan Julai dan Januari. Ini menunjukkan sumber hakisan yang sama terutamanya dari pokok yang berkayu seperti pokok hutan, getah dan kelapa sawit. Nilai 15N yang berbeza dapat diperhatikan pada bahan organic tanah pada bulan Januari (NEM) yang menunjukkan pembersihan yang berlebihan (hakisan), natijah dari peranan iklim terhadap peningkatan pemendapan. Permerhatian terhadap nisbah C/N yang dicirikan oleh sedimen di Sungai Kelantan adalah autochthonous, menunjukkan perolehan dari sumber akuatik. BOD, COD dan SS adalah parameter utama yang menentukan kualiti air Sungai Kelantan.
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