本研究使用各種實驗室合成的先進吸附劑，包括銅改性弱鹼陰離子交換樹脂(Cu-WAER) 和各種氧化鐵，研究了營養物鹽（NH4
+-N 和 P）和砷的去除機制。為了更好地了解相應的吸附過程，對各種系統物理化學性質的影響進行了分析，例如 pH值、競爭離子、溫度等，以及常規動力學、等溫線和熱力學研究。弱陰離子交換樹脂經過 Cu2+ (Cu -WAER) 改性，能夠選擇性吸附銨和磷酸鹽；銨在吸附過程中先吸熱去質子化後與 Cu2+ 離子發生放熱錯合反應 (H0= -68.03 kJ/mol)，這種化學吸附符合朗繆爾等溫和二級動力吸附，在 60 分鐘內，吸附達到平衡，速率常數非常高，為 0.01-0.3g/mg-min，此外，也獲得了 7.9-13.6 mg/g 的顯著 NH4+ 吸附容量。由於-NH/CuCl2/NH3體系的緩衝作用，最終pH 維持在5.3-5.8，隨著初始pH 值的升高，吸附能力有效提高， NaCl、KCl、CaCl2 和 MgCl2 等氯鹽為 1.0-5.0 mM 時，可使 NH4+ 的吸附量增加了 1.5-1.9 倍，但是，過量的鹽卻會阻止吸附。使用過的吸附劑通過浸泡在 0.15 M NaCl 溶液中可成功回收，經過四個回收循環，其吸附能力仍保留了 94.37-99.97%。另一方面，雖然金屬複合吸附劑具有顯著的吸附能力，但由於緊密結合，難以再生，基於磷酸鹽結合蛋白 (PBPs)，通過將磷酸鹽物質與多個氫鍵結合，在高吸附和再生能力之間取得平衡的啟發，本研究開發Cu-WAER 作為先進的磷酸鹽吸附劑。對磷酸鹽而言與金屬物質在現有雜化吸附劑吸附的作用不同，Cu2+離子主要驅動磷酸鹽從液體擴散到樹脂，然後誘導磷酸鹽物質與多個-NH2+/-NH 基團鍵合，這種吸附不僅非常有效
（G0 = -16.83 ~ -20.14 kJ/mol）且具有高熵（S0 = 132.47 J/mol-K），此外，錯合增強了吸附過程中磷酸鹽的選擇性。再生過程中， Cu2+ 在弱鹼條件下發生 -Cu-O- 的轉變，因此藉由斥力幫助磷酸鹽物種脫附。整體而言， Cu-WAER 樹脂具有很強的磷酸鹽吸附能力（31.94 至 61.03 mg-P/g）和良好的競爭陰離子耐受性，同時也可以使用稀NaOH 溶液（0.05 N）成功回收，即使經過 5 次循環，也可以有 95.07% 的吸附能力。另外動態填充床柱研究結果顯示，當初始濃度和流速分別為 10 mg-P/L 和 2 ml/min 時，Cu-WAER 在達到其耗盡閾值之前可以處理超過 140 倍柱體積（BV )。在砷物種吸附方面，本研究合成了一系列氧化鐵，包括針鐵礦、赤鐵礦、磁赤鐵礦和磁鐵礦作為吸附劑，以比較 As(V) 和 As(III) 的去除率。即便具有與-Fe-OH 和-Fe=O 相同的官能團，不同晶系的氧化鐵表現出不同的除砷能力，根據 XPS 和 EDS 結果，砷明顯通過表面錯合和/共沉澱附著在氧化鐵表面，此外，與 EDS (14.5%) 結果相比，XPS (19.23%) 中O/Fe 的上升幅度略大，這表明吸附主要以表面錯合為主，而不是大量的共沉澱。將As(V) 和 As(III) 吸附結果與支持化學吸附的 Langmuir 等溫線進行了比較。發現最高的 As(V) 和 As(III) 吸附能力分別出現在針鐵礦 (0.096 mg/m2) 和磁赤鐵礦 (0.157mg/m2)的斜方晶系和立方晶系中，而動力學研究表明，As(V) 和 As(III) 分別在 200-360 分鐘和 50-360 分鐘內達到平衡，As(V) 和 As(III) 的最大吸附速率常數分別出現在針鐵礦
(1.837 L/mg-h) 和磁鐵礦 (12.227 L/mg-h) 中，而最高脫附常數在針鐵礦與磁赤鐵礦中則為0.696 與1.896/h。此外，提出了考慮非平衡吸附的通用速率模型（GRM）來預測填充床柱研究的突破曲線。 GRM 的數值解顯示了模型預測與實驗結果的良好擬合(Adj R2=0.922-0.992)，這表明該模型有可能在不進行柱研究的情況下預測突破曲線。

The removal mechanisms of nutrients (NH4+-N and P) and arsenic are investigated in this work using various laboratory-synthesized advanced adsorbents, including Cu-modified weak base anion exchange resin (Cu-WAER) and various iron oxides. For a better understanding of the corresponding adsorption processes, investigations on the effects of various system physicochemical properties—such as pH, competing ions, temperature, etc. along with customary kinetic, isotherm, and thermodynamic studies are conducted. Considering high formation complex between Cu specie and NH3(K_f=1.1×〖10〗^13); a weak anion exchange resin has modified by Cu2+ (Cu-WAER) to enable the selective adsorption of ammonium-N and phosphate. Exothermic complexation (H0= -68.03 kJ/mol) to the Cu2+ ions followed endothermic deprotonation in the ammonium adsorption process. Such chemisorption adhered to the Langmuir isotherm and second-order kinetics. Within 18-60 min, the adsorption achieved equilibrium with a very high rate constant of 0.01-0.3 g/mg-min. Additionally, a significant NH4+ adsorption capacity of 7.9-13.6 mg/g was attained. Because of the buffering action of the -NH/CuCl2/NH3 system, the final pH was maintained at 5.3-5.8, and the adsorption ability effectively increased with rising initial pH values. The coexistence of salts with a chloride ion of 1.0–5.0 mM, such as NaCl, KCl, CaCl2, and MgCl2, increased the adsorption of NH4+ by 1.5–1.9 times. Salt in excess prevented the adsorption, though. The utilized adsorbent was successfully recovered by soaking in a 0.15 M NaCl solution, and following four recovery cycles, 94.37–99.97 % of its adsorption ability was retained.Meanwhile, though hybrid-based phosphate adsorbents offer significant adsorption capacity, regeneration is difficult due to strong bonding. Considering that limitation and inspired by phosphate-binding proteins (PBPs) which reached a trade-off between high adsorption and regeneration ability by binding phosphate species with multiple hydrogen bonds, the same Cu-WAER is used for an alternative advanced phosphate adsorbent. Different from the role of metal species in the promoted adsorption of existing hybrid-based adsorbents, the Cu2+ ions mainly drove phosphate diffusion from the liquid to the pores of resin and then induced the phosphate species to bond with multiple hydrogen or electrostatic bond through –NH2+/–NH groups. This adsorption was extremely exergonic (G0= -16.83 ~ -20.14 kJ/mol) and had an entropy of S0 = 132.47 J/mol-K. Furthermore, because the complexation enhanced the sorption process, it improved the phosphate selectivity. During the regeneration, the Cu2+ to -Cu-O- transformation could occur under high alkaline conditions and repelled the adsorbed phosphate species to facilitate desorption. Since the Cu-WAER resin had strong phosphate adsorptions (31.94 to 61.03 mg-P/g) and good competing-anion tolerance, it could also be successfully recovered using a dilute NaOH solution (0.05 N). Using 0.1 N NaOH as the desorption solution, it is possible to recover the adsorbent with a recovery efficiency of 95.07 percent, even after five recycles. The results of a dynamic packed bed column investigation showed that when the initial concentration and flow rate were 10 mg-P/L and 2 ml/min respectively, Cu-WAER could treat water with a column volume more than 140 times bed volume (BV) before reaching its exhaustion threshold. Moreover, a General Rate Model (GRM) considering non-equilibrium adsorption is proposed to predict the breakthrough curve of a packed bed column study. Numerical solution of GRM shown a good fitting (Adj R2=0.922-0.992) of model prediction with experimental result which suggested potential use of the model to predict the breakthrough curve without performing the column study. In a separate investigation, a range of iron oxides, including goethite, hematite, maghemite, and magnetite, were synthesized as adsorbents to compare As(V) and As(III) removal to understand mainly the effect of crystal system. Having though same functional groups as -Fe-OH and –Fe=O; different crystal systems of iron oxides shown a wide range of arsenic removal ability. However, a thorough study is yet to be performed to understand the best performed iron oxide for As(III) and As(V). Synthesized iron oxide phases were examined using XRD solid-phase characterization. According to XPS and EDS results, arsenic had apparently attached to surfaces of iron oxide through surface complexation along with possible co-precipitation. Additionally, a marginally greater rise in O/Fe in the XPS (19.23%) compared to the EDS (14.5%) result would point to dominating surface complexation rather than co-precipitation in bulk. The As(V) and As(III) adsorption findings were compared to the Langmuir isotherm, which supported chemisorption inner-sphere complex. The highest As(V) and As(III) adsorption capabilities were found to be in the orthorhombic and cubic crystal systems of goethite (0.096 mg/m2) and maghemite (0.157 mg/m2), respectively. Kinetic investigations showed that As(V) and As(III) reached equilibrium in 200–360 minutes and 50–360 minutes, respectively which indicated good removal rate for potentially harder As(III) removal. The Langmuir kinetic model and pseudo-second-order fit the experimental results far better than pseudo-first-order. The maximum adsorption rate constant for As(V) and As(III) respectively, were found in goethite (1.837 L/mg-h) and magnetite (12.227 L/mg-h), while the highest desorption rate constant for As(V) and As(III) were found in goethite (0.696 /h) and maghemite (1.896 /h). The current study can help to understand the general concept of selecting the optimum iron oxide. Finally, using the General Rate Model (GRM), probable breakthrough and exhaustion times for As(III) and As(V) are estimated for optimized iron oxide packed column.

摘要 i
Abstract ii
Table of Contents iii
List of Figures vii
List of Tables x
Chapter 1. Introduction 1
1.1. Background and Motivation 1
1.2. Research objectives 4
Chapter 2. Literature Review 6
2.1. Few selected pollutants and their effect on environment 6
2.1.1. Influence of ammonium and phosphate on eutrophication 6
2.1.2. Arsenic contamination in the environment 7
2.2. Selective ammonium (NH4+) removal by Cu-modified resin 7
2.2.1. Traditional ammonium adsorbents and their drawbacks 7
2.2.2. Metal-supported hybrid ion exchange resin as ammonium adsorbents 9
2.2.3. Challenges and limitations of ammonium removal 9
2.2.4. Cu-supported ion exchange resin for ammonium removal 9
2.3. Selective phosphate removal by Cu-modified weak anion exchange resin 10
2.3.1. Traditional adsorbents for phosphate and their drawbacks 10
2.3.2. Metal-supported hybrid ion exchange resin as phosphate adsorbents 10
2.3.3. Bio-inspired Cu-supported anion exchange resin for phosphate removal 11
2.4. Comparative and insightful study on arsenic complexation employing synthesized iron oxide minerals 12
2.4.1. Arsenic interaction with iron substance 12
2.4.2. Research scope on arsenic removal by iron oxide 15
2.5. Development of a column breakthrough model with non-equilibrium reactions 15
2.5.1. Existing empirical models and General Rate Model (GRM) for breakthrough curve and their limitations 15
2.5.2. Development of a General Rate Model with non-equilibrium reactions 17
Chapter 3. Experimental Section 21
3.1. Selective ammonium (NH4+) removal by Cu modified resin 21
3.1.1. Preparation of Cu modified weak anion exchange resin (Cu-WAER) 21
3.1.2. NH4+ adsorption study 21
3.1.3. Regeneration study 22
3.2. Phosphate removal by Cu modified weak anion exchange resin 22
3.2.1. Phosphate adsorption study 22
3.2.2. Regeneration study 22
3.2.3. Column study 23
3.3. Arsenic complexation employing synthesized iron oxide minerals 25
3.3.1. Chemical reagents and arsenic solution 25
3.3.2. Quantification of As(III) and As(V) 25
3.3.3. Synthesis of different iron oxides 26
3.3.4. Kinetic and Isotherm study of arsenic adsorption by iron oxide 28
3.4. Material Characterization and Analytical Instruments 28
3.4.1. Brunauer–Emmett–Teller (BET) Surface Area Characterizations 28
3.4.2. Scanning Electron Microscopy (SEM)-Energy Dispersive X-ray Spectroscopy (EDS) 28
3.4.3. X-ray Photoelectron Spectroscopy (XPS) 28
3.4.4. Zeta Potential Analyzer 29
3.4.5. Fourier Transform Infra Red (FTIR) Spectroscopy 29
3.4.6. X-Ray Diffraction (XRD) 29
3.4.7. Ion Chromatography (IC) 29
3.4.8. Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) 29
3.5. Development of Langmuir Kinetic Model 30
3.6. Data Management 33
3.6.1. Kinetic models 33
3.6.2. Adsorption isotherm models 34
3.6.3. Empirical model for column study 34
3.6.4. Statistical analysis for evaluation of model validity of different model 35
Chapter 4. Removal of Ammonium-N (NH4+-N) by Cu modified amino functionalized resin 36
4.1. Introduction 36
4.2. Results and Discussion 37
4.2.1. Solid phase characterization 37
4.2.2. NH4+-N adsorption by Cu-WAER 39
4.2.3. Influence of salts 46
4.2.4. Reusability study 48
4.3. Conclusion 48
4.4. Appendix 50
Chapter 5. Bio inspired phosphate adsorption by Cu modified amino functionalized resin 52
5.1. Introduction 52
5.2. Results and Discussion 53
5.2.1. Solid phase characterization 53
5.2.2. Phosphate adsorption by Cu-WAER 56
5.2.3. Influence of salts 71
5.2.4. Reusability study 72
5.2.5. Packed bed column studies 72
5.3. Conclusions 75
5.4 Appendix 76
Chapter 6. Comparative and insightful study on arsenic complexation employing synthesized iron oxide minerals 79
6.1. Introduction 79
6.2. Results and Discussion 80
6.2.1. Solid phase characterization 80
6.2.2. Isotherm study of As(III) and As(V) removal 85
6.2.3. Kinetic study of As(III) and As(V) removal 89
6.2.4. Effect of crystal structures on arsenic removal 95
6.3. Conclusion 96
6.4. Appendix 97
Chapter 7. Development of a column breakthrough model with non-equilibrium reactions 99
7.1. Introduction 99
7.2. Results and Discussion 99
7.2.1. Comparison of model prediction with the experimental result of the breakthrough curve for phosphate removal by Cu-WAER 100
7.2.2. Effect of inlet flow rate on prediction of the breakthrough curve for arsenic removal by iron oxide 102
7.2.3. Effect of inlet arsenic concentration on prediction of the breakthrough curve for arsenic removal by iron oxide 103
7.2.4. Effect of sorbent bed height on prediction of the breakthrough curve for arsenic removal by iron oxide 104
7.3. Conclusion 104
7.4. Appendix 106
Chapter 8. Conclusion and Perspectives 110
Reference 112

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