以二氧化鈦/單壁奈米碳管/網版印刷電極 進行COD快速量測

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以二氧化鈦/單壁奈米碳管/網版印刷電極進行COD快速量測
(Rapid Detection of Chemical Oxygen Demand by Titanium Dioxide/Single-Walled Carbon Nanotubes/Screen-Printed Electrode)

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摘要(中)

環境保護和水質監測是當今社會面臨的重要課題之一，化學需氧量（COD）的檢測對於評估水體中有機污染物的含量至關重要。傳統COD分析方法仍存在許多缺點，例如：分析時間長、氧化能力受限、有毒性試劑的二次污染等。而電化學方法不僅具有快速分析、高靈敏度、環境友善等優點，還可應用於現場監測及分析，使其逐漸受到關注。
本研究透過溶膠-凝膠法製備二氧化鈦/單壁奈米碳管複合材料並用於修飾電極，以線性掃描伏安法在最佳掃描條件（電解質為0.1 M氯化鈉緩衝溶液、掃描速度為0.15 V s–1）下進行水樣之COD分析，包括模擬水樣及真實水樣。其中，模擬水樣分為單一水樣及複合水樣，選用的有機物包含：鄰苯二甲酸氫鉀、葡萄糖、乙醇胺、水楊酸、二甲基甲醯胺。理論需氧量（ThOD）線性範圍介於20–100 mg L–1。此外，選用了其中三種有機物倆倆混合成不同比例的複合水樣，以探討有機物間彼此的相互作用。結果顯示，分析所得的峰值電流與ThOD皆呈現正相關。對於修飾電極的再現性分析，相對標準偏差為4.93%。真實水樣的部分則是將製備的修飾電極用於測定平鎮工業區污水廠之放流水，結果表明良好的線性特性使其在真實水樣中的應用變得更為實際。因此，證實了二氧化鈦/單壁奈米碳管/網版印刷電極在COD量測方面具有良好的潛力，使其在環境監測、水質管理和相關領域中具有廣泛的應用前景。

摘要(英)

Environmental protection and water quality monitoring are one of the important issues facing today′s society. The detection of chemical oxygen demand (COD) is crucial for assessing the content of organic pollutants in water bodies. Traditional COD analysis methods still have many shortcomings, such as long analysis time, limited oxidation capacity, and secondary pollution from toxic reagents. The electrochemical method not only has the advantages of rapid analysis, high sensitivity, and environmental friendliness, but can also be applied to on-site monitoring and analysis, making it gradually attract attention.
In this study, titanium dioxide/single-walled carbon nanotube composites were prepared by the sol-gel method and used to modify screen-printed electrodes (SPE). Linear scan voltammetry (LSV) was used under optimal scanning conditions (the electrolyte was 0.1 M sodium chloride buffer solution, COD analysis of water samples, including simulated water samples and real water samples, is performed at a scanning speed of 0.15 V s–1). Among them, simulated water samples are divided into single water samples and composite water samples. The selected organic substances include: potassium hydrogen phthalate, glucose, ethanolamine, salicylic acid, and dimethylformamide. The theoretical oxygen demand (ThOD) linear range is between 20–100 mg L–1. In addition, three of the organic compounds were mixed into composite water samples in different proportions to explore the interaction between the organic compounds. The results showed that the peak current analyzed and ThOD showed a positive correlation. For the reproducibility analysis of the modified electrode, the relative standard deviation was 4.93%. For real water samples, the prepared modified electrode was used to measure the discharge water from the sewage treatment plant in Pingzhen Industrial Zone. The results showed that the good linear characteristics made its application in real water samples more practical. Therefore, it is confirmed that the TiO2/SWCNT/SPE has good potential in COD measurement, making it have broad application prospects in environmental monitoring, water quality management, and related fields.

關鍵字(中)

★ 化學需氧量
★ 線性掃描伏安法
★ 二氧化鈦
★ 單壁奈米碳管
★ 網版印刷電極

關鍵字(英)

★ chemical oxygen demand
★ linear sweep voltammetry
★ titanium dioxide
★ single-walled carbon nanotube
★ screen-printed electrode

論文目次

Contents
摘要 i
Abstract i
Contents iii
List of Figures v
List of Tables vii
Chapter 1 Introduction 1
1.1 Background 1
1.2 Objectives 3
Chapter 2 Literature Reviews 6
2.1 Detection method of organic compounds 6
2.1.1 Chemical oxygen demand (COD) 7
2.1.2 Detection of COD by electrochemical analysis method 7
2.1.3 Theoretical oxygen demand (ThOD) 9
2.2 Electrochemical analysis technology 10
2.2.1 Electrochemical reaction 10
2.2.2 Electrochemical system and principle 11
2.2.3 Voltammetric reactions and principles 14
2.3 Electrode modified materials for COD analysis 20
2.3.1 Carbon nanotube (CNT) 21
2.3.2 Titanium dioxide (TiO2) 25
2.3.3 Synergy of titanium dioxide and single-walled carbon nanotubes 31
2.4 Electrochemical analysis of organic matter 32
Chapter 3 Materials and Methods 34
3.1 Instrumentation 34
3.2 Materials and Chemicals 35
3.2.1 TiO2/SWCNT/SPE 35
3.2.2 Analyte for voltammetric analysis 36
3.3 Modification of working electrode (TiO2/SWCNT/SPE) 37
3.3.1 Functionalized SWCNT 37
3.3.2 Synthesis of TiO2/SWCNT composite 37
3.3.3 Preparation of TiO2/SWCNT /SPE 39
3.4 Characterization analysis of the TiO2/SWCNT composite 39
3.5 Electrochemical performance analysis 39
3.5.1 Optimizing the parameters of modified electrode 39
3.5.2 COD detection of single-compound simulated water sample 40
3.5.3 COD detection of multiple-compounds simulated water samples 41
3.5.4 Real water sample analysis 41
Chapter 4 Results and Discussion 42
4.1 Crystal phase analysis of composite (XRD) 43
4.2 Effect of scan rate on COD determination 44
4.3 COD analysis of TiO2/SWCNT/SPE in simulated water samples 46
4.3.1 Analysis of single-compound simulated water 46
4.3.2 Analysis of multi-compounds simulated water 57
4.4 Reproducibility of modified electrode 68
4.5 COD analysis of real water samples 69
Chapter 5 Conclusions and Suggestions 71
5.1 Conclusions 71
5.2 Suggestions 72
Reference 73
Appendix 86

List of Figures
Figure 1-1 Framework of this research 5

Figure 2-1 Effects of the electrochemical reaction for variables 11
Figure 2-2 Scheme of three-electrode system 12
Figure 2-3 The relationship between scan time and potential of different voltammetry 15
Figure 2-4 Typical cyclic voltammogram 16
Figure 2-5 Diffusion-controlled and adsorption-controlled of cyclic voltammetry 18
Figure 2-6 Linear sweep voltammogram, linear potential sweep starting Ei vs. time and resulting i-E curve 20
Figure 2-7 The diagram of single-walled carbon nanotubes and multi-walled carbon nanotubes (MWCNTs) 22
Figure 2-8 Crystal structures of TiO2 anatase, rutile, brookite and TiO2 (B) 26
Figure 2-9 The phase diagram of TiO2 27
Figure 2-10 The process of the sol-gel method for synthesizing crystalline TiO2 metal oxide 30

Figure 3-1 Purification processes of SWCNT 37

Figure 4-1 XRD pattern of SWCNT and TiO2/SWCNT composite. 43
Figure 4-2 The LSV response of TiO2/SWCNT/SPE in 50 mg L-1 of KHP in 0.1 M NaCl with different scan rate 46
Figure 4-3 The LSV response of KHP and the correlation between oxidation peak current and KHP of 20 to 100 mg L–1 48
Figure 4-4 The LSV response of glucose and the correlation between oxidation peak current and glucose of 20 to 100 mg L–1 50
Figure 4-5 The LSV response of SA and the correlation between oxidation peak current and SA of 20 to 100 mg L–1 52
Figure 4-6 The LSV response of MEA and the correlation between oxidation peak current and MEA of 20 to 100 mg L–1 54
Figure 4-7 The LSV response of DMF and the correlation between oxidation peak current and DMF of 20 to 100 mg L–1 56
Figure 4-8 The LSV response in the mixture of MEA and KHP with different ratio of ThOD 60
Figure 4-9 Peak current trends of MEA and KHP mixed water samples at different ratio. 61
Figure 4-10 The LSV response in the mixture of MEA and SA with different ratio of ThOD 62
Figure 4-11 Peak current trends of MEA and SA mixed water samples at different ratio. 63
Figure 4-12 The LSV response in the mixture of KHP and SA with different ratio of ThOD 65
Figure 4-13 Peak current trends of KHP and SA mixed water samples at different ratio. 66
Figure 4-14 Reproducibility of six modified electrode in 0.1 M NaCl containing KHP with 50 mg L–1 68
Figure 4-15 The correlation between peak current and COD of four outflow water 69
Figure 4-16 Blind sample test results using effluent from the sewage treatment plant in Pingzhen Industrial Park. 70

List of Tables
Table 4-1 The fitting equation and adjusted R2 in the mixture of MEA and KHP with five different ThOD ratios. 61
Table 4-2 The fitting equation and adjusted R2 in the mixture of MEA and SA with five different ThOD ratios. 64
Table 4-3 The fitting equation and adjusted R2 in the mixture of KHP and SA with five different ThOD ratios. 67

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指導教授

秦靜如(Qin Jingru)

審核日期

2024-1-25

推文