博碩士論文 105326014 詳細資訊




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姓名 張佳琦(Chia-Chi Wahang)  查詢紙本館藏   畢業系所 環境工程研究所
論文名稱 運用氧化石墨烯/單壁奈米碳管/碲化鉍修飾玻璃碳電極進行水中鎘之方波陽極析出伏安法分析
(Determination of Cd(II) by square wave anodic stripping voltammetry using graphene oxide/single-walled carbon nanotubes/Bi2Te3 modified glassy carbon electrode)
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摘要(中) 重金屬鎘具有高毒性,若人體攝入過多的鎘,可能會導致骨骼、腎功能、呼吸系統的危害。目前分析重金屬的方式耗時長、樣品需要前處理、且無法即時反應水質狀況,然而電化學伏安法由於操作方便、便宜、簡單、快速、能即時分析等優點而受到重視。本研究開發氧化石墨烯/單壁奈米碳管/碲化鉍修飾玻璃碳電極進行方波陽極析出伏安法分析水中的鎘。首先選定適宜的伏安法掃描方式,再進行材料配比的比較及確認,經過參數最佳化後(電解液pH 5、沉積電位-1.1 V),探討該修飾電極在120 s和360 s偵測鎘(II)的性能,同時也對該電極的穩定性進行評估。結果顯示,氧化石墨烯/單壁奈米碳管/碲化鉍修飾電極使用方波陽極析出伏安法偵測鎘(II)呈現良好的線性關係,在沉積電位120 s的情況下,LOD為0.99 µg/L;在沉積電位360 s的情況下,LOD為0.14 µg/L,遠低於放流水標準(20–30 µg/L)和飲用水標準(5 µg/L),而重複性及再現性分別為0.5%和3.7%。另外,經過測試該電極不會受到水中Pb(II)、Zn(II)、Cr(III)、Cr(VI)、As(III)、As(V)的干擾,不過由於Cu(II)的還原電位較低,因此鎘的剝離電流易受到高濃度銅的影響,最後本研究在環境水體中進行鎘(II)的分析,證實了在自來水及地下水中有良好的回收率。
摘要(英) Cadmium is highly toxic and ingestion by humans may harm to humans, such as bone, kidney function, and respiratory system. At present, the method of analyzing heavy metals require pretreatment and long time so it cannot give the results of water quality promptly. However, electrochemical voltammetry is valued due to its advantages of convenient operation, low cost, simplicity and rapid analysis. In this study, determination of Cd(II) by square wave anodic stripping voltammetry using graphene oxide/single-walled carbon nanotubes/Bi2Te3 modified glassy carbon electrode was developed. First, the appropriate voltammetric scanning method is selected, and then the SWCNT/GO ratio was confirmed. The performance of the modified electrode in detecting Cd(II) at 120 s and 360 s was investigated after parameter optimization (electrolyte pH 5, deposition potential -1.1 V). The stability of the electrode was also evaluated. The results showed that the GO/SWCNT/Bi2Te3/GCE can successfully determine Cd(II) by SWASV. At a deposition potential of 120 s, the LOD is 0.99 μg/L; at a deposition potential of 360 s, the LOD is 0.14 μg/L, which is lower than the effluent standard (20–30 μg/L) and the drinking water standard (5 μg/L). Repeatability and reproducibility were 2.6% and 3.7%, respectively. Moreover, the electrode developed in this work is also free from the interference of Pb(II), Zn(II), Cr(III), Cr(VI), As(III), As(V) in water, but the stripping current of Cd(II) is easily affected by high concentration copper due to the low reduction potential of Cu(II). Finally, the analysis of Cd(II) in environmental waters confirmed the good recovery in tap water and groundwater.
關鍵字(中) ★ 氧化石墨烯
★ 單壁奈米碳管
★ 碲化鉍
★ 方波陽極析出伏安法
★ 鎘
關鍵字(英) ★ graphene oxide
★ single walled carbon nanotubes
★ Bi2Te3
★ square wave anodic stripping voltammetry
★ cadmium
論文目次 Contents
摘要 i
Abstract ii
誌謝 iv
Contents vi
List of Figures x
List of Tables xiv
Chapter 1 Introduction 1
1.1. Background 1
1.2. Objectives 3
Chapter 2 Literature Reviews 6
2.1. Patterns and detection methods of cadmium 6
2.2. Electrochemical technology 9
2.2.1. Electrochemical reaction and principle of Voltammetry 10
2.2.2. Potential scanning method of Voltammetry 14
2.2.3. Stripping analysis (anodic stripping voltammetry) 27
2.2.4. Electrochemical impedance spectroscopy (EIS) 30
2.2.5. The application and modification of voltammetry of cadmium 34
2.3. Electrode modified materials for cadmium analysis 38
2.3.1. Graphene oxide (GO) 39
2.3.2. Carbon nanotubes (CNTs) 43
2.3.3. Bismuth telluride (Bi2Te3) 48
Chapter 3 Materials and Methods 51
3.1. Instrumentation and Chemicals 51
3.1.1. Instrumentation 51
3.1.2. Materials and Chemicals 52
3.2. Modification of working electrode (GCE) 54
3.2.1. Pretreatment of SWCNT 54
3.2.2. Pretreatment of exfoliation Bi2Te3 suspension 55
3.2.3. Preparation of GO, GO/Bi2Te3, GO/SWCNT, GO/SWCNT/Bi2Te3 composite suspension 56
3.2.4. Preparation of the modified GCE 58
3.3. Characterization of modified electrodes 59
3.4. Voltammetric analysis 60
3.4.1. The choice of voltammetry 60
3.4.2. Optimization of determination modification 60
3.4.3. Detection of cadmium (II) 61
3.4.4. Interference and real sample analysis 62
Chapter 4 Results and Discussions 64
4.1. Characterization of modified electrode 64
4.1.1. Electrochemical characteristics of modified electrodes 64
4.1.2. Electrochemical impedance spectroscopy (EIS) 71
4.1.3. SEM & TEM & EDS analysis 73
4.2. Selection of modified electrode and voltammetry 77
4.2.1. Comparison of different voltammetry 77
4.2.2. Select the best modified electrode 79
4.2.3. Selection of the loading quantity of GO/SWCNT/Bi2Te3 82
4.3. Scaning parameter optimization 83
4.3.1. Selection of electrolyte pH 84
4.3.2. Selection of optimal deposition potential 85
4.3.3. Selection of optimal deposition time 86
4.4. Analytical performance of Cd(II) 88
4.5. Interference measurement of other metals & Analysis of Environmental waters 94
4.5.1. The interference of Pb(II), Cu(II), Zn(II), Cr(III), Cr(VI)6 As(III) and As(V) 94
4.5.2. Analysis of Environmental waters 98
4.6. Stability of modified electrode 102
Chapter 5 Conclusions and Suggestions 104
5.1. Conclusions 104
5.2. Suggestions 105
References 106
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指導教授 秦靜如(Ching-Ju Chin) 審核日期 2019-1-17
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