臺灣博碩士論文加值系統

第一部分
本研究係利用較高導電率與適合之官能基團，透過簡易的化學合成方法製備，藉以提升電化學感測器之電催化活性，以達成高靈敏度、線性範圍廣和低檢測極限之目標。4-氨基安替比林(4-Aminoantipyrine, 4-AAP)由於具有解熱、鎮痛和抗炎等特性而被廣泛地使用在生物醫學領域，惟長期使用勢必會對人體造成嚴重之副作用，然而，4-AAP的傳統檢測方法耗時較長、成本高，或需先執行分離程序等。另一方面，聚吡咯(Polypyrole, PPy)由於其低電荷轉移電阻、高功率與高能量密度、具高度選擇性，以及高敏感的電催化性能與循環穩定性高等因素，適合使用於太陽能電池、超級電容器、電池、生物燃料電池與電化學感測器等多種產品，但是PPy在電極表面上的分子相互作用較小，致使其在電極表面上的黏附性較差。為了提升4-AAP的檢測效率，我們利用聚多巴胺(Polydopamine, PDA)優異的黏合性，透過簡易化學方法連接PPy分子鏈，進一步加強其導電性與功能，再修飾於玻璃碳電極(GCE)，以提升測定4-AAP的效率。經由使用各種儀器，如X-射線繞射分析(XRD)和傅立葉紅外光(FTIR)光譜來確認聚合情形、掃描式電子顯微鏡（SEM）分析複合物的形態、電化學阻抗譜(EIS)和FTIR光譜確認PDA @ PPy複合材料的導電性和適用功能。在電化學研究中顯示，PDA @ PPy複合材料具有選擇性檢測4-AAP的能力、較高靈敏度(250.78 µA mM-1 cm-2)、線性範圍廣(0.0005 ~ 4.2 mM)以及低檢測極限(0.43 µM)，最後透過人體尿液真實樣品分析，PDA@ PPy/GCE修飾電極表現出良好的4-AAP氧化電催化活性，相關結果顯示其具高度實用性與價值。
第二部分
本研究主要透過使用程序簡易、成本較低之超音波輔助途徑，以製備出微觀結構的硫化鋅（ZnS）。並藉由使用各種技術系統地包括X射線衍射（XRD），X射線光電子能譜（XPS）和透射電子顯微鏡（TEM）分析所製備的ZnS的物理化學性質。在確認ZnS微觀結構均勻分佈且顆粒呈現片狀結構之後，將其運用於製造亞硝酸鹽傳感器的有效電催化劑。在相關電化學研究中，ZnS修飾電極顯示出優異的電催化活性，並且在20 nM至1.35 mM的濃度範圍內具有更好的分析性能，對於亞硝酸鹽的檢測具有8.5 nM的低檢測限，這與先前報導的文獻相當。此外，它對各種干擾物種具有高選擇性，並進一步應用於水樣中亞硝酸鹽的實時監測，並獲得了令人滿意的準確度。

Part I
This research uses simple chemical synthesis methods to produce higher conductivity and suitable functional groups to enhance the electrocatalytic activity of electrochemical sensors, achieve high sensitivity, wide linear range, and low detection limit. 4-Aminoantipyrine (4-AAP) is widely used in biomedical applications due to its antipyretic, analgesic and anti-inflammatory properties, but it can cause serious side effects if used for a long time. However, the traditional detection methods of 4-AAP are time-consuming extraction and high cost and separation procedures, etc. On the other hand, polypyrole (PPy) is suitable for solar cells, supercapacitors, batteries, biofuel cells and electrochemical sensors due to its low charge transfer resistance, high power and high energy density, selectivity, and sensitive electrocatalytic performance and high cycle stability, However, the molecular interaction of PPy on the surface of the electrode is small, resulting in poor adhesion on the surface of the electrode. In order to improve the efficiency of 4-AAP detection, Here we use the excellent adhesion of polydopamine (PDA) to connect the PPy molecular chain through simple chemical synthesis methods to further enhance its conductivity and function, and then modify it to the glassy carbon electrode (GCE) to improve the efficiency of 4-AAP. Then we have been used such as X-ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) to confirm the polymerization situation, scanning electron microscopy (SEM) to analyze the morphology of the composite. Electrochemical impedance spectroscopy (EIS) and FTIR spectra show the electrical conductivity and suitable function of the PDA@PPy composite. In electrochemical studies, PDA@PPy composites have the ability to selectively detect 4-AAP, higher sensitivity (250.78 µA mM-1 cm-2), high linear range (0.0005 ~ 4.2 mM), and low detection limits (0.43 μM). Finally, through the analysis of human urine samples, PDA@PPy/GCE modified electrode showed good 4-AAP oxidation electrocatalytic activity, and the related results revealed its practical value.
Part II
This study mainly produces micro-structured zinc sulfide (ZnS) through the use of a simple, low-cost ultrasonic-assisted approach. The physicochemical properties of the prepared ZnS were systematically analyzed by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) using various techniques. After confirming that the ZnS microstructure is uniformly distributed and the particles exhibit a sheet-like structure, they are applied to an effective electrocatalyst for the manufacture of a nitrite sensor. In related electrochemical studies, ZnS modified electrodes show excellent electrocatalytic activity and have better analytical performance in the concentration range of 20 nM to 1.35 mM, and a low detection limit of 8.5 nM for nitrite detection. Corresponding to previously reported literature. In addition, it has high selectivity for various interfering species and is further applied to real-time monitoring of nitrite in water samples with satisfactory accuracy.

摘 要 i
ABSTRACT iii
致謝 vi
目錄 vii
表目錄 x
圖目錄 xi
第一章 緒論 1
1.1電化學簡介 1
1.2電化學感測器簡介 2
1.3電極簡介 3
1.3.1化學修飾電極簡介 4
1.4藥品簡介 4
1.4.1 4-氨基安替比林(4-Aminoantipyrine, 4-AAP) 4
1.4.2吡咯(Pyrrole) 5
1.4.3多巴胺(Dopamine) 7
1.4.4亞鐵氰化鉀(Potassium ferrocyanide) 8
1.4.5硝酸鋅(Zinc nitrate) 8
1.4.6硫化鈉(Sodium sulfide) 9
第二章 實驗藥品、器材與分析方法 10
2.1實驗藥品 10
2.2實驗器材 11
2.3分析方法 12
2.3.1循環伏安法(Cyclic Voltammetry，CV) 12
2.3.2電化學阻抗譜(Electrochemical Impedance Spectroscope, EIS) 14
2.3.3安培法(Amperometry) 15
2.3.4掃描式電子顯微鏡(Scanning Electron Microscope，SEM) 16
2.3.5 能量散佈光譜儀 (Energy Dispersive Spectrometer，EDS) 18
2.3.6 X射線繞射分析儀(X-ray Diffractometer，XRD) 19
2.3.7 傅立葉轉換紅外線光譜儀(Fourier Transform Infrared Spectrometer, FT-IR) 21
2.3.8電化學分析儀(Electrochemical Instrument) 22
第三章 聚多巴胺與聚吡咯結合修飾玻璃碳電極應用於抗炎藥物4-氨基安替比林檢測之研究 24
3.1前言 24
3.2實驗步驟 25
3.2.1 PDA@PPy複合材料的合成 25
3.2.2 PDA@PPy/GCE修飾電極的製備 26
3.3 結果分析與討論 26
3.3.1 材料結構分析 26
3.3.2 材料組成分析 27
3.3.3 修飾電極的導電率分析 28
3.3.4 PDA@PPy/GCE修飾電極的電化學性能 30
3.3.5 PDA@PPy/GCE修飾電極的安培法檢測 31
3.3.6 干擾物研究 33
3.3.7 再現性、重複性和穩定性 33
3.3.8 真實樣品分析 34
3.4 結論 35
第四章 簡易合成硫化鋅修飾玻璃碳電極應用於水中亞硝酸離子檢測之研究 36
4.1前言 36
4.2實驗步驟 37
4.2.1 硫化鋅之合成 37
4.2.2 ZnS修飾電極的製備 38
4.3結果分析與討論 39
4.3.1 材料結構分析 39
4.3.2 材料組成分析 40
4.3.3 ZnS/GCE修飾電極之導電率分析 41
4.3.4 Zns/GCE修飾電極的電化學性能 43
4.3.5 ZnS/GCE修飾電極之安培法檢測 45
4.3.6 再現性、重複性和穩定性 48
4.3.7 真實樣品分析 49
4.4 結論 50
參考文獻 51

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