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研究生： 趙芷君
Chao, Chih-Chun
論文名稱： 金奈米顆粒誘導氮摻雜石墨烯量子點之內濾效應用於水體中得恩地檢測
Gold Nanoparticles-induced Inner Filter Effect of Nitrogen-doped Graphene Quantum Dots for Thiram Detection in Aqueous Solutions
指導教授： 董瑞安
Doong, Ruey-An
口試委員: 劉耕谷
Liu, Keng-Ku
林芳新
Lin, Fang-Hsin
學位類別： 碩士
Master
系所名稱： 原子科學院 - 分析與環境科學研究所
Institute of Analytical and Environmental Sciences
論文出版年： 2022
畢業學年度： 110
語文別： 中文
論文頁數： 105
中文關鍵詞： 得恩地 、石墨烯量子點 、金奈米顆粒 、內濾效應 、螢光
外文關鍵詞： Thiram, Graphene quantum dots (GQDs), Gold nanoparticles (AuNPs), Inner filter effect (IFE), Fluorescence
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    • 農藥在全球農業中扮演著舉足輕重的地位，然而隨著農藥的使用量增加，也逐漸衍伸出許多環境問題，其中得恩地為廣效性農藥，也經常使用在工業用途及民生用品中，其對水生生物危害極大，故偵測環境中的得恩地汙染顯得更加迫切。近年來檢測農藥的方式多為液相層析儀或拉曼光譜儀，這些檢測方法依賴昂貴、檢測耗時的實驗室分析儀器，不符合民生需求。故本研究期望開發出兼具簡單、經濟、環保、快速檢測及高靈敏度與選擇性之方法，以檢測水中之得恩地汙染。本研究基於檸檬酸鹽穩定的金奈米顆粒(AuNPs)誘導氮摻雜石墨烯量子點(N-GQDs)螢光的內濾效應(Inner filter effect, IFE)開發一種簡易的得恩地感測系統。AuNPs可以有效地淬滅N-GQDs的螢光，而當得恩地存在時，由於得恩地與AuNPs的化學鍵生成，從而導致AuNPs聚集並使N-GQDs因內濾效應減少的螢光相應恢復。通過測量N-GQDs的螢光，評估得恩地的濃度。所開發之系統對得恩地的檢測範圍為300-1000 nM，最低偵測極限(LOD)為38.5 nM。此外，該方法對得恩地具有良好的選擇性，以及成功應用於湖水與河水中的得恩地測定，為檢測水樣中的得恩地汙染提供一個具有發展潛力的分析方法。

    Pesticides play an important role in global agriculture. However, many environmental problems have emerged gradually with the increase in the use of pesticides. Thiram is a wide-ranging pesticide and is often used in industrial and domestic sectors. It is extremely harmful to aquatic organisms. Therefore, it is more urgent to detect thiram residues in the environment. In recent years, detection of pesticide residues mainly performed with high-performance liquid chromatography or surface enhanced Raman spectroscopy. These methods depend on expensive and time-consuming laboratory analytical instruments, which is not practical for domestic cases. Herein, we hope to develop a simple, economical, environmentally friendly, rapid detection, high sensitivity and selective method to detect the thiram pollution in the water. In this study, we demonstrated a feasible thiram indicating system based on the inner filter effect (IFE) of citrate-stabilized Gold nanoparticles (AuNPs) on the fluorescence of nitrogen-doped graphene quantum dots (N-GQDs). AuNPs can quench the fluorescence of N-GQDs significantly. The presence of thiram in the system resulted in the remarkable aggregation due to the formation of covalent bond with AuNPs. Consequently, the inner filter effect induced by AuNP is relieved, accompanying with the recovery of emission of N-GQDs. The concentration of thiram is evaluated by measuring the fluorescence of N-GQDs. The developed system shows the concentration range of 300-1000 nM for Thiram with a lowest detection limit (LOD) of 38.5 nM. In addition, this method has good selectivity for thiram, and it has been successfully applied to detect thiram in lake and river water. In conclusion, it provides an analytical method with development potential for detecting thiram pollution in aqueous solutions.

    中文摘要 I Abstract II 致謝 III 目錄 V 圖目錄 VIII 表目錄 X 第一章 緒論 1 1-1 前言 1 1-2 研究動機 2 1-3 研究目的 3 第二章 文獻回顧 5 2-1 得恩地之汙染與介紹 5 2-1-1 得恩地之感測 8 2-2 內濾效應於感測器之應用 11 2-2-1 金奈米顆粒於內濾效應之應用 15 2-3 碳材量子點之介紹 19 2-3-1 一般石墨烯量子點與元素摻雜之石墨烯量子點之介紹 21 2-3-2 石墨烯量子點於螢光感測器之應用 28 2-3-3 元素摻雜石墨烯量子點於螢光感測器之應用 31 第三章 實驗方法與步驟 33 3-1 實驗藥品與清單 33 3-2 實驗架構與流程 34 3-3 氮摻雜石墨烯量子點(N-GQDs)之合成方法 36 3-4 金奈米顆粒(AuNPs)之合成方法 37 3-5 氮摻雜石墨烯量子點之光學性質檢測 38 3-5-1 吸收光譜量測 38 3-5-2 激發與放射光譜量測 38 3-5-3 螢光量子產率(Fluorescence quantum yield) 38 3-6 系統之參數優化 40 3-6-1 反應系統酸鹼度(pH)之優化 40 3-6-2 金奈米顆粒反應濃度之優化 40 3-6-3 反應時間之優化 41 3-7 內濾效應之檢測步驟 41 3-7-1 氮摻雜石墨烯量子點螢光強度檢測 41 3-7-2 金奈米顆粒誘導氮摻雜石墨烯量子點之內濾效應 42 3-8 得恩地之檢測步驟 43 3-8-1 靈敏度檢測 43 3-8-2 選擇性 44 3-8-3 真實樣品 44 3-9 材料特性鑑定 46 3-9-1 穿透式電子顯微鏡 (Transmission Electron Microscopy, TEM) 46 3-9-2 高解像能電子顯微鏡 (High Resolution Transmission Electron Microscope, HRTEM) 46 3-9-3 原子力顯微鏡 (Atomic Force Microscope, AFM) 47 3-9-4 X光繞射儀 (X-ray Diffractometer, XRD) 47 3-9-5 拉曼散射光譜儀 (Raman Spectroscopy) 48 3-9-6 傅立葉轉換紅外光譜儀 (Fourier Transform Infrared Spectroscopy, FTIR) 49 3-9-7 X光光電子暨歐傑電子能譜儀 (X-ray Photoelectron and Auger Electron Epectroscopy, XPS/AES) 49 3-9-8 紫外光-可見光分光光譜儀 (Ultraviolet/Visible Spectrophotometer, UV-Vis) 50 3-9-9 螢光分光光譜儀 (Fluorescence Spectrophotometer, FL) 51 3-9-10 動態光散射儀 (Dynamic Light Scattering, DLS) 51 3-9-11 感應耦合電漿質譜分析儀 (Inductively Coupled Plasma-Mass Spectromete, ICP-MS) 52 第四章 結果與討論 53 4-1 氮摻雜石墨烯量子點之鑑定 53 4-1-1 TEM、AFM及XRD之鑑定 53 4-1-2 Raman、FTIR及XPS之鑑定分析 56 4-1-3 UV與FL光學性質鑑定 60 4-2 金奈米顆粒之鑑定 61 4-2-1 TEM、DLS及XRD之鑑定 61 4-2-2 FTIR及XPS之鑑定 63 4-2-3 UV圖譜之鑑定 65 4-3 氮摻雜石墨烯量子點與金奈米顆粒之鑑定 65 4-3-1 TEM、DLS及XRD 65 4-3-2 FTIR及XPS鑑定分析 67 4-4 反應機制之探討 70 4-4-1 UV與FL光學鑑定 70 4-4-2 FTIR與XPS之鑑定 71 4-4-3 TEM、DLS及Zeta potential鑑定 75 4-5 抑制內濾效應之條件優化 77 4-5-1 pH值與檢測系統之影響 77 4-5-2 金奈米顆粒反應濃度與檢測系統之影響 80 4-5-3 反應時間之優化 81 4-6 得恩地之檢測 83 4-6-1 靈敏度及偵測極限 84 4-6-2 選擇性 86 4-6-3 真實水樣之應用 88 第五章 結論與建議 93 5-1 結論 93 5-2 成本計算 94 參考文獻 98

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