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研究生:詹博淵
研究生(外文):Bor Iuan Jan
論文名稱:超微量農藥電化學分析
論文名稱(外文):Trace Electroanalysis for the Pesticides Determination
指導教授:林孟山
指導教授(外文):Meng Shan Lin
學位類別:博士
校院名稱:淡江大學
系所名稱:化學學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:1999
畢業學年度:87
語文別:中文
論文頁數:265
中文關鍵詞:農藥電分析化學二氧化錳化學修飾電極超音波電極清除脈衝技術差分脈衝伏安法吸附剝除伏安法
外文關鍵詞:PesticidesElectroanalytical ChemistryManganese DioxideChemical Modified ElectrodesSonicationCleansing Pulse TrainDifferential Pulse VoltammetryAdsorptive Stripping Voltammetry
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論文提要內容:
利用新的修飾電極的方法來發展電化學的微量農藥量測技術,並且提高偵測的靈敏度、選擇性並且縮短量測時間。同時這些新的電化學量測技術亦適合發展並運用於環境中有毒物質的微量分析工作。這些修飾電極的方式,諸如清除脈衝電極處理技術和吸附濃縮過程等技術皆已被運用於環境及臨床分析上。MnO2修飾電極被運用來發展新型態的芳香胺類及二硝基酚類電化學量測方法,而雙電極碳糊及碳墨電極則分別被使用來作為被分析物的產生電極。高選擇性的優點乃是導因於在修飾電極與被分析物之間,施加低的還原電壓取代傳統高氧化電壓的缺點。利用超音波加速化學反應進行的方法,縮短水解反應時間用來發展新型態之巴拉松農藥電化學量測方法。
對於芳香胺類和其衍生物而言,MnO2為一強氧化劑,並且可將芳香胺類化合物在酸性條件下快速地氧化生成Quinone和類似Quinone的化合物。這樣的轉變對於電化學量測技術而言是一大優點,可以將量測的方法由氧化偵測模式轉變為還原偵測模式,而同時避開電聚合反應所造成的電極毒化現象。因此,低外加電壓與操作重現性的提昇乃是利用MnO2化學修飾電極發展芳香胺類及其衍生物電化學量測技術的優點。
利用超音波誘導化學反應並配合以流注分析雙電極系統(Flow Injection Analysis- Dual Electrode System)來發展新型態巴拉松農藥電化學量測機制。相對於巴拉松松農藥的自然水解反應,超音波誘發化學反應有效地增加巴拉松農藥分子在酸性溶液中的水解速率。超音波操作的過程中,當微泡崩潰的時候所釋放出來的高溫高壓的反應條件,促使化學反應迅速地進行。另一方面,電化學方法則是利用還原偵測模式來避開環境中所存在易氧化物質的干擾。
線上快速電化學處電極理技術-清除脈衝技術已被發展,並且被應用於玻璃碳電極的電極表面清除工作。清除脈衝處理技術有效地清除由Maleic Hydrazide氧化反應後於電極表面所形成之鈍性薄膜。相對於未經處理的玻璃碳電極表面,經由清除脈衝處理程序作用後之電極提供了電極穩定的量測狀態,包括固定的電極表面積與固定的電極活性,此現象可經由循環伏安法(Cyclic Voltammetry)與微差脈衝伏安法(Differential Pulse Voltammetry)分別得到證明。另外,清除脈衝處理技術提供了幾乎維持一定的電極活性的電極表面,並同時提高了系統對於農藥Maleic Hydrazide的偵測靈敏度。
有效率的預沈積過程,利用微差脈衝剝除伏安法或稱為陰極吸附剝除法,來發展二硫代胺基甲酸鹽 (Dithiocarbamate)農藥的量測方法。預沈積的過程可以將系統的偵測極限濃度大幅地降低至10-9M的範圍。另外,預沈積技術的最佳化條件,包括:預沈積電壓、電極沈積時間、溶液酸鹼值以及溶液之離子強度等等。以上這些化學修飾電極的技術,可以提昇電分析化學在環境分析方面之應用。
Abstract:
The schemes of modified electrodes for the electrochemical pesticides determination have been developed to improve the sensitivity, selectivity and speed. These schemes also are suitable for the developing to the environmental trace analysis. These chemical modified electrodes, as well as cleansing pulse training and adsorptive accumulation process, have been employed previously. The MnO2 modified electrodes are used to develop a new type of aromatic amines and dinitrophenol based pesticide electrochemical determination. A dual carbon paste and carbon ink electrodes use as the analyte generator electrodes. A sonication process induces the chemical reaction is used to develop a new electrochemical scheme for the parathion determination. The selective advantage is attributed to the lower applied potential for the reductive determination between the modified electrode and analyzes.
The MnO2 is a strong oxidative agent for the aromatic amine and its deviation and produce benzoquinone and quinone-like products, respectively. These oxidative chemical reactions also give the advantages for electrochemical scheme from oxidative mode to reductive mode and avoid the electropolymerization on the electrode surfaces. The lower applied potential and improvement reproducibility are the characteristics of MnO2 modified electrode for the aromatic amine and its deviation determination.
The sonication induces process and the flow injection system with the dual working electrodes for the parathion pesticide determination is developed. In contrast to the natural parathion hydrolytic reaction, the sonication induces scheme can improve the hydrolytic rate of parathion in acidic solution effectively. The sonication process will produce a high temperature and a high pressure for the chemical reaction when the bubble collapsed. The electrochemical measurement used the reductive mode to eliminate the easily oxidizable species interference.
A rapid in situ electrochemical scheme- cleaning pulse train for the regenerated of the surface of the glassy carbon electrode is developed. The cleaning pulse train can remove the passive layer from the oxidative process of maleic hydrazide effectively. In contrast to the untreated glassy carbon electrode, the treated electrode provides significant stability in measurements, which are demonstrated by a series of cyclic voltammetry and differential pulse voltammetry, respectively. Also, the cleaning pulse train provided a constant electrode surface and improved the sensitivity for the maleic hydrazide measurements.
An effective accumulation scheme, followed by a differential pulse voltammetric measurement, or cathodic stripping voltammetry, was used to measure the dithiocarbamate-based pesticides. The accumulation step will improve the sensitivity up to submicro-molar level of dithiocarbamate pesticides. The preconcentration scheme was achieved by the optimization of preconcentration potential, deposition time, solution pH, and ionic strength. These strategies enhance greatly the power of electroanalysis in the area of environmental analysis.
封面
目錄
中文摘要
英文摘要
圖 目 錄
表 目 錄
第一章 緒論
前言
1-1 農藥簡介及其影響
1-2 電分析化學的沿革
1-3 修飾電極
1-4 宿極再生技術在電化學上的應雨土
1-5 吸附剝除伏安法
1-6 超音波在學反應上的應用
1-7 本研究之目的
第二章 MnO2修飾碳糊電極在農藥代謝物對-胺基酚分析上的應用
2-1 簡介
2-2 實驗部份
2-2-1 藥品部份
2-2-2 儀器部份
2-2-3 修飾電極的製備
2-2-4 操作步驟
2-3 結果與討論
2-3-1 工作原理之探討
2-3-2 最佳化條件之探討
2-3-3 分析特性之探討
2-3-4 MnO2修飾電極的應用
2-3-5 結論
第三章 MnO2修飾碳墨電極在農藥DNOC分析上的應用
3-1 簡介
3-2 實驗部份
3-2-1 藥品部份
3-2-2 儀器部份
3-2-3 修飾電極的製備
3-2-4 操作步驟
3-3 結果與討論
3-3-1 原理探討
3-3-2 最佳化條件的探討
3-3-3 系統分析特性的探討
3-3-4 結論
第四章 利用超音波誘導反應發展巴拉松農藥的電化學量測機制
4-1 簡介
4-2 實驗部份
4-2-1
4-2-2 儀器部份
4-2-3 實驗系統設計
4-2-4 操作步驟
4-3 結果與討論
4-3-1 反應原理的探討
4-3-2 最佳化條件的探討
4-3-3 系統分析特性的探討
4-3-4 結論
第五章 利用交流電壓脈衝處理技術來發展具高靈敏度之農藥量測法
5-1 簡介
5-2 實驗部份
5-2-1 藥品部份
5-2-2 儀器部份
5-2-3 樣品的處理
5-2-4 實驗步驟
5-3 結果與討論
5-3-1 原理探討
5-3-2 交流電壓處理條件之探討
5-3-3 最佳化條件的探討
5-3-4 系統分析特性的探討
5-3-5 結論
第六章 利用陰極吸附剝除法來發展二硫代胺基甲酸鹽(Dithiocarbamate)系列農藥的量測技術
6-1 簡介
6-2 實驗部份
6-2-1 藥品部份
6-2-2 儀器部份
6-2-3 陰極吸附剝除伏安法的操作步驟
6-3 結果與討論
6-3-1 量測機制的探討
6-3-2 電化學的行為表現
6-3-3 最佳化條件的探討
6-3-4 分析特性的探討
6-3-5 結論
第七章 結論
參考資料
附號對照表
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