Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/16623
標題: 可拋棄式超微電極電化學分析系統的研發與應用
The Development and Application of Disposable Ultramicroectrodes in Electroanalysis
作者: 張仁麟
Chang, Jen-Lin
關鍵字: Screen printed
網版印刷
Ultramicroelectrode
Disposable
Nitrite
Iodide
超微電極
電化學
可拋棄
亞硝酸根
碘離子
出版社: 化學系所
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摘要: 本篇研究開發了一個完整的拋棄式網版印刷超微電極分析系統,涵括了拋棄式網版印刷(帶狀)超微電極(screen-printed edge band ultramicroelectrode,簡稱SPUME)及超微電極電化學偵測器(screen printed edge band ultramicroelectrodes electrochemical detector,簡稱SPUME-ECD)之研發與應用。並在研究過程中,發展出一個全新的多層網版印刷製程技術,利用此製程製作出成本低、可拋棄且多功能性之網版印刷(帶狀)超微電極試片,此試片可利用其獨特之電極外觀搭配簡易機械力切割,控制其電極長度而得到不同面積之電極。多層印刷堆疊出的電極形式,使其電極組合具多變性,例如同樣的三電極系統,其工作電極可以是碳(SPUME-1),也可以是銀(SPUME-2)。且隨研究領域之不同,可隨之更改電極面積與電極組合。除此之外,此電極可在微量或不添加輔助電解質的環境中進行相關電化學分析,因此在實際應用分析上,本研究利用SPUME-1直接偵測10 uM H2SO4水溶液、礦泉水、地下水與與市售香腸中的亞硝酸鹽含量;在H2SO4水溶液中得到良好的偵測線性範圍(0.005-3 mM,r2=0.9993)與偵測極限(0.38 uM,S/N=3)。於真實水樣之回收率亦佳,分別為99.0%(地下水)與99.4%(礦泉水)。香腸中的亞硝酸鹽含量測定結果與傳統光學法比對,其誤差小於5%。論文中,亦使用SPUME-2在直接偵測純水中鹵素離子(Cl-, Br-, I-)並發現各離子之還原電位有所差異,藉此特點,將在後續的研究中將朝同步偵測之方向進行相關研究。至於SPUME-ECD,則使用製作過程簡易、成本低的凸模塑型的技術製作研發,並搭配SPUME結合流動注入分析系統(flow-injection analysis)進行應用分析並獲得不錯的實驗結果。未來希望在更多領域中應用此分析系統,來提升其實用性與產業價值。
The development and application of disposable ultramicroectrodes in electroanalysis is fouced on this study. The system contains a disposable screen printed edge band ultramicroelectrodes (designated as SPUMEs) together with an SPUME electrochemical detector (designated as SPUME-ECD) for flow injection system analysis. First, the SPUMEs were fabricted with a built-in three-electrode pattern of alternating printed-layer of carbon, silver, and insulator on a non-conducting polypropylene substrate. Central idea is that the edge of the carbon and/or metal-sandwiched films between the insulator layers can serve as a band type ultramicroelectrode. Simply by slicing the edge of working window, the SPUME dimension can be easily varied (e.g., in the range of 0.18-1.35 mm length with a width of 20 um this study). Cyclic voltammograms of ferricyanide in aqueous media displayed low-noise, low-background, sigmoidal responses with virtually no current hysteresis similar to that of a hemicylindrical electrode. The proposed SPUMEs exhibit very low electrical noise and can be reproduced multiple times by repetitively cutting the strip. The application for sensitive determination of nitrite by using the SPUME was demonstrated in this study. The measurement with the SPUME can be performed in solutions of low ionic strength, e.g., natural waters, because the ohmic loses are negligible. The limiting oxidation current of nitrite showed a wide linear range up to 3 mM at the SPUME. A relative standard deviation of 2.46% (n = 5) for analyzing 5 uM nitrite indicated a detection limit (S/N = 3) of 0.38 uM. Real sample analysis of mineral and ground water samples as well as bratwurst food product showed satisfactory results. Finally, the SPUME-ECD (wall-jet cell) was fabricated with two pieces of polydimethoxy silane (PDMS) plates with the ‘T' type void (containing 1.15 mm width and 1.15 mm height) including compatibility of fixing the SPUME-3EC. The performance trait of the cell in flow injection mode was evaluated using the Fe(CN)63-/4- model compound. Optimization of distance between capillary and SPUME-3EC as used as flow rate were performed in order to get higher sensitivity through minimization of diffusion layer thickness and type of flow. With the arrangements voltammetry can be performed under flow conditions where the mass transport coefficient approaches 0.48 cm/s. Since all of them are cheap and easy for mass production, the disposable nature further offers to application in diverse field of electroanalytical chemistry.
URI: http://hdl.handle.net/11455/16623
其他識別: U0005-2404200714395500
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