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  • 學位論文

摻硼鑽石電極對鉈(I)的偵測

Novel boron-doped diamond based electrode with determination of thallium (I)

指導教授 : 林孟山

摘要


本研究的主要目的分為二部分。第一部分是利用微波電漿氣相化學沉積法之技術製作摻硼鑽石薄膜電極,探討製程參數對電化學行為的影響;第二部分是將摻硼鑽石電極結合微差脈衝剝除法偵測環境毒物-鉈(I)。 摻硼鑽石薄膜電極製備在微波功率1500W、氣體總壓55torr、氫氣流速300sccm、甲烷流速12sccm、B(OCH3)3流速0.8sccm下,並施加-135V直流偏壓成核15分鐘、成長300分鐘即完成電極製備,此摻硼鑽石薄膜電極對1mM K3Fe(CN)6在循環伏安法的可逆性標準偏差值為4.73% (n=10),鑽石純度平均為94% (n=10)。 第二部分將自製的摻硼鑽石電極作為工作電極,並使用微差脈衝剝除伏安法(Differential Pulse Stripping Voltammetry)進行偵測環境毒物-鉈(I),在沉積電位-1200mV下,沉積時間150秒,緩衝溶液條件為0.05M、pH4磷酸緩衝溶液,脈衝振幅50mV,脈衝時間25ms,取樣時間17ms,其線性範圍為50nM-10μΜ (R=0.998),靈敏度4.65μA/μM,偵測極限(S/N=3)為6.72nM,在連續偵測1μM鉈(I)20次的相對標準偏差為3.95%,而利用此系統量測池塘水 及淡水河水的回收率(1μΜ Tl+)分別為97.3%及99.7%。

並列摘要


The boron-doped diamond (BDD) electrode has attractive intensive attention recently. There are two parts in this study. The first one, we used the microwave plasma enhanced chemical vapor deposition (MPECVD) prepared the boron-doped diamond electrode, and study the various factors influence of the diamond quality and electrochemical behavior, including C/H ratio、B/C ratio and growth time. Subsequently the boron-doped electrode was used to measure thallium. Thallium was measure by difference pulse stripping voltammetry(DPSV) at the optimum condition of buffer solution:0.05、pH4 phosphate buffer. The measure peak current at 810mV (vs. /AgCl) for deposition potential at -1200mV、deposition time 150 sec. The differential pulse optimal condition, including the pulse amplitude 50mV、pulse width 25ms、sampling time 17ms.According the optimum conditions, the linear range of thallium is between 0.05μM to 10μM(R=0.998), and sensitivity is 4.65μA/μM. The estimated detection limit(S/N=3) is 6.72nM.The relative standard deviation of twenty repetitive detection is 3.95%.Typical recovery rates are 97.3 and 99.7 from the spikes of 1μM Thallium samples from pond water and Tamsui River,respectively.

參考文獻


Robert F. Davis
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