利用汞薄膜電極配合陽極剝除伏安法來偵測重金屬是一種有效且常見的方法，本實驗即是利用汞薄膜預氧化網版印刷碳電極（簡稱HgSPE*）來增加偵測重金屬鉛、鎘的靈敏度。HgSPE*的製作流程為：在0.1 M H2SO4中前處理網版印刷碳電極，先以預氧化電位2.2 V vs. Ag/AgCl預氧化時間10秒，接著再鍍上一層汞薄膜，即完成電極的製備。本實驗室先前的研究發現，光滑碳電極(glassy carbon electrode)預氧化後對於Pb2+的偵測訊號有顯著的提升，實驗結果顯示碳電極表面的碳氧官能基(>C=O)有助於增加沈積金屬的能力。然而在預氧化網版印刷碳電極上卻只得到微小的預濃縮剝除訊號，所以加上一層汞薄膜來增加偵測鉛、鎘的靈敏度。在偵測鉛最佳化的實驗條件下，HgSPE*得到兩段線性，範圍分別是1─15 ppb 與15─100 ppb，偵測極限(S/N = 3)為0.11 ppb。在偵測鎘最佳化的實驗條件下，HgSPE*線性範圍2─50 ppb，偵測極限(S/N = 3)為0.45 ppb。最後實際分析真實樣品，證明此方法可成功的檢測樣品中重金屬鉛、鎘含量。

Anodic stripping voltammetry using mercury film electrodes (MFEs) is one of the most effective approaches for heavy metals detection. In this work, we further improve the sensitivity using an activated Hg-coated screen-printed electrode (designated as HgSPE*). The HgSPE* was prepared by preanodizing in 0.1 M H2SO4 at 2.2 V vs. Ag/AgCl for 10 s prior to the Hg plating. Our recent work observed an enormous increase in the deposition/stripping signals for Pb2+ on a glassy carbon electrode after preanodization.1 The carbonyl functional (>C=O) group residing on the carbon surface has strong influence to trap relatively high amount of depositing metal on the inter-phase. However, due to poor availability of the carbonyl functional group on the SPE*, very feeble Pb deposition/stripping signals were observed. Nevertheless, Hg plating resulted in a considerable increase in Pb2+ and Cd2+ current signals. Under optimized conditions, the HgSPE* showed two linear range of 1─15 ppb and 15─100 ppb with a detection limit (S/N = 3) of 0.11 ppb for Pb2+. In the detection of Cd2+, a linear range of 2─50 ppb with a detection limit (S/N = 3) of 0.45 ppb was observed. Finally, a practical assay was demonstrated for the detection of Pb2+ and Cd2+ in real samples.

目錄
摘 要 i
Abstract ii
目錄 iii
圖目錄 vi
表目錄 ix
第一章 緒論 1
1-1 前 言 1
1-2 電化學分析法之簡介 5
1-2-1 循環伏安法（Cyclic Voltammetry）[6][7] 5
1-2-2 剝除伏安法 7
1-2-3 方波伏安法（Square-Wave Voltammetry）[7] 8
1-3 汞薄膜 10
第二章 實驗部分 11
2-1 儀器設備 11
2-2 藥品 12
2-3 溶液配製 13
2-4 樣品前處理 14
2-5 網版印刷電極之製作過程 18
2-6 實驗過程 20
2-7 電極的製備 21
第三章 鉛的偵測結果與討論 22
3-1 鉛簡介 22
3-2 利用方波伏安法偵測鉛離子 25
3-3 測鉛時硫酸的干擾 26
3-4 HgSPE*測鉛鍍汞時間探討 27
3-5 HgSPE*測鉛預濃縮電位探討 28
3-6 HgSPE*測鉛預濃縮時間探討 29
3-7 HgSPE*測鉛方波伏安法最佳參數探討 30
3-8 電極再現性的探討 32
3-9 線性範圍及偵測極限 33
3-10 干擾的探討 35
3-11 真實樣品之探討 36
3-11-1 豬血盲樣 36
3-11-2 標準水樣品 41
3-11-3 尿液樣品 43
3-11-4 土壤樣品 45
3-11-5 水樣品 47
第四章 鎘的偵測結果與討論 52
4-1 鎘簡介 52
4-2 利用方波伏安法偵測鎘離子 54
4-3 HgSPE*測鎘鍍汞時間探討 56
4-4 HgSPE*測鎘預濃縮電位探討 57
4-5 HgSPE*測鎘預濃縮時間探討 58
4-6 HgSPE*測鎘方波伏安法最佳參數探討 59
4-7 電極再現性的探討 61
4-8 線性範圍及偵測極限 62
4-9 真實樣品之探討 63
第五章 結論與未來展望 68
5-1 結論 68
5-2 未來展望 69
參考文獻 71

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