本研究利用化學還原法及電鍍沉積法，以SWCNT為載體，透過前驅物四氯化金酸(HAuCl4)，製備GNP/SWCNT複合材料，進行材料特性分析與As(III)之伏安法分析。特性分析的部分，觀察材料的表面特性、表面積與孔洞大小、晶相變化、元素組成、官能基與製備條件在伏安法分析表現之影響，選出最佳金奈米粒子與奈米碳管合成比例。根據UHR-SEM與TEM觀察得知，金奈米粒子會隨著濃度高低附著或包覆於奈米碳管上，特別是電鍍形成的金奈米顆粒約2－5 nm，較容易均勻控制大小與分散於碳管表面。伏安法分析的同時也發現2－5 nm顆粒大小的金奈米顆粒測定As(III)造成的氧化峰電流最為尖銳，碳管能放大氧化峰電流值約3.8倍。後續以最佳比例進行As(III)之伏安法分析，選定最佳掃描條件，如掃速、pH。以及觀察修飾電極在掃描電位範圍上的限制，探討氧化峰電流與濃度之間的關係。結果顯示電鍍複合材料修飾電極以LSV測定50－5000 μg/L As(III)，得到良好濃度與電流的線性關係。最後推測干擾物Cu(II)對As(III)伏安法分析的影響與記憶效應。發現以LSV偵測As(III)及Cu(II)氧化峰電流的優點在於無明顯的記憶效應。具有開發線上即時監測放流水中As(III)之潛力與應用價值。;Gold nanoparticle/SWCNT (GNP/SWCNT) composites were synthesized via chemical reduction and electro-plating using HAuCl4 as precursor. The surface characteristics of GNP/SWCNT, such as surface area as well as pore size, crystallinity, elemental composition, and functional groups were examined. From SEM and TEM analysis, it was shown that GNP synthesized via electroplating were about 2－5 nm and evenly distributed on the surface of SWCNT. Besides, it was found that when GNP were about 2－5 nm, the oxidation peak of As(III) was the sharpest and the peak current was about 3.8 times larger than the GCE electrode coated with GNP only. The linear scanning voltammetry of As(III) at different concentrations showed that the peak current has good relationship to the concentration of As(III) in the range of 50－5000 μg/L. At last, the interference of copper and the memory effects were also investigated. It was found that when analyzing As(III) via LSV, the was not obvious interference of copper and the memory effects.