標準COD檢測方法操作繁瑣、耗時,且需使用有害化學試劑,對環境與人員安全造成潛在風險。相較之下,伏安法具有反應快速、靈敏度高與可攜帶式等優勢,成為環保且高效的替代方案。本研究旨在利用伏安法,結合二氧化鈦/單壁奈米碳管/玻璃碳電極 (Titanium dioxide/Single-walled carbon nanotubes/Glassy carbon electrode, TiO2/SWCNT/GCE) 與攜帶式電化學分析儀,發展即時現地測定自然水體中的化學需氧量 (Chemical oxygen demand, COD)的方法。本研究所製備TiO2/SWCNT/GCE具有良好的電化學特性、穩定性與再現性。在模擬水樣中,以鄰苯二甲酸氫鉀與水楊酸進行分析,結果顯示電極對不同COD濃度具良好線性關係。在自然水體中 (中大湖、百花川與老街溪) ,伏安法測得的電流峰值與標準方法所測得之COD結果具有高度一致性。最終運用攜帶式電化學儀進行現地測量驗證,所得到的COD值與標準方法的誤差在8%以內,證實該方法具備簡便快速的操作性與良好的應用性。;Traditional analyses of chemical oxygen demand (COD), such as dichromate reflux, are time-consuming and require hazardous reagents. Voltammetric analysis has several advantages, such as high sensitivity, fast response, and environmental friendliness. This study developed an on-site and rapid COD determination technique, which was integrated by titanium dioxide/single-walled carbon nanotube/glassy carbon electrodes (TiO₂/SWCNT/GCE) and a portable electrochemical analyzer. Electrochemical characterization demonstrated the electrodes had good stability and reproducibility. Measurements of potassium hydrogen phthalate and salicylic acid showed that there were strong linear correlations between the peak oxidation current and the COD concentration. Application of the developed technique to real water samples from Zhongda Lake, Baihua Creek, and Laojie Creek revealed excellent agreement between voltammetric and conventional COD measurements. The blind tests of the natural waters successfully determined COD on-site and the errors were within 8%. This confirmed the reliability and practicality of the technique for on-site COD determination in different aquatic environments.