研究分為兩部分，第一部分研究利用化學蒸氣生成技術結合感應耦合電漿質譜儀分析茶葉中之鈷及鎳的含量。為得到最佳之分析物訊號靈敏度，實驗中將依序對增益試劑8-hydroxyquinoline濃度、HNO3濃度、NaBH4濃度、反應試劑流速、混合線圈體積做最適化探討。CVG系統中所使用之氣液分離裝置幫助分析物從基質分離，減輕了鈣的光譜干擾。分析物訊號波峰面積及波峰高度皆在5% (n=5)。實驗中會比較水溶液校正法(External calibration)及標準添加法(Standard addition)之斜率，證明基質的存在影響了氫化物的生成效率，故選擇標準添加法進行分析物之定量，本方法鈷及鎳方法偵測極限分別為0.4、3.9 ng g-1。最後以最適化條件分析兩種標準參考樣品及兩種市售茶葉來證實方法之準確性及可行性。
第二部分研究利用泥漿進樣結合流動注入化學蒸氣生成技術結合感應耦合電漿質譜儀分析指甲油中之砷、鎘、銻、汞及鉛之含量。經最適化後，實驗中會配製成以0.5% /m/v 指甲油、1% m/v thiourea、0.75 mg L-1 Co 及 1.2% v/v HCl所組成之泥漿樣品溶液。而以指甲油基質中添加適量元素標準溶液，分析物之波鋒面積及高度之相對標準偏差(RSD)均在4%之內(n=4)。不同物種之元素會具不同的蒸氣生成效率，可能導致定量上的偏差，故比較As(III)、As(V)及Sb(III)、Sb(V)在經過泥漿製備法後之化學蒸氣生成效率，結果證實泥漿製法之預還原效果。實驗中比較標準添加法(Standard addition method)及水溶液校正法(External calibration method)之斜率，證明基質會影響蒸氣生成效率，故最後選擇以標準添加法作為定量方式，且搭配同位素稀釋法來驗證方法。本方法所得之砷、鎘、銻、汞及鉛方法偵測極限分別為0.06、0.12、0.14、0.20及12 ng g-1。最後以本方法分析三種不同品牌之市售指甲油且比較ETV-ICP-MS分析之結果來證實方法準確性及可行性。

First research analyze Co and Ni in leaves by FI-CVG-ICP-MS. To get better signal in experiments, subsequently testing concentration of 8-hydroxyquinoline, HNO3 and NaBH4. In addition, testing reagent flow rate and volume of mixing coil, too. Gas-liquid separator used in the CVG system separate analytes from the matrix, and thereby reducing the spectral interference of calcium. The existence of the matrix affect the hydride generation efficiency, so we use standard addition as our quantitative method. Under the optimum operating conditions, the detection limit obtained from the curve were in the range of 0.4-3.9 ng g-1 for Co and Ni in tea leaves sample. Besides, the analytical results of SRM 1573a and SRM 1547 determined by standard addition were in a good agreement with certified value. Finally, the method has been applied for determination of Co and Ni in commercially available tea leaves.
Second research using slurry sampling as pretreatment, and to determine As, Cd, Sb, Hg and Pb in nail polish by FIA-CVG-ICP-MS. The nail polish slurry containing 0.5% m/v nail polish, 1% m/v thiourea, 0.75 mg L-1 Co and 1.2% v/v HCl. Then, we compare the slope of external calibration and standard addition to ensure that if the matrix will affect the efficiency of vapor generation. We choose standard addition and isotope dilution as our quantitative method. The method has been applied for determination of As, Cd, Sb, Hg and Pb in commercially available nail polish. Under the optimum operating conditions, the detection limit obtained from the curve were in the range of 0.06-12 ng g-1 for As, Cd, Sb, Hg and Pb in nail polish sample.

審定書 i
謝誌 ii
中文摘要 iii
Abstract iv
目錄 v
圖目錄 viii
表目錄 x
第一章 流動注入化學蒸氣生成技術結合感應耦合電漿質譜儀於茶葉中鈷、鎳分析之應用 1
壹、前言 1
一、研究背景 1
二、金屬的毒性及對人體的危害 4
三、流動注入分析法(Flow Injection Analysis，FIA)原理 4
四、化學蒸氣生成法(Chemical vapor generation)原理 5
貳、實驗部分 6
一、儀器裝置 6
二、試劑藥品及溶液配置 7
參、實驗過程 10
一、化學蒸氣生成系統各參數之探討 10
二、ICP-MS系統操作條件之探討 11
三、樣品稀釋倍數探討 12
四、光譜干擾探討 12
五、最適化參數之調整 12
六、分析訊號之再現性 13
七、校正曲線及偵測極限估計 13
八、樣品的前處理與分析 13
肆、結果與討論 16
一、化學蒸氣生成系統參數之探討 16
二、ICP-MS系統操作條件之探討 25
三、樣品稀釋倍數探討 25
四、光譜干擾探討 25
五、最適化參數之調整 29
六、分析訊號之再現性 29
七、校正曲線及偵測極限估計 29
八、樣品的前處理與分析 33
伍、結論 39
陸、參考文獻 40
第二章 泥漿進樣流動注入化學蒸氣生成技術結合同位素稀釋法感應耦合電漿質譜儀於指甲油中砷、鎘、銻、汞及鉛之應用 45
壹、前言 45
一、研究背景 45
二、金屬的毒性及對人體的危害 47
三、同位素稀釋法 (Isotope dilution，ID) 48
貳、實驗部分 49
一、儀器裝置 49
二、試劑藥品及溶液配置 50
參、實驗過程 53
一、化學蒸氣生成系統各參數探討 53
二、ICP-MS系統操作條件之探討 54
三、樣品稀釋倍數探討 55
四、分析訊號之再現性 55
五、光譜干擾探討 55
六、校正曲線及偵測極限估計 56
七、樣品的前處理與分析 56
肆、結果與討論 58
一、化學蒸氣生成系統各參數之探討 58
二、ICP-MS系統操作條件之探討-氣體流速對分析訊號之影響 68
三、樣品稀釋倍數探討 68
四、分析物訊號之再現性 68
五、光譜干擾探討 71
六、校正曲線及偵測極限估計 71
七、樣品的前處理與分析 76
伍、結論 81
陸、參考文獻 82

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