第一篇研究為電熱式揮發感應耦合電漿質譜儀於鎳基質合金中的多元素分析之應用。本研究中將以溫度揮發的方式，藉由分析物（鍺、砷、硒、碲、鉈及鉛）與鈷鎳基質之不同揮發行為，在特定溫度時將待測分析物與基質分離並將分析物揮發進入ICP-MS中進行偵測。研究中，將對修飾劑選擇、儀器操作條件及光譜干擾等參數進行探討。由實驗結果發現以 1.0% m/v Ascorbic acid 及0.1% m/v Thioacetamide（TAC）作為修飾劑有助於改變分析物的揮發行為，提升分析物的訊號。樣品濃度的配製則選擇0.2% m/v的樣品濃度，並將揮發溫度設定為1700oC時，最能夠有效的減輕鈷鎳基質對於分析元素所造成的光譜及非光譜干擾，並於研究中探討是否會有會有其它干擾物對分析物造成光譜干擾；最後對於三種標準參考樣品SRM 897、898、899，分別使用標準添加法與同位素稀釋法來進行定量分析，以驗證本實驗方法的可行性，並與消化超合金樣品後以傳統氣動式霧化器進行定量所得的結果比較。此方法對於鍺、砷、硒、碲、鉈及鉛元素之方法偵測極限分別為 2.0、1.4、3.0、1.6、1.5、2.6 ng g-1。
第二篇研究為電熱式揮發感應耦合電漿質譜儀於指甲油中鉻、砷、鎘、銻、汞及鉛元素分析之應用。研究中將對動態反應室（Dynamic reaction cell，DRC）系統的條件、修飾劑選擇、乳濁狀液體樣品的配製、光譜干擾及儀器操作條件等參數進行探討。在DRC系統選擇以氧氣作為反應氣體來減輕樣品及石磨爐中碳原子對於分析物所造成的光譜干擾。由實驗結果發現以0.5% m/v Tartaric acid及0.5% m/v Thioacetamide（TAC）作為混合修飾劑有助於提升分析物的訊號。樣品濃度的配製則選擇2.0% m/v的樣品濃度，並將灰化溫度和揮發溫度分別設定為150oC與2000oC，並於研究中探討是否會有會有其它干擾物對分析物造成光譜干擾。於各分析條件最適化後，將本系統運用在市售指甲油的定量分析上，但由於指甲油無標準參考樣品，實驗中將分別使用標準添加法與同位素稀釋法來進行定量分析，以驗證本實驗方法的可行性，同時與指甲油樣品消化後以傳統氣動式霧化器進行定量所得的結果相互比較。此方法對於鉻、砷、鎘、銻、汞及鉛元素的方法偵測極限分別為0.3、0.2、0.1、0.1、0.5、0.3 ng g-1。

The first research, the determination of Ge, As, Se, Te, Tl and Pb in Nickel-based alloy by ETV-ICP-MS was studied. Ascorbic acid and Thioacetamide（TAC）was used as the modifier. In the experiment procedure, we will study the operation conditions, sample concentration and spectral interference etc. Vaporization Temperature was set as 1700oC, which can separated the analyte from the major matrix component, nickel and cobalt. Finally, for the three standard reference samples SRM 897, 898 and 899, using the standard addition method and isotope dilution method for quantitative analysis to verify the feasibility of the method. After digestion, compare with the quantitative results obtained from the conventional pneumatic nebulizer. The method detection limit estimated from standard addition curves was 2.0, 1.4, 3.0, 1.6, 1.5 and 2.6 ng g-1 for Ge, As, Se, Te, Tl and Pb respectively.
The second research, electrothermal vaporization-dynamic reaction cell-inductively coupled plasma mass spectrometry（ETV-DRC-ICP-MS）has been used to determine Cr, As, Cd, Sb, Hg and Pb in Nail-polish sample. Tartaric acid and Thioacetamide（TAC）was used as the modifier to enhance the ion signals. In the experiment procedure, we will study the operation conditions, DRC system, sample concentration and spectral interference etc. In the DRC systems, we selected O2 as the reaction gas to reduce spectral interference caused by the ArC+, while the Rpq value was set as 0.55. Vaporization temperature and ash temperature was set as 2000oC and 150oC respectively. Finally, Standard addition and isotope dilution method has been applied to the determination of Cr, As, Cd, Sb, Hg and Pb in three Nail-polish samples purchased from the department store. After digestion, compare with the quantitative results obtained from the conventional pneumatic nebulizer. The method detection limit estimated from standard addition curves was 0.3, 0.2, 0.1, 0.1, 0.5, 0.3 ng g-1 for Cr, As, Cd, Sb, Hg and Pb respectively.

目錄
論文審定書i
謝誌 ii
摘要 iii
Abstract iv
目錄 v
圖目錄 vii
表目錄 ix

第 一 章 電熱式揮發感應耦合電漿質譜儀於鎳基質合金中微量元素分析之應用
壹、前言 1
一、研究背景 1
二、超音波泥漿取樣法結合電熱式揮發樣品輸入簡介 3
三、鍺、砷、硒、碲、鉈、鉛之各論 6
四、同位素稀釋法 8
貳、實驗部分 9
一、儀器裝置及操作簡介 9
二、試劑藥品及溶液配製 14
參、結果與討論 22
一、修飾劑的選擇 22
二. 酸對分析物訊號的影響 28
三.樣品稀釋倍數探討 31
四、灰化溫度（Ash Temperature）及揮發溫度（Vaporization Temperature）的選擇 33
五、光譜(同質量)干擾 36
六、校正曲線 40
七、樣品定量分析 43
肆、結論 49
伍、參考文獻 50

第 二 章 電熱式揮發感應耦合電漿質譜儀於指甲油中多元素分析之應用
壹 前言 56
一、研究背景 56
二、動態反應室(Dynamic reaction cell，DRC) 58
三 鉻、砷、鎘、銻、汞及鉛之個論 60
貳、實驗部分 62
一、儀器裝置及操作條件 62
二、試劑藥品及溶液的配製 65
參、結果討論 74
一、ETV-ICP-MS系統中修飾劑的選擇 74
二、界面活性劑對分析物訊號的影響 79
三、酸對分析物訊號的影響 81
四、樣品稀釋倍數探討 83
五、DRC系統之最適化 85
六、灰化溫度（Ash Temperature）及揮發溫度（Vaporization Temperature）的選擇 92
七、光譜(同質量)干擾 95
八、校正曲線 98
九、樣品定量分析 101
肆、結論 105
伍、參考文獻 106

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