感應耦合電漿質譜儀是一種微量多元素分析及同位素分析技術，具有高靈敏度、低偵測極限、同時偵測多元素、同位素分析及線性範圍廣等優點。本論文將使用雷射剝蝕進樣以及毛細管電泳兩種技術分別與感應耦合電漿作結合，並進行一連串最適化探討以及真實樣品的應用。
本研究第一部分係使用雷射剝蝕結合感應耦合電漿質譜儀 ( Laser Ablation Inductively Coupled Plasma Mass Spectrometry， LA-ICP-MS ) 針對鋼鐵中硼、鋁、矽、磷與硫等輕元素進行分析，該技術是利用高能量的雷射照射在固體樣品表面而產生微小粒子後，再以載氣送入ICP-MS中進行分析，為一快速、直接且不需前處理之定量技術。
以 ICP-MS 偵測輕元素時，同質量離子和多原子離子產生之光譜干擾較為嚴重，故本研究結合動力反應室 ( Dynamic Reaction Cell，簡稱DRC )，使用氧氣做為反應氣體，將矽、磷與硫等元素反應至干擾較少之 m/z = 44、47及48進行偵測，例如將 32S 轉移至 32S16O，便可避免氧所造成之 16O16O 的干擾。將動態反應管與 LA-ICP-MS 系統最佳化後，利用標準品建立檢量線，對碳鋼與不?袗?樣品進行定量分析，各元素之方法偵測極限在 0.007 至 0.7 μg g-1之間。
本研究第二部份係利用毛細管電泳系統透過CEI-100介面結合動態反應管感應耦合電漿質譜儀對環境樣品中砷及硒進行物種分析。研究中使用內徑75 μm、長60 cm的毛細管，以含有0.5 mM SDS之25 mM CAPS ( 3-Cyclohexylamino-1-propanesulfonic acid ) pH 9.5作為分離電解質，在 +25 kV的分離電壓下，在600秒內可成功分離AsB、DMA、MMA、As(III)、As(V)、SeMet、MeSeCys、SeCys2、Se(IV) 及Se(VI) 等十個物種，各物種遷移時間之再現性均優於5.0%。
感應耦合電漿質譜儀之電漿氣體氬氣產生的38Ar40Ar+ 和38Ar40Ar+，會對78Se+、80Se+產生同質量多原子離子干擾，本研究使用通有甲烷 ( CH4 ) 氣體之動態反應室系統，可降低此干擾。
在系統最適化下，各物種偵測極限介於0.5~1.8 ng mL-1。將上述毛細管系統應用於魚肝標準樣品、健康食品硒錠以及飛灰標準樣品等三種真實樣品，並應用微波輔助酵素萃取 ( microwave assisted enzymatic extraction )提升硒錠和魚肝樣品中硒物種之萃取效率。使用蛋白酶 ( protease ) 與脂肪酶 ( lipase ) 配合微波輔助，三個樣品的砷與硒之萃取效率皆可達86%~107%。以毛細管電泳系統分析樣品萃取液，皆可成功分離並進行物種定量。spike recovery則介於 91%~103% 間。

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第一章 以雷射剝蝕結合感應耦合電漿質譜儀分析鋼鐵中輕元素之應用 1
第1節 前言 1
1.1 鋼鐵概論 1
1.2 分析技術 2
1.3 LA-ICP-MS系統 3
1.4 動態反應管 6
1.5 研究目的 7
第2節 儀器原理 8
2.1 LA-ICP-MS原理 8
2.2 動態反應管原理 16
第3節 實驗部分 21
3.1 儀器設備 21
3.2 試劑藥品 21
3.3 藥品配製 22
3.4 樣品 22
3.5 實驗操作 22
第4節 結果與討論 25
4.1 動態反應管系統探討 25
4.1.1 反應氣體流速探討 29
4.1.2 Rejection parameter q探討 41
4.1.3 軸場電壓探討 41
4.2 雷射剝蝕系統條件探討 46
4.2.1 雷射能量探討 46
4.2.2 雷射spot size探討 46
4.2.3 雷射repetition rate探討 47
4.2.4 雷射scan rate探討 47
4.2.5 載氣組成及流速探討 52
4.3 校正曲線及定量結果 57
第5節 結論 68
第6節 參考文獻 69
第二章 毛細管電泳結合感應耦合電漿質譜儀於砷及硒物種分析之應用 74
第1節 前言 74
1.1 毛細管電泳 74
1.3 分析技術 78
第2節 儀器簡介 80
2.1 毛細管電泳分離原理 80
2.2 毛細管電泳與ICP-MS介面 ─ CEI-100介紹 84
第3節 實驗部份 86
3.1 儀器裝置與設備 86
3.2試劑藥品 87
3.3 溶液配製 90
3.3.1 分析物標準溶液 90
3.3.2電解質溶液 91
3.3.3 輔助溶液 92
3.4 實驗操作 92
3.4.1 實驗準備 92
3.4.2 分離電解質之更換 93
3.4.3 樣品之注入 93
3.4.4 實驗完成 93
3.5 萃取步驟 94
3.5.1 魚肝標準參考樣品（NRCC DOLT-3） 94
3.5.2 市售硒錠營養品 95
3.5.3 飛灰標準樣品（SRM 1633b） 95
第4節 結果與討論 97
4.1 CE分離條件最適化 97
4.1.1 分離電解質的選擇 97
4.1.2 不同pH值之分離電解質對物種分離之影響 97
4.1.3 不同分離電解質濃度對物種分離之影響 98
4.1.4 不同界面活性劑濃度對物種分離之影響 101
4.1.5 分離電壓對物種分離之影響 101
4.1.6 進樣時間對物種分離之影響 102
4.2動態反應管系統探討 106
4.2.1 反應氣體流速探討 106
4.2.2 Rejection parameter q探討 110
4.2.3 軸場電壓探討 110
4.3 重複性 116
4.4 校正曲線 116
4.5 真實樣品分析應用 119
4.5.1魚肝標準品（NRCC DOLT-3） 119
4.5.2 市售硒錠 125
4.5.3 飛灰標準參考樣品（SRM 1633b） 128
第5節 結論 131
第6節 參考文獻 132

part.1
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part.2
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