動力反應室感應偶合電漿質譜儀（Dynamic reaction cell inductively coupled plasma mass spectrometry，DRC-ICP-MS）是一種偵測微量多元素及同位素之分析技術，它結合了ICP原子化及游離化的特性，以及質譜儀的高靈敏度和測定同位素比的能力。ICP-MS雖已成功地應用於許多不同種類樣品的分析，但仍須面對光譜性干擾（質量重疊干擾）和非光譜性干擾之問題。而動力反應室(Dynamic reaction cell, DRC)在近年來的發展，已可有效減輕ICP-MS分析中的光譜性干擾。本研究將以動力反應室結合感應偶合電漿質譜儀對於泥土及沉積土中鍺、砷、及硒分析之應用。
本研究首先利用超音波泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀（USS-ETV-DRC-ICP-MS），直接同時測定土壤樣品中砷及硒的濃度，以建立固體樣品的直接分析方法。實驗中將使用ascorbic acid和Pd為混和修飾劑來增加分析物之訊號及熱穩定性。而DRC系統中是以氧氣為反應氣體，期望降低Ar2＋對Se分析的多原子離子干擾，並偵測75As16O+來避開40Ar35Cl+對75As+之干擾。最後，以本實驗所建立的USS-ETV-DRC-ICP-MS方法運用在泥土標準參考樣品（NIST SRM 2709、2711）及蔬菜園泥土中砷及硒的定量分析。
第一部份實驗中，以氧氣作為反應氣體並無法完全地避免As及Se分析的光譜干擾問題。因此，在第二部份實驗時，選用其它氣體（甲烷及氫氣）為反應氣體，來降低泥土、沉積土中基質對於鍺、砷及硒分析所造成的多原子離子干擾。實驗中將泥土、沉積土消化後直接進樣，並配製模擬基質溶液來對分析物（Ge、As及Se）所造成的光譜干擾作一系列探討。最後選擇以氫氣作為反應氣體，氣體流速為1.5ml min-1，q值設為0.8，藉著分析物與干擾離子間不同的化學反應，以去除樣品基質所產生的同質量干擾。因為所分析樣品中Se的含量甚低，研究中使用超音波霧化器為進樣系統。並證實以USN-DRC-ICP-MS直接分析土壤及沉積土樣品中Ge、As及Se的可行性。
研究的最後，我們結合USS-ETV-DRC-ICP-MS並以氫氣為反應氣體，可成功地分析土壤（SRM 2709、2711）及沉積土（SRM BCSS-1）中鍺、砷及硒的含量，證實了使用USS-ETV-DRC-ICP-MS結合標準添加法，直接分析土壤及沉積土樣品中Ge、As及Se的可行性。

Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cellTM inductively coupled plasma mass spectrometry (USS-ETV-DRC-ICP-MS) has been applied to the determination of As and Se in soil and sediment samples. The influences of instrument operating conditions and slurry preparation on the ion signals were reported. Ascorbic acid and Pd were used as the modifiers to enhance the ion signals. The background ions at the selenium masses were reduced in intensity significantly by using 1.5 ml min-1 H2 as reaction cell gas in the DRC while a q value of 0.65 was used. Since the sensitivities of As and Se in slurry solution and aqueous solution were quite different, standard addition method was used for the determination of As and Se in these samples. This method has been applied to the determination of As and Se in NIST SRM 2711 Montana soil and SRM 2709 San Joaquin soil reference materials and NRCC BCSS-1 marine sediment reference sample. The analysis results of the reference materials were agreed with the certified values. The method detection limits estimated from standard addition curves were about 0.046-0.082 and 0.019-0.024 mg g-1 for As and Se, respectively, in original soil and sediment samples.

論文摘要………………………………………………Ⅰ
謝誌……………………………………………………Ⅲ
目錄……………………………………………………Ⅳ
圖表目錄………………………………………………Ⅶ

第一章 感應偶合電漿質譜儀簡介…………………1
壹、前言………………………………………………1
貳、感應偶合電漿質譜儀基本原理…………………2
參、分析功能與限制…………………………………5
一、光譜性干擾…………………………………6
二、非光譜性干擾……………………………………7
肆、Dynamic Reaction Cell原理…………………10
伍、應用實例………………………………………14
一、同位素測量………………………………14
二、元素分析…………………………………16
陸、結論……………………………………………17
柒、參考文獻………………………………………18
第二章 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於泥土樣品中砷及硒分析之應用…………………20
壹、前言……………………………………………20
貳、分析技術………………………………………………………………24
參、實驗部分………………………………………………………………27
一、儀器裝置及操作條件……………………………………………27
二、試劑藥品及溶液的配製…………………………………………32
三、泥漿樣品的製備………………………………………………………33
肆、結果與討論……………………………………………………………36
一、稀釋倍數的探討………………………………………………………36
二、修飾劑的選擇…………………………………………………………38
三、酸及界面活性劑對分析物訊號的影響………………………………44
四、灰化溫度及揮發溫度的選擇…………………………………………45
五、DRC系統的最佳化……………………………………………………51
六、樣品的定量分析……………………………………………………58
伍、結論…………………………………………………………………62
陸、參考文獻-……………………………………………………………63

第三章 動力反應室結合感應偶合電漿質譜儀測定土壤及沉積土中鍺、砷 及硒分析之應用……………………………………………………67
壹、前言…………………………………………………………………67
貳、實驗部份………………………………………………………………70
一、儀器裝置及操作條件……………………………………………70
二、試劑藥品及溶液的配製…………………………………………70
三、實驗過程……………………………………………………………72
參、結果與討論…………………………………………………………73
一、DRC-ICP-MS操作條件的最佳化…………………………………73
二、樣品基質在反應槽中形成副產物對分析物訊號的影響…………84
三、校正曲線與偵測極限的估計………………………………………95
四、土壤及沉積土的分析………………………………………………95
肆、結論…………………………………………………………………99
伍、參考文獻……………………………………………………………100

第四章 泥漿取樣法結合電熱式揮發感應偶合電漿質譜儀於泥土及沉積土中鍺、砷及硒分析之應用……………………………………………………………………103
壹、DRC系統之最佳化…………………………………………………103
貳、土壤及沉積土分析…………………………………………………105

1.http://home.netvigator.com/~f704/trad/index.html
2.M. Krachler and H. Emons, J. Anal. At. Spectrom., 2001, 16, 20.
3.D. T. Heitkemper, N. P. Vela, K. R. Stewart and C. S. Westphal, J. Anal. At. Spectrom., 2001, 16, 299.
4.M. Kotrebai, M. Birringer, J. F. Tyson, E. Block and P. C. Uden, Analyst, 1999, 125, 71.
5.K. Falk and H. Emons, J. Anal. At. Spectrom., 2000, 15, 643.
6.M. Song and T. U. Probst, Anal. Chim. Acta, 2000, 413, 207.
7.S. M. Maia, J. B. B. Dasilva, A. J. Curtius and B. Welz, J. Anal. At. Spectrom., 2000, 15, 1081.
8.D. Pozebon, V. L. Dressler and A. J. Curtius, Talanta, 2000, 51, 903.
9.H. H. Lu and S. J. Jiang, Anal. Chim. Acta, 2001, 429, 247.
10.J. X. Li, F. Lu, T. Umemura and K. Tsunoda, Anal. Chim. Acta, 2000, 419, 65.
11.Y. Cai, M. Georgiadis and J. W. Fourqurean, Spectrochim. Acta, PartB, 2000, 55, 1411.
12.A. A. Menegario and M. F. Gine, Spectrochim. Acta, PartB, 2000, 55,355.
13.G. Centineo, MM. Bayon and A. Sanzmedel, J. Anal. At. Spectrom., 2000, 15, 1357.
14.L. Moens, Fresenius´ J. Anal. Chem., 1997, 359, 309.
15.S. Sakao, Y. Ogawa and H. Uchida, Anal. Chim. Acta, 1997, 355, 121.
16.M. Bettinelli and U. Baroni, At. Spectrosc., 1995, 16, 203.
17.M. V. B. Krishna, D. Karunasagar and J. Arunachalam, Fresenius´ J. Anal. Chem., 1999, 363, 353.
18.L. Jian, W. Goessler and K. J. Irgolic, Fresenius´ J. Anal. Chem., 2000, 366, 48.
19.M. Resano, M. Verstraete, F. Vanhaecke, L. Moens, A. Vanalphen and R. Denoyer, J. Anal. At. Spectrom., 2000, 15, 389.
20.J. M. B. Moreno, M. Betti and G. Nicolaou, J. Anal. At. Spectrom., 1999, 14, 875.
21.J. R. Encinar, J. I. G. Alonso, A. Sanzmedel, S. Main and P. J. Turner, J. Anal. At. Spectrom., 2001, 16, 322.
22.T. Meisel, J. Moser, N. Fellner, W. Wegscheider and R. Schoenberg, Analyst, 2001, 126, 322.
23.A. G. Coedo, T. Dorado, I. Padilla and F. J. Alguacil, J. Anal. At. Spectrom., 2000, 12, 1564.
24.L. moens, F. Vanhaeche, J. Riondato, and R. Dams, J. Anal. At. Spectrom., 1995, 10, 569.
25.S. D. Tanner, At. Spectrosc., 1995, 10, 905.
26.J. W. H. Lam, J. W. Mclaren, and B. A. J. Methven, J. Anal. At. Spectrom., 1995, 10, 551.
27.S. J. Hill, M. J. Ford, and L. Ebdom, J. Anal. At. Spectrom., 1992, 17, 719.
28.S. Branch, L. Ebdom, M. Ford, M. Foulkes, and P. Oneill, J. Anal. At. Spectrom., 1997, 6, 151.
29.D. Bandura, V. I. Baranov, and S. D. Tanner, J. Anal. At. Spectrom., 2000, 15, 921.
30.J. Sloth, and E. Larsen, J. Anal. At. Spectrom., 2000, 15, 669.
31.S. D. Tanner, and V. I. Baranov, and U. Vollkopf, J. Anal. At. Spectrom., 2000, 15, 1261.
32.K. Neubauer, and U. Vollkopf, At. Spectrosc., 1999, 20, 64.
33.S. F. Boulyga, J. S. Becker, Fresenius´ J. Anal. Chem., 2001, 370, 618.
34.B. Hattendorf, D. Gunther, Spectrochim. Acta, PartB, 2003, 58, 1.
35.D. E. Nixon, K. R. Neubauer, S. J. Eckdahl, J. A. Butz, M. F. Burritta, Spectrochim. Acta, PartB, 2003, 58, 97.
36.M. Iglesias, N. Gilon, E. Pousselb, J. M. Mermetb, J. Anal. At. Spectrom., 2002, 17, 1240.