透過您的圖書館登入
IP:18.224.38.43
  • 學位論文

氣相層析質譜儀電子撞擊游離化法與正化學游離化法及氣相層析儀-火焰離子化偵測器應用於含氟鏈聯吡啶螯合劑之研究

GC/MS Electron Ionization and Positive Chemical Ionization modes and GC-FID Studies of a series of 4,4’- and 5,5’-bis(fluorous-ponytail)-2,2’-bipyridine

指導教授 : 呂良賜
若您是本文的作者,可授權文章由華藝線上圖書館中協助推廣。

摘要


本研究室已成功利用含氟醇類分別合成出在聯吡啶的4,4’位置以及在聯吡啶5,5’位置上有兩個含氟鏈的聯吡啶螯合劑〔4,4’-bis(RfCH2OCH2)-2,2’-bpy (1a-k) and 5,5’-bis(RfCH2OCH2)-2,2’-bpy (2a-f), Rf = n-CF3 (a), HCF2CF2 (b), n-C2F5 (c), n-C3F7 (d), HCF2(CF2)3 (e), HCF2(CF2)5 (f) , n-C7F15 (g) , HCF2(CF2)7 (h) , n-C8F17 (i) , n-C9F19 (j) , n-C10F21 (k)〕。本研究利用氣相層析質譜儀的電子撞擊游離化法與正化學游離法以及氣相層析儀-火焰離子化偵測器來分析鑑定這些螯合劑並探討之。由氣相層析質譜儀分析的結果中我們可以發現在電子撞擊游離化模式下分析時,質譜圖中螯合劑的分子離子峰具有較小的訊號強度,甚至會消失而無法辨識;而在正化學游離化模式下分析時,螯合劑的分子離子峰[M+H]+則具有較強的訊號強度,除此之外更可以觀察到[M+C2H5]+ 以及[M+C3H5]+的離子峰。另外,本研究更進一步地探討利用氣相層析儀-火焰離子化偵測器作為螯合劑定性分析的研究與定量分析的可能性。

並列摘要


With the readily available fluorous alkanols, RfCH2OH, two series of novel fluorous-ponytailed bpy ligands, 4,4’-bis(RfCH2OCH2)-2,2’-bpy (1a-k) and 5,5’-bis(RfCH2OCH2)-2,2’-bpy (2a-f), where Rf = n-CF3 (a), HCF2CF2 (b), n-C2F5 (c), n-C3F7 (d), HCF2(CF2)3 (e), HCF2(CF2)5 (f) , n-C7F15 (g) , HCF2(CF2)7 (h) , n-C8F17 (i) , n-C9F19 (j) , n-C10F21 (k) were successfully synthesized. The new ligands were not only spectroscopically characterized but also extensively studied by gas chromatography, e.g. using GC/MS electron ionization (EI) mode, positive chemical ionization (PCI) mode, GC-FID and so on. As expected, using the EI mode the molecular ion is either not detected or present with very low abundance. When using the PCI mode, the molecular ion [M+H]+ peak becomes highly abundant peak. In addition to [M+H]+ peak, the peaks with [M+C2H5]+ and [M+C3H5]+ fragments also appear as the fingerprints of these two types of compounds. The details of these mass studies will be presented. Furthermore, using the GC-FID to quantify these fluorous bipyridyl ligands will also be addressed.

參考文獻


[8] 陳世傑,含氟長鏈雙吡啶Pd金屬錯合物之Heck以及Suzuki反應研究,碩士論文,國立台北科技大學有機高分子研究所,台北,2008。
[1] Robert M. Silverstein and Francis X. Webster, Spectrometric Identification of Organic Compounds, 6th Edition, New York: John Wiley & Sons, Inc. 1997.
[2] Skoog, Holler and Nieman, Principles of Instrumental Analysis, 5th Edition, Philadelphia: Saunders College Publishing, 1998.
[3] Skoog, West and Holler, Fundamentals of Analytical Chemistry, 7th Edition, Philadelphia: Saunders College Publishing, 1996.
[4] Agilent Technologies, Operation Manual Vol. 2 Inlets, Wilmington: Agilent Technologies, Inc., 2000.

延伸閱讀