研究生: |
高貫洲 Gau, Guann-Jou |
---|---|
論文名稱: |
碳六十/大環胺醚複合物壓電晶體氣體層析偵測器研製與應用 Preparation and Application of Fullerene/Ctrytand Complex Piezoelectric Crystal Gas Chromatographic Detector |
指導教授: |
施正雄
Shih, Jeng-Shong |
學位類別: |
碩士 Master |
系所名稱: |
化學系 Department of Chemistry |
畢業學年度: | 85 |
語文別: | 英文 |
論文頁數: | 131 |
中文關鍵詞: | 碳六十 、大環胺醚複合物 |
論文種類: | 學術論文 |
相關次數: | 點閱:124 下載:0 |
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由本研究研製碳六十/大環胺醚複合物壓電晶休氣休層析偵測器,偵測常見的揮發性有機化合物,並與商業化之熱傳導偵測器做比較。利用石英晶体膜表面吸附化合物產生頻率變化的特性,經由自行設計之計頻系統及8255微電腦介面來讀取振盪頻率及變化,並以自行撰寫軟体控制介面、記錄數據及繪圖。本研究在石英晶片表面上塗佈碳六十/大環胺醚複合物,對於由氣体層析管柱分離之有機化合物產生吸附現象而達成偵測的效果。
本研究首先由靜相系統探討碳六十/大環胺醚和有機揮發化合物的吸附現象,研究不同官能基、不同碳數及同分異構物對訊號產生之影響。就官能基而言為:酸>胺>醇>酮、炔>烯>烷;就不同碳數為:碳鏈愈長訊號愈強;就同分異構物為:一級胺>二級胺>三級胺、2-己炔≒3-己炔>1-己炔。再由動相系統探討極性不同化合物之訊號強弱及系統可逆性,發現若塗佈碳六十/大環胺醚複合物對於不同極性化合物之偵測效果比分別塗佈碳六十及大環胺醚為好,並可使系統有不錯的可逆性。最後將系統與 GC 連線,以碳六十/大環胺醚石英壓電晶体膜作為氣相層析偵測器。本系統除了有良好的靈敏度及再現性,對於不同碳數(碳數愈大訊號愈強)及同分異構物(一級化合物>二級化合物)有良好的鑑別力。
本研究所用的碳六十/大環胺醚氣体層析壓電晶体偵測器從晶片塗佈、振盪線路的焊接,到訊號處理及儲存由於自行設計及製作,成本低廉。而其靈敏度及偵測極限與商業化的 TCD 不相上下。
A C6o/Cryptand complex coated piezoelectric quartz crystal membrane sensor with a home-made computer interface was prepared and applied as a Gas Chromatographic detector for various organic molecules. The computer interface includes the oscillating circuit and data processing with 8255. A software was written to control the interface and data acquisition.
Effects of functional groups, molecular weight, and steric hindrance in static cell were studied. The frequency shift of the C6o/Cryptand coated crystal for various organic molecules and isomers were in the orders: R-COOH >R-NH2 >R-OH >R-COR1, Hexyne >Hexene>Hexane and 1°amine(R-NH2)>2°amine(R2-NH)>3°amine(R3-N) respectively. The greater frequency shift of a molecule with larger molar mass was also found. The polarity of organic molecules and reversibility in mobile system was investigated. The C60/Cryptand coated PZ detector exhibited more sensitive to polar and non-polar molecules than Fullerene or cryptand coated system individually. The C60/Cryptand complex piezoelectric crystal as Gas Chromatographic detector has performed not only high sensitivity, good reproducibility, but also distinguished to different molecular weight and isomer.
The home-made C6o/Cryptand piezoelectric crystal Gas Chromatographic detector with limit of quantitation 3.65 × 140-6g, showed good competition with commercial TCD (Thermal conductivity Detector).