研究生: |
宋美芳 Sung, Mei-Fang |
---|---|
論文名稱: |
長鏈冠狀醚無機壓電晶體液體層析偵測系統之研製與應用 Preparation and Application of Alkyl(C18)-benzo-15-crown-5 Piezoelectric Crystal Liquid 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: | 中文 |
論文頁數: | 121 |
中文關鍵詞: | 壓電晶體 、長鏈冠狀醚 、液體層 |
論文種類: | 學術論文 |
相關次數: | 點閱:162 下載:0 |
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本研究利用自行合成的長鏈 B15C5 冠狀醚,將其塗佈在石英晶體表面作為石英壓電晶體偵測器 (piezoelectric quartz Crystal detector),石英晶體振盪器的石英膜表面會因吸附離子或分子化合物,而使負載之重量增加,造成石英晶體振盪頻率隨之遞減,再經由自製微電腦介面中的頻率-電壓 (F/V) 轉換器,將頻率訊號轉為電壓訊號並以放大器 (OPA) 放大,再經類比/數位 (A/D) 介面卡轉換成數位訊號,輸入電腦讀取記錄並繪圖。
本研究中,分別探討長鏈冠狀醚石英壓電晶體偵測器對各種有機/無機分子的威應,其中對各種極性有機分子的威應大小為:胺類 > 有機酸 > 醇類 > 酮類,並對有機物質之分子量的大小及異構物的立體結構等加以研究。長鏈冠狀醚石英壓電晶體偵測器對丙胺具有不錯的再現性及靈敏度,其偵測極限大約為 6xlO-5M。在無機金屬離子方面,分別偵測各種重金屬離子的感應,其大小順序為:Cr3+ > Pb2+ > Co2+ > Cd2+ > Ni2+ > Cu2+,而且皆具有良好的濃度線性關係及低偵測極限。
本研究亦自行建立電化學微量石英天平系統,利用繼電器的切換可以決定工作電極與石英晶體振盪線路連接,或與電位儀接通,將此系統應用在重金屬離子溶液偵測,利用氧化還原的原理將重金屬沈積在石英晶體表面,因此可以觀察到還原時間對頻率的影響,結果發現此系統具有很好的濃度效應;亦可將電壓-電流變化圖及電壓─頻率變化圖結合,藉以更加了解氧化還原的過程。
A water insoluble crown ether alkyl(C18)-benzo-15-crown-5 was synthesized and applied as a coating material on piezoelectric quartz crystal membranes. The oscillating crown ether coated piezoelectric crystal with a home-made computer interface was prepared as a liquid chromatographic detector for various organic/inorganic species. The variation of the crystal frequency were converted to voltage with a frequency to voltage (F/V) converter, and followed by amplification with OPA and data acquisition with analog to digital (A/D) converter.
The alkyl(C18)-benzo-15-crown-5 piezoelectric quartz crystal dectector was applied to detect various organic/inorganic species. The sensitivity of the crown ether coated piezoelectric crystal detector for these organic molecules were in the order: amine > carboxylic acid > alcohol > ketone respectively. The effect of organic molecule weight and strike hindrance on the crown ether piezoelectric crystal detector had been investigated. The detection limits with the long-chain crown ether PZ detector was 6xlO-5M for propaylamine and exhibited good reproducibility and high sensitivity. In heavy metal ions, the frequency shift was in the order: Cr3+>Pb2+>Co2+>Cd2+>Ni2+>Cu2+. The crown ether piezoelectric crystal detector also had good sensitivity for some heavy metal ions with quite low detection limits.
The electrochemical quartz crystal microbalance was set-up and applied to detect the heavy metal ions. The working electrode was connected to the circuit of oscillator or potential meter with switching of applied to detect the heavy metal ions. The working electrode was connected to the circuit of oscillator or potential meter with switching of the relay. The heavy metal ions were reduced to the Au electrode of piezoelectric crystal, thus the variation of frequency was observed and the good concentration effect of this system was demonstrated. To combine the I-V and V-F curves, the more sophisticated oxidation and reduction processes can be readily realized.