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an, Shih yi
|關鍵字:||Microwave assisted;微波輔助;Headspace;Liquid phase microextraction;頂空;液相微萃取;氯酚;MA/HS-LPME||出版社:||化學系||摘要:||
本研究開發以微波輔助頂空液相微萃取技術結合氣相層析法分析環境水中的氯酚類污染物，發展為水溶液中氯酚類分析之快速樣品前處理技術。存於水基質的氯酚類藉由微波照射加熱，使其蒸氣壓迅速上升，汽化至頂空氣相中為中空纖維含有的萃取溶劑所萃取，待樣品萃取後，將萃取溶劑注入於氣相層析儀，結合電子捕捉偵測器進行分離與偵測。實驗中就影響萃取之因素，例如萃取位置及萃取溶劑的選擇、萃取水溶液之pH值、鹽析效應、微波照射時間與功率等參數作詳盡探討。實驗結果顯示使用MA/HS-LPME 方法於水樣中分析氯酚的最佳研究參數為：微波照射功率167 W，微波照射時間10分鐘，以正辛醇作萃取溶劑，pH 1且不添加鹽類的萃取液。以最佳條件進行氯酚類分析，其線性範圍為0.5~100 μg/l，相對標準偏差在小於11 %，偵測極限為DCP 0.66 μg/l、TCP 0.04 μg/l 、TeCP 0.07 μg/l、 PCP 0.08 μg/l。為驗證本研究方法的可行性，將此技術應用於真實樣品中氯酚化合物之測定，其回收率在83 % ~102 % 之間。因此，利用微波輔助頂空液相微萃取技術結合氣相層析法，偵測水中氯酚化合物為一快速、操作簡便、價格低廉、不受基質干擾、使用少量有機溶劑，且有良好的再現性與靈敏度之新方法。
The purpose of this paper is to detect chlorophenols in water by developing a new sample pretreatment technique, microwave assisted headspace liquid-phase microextraction (MA/HS-LPME). The analytical species in aqueous matrix are heated by using microwave irradiation. Because their vapor pressures rise quickly, species in headspace are dissolved in the organic solvent. After the compounds were collected, they were injected in a GC injection port and analyzed by GC/ECD. Parameters affecting the extraction efficiency such as pH in the solution, addition of salt to sample solution, the power and irradiation time of microwave as well as the time of extraction were investigated.
The optimum extraction efficiency of CPs in aqueous matrix was obtained by using octanol as extract solvent and the sample solution at pH 1 with irradiation power 167 Watt for 10 minutes. The detection was linear with r2 > 0.9911. The detection limits varied from 0.04 to 0.66 μg/l. We also applied it to detect the CPs of real water sample and the results showed that the recovery is between 83% and 102 %. The proposed method provided a simple, fast, inexpensive and organic solventless procedure for collect CPs from complicated sample matrix.
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