本計畫完成多氯萘檢測方法開發，含前處理程序及儀器分析條件測試，並以此方法分析灰份中多氯萘濃度及物種分布。前處理程序分為萃取及淨化測試，分別測試極性及非極性物質作為吸附劑之影響，結果顯示分離效果受吸附劑之吸附力影響甚大，非極性吸附劑對多氯萘之吸附力較佳且具有去除高沸點雜質之優勢，但卻有高成本、耗時等缺點; 氧化鋁及矽酸鎂測試結果指出矽酸鎂吸附力較佳，對多氯萘分離效果較佳; 萃取方面則以二氯甲烷、正己烷/丙酮(1:1 , v/v)及甲苯進行測試，測試結果顯示二氯甲烷對單氯萘至三氯萘效果較佳，甲苯對四氯萘至八氯萘效果較佳，且對高含碳量基質具萃取優勢。品保/品管測試結果指出本方法之多氯萘方法偵測極限濃度為0.1 ng/mL；精密度測試結果顯示待測物多氯萘回收率為99.4%-106%，而內標準品回收率為51%-90.7%。此外，高解析度氣相層析/高解析度質譜儀及高解析度氣相層析串聯質譜儀之平行比對結果發現層析管柱之種類差異對多氯萘濃度及回收率影響甚大，多氯萘於60 m管柱之分離效果較40 m為佳，若分離效果不佳將進而導致異構物定量受雜質干擾，此外，由於四氯聯苯於串聯質譜儀中受雜質干擾導致正偏差，使單氯萘至四氯萘之內標準品回收率較低，定量較不準確。 ;The project for developing the method for the analysis of polychlorinated naphthalene (PCNs) in fly ash has been completed. The tests of pretreatments and instrument parameters have been carried out. The pretreatment tests were devided into extraction and clean-up process. The results of clean-up tests indicate that the effects of adsorbents on PCNs separation are significant and depend on the adsorption capability of adsorbent. Non-polar adsorbent such as activated carbon with a high specific area has the advantage of high adsorption capacity and can separate high boiling point interferences from analyzte, however, it has the disadvantages of being costly and time-comsuming. Additionally, in the test of the polar adsorbents, Aluminum exhibits a higher adsorption ability than Florisil. For the extraction test, dichloromethane (DCM), hexane/acetone (1:1, v/v) and toluene have been selected as solvents. The results show that DCM has a high extraction efficiency for Mono-CN to Tri-CN while higher extraction efficeiencies can be achieved for Tetra-CN to Octa-CN as toluene is applied as solvent. Besides, toluene also can effectively extract aromatic compounds from the high-carbon matrix such as flyash and sediment. Thus, toluene is selected to extract samples in this study. The Quality Assurance and Quality Control (QAQC) have also been conducted. The method detection limit has been evaluated repeatedly with 0.1 ng/mL PCN following the methods of NIEA-PA107. Furthermore, the results of the precision test indicate that the recovery efficiencies PCNs analyte and internal standard are within the range of 99.4%-106% and 51%-90.7%, respectively. The control standards of PCN recovery efficiency for NIEA are suggested according to the results. Comparison of PCNs analysis between High Resolution Gas Chromatography/High Resolution Mass Spectrometry (HRGC/HRMS) with 60 m column and Gas Chromatography/Tandem Mass Spectrometry (GC-MS/MS with 40 m) column has been made. The results point out that the properties of column are the critical to affect the separation efficiency of PCNs compounds. From Mono-CN to Tri-CN pattens, MonoCNs and DiCNs exhibit higher resolution with HRMS than that with GC/MSMS. However, low resolution results may cause uncertainty of quantification. Besides, higher peak of RS (13C-tetra-PCB) is attributed to low recovery efficiencies of Mono-CN to Tetra-CN as GC/MSMS is applied for the analysis.
