Application of Integrated HPLC System to Environmental Analysis of Phenols

• Main Authors: Jeng, Hung-Hong, 鄭惠紅
• Other Authors: Cheng, Show-Chuen
• Format: Others
• Language: zh-TW
• Online Access: http://ndltd.ncl.edu.tw/handle/32745287742457671831

碩士 === 輔仁大學 === 化學學系 === 81 === U.S. EPA 之標準方法 604 係分析水樣中之酚類污染物， 8040 則係分析 土壤中之酚類污染物；兩方法都使用二氯甲烷作為萃取劑。但在實際操作 時，兩相之間會因乳化現象而分離不易，而後續之減壓濃縮步驟也會導致 揮發性酚類化合物之逸失。本文係利用酚類在鹼性條件下的親水性，以正 己烷將有機雜質從 pH ≧ 11 的水溶液中萃取出。將 pH 調至 3.8附近後 ，再利用本實驗室之整合液相層析系統作線上濃縮及分析。 結果顯示回 收率可達 78-94 % ，再現性亦達 0.2-8.8 % RSD ，比 U.S. EPA 604 的 23-88 % ，以及 8040 的 35-93 % 都改善許多。尤其是，上述的兩種 標準方法中無法處理的干擾峰問題，可以在本方法中由光極列偵測器所得 之全光譜來判別。水樣之方法偵測極限為 0.8-8.0 ppb，而土壤為 9-87 ppb 。 The extraction solvent of dichloromethane as employed in the EPA Method 604 for analysis of phenols in water or 8040 for soil may give rise to incomplete phase separation and long settling time as a result of emulsification. Subsequent enrichment in a rotary evaporator at subatmospheres as required by either method would also impart significant loss of samples. Alternatively, the sample cleanup can be done at pH ≧ 11 using n-hexane as the extractant to rid organic interferents. The extracted aqueous solution after pH adjustment to 3.8 can then be enriched on-line prior by HPLC analysis. Results indicated that give 78-94 % of recoveries with 0.2-8.8 % RSD of reproducbilities, which were considerably better than 23-88 % by Method 604 or 35-93 % by Methods 8040. This method gave 0.8-8.0 ppb of detection limit for water sample and 9-87 ppb soil. The problem of unresolved peaks or complete overlaps in the real sample analysis can be tackled by the chemometric analysis following full spectrum monitoring via a Diode Array Detector.