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Title 油污染鑑識新檢測技術建立及應用（2/2）
Abstract GC-FID或GC-MS等一維氣相層析方法對於樣品分析解析度與峰容量有其極限，當樣品組成複雜時，例如分析油品，在其解析分離過程中，會產生共沖提現象。為了克服此共沖提問題，二維氣相層析技術的提出，利用了兩根極性或性質不同的管柱，有效的解決了對於過去分離複雜樣品所產生共沖提的問題。本計畫進行油污染鑑識之全面型二維氣相層析技術建立研發之GCxGC-TOFMS油品分析技術的建立部分，藉由質譜儀協助GCxGC分析生物標誌物鑑識並進行其鑑識適用可行性探討。本報告完成二維氣相層析質譜儀及相關油污染指紋鑑識文獻資料蒐集彙整研析，共計20篇，並彙整國內外漏油污染指紋鑑識資料與和技術報告，完成「漏油污染鑑識指引及案例評析技術手冊-化學特徵鑑識技術（草案）」之撰寫工作。在GCxGC-TOFMS油品上機分析條件建立方面，運用98年度環檢所委辦計畫中提供的2個進口原油樣品及4個柴油樣品，根據GCxGC-TOFMS分析條件建立，包括上機分析條件、儀器線性分析與精確度（再現性分析）項目，建立上機分析條件。利用NIST資料庫比對GCxGC-TOFMS圖譜，加上標準品確認與相關文獻報告圖譜比對，建立GCxGC-TOFMS分析原油及柴油之TIC及不同生物標誌物指紋圖譜。運用由98年度已建立完整GC-MS生物標誌物分析結果具差異性與關聯性的2個原油樣品，藉由GC-MS分析與GCxGC-TOFMS分析之指紋圖譜分布模式和診斷比值計算，完成GCxGC-TOFMS油污染鑑識適用性探討。進一步利用具來源特性差異的8個原油樣品，進行建立之GCxGC-TOFMS分析技術適用性驗證。分析結果顯示，GCxGC-TOFMS分析與GC-MS分析皆獲得類似的指紋圖譜，藉由樣品碳數分布、具來源特性與生成特性的生物標誌物及診斷比值可鑑別不同地區原油樣品。由於GC-MS與GCxGC-TOFMS儀器性質的差異性，因此分析所計算的診斷比值亦有所差異，此乃分析技術特性所致，唯皆可達到區分來源特性異同目標，結果驗證GCxGC-TOFMS分析技術之適用性。本計畫將已建立的GCxGC-TOFMS分析技術應用於2件現地漏油場址案例，其具有區分不同油品類型的能力。對於組成較複雜（例如原油）或生物標誌物含量較低樣品，使用GC-MS與GCxGC-TOFMS分析顯示，GCxGC-TOFMS具有較好的分離效果與降低共沖提效應，尤其是對於油樣品之烷基PAHs指紋圖譜，可針對特定斷裂碎片離子層析圖掃描，去除干擾化合物，具有提高分辨率、靈敏度及族群分離效應的強大優點。
EngTitle Establishment and Application of New Measuring Technology for Oil Pollution Identification（2/2）
EngAbstract One-dimensional gas chromatography method such as GC-FID or GC-MS for the analysis of samples resolution and peak capacity has its limits; especially for the unresolved complex mixtures (UCMs). For example, the co-elution phenomenon has occurredduring the oil analysis resolution separation process. Two-dimensional gas chromatography technique is proposed by using the two different polar or property columns to overcome the co-elution problem. This project is to establish and develop the comprehensive GCGC-TOFMS techniques and employ mass spectrometer assist GC for forensic analysis of biomarkers and their forensic applicable feasibility investigation. The report has collected 20 literature surveys of a two-dimensional gas chromatography mass spectrometry and related oil pollution fingerprint forensic data, meanwhile, converge domestic and international oil pollution aggregated data and fingerprint forensic and technical reports, and completes the [Oil pollution forensic guidelines and case analysis - chemical characteristics of forensic Technical Manual (Draft)]. On the side of GCGC-TOFMS analysis conditions established, applied 2 imported samples of crude oil and 4 diesel samples provided by EAL’s 98s project to establish analytical conditions, instrument linear analysis, and precision (reproducibility analysis). The biomarker fingerprint and TIC of crude oil and diesel fuel have established by utilizing NIST database compared with TOFMS spectrum and standard spectra with relevant literatures.The GCxGC-TOFMS oil pollution forensic applicability investigation has completed by calculate the ratio of the sum of the diagnosis which is provided by GC-MS biomarker resultsfrom differentiation and association of 2 crude oil samples (established by 98ys). In order to build an applicability GCxGC-TOFMS analysis verified, the differentiation of 8 crude oil samples had compared. The analytic results indicate that GCxGC-TOFMS and GC-MS present similar fingerprint, which mean the samples can be identified by carbon number distribution, biomarkers and diagnostic odds with the source characteristics and formation characteristics. The calculated rations of diagnosis are presented differences as the differentiation of instrument properties between GC-MS and GCxGC-TOFMS. However, the source characteristic can be recognized by both MS. It shows that the GCxGC-TOFMS analysis is an applicability of analytic technology. The GCxGC-TOFMS analysis technique has been proved the ability to distinguish between different types of oil from two real oil pollution cases.The GCxGC-TOFMS has better separation factor and less co-elution phenomenon compare with GC-MS under more complex composition (such as crude oil), or a low content of biomarker samples conditions. Particularly for alkyl PAHs fingerprint sample, the GCxGC-TOFMS has given high distinguish, selectivity and separation of interfering compounds.
ProjectYear 103
SponsorOrg 環檢所
ExecutingOrg 工業技術研究院
PublicFullVersionURL http://epq.epa.gov.tw/project/filedownload.aspx?fid=73626