| 研究生: |
楊竣富 Yang, Jyun-Fu |
|---|---|
| 論文名稱: |
分析底泥中多環芳香烴前處理方法之研究 Study of Pretreatment Method for Determination of Polycyclic Aromatic Hydrocarbons in Sediments |
| 指導教授: |
桂椿雄
Kuei, Chun-Hsiung |
| 學位類別: |
碩士 Master |
| 系所名稱: |
理學院 - 化學系 Department of Chemistry |
| 論文出版年: | 2014 |
| 畢業學年度: | 102 |
| 語文別: | 中文 |
| 論文頁數: | 106 |
| 中文關鍵詞: | 多環芳香烴 、底泥 、熟化 、前處理方法 、加壓流體萃取 |
| 外文關鍵詞: | Polycyclic aromatic hydrocarbons, Sediments, Ageing, Pretreatment method, Pressurized fluid extraction |
| 相關次數: | 點閱:70 下載:1 |
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本研究的前處理方法利用甲苯/甲醇(9/1 ,v/v)萃取底泥中16項多環芳香烴,在 100℃下萃取三次各10分鐘,再以矽膠管柱淨化,濃縮後完成檢液製備,續以氣相層析質譜儀分析,以分析標準參考物質1941b來驗證方法,naphthalene、fluorene、dibenz[a,h]anthracene的平均回收率分別是41.9%、55.4%、206.2%,其他10項多環芳香烴的平均回收率在72.9-113.2%。以相同溶劑組成及相同淨化步驟,比較本研究前處理方法與加壓流體萃取方法的差異,兩種方法中低分子量的多環芳香烴回收率差異小,而加壓流體萃取設備提供較高的萃取溫度,因此加壓流體萃取方法對於高分子量多環芳香烴的回收率較高,再以標準參考物質為樣品來比較本研究前處理方法與索氏萃取方法及本研究前處理方法與QuEChERS方法之差異,對於高分子多環芳香烴,本研究前處理方法比索氏萃取方法有較好的回收率,對於低分子量多環芳香烴的回收率較索氏萃取方法低,而QuEChERS方法對於多環芳香烴的回收率皆低於本研究前處理方法。此外,文中探討添加多環芳香烴標準品至底泥樣品的熟化時間對回收率的影響,結果顯示熟化一天、十天與二十天的回收率差異小,其原因可能是熟化一天後達飽和吸附量所導致。本研究前處理方法有效、便宜、可同時處理數個樣品、萃取時間小於索式萃取及溶劑耗費少的優點,具有潛力來取代傳統的前處理方法。
In this study, a simplified pretreatment method which can extract polycyclic aromatic hydrocarbons(PAHs) form contaminated sediments was developed. The PAHs were extracted 3 times with toluene/methanol (9/1, v/v) at 100℃, and sample extracts were cleaned up by silica gel. After clean-up and concentration, sample extracts were analyzed by gas chromatography coupled with mass spectrometer. The accuracy was evaluated by the standard reference material. The average recoveries of PAHs were 72.9~113.2% (except those of naphthalene, fluorene and dibenz[a,h]anthracene were 41.9%, 55.4% and 206.2%, respectively). The simplified pretreatment method were compared with pressurized fluid extraction method by recoveries of PAHs. The recoveries of low molecular weight PAHs are not obviously different. For high molecular weight PAHs, the recoveries resulted from the pressurized fluid extraction were higher. Furthermore, the different analytical method were be compared. For high molecular weight PAHs, the recoveries of simplified pretreatment method were higher and more reasonable than that of soxhlet method. The recoveries of low molecular weight PAHs resulted from simplified pretreatment method were lower. The recoveries of PAHs resulted from QuEChERS was obviously lower than that of the simplified pretreatment method. Moreover, the relationship between the recovery of PAHs and the ageing time of the spiked sample was discussed. The minor difference in recoveries resulted from different aging time. The simplified pretreatment method is fast, cheap, simplified and effective. It has potential to replace traditional pretreatment method in the future.
[1] E.J. Kim, Effects of forest fire on the level and distribution of PCDD/Fs and PAHs in soil, The Science of the Total Environment, vol.311, p.177-189(2003).
[2] B.A.M. Bandowe, Polycyclic aromatic hydrocarbons(PAHs) and their oxygen-containing derivatives(OPAHs) in soils from the Angren industrial area, Uzbekistan, Environmental Pollution, vol.158, p.2888-2899(2010).
[3] A.L.C. Lima, Combustion-derived polycyclic aromatic hydrocarbons in the environment—a review, Environmental Forensics, vol.6, p.109-131(2005).
[4] J.H. Christensen, A novel approach for characterization of polycyclic aromatic hydrocarbon (PAH) pollution patterns in sediments from Guanabara Bay, Rio de Janeiro, Brazil, Environmental Pollution, vol.158, p.3290-3297(2010).
[5] W.L. Xue, Metabolic activation of polycyclic and heterocyclic aromatic hydrocarbons and DNA damage: a review, Toxicology and Applied Pharmacology, vol.206, p.73–93(2005).
[6] W.B. Jensen, The origin of the soxhlet extractor, Journal of Chemical Education, vol.84(2007).
[7] B.E. Richter, An accelerated solvent extraction system for the rapid preparation of environmental organic compounds in soil’, American Laboratory, vol.27, p.24-28 (1995).
[8] B.E. Richter, Accelerated solvent extraction: a technique for sample preparation, Analytical Chemisry, vol.68, p.1033-1039(1996).
[9] B. Kaufmann, Recent extraction techniques for natural products microwave-assisted extraction and pressurized solvent extraction, Phytochemical Analysis, vol.13, p.105–113(2002).
[10] M. Anastassiades, Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce, Journal of AOAC international, vol.86, p.412-431(2003).
[11] 去硫淨化法(NIEA M816.01c),行政院環境保護署環境檢驗所,台灣,頁 1-6(2013)。
[12] N. Barco-Bonilla, Comparison of ultrasonic and pressurized liquid extraction for the analysis of polycyclic aromatic compounds in soil samples by gas chromatography coupled to tandem mass spectrometry, Talanta, vol.78, p.156–164(2009).
[13] S.B. Hawthorne, Comparisons of soxhlet extraction, pressurized liquid extraction, supercritical fluid extraction and subcritical water extraction for environmental solids: recovery, selectivity and effects on sample matrix, Journal of Chromatography A, vol.892, p.421– 433(2000).
[14] S. Lundstedt, Simultaneous extraction and fractionation of polycyclic aromatic hydrocarbons and their oxygenated derivatives in soil using selective pressurized liquid extraction, Analytical Chemisry, vol.78, p.2993-3000(2006).
[15] M. Choi, Development of a one-step integrated pressurized liquid extractionand cleanup method for determining polycyclic aromatichydrocarbons in marine sediments, Journal of Chromatography A, vol.1340, p.8–14(2014).
[16] J.A. Padilla-Sánchez, Application of a quick, easy, cheap, effective, rugged and safe-based method for the simultaneous extraction of chlorophenols, alkylphenols, nitrophenols and cresols in agricultural soils, analyzed by using gas chromatography–triple quadrupole-mass spectrometry/mass spectrometry, Journal of Chromatography A, vol.1217, p.5724–5731(2010).
[17] M.V. Salvia, Development of a multi-residue method using acetonitrile-based extraction followed by liquid chromatography–tandem mass spectrometry for the analysis of steroids and veterinary and human drugs at trace levels in soil, Journal of Chromatography A, vol.1245, p.122–133(2012).
[18] A. Rashid, Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soil using gas chromatography–tandem mass spectrometry, Journal of Chromatography A, vol.1217, p.2933–2939(2010).
[19] N.D. Forsberg, Determination of parent and substituted polycyclic aromatic hydrocarbons in high-fat salmon using a modified QuEChERS extraction, dispersive SPE and GC-MS, Journal of Agricultural and Food Chemistry, vol.59, p.8108-8116(2011).
[20] S.L. Zhao, Screening PAHs in soil using RTL database with sampliQ QuEChERS extraction kits and agilent 5975T LTM GC/MS, Agilent technologies Inc., USA, p.1-7(2010).
[21] A. Albinet, A really quick easy cheap effective rugged and safe (QuEChERS) extraction procedure for the analysis of particle-bound PAHs in ambient air and emission samples, Science of the Total Environment, vol.450–451, p.31–38(2013).
[22] V. Camel, Influence of ageing on the supercritical fluid extraction of pollutants in soils, Journal of Chromatography A, vol.693, p.101-111(1995).
[23] 半揮發性有機物檢測方法─毛細管柱氣相層析質譜儀法(NIEA M731.01c),行政院環境保護署環境檢驗所,台灣,頁1-52(2012)。
[24] 環境檢驗檢量線製備及查核指引(NIEA-PA103),行政院環境保護署環境檢驗所,台灣,頁1-6(1995)。
[25] M.C. Olson, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory—determination of polycyclic aromatic hydrocarbon compounds in sediment by gas chromatography/mass spectrometry ,U.S. Geological Survey, USA, p.1-32(2004).
[26] 底泥品質指標項目低濃度限值檢測技術建立及調查,行政院環境保護署環境檢驗所,台灣,頁1-361(2013)。