簡易檢索 / 詳目顯示

回結果列表
研究生： 郭鉑漳
論文名稱： 建立超音波震盪固相微萃取自動化分析系統及水中揮發性有機化合物之現場自動化即時監測
Development of Ultrasonication coupled Autosampler HS SPME/GC/FID And In-situ Automatic Real Time Monitoring of VOCs
指導教授： 羅俊光
吳劍侯
口試委員:
學位類別： 碩士
Master
系所名稱： 原子科學院 - 生醫工程與環境科學系
Department of Biomedical Engineering and Environmental Sciences
論文出版年： 2004
畢業學年度： 92
語文別： 中文
論文頁數： 87
中文關鍵詞： 超音波震盪 、即時監測 、揮發性有機化合物
相關次數： 點閱：2  下載：0 
分享至:
查詢本校圖書館目錄 查詢臺灣博碩士論文知識加值系統 勘誤回報

    • 本研究為建立連續進樣搭配超音波前處理技術自動化分析系統，針對高科技廠業污水中常見的揮發性有機物(VOCs)的分析，分析的有機物分別為Acetone、IPA、DMS、MTBE、EA(ethyl acetate)、BA、THF、PGMEA、2-Butanol。
    本分析系統的檢量線線性良好其RSD(%)皆小於15%，精密度與回收率皆在法規規定內，方法偵測極限在3.19ppb~7.57ppb。為了使頂空固相微萃取更有效的進行分析及縮短分析時間，因此便以現場即時監測為發展方向，進而將儀器移至污水處理場進行連續進樣自動化分析。
    本研究並將所建立分析系統置於污水廠放流口進行分析，分析時間為5月25日晚間十點至5月28日上，由分析結果可以建立偵測物種隨時間變化的趨勢圖，而污水廠放流口最主要排放至環境水體的物種為二甲基硫(DMS)與丙酮(Acetone)，在量測期間並無量測到異丙醇(IPA)，有可能在處理廠內各單元處理已將之處理掉。量測期間污水廠的放流水量為18141m3/day，因此可推估於此段期間DMS排放4.3kg，Acetone排放19kg至環境水體中。且可藉由濃度變化趨勢圖評估污水處理廠處理成效。

    In this study, an in-situ continuous measuring sonicator pre-treatment coupled autosampler HS-SPME GC/FID system is used to analyze 9 VOCs -MTBE, DMS, Acetone, THF, EA, 2-Butanol, IPA, BA and PGMEA in industrial wastewater. Perior calibration of the system exhibited good linearity with RSD less than 15%, recovery of 90% ~ 110%, precision 6.5% ~ 11.5%, and MDL in the range 3.19ppb ~ 7.57ppb.
    On site real sample continuous analysis from a treatment plant in two different sampling campaigns (25-28 May and 15-17 June 2004) showed that acetone and DMS were dominant pollutants in the first measuring campaign while acetone, DMS, IPA, THF, BA and 2-Butanol were major pollutants in second campaign. The estimated VOCs in the effluent were acetone-19kg/day and DMS-4.3kg/day in the first measuring campaign while DMS-3.1kg/day, acetone-17.6kg/day, THF-230g/day, 2-Butanol-320g/day, IPA-1kg/day and BA-330g/day were estimated in second campaign.

    摘要-----------------------------------------------------------------------i 英文摘要(Abstract)----------------------------------------------------ii 誌謝----------------------------------------------------------------------v 總目錄------------------------------------------------------------------iii 圖目錄------------------------------------------------------------------vi 表目錄------------------------------------------------------------------ix 第一章 緒論-----------------------------------------------------------1 1-1 緣起---------------------------------------------------------------------1 1-2 目的---------------------------------------------------------------------2 1-3 方法---------------------------------------------------------------------3 第二章 文獻回顧-----------------------------------------------------5 2-1 固相微萃取(SPME)方法概要------------------------------------------5 2-1-1 固相微萃取原理---------------------------------------------------------6 2-1-2 固相微萃取參數探討---------------------------------------------------9 2-2 SPME的應用-------------------------------------------------------------17 2-3 水中VOCs與環境之間的關係----------------------------------------18 第三章 研究方法-------------------------------------------------26 3-1 超音波震盪前處理系統建立-------------------------------------------27 3-2 超音波震盪-自動化頂空-固相微萃取/氣相層析儀系統說明----28 3-2-1 分析儀器與設備-------------------------------------------------------28 3-2-2 分析目標化合物性質-------------------------------------------------29 3-2-3 實驗標準試劑-------------------------------------------------------29 3-2-4 品保品管-------------------------------------------------------31 3-2-5 分析樣品應注意事項-------------------------------------------------33 3-3 HS-SPME/GC/FID系統最佳化參數探討與測試-------------------33 3-4 玻璃器皿管理-----------------------------------------------------36 3-5 真實樣品採樣及規劃----------------------------------------------------37 3-5-1 真實樣品採樣實驗室進行分析-------------------------------------37 3-5-2 污水處理廠自動化連續監測部分----------------------------------38 第四章 結果與討論-------------------------------------------------45 4-1 超音波震盪-自動化頂空固相微萃取系統---------------------45 4-1-1 超音波震盪片安裝及可行性和不同功率測試-------------------45 4-1-2 超音波震盪槽與GC/FID的聯接---------------------------------46 4-2 HS-SPME/GC/FID系統最佳化參數探討與測試-------------------46 4-3 真實樣品量測的結果與討論-------------------------------------------51 4-4 自動化連續進樣即時監測----------------------------------------------52 4-4-1 5/25至5/26連續24小時進樣量測---------------------------------52 4-4-2 5/26至5/27連續24小時進樣量測--------------------------------53 4-4-3 5/27晚上11點14分至5/28早上9點20分連續進樣量測----53 4-4-4 連續進樣自動化即時監測結論-------------------------------------54 4-4-5 6/15 ~ 6/17 連續進樣量測-------------------------------------------55 第五章 結論---------------------------------------------------------85 5-1 結論-----------------------------------------------------------------------85 5-2 未來展望-----------------------------------------------------------------87 參考文獻---------------------------------------------------------------xi

    1. Magdalena Ligor, Boguslaw Buszewski,“Determination of menthol and menthone in food and pharmaceutical products by solid-phase microextraction–gas chromatography”Journal of Chromatography A, 847,161-169(1999)
    2. Beatriz Cancho, Francesc Ventura, M Teresa Galceran,“Determination of aldehydes in drinking water using pentafluorobenzylhydroxylamine derivatization and solid-phase microextraction”Journal of Chromatography A, 43,1-13(2001)
    3. Watson Susan B., Brian Brownlee, Trevor Satchwill, Erika E. Hargesheimer,“Quantitative analysis of trace levels of geosmin and MIB in source and drinking water using headspace SPME”Water Research Vol.34,2818-2828(2000)
    4. Page B. Denis, Gladys Lacroix,“Application of solid-phase microextraction to the headspace gas chromatographic analysis of semi-volatile organochlorine contaminants in aqueous matrices”Journal of Chromatography A, 757, 173-182(1997)
    5. Neppolian B., Haeryong Jung, Heechul Choi, Jai H. Lee, Joon-Wun Kang,“Sonolytic degradation of methyl tert-butyl ether: the role of coupled fenton process and persulphate ion”Water Research Vol.36,4699-4708(2002)
    6. Patrick Roose, Udo A.Th. Brinkman, “Determination of volatile organic compounds in marine biota”Journal of Chromatography A, 799,233-248(1998)
    7. Wheat P.E., M.A. Tumeo,“Ultrasound induced aqueous polycyclic aromatic hydrocarbon reactivity”Ultrasonics Sonochemistry ,4 , 55-59(1997)
    8. Anton Gáplovský, Jana Donovalová, Štefan Toma, Robert Kubinec,“Ultrasound effects on photochemical reactions, Part 1: photochemical reactions of ketones with alkenes”Ultrasonics Sonochemistry ,4 , 109-115(1997)
    9. 林瑞聰，“惡臭污染防治”，環保資訊雜誌第6期，PP.14~15，1993。
    10. 劉國棟，“VOC管制趨勢展望”，工業污染防治，第48期，PP15-31，1993。
    11. Aaron L. Theis, Adam J. Waldack, Susan M. Hansen, Michael A. Jeannot,“Headspace Solvent Microextraction”Anal. Chem.,73, 5651-5654 (2001)
    12. Buchholz K. D. and J. Pawliszyn,“Determination of phenols by solid-phase microextraction and gas chromatographic analysis”Environ. Sci. Technol., 27, 2844 (1993).
    13. Pawliszyn,“Solid phase microextraction with thermal desorption using fused silica optical fibers”Anal. Chem., 62, 2145 (1990).
    14. Application Note of Supelco, “Solid Phase Microexaction:Theory and Optimization of Conditions”, Bulletin 923, Supelco.
    15. 黃敬德、謝有容，”固相微萃取技術之原理及其應用”，Chemistry, Dec.,(1998).
    16. J.Pawliszyn,“Solid Phase Microextraction：Theory and Practice”,Wiley-Vch, Inc.(1997)
    17. J.Pawliszyn,“Application of Solid Phase Microextraction”,RS.C, Inc.(1999)
    18. Application Note of Supelco, “SPME Application Guide”, Bulletin 925, Supelco.
    19. David. W. Potter and J. Pawliszyn,“Rapid determination of polyaromatic hydrocarbons and polychlorinated biphenyls in water using solid-phase microextraction and GC/MS”Environ. Sci. Technol., 28, 298 (1994).
    20. Homepage of Sigma-Aldrich Corporation, Supelco Group, “Product Information of SPME”, http://www.sigma-aldrich.com
    21. R. Eisert and K. Levsen, “Review – Solid Phase Microexaction Coupled to Gas Chromatography : A New Method for the Analysis of Organics in Water”, Journal of Chromatography A, 733,143-157(1996).
    22. J. L. Schnoor, “Environmental Modeling – Fate and Transport of Pollutants in Water, Air and soil”, John Wiley & Sons Inc., pp.42~51, 328-331(1996).
    23. C. Rivasseau and M. Caude, “Comparison of On-Line SPE-HPLC and SPME-GC for the Analysis of Microcontaminants in Water”, Chromatographia, Vol.41, pp.462-470 (1995)
    24. Application Note of Supelco, “Optimizing SPME : Parameters to Control to Ensure Consistent Results”, Note 95, Supelco.
    25. Z. Zhang and J. Pawliszyn, “Sampling Volatile Organic Compounds Using a Modified Solid Phase Microextraction Device” Journal of High Resolution Chromatography, 19,155-160 (1996)
    26. A. Saraullo, P. A. Martos and J. Pawliszyn, “Water Analysis by Solid Phase Microextraction Based on Physical Chemical Properties of the Coating”, Analytical Chemistry, 69, pp.1992-1998 (1997)
    27. 新竹科學工業園區管理局首頁，http://www.sipa.gov.tw
    28. Homepage of Varian Instrument Corporation, “Automation of the SPME Devices”, http://www.varian.com
    29. 陸志德，羅俊光，“高科技產業相關水體中揮發性有機物分析之研究”，國立清華大學碩士論文 (2000)
    30. 許慧萍，羅俊光，“環境水體中揮發性有機化合物分析方法建立與驗證”，國立清華大學碩士論文 (2001)
    31. Ashish Bhatnager and H. Mlchael Cheung,“Sonochemical Destruction of Chlorinated C1 and C2 Volatile Organic Compounds in Dilute Aqueous Solution” Environ. Sci. Technol.,28 , 1481-1486 (1994)
    32. Carvalho L.R.F, S.R. Souza, B.S. Martinis, M. Korn,“Monitoring of the ultrasonic irradiation effect on the extraction of airborne particulate matter by ion chromatography”Analytica Chimica Acta, 317 , 171-179 (1995)
    33. Wen Lai Huang, Kai Ming Liang, Shi Hua Cui, Shou Ren Gu,“Influene of ultrasonic vibration on the mesoporosity and surface fractal dimensions of resultant silica xerogels”Materials Research Bulletin, 36 , 461-470 (2001)
    34. Maria S. Kuyukina, Irena B. Ivshina, Jim C. Philp, Nick Christofi, Sandra A. Dunbar, Marina I. Ritchkova,“Recovery of Rhodococcus biosurfactants using methyl tertiary-butyl ether extraction”Journal of Microbiological Methods, 46 , 149-156 (2001)
    35. Michael R. Hoffmann,“Kinetic and Mechanism of the Sonolytic Destruction of Methyl tert-Butyl Ether by Ultrasonic Irradiation in the Presence of Ozone” Environ. Sci. Technol.,32 ,3194-3199 (1998)
    36. Inez Hua and Michael R. Hoffmann,“Optimization of Ultrasonic Irradiation as an Advanced Oxidation Technology” Environ. Sci. Technol.,31 ,2237-2243 (1997)
    37. Joon-Wun Kang, Hui-Ming Hung, Angela Lin and Michael R. Hoffmann,“Sonolytic Destruction of Methyl tert-Butyl Ether by Ultrasonic Irradiation: The Role of O3 H2O2 Frequency and Power Density” Environ. Sci. Technol.,33 , 3199-3205 (1999)
    38. Lingshuang Cai, Jun Xing, Li Dong, Caiying Wu,“Application of polyphenylmethylsiloxane coated fiber for solid-phase microextraction combined with microwave-assisted extraction for the determination of organochlorine pesticides in Chinese teas”Journal of Chromatography A,1015 ,11-21 (2003)
    39. Sandra Babic, Mira Petrovic, Marija Kastelan-Macan,“Ultrasonic solvent extraction of pesticides from soil”Journal of Chromatography A,823 ,3-9 (1998)
    40. Gokhan Savaroglu, Ertunc Aral,“Ultrasonic Velocity and Isentropic Compressibilities of the Ternary Mixture Benzene + Acetone + Chloroform and their Corresponding Binary Mixtures at 298.15K”Journal of Molecular Liquids, 105 ,79-92 (2003)
    41. Lowri S. de Jager, Anthony R.J. Andrews,“Development of a screening method for cocaine and cocaine metabolites in urine using solvent microextraction in conjunction with gas chromatography”Journal of Chromatography A,911 ,97-105 (2001)
    42. Elefteria Psillakis, Nicolas Kalogerakis,“Application of solvent microextraction to the analysis of nitroaromatic explosives in water samples”Journal of Chromatography A,907 ,211-219 (2001)
    43. Guillard C., P. Theron, P. Pichat, C. Petrier,“Evaluation of 1-octanol degradation by photocatalysis and ultrasound using SPME” Water Research,36 ,4263-4272 (2002)
    44. Gyorgy Szo llo si , Istvan Kun, Bela Torok, Mihaly Bartok, “Ultrasonics in chemoselective heterogeneous metal catalysis Sonochemical hydrogenation of unsaturated carbonyl compounds over platinum catalysts” Ultrasonics Sochemistry,7 ,173-176 (2000)

    無法下載圖示 全文公開日期 本全文未授權公開 (校內網路)
    全文公開日期 本全文未授權公開 (校外網路)

    QR CODE