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Analysis of Phenol in Occupational Air Oxadiargyl in Plant and Soil Samples by Solid Phase Microextraction in Combination with Gas Chromatography-Mass Spectrometry

Bagherbejad, Masoud | 2011

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  1. Type of Document: M.Sc. Thesis
  2. Language: Farsi
  3. Document No: 42739 (03)
  4. University: Sharif University of Technology
  5. Department: Chemistry
  6. Advisor(s): Bagheri, Habib; Eshaghi, Ali
  7. Abstract:
  8. In this study different kinds of solid phase microextraction fibers based on sol-gel technology were employed for extraction and pre-concentration of phenol in occupational air and oxadiargyl in plant and environmental samples. In the first work, a SPME method followed by on-fiber derivatization and gas chromatography-mass spectrometry detection (GC-MS) was developed for the analysis of phenol in the air. The application and feasibility of three different sol-gel based SPME fibers with different polarities, polar and non-polar poly (dimethylsiloxane) (PDMS) and polyethylene glycol (PEG), have been studied. Influential parameters such as fiber coating type, type of derivatization reagent, derivatization time, volume, and temperature, extraction time and desorption parameters were investigated and optimized.Under the optimized conditions, a detection limit of 5 ngL-1 and RSD of 5% were obtained. Linear range was obtained in the range of 20 ngL-1 to 500 0gL-1 with correlation coefficient of 0.996. The optimized method was applied to sampling of phenol from the production area of tuberculin purified protein derivative of Razi Vaccine & Serum research institute. In the second work, first, new sol-gel based solid phase microextraction fibers were prepared on the stainless steel wire. For this purpose, the surface of stainless steel was modified initially with (3-mercaptopropyl) trimethoxy silane under determined conditions and was validated Using cyclic voltammetry and energy dispersive X-ray spectroscopy. After modifying the surface of stainless steel, four different sol-gel based SPME fibers with different polarities, polar and non-polar poly(dimethylsiloxane) (PDMS), polyethylene glycol (PEG), and UCON have been studied for determination of oxadiargyl in plant and environmental samples prior to gas chromatography- mass spectrometry determination. Most important parameters that affect the extraction efficiency were also studied. Under optimized condition, the proposed method was linear from 100ngL-1 to 2 mgL-1 with R2=0.997. LOD of 40 ngL-1 and RSD of fewer than 10% were acquired. Relative recovery in Paddy water, Rice, Lettuce, and soil samples matrices was investigated and were 95.49, 79.03, 70.41, and 73.15
  9. Keywords:
  10. Solid Phase Microextraction ; Gas Chromatography/Mass Spectrometry (GC/MS) ; Phenol ; Oxadiargyl ; On-Fiber Derivatization

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