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Novel Unbreakable Solid Phase Microextraction Fibers by Electrodepositon of Silica Sol-Gel

Sistani, Habiballah | 2009

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  1. Type of Document: M.Sc. Thesis
  2. Language: Farsi
  3. Document No: 41485 (03)
  4. University: Sharif University of Technology
  5. Department: Chemistry
  6. Advisor(s): Bagheri, Habib
  7. Abstract:
  8. Commercial solid phase microextraction fibers posses a few drawbacks such as relatively low recommended operating temperature, instability and swelling in organic solvents, breakage of the fiber, stripping of coatings, and bending of the needle. Some of these problems have been obviated by covalent bonding of the polymer phase to the fused-silica substrate by sol-gel technology, but the easy breakage of the fiber remains a problem. In this study a new technique for preparation of unbreakable, thin and very porous fiber coatings for solid phase microextraction was proposed. In this technique firstly an intermediate film consisting of an ultrathin two-dimensional polymer was prepared by hydrolysis of a (3-mercaptopropyl) trimethoxysilane (ethanol, 10-3 M) self-assembled monolayer grafted onto gold, and then a stationary phase by electrodepositioning of poly ethylene glycol was produced. The prepared fiber coating was used for solid phase microextraction of four selected Poly Aromatic Hydrocarbons (PAHs) were subsequently analyzed by GC-MS. The parameters that affect the extraction procedure have been optimized. The optimized parameters were: extractio temperature: 50°C, extraction time: 20 min, salt (NaCl) concentration: 15% desorption temperature: 200°C, desorption time: 5 min. The Limit of Detection (LOD) and Relative Standard Deviation (RSD) values for PAHs by this sorbent were between 10 - 20 pg/mL and 4.2 – 16.3% at 1 ng/mL, respectively
  9. Keywords:
  10. Sol-Gel Method ; Polynuclear Aromatic Hydrocarbons (PAHs) ; Gas Chromatography ; Gas Chromatography/Mass Spectrometry (GC/MS) ; Solid Phase Microextraction Based on Metal

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