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Detemination Of Trace Pollutant In Water By Three-phase Hollow Fiber Liquid-phase Microextraction Combined With High Performance Liquid Chromatography

Posted on:2013-06-24Degree:MasterType:Thesis
Country:ChinaCandidate:X W TanFull Text:PDF
GTID:2231330374963683Subject:Environmental Engineering
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The liquid phase microextraction is a new environment friendly sample pretreatment technique which integrates sampling extraction and concentration into one step. This novel technique has many advantages, such as, low-cost, farthing solvent consumption, convenience and high sensitivity. The technique can provide high enrichment factors and extraction recovery. At present, the hollow fiber LPME technique has been applied in environment analysis, biology and so on. This dissertation studies the followings:1. Detemination of trace bisphenol A by three-phase hollow fiber liquid-phase microextraction combined with high performance liquid chromatography. The experimental conditions of three-phase hollow fiber liquid-phase microextraction were optimized. The optimum extraction conditions were as follows:1-octanol was used as the extraction solvent, The concentration of NaOH solution as acceptor phase was0.09mol/L, the pH value of sample solution was4, the NaCl concentration was30g/L, the stirring rate was900r/min and the extraction time was60min. The calibration curves of BPA were obtained in the concentration ranges of0.5~200μg/L(r>0.999), RSD was lower than3.2%, The method under the optimal conditions, the detection limits (S/N=3) of BPA was0.2μg/L, the enrichment factor was241.12. The average recovery in BPA was in the ranges of92.8%-101.9%, This method proved to be a simple and accurate for the determination of trace amounts of BPA.2. Application of hollow fiber liquid-phase microextraction combined with high performance liquid chromatography on the determination of trace phenol in water was studied. The variable experimental conditions of three-phase hollow fiber liquid-phase microextraction were optimized, such as the nature of extraction solvent, the concentration of acceptor phase, the pH value of sample solution, salt concentration, stirring rate, extraction time. The ideal extraction conditions were identified. Under these conditions,the concentration factors for the phenol was253.7. The calibration curve of phenol was obtained in the concentration ranges of0.5~200μg/L(r>0.999), the detection limits (S/N=3) was0.2μg/L, RSD was4.2%. The average recovery for Huangpu river water sample which spiked with the standards at20μg/L was91.7%.3. In order to realize the selective extraction of BPA-Phenol mixture solution, the molecularly imprinted polymers are prepared, which was choosing bisphenol A as template molecule, methacrylic or acrylamide as functional monomers, N,N’-methylene-bis-acrylamide as cross-linker. Finally make sure that take MAA as functional monomers, MBA as cross-linker prepared the best molecularly imprinted polymer. The experimental carried out specific selective study on BPA-Phenol mixture solution. The results show that the best molecularly imprinted polymer with high selectivity for BPA-Phenol mixture solution.4. The experiment coated the hollow fiber by the best molecularly imprinted polymer. Application of these hollow fiber liquid-phase microextraction combined with high performance liquid chromatography on the determination of BPA-Phenol mixture solution in water. This method realize the selective extraction in BPA-Phenol mixture solution, but the results also show that the selective extraction should be improved from the enrichment factor and precision.
Keywords/Search Tags:Hollow fiber, Three-phase liquid-phase microextraction, High performanceliquid chromatography, Bisphenol A, Molecularly imprinted polymers, Selective extraction
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