Polymer monolithic columns with I.D. between 100 and 320m were prepared by in-situ polymerization of styrene and divinylbenzene in fused silica capillaries. The effects of monolithic column I.D. on the separation of proteins in reversed-phase capillary-liquid chromatography under gradient elution were systemically studied. The loading capacity was positively proportional to the volume of the stationary phase. It was found that the smaller diameter columns showed better performance for protein separation. The minimum plate height decreases from 34.99m (320m I.D. column) to 5.39m (100m I.D. column) for a retained protein. After studying the three parameters of the Van Deemter equation, it was interpreted that the smaller diameter can provide less flow resistance and the better performance may also be improved by the increasing of the effective diffusion. This conclusion was also supported by the data of separation permeability and breakthrough curves.

The high energy cost of an electrochemical method is the fatal drawback that hinders its large scale application in wastewater treatment. In traditional single-chamber electrolysis cell, only direct oxidation at an anode exists. Although a small amount of hydrogen peroxide is produced at the cathode by reduction, it is transferred to the anode and destroyed there without adding much benefit to organic decomposition. A two-chamber electrolytic cell, connected with an electrolyte bridge, was developed in this work. In this new reactor, direct oxidation at anode and indirect oxidation by hydrogen peroxide at cathode can occur simultaneously. Therefore "dual electrodes oxidation" in one electrochemical reactor was achieved successfully. Compared to a traditional one cell reactor, this reactor cuts the energy cost by 50%, and thus might lead to reconsideration of the electrochemical role in wastewater treatment. A Pt/C gas diffusion electrode (GDE) is fabricated and used as a cathode fed with oxygencontaining gases to produce hydrogen peroxide. When purified air diffuses through the active layer on the GDE, oxygen is reduced to hydrogen peroxide with a high yield to decompose organics. It has been found that the direct oxidation process at an anodic zone is slightly affected by factors such as pH variation, Fe (Ⅱ) existence and aeration, while indirect oxidation at the cathodic zone is strongly affected. Dye used as a model pollutant was oxidized into small organic acids in both anode and cathode regions in this electrolytic reactor. GC-MS and IR spectrum were employed to analyze the intermediates formed during the degradation. Twenty intermediates have been detected, including 14 esters, 3 acids and 3 compounds with NO2 or N-OH groups. Thereafter, the degradation pathways of dye Acid Red B are proposed.

A surfactant-bound monolithic stationary phase based on the co-polymerization of 11-acrylaminoundecanoic acid (AAUA) is designed for capillary high performance liquid chromatography (HPLC). Using D-optimal design, the effect of the polymerization mixture (concentrations of monomer, crosslinker and porogens) on the chromatographic performance (resolution and analysis time) of the AAUA-EDMA monolithic column was evaluated. The polymerization mixture was optimized using three proteins as model test solutes. The D-optimal design indicates a strong dependence of chromatographic parameters on the concentration of porogens (1, 4-butanediol and water) in the polymerization mixture. Optimized solutions for fast separation and high resolution separation, respectively, were obtained using the proposed multivariate optimization. Differences less than 6.8% between the predicted and the experimental values in terms of resolution and retention time indeed confirmed that the proposed approach is practical. Using the optimized column, fast separation of proteins could be obtained in 2.5min, and a tryptic digest of myoglobin was successfully separated on the high resolution column. The physical properties (i.e., morphology, porosity and permeability) of the optimized monolithic column were thoroughly investigated. It appears that this surfactant-bound monolith may have a great potential as a new generation of capillary HPLC stationary phase.

Electrosorption-enhanced solid-phase microextraction (EE-SPME) based on activated carbon fiber (ACF) was developed for determination of aniline in aqueous solution. A porous ACF, served as working electrode in electrosorption procedure, was prepared and attached to a commercial manual SPME device. Parameters affecting the adsorption efficiency were investigated. Under optimized condition, whichwas 400mVelectrosorption potential, 0.01M Na2SO4 electrolyte, pH 7, and electrosorption at 40℃ for 10min, the method exhibited wide linear range (0.1-100gL−1, R2=0.9980), good repeatability of adsorption (RSD 6.15%, n=6), and low detection limit (0.02 gL−1). The feasibility of the method was evaluated by analyzing lake water spiked with aniline. Comparison was made with direct immersion (DI) ACF-SPME without electrosorption enhancement. The proposed procedure was demonstrated to be a simple, fast, sensitive sample preparation method for determination of aniline in water samples.

A bio-anode reactor and a bio-cathode reactor were developed to investigate the microenvironments around anodes and cathodes and their effects on denitrification. With an applied current of 40mA, the oxidation-reduction potentials (ORPs) in the bio-cathode and bio-anode reactors were 100-200 mV lower and 50mV higher, respectively, than that in the control reactor (a normal bio-reactor). The cathode reaction enhanced denitrification and the anode reaction inhibited denitrification. At 40 mA, the denitrification rate in the bio-cathode reactor was 55.1% higher than that in the control reactor. At 75mA, the denitrification rate in the bio-anode reactor was just 33.5% of that in control reactor. Electric current of less than 20mA had no effect on the most probable number (MPN) of denitrifiers, but at 75mA, the MPN of denitrifiers decreased by 90% in the bio-anode reactor. In the bio-cathode reactor, the MPN of denitrifiers increased more than 100% for the lower ORP environment produced by a cathode reaction at 75mA.