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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
1

UV Laser and LED Induced Fluorescence Spectroscopy for Detection of Trace Amounts of Organics in Drinking Water and Water Sources

Sharikova, Anna V 21 May 2009 (has links)
A UV Laser Induced Fluorescence (LIF) system, previously developed in our laboratory, was modified and used for a series of applications related to the development and optimization of UV LIF spectroscopic measurements of trace contaminants in drinking water and other water sources. Fluorescence spectra of a number of water samples were studied, including those related to the reverse osmosis water treatment and membrane fouling, domestic and international drinking water, industrial toxins, bacterial spores, as well as several fluorescence standards. Of importance was that the long term detection of the trace level of Dissolved Organic Compounds (DOC) was measured, for the first time to our knowledge, over a one week period and with a time resolution of 2.5 minutes. A comparison of LIF emission using both 266 nm and 355 nm excitation was also made for the first time. Such real-time and continuous measurements are important for future water treatment control. The LIF system was modified to accommodate UV Light Emitting Diodes (LED) as alternative excitation sources, and tested for the detection of trace organic species in water. In addition, a compact system using LED excitation and a spectrometer was xviii developed and underwent initial testing. The original LIF system had two laser sources, 266 nm and 355 nm. The additional sources incorporated in the system were UV LEDs emitting at 265 nm, 300 nm, 335 nm and 355 nm. The LED spectral emission was studied in detail, in terms of spectral variability and power output. It was found that all LEDs had some emission in the visible spectrum, and an optical filter was used to remove it. The signal-to-noise ratio for the LED-based systems was determined and compared with that of the LIF system. The fluorescent signal of the LED-based system was smaller by 1 to 2 orders of magnitude, despite the fact that the LED pulse energy was 2 to 3 orders of magnitude less than the laser's. As such, the fluorescent signal from the LED was greater than expected. Therefore, a UV LED may be a compact and much cheaper optical source for future water measurement instruments.
2

Application of Sol-Gel Derived Silica Particulates as Enzyme and Reagent Immobilization Support in Electrochemiluminescence-Based Flow Injection Analysis

Wang, Jen-Ya 24 June 2004 (has links)
Based on the linear relationship between concentration of H2O2 and the decrease of electrochemiluminescence (ECL) intensity in a Ru(bpy)32+/TPA system, procedures for the indirect determination of glucose with a flow injection analysis were developed. By passing solutions of glucose through a FIA system containing a glucose oxidase (GOx) immobilized sol-gel column and an ECL system of Ru(bpy)32+ and TPA, glucose can be determined optimally with a detection limit of 1.0 £gM in a linear dynamic range of 1.0 ¡V 200.0 £gM. A repetitive injection of glucose (100 £gM) and human serum solutions gave satisfactory reproducibility with relative standard deviations of 1.3 (N=31) and 3.9 % (N=42) respectively. Interference due to the presence of ascorbic acid, uric acid or other reducible agents in solution can be corrected by passing sample solutions through another sol-gel column that contained no GOx. From the agreement between the contents of glucose in human serum and soft drink analyzed by the developed method and those obtained by the spectroscopy method based glucose assay kit and satisfactory recovery of glucose from interferent containing solutions, the feasibility of the developed method for real sample analysis was confirmed. One of the major purposes of this study was to develop new immobilization approaches and flow cell designs for the fabrication of regenerable ECL-based sensors with improved sensitivity, convenience and long-term stability. Silica particulates were used as immobilization support in ECL sensors for TPA and NAD(P)H and in biosensors for glucose and glucose-6-phosphate¡]G6P¡^. The first ECL flow cell was fabricated from a glass tube, and a platinum wire was used as working electrode held at +1.3 V. The volume of the flow cell was about 50 £gL. An Ag/AgCl electrode and a piece of Pt wire were used as the reference and counter electrode respectively and placed downstream of the working electrode. Ru(bpy)32+ immobilized silica particulates with 1/3 silica sol content showed the best performance for TPA determination, and the sensitivity of TPA determination was dependent upon the amount of Ru(bpy)32+ immobilized in silica particulates. The lowest level of analyte detected for TPA was 0.02£gM, and linear range was from 0.02£gM to 5£gM. Up to a certain concentration level, it was found that Ru(bpy)32+ was tightly held in silica particulates and did not leach out into aqueous solutions, even with continuous flow for up to ten hours. Ru(bpy)32+ immobilized silica particulates were characterized of well activity and high stability; that stored at 0¢J exhibited its original activity for up to one year. The second ECL flow cell was fabricated from a piece of epoxy block supported Pt electrode (1 ¡Ñ 2 cm) as counter electrode, a piece glass window and a polyethylene spacer with 78 £gL cell volume, two 2.0-cm length of 0.6-mm diameter platinum wires were used as working electrodes held at +1.1 V, and an Ag/AgCl electrode as reference electrode. All three electrodes were incorporated within the main body of the cell. One of the biosensor design packed Ru(bpy)32+ incorporated silica particulates in the ECL flow cell, and a glucose dehydrogenase (GDH) immobilized silica sol-gel column is placed between the sample injection valve and the flow cell. The ECL response to samples containing glucose and cofactor (NADP) results from the Ru(bpy)33+ ECL reaction with NADPH produced by glucose dehydrogenase. This ECL biosensor was shown applicable for both NAD+- and NADP+- dependent enzymes, where NADH detection ranged from 0.50£gM ¡V 5.0 mM NADH and NADPH detection ranged from 1.0£gM - 3.0 mM NADPH. Glucose can be determined in a linear dynamic range of 5.0 - 500 £gM. Another biosensor design immobilized glucose-6-phosphate dehydrogenase¡]G6PDH¡^onto the Ru(bpy)32+ -doped silica particulates through silica chemistry and then packed these particulates into the ECL flow cell. By passing samples containing G6P and cofactor (NAD) through the ECL flow cell, G6P can be determined in a linear dynamic range of 10.0 £gM-1.0 mM. The regenerable ECL biosensor was characterized of good reproducibility and well stability for flow injection analysis. A repetitive injection of NADH (100 £gM) and G6P¡]500£gM¡^gave satisfactory reproducibility with relative standard deviations of 2.8 %¡]N=105¡^and 2.8 % (N=40) respectively.

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