Analytical Chemistry Commons^™

Development And Optimization Of Hplc-Icpms For The Determination Of Iodine Speciation In Groundwater, Yun Qiu

All-Inclusive List of Electronic Theses and Dissertations

High performance liquid chromatography has been coupled with online inductively coupled plasma mass spectrometry detection for the determination of iodine speciation in drinking and groundwaters. Using ion exchange chromatography, the method is applied to quantify the concentrations of iodine species in groundwaters. The HPLC-UV detection was used first to examine the separation efficiency of the HPLC method. The limit of quantification was obtained for the HPLC-UV analysis. Direct ICPMS analysis of iodine species has been validated and optimized using an HC03"/C03 2 - aqueous solvent. HPLC was then interfaced to the ICPMS T-shape connection to allow online addition of internal …

Immobilization Of Fission Iodine By Reaction With A Fullerene Containing Carbon Compound And Insoluble Natural Organic Matrix: Quaterly Report September-December 2003, Spencer M. Steinberg

Separations Campaign (TRP)

The recovery of iodine released during the processing of used nuclear fuel poses a significant challenge to the transmutation of radioactive iodine. This proposal will develop and examine the use of Fullerene Containing Carbon (FCC) compounds as potential sorbents for iodine release from the reprocessing of nuclear fuel. This work will also include the development of bench-scale testing capabilities at UNLV to allow the testing of the FCC material in a simulated process off-gas environment. This experimental capability will also be used to test other potential sorption materials and processes, such as natural organic matter (NOM) and other promising alternatives. …

Determination Of Cystine By Second Order Differential Simple Oscillographic Voltammetry, Fu-Fang Tao, Jian-Bin Zheng

Journal of Electrochemistry

In 0.2 mol/L NaOH, cystine can cause an sensitive incision at -0.5 V (vs.SCE) of cathodic branch of dE/dt-E curve or second order differential simple oscillogram. Based on the oscillographic charateristic, second order differential simple oscillographic voltammetry was applied to the determination of cystine in tablet. The linear range and the detection limit for determination of cystine were 2.5×10^-6～3.5×10^-5 mol/L and 1.0×10^-6 mol/L, respectively. The relative standard deviation for 2.000×10^-5 mol/L cystine was 1.8% (n=5).

Support For The Nye County Early Warning Drilling Program, Irene Farnham, Klaus J. Stetzenbach, Amy J. Smiecinski

Publications (YM)

This final report details the activities completed for Task 8 of the University and Community College System of Nevada (UCCSN) Cooperative Agreement with the US Department of Energy (DOE). Task 8, titled "Support for the Nye County Early Warning Drilling Program" provided for a variety of hydrochemical analyses. The requirements of the University and Community College System of Nevada (UCCSN) Quality Assurance (QA) Program were followed for all work performed on this task. The primary activity performed by the Harry Reid Center for Environmental Studies (HRC) for Task 8 was to provide hydrochemical analyses of the groundwater samples collected from …

Immobilization Of Fission Iodine By Reaction With A Fullerene Containing Carbon Compound And Insoluble Natural Organic Matrix, Spencer M. Steinberg, David W. Emerson, Gary Cerefice

Separations Campaign (TRP)

The recovery of iodine released during the processing of used nuclear fuel poses a significant challenge to the transmutation of radioactive iodine. During the first year of this program we have examined the potential of Fullerene Containing Carbon compounds (FCC) developed by KRI, and natural organic matter (NOM) as sorbents for iodine released during the reprocessing of nuclear fuel. This work involved the development of bench-scale testing of the FCC and NOM material in a simulated process off-gas environment.

During the first two quarters of this program we explored various analytical methods available for measurement of iodine, iodide, and iodate. …

Measurement Of Anti-Cancer Agent Methoxyamine In Plasma By Tandem Mass Spectrometry With On-Line Sample Extraction, Shuming Yang, Lili Liu, Stanton L. Gerson, Yan Xu

Chemistry Faculty Publications

In this work, we present the development and validation of a tandem mass spectrometry method for the quantitative determination of methoxyamine (CH3ONH2), a potential new chemotherapeutic agent, in human and mouse plasma. Methoxyamine together with the internal standard (I.S.) methoxyl-D3-amine was directly derivatized in plasma sample with a novel chemical agent 4-(N,N-diethylamino)benzaldehyde. The product solution was injected into an on-line Oasis® HLB extraction column ( mm) for analyte extraction. After the elution of extractives, the derivatized analytes were monitored by the positive-electrospray-ionization mass spectrometry (ESI-MS-MS). The structures of derivatized analytes were elucidated by fragmentation. Quantitation of plasma methoxyamine was carried …

Fabrication Of Scanning Micro Cl- Probe And In Situ Imaging Of Cl- At The Interface Of 2024 Al Aloy/Solution, Yu-Hua Lin, Min-Hua Shao, Rong-Gang Hu, Yan Li, Rong-Gui Du, Chang-Jian Lin

Journal of Electrochemistry

Micro combination Ag/AgCl electrode with a tip measuring tens micron in diameter was fabricated. The probe satisfied in situ imaging of Cl^- distribution at metal surface in chloride solution because of its excellent linearity between potential and Cl- concentration, rapid response, good stability and selectivity. With the aid of the home made Micro Electrode Scanning system and scanning Cl^- probe, the effect of the [Cl^-] at 2024-Al/solution interface on localized corrosion process was investigated. It was demonstated directly that Cl^- ion in solution immigrated toward, then adsorbed preferentially and accumulated at the junction between the …

Photofragmentation Dynamics Of Core-Excited Water By Anion-Yield Spectroscopy, Wayne C. Stolte, M. M. Sant'anna, Gunnar Ohrwall, Maria Novella Piancastelli, I. Dominguez-Lopez, Dennis W. Lindle

Chemistry and Biochemistry Faculty Research

Partial-anion and- cation yields from H₂O are presented for photon energies near the oxygen K edge. The O^- yield exhibits a feature above threshold attributed to doubly excited states, in contrast to the H^- and cation yields, which are nearly featureless above threshold. Additionally, the lack of the OH^- fragment indicates radiative decay and provides a negligible amount of anion formation.

Immobilization Of Fission Iodine By Reaction With A Fullerene Containing Carbon Compound And Insoluble Natural Organic Matrix: Quarterly Report April-June 2003, Spencer M. Steinberg

Separations Campaign (TRP)

The recovery of iodine released during the processing of used nuclear fuel poses a significant challenge to the transmutation of radioactive iodine. This proposal will develop and examine the use of Fullerene Containing Carbon (FCC) compounds as potential sorbents for iodine release from the reprocessing of nuclear fuel. This work will also include the development of bench-scale testing capabilities at UNLV to allow the testing of the FCC material in a simulated process off-gas environment. This experimental capability will also be used to test other potential sorption materials and processes, such as natural organic matter (NOM) and other promising alternatives. …

Study Of Marine Biocorrosion Using Afm And Molecular Techniques, Herbert H.P.Fang, Lichong Xu, Tong Zhang

Journal of Electrochemistry

Biofilm is ubiquitous in nature.However,corrosin caused by biofilm is still by and large overlooked. This presentation is to demonstrate the applications of several newly developed analytical techniques in chemisrty and microbiology for the study of marine biocorrosion on steel. AFM(atomic force microscopy) was applied to investigate the initial formation mechanism of biofilm and the degree of corrosion of steel in polluted seawater. DNA/RNA-related molecular techniques were used to analyze the microbial composition corrosive biofilm. Results showed that microbial corrosion began within six days, and the corroded volume in the increased as a power function of time with an index 2.83. …

Perfluorinated Sulfonic Acid Lithium Conductivity Humidity Sensor, Hong-Feng Xu, Jing Liu, Li Wan

Journal of Electrochemistry

Treat carbon paper with 3% PTFE solution and dried in 340 ℃ for 40 minutes to enhance its intension, and level off the surface of the carbon paper with a mixture of XC-72 carbon black and PTFE solution. With those treated carbon paper as electrodes, recast Nafion thin film from 5% Nafion solution as humidity sensitive material, a solid polymer electrolyte humidity sensor was prepared on a thin PET film. Take the relative humidity data from several saturated salt solutions, the relationship between conductivity response and relative humidity was studied at different relative humidies .The results showed: when the polymer …

Immobilization Of Fission Iodine By Reaction With A Fullerene Containing Carbon Compound And Insoluble Natural Organic Matrix, Spencer M. Steinberg

Separations Campaign (TRP)

The recovery of iodine released during the processing of used nuclear fuel poses a significant challenge to the transmutation of radioactive iodine. This proposal will develop and examine the use of Fullerene Containing Carbon (FCC) compounds as potential sorbents for iodine release from the reprocessing of nuclear fuel. This work will also include the development of bench-scale testing capabilities at UNLV to allow the testing of the FCC material in a simulated process off-gas environment. This experimental capability will also be used to test other potential sorbtion materials and processes, such as natural organic matter (NOM) and other promising alternatives. …

Immobilization Of Fission Iodine By Reaction With A Fullerene Containing Carbon Compound And Insoluble Natural Organic Matrix: Quarterly Report January-March 2003, Spencer M. Steinberg

Separations Campaign (TRP)

The recovery of iodine released during the processing of used nuclear fuel poses a significant challenge to the transmutation of radioactive iodine. This proposal will develop and examine the use of Fullerene Containing Carbon (FCC) compounds as potential sorbents for iodine release from the reprocessing of nuclear fuel. This work will also include the development of bench-scale testing capabilities at UNLV to allow the testing of the FCC material in a simulated process off-gas environment. This experimental capability will also be used to test other potential sorption materials and processes, such as natural organic matter (NOM) and other promising alternatives. …

In Situ Measurements Of Solution Conductivity In Microwave Field, Yong-Qing Su, Chun-Peng Liu

Journal of Electrochemistry

The curves of the conductivity as a function of temperature for 24 kinds of solutions have been in situ measured both in the microwave field and in absence of microwave field. The results indicated that the relationship between the conductivity in microwave field (L_w) and temperature (T) can be expressed by an equation L_w=a′+b′T+c′T² , similar to the one that is valid in absence of the microwave field L_n=a+bT+cT². Conductivity in the absence and presence of microwave field can be linked by the equation lnL_w=A+BL_n+CL²_{n …}

Measurement Of The Anti-Cancer Agent Gemcitabine In Human Plasma By High-Performance Liquid Chromatography, Bruce Keith, Yan Xu, Jean L. Grem

Chemistry Faculty Publications

A reversed-phase HPLC assay has been developed to determine the concentration of the anti-metabolite 2′,2′-difluorodeoxycytidine (gemcitabine, dFdC) in human plasma over the concentration range of 0.5–150 μM (0.13–39.44 μg/ml), and 2′,2′-difluorodeoxyuridine (dFdU), the deaminated, inactive metabolite, over the range of 1.0–227 μM (0.26–60 μg/ml). After the addition of 20 nmol 2′-fluorodeoxycytidine (FdC) as an internal standard, 0.5-ml samples of plasma were subjected to acetonitrile precipitation, followed by analysis using a gradient reversed-phase HPLC assay with UV detection. A Phenomenex Columbus™ C18 column, 5 μm, 150×4.6 mm, and a Waters C18, 4 μm, Nova-Pak Sentry guard column were used to achieve …

Liquid Chromatography–Mass Spectrometry Method For The Analysis Of The Anti-Cancer Agent Capecitabine And Its Nucleoside Metabolites In Human Plasma, Yan Xu, Jean L. Grem

Chemistry Faculty Publications

A reversed-phase high-performance liquid chromatography method with electrospray ionization and mass spectral detection is described for the determination of capecitabine, 5′-deoxy-5-fluorocytidine and 5′-deoxy-5-fluorouridine in human plasma with 5-chloro-2′-deoxyuridine as the internal standard. An on-line sample clean-up procedure allows dilution of the plasma sample with the initial mobile phase. The linear dynamic range is 0.0500–10.0 μg/ml for capecitabine, and 0.0500–25.0 μg/ml for the metabolites, 5′-deoxy-5-fluorocytidine and 5′-deoxy-5-fluorouridine, respectively. This method has been used to analyze plasma samples from patients receiving capecitabine in combination with oxaliplatin.

Investigations Of Supramolecular And Catalytic Properties Of Ppi Dendrimers, Aaron K. Holley

Theses, Dissertations and Capstones

The research reported in this thesis focused on supramolecular and catalytic properties of poly(propylene imine) (PPI) dendrimers. Analytical techniques used in this research included high resolution NMR spectroscopy, as well as UV-vis and fluorescence spectroscopies and scanning electron microscopy. This investigation showed that: (1) PPI dendrimers interact with diacids to form interlock self-assemblies by electrostatic interactions (with an increase in dendrimer generation, smaller diacids are required to form the most efficient self-assembly); (2) PPI/diacid self-assemblies are able to encapsulate fluorescent dyes within the void spaces of the PPI/diacid moieties; (3) PPI-3 can chelate many types of metal cations, and these …

Oligothiophenes And Synthesis Thereof, Andrzej Rajca

Department of Chemistry: Faculty Publications

Novel oligothiophenes and intermediates therefor are disclosed together with a process for synthesizing them. The oligothiophenes are in the form of a helix which contains five-membered rings unsaturated heterocycles that are cross-conjugated and annelated into a helix.

Analysis Of Phycotoxin And Mycotoxin, Contaminants In Foods, Using Liquid Chromatography - Mass Spectrometry Techniques, Ana Brana Magdalena

Theses

The impact of phycotoxins and mycotoxins on human and animal health are of important concern for worldwide authorities and the scientific community. Liquid chromatography-mass spectrometry (LC-MS) techniques have been developed, optimised and validated for the analysis of these toxins.

Phycotoxins are potentially toxic substances, which are produced by marine phytoplankton and which may accumulate in shellfish or finfish. Azaspiracid poisoning (AZP) is a recently discovered syndrome that has been implicated in several incidents of human intoxications. A study was undertaken to examine the distribution of azaspiracids (AZA) in scallops {Pecten maximiis) and mussels {Mytiliis edulis). Domoic acid (DA) is an …

Simulation Of Dynamic Electrochemical Processes, John Cassidy

Articles

This work is designed to introduce electrochemists in a tutorial manner to the basics of modeling of electrochemical systems based primarily on diffusion equations. There is an introduction to analytical and numerical methods with examples taken from typical electrochemical experiments. The Laplace transform is used to derive the Cottrell equation and chronopotentiometry. The response of an electrode to a Gaussian concentration profile is detailed. Laplace’s equation is solved for a simple cell to determine the potential distribution. Discrete methods are employed to calculate the current time behavior following a potential step using the explicit finite difference method. Cyclic voltammetry is …

Possible Cobalt-Cobalt Bridging By A Hemiacetal In The Dinuclear Cobalt Complex Bearing The Ligand Bis(3-(2-Pyridylmethyleneamino)Phenyl) Sulfone, Armando M. Guidote Jr, Tomoko Imajo, Yasuhiko Kurusu, Yoshiro Masuyama

Chemistry Faculty Publications

A dinuclear cobalt complex bearing the ligand bis(3-(2-pyridylmethyleneamino)phenyl) sulfone (BPMAPS) was prepared. It is proposed that the structure of this is [Coz(BPMAPS)(m-0AcMhemi-Et)]PF6 wherein the cobalt centers are bridged by two carboxylato groups in m-fashion and a hemiacetal with an ethoxy group (hemi-Et). This proposal is based on the similarity of the FT-IR, UV-Vis, and FAB-MS results with the crystallographically characterized dinuclear manganese complex [Mn2(BPMAPS)(m-OAcMhemi-Me)]PF6, and elemental analysis results.