Chemistry Commons^™

A Study Of The Thermal Properties Of Peti-5/Im7, Yan Tang

Masters Theses & Specialist Projects

PETI-5 (Phenylethynyl-terminated polyimide) is a substance that shows a great deal of potential in the high-speed aircraft and the aerospace industry. PETI-5 has been used for the High Speed Civil Transport (HSCT), a supersonic passenger aircraft in development at NASA. In this project, four staging samples, one fresh sample, one fully cured sample and one partially cured sample were analyzed and compared using thermal analytical techniques. The sample staged at 450°F with full vacuum showed the highest thermal properties among four staging samples. The results indicated that vacuum is helpful in improving the thermal stability of PETI-5. The mechanism of …

Analysis Of Galvanized Steel Plates Using Glow Discharge-Atomic Emission Spectrometry, Liang Wang

Masters Theses & Specialist Projects

Combining an intense emission source and a high-speed sputtering source in one, glow discharge atomic emission spectrometer (GD-AES) provides an efficient technique for analyzing surfaces, coatings and bulk solids. The purpose of our work is to explore the optimum lamp operation parameters of SA-2000 for analysis of galvanized steel plate and to investigate the method for qualitatively and quantitatively analyzing the zinc coating. Under the optimum experimental conditions found in our study, which are current of 19-21 mA; voltage of 900-1200 V; pressure 2.0-2.5 torr, the calibration curve is constructed, so that specific zinc concentration can be assign to the …

Comparison Of An Advanced Mercury Analyzer With The Cold Vapor Atomic Absorption Technique For The Determination Of Mercury In Coal, Dong Li

Masters Theses & Specialist Projects

For over 30 years the industry standard method for mercury analysis has been the cold vapor atomic absorption spectrometric technique (CVAAS). Recent developments in improving this technique have focused on procedures for concentrating mercury in the analyte or materials to improve detection. The LECO Corporation produces an Advanced Mercury Analyzer, the AMA-254, for analysis of the solid and liquid samples. The system allows for the thermal heating of the sample to decompose the sample and release mercury, which is concentrated in a gold amalgam. Thermal desorption of the mercury from the amalgam is detected by atomic absorption spectroscopy. A comparison …

An Immobolized Surfactant Extraction Technique Compatible With High Performance Liquid Chromatography-Ultraviolet Visible Detection, Ming Zhu

Masters Theses & Specialist Projects

Surfactant mediated extractions are analogous to liquid-liquid extractions (LLE) except surfactants are used as extractants instead of organic solvents. The benefit for using surfactants for extractions includes lower toxicity, lower associated costs and direct compatibility with high performance liquid chromatography techniques. In this study, a novel immobilized surfactant extraction method was developed. In this method, the cationic alklytrimethylamrnonium surfactants are immobilized onto a strong cationic exchange resin through ion exchange. This surfactant-resin material is placed in a column and aqueous solutions containing analytes are passed through. The analytes are retained by the long carbon chain of the surfactant molecules and …

Analysis Of Fats And Fat-Soluble Components In Foods Using Supercritical Fluid Extraction And Chromatographic Techniques, Sneha Patel

Masters Theses & Specialist Projects

The purpose of this study was to develop experimental procedures for the extraction of fats from common foods using SFE and to determine by chromatographic techniques the fat-soluble components that are extracted with the fats. In this study various food samples were examined including french fries from Wendy's, McDonald's and Burger King, as well as potato chips, peanut butter and donuts. Soxtec extraction was used as the standard method for comparison of results (percentage of fat) obtained from SFE. Gas chromatography and gas chromatography/mass spectrometry were used for the determination of fat-soluble components (fatty acids), after extraction of fat from …

An On-Line Test For Polycyclic Aromatic Hydrocarbons In The Flue Gas From Coal Combustion In An Fbc System, Wenjun Han

Masters Theses & Specialist Projects

Polycyclic Aromatic Hydrocarbons (PAHs) are environmental pollutants that have received considerable attention because of their carcinogenic and mutagenic effects. Due to the extensive amount of data suggesting the hazards of these compounds, 16 PAHs are on the Environmental Protection Agency (EPA) Priority Pollutant List. These compounds are often emitted into the atmosphere by way of combustion processes. Thus, analysis of these compounds during coal combustion is an important task. Three 1000-hour coal combustion burns were performed using the 0.1 MW (0.3 m) bench-scale Fluidized Bed Combustor (FBC) in the Combustion Laboratory at Western Kentucky University. The data for this thesis …

Capillary Zone Electrophoresis Studies Of Sulfur Containing Compounds, Francisco Rodriguez

Masters Theses & Specialist Projects

Up to this point in time, complex mixtures of tertiary sulfonium ions have been separated or analyzed employing conventional methods like HPLC or NMR procedures. In this thesis the researcher presents a new approach, the use of Capillary Zone Electrophoresis (CZE) for the analysis of these types of ions as well as the closely related thiophenium ions. CZE offers an unprecedented advantage in that separations can be employed for speciation or quantitation of complex mixtures by using the appropriate standards or specific detectors. For the study, model sulfonium and thiophenium ions were used to determine the feasibility of the separation …

Capillary Electrophoretic Separation Of Sulfoxides, Clair Davies

Masters Theses & Specialist Projects

Chiral sulfoxides are most widely used in asymmetric synthesis. Their application as chiral synthons has now become a well-established and reliable strategy, mainly due to availability and high asymmetric induction exerted by the chiral sulfinyl group. Very few articles have been published on the separation of chiral sulfoxides; most involve HPLC or GC. The first separation of optically active sulfoxides was described by Phillips and co-workers. To date no work has been reported using capillary electrophoresis for the separation of alkylaryl sulfoxides. A series of alkylaryl sulfoxides were synthesized. Conditions for their separation were investigated using a modified 125 mM …

A Study Of High Temperature Corrosion In An Afbc System, Wie Xie

Masters Theses & Specialist Projects

The occurrence of furnace wall and superheater corrosion in fluidized bed combustor systems has caused some operational and economic concerns. It is generally accepted that chlorine and sulfur may play roles in this corrosion. In order to predict the performance of high chlorine or high sulfur coals in these combustion systems, it is necessary to have a better understanding of the different corrosion mechanisms in which chlorine and sulfur may be involved. It is also important to evaluate the critical point of coal chlorine content which may cause initial corrosion. The laboratory-sized atmospheric bed combustor (AFBC) at Western Kentucky University …

The Effects Of So2 On The Formation Of Cl2 During Co-Firing Muncipal Solid Waste With Coal, Ying Xie

Masters Theses & Specialist Projects

The Deacon Reaction was proposed as a mechanism for the formation of molecular chlorine during the combustion of municipal solid waste (MSW): 4HCl + O2 ↔ 2Cl2 + 2H2O As suggested by some researchers, co-firing high sulfur coal with MSW may reduce the emission of toxic chlorinated organics, resulting from the reaction between S02 and Cl2: SO2 + Cl2 + H2O → SO3 + 2HCl The effect of sulfur dioxide on the formation of chlorine through the Deacon Reaction is investigated in this study. A Lindberg Furnace was utilized and preheated to 800°C to simulate the conditions in the AFBC …

Forensic Soil Analysis: Characterization Of The Sand Fraction, John Baize

Masters Theses & Specialist Projects

The purpose of this project was to develop a comprehensive analytical method for the characterization of soil by examining particle size, elemental composition, and percent organic matter in soil, and to determine its forensic applicability. In this study, five soils of varying geological locations were examined including two samples from Kentucky; two samples from Pennsylvania; and one from Washington D C A Gilson sonic sieve shaker was used to separate fractions of soil to determine particle size, and a JEOL scanning electron microscope with a Kevex EDS detector was used to determine elemental composition. These techniques coupled with percent total …

Development Of An Atmospheric Fluidized Bed Combustor (Afbc), William Orndorff

Masters Theses & Specialist Projects

The relatively recent interest in the U.S. in the development of atmospheric fluidized bed combustion (AFBC) has been preceded by two main factors. First of these is the ever present problem of acid rain and growing public support for cleaner burning fossil fuels. Second is the increasing demand on public landfills and subsequent need for burning of municipal solid waste. From these factors and their corresponding influences, Western Kentucky University has the impetus and has received the financial assistance necessary to build and develop a laboratory scale AFBC system. A brief history of the events leading to this development, as …

Studies On Resolution Of Enantiomeric Dialkylaryl Sulfonium Ions With Nmr Shift Reagents, Ea-Ji-Ru Son

Masters Theses & Specialist Projects

Praseodymium(III) NMR shift reagent, which is an upfield shift reagent, is focused on for assessment of enantiomeric excess and resolution of methyl sulfonium ions. A series of alkylmethylphenylsulfonium ions were analyzed, where alkyl is ethyl (I), butyl(H), octyl (III), and benzyl(IY). The praseodymium agent gives base-lined resolution of the ortho hydrogens resonance for I and IH. All spectra are strongly temperature-dependent. I is shifted more than ED, consistent with a steric effect. Assignments for I were made by gradually increasing the concentration of the shift reagent and by analyzing R-enriched I. Racemization of R-enriched isomer of I by pyramidal inversion …

A Study Of Polycyclic Aromatic Hydrocarbons During Combustion In An Afbc System, Laura Dicken

Masters Theses & Specialist Projects

The purpose of this study was to develop the on-line method of analysis which leads to the study of polycyclic aromatic hydrocarbons (PAHs) during combustion in an atmospheric fluidized bed combustor (AFBC) system. The study of PAHs is important because they may be produced upon the combustion of coal. The US EPA prioritizes PAHs as major pollutants due to their mutagenic and carcinogenic effects. Standards of PAHs were analyzed by injection into the gas chromatograph-mass spectrometer (GC-MS). These standards were then analyzed using the on-line method. Two coals were burned in the AFBC system and effluent samples were collected. These …

Fundamental Investigations Of Mechanistic Pathways Of Selected Organic Reactive Intermediates, Carl Whittle

Masters Theses & Specialist Projects

Part 1 of this thesis deals with the role that it -electron density plays in the formation of it -complexes in electrophilic aromatic substitution. Using commercial and synthetic compounds of varying it-electron density, the fact that % -complexes actually exist in these species was determined by a mass spectral investigation that was designed to monitor alkyl side-chain isomerizaitons. Also, the amount of it-complex was determined for each compound by measuring the amount of alkyl carbenium ion loss in each compound's mass spectrum. Found within the systems was an internal trend showing that the greater the amount of 7t-electron density in …

A Study Of The Volatile Matter Of Coal As A Function Of The Heating Rate, Enrique Santos

Masters Theses & Specialist Projects

A study of volatile matter yields as a function of the heating rate was conducted. A suite of 21 coal and coke samples varying in rank from anthracitic to lignitic and heating rates from 10°C/min to about 450°C/min were used in the study. Heating rates up to 60°C per minute, which are typically used in ASTM Test Method 5142 (instrumental Proximate Analysis), were achieved in a macro thermogravimetric analysis (TGA) system. Heating rates of 50-200°C/min were obtained in a micro TGA system. All measurements were made in a nitrogen atmosphere. The results of the study illustrate the dependance of the …

Development Of Methods For The Determination Of Major And Minor Elements And Hydrocarbon Residues In Solid Combustion Products, Xiaoliu Chi

Masters Theses & Specialist Projects

Methods for the determination of inorganic constituents in coal fly ash by glow discharge spectrometry (GDS) and for the extraction of the organic compounds from coal and ash by supercritical fluid extraction (SFE) at temperatures below 150°C are reviewed. The inorganic elements studied included Al, Ca, C, Cu, Fe, Mg, Mn, P, S, Si and Ti. The organic compounds were measured by weight loss of the sample. The goal of this research was to find easier and faster ways to measure the concentration of inorganic elements in coal ash and to measure extractability of the coal itself, to make coal …

A Study Of Combustion Profiles Of Co-Fired Coal/Biomass/Limestone Samples In A Fluidized Bed Combustor, Beverly Campbell

Masters Theses & Specialist Projects

Concerns over declining landfill space and a renewed interest in waste-toenergy technologies have increased the possibilities of co-firing different types of fuels in atmospheric fluidized bed combustion systems. The laboratory sized atmospheric fluidized bed combustor (AFBC) at Western Kentucky University was designed to serve as a highly flexible research and development facility to gain operating experience, evaluate combustion performance, and estimate the effect of flue gas emissions on the atmosphere. The operating conditions for the AFBC system are similar to those used at the TVA 160-MW AFBC Pilot Plant located near Paducah, Kentucky. AFBC systems are ideal for co-firing because …

Mass Balance Of Major, Minor And Trace Elements During Afbc Combustion Of Fuels, Qianwen Cao

Masters Theses & Specialist Projects

The proposed ASTM procedures for the determination of 13 major and minor., and 11 trace elements, in solid coal and coke combustion residues by inductively coupled plasma-atomic emission spectrometry (ICP-AES) were checked for routine use. In this study, the ICP analysis values and XRF analysis values of major and minor elements in two kinds of coal and two kinds of limestone were compared. It was shown that over 95% closure of the mass balances of the 24 major, minor, and trace elements was obtained with the proposed ASTM procedure. Also, it was demonstrated that trace elements may be lost through …

The Resolution Of Chiral Dialkylarylsufonium Ions By 1h Nmr Spectroscopy, Johnathan Whetstine

Mahurin Honors College Capstone Experience/Thesis Projects

The goal of this research was to design a rapid Nuclear Magnetic Resonance method to measure enantiomeric excess of chiral sulfonium ions by using chiral lanthanide shift reagents. The sulfonium ions studied were dialkylarylsulfonium ions. The shift reagent that was employed was Europium (III) surrounded by chiral ligands of 3-trifluoroacetyl-d-camphor (tfc), which is derived from (+)-camphor. Ethylmcthylphenylsulfonium ion was synthesized for study as a racemic and enantiomerically enriched mixture. The sulfonium ion was then ion-paired with the shift reagent for resolution of R and S enantiomers. The best resolution was obtained with the Eu(fod)4- shift reagent, with nearly baseline resolution …

A Chemical Pathway To The Formation Of Chlorinated Compounds During Combustion, Xiaodong Yang

Masters Theses & Specialist Projects

Two reactions, the Deacon reaction and the chlorination of phenol, which are the postulated starting steps for the formation of chlorinated dioxins during the incineration of the refuse derived fuel, were investigated in this work. Reactions were conducted in a tube furnace, and the products were trapped and analyzed by gas chromatography/mass spectroscopy. It was shown that the Deacon reaction was favored at higher temperatures. The chlorination of phenol in vapor phase was found to begin at temperatures as low as 250°C and to be favored at higher temperatures. The ortho and para positions in the phenol ring are the …

A Study Of The Behavior Of Chlorine And Organic Compounds During Combustion In An Afbc System, Jenny Heidbrink

Masters Theses & Specialist Projects

The purpose of this study is to understand the behavior of chlorine and the emission of organic compounds during combustion in an atmospheric fluidized bed combustion (AFBC) system. Inefficient, uncontrolled use of coal gives rise to organic emissions which can be detrimental to health. The chlorine in coal may cause corrosion problems during utilization, if its concentration is high enough. The method for collection of the emissions of organic compounds involved the use of a Tenax resin as an absorbent for the organic compounds as they were emitted from the combustor. A combined gas chromatography - mass spectrometry (GC-MS) technique …

Degradation Product Analysis Of Bismaleimide Composite, Wendy Zhong

Masters Theses & Specialist Projects

This study evaluates the thermal and oxidative stabilities of a bismaleimide (BMI) polymer composite reinforced with an intermediate modulus graphite fiber, Cytec®5260/IM7. The composite is aged in helium, nitrogen, and air at elevated temperatures up to 600°C. Its weight change is followed thermogravimetrically for stability assessment. The effect of aging gas environment is also studied. The use of on-line gas cell fourier transform IR spectrometer (FTIR) and mass spectrometer (MS) allows for the identification of decomposition products by evolved gas analysis. This combination of thermogravimetric analysis (TGA) and evolved gas analysis by FTIR and MS yields complementary information regarding pyrolysis …

Directed Ortho-Metalation Of The Three Methyl Anisoles In Various Media, Carl Friesen

Masters Theses & Specialist Projects

Directed ortho-metalation (DoM) is a very useful alternative to electrophillic aromatic substitution (EAS) for the synthesis of substituted aromatic compounds. DoM is highly regiospecific providing metalation chiefly in the ortho-position. However, lateral (a-) metalation of an alkyl side-chain and ortho-metalation of a second ortho-position can compete. Investigation of the three methylanisoles was therefore undertaken to determine the interplay between these factors and to discover metalation conditions to achieve selectivity. This goal was uniquely achieved for p-methylanisole where conditions were discovered which allowed > 85% ortho-metalation as determined by GC analysis with virturally no competing lateral metalation. Three derivitives of this ortho-lithio …

A Study Of The Effect Of The Extraction Procedure In The Analysis Of Organic Compounds Adsorbed On Coal Ash, Shobha Purushothama

Masters Theses & Specialist Projects

The organic compounds found adsorbed on coal fly ash have been a cause for concern since the early days of the industrial revolution. A vast majority of the compounds reported as being adsorbed on the ash are polyaromatic hydrocarbons (PAHs). This study represents an attempt to evaluate the parameters involved in the extraction, detection and quantitation of these organic compounds. Though no definite conclusions could be reached as to the most efficient method of extraction, interesting results were obtained with regarding the choice of the solvent and the temperature programming on the GC/MS used for analysis. The solvent of choice …

A Study Of On-Line Analysis Of Hydrogen Chloride Evolution During Coal Combustion, Jennifer Humble

Masters Theses & Specialist Projects

This study involved the use of a thermogravimetric analyzer (TG) interfaced with a fourier transform infrared spectrometer (FTIR) and a mass spectrometer (MS) to determine the evolution of hydrogen chloride from coal during combustion as a function of the chlorine content and mesh size of the coal. It was determined that combined TG-FTIR and TG-MS systems offer the user an efficient means to investigate the mechanism of hydrogen chloride evolution from coal combustion. From the HC1 evolution profiles, it was determined that a good correlation exists between the chlorine content in the coal and the total amount of HC1 evolved. …

Characterization And Catalytic Properties Of Sulfated Zirconia, Melody Bi

Masters Theses & Specialist Projects

Sulfated zirconia has attracted extensive attention due to its superactivity to isomerize alkane and alkenes. Platinum or iron/manganese promoted sulfated zirconia has been shown to increase the reaction rate. These catalysts are normally activated to 650-725°C in air before use. Through on-line analysis of evolved gas species during dynamic heating of the catalysts, some significant information can be obtained concerning the activation mechanism. In the present investigation, combined TG-FTIR, TG-MS and TGDTA techniques were utilized to measure the weight loss of the samples, analyze the evolved gas species and to monitor the phase transformation temperature of the solid. Four samples …

Ua35/11 Student Honors Research Bulletin, Wku Honors Program

WKU Administration Documents

The WKU Student Honors Research Bulletin is dedicated to scholarly involvement and student research. These papers are representative of work done by students from throughout the university.

• Allen, Melody. Women in Control of Courtship in As You Like It, The Merchant of Venice and All's Well That Ends Well
• Amlani, Islamshah. Electron Stimulated Desorption of Alkali Halides
• Brillhart, Kelly. Women Without Men: Hemingway's Female Characters
• Burton, Lori. Financial Statements with Environmental Concerns: An Exploratory Study of the Impact on the Auditor's Role and Responsibilities
• Combs, Vicki. Dancing the Descent: Energy and Entrophy in William Carlos Williams
• Davis, Julie. Prelude to …

Specification Of Sulfur Forms In Coal, Weihao Wang

Masters Theses & Specialist Projects

Over a century of studies of the organic chemistry of coal has led to many accomplishments in coal chemistry. The recognition of the role that sulfur plays in coal makes the speciation of sulfur in coal one of the most important research goals. In this research solvent extraction, ultimate analysis, FTIR, TG-FTIR, sulfur methylation, and NMR techniques were employed to make quantitative and qualitative determinations of the organic sulfur in coal and its extracts. The data obtained from those methods are discussed with regard to the analytical and synthetic approaches used. Carbon-sulfur bond cleavage at room temperature was observed during …

Icp Analysis Of Solids/Waste Slurries, Buqian Wang

Masters Theses & Specialist Projects

The direct injection of solids/water slurries into an inductively coupled plasma (ICP) spectrometer offers a rapid and easy method for the analysis of major, minor, and trace elements in coal, coal ash, cements, and refractory materials. In this study aqueous slurries of 6 coals were prepared by milling with a stirred-ball slurry attritor mill and an air impact pulverizer. ICP analysis values obtained for the six coals by the two different grinding methods were compared. Five coal ashes and five check standard reference materials were ground by an attritor mill and analyzed with an ICP spectrometer. Slurries of standard reference …