Analytical Chemistry Commons^™

A Chloride Selective Calix[4]Arene Optical Sensor Combining Urea Functionality With Pyrene Excimer Transduction, Benjamin Schazmann, Dermot Diamond

Articles

A neutral 2-site chloride selective compound has been developed (3), based on a 1,3- alternate tetrasubstituted calix[4]arene providing a preorganised supramolecular scaffold. The resultant supramolecular cavity is amongst the first to combine urea functional groups bridged with single methylene spacers to pyrene moieties. It combines a naturally and synthetically proven H-bonding system with the elegant ratiometric fluorescent signalling properties of an intramolecular pyrene excimer system, triggered by conformational changes upon anion coordination. The excimer emission of 3 is quenched, with a simultaneous rise in the monomer emission solely by the chloride anion amongst a wide variety of anions tested. 3 …

Synthesis, Structural Studies And Desilylation Reactions Of Some N-2-(Trimethylsilyl)Ethyl-N-Nitrosocarbamates, Arpitha Thakkalapally, Vladimir Benin

Chemistry Faculty Publications

The present report describes the preparation and characterization of several N-2-(trimethylsilyl)ethyl-N-nitrosocarbamates, designed as precursors to thermally unstable secondary N-nitrosocarbamate anions via fluoride-assisted cleavage. X-ray structural studies demonstrate that the core N-nitrosocarbamate moiety has a nearly planar geometry, with an s-E orientation at the N–N bond. DFT calculations (B3LYP/6-31+G(d)) reproduce accurately the structural features of the title compounds and detailed conformational analysis at the same level of theory addresses the long-standing issue of preferred geometries for three classes of related structures: N-nitrosocarbamates, N-nitrosoureas and N-nitrosoamides. Desilylation studies demonstrate that both the …

Identification And Recovery Of An Asymmetric Calix[4]Arene Tetranitrile Derivative Using Liquid Chromatography And Mass Spectrometry, Benjamin Schazmann, Dermot Diamond

Articles

A simple analytical LC-MS (Liquid Chromatography Mass Spectrometry) method and associated instrumentation has been adapted for use by the organic chemist to yield mg quantities of target compound from a reaction mixture. Calix[4]arene 3 was identified as representing 51% of total peak area of a reaction mixture containing no less than 10 components, using LC-MS. This peak corresponded to a mass of 878.8, equivalent to a complex of 3 and an ammonium cation. Molecular models further rationalise this observation by showing that the asymmetric binding cavity of 3 is suitable for binding tetrahedral guests like the ammonium ion. By scaling …

Analysis Of Fuel Additives And Impurities In Gasoline, Nicholas Lentz

Honors Capstones

Capstone submitted as a graduation requirement for the BSU Honors Program.

Cerumen Composition By Flash Pyrolysis-Gas Chromatography/Mass Spectrometry, Craig N. Burkhart, Michael A. Kruge, Craig G. Burkhart, Curtis Black

Department of Earth and Environmental Studies Faculty Scholarship and Creative Works

Objective: To assess the chemical composition of cerumen by flash pyrolysis-gas chromatography/mass spectrometry.

Study Design: Collected earwax specimens were fractionated into residue and supernatant by means of deoxycholate. This natural bile acid produces significantly better disintegration of earwax in vitro than do presently available ceruminolytic preparations, and also has demonstrated excellent clinical results in vivo to date.

Patients: The sample for analysis was obtained from a patient with clinical earwax impaction.

Results: The supernatant is composed of simple aromatic hydrocarbons, C₅-C_{l 7} straight-chain hydrocarbons, a complex mixture of compounds tentatively identified as diterpenoids, …

Fourier Transform Raman Spectroscopy For Process Control In The Petroleum Industry, Kent Lawson Wise

Chemistry & Biochemistry Theses & Dissertations

As early as 1950, Raman spectroscopy was proposed as a method to determine aromatics and olefins in hydrocarbon mixtures. Until recently, extensive use of Raman spectroscopy in the characterization of hydrocarbons has not been practical due to several limitations. One early limitation to Raman analysis was the absence of a high intensity and stable excitation source. This problem has been overcome with the advent of lasers. Another limitation was the presence of fluorescence in hydrocarbon fuels when excited by visible lasers. However, the development of Fourier-transform Raman spectrometers now allows Raman spectra to be collected using near-IR lasers (e.g …

Environmental And Botanical Controls On Peatification - A Comparative Study Of Two New Zealand Restiad Bogs Using Py-Gc/Ms, Petrography And Fungal Analysis, Tomasz K. Kuder, Michael A. Kruge, J C. Shearer, S L. Miller

Department of Earth and Environmental Studies Faculty Scholarship and Creative Works

This study shows that chemical properties of two restiad species, Empodisma minus and Sporadanthus traversii, may contribute to their success as peat-formers in a climate of the North Island of New Zealand which is not conducive to raised mire development. Unlike Sphagnum, the equivalent northern hemisphere peat-former, restiads possess lignin in their tissues. In addition, the presence of non-lignin polyphenols (including tannins and phenolic acids) in restiads may be an important factor in peat formation due to the allelopathic decay retardation. Patterns of degradation of plant biopolymers have been examined and the pathway of degradation of monocotyledons (loss …

Petrographic And Chemical Properties Of Carboniferous Resinite From The Herrin No. 6 Coal Seam, John C. Crelling, Michael A. Kruge

Department of Earth and Environmental Studies Faculty Scholarship and Creative Works

Resinite is a naturally occurring substance found in coal and derived from original plant resins. It is ubiquitous in North American coals and comprises 1 to 4% by volume of most Illinois coals. It has been commercially exploited in the western USA for use in adhesives, varnishes and thermal-setting inks. The major objectives of this study were: (1) to separate resinite macerals from the Herrin No. 6 coal seam and to carefully verify, by petrographic and fluorescence microspectrophotometric methods, that the separated material was indeed resinite; (2) to characterize the chemical composition of the separated resinite by Py–GC–MS techniques; and …

Characterization Of Organic Sulfur Compounds In Coals And Coal Macerals, Stephen R. Palmer, Edwin J. Hippo, Michael A. Kruge, John C. Crelling

Department of Earth and Environmental Studies Faculty Scholarship and Creative Works

Peroxyacetic acid oxidation has been used to investigate the type and distribution of organic sulfur species in samples of vitrinite, sporinite and inertinite, separated from the Herrin No.6 and an Indiana No.5 coal seam. It was established that organic sulfur species were selectively preserved during oxidation and their analysis led to some of the first sulfur-33 NMR spectra obtained for coal. The effects of maceral separation processes on model compounds were also studied. Results from our studies support the following conclusions: 1). Different macerals have different distributions and types of organic sulfur species. 2). Organic sulfur compounds in coal occur …

Benzoylation Studies With A Compound Reported To Be Benzoyl Acid Sulfate And Analytical Studies On The Sample, Robert J. Peanasky

Bachelors’ Theses

A very valuable reagent in organic characterization work is benzoyl chloride. By interacting benzoyl chloride with any one of the general classes of compounds termed phenols, alcohols, and amines, solid and very satisfactory derivatives are usually produced. However, the action of this compound occurs rather slowly and the operator, unless especially careful, suffers from the lachrimatory effects of the reagent, benzoyl chloride. A sample was submitted to my major professor, Dr. C. R. Haymaker, by Gene LaFave who claimed that it was benzoyl acid sulfate. This compound was a solid not difficult to manipulate in contradistinction to the lachrimatory liquid …

The Determination Of Interfacial Tension Using Pendant Drop Method, Katherine Tellor

Bachelors’ Theses

Boundary tension is a measure of the free energy of a fluid interface. It is a term derived from the superficial analogy between the surface of a liquid and a stretched membrane. Just as the potential energy of a fluid mass in foot pound per pound is spoken of as a "head" in feet, so it is useful to speak of free energy of a fluid surface in ergs per square centimeter as a "tension" in dynes per centimeter.

The Effect Of Time, Temperature, And Pressure On The Hydrogenation Of A Mixture Of Linoleic And Oleic Acids, Gordon S. Wepfer

Bachelors’ Theses

During the past few years interest and experimentation in the field of hydrogenation of different fats and oils has increased enormously. Strides made in the oil-hardening industry have surpassed all expectations. These advances were brought about by simplifying old methods and creating new ones. The probable reasons for this impetus in research is due to the fact that unexpected uses for hydrogenated oils and fats have been found and will continue to be found. With the increase in use of these products the market for them will also increase. Recently, the resin industries have produced useful products by condensing pure …

A Study Of Resins From Carbohydrates, Edward F. Sullivan

Bachelors’ Theses

The availability of large amounts of carbohydrates, and the need in the past years of larger markets for the available supplies of sugar have lead a number of sugar companies to investigate the possibilities of synthetic resins from carbohydrates. Although in the last ten or twelve years, a number of steps have been taken in the investigation of sugar resins, the information available has been restricted to a few patents. Consequently, information on the chemistry of the problem has been neglected. Thus, this work, for the most part, covers partially the possibilities of producing alkyd resins from saccharides, as well …

A Method For Comparing And Measuring The Drying Time Of Glues, William C. Strutz

Bachelors’ Theses

The measurements or quality in glue testing are arbitrary and are of value only when compared to a standard glue or when comparing one glue to another. Glues have been used for hundreds of years, but it has been only in the last forty or fifty years that any scientific investigations of any consequence have been made. Prior to this time glues were made by rule of thumb by practical men who learned the art of glue making from other practical men in the business and by contact with the industry. "When the United States entered the Great War and …

A Comparison Of The Caffeine Content Of Various Coffees, Emil J. Petrusek

Bachelors’ Theses

Coffee must be rated as one of the most important commodities in the commercial world due to the statistics or output and consumption. There are various brands and kinds of coffee produced by the different growers and roasters. Now to sell the brands, the various concerns base their advertising upon the flavor and price of the coffee. It is a fact that the flavor of coffee is in some way affected by the caffeine present. One popular brand is advertised as decaffeinated, that is, the caffeine has been removed. Confronted with these facts, it occurred to the author to test …

The Extraction Of Tantalum And Columbium From Tantalite, Stanley P. Wisniewski

Bachelors’ Theses

In the summer of 1932, the Milwaukee Public Museum, sent an expedition to the Bad Lands and Black Hills of South Dakota, under the direction of Dr. Ira Edwards, Curator of Geology in that institution. It was at this time that the author, a member of this group, while studying the pegmatites of the Black Hills, became interested in the tantalum-columbium bearing minerals of that region, namely tantalite and columbite. At that time the writer made a detailed mineralogical study of these two minerals, as well as a thorough investigation of their occurrence in that region. In the fall of …

Wax Analysis With Special Reference To Montan, Spermaceti, And Chinese Insect Wax, Margaret M. Plonsker, Margaret E. Seippel

Bachelors’ Theses

The presentation of this thesis under joint authorship finds its justification in the fact that much of the experimental work, though performed individually, is of such a nature as to warrant a unified description. In this way the reader is afforded a better representation and clearer conception of the problem, and a substantial guide for further investigation. Though much work has been done in the field of wax analysis, little is known of the higher fatty acids and alcohols of many of the waxes. Their isolation has been infrequent, and few if any of their derivatives have been formed. It …

The Study Of The Effects Of Different Metallic Soaps On The Water Content Of Water-In-Gasoline Emulsions, Lynn D. Wilson

Bachelors’ Theses

The study of emulsions and emulsification is of very great theoretical and practical interest. From the standpoint of pure science it throws much light on the problems of surface tension, surface concentration, absorption, surface films, electrical double layers. Brownian movement, and the general theory of disperse systems and colloids. It is also of importance in biological science, e.g., the adsorption of fats and the permeability of membranes. When industrial and applied science are considered, it is remarkable how many subjects of interest and importance are dependent on a knowledge of the formation, behavior, and stability of emulsions. In this connection, …

A Study Of Phytosterol Obtained From Cocoa Beans And Cocoa Butter, Norman Anthony Pokorny

Bachelors’ Theses

Despite the fact that considerable work has been done on cholesterol, relatively little is known about its isomer, phytosterol. Both cholesterol and phytosterol belong to the general group of sterols. Cholesterol is described as an aromatic sterol, a mono~atomic secondary alcohol, containing an iso-propyl and a vinyl group, with a terpene-like structure. Cholesterol was first discovered by Conradi in 1775, then by Gren (1788) in biliary calculi. In 1785 Fourcroy isolated cholesterol from gall-stones, one variety of which is composed almost wholly of it, but it was confused with adipocere, until Chevreul (1814) discovered its true nature, when he declared …