Engineering Commons^™

Heat And Mass Transfer In The Lyophilizatiuon Of Pharmaceuticals In Vials By Conduction Heating, William Warren Walsh

Theses

This thesis investigates the lyophilization of pharmaceuticals in vials by conductive heat transfer. The process phase diagram and methods of determining the solution eutectic temperature are reviewed. The theoretical considerations of heat and mass transfer pertaining to this process are discussed.

Lyophilization tests of distilled water and of mannitol solutions are used to indicate the relationship between vacuum chamber total pressure and the product/vial interface temperature. Experiments with 10% lactose solutions are used to determine the effect of shelf fluid temperature, product height and chamber vacuum on product/vial interface temperature. Test on a pharmaceutical product are used to confirm the …

The Transferability Of Force Constants Among Olefins, John Martin Comerford

Theses

A normal coordinate analysis of the in-plane vibrations of ethylene was performed using a modified valence force field, a modified Urey-Bradley force field and a hybrid orbital force field. The B_2u species of isobutene was also analyzed. An attempt was made to transfer force constants from ethylene and thereby solve the A₁ species of isobutene, but a solution could not be obtained. This suggests that simple transference of force constants is not feasable in this case.

The potential energy distributions obtained for ethylene are discussed. The normal coordinates calculated in this work are appended.

A Modified Redlich-Kwong Equation For Nonpolar And Slightly Polar Gases, David G. Skamenca

Theses

The PVT prediction capability of the Redlich-Kwong equation is substantially improved through the use of a generalized correlation based on the acentric factor. No experimental data is required to obtain the improved constants. Only the acentric factor and the critical properties of the pure gas are needed. The correlation of improved constants is limited to non-polar and slightly polar pure gases and mixtures in the supercritical temperature range.

The correlation applies to a reduced temperature range 1.00 le; T_R le; 1.60 and a reduced pressure range of 0.030 le; P_R le; 3.00. The correlation reduces deviations by as …

A Computer Program For The Design Of Packed Extraction Columns, George P. Gaccione

Theses

A computer program for the design of packed extraction columns has been developed. This program can operate with a minimum of data of the type that can easily be determined or estimated. The program can be used to investigate design alternates during the preparation of project cost estimates and for the final design of extraction columns.

Viscoelastic Properties Of Polymer Melts, Wu-Shiong Lee

Theses

Thirteen samples of molten polymers were used to test Spriggs and Careau Models. Two empirical equations, one for apparent viscosity and the other which is new, for primary normal stress difference, were checked with these samples also.

In order to test the models, material functions were sought for some specific flow patterns under which the experimental data were collected, and then these functions were compared with data.

Careau Model was found to be better than Spriggs Model in representing molten polymer properties but still yield large deviations. Two empirical equations fitted data quite well and were expected to be useful …

Combined Feedforward-Feedback Control Of A Fluidized-Bed Reactor, Reginald Eugene Mitchell

Theses

Feedforward control, feedback control, and combined feedforward-feedback control were studied on an analog computer to evaluate their effectiveness in controlling a fluidized-bed reactor used for the decomposition of cumene. Proportional, proportional-integral, proportional-derivative, and proportional-integral-derivative modes of control were investigated. Step changes in set-point and load were used as disturbances. The Ziegler-Nichols method and the process reaction curve method of Cohen and Coon were compared in determining values of KC, Ti, and Td which gave optimum control of the fluidized-bed reactor.

Control equation were obtained from the block diagrams of the systems and solved on an EAI TR-20 Analog Computer.

It …

The Application Of A Non-Newtonian Rheological Equation To Low-Density Polyethylene, Jeffrey N. Goldstein

Theses

A generalized non-Newtonian equation describing the rheology of molten thermoplastics is verified for low-density polyethylenes. The equation is extended to account for both rheological temperature dependency and polyethylene molecular weight dependency. The prediction of the rheology of new polyethylenes without additional experimentation is thus possible.

The Oxidation Of Sulfur Dioxide In A Regenerative Reactor, Raymond Henry Edgecomb

Theses

A novel dual-unit sulfuric acid converter is depicted that performs in cyclic operation in unsteady state. A mathematical model and IBM 1130 Computer program were developed to show the temperature and conversion profiles in commercial-sized vanadium oxide catalyst beds. In the catalytic oxidation of sulfur dioxide conversions of 95-97% were attained without benefit of conventional heat exchangers. A single exchanger operating in conjunction with the dual-unit system might attain conversions as high as 99%.

Determination Of The Electronic State Of Aryl Nitrenes In An Intramolecular C-H Insertion Reaction, Ali Mohammad Khonsari

Theses

β,γ-Dideuteriopropylbenzene was obtained in 84% yield from deuteration of allylbenzene. Nitration of this compound resulted in o-nitro (β,γ-dideuteriopropyl)-benzene. Reduction of this compound gave o-(β,γ-aideuterio-propyl)aniline. o-(β,γ-Dideuteriopropyl)phenyl azide was prepared by dizotization of the aniline compound, followed by treatment with sodium azide.

Decomposition of the azide in isooctane solution by photolysis at room temperature gave no trace of deuterio-2-methylindoline (intramolecular insertion product).

Photolysis of the azide at the reflux temperature of the solvent (99?C) resulted in the formation of deuterated-2-methylindoline as the major product (40%) yield. The reaction is presumed to proceed through an aryl nitrene intermediate. Analysis of the nuclear magnetic …

An Economic Evaluation Of A Pressure Sulfuric Acid Manufacturing Plant, Daniel A. Marlin

Theses

The production of Sulfuric Acid at elevated pressures is presented with the economics for operating at one, three, five, seven, nine and thirteen atmospheres. The conventional and pressure plants are compared operating on the same basis.

The basis for a pressure plant design is obtained from an I.B.M. 1130 computer program developed for One Thousand Net Tons per Day of Sulfuric Acid. Recognized operating conditions for a conventional acid plant are incorporated in the pressure plant design program.

Sulfuric Acid manufacture with operating pressures higher than atmospheric, but less than five atmospheres, results in maximum rate of return on investment …

A Computer Program For The Optimization Of Binary Distillation In A Dual-Column System, Richard Vincent O'Lenick

Theses

A computer program is presented for the optimization of a two-column distillation system involving a two-component mixture. The economic reflux ratios in each column are determined using the McCabe-Thiele Method. Activity coefficients are computed by either the Wilson equation, the Margules equation, or both. The program is general and may be used for any binary system where the assumption of constant molal overflow is valid.

Options in the program permit use of either column in separate calculation schemes.

While the optimization effort was prepared in general terms, the initial work was directed toward the acetone-water system. Full data for this …

The Optimization Of A Catalytic Methanol Reactor Using Quench Feed, John Paul Mcburney

Theses

The production of methanol in a catalytic quench feed reactor is studied by means of a computerized model and optimized in terms of total reactor length necessary to achieve a given production rate. The methanol reaction rate can be maximized in a quench reactor through the use of cold stream feeds along the length of reactor.

Since the methanol reaction temperature is restricted to an upper limit of 405°C, the addition of cold stream feed along the adiabatic reactor enables the desired conversion to be reached. For two given levels of conversion, 12% and 15%, an optimum inlet temperature, quench …

Effect Of Column Diameter On Mixing In Water Fluidized Beds, Donald P. Schiesl

Theses

In this investigation, the effect of column diameter and flow rate on the mixing characteristics of fluidized beds were studied.

Tests were made on columns of 4, 6, 8 and 10 inches in diameter using water to fluidize glass beads of 0.0185 inches in diameter. The tests were run both at minimum and three times minimum fluidization. Step, impulse, and sinusoidal forcing signals were fed to the columns, using a sodium chloride solution as a tracer with the inlet and outlet concentrations being monitored continuously by a conductivity recorder.

The result of this study showed increased fluid dispersion with increasing …

Packed Column Simulation, Frederick W. Schmidt

Theses

The most difficult and time consuming aspect of the design of packed columns is the hydraulic part. If the designer wants to try many different conditions, many repetitive calculations will have to be performed. Also, some inaccuracy is incurred when trying to use the U.S. Stoneware curves. The graphs are hard to read and almost impossible to interpolate between the parametric lines. The purpose of the program is to give a more accurate calculation by using equations for the pressure drop lines, interpolating between them and correcting for gas density for each foot of packing. The program also allows changes …

Batch Heat Transfer To Suspensions In An Agitated Vessel, John Philip Horzepa

Theses

Batch heat transfer data was experimentally determined for two phase (solid?liquid) systems in a baffled agitated vessel. Three iron oxide and water and two kaolin and water suspensions were evaluated and were found to be pseudoplastic. A total of 231 heating and cooling data points were examined. Each suspension was evaluated using anchor, paddle, propeller and turbine impellers. Various sizes of the latter three impellers were used.

The experimental heat transfer results for suspensions were compared with the Hagedorn and Salamone correlation for pseudoplastic liquids. Only partial agreement with the more dilute suspensions was obtained. Overall, the data for suspensions …

A Comparative Analysis Of Multicomponent Distillation Minimum Reflux Methods, Joesph H. F. Loozen

Theses

One of the most important factors to know in the design of distillation columns is the minimum reflux ratio. Numerous procedures have been developed for the determination of the value of the minimum reflux ratio for multicomponent mixtures requiring various degrees of computational effort. Shortcut techniques are obviously advantageous with respect to computation time. After reviewing the available methods, those by Underwood, Colburn, Scheibel and Montross, Murdoch and Holland, and Shiras et al. were selected for further evaluation, mainly on the basis of practical potential.

Comparison of these procedures was accomplished by calculating the minimum reflux ratio for a large …

The Effect Of Polymerization Variables On Reaction Rate And Intrinsic Viscosity, David H. Smith

Theses

The free radical solution polymerization of vinyl acetate in benzene was studied under simulated commercial conditions. The effects of monomer, initiator, inhibitor, and chain transfer agent concentration on the reaction rate and intrinsic viscosity were examined. The initial reaction rates with monomer concentrations from 40% to 70% and AIBN concentrations from 0.2% to 0.5% were in agreement with the kinetic equation, - d[M]/dT = K[M]² [I]^1/2. After the initial reaction there was an increase in the reaction rate apparently associated with high viscosities, which is consistent with the Trommsdorff effect. The addition of hundredths of a percent …

An Investigation Of A Gas Measurement Technique Employing Ultraviolet Excitation, Alphonso Vincent Diaz

Physics Theses & Dissertations

A study was undertaken to determine the general applicability of a temperature measurement technique which uses the fluorescence stimulated by a vacuum ultraviolet continuum as the indicator. This study was directed toward determining the temperature of nonradiating carbon monoxide. A number of ultraviolet radiation sources which produced high intensity in the region of l,150 A were investigated. This study led to the conclusion that the technique was not applicable to measurements in carbon monoxide within the present limits of' detectability.

A Study Of The Reduction Of Nickel Oxide Single Crystal By Hydrogen In A High Vacuum System., Jong In Joung

Chemical and Biological Engineering ETDs

Wafers of well-characterized nickel oxide single crystal, with (110) faces, were etched in hydrochloric acid and reduced by hydrogen in a high vacuum system. Reduction took place at temperatures of 280-310°C and pressures of 1.0-1.3 torr. The reduced wafers were replicated by carbon film and the replicas were examined by an electron microscope.

A series of reduction patterns at various stages of surface change were obtained. After a period of incubation, hemispherical metallic nickel particles, about 400 A in diameter, appeared on the parent nickel oxide surface. The number of hemispheres increased but the size of the hemispheres did not …

Fabrication Of The Pewee Nozzle; Brazing Nozzles For Rockets Powered By Nuclear Reactors, William C. Turner

Chemical and Biological Engineering ETDs

This thesis describes the steps taken to develop an improved process for brazing nozzles for nuclear-powered rockets. It defines the state of the art prior to this work. It gives an evaluation of the brazing alloys available for use. It shows the methods employed to develop the use of positive fixturing. It describes the use of full-scale sectors to refine processing. This thesis also describes the use of such new processing techniques in the successful production of two nozzles. Gold-nickel-palladium brazing alloys are used. Vacuum atmosphere performs superbly. Bands are used to hold U-tubes into slots in the shell. Problems …

Fluid Friction Reduction By Water Soluble Linear High Polymers, Arthur Edward Davis

Theses

The effects of various dilute aqueous linear high polymer solutions on turbulent pipe flow were studied to determine the polymer most suitable for testing as the drag reducing component in the proposed coating. Results of this study are presented for commercial schedule 40 1/4 inch NPS black iron pipe. Tests were conducted at Reynolds numbers of 6.2x10⁴,8.3x10⁴ and 9.8x10⁴.

Attempts were made to prepare a coating containing a friction drag reducing polymer - Polyhall 295 polyacrylamide - utilizing various techniques of polymer incorporation into the paint including several grinding and dispersion methods, adding the polymer …

A Case For University Credits For Industry's In-House Continuing Education Programs, Robert E. Carlile

Geosciences and Geological and Petroleum Engineering Faculty Research & Creative Works

The minerals industries have long recognized the tangible and intangible returns from continuing education programs for their technical scientific and administrative personnel. These programs originate from the mutual desires of the employer to upgrade the professional competence of the employee and the employee's concurrent desires to keep abreast of new developments to review the state of the art of specialized subjects and to better qualify himself to compete in an every changing technology. In-house training and continuing education programs to provide such review and education for the employee are becoming a recognized function of companies comprising this industry. These company-sponsored …

Effect Of Axial Dispersion On Interphase Mass Transfer In Packed Absorption Columns, Virendra Kumar Mathur

Doctoral Dissertations

"A steady state approach was followed in this investigation to determine the effects of liquid and gas flow rates, packing size and packing height on the interphase mass transfer coefficient and gas phase axial mixing Peclet numbers. Experiments were performed on the absorption of carbon dioxide from a mixture of carbon dioxide and nitrogen in a packed column. Absorption was performed using 1/4, 3/8 and l/2 inch Raschig rings, with a packing height of 3 feet and also using 3/8 inch Raschig rings with a packing height of 5 feet. The liquid and gas flow ranges used were 2865 to …

Drag Reduction Correlations, Gary Kent Patterson, J. L. Zakin, J. M. Rodriguez

Chemical and Biochemical Engineering Faculty Research & Creative Works

No abstract provided.

Mass Transfer From Spherical Gas Bubbles And Liquid Droplets Moving Through Power-Law Fluids In The Laminar Flow Regime, Robert M. Wellek, Cheng Chun Huang

Chemical and Biochemical Engineering Faculty Research & Creative Works

Calculated mass transfer coefficients for the continuous phase are presented for internally circulating spheres of a Newtonian fluid traveling through a power-law-type continuous phase in the so-called creeping-flow region. The Nakano and Tien stream functions allow the Sherwood number to be computed as a function of the Peclet number, power-law index, and a viscosity ratio parameter. The Hirose and Moo-Young relation is shown to be a limiting case of this numerical solution. Mass transfer rates increase as the fluids become more pseudoplastic and/or the continuous phase consistency index increases, all other factors held constant. © 1970, American Chemical Society. All …

The Cathodic Reduction Of Bromate Ions On Mercury In Neutral And Basic Solutions, Jaw-Shin Chang

Masters Theses

"The reduction of BrO⁻₃ was studied in neutral and basic solutions on a stationary Hg surface under activation controlled conditions. Coulombic efficiency studies showed that BrO⁻₃; was reduced to Br⁻ with high efficiencies. The polarization measurements lead to a proposed reaction scheme which is consistent with the experimental observations"--Abstract, page 1.

An Sem Surface Study Of Nucleate Pool Boiling Heat Transfer To Saturated Liquid Nitrogen Reduced Pressures From 0.1 To 0.9, David Virgil Porchey

Doctoral Dissertations

"This study constituted an examination of both nucleate boiling and maximum heat flux characteristics of liquid nitrogen boiling from characterized surfaces. Several textures of gold plated copper surfaces were studied in addition to silver and silver oxide surfaces. Data were taken over a wide range of reduced pressures. All surfaces were examined using a Scanning Electron Microscope (SEM). Data and micrograph comparison revealed that both surface chemistry and surface roughness affect the nucleate boiling characteristics of liquid nitrogen. These effects are separated from each other showing that nucleate boiling is a function of both surface chemistry and topography. Surface roughness …

A Study Of The Anodic Oxidation Of 1, 3-Butadiene On Platinum And Gold Electrodes, Arun Kumar Agrawal

Doctoral Dissertations

"The anodic oxidation of 1,3-butadiene on Pt and Au electrodes was studied at 70°C in solutions of H₂SO₄, K₂SO₄, K₂CO₃, and KOH with pH's ranging from 0.35 to 12.5. Reaction rates (current) were measured as a function of potential, pH, temperature, and butadiene partial pressure. A transition region (apparently a shift in the rate determining step) in case of Pt was observed in the Tafel plots. The coulombic efficiencies of oxidation to CO₂ were 85 percent in 1 N H₂SO₄ on Pt, 93 percent in 1 N KOH on Pt, and 72 percent in 1 N KOH on Au"--Abstract, Page …

The Anodic Dissolution Of Molybdenum In Acidic Nitrate Solutions, Kuan-Hsiung Hoh

Masters Theses

"The anodic dissolution of molybdenum in 1.0 N HNO₃ (pH = 0.3) , 0.1 N HNO₃-0.9 N KNO₃ (pH = 1.2), and 0.01 N HNO₃ -0.99 N KNO₃ (pH = 2.1) was investigated. The following conclusions were possible: 1. Mo is in general electrochemically oxidized to the Mo-VI state during anodic dissolution. 2. The resultant ions in solution are HMOO⁻₄. 3. The Mo surface in aqueous solutions is covered with an oxide whose approximate composition is Mo₂O₅. 4. The polarization curves have a linear Tafel region at potentials slightly above the rest potential. 5. There is no significant effect of …

Anodic Dissolution Of Zinc In Potassium Bromide-Potassium Bromate Solutions, Ying-Cheh Chuang

Masters Theses

"The purpose of this investigation was to study the anodic dissolution of zinc at a temperature of 25°C in Br⁻-BrO₃; solutions. In Br⁻ solutions, it was found that the apparent valences of zinc ions going into solution were approximately the normal value of two. Smaller values were obtained in BrO⁻₃ solutions, with the most pronounced changes occurring in the higher concentrations of BrO⁻₃. An empirical equation was derived relating the apparent valence (z_i) to the current density (amp·cm⁻²) and BrO⁻₃ concentration (gmol/liter): 2- z_i = 3.11 X i⁰̇̇¹³(C_BrO⁻₃)⁰̇⁵⁷ The mechanism for the dissolution of zinc …