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By R. L. Hopkins

Some typical thiacyclopentanes and thiacyclohexanes were synthesized to provide reference compounds needed for the identification of sulfur compounds in crude oils. Two general methods of synthesis were employed: (1) cleavage of 2-alkyltetrahydropyrans with hydrogen bromide followed by the reaction of the resulting dibromoalkanes with sodium sulfide and (2) the catlyzed reaction of cyclic ethers or 1)4-or 1)5-alkanediols with hydrogen sulfide. Both methods produced mixtures of 2-alkylthiacyclopentanes and 2-alkylthiacyclohexanes with 2-alkyltetrahydropyran as the starting material. The structures of the reaction products were established by analysis for sulfur; desulfurization; gas-liquid chromatography (GLC); mass, infrared, and nuclear magnetic resonance (NMR) spectra; and an alternate synthesis. The synthesis of the cyclic sulfides contributed substantially to the identification of 10 members of this class of sulfur compounds in crude oil.

Jan 1, 1967

By K. P. V. Lei

The Bureau of Mines investigated molten salt electrorefining 'n helium atmosphere cells as a means for the production of ductile vanadium. 'Electrolytes composed of NaCl-VCl2, LiCl-NaCl-VCl2, BaCl2-KCl-NaCl-VCl2 KCl-LiCl-VCl2, and CaCl2-NaCl-VCl2 were tested. Two electrolytes, KCl-LiCl-VCl2 and CaCl2-NaCl-VC12, were selected for laboratory-scale production tests. A molten salt electrorefining process was developed for the production of ductile 99.6 percent vanadium from a commercial 90-percent grade. Using the CaCl2-NaCl-VC12 electrolyte, an 87-percent recovery of ductile vanadium was made; an 85-percent recovery was made with the KCl-LiCl-VCl2 electrolyte.

Jan 1, 1967

By Hillary W. St. Clair

The reduction zone of the iron blast furnace is represented by a mathematical model of the chemical reactions and heat transfer that occurs between gas and solids during the deoxidation of iron oxide. The model consists of a set of equations and an algorithm whereby the equations may be solved to give the temperature and composition of gas and solids at any position in the reaction zone and at any time after a specified initial state. The model is applied to the special case in which ferric oxide is reduced by graphitic carbon and carbon monoxide produced by burning carbon in dry air. The rate of reduction, carbon consumption and maximum temperature are shown as functions of the temperature and rate of flow of the incoming reducing gas and external heat loss. The model of the reduction zone is the essential part of a general mathematical model for simulation of the iron blast furnace. The simulation model will serve as a research tool to be used in conjunction with an experimental or operating furnace. After the simulation model has been correlated with the real furnace, it is proposed that further experimentation be done mostly with the model. The real furnace will then be operated primarily to test and confirm the model.

Jan 1, 1967

By James A. Wasson

This report analyzes the petroleum-production potential of the basal Greenbrier dolomite zone, Sycamore-Millstone field, Sherman District, Calhoun County, W. Va., through the application of certain secondary-recovery methods. The well logs obtained and the core recovered from a well in this formation permitted an evaluation of the productive capability of the reservoir, Approximately 120,000 stb of oil may be produced from a 20-acre five-spot unit at breakthrough if the property is waterflooded. At an assumed limiting producing gas-oil ratio of 20)000 sef/stb, approximately 69,000 stb of oil should be recovered by low-pressure gas drive.

Jan 1, 1967

By Francis X. Cannaday

Equipment and techniques were developed with Bureau of Mines facilities for measurement in the laboratory of sonic shear wave velocity in variously shaped rock specimens in a wide range of sizes. A variety of rock types was tested. The shear wave front is produced by electronically excited, piezo-electric ceramic) disk-shaped transducers. Transmitter and receiver are interchangeable. Special equipment components were Bureau produced; other components were commercially available. The equipment permits quick measurement of shear wave velocity on variously shaped specimens with a minimum of specimen preparation. The technique, under favorable conditions, allows for determination of the moment of arrival of the shear wave when it is superimposed on a weak longitudinal wave.

Jan 1, 1968

By William R. Barton

Sampling to determine development potential of beryllium deposits was conducted at 31 New England localities. A total of 54 additional areas where the geochemical environment appeared favorable were sampled to determine if economically interesting percentages of beryllia (BeO) might occur. Newry Hill-Plumbago Mountain, Maine, Iron Mountain, N.H., and Long Island, Maine, were investigated in some detail to determine the size and grade of deposits. The mineralized pegmatites at Newry Hill-Phunbago Mountain are extensive but very low grade; at Iron Mountain the ore bodies are very rich but of small volume; at Long Island beryl occurs with molybdenite, wolframite, and scheelite, but the tonnage of ore was not determined.

Jan 1, 1968

By R. V. Higgins

This paper describes a method and a computer program for calculating shape factors and areas of channels that turn more than 90° and conduct fluids into the backs of wells. The program represents an improvement over a previous Bureau of Mines investigation by using a 4-point Lagrange interpolation equation instead of a 3-point and by summing areas of trapezoids with either x altitudes or y altitudes. Some of the techniques reported in this paper can also be used to compute the areas between contours and the lengths of lines that turn more than 90°.

Jan 1, 1968

By B. D. Nash

The object of this research was to investigate the technical feasibility of preparing chromium metal by the thermal decomposition of bisbenzene chromium. Bisbenzene chromium, a pi-bonded sandwich type organometallic compound, was thermally decomposed under reduced pressure to form a metal plate on a heated substrate. Metal recovery was close to 100 percent of theoretical, with deposition rates up to 20.8 mg/hr/cm2. Metal purity was dependent not only upon the purity of the starting material, but also upon the sublimation rate of bisbenzene chromium. Total detectable metallic impurities ranged from a low of 18 ppm to several hundred ppm. In general, metallic impurities were less than 100 ppm. Carbon, the major nonmetallic impurity, ranged from less than 0.3 percent to more than 10 percent. The carbon contamination is most likely a result of the decomposition of the organic portion of bisbenzene chromium. An unusual property of some of the deposits was their outstanding corrosion resistance. Unlike pure electrolytic chromium, which dissolves readily, these deposits were insoluble in hot mineral acids.

Jan 1, 1968

By N. E. Hanna

An investigation was made of pressure pulses produced by unconfined explosive blasts in underground openings. Four tests were made with TNT or modified amatol charges ranging in weight from 60 to 2,000 pounds; each test involved either single or multiple charges. Pressure-time profiles were obtained using mechanical self-recording pressure gages. The cube-root scaling law for peak pressure was found to be valid within about 1 tunnel diameter; at greater distances, the pressures obtained along direct paths were generally higher than this scaling law would indicate.

Jan 1, 1968

By F. W. Wood

The use of consumable.-electrode arc melting as a production technology is growing. One advantageous feature of this process is that it avoids ingot contamination by soluble crucible materials by employing a chilled metal crucible. Because the thermal balance under these conditions is rather delicate and does not necessarily provide a favorable environment for solidification, catastrophic imbalances can occur. The effectiveness and mechanistic roles of various factors are mostly unknown, and more intelligent insight regarding the distribution of temperature and heat is needed. Experience has provided several pertinent observations, some of which are quite superficial. The most meaningful data have resulted from studies of molten pool shapes and sizes and from measurements of heat flow through crucible walls. Overall experience, intuitively interpreted and supplemented, is sufficient nevertheless as a basis for a boundary-value treatment of the problem. A mathematical analysis based on a separation of variables, using conventional differential equation methods, provides a useful solution. For a cylindrical ingot, the temperature varies as a Bessel function of an argument proportional to the radius and as an exponential function of longitudinal position. Trial calculations using the problem solution seem to verify the general correctness of the result as compared with experience. The role and nature of solution parameters are also clarified, though not entirely resolved. It is revealed that the barrier to heat flow at the ingot-crucible surface has a prominent influence. Utility of the model embodied in the problem solution is readily demonstrated by considering a variety of contemporary questions about arc melting, and it is hoped that utility can be enhanced by improvement of the model.

Jan 1, 1968

By M. E. Tyrrell

Research objectives were to determine the reasons for erratic behavior of semisilica horizontal zinc retorts in service; to investigate potential corrective measures including the possible utilization of more refractory materials in the retort body; and to delineate laboratory tests suitable for process control in the manufacture of retorts. Correlation of laboratory test results and data supplied by the cooperating smelters indicated that structural failures due to thermal shock and laminations in the retort body are largely responsible for the erratic behavior of horizontal zinc retorts in service. The most promising modifications made in the retort body and evaluated on a laboratory scale included finer grinding of the plastic clay fraction, substitution of mullite grog for calcined fire clay and grain alumina for silica, plus the use of an organic binder. Lamination-free extrusions having excellent thermal shock resistance were prepared from a mixture composed of 50 percent low-silica Missouri plastic clay through 100 mesh, 25 percent mullite grog through 6 mesh, and 25 percent alumina through 100 mesh. The mix was pugged under 28-inch vacuum with 1 percent ligno sulfonate binder in 12 percent tempering water. Laboratory tests suitable for process control in the manufacture of retorts are described.

Jan 1, 1969

By Thys B. Johnson

Operations Research techniques for determining optimal shipping schedules and production and product allocation are discussed. A hypothetical mining operation model is formulated by the Bureau of Mines, and optimal production and product allocation are determined. The technique of sensitivity analysis is discussed and is used to illustrate the effect of the variability in a mining operation on the optimal production and product market plan.

Jan 1, 1969

By Manuel Gomez

The Bureau of Mines used data from 31 core samples to develop prediction equations for evaluating chemical and carbonization properties of six seam units in a lignite deposit approximately 2 miles wide and 8 miles long in the Wilcox Formation of central Texas. Statistical response surfaces, based on core analyses, were computed for 14 parameters indicative of lignite quality. These computed surfaces, and their mathematical equations, can be used to predict values of the selected properties of the lignite seams at any desired surface coordinate position between core hole locations. The wide range of application shown by this study indicates that the methods of statistical regression analysis may be useful to evaluate large deposits of lignite or higher rank coal.

Jan 1, 1969

By R. L. Rough

The Bureau of Mines analyzed rotary-coring-operations data to compare mud and air as coring mediums, and to compare core recoveries, penetration rates, and cost data for the respective mediums as part of an investigation of the susceptibility to secondary-recovery techniques of petroleum reservoirs in Ohio, Pennsylvania, and West Virginia. This report describes the rotary-diamond coring equipment and operations employed while coring 20 wells--10 cored using mud, and 10 cored using air. Data relevant to the draw works, rotary-table power, drill pipe, drill collars, core barrel, core head, mud pumps, or air compressors are tabulated. Average bit weight and rotary speed, core recovery, and penetration rates are listed for each formation cored. In general, core recoveries were better from the mud-cored wells, whereas penetration rates were faster for the air-cored wells. Coring costs were about the same for single-formation wells cored with either mud or air; however, costs increased considerably when multiple-formation wells were cored with air.

Jan 1, 1969

By R. L. Crosby

The Bureau of Mines investigated alloys of copper with 2, 3, and 4 vol pct alumina and with 2 vol pct yttria. Alloys were prepared by a coprecipitation process and were fabricated by pressing and sintering of powders, extrusion, and swaging. Tensile properties at room and elevated temperatures, stress-rupture strength, electrical conductivity, and density were measured. The superiority in elevated temperature strength of dispersion-strengthened copper to OFHC copper was confirmed. Increasing the oxide content from 2 to 4 vol pct produced only a small improvement in strength properties and decreased the electrical conductivity. The 3 vol pet alumina alloy had the best overall combination of properties.

Jan 1, 1969

By Donald R. Corson

The effects of adding varying amounts of type I portland cement to hydraulic backfill are described. Six different fill materials, each with three cement contents, were tested to determine which fill properties have the most significant effect on cemented strength. Two strength prediction equations, based on the physical and mineralogical properties of the fills, were formulated, and these accounted for 96 and 99 percent of the variability of the data. Results of both unconfined compression and triaxial tests of cemented fills are given, and the effects of moist curing and fill densification on the 7-day strength are discussed. Permeability test data are given, and the decreased permeability due to cement content and curing time is shown graphically. A discussion of the limited evaluation of other potential stabilization additives (expansive cement, fly ash, sodium silicate, gypsum, and asphalt) is included in an appendix.

Jan 1, 1970

By Robert G. Lundquist

The Bureau of Mines compared longitudinal strain energy output of a percussive drill to energy determined by measuring maximum piston velocity. Strain gages were used to determine the strain-time waveform and its amplitude at seven levels of operating pressure and eight levels of thrust. The longitudinal strain energy was found to be approximately 14 ft lb less than the maximum piston energy at comparable operating conditions.

Jan 1, 1969

By D. A. Keefe, O&apos

The electrowinning of beryllium from beryllium oxide (BeO) using a molten-salt electrolyte composed of 56 LiF-37 BeF2-7 BeO (mole-percent) was investigated. Anodes made of porous carbon were found to be superior in current-carrying capacity and gave a lower cell voltage than other types of anode material tested. When porous carbon anodes were used) the resultant increase in anode area prevented anode passivation. The cell voltage was 3.3 volts) and electrode current efficiencies of 50 to 70 percent were obtained. The electrodeposited beryllium was recovered as beryllium powder or was coalesced to metal beads by heating to 1,300° C.

Jan 1, 1970

By Karl C. Dean

All components of 15 automobiles manufactured between 1954 and 1965 were analyzed, and it was determined that a representative junk automobile would have the following composition (all figures in pounds): steel, 2,532; cast iron, 511; copper, 32; zinc, 54; aluminum, 51; lead, 20; rubber, 145; glass, 87; miscellaneous, 142. Time and motion studies and a cost evaluation were made to determine if such a typical vehicle could be economically burned in a smokeless incinerator and hand-dismantled, and if the resultant steel could be baled into a high-quality No. 2 bundle containing less than 0.10 percent copper. The cost evaluation showed that processing the composite car would cost about $51 to produce about $56 worth of marketable ferrous and nonferrous metal products and provide an annual rate of return on investment of 19 percent.

Jan 1, 1969

By G. L. Gates

Five possible sources of water for waterflooding of petroleum reservoirs in the arid San Joaquin Valley of California were considered. Three of them (water produced with petroleum, water from a shallow saline aquifer, and waste irrigation water) were analyzed chemically; laboratory information for one (sea water) had been developed during a previous study. A series of laboratory tests made on the fifth source (fresh water) determined the solubility of calcium sulfate dihydrate in water. Laboratory analyses included the following: Chemical analyses of water produced with petroleum and waste irrigation water; solubility of calcium sulfate dihydrate in water and brines; the effect of excess sulfate on the solubility of calcium sulfate in brines; the presence of sulfate-reducing bacteria; and the permeability of cores from a petroleum reservoir to air, to water from other petroleum reservoirs, and to waste irrigation water. The results showed that most of the waters and mixtures of waters are compatible with petroleum reservoir waters and are generally suitable for injection. The calcium content of some of the formation waters is quite high, and care must be taken to prevent precipitation of calcium sulfate dihydrate. The permeability of the few cores tested was about the same to water and brines as to air, indicating that formation damage due to clay swelling will not be serious. The waters most likely to be available for injection are water produced with petroleum, water from shallow saline aquifers, and waste irrigation water.

Jan 1, 1970