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By E. G. King

Cerium and thorium sulfides have found use as crucible materials for melting certain radioactive metals. However, thermodynamic treatment of these sulfides has been hampered by lack of experimentally derived entropy values. This Bureau of Mines report describes heat-capacity measurements between 51° and 298° K, and entropy evaluations at 298.15° K, for cerium monosulfide (CeS), cerium sesquisulfide (Ce2S3), and thorium disulfide (THS2). The entropy values, with Literature results for the heats of formation, are used to obtain free energies of formation at 298.15°K. MATERIALS The samples used in this work were supplied by Prof, Leo Brewer of the Department of Chemistry, University of California. The methods of preparation and some of the physical and chemical properties of these sulfides were given by Eastman and coworkers.3 4/ Chemical analyses, conducted in our laboratory, gave the following results:

Jan 1, 1959

By R. L. Grant

An investigation was undertaken by the Bureau of Mines to determine the relationship between freespace and ignition probability for borehole shots. A series of experiments was concluded which covered six freespace conditions for a pemissible explosive in a 3/4-inch borehole and encompassed some 700 shots. The results were analyzed statistically. From the analysis of variance, it was concluded that the freespace means were different and that this conclusion is not impaired by possible differences in the explosives used. Within the limitation of this experiment, a definite relationship was found between the freespace and the ignition probability. Specifically, the incendivity increases with increased freespace up to a maximum; beyond this maximum there is some indication of decreasing incendivity. Further investigations are in progress to establish whether the effects of freespace on ignition probability reported here are applicable to the large test gallery, INTRODUCTION A borehole loaded with an explosive charge is a common feature of the routine gallery tests for determining the permissibility of coal-mine explosives, of Experimental Coal-Mine shots, and of the small steel cannon shots used in connection with certain research programs on the ignition of firedamp (6, 10).6/ The question of the interrelationship of freespace, weight of charge, and ignition probability of the methane-air atmosphere has been raised

Jan 1, 1959

By K. K. Kelly

METALLURGICAL thermochemistry of titanium is a broad subject and (if data were available) could include a wide variety of topics. The present report is restricted to extractive metallurgy and to substances and reactions that bear upon the magnesium, sodium, and hydrogen-reduction processes employing titanium tetrachloride. The aim has been to present enough data so that the reader not only can check: the calculations for the reactions discussed but also can conduct related calculations if he so desires, without recourse to other compilations of data. The subject matter divides naturally into two parts-the selection of the data to be adopted and the application of these data to pertinent metallurgical reactions.

Jan 1, 1959

By O. Q. Leone

Excellent metal quality, with lower power requirement, is attained in electrorefining titanium by using internal heating of the fused-salt bath. An internal heater provides more effective heat utilization, simplifies structural components in cell design, and prolongs cell life by eliminating direct application of heat to the cell container. This Bureau of Mines report covers one phase of the research in progress at the Electrometallurgical Experiment Station at Boulder City, Nev., for improving the techniques and lowering the total power requirement for electro-refining titanium metal.

Jan 1, 1959

By William A. Stickney

The zirconium-hafnium separation plant at Albany, Oreg., was the result of a chain of events that started with studies by A. R. Kaufmann at the Massachusetts Institute of Technology. Variations in the listed neutron-absorption cross-section of zirconium caused him to suspect a misprint. As a result of these discrepancies and following his suggestions, Oak Ridge scientists made studies establishing a value of 0.4 barn or lower. This meant that the potential of zirconium for reactor application was greatly enhanced. Since hafnium is invariably associated with zirconium and has a high neutron cross-section, it was necessary that an efficient hafnium-separation method be developed before the superiority of zirconium as a structural material in nuclear reactors could be realized. The Albany plant was built and operated for the Atomic Energy Commission (AEC) under Letter Agreement AT-(11-1) -140, patterned after a plant operated by the Carbide and Carbon Chemicals Corp. at Oak Ridge, Tenn. Construction was begun in April 1951. Hafnium was to be extracted preferentially as hafnium thiocyanate from an aqueous mixture of zirconyl and hafnyl chlorides in hexone (methyl isobutyl ketone) by a liquid-liquid countercurrent system.

Jan 1, 1959

By Carl Rampacek

Recent research by the Bureau of Mines has demonstrated that the segregation process has merit for treating oxidized and mixed oxide-sulfide copper ores. The process comprises heating the crushed ore with salt and coke or other carbonaceous materials at about 700° C. to produce fine flake copper, which then is recovered by conventional copper-flotation methods. Bench-scale laboratory tests of a number of oxidized and mixed copper ores assaying 0.78 to 5 percent Cu gave copper recoveries of 73 to 96 percent. The flotation concentrates assayed 21 to 76 percent Cu, depending on the ore being treated.

Jan 1, 1959

By E. G. King

This paper reports measurements of low-temperature heat capacities and entropies at 298.15° K. of two copper ferrites (CUFe204 and CU0.75Fe2.2504). These substances, which occur in copper-smelting slags, have not been sujected to any previous direct thermodynamic investigation. The two copper ferrites are spinel minerals of the variate class. In previous investigations similar data were obtained for 13 other spinel minerals -7 of the normal class and 6 of the variate class. The entropies at 298.15° K. of these minerals have been compiled and revised as necessary in the light of present knowledge regarding structural randomness; entropy values, recommended for use in thermodynamic calculations, are listed.

Jan 1, 1959

The complex organic chemicals in coal differ from those in petroleum mainly by the ratio of carbon atoms to hydrogen atoms; this ratio is about 2 for coal and 1 for petroleum. By changing the ratio, coal can be converted into compounds similar to those found in petroleum. In. very simplified form, omitting here the special conditions required, the paths by which this can be done are: [ ] Part or all of the coal is first gasified by reaction with steam and oxygen, either in a gasifier or while the coal is still in place underground. The resulting gas is mainly hydrogen and carbon monoxide, with impurities that .must be removed before further processing by one of the following routes.

Jan 1, 1959

By Victor Kalcevic

A gas-flow retort for thermal processing of oil shale to recover shale oil was developed by the Bureau of Mines at its Oil-Shale Demonstration Plant, Rifle, Colo., from 1948 to 1952. The retort is a crossflow gas-to-broken-solids heat exchanger. The heating medium is the gas produced in the shale retorting process. The gas is heated in specially designed stoves outside the retort and recycled to the retort. Oil shale from the Mahogany ledge section of the Green River formation in northwestern Colorado was the material processed. Indicated maximum oil recoveries for 20-to 25-gallon-per-ton shale in a l2-inch-thick shale bed and a 20-inch bed are 96 and 91 weight-percent of Fischer assay, respectively. Heat requirements for maximum recovery are 600 to 750 B.t.u. per pound of shale. Properties of the recovered shale oil are affected slightly by shale-bed thickness and extent of retorting. Oil recovery from oil shales assaying over 30 gallons per ton is lower than that from leaner shales.

Jan 1, 1959

By Thomas C. Atchison

The purpose of this Bureau of Mines investigation was to measure the amplitude and shape of the strain pulse and the size of the crushed zone produced in a granite by different explosives and to determine how these quantities are related to the detonation properties of the explosives. The reflection theory of rock breakage has shown that the amplitude and shape of the strain pulse incident at a free surface determine the fragmentation and volume of rock broken. Determination of the properties of an explosive that control the characteristics of the strain pulse produced in the rock will help in evaluating explosives for use in blasting. The investigation showed the different explosives produced a twofold variation in the amplitude of the strain pulse but little variation in the shape of the pulse. The explosives also produced a twofold variation in the volume of the crushed zone, but differences among the explosives were more accurately determined by strain-amplitude measurements than by crushed-zone measurements. The peak amplitude of the strain pulse and the volume of the crushed zone correlated with the calculated detonation pressure of the explosive.

Jan 1, 1959

By E. G. King

Existing thermodynamic data for compounds of the rare-earth metals are few in number and often inaccurate because, in the past, it was difficult to obtain samples that were pure enough and reasonable in cost--a situation that is rapidly improving. This paper reports the results of low-temperature heat-capacity and high-temperature heat-content measurements for cerous fluoride (CeF3) and supplies the first such published data for a rare-earth fluoride. The low-temperature heat-capacity data cover the temperature range 51°-298° K. and serve to evaluate the entropy at 298.15° K. The high-temperature heat-content data cover the temperature range 298°-1,799° K., including the temperature and heat of fusion. The results are assembled for ready use in thermodynamic calculations. Cerous fluoride is one of the important intermediate compounds in the production of cerium metal.

Jan 1, 1959

By R. F. Zaffarano

Data presented on the physical characteristics of the reservoir oil, Aneth field, represent the initial phase of a study of Paradox basin reservoir oils being made by petroleum engineers of the Federal Bureau of Mines, Petroleum Research Center, Laramie, Wyo. The purpose of the study is to determine the original reservoir-oil characteristics in several important new discoveries in the Paradox Basin and to investigate correlations between the properties of these reservoir oils and structural or areal position within the basin, If migration is limited and oil accumulates near its source, then it seems probable that few differences should be found in the composition and characteristics of reservoir oils occurring in given age rocks and within the confines of a geological basin. Within these limits, conditions that effected the formation of oil and its transfer from parent to storage rocks probably were rather uniform in an area the size of most of our geological basins. However, if oils should migrate considerable distances, it seems logical to expect that the relative quantities of gas and liquid components may differ in traps occurring along the direction of migration, corresponding with the theory of differential entrapment (5).4/

Jan 1, 1959

By W. V. Kuster

The investigation described in this report is part of a survey by the Federal Bureau of Mines of the titanium resources of the United States. The purpose of this project was to study a typical coastal deposit of beach sands in the Middle Atlantic States, particularly in the area surrounding the Delmarva Peninsula. The field investigation consisted of a reconnaissance survey of the Eastern Shore of Maryland, followed by surface sampling and drilling of the sands on Assateague Island, off the Atlantic coast of Maryland. The study covered the period January-December 1957. Detailed analyses were made of 5-foot sections of eight drill holes along the Maryland section of the island. The heavy-mineral fraction of these samples was separated by sink-float tests, using acetylene bromide as the heavy liquid. The minerals comprising the heavy fraction were examined microscopically, and mineral counts were made on selected samples.

Jan 1, 1959

By D. A. Douglass

This report describes the tri-n-butyl phosphate extraction of cerium (IV) from a sulfate leach liquor prepared from a bastnaesite concentrate as well as from pure eerie nitrate solutions. The work was done on a laboratory scale using separatory funnels. Extraction from pure cerium solutions entailed no great difficulties; however, extraction from the bastnaesite solution proved more difficult, mainly because of the inhibiting effect of the sulfate ion. Despite this, procedures were developed for obtaining good single-state cerium extraction (95+ percent) and a high-purity product (99+ percent), although the maximization of both cannot be achieved simultaneously. This necessitates a compromise in any extraction scheme.

Jan 1, 1959

By David E. Fogelson

The breakage of rock by explosives depends largely on the ability of an explosive to transfer its stored potential energy to the rock as strain energy. Therefore, the relative rock-breaking abilities of explosives can be determined indirectly by determining the relative amounts of strain energy transferred to the rock at the time of detonation. This report presents experimental data on the strain energy contained in explosion-generated strain pulses in a granite gneiss. Six explosives were tested. The scaled total radial strain energy Es/W flowing outward through a spherical shell of scaled radius R/W1/3 surrounding the point of detonation was found to follow an exponential decay propagation law of the form [ ]

Jan 1, 1959

By Lloyd H. Banning

ELECTRIC smelting tests were conducted at the Northwest Electro-development Experiment Station, Albany, Oreg., to develop a feasible process for producing silicomanganese from siliceous manganiferous material. The Jackson County, Oreg., material used was massive and contained rhodonite as the most abundant mineral. Both raw and beneficiated materials were tested; various proportions and types of fluxes and reductants were used to make up the furnace charges. The silicomanganese product was used successfully in manufacturing various steels at industrial plants. The manganese content of the samples ranged from 23 to 28 percent; silica plus alumina content was as high as 55 percent-about four times the maximum specification for Metallurgical-grade ore. Sink-float laboratory tests indicated that the manganiferous material was amenable to beneficiation. Over 2 tons of rhodonite concentrate was prepared for smelting tests in a sink-float operation. Only the minus-3/4-inch, plus-8-mesh fraction was fed to a heavy-medium cone; over 97 percent of the manganese was recovered in the sink product, which contained 32.4 percent manganese and 44 percent silica plus alumina. About 25 percent of the silica was removed in the float product.

Jan 1, 1959

By V. B. Dale

This is one of a series of reports covering the mineral resources of the Nation. It describes briefly most of the known tungsten deposits in Yuma, Maricopa, Pinal, and Graham Counties, Ariz. Most of those described were examined by the author. An effort was made to determine the position of the various deposits by section, township, and range and to give accurate road direction to each property from a prominent landmark. All available maps have been used in making these determinations, but in unsurveyed areas it was necessary to make approximate projections of subdivisions. The township and range numbers refer to the Gila and Salt River base and meridian.

Jan 1, 1959

By V. B. Dale

This paper is one of a series covering the mineral resources of the Nation. It briefly describes most of the known tungsten deposits of New Mexico. Most of the descriptions are from field examinations by the senior author. Reported tungsten occurrences that were not visited are listed below: Colfax County: Occurrences of ferberite in thin veins in Willow Creek near Elizabethtown.4/ Dona Ana County: Small, low-grade occurrences of scheelite near the summit of the Organ Mountains about 15 miles east of Las Cruces. Hidalgo County: Scheelite reported in the Daisy mine 7 miles southeast of Hachita. Ores are carbonates containing copper, gold, silver, and bismuth.5/

Jan 1, 1959

By R. J. Leary

The natural gas-air burner described in this report was designed and constructed to meet the thermal requirements of a convective process for heating steel scrap. This process involved downward combustion of natural gas with air, blending the combustion products with diluent air, and then passing this tempered stream of gases downward through a porous bed of steel scrap contained in the furnace chamber. The scrap would be heated to a temperature limited by the adiabatic flame temperature of the gas stream in a period that depended on the rate at which heat was supplied per unit of bed cross section. The temperature of the gas stream would be limited to that beyond which an objectionable degree of oxidation would occur; for carbon steel this limit had been found to vary from 1,900° to 2,100° F. with the superficial velocity of the gas stream. The productivity of the process was dependent on the rate of heat input per unit of furnace cross section; for the 3-foot-diameter experimental furnace an input of 680,000 B.t.u. per hour was desired. The burner described was designed to meet these conditions of temperature and heat input. It provided for three streams of entering gases: (1) A primary air-fuel mixture too rich to be combustible, that is, above the upper flammable limit; (2) secondary air for combustion of the primary mixture; and (3) tertiary air, principally for cooling the combustion products to the temperatures desired for process operation. Downward combustion of the primary and secondary streams occurred in a flame stabilized on an annular port, while tertiary air flowed in an annular path surrounding the port and also through an axial channel whose wall formed the inner ring of the annular port. This burner performed beyond the designed heat-input rates while producing stable flames, which were adjusted readily to the temperatures desired. Gas-stream temperatures were easily controlled to within 15° F. of the desired value by simple manual adjustment of the flow valves.

Jan 1, 1959

By John J. Mulligan

Since 1941 the Federal Bureau of Mines has been conducting an intermit-tent program of placer and lode investigations to evaluate the potential tin resources of the western Seward Peninsula tin belt. Previous investigations were made in the Potato, Cape, Brooks (Lost River), and Ear Mountain areas. As part of this program the Bureau made a reconnaissance of reportedly tin-bearing stream gravels in areas adjacent to the previously worked tin deposits at Lost River and Potato Mountain. The objective of the reconnaissance was to determine if additional areas might be favorable for lode or placer exploration. The work was begun late in the fall of 1956 and completed during the following summer. The streams sampled were the Lost River and York Creek in the Brooks Mountain area and the Anikovik River and Kigezruk and Baituk Creeks in the York area. Samples were obtained by churn-drilling methods employing conventional placer-evaluation procedures. Holes were drilled at wide intervals at sites chosen as being representative of drainage areas rather than of individual gravel deposits. Minor to trace amounts of tin were found in the gravels of all these streams, but the highest grade was 0.35 pound of tin per cubic yard in the gravels of Lost River below the mouth of Tin Creek. Small amounts of gold were found on Baituk Creek and in one hole on the Anikovik River; the highest grade did not exceed 10 cents per cubic yard. Traces of scheelite and barite were found on York Creek, chromite was encountered in one hole on the Anikovik River, and minor amounts of titanium minerals (probably derived from basaltic intrusives) were found in the York area.

Jan 1, 1959