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By W. J. Wenger

Oil fields in the Powder River Basin of Wyoming have produced 731 million barrels of petroleum through 1959. Production in 1959 was 32 million barrels, the highest production since 1924. The record production was in 1923, when the Basin produced 38 million barrels of oil and the Salt Creek field, then at its peak, produced 35 million barrels. In this report, the characteristics of crude oils found in the Basin are used as a basis for determining the best re-fining uses for the oils and for predicting the characteristics of oils that may be discovered in the Basin in the future. Analyses of 108 oils sampled over a period of 30 years are presented Crude oils of two major types are produced from the Powder River Basin. One has a low sulfur content and occurs in younger formations, and the other has a high sulfur content and occurs in older formations. The oils with low sulfur contents are generally light colored and waxy, and may be either paraffinic or naphthenic. The oils with high sulfur contents are usually dark colored and asphaltic; only their low boiling fractions are paraffinic. Alteration appears to account for the anomalous properties of some oils found at shallow depths. Shapes and slopes of correlation index curves classify the oils into the same two groups as their sulfur contents, with gently sloping curves representing the low-sulfur oils and steep curves representing high-sulfur, asphaltic oils,

Jan 1, 1961

By R. S. McClain

The Federal Bureau of Mines investigated residues from aluminum plants, to determine if carbon could be removed by flotation while recovering fluorine and aluminum compounds for recycling to the reduction process. This publication summarizes studies on samples representing three types of plant waste products, supplied by three aluminum-producing companies. Samples of flue dust, pot skimmings, and pot linings from the various plants all responded to a simple turpentine flotation scheme to reject 90 to 97 percent of the carbon. Aluminum compound recoveries ranged from 42 to 94 percent on the flue dust, were about 95 percent on the pot skimmings, and ranged from 75 to 89 percent on the pot linings. Fluorine recoveries from the same samples ranged from 35 to 63, 92 to 95, and 77 to 86 percent, respectively. The pot linings contained soluble salts of aluminum and fluorine which were recovered by precipitation with sodium aluminate and carbon dioxide gas. Composites of residues from each plant responded to flotation much the same as the individual samples. Aluminum is produced by the electrolysis of alumina in a molten cryolite bath. The electrolytic reduction cell consists of a carbon-lined box containing a pad of molten aluminum which serves as a cathode, a carbon anode, and an electrolyte of molten cryolite in which the alumina is dissolved. Alumina is reduced to aluminum at the cathode, and carbon is oxidized at the anode.

Jan 1, 1961

By H. D. Hess

This report presents the results of laboratory mineral evaluations conducted by the federal Bureau of Mines under the joint sponsorship of the U.S. Atomic Energy Commission (AEC) and the Bureau a! Ships, U. S. Department of the Navy. The major purpose of this investigation was to examine and evaluate zirconium minerals representing sizeable deposits in an effort to locate com¬mercial sources of high-hafnium ores. Although determination of the hafnium content was the principal objective, each of the zirconium minerals also was analyzed for combined zirconium-hafnium oxide, silica, uranium, thorium, yttrium, and cerium. The general laboratory procedure involved microscopic examination of the test samples, concentration of the hafnium-bearing zirconium mineral by standard laboratory techniques, and analysis of the derived concentrate by quantitative microscopic, chemical, and X-ray spectrographic methods. Of the several hundred samples tested under this program, 147 are discussed in this report, including 94 from domestic occurrences and 53 from widespread foreign sources.

Jan 1, 1962

By F. E. Brantley

Research was undertaken by the Bureau of Mines to assess the technical feasibility of smelting cement-copper precipitate in an electric furnace to produce commercial-grade copper. The blister-grade copper produced in smelting was refined by gaseous oxidation and reduction methods to rive a product equal in quality to fire-refined copper. The cement copper used in the study was typical of the material produced in commercial operations. The sample product was received in a partially oxidized state and analyzed 77.5 percent Cu, 3.4 percent Fe, 0.8 percent Pb, 0.05 percent Ni, 0.6 percent Sn, and 0.9 percent S. Smelting tests were made on the precipitate using laboratory-size induction and electric-arc furnaces. Three types of furnace linings were tested during, the investigation: Carbon, including graphite; clay-graphite; and silicon carbide. Although all proved satisfactory, either carbon or graphite was preferred because of their superior refractory properties and low permeability to molten copper. Copper recoveries in the induction and arc smelting tests averaged 92 percent in commercial-grade metal assaying 99.8 percent copper. Refining the molten copper by oxidation and gaseous reduction or by chlorine lancing increased the purity to plus 99.9 percent.

Jan 1, 1961

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By E. D. Calvert

This Bureau of Mines report discusses the electric-arc reduction of zirconium and hafnium oxides with carbon yielding a metal-metallic carbide mixture. The carbon to oxide ratio in the feed determines the metal to carbide ratio in the product. A sample of this product was produced -or testing as a feed for the deBoer iodide-dissociation process. A new technique for producing pure carbides is described, which uses the intense heat of the arc to volatilize the carbide. The condensed vapor form , crystals of nearly stoichiometric carbide, INTRODUCTION This research examines the preparation of refractory metal carbides in the controlled atmosphere electric-arc furnace.

Jan 1, 1962

By R. Barany

In this paper, closed expressions have been obtained for the frequency spectrum of a Born-Karman square lattice in terms of elliptic and hyperelliptic integrals. This work is part of continuing research by the Bureau of Mines with the thermodynamic properties of metals and minerals. Although other workers have obtained various types of approximations for the general case of the frequency spectrum of a square lattice, no one previously has obtained closed analytic expressions for this spectrum. To understand the optical and thermodynamic properties of crystals, several investigators have studied the distribution of frequencies of normal modes of vibration of the crystal lattice. Born and Karman3 laid the foundation for the theory of lattice dynamics and obtained detailed results for the case of a one-dimensional lattice. Blackman4 used numerical techniques to estimate the frequency distribution of a two-dimensional square lattice. Mbntroll5 analytically determined the frequency distribution of a square lattice for a particular value of the force constants. He also studied the more general problem and obtained some analytic approximations, using the method of moments. However, the calculations by this method were so difficult that it was not always practicable to carry them out. Van Hove6 and Montroll7 studied the nature of the singularities in the frequency spectrum of both a two and

Jan 1, 1962

By Frank A. Peters

This evaluation of the sulfurous acid process for the production of metallurgical-grade alumina is the first of a series concerning various known methods of extracting alumina from low-grade aluminous materials and was undertaken to permit comparison with other processes. In the process with which this Bureau of Mines report is concerned, calcined clay is leached under pressure with 20 percent sulfurous acid and then filtered to remove a siliceous residue. The aluminum sulfite remaining in the filtrate is precipitated as a monobasic sulfite which, together with iron sulfite, is then decomposed under pressure to form a crude alumina hydrate and iron oxide. This intermediate product is purified in a modified Bayer process to yield alumina suitable for electrolytic reduction to aluminum. A study estimate (16)3 is used for these evaluations. The capital cost, not including land, is estimated at $95,701,600 on a Marshall and Stevens index basis of 240.0 for a plant producing 1,000 tons a day of alumina or 350,000 tons a year. The annual operating cost for this size plant is estimated at $22,831,100 or $65.23 per ton of alumina using clay at $1 per ton. Depreciation and local taxes are included in the estimate, but profit and Federal taxes are not considered.

Jan 1, 1962

By David E. Fogelson

One model each of three different makes of portable displacement seismographs was calibrated on a shaking table capable of 5,000 pounds of force, Calibration tests were conducted in the frequency range of 5 to 200 c.p,s, and in the amplitude range of 0,002 to 0.05 inch peak-to-peak, The seismographs were tested under two mounting conditions: (1) The feet of the instrument were bolted to the shaking table, and (2) the feet were resting on emery cloth affixed to the table, The results of these tests show that, in the frequency range of 5 to 40 c.p,s, and for vibration levels less than 0.2 g, the magnification for all three instruments is constant with input level but varies slightly with frequency. For vibration levels greater than 0.4 g. and for frequencies greater than 40 c.p.s., the magnification of all three instruments shows large variations with frequency and amplitude of table motion.

Jan 1, 1962

By E. D. Calvert

The objective of this research was to examine variations in melting and forging practice for four titanium-base alloys and to determine their effect on the resultant product. Of particular interest was the evaluation of the skull-casting technique. The data should serve as a guide to producers and consumers of titanium products. Physical properties of four titanium-base alloys in ingot form and in sheet form were evaluated and correlated, where possible, with variations in the melting and casting procedure. Consumable-electrode melting was used throughout, but arc current and furnace backfill pressure were varied, and ingots were formed both by melting directly into a water-cooled copper mold and by skull melting followed by pouring into a graphite mold. Alloying metal additions for the alloys tested were (1) 8 percent manganese, (2) 6 percent aluminum and 4 percent vanadium, (3) 6 percent molybdenum and 2 percent aluminum, and (4) 16 percent vanadium and 2.8 percent aluminum.

Jan 1, 1962

By E. G. King

As low-temperature heat-capacity and entropy data were available for only one sesquisulfide (cerium sesquisulfide), it appeared desirable to augment the information for this class of compounds by measuring the sulfides of antimony and indium. In addition a pressing need existed for data on indium sulfide to supplement vaporization studies in progress in the Department of Mineral Technology, University of California. This Bureau of Mines paper reports low-temperature heat-capacity measurements and entropy evaluations at 298.15° R. of antimony sesquisulfide of stoiehiometric composition (Sb2S3) and of indium sesquisulfide which was somewhat deficient in sulfur (In2S2.93). The data for the latter substance were adjusted to correspond to the stoichiome tric composition (In2S3 ) . Indium sesquisulfide has a lower entropy at 298.15' K, than either antimony sesquisulfide or cerium sesquisulfide, in line with the higher atomic density of the indium compound.

Jan 1, 1962

By J. P. Capp

The Bureau of Mines conducted field-scale experiments in underground gasification of coal with oxygen-enriched air. A path about 140 feet long was linked at the rate of LO feet per day through a coalbed hydraulically fractured with a mixture of starch gel and sand. During the best gasification period, which extended for 2-1/2 days, 785,000 std. c.f. per day of 124-B.t.u. gas was produced. In other periods the heating value at times was almost 300 B.t.u. per std, c.f,, but sustained production of such gas was not achieved. During gasification, a total of 50 tons of coal was gasified and 114 tons of coal was carbonized. Approximately 12 million B, t .u. per foot of nominal path was recovered at the surface.

Jan 1, 1962

By Oliver C. Fursman

These investigations were conducted to determine conditions for recovery of nickel and copper from Funter Bay, Alaska, sulfide ore and recovery of nickel from nickel-silicate ore, Nickel Mountain, Riddle, Oreg. Samples of Funter Bay cupriferous and nickeliferous pyrrhotite ore, were treated by beneficiation, roasting, electric smelting of roasted are for matte production, chlorination, leaching, and sulfatizing roasting with subsequent leaching. Funter Bay and Nickel Mountain ores were smelted together to produce matte. Total sulfide flotation, followed by magnetic separation of the tailings to recover entrained nickel-bearing pyrrhotite, resulted in the highest nickel recovery in beneficiation tests on Funter Bay are. Overall beneficiation resulted in recovery of 98.5 percent of the copper and 95.4 percent of the nickel in the concentrate that contained 3.5 percent copper and 1.7 percent nickel.

Jan 1, 1962

By John J. S. Sebastian

A laboratory-scale investigation was made of the basic problems involved in developing a ceramic heat exchanger to operate at high temperatures for using nuclear heat from gas-cooled process-heat reactors. Technical data were obtained on transferring heat by forced-convection from helium to air in a single-tube vitreous-alumina heat exchanger. Coolant air was passed through the annulus parallel with, and either concurrently or counter to, the flow of helium inside the tube. The data obtained pertain to removing heat from the helium. Average inside film coefficients were determined at mean surface temperatures of 200° to 1,570° F., inlet-gas temperatures of 1,450° to 2,665° F., and Reynolds numbers up to 560. The gas-to-surface temperature ratios were varied from 1.05 to 7.6. The tabulated results are shown in the appendix at the end of this report. The film coefficients of heat transfer were correlated by taking into account the physical properties of the helium at the average fluid temperature. With experimental conditions pointing to a laminar flow, the Nusselt number was found to decrease as the ratio of gas-to-wall temperature was increased to a value of 3. However, within the range tested, gas-to-wall temperature ratios above 3 did not affect the Nusselt number, regardless of the value of the Graetz number. Thus, beyond this point any increase in this ratio ceased to influence the heat-transfer relationship.

Jan 1, 1962

By E. R. Palowitch

Two samples of the Lower Hartshorne (Spadra) bed were collected: A sample of the raw coal with the machine cuttings excluded, and a sample of the machine cuttings exclusively. Analysis of the 5-inch by 200-mesh size fraction of the raw coal, excluding machine cuttings, showed that a product meeting minimum quality specifications could be produced by washing at 1.60 specific gravity, yielding a theoretical 93.7 percent of clean coal. A negligible amount of near-gravity material at the separation gravity indicated an easy washing problem. The sample of machine cuttings had a maximum size of 2 inches and contained about 50 percent ash. Washability tests of the 2-inch by 200-mesh size fraction indicated that a theoretical yield of 30.0 percent of specification-grade coal could be achieved by washing at 1.49 specific gravity. As the machine cuttings represent an estimated 10 percent of the total coal mined, their inclusion in the mine output would increase the theoretical net yield of salable coal by only 3.7 percent. Because the machine cuttings contained a high percentage of sink 1.80 specific-gravity material, they had neither an effect on the separating gravity required to clean the raw coal nor on the difficulty of separation. Gabbing underground versus transporting the cut-tings to the surface for disposal or washing either separately or combined with the raw coal involves a number of practical, economic; and intangible factors; hence, no specific recommendations could be made. A discussion of some of the factors involved in dealing with a similar problem is given by Gandrud and Riley.4

Jan 1, 1962

By Eugene L. Grumer

High-expansion foam was applied to the flames of six fuels burning in a 1-foot-diameter tray. The flames of three hydrocarbon fuels were more readily extinguished than the flames of methanol, acetone, or unsymmetrical dimethyl hydrazine. The result is rationalized on the basis that heat transfer from flame to fuel surface is primarily radiative with the hydrocarbons and more largely convective with the nonhydrocarbons. INTRODUCTION Equipment for producing high-expansion foams has been developed by the Bureau of Mines to control coal mine fires.5 Recently such equipment has been redesigned for portability and has now been produced commercially for other fire-fighting applications. In May 1961, a 50-by 50-foot gasoline fire was extinguished within 2 minutes by a trailer-mounted foam unit that produced 12,000 cu.ft./min. of high-expansion (1,000:1) foam.6

Jan 1, 1962

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1962

By P. R. Tisot

Knowledge acquired from this research contributes to a better understanding of the physical structure of Green River oil shale and provides fundamental data and concepts that may serve to improve oil-shale technology. This study by the Bureau of Mines indicates that oil shale is a highly consolidated organic-inorganic system with no significant micropore structure, pore volume, or internal surface. This system is a form of physical structure that precludes rapid diffusion of either gases or liquids. The mineral matter consists essentially of nonspherical particles that tend to follow a log-normal size distribution. An excess of 99 weight-percent of these particles have equivalent spherical diameters of less than 44 microns--75 weight-percent are from 2 to 20 microns, and 15 weight-percent are less than 2 microns. The surface area (3 to 5 square meters per gram) of these mineral constituents is mainly external surface. The mineral constituents contain some micropore structure--pore radii ranging from 10 to 100 Angstrom--with the pore sizes randomly distributed. Distribution of the organic matter within the inorganic matrix is essentially interparticle and not intraparticle. The organic matter within the micropores of the mineral constituents is less than 4 percent of the total. Estimates made from surface area data suggest that perhaps only a small amount of the organic matter is bonded either physically or chemically to the mineral constituents.

Jan 1, 1963

By D. Bienstock

To develop a rugged catalyst capable of withstanding hydraulic attrition resulting from the oil-circulation process for synthesizing liquid fuels, use of an iron catalyst containing an active coating surrounding an inert solid core of metal was investigated. This massive-iron catalyst in the form of steel shot and lathe turnings was activated by partial oxidation with steam at 600° C, impregnated with alkali, and reduced with hydrogen at 450° 6. The massive-iron catalysts were resistant to oxidation and spalling, and a 6-month catalyst life was attained. Higher operating temperatures could be employed than with fused iron oxide catalysts, resulting in greater gasoline yields. Because the lathe turnings pack with void volumes of 70 to 90 percent, it has become possible to employ a fixed bed without the danger of cementation that occurs with fused iron oxides.

Jan 1, 1963

By C. J. Chindgren, L. C. Bauerle, J. B. Rosenbaum

Modifications of the conventional method of preparing ductile vanadium metal by calcium reduction of V2 05 in a bomb were explored for clues to a more economical procedure . The modifications examined included ( 1 ) omitting the gas purge of the bomb ordinarily used for eliminating atmospheric nitrogen , (2 ) using low- grade vanadium feed materials , ( 3 ) using alternative reductants , such as aluminum , magnesium , and silicon , and reductant mixtures , and ( 4 ) bomb refining of aluminothermic metal produced in open- vessel reductions . The most promising modification appeared to be bomb refining , using calcium to purify vanadium metal -- of low aluminum but high oxygen content-- prepared by open- vessel aluminothermic reduction of vanadium pentoxide .

Jul 1, 1960