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By Paul V. Mullins

Review and evaluation of all available data on the vapor pressure of car-bon dioxide at the ice point, including previously unpublished results obtained by the Bureau of Mines, are presented. Suggested corrections and adjustments to all the data yield an average value of 26,136.4 mm mercury. Indicated agreement is within plus 1 part in 8,000 to minus 1 part in 11,000. A novel pressure bomb in which a sample of pure carbon dioxide is placed and sealed by a diaphragm fluid separator and its use as a reference pressure standard for extended and repeated use in the calibration of deadweight gages is described.

Jan 1, 1966

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 instructions4 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; 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, 1966

By C. J. Walker

The Bureau of Mines undertook a theoretical and laboratory study to determine the feasibility of using ethylene as a tracer for natural gas in underground gas-storage reservoirs. The study indicated that ethylene was a useful gas tracer in underground gas storages. Tracer losses were not excessive. Laboratory tests were conducted at pressures as high as 500 psia in both wet and dry consolidated-sandstone cores, evaluating tracer loss with gas blends containing natural gas with different concentrations of ethylene tracer. Under certain conditions losses were less than 17 percent.

Jan 1, 1966

By H. C. Fuller

A method was devised and developed by the Bureau of Mines for decomposing manganese sulfate at significantly lower temperature than that required by the conventional procedure of using heat alone. This technique, called the partial reduction method, effected decomposition at 700° to 800° C, as compared to 900° 1,000° C normally required. The process consisted of heating, in the absence of oxygen, a mixture of manganese sulfate and a controlled quantity of a reducing agent. The suitability of commercial-type equipment was tested in laboratory-size models of an externally heated rotary kiln, a r bbled muffle-hearth furnace, and a fluidized-bed reactor. The rabbled-hearth furnace gave the best results with the least operating difficulty produced a gas containing more than 80 percent SC and eliminated 96 percent of the sulfur when coal was used as the reductant. Sintering of the powdery decomposition product produced an agglomerate containing, in percent, 63.6 Mn and 0.4 S.

Jan 1, 1966

By R. L. Hopkins

Fifteen alkyl cycloalkyl sulfides and three dicycloalkyl sulfides were synthesized to provide reference compounds in the search for these classes of sulfur compounds in crude oils. In synthesizing sulfides by alkaline alkylation the order in which the reactants were added was shown to determine the yield and purity of the product.

Jan 1, 1966

By A. J. Forney

This report summarizes the findings of methods of treating caking coals in a fluid bed to destroy their caking properties. In batch tests it was found that several coals, including those with a free-swelling index greater than 8, could be decaed at temperatures from 400° to 425° C with a fluidizing gas composed of inert gas or steam containing 0.2 percent oxygen and a minimum residence LS,-;,' of 5 minutes. When treatment decreased the free-swelling index from about 8 to 1-1/2 or lower, the resulting treated coal was noncaking. In a continuous unit with continuous feed and discharge of coal, slightly more severe conditions were required to decake the coal. For 18- to 100-mesh coal a temperature of 430° to 440° C and an oxygen-to coal ratio of 0.4 cubic foot of oxygen per pound of coal feed was necessary. Finer mesh sizes required lower oxygen-to-coal ratios. In tests using air only as the fluidizing medium and treatment temperatures well below the softening range, the caking properties of 150- to 200-mesh coal were destroyed in 30 to 40 minutes of residence time at 200° C. Coarser sizes of 18 to 48, 48 to 100, and 100 to 150 mesh required longer residence time.

Jan 1, 1966

By Leo A. Schrider

This report analyzes the successful low-pressure gas drive in the Keener sand of the Bonds Creek oilfield, Pleasants and Ritchie Counties, W. Va.) and predicts its future performance. Core analysis from two wells and electrical and radioactivity logs were used to evaluate the reservoir characteristics. Production records over a 37-year period indicate that over 240,000 barrels of oil have been produced from the Keener sand by low-pressure gas injection. Decline-curve analysis shows that 165,000 additional barrels should be recovered from 108 acres of productive sand by continuing this secondary-recovery method.

Jan 1, 1966

By Charles M. Mason

The Bureau of Mines evaluated equipment and procedures for drop-weight testing of explosive liquids as prescribed by Test 4) a widely used method. It was demonstrated that partial ignitions, originally designated as negative results, should be designated positives; it was also shown that wear or erosion of the sample cups and the type of mount used for the apparatus had important effects on the results. Relative sensitivity as measured by Test 4 was found to vary slightly with temperature. The Bureau also designed a fixed 2-kg weight and associated electromagnetic release, which subsequently were incorporated as standard in a revision of Test 4. The original concept that the test involves only adiabatic compression was found to be an oversimplification; an alternate mechanism for the initiation process is proposed in which due consideration is given to the effects of cavitation and microjets.

Jan 1, 1966

By Robert M. Doerr

The oxidation kinetics of Ni-Y alloys in the range 0.04 to 8 weight-percent Y, and of high-purity Ni, were compared by the use of a sensitive volumetric apparatus. The reactions followed approximately the parabolic rate law; for oxidations in 02 at 0.5 atm and 1,200° C, the parabolic rate constant was about 0.37 + (0.064) (Y-2.11) mg cm-2 min-1/2, where Y represents the weight-percent Y in the alloy. Internal oxidation of Y occurred in the alloy specimens and the resultant Y203 particles, which were in patterns related to the eutectic structure of the alloys, served as markers showing that the subsequent oxidation of the surrounding Ni was by inward diffusion of O. The scale consisted in each case of NiO, but the inner parts of the scale on the alloy specimens included the patterned Y203 particles. The thicknesses of the inner parts of the scale depended directly on the Y concentration, and the thicknesses of the Y2O3-free outer parts of the scale were inversely related to the Y content of the alloys. There is thus a relationship between the thickness of the outer part of the scale and the protectivity of the scale. Outward diffusion of Ni and inward movement of 0, from the inner boundary of the Y2O3-free part of the scale, is proposed as a mechanism for these results.

Jan 1, 1966

By A. L. Service

Idaho has nearly 6 billion tons of potential sources of phosphorite, 10 to 31 percent P2O5' above and within 100 feet below entry level, the largest potential of any State in the United States. In 1963 Idaho ranked third after Florida and Tennessee in total mine and marketable production of phosphate rock; Montana ranked fourth. This report describes phosphate deposits, mines, and prospects in 10 districts covering most of the Idaho phosphate field. All mine production of phosphate rock in Idaho comes from surface mines and is processed to phosphate fertilizers, phosphoric acid, and elemental phosphorus. Producing districts are Fort Hall (Gay mine), Trail Creek (Conda and Ballard mines), and Crow Creek (Georgetown Canyon mine). FMC Corp. and J. R. Simplot Co. at Pocatello have the largest elemental phosphorus and fertilizer production facilities, respectively, in the State, followed by Monsanto Co. and El Paso Natural Gas Products Co. (formerly Central Farmers Fertilizer Co.). The only other major phosphate processing plant in the State is the phosphoric acid and phosphate fertilizer complex at Kellogg operated by the Bunker Hill Co. In 1963 a plant was constructed and put on line at Monsanto, Idaho, to recover vanadium from ferrophosphorus produced by electric furnace operations in the area. El Paso Natural Gas Products Co. completed construction of a fertilizer and phosphoric acid plant near Conda in 1965. There is a small fertilizer plant producing phosphate fertilizers for local consumption in Soda Springs.

Jan 1, 1966

By H. J. Coleman

Knowledge of the types of naturally occurring sulfur compounds in petroleum is of both theoretical and practical interest to petroleum chemists and geologists. This knowledge has been extended by the identification of 77 sulfur compounds, including 36 thiols, 23 chain sulfides, and 18 cyclic sulfides in a 111° to 150° C boiling range distillate of Wasson, Texas, crude oil. The characterization procedure used in separating and identifying these compounds included isothermal distillation, vacuum fractionation, liquid-solid chromatography (alumina adsorption), chemical treatment, gas-liquid chromatography, microdesulfurization, and infrared analysis. The procedural steps described represent a systematic method of sulfur compound analysis considered applicable for determining the nature and concentration of the sulfur constituents present in any straight-run petroleum distillate of the above-boiling range.

Jan 1, 1966

By Eliot J. White

The Bureau of Mines tested cores from 35 wells from 14 oil-producing zones in southern Illinois, southern Indiana, and western Kentucky to determine why rates of water injection were apparently low in some zones. Since these zones contain only minor amounts of clay minerals, it is concluded that permeability reduction results from movement of dislodged silica particles and other material, including the clays, that lines the pores. Both single-phase and two-phase permeability measurements, however, indicated that most samples had only low to moderate water sensitivity, so that permeability reduction due to such particle movement should usually not be of practical significance. The effective permeability to water was considerably lower than the effective permeability to oil during two-phase flow measurements, as is typical of most reservoir rocks. It can be concluded, therefore, that relatively high injection pressures will be required in waterflooding thin zones or zones having low permeabilities.

Jan 1, 1966

By John M. Gomes

In the repetitive electrowinning of tungsten from scheelite, the calcium impurity buildup in the molten electrolyte results in decreased metal purity, metal recovery, and current efficiency. Periodic addition of B2O3, which reacts with the lime liberated from the scheelite, more than tripled the life of the electrolyte in winning 99.9-percent-pure tungsten and also reduced the number of units of electrolyte required per unit of tungsten recovered from six to four.

Jan 1, 1966

By Nicholls Harry R.

The Bureau of Mines studied the effect of varying the, diameter of explosive charges on the generation and propagation of strain waves. The parameters compared were strain amplitude, impulse, energy, and pulse shape. Three different explosives were detonated in three different charge diameters. Charges of cast 50/50 pentolite-detonated at the same velocity in 5-, 2.5-, and 1.5-inch diameters. Charges of ammonium nitrate-fuel oil prills and 45-percent semigelatin dynamite showed a strong detonation rate-diameter dependency. Detonation of these two explosives was considered nonideal. Differences in the diameter of the charge caused less difference in the strain-generating abilities of pentolite than in those of the other two explosives. This was also true for impulse and energy. Rise and fall times of the strain pulses for all three explosives were proportional to detonation time and cavity volume, respectively.

Jan 1, 1966

By C. W. Schultz

The vapor pressure of manganese in equilibrium with a series of liquid iron-manganese alloys was determined by the carrier gas method over a broad range of alloy composition. From these data the activities of manganese in the iron-manganese system were calculated. The system appears to be ideal.

Jan 1, 1966

By Martin H. Stanezyk

The Bureau of Mines investigated leaching of selected copper sulfide minerals and a composite of impure flotation concentrates at elevated temperatures and pressures with ammoniacal solutions. Copper 1 (tractions of 96 percent were obtained by leaching chalcopyrite at 75° C under oxidizing conditions for 60 minutes. An extraction of 99 percent of the copper contained in the composite concentrate was obtained by leaching the product for 90 minutes at 75° C. In tests of bornite, chalcocite, and covellite, 90 to 97 percent of the copper was extracted at 20° C provided an 8-hour reaction period was used. At 75° C essentially complete dissolution of the copper from these three minerals was accomplished in 60 minutes. Additions of ammonium sulfate to the leach solutions were required to obtain high-percentage extractions of the copper from bornite, chalcocite, and covellite. Although ammonium sulfate was not required when digesting chalcopyrite, copper extraction was enhanced and less free ammonia was required when ammonium sulfate was added to the leach pulps. The chemistry of leaching copper minerals was studied. It was C, termined that chalcocite altered to covellite as one step in the dissolution When leaching iron-bearing copper sulfides, hydrated iron oxide formed on the mineral surfaces, indicating that a diffusion process prevailed. No evidence of covellite was detected.

Jan 1, 1966

By Francis X. Cannaday

The Bureau of Mines developed equipment to measure the sonic velocity of pulses transmitted through rock samples varying in size from laboratory specimens to mine pillars in place. Pulses are produced by electronically excited piezoelectric ceramic transducers. Special equipment components were developed by Bureau facilities; other components are commercially available. The technique permits a nondestructive, repetitive, stable, shaped pulse to be used in place of explosive caps or hammer blows. Longitudinal wave travel time measurements were taken on an oscilloscope screen; transverse wave measurements were taken under special field conditions. Results were consistently repeatable within the accuracy of the oscilloscopes utilized.

Jan 1, 1966

By John Nagy

The Bureau of Mines adapted thermal theories explaining combustion of gases to correlate parameters affecting ignition of dust dispersions. The dust dispersions were ignited in a Godbert-Greenwald furnace at atmospheric pressure. Ignition temperature and the concentrations of fuel, admixed inert powder, and atmospheric oxygen were related mathematically. Values for these parameters obtained in laboratory experiments for cornstarch agreed with theory. The developed equation permits extrapolation; the predicted upper igni-tion limits correspond with limited experimental data from laboratory and large-scale tests. Explanation of the effect of fineness of dust on ignition parameters is attempted by introducing a surface-area constant to modify the activation energy. Arguments are presented to show that the ignition process is a solid-gas phase reaction rather than an ignition of prevolatilized gases.

Jan 1, 1966

By M. S. Oudenhoven

This Bureau of Mines investigation was conducted to obtain an experimental solution of stress changes in the vicinity of a circular opening in an infinite plate. Plates were stressed biaxially in compression and subjected, by four different-length shoes, to a uniform pressure at opposing points on the opening periphery. The principal stresses along the vertical and horizontal axes, which result from peripheral pressure, were obtained from the photoelastic analysis of four frozen-stress epoxy models. These principal stresses were then super-imposed on the mathematically determined principal stresses (along the same axes) obtained from a theoretical biaxial stress field in which the magnitude of the lateral pressure was one-third that of the vertical pressure. The results indicate that an increase in shoe length increases the radial compressive stress and the tangential tensile stress (except tangential compression at r/a = 1, which exists for all shoe lengths). Also, a partial control of the stresses within one-half radius of the opening surface is accomplished by a change in the magnitude and placement of peripheral pressure.

Jan 1, 1966

By V. E. Homme

Low- and high-temperature reduction techniques were employed by the Bureau of Mines in study of conditions favorable to the formation of massive titanium crystals. '1,1,2 low-temperature method, feeding molten sodium to solidified titanium lower chloride-sodium chloride, produced higher quality and high quantity crystalline metal. The percentage of crystalline titanium was increased with increasing reactor diameter, melt depth, and titanium dichloride concentration. The high-temperature technique, feed molten sodium to melts above 8000 C, producing needle-type crystals of lower quality and with less consistent results than the low-temperature method. Layers of titanium foil, sponge, fine needles, wool, and crusts of sin-tered granules were formed during the earl, -art of the low-temperature reduction, and massive crystals were produced beneath this barrier in the latter part of the reduction. Crystalline titanium having an average hardness of Bhn 76 and representing 58 percent of the total titanium was obtained. Lamellar crystals up to 1 1/2 inches long with a hardness as low as Bhn 54 were also produced. A second-stage reduction for reclaiming titanium from offgrade sponge is described. Titanium produced by this method was comparable in quality to that from sodium reduction of titanium tetrachloride.

Jan 1, 1966