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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 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 D. J. Bauer

The Bureau of Mines demonstrated the feasibility of fractionating lanthanide nitrates with a tertiary amine on lanthanum-cerium and thulium-ytterbium pairs. Optimum values were determined for pH, phase concentration, and percent chelation of metal ions in the aqueous phase. Percent extraction is markedly dependent on the concentration of lithium nitrate in the aqueous phase. Selective masking of the heavier element in each extraction system with DTPA or EDTA aqueous-phase chelating agents resulted in lanthanum-cerium separation factors of 8.5 and thulium-ytterbium separation factors of 3.4.

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 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

By N. E. Hanna

Experience with the current version of gallery test 4, in use since 1913 to evaluate the incendivity of permissible explosives in the presence of coal dust, has shown the procedure to have inadequate discrimination. Consequently the Bureau of Mines used the up-and-down method of statistical design to investigate the incendivity of permissible explosives in the presence of coal dust and gas. A suitable device was developed to measure coal dust concentrations in the air-gas mixtures and to disperse the dust in the gallery atmosphere. A proposed testing method which uses suspended shots in a predispersed coal dust-gas-air mixture was evaluated. The new method can discriminate between different explosives with respect to their incendivity. Maximum ignitibility of the coal dust cloud by permissible explosives occurred in the vicinity of 0.3 oz/cu ft. About 10% sodium chloride in permissible explosive formulations had a very significant effect in reducing the probability of igniting coal dust. Bundled charges were more incendive than column charges.

Jan 1, 1966

By R. E. Coleman

The molecular species occurring at the mineral-reagent interface of the galena-aqueous potassium ethyl xanthate system was studied by developing a technique for using an attenuated reflection method in conjunction with standard infrared spectroscopy procedures. Lead ethyl xanthate was detected from the infrared spectra of all galena surfaces treated in the pH range of 7 to 11. At pH 8.5, lead ethyl xanthate formed as a film chemically bonded to the galena surface. A solvent extraction sampling method was employed with infrared spectroscopy to obtain quantitative data on the lead ethyl xanthate removed from the galena surface. The data showed that between pH 7 and 11 thy quantity of lead ethyl xanthate physically adsorbed decreased as the pH was decreased; in the same pH range, the quantity of free lad ethyl xanthate in the aqueous medium remained constant, and the amount of unreacted xanthate varied.

Jan 1, 1966

By Jack G. Croeni

The Bureau of Mines developed a method to extrude low-density tungsten powder billets into rods and sheet bar with high-energy-rate forming equipment. Billets were compacted and sintered in an atmosphere of hydrogen to obtain a density of approximately 60 percent. Extrusion was conducted at reduction ratios of 6.25 to 1 and 9 to 1 at 1,800° C to prod e high-density, sound material. Yield strengths obtained were higher than those of material produced by conventional powder-metallurgy techniques, but ductility was lower at high temperatures.

Jan 1, 1966

By M. M. Wong

Salt mixtures consisting of KC1, BaC12, and HfCl4 with RbCl or CsCl were investigated as electrolytes for refining hafnium. The presence of RbCI or CsCl in the electrolyte appeared to suppress the volatility of. Best electrorefining was obtained with an electrolyte containing 50.7 percent KCl, 27.l percent BaCl2, 15.7 percent CsCl, and 6.5 percent HfCl4. In this electrolyte, hafnium metal with an average oxygen content of 470 ppm was produced from an anode feed containing l,600 ppm oxygen. All metallic impurities were lowered, except titanium, manganese, and tin.

Jan 1, 1966

By C. M. McKinney

The Bureau of Mines analyzed 626 crude oils from 546 oilfields in the United States that produced 2,500 BOPD or more during at least 1 of the last 3 years. Included also are crude oil analyses from eight fields that produced less but which were located in areas having few or no fields that produced 2,500 BOPD. The tables show the geographical and geological source, general characteristics. and determined and computed analytical data for each sample. The analyses were made according to the Bureau of Mines routine method and are directly comparable to other previously published analyses.

Jan 1, 1966

By Kenneth R. Farley

The Bureau of Mines developed a rapid and accurate flame photometric procedure for determining cesium and rubidium in ores and in products associated with the extractive metallurgy of these elements. The effect of associated ions is neutralized by addition of buffer solution; alkali metal effects are neutralized by parallel analyses made on standard solutions similar in composition to the sample being studied. The overall accuracy of the method is within 2.5 pct of the amount of cesium or rubidium present; the range from 1 to 25 pct is the most accurate.

Jan 1, 1966

By J. A. Cavallaro

To determine whether magnetite consumption could be reduced and salable coal production increased by using froth flotation units in series with magnetic separators, the Bureau of Mines conducted laboratory froth flotation tests on primary magnetic separator effluents obtained from three coal preparation plants. Tests were performed in a standard 500-gram-capacity laboratory batch flotation cell. Oleic acid and methylisobutyl carbinol were used as the collector and frother, respectively. Magnetite recovery was comparable to that expected from secondary magnetic separation, and salable float coal recoveries of 0,8 to 7.6 tons per hour were obtainable. The economics of the proposed technique appear to be sound.

Jan 1, 1966

By J. A. Cavallaro

The heats of formation of anhydrous barium carbonate (witherite), strontium carbonate (strontianite), and lead carbonate (cerussite) were determined by solution calorimetry. The solution mediums were hydrochloric acid for barium and strontium carbonates and perchloric acid for lead carbonate. The heats of formation at 298.15° K are as follows: BaCO3 -297.5 ± 0.8 kcal/mole; SrCO3 -294.6 ± 0.5 kcal/mole; and PbCO3 -168.0 ± 0.3 kcal/mole.

Jan 1, 1966

By T. S. Chen

A study was made by the Bureau of Mines of the temperature and thermal stress distributions in thin circular disks subjected to peripheral thermal shock at various rates of heat transfer. The theoretical analysis is based on one-dimensional radial heat flow by conduction in the disk, and on heat exchange by convection between the disk and its surroundings. Preliminary experimental data obtained from shock tests on thin circular disks of basalt, quartzite, and taconite show reasonably good agreement with theory. The case of constant properties and plane stress is treated. Solutions of the stress distribution are presented for both cooling and heating shocks. The elastic energy stored at fracture is examined, and on this basis an average stress theory is formulated. Physical properties vital to the studies include thermal conductivity, thermal diffusivity, tensile strength, Young's modulus, and linear coefficient of thermal expansion. This work is of importance in predicting the thermal shock responses of a rock body of finite size.

Jan 1, 1966

By Earle S. Burnett

Rotating piston deadweight gages have been used for many years for measurement of pressure to several hundred atmospheres. They have been calibrated by comparison of fluid pressures produced by various loads bearing on the piston bases, as measured by corresponding heights of balancing columns of mercury. When expressed in appropriate units, these ratios of column heights to piston loads are called piston constants. Experimental arrangements and procedures for their determination are presented in this paper, followed by a discussion of their significance and of their subsequent applications.

Jan 1, 1966

By A. W. Deurbrouck

This report describes the preparation characteristics of the significant coalbeds from which samples could be obtained in Webster County, W. Va. In 1964, approximately 825,000 tons of coal was produced in the county, of which 732,000 tons was mechanically cleaned in three preparation plants. The Sewell coal bed accounted for 94 percent of the coal produced. Twelve samples were collected from five coalbeds. Four of the samples would require upgrading to meet metallurgical requirements; two others of just over 8.0 percent ash would require some upgrading. In general the coalbed samples collected in the county were of medium-sulfur and medium-to low-ash content as received or after removal of the sink 1.58-specific-gravity material.

Jan 1, 1966

By Erie C. Donaldson

Gas-displacement tests were made in Berea Sandstone and Arbuckle Lime-stone cores to determine the relative permeabilities to gas, oil, and water for two-and three-phase dynamic systems. Three-phase relative permeabilities were obtained by displacing oil and water from the core with gas and measuring the flow rates of the three fluids simultaneously. It was found that relative permeabilities to fluids in a porous medium are affected by the saturation distributions of other fluids in the medium as well as by their own saturation distributions.

Jan 1, 1966

By J. P. Hansen

Reducibility tests were run by the Bureau of Mines on an open hearth lump ore and four groups of pellets whose smelting characteristics had been deter-mined previously in the Bureau's experimental blast furnace. When reduction data from various tests were plotted on specially prepared paper l-(l-percent reduction/100)1/3 against time, the plots were linear. The iron-wustite inter-face therefore advances at a constant rate. The rate of the interface advance in mm/min was used as a reducibility index. The reducibility index measured at 900° C, using 0.45 cu ft hydrogen per minute varied inversely with the surface area of the sample. Even with carefully controlled surface areas, how-ever, duplicate reducibility indices varied considerably. When enough tests were run to give a stable mean, the mean reducibility index did correlate with blast furnace production for the four pellet groups. Results indicated that if the interface speed itself were to be used for correlation with blast furnace production, a sample size of about 180 grams of minus 0.742-plus 0.525-inch particles should be used with a test temperature of 900° C and a flow of 0.45 cu ft hydrogen per minute.

Jan 1, 1966