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By Leroy Dockter

The grinding characteristics of lignite in a ball mill were investigated. The variables studied were initial lignite moisture content, degree of in-the-mill drying, and lignite source. The mill tested was a pilot-p1ant-size conical ball mill which had a maximum output of from 80 to 180 lb/hr pulverized product depending on the lignite and test conditions. The capacity of the test mill ranged from 82 to 103 lb/hr depending upon mine source, in pulverization of as-mined lignite with minimum drying, The capabilities of the ball mill could not be correlated to Hardgrove index of the individual lignites or other observed physical properties. Predrying lignite from its 35 to 40 percent raw moisture content to about 10 percent moisture before grinding improved the mill capacity 87 percent, compared to an increase in capacity of 74 percent with in-the-mi11 drying to the same product moisture.

Jan 1, 1967

By R. V. Higgins

This report presents computer instructions for calculating the performance of three-phase flow of gas, oil, and water. The calculated results for an illustrative example are presented. The example is the waterflood of a reservoir containing free gas in the reservoir as a result of the partial depletion of the oil by the expansion of the gas initially in solution. The flood pattern for the example is a 5-spot.

Jan 1, 1967

By G. A. Brady

Laboratory tests were conducted to determine the technical feasibility of separating anthracite particles from a water-anthracite slurry by atomizing the water and removing the resulting mist in an air current. Products containing 21 percent or less moisture were obtained from slurries made with minus 60-mesh anthracite. Typical recoveries ranged between 67 and 79 percent of the feed when the slurries were atomized in air currents with velocities below 70 ft/min.

Jan 1, 1967

By George L. Gates

The Bureau of Mines studied pressure-buildup data from a number of California gas wells to determine if the reservoir properties calculated from these data correlated with field-observed reservoir properties. Pressure-buildup curves from 24 wells showed distinct changes in slope, indicating changes in permeability of the reservoir rock. Calculated distances from the wells to indicated permeability changes were in fair agreement with distances deter-mined in the field. Pressure-buildup curves from three wells had more than one distinct change in slope, indicating multiple permeability changes. Thus field data supported the theoretical relations used to calculate reservoir properties from pressure-time relations measured in gas wells.

Jan 1, 1967

By W. E. Anable

The Bureau of Mines studied the purification of commercially available vanadium in the 100-kw electron-beam furnace. Purification studies were conducted on a 100-gram button scale by melting and holding the liquid vanadium at temperatures ranging from 2,060° to 2,080° C at pressure of 5(10)-5 torr for periods ranging from 5 to 20 minutes. The effect of doping vanadium with carbon and metallic additions was determined. This study demonstrated that hydrogen was readily removed to 3 ppm or less, oxygen and carbon were reduced to less than 100 ppm each, and the metallic impurities were reduced Co the range of 10 to 500 ppm. The nitrogen content was not reduced in any of the buttons; rather, the nitrogen concentration generally increased as samples were held for successively longer periods. Oxygen was removed much faster and more completely when vanadium was doped with small carbon additions or one of several dopes prior to melting.

Jan 1, 1967

By Robert H. Merrill

This Bureau of Mines report summarizes the design and tests of a gage that will simultaneously measure the deformation of a borehole along three diameters 60 degrees apart; the measurements are in a single plane normal to the axis of the borehole. The inherent errors in measurement are considered together with the problems associated with the use of the gage in the relatively severe environments in and around mine openings. These problems were treated in the design and tests of the gage and the results establish that the gage can be used to satisfactorily is determine estimates of the stresses in rock.

Jan 1, 1967

By Stephen D. Cramer

The objective of the present studies was to develop thick adherent and coherent coatings of platinum and palladium on refractory metals and other substrates of industrial and engineering importance. Existing platinum and palladium electrolytes were modified to make them suitable for the electrodeposition of thick deposits. The optimum operating conditions for these electrolytes were established. Pretreatment procedures for columbium, copper, graphite, molybdenum, nickel, stainless steel, tantalum, titanium, tungsten, vanadium, and zirconium substrates were studied. New pretreatment procedures for columbium, molybdenum, stainless steel, tantalum, tungsten, and nickel were developed. The internal stress and hardness of selected electrodeposits were measured. The effects of heat treatment upon the properties of electrodeposits were studied.

Jan 1, 1967

By Heinz W. Sternberg

A method for the electrochemical reduction of the benzene ring was developed and applied to the electrochemical reduction of coal. Successive electrochemical reductions of a vitrain from low-volatile bituminous coal in ethylenediamine saturated with lithium chloride resulted in the addition of 53 hydrogens per 100 carbon atoms. Ultimate analyses and pyridine solubility of the vitrain recovered after each reduction showed that hydrogen added at the beginning has a much greater effect on solubility than hydrogen added at a later stage. Surprisingly, the removal of sulfur from the vitrain takes place only after the more reactive aromatic rings are reduced. Nuclear magnetic resonance analysis and average molecular weight determination of the extracts of the reduced vitrain samples, representing about 18 percent of the vitrain, showed that these fractions had 95 percent of their hydrogen content on saturated carbon atoms and an average molecular weight of 800 to 900. A study of the effect of operating variables on current efficiency showed that current efficiency is highest with aluminum as cathode material and with lithium chloride as electrolyte. A substantial increase in current efficiency of difficulty reducible olefinic double bonds was achieved by adding a proton donor. This result is significant in connection with the electrochemical reduction of coal which proceeds from readily reducible aromatic double bonds to difficultly reducible isolated double bonds. It is proposed that reduction is achieved by electrolytically generated and subsequently solvated electrons and hence does not require prior adsorption of the substrate at the electrode surface. This offers a distinct advantage for electrolytic reduction of sparingly or insoluble substrates such as coal.

Jan 1, 1967

By C. C. Merrill

Studies were made to determine the amenability of yttrium to fused-salt electrorefining in a controlled atmosphere. Tests were conducted in a LiCl- YCl3 electrolyte system at 710° C. The major variables studied were the YCl3 content of the electrolyte, from l.7 to 13.4 mol percent, and the initial cathode current density, from 410 to 1,630 amperes per square foot. Vacuum distillation was employed to remove salt from the deposited metal. Metallic impurities, except for lithium, could be reduced to near or below their lower analytical limits, ranging from 10 ppm for Cu to 300 ppm for Ta; reduction of oxygen content, however, was accomplished only in metal produced from electrolytes with 5.4 mol percent YCl3 or less. Initial cathode current density had little effect on the purity of the product.

Jan 1, 1967

By Robert E. Barieau

This report describes a method for treating pressure-volume-temperature (PVT) data obtained with a Burnett compressibility apparatus. The method makes use of a general nonlinear least-squares technique developed at the Bureau of Mines Helium Research Center. It is assumed that an adequate functional form is available for the expression of the compressibility factor as a function of either the molal density or the pressure. The functional form of the compressibility factor can be either linear or nonlinear in the parameters to be evaluated. Formulas are given for calculating variances and covariances of all parameters evaluated and for calculating the variance of calculated quantities of interest.

Jan 1, 1967

By D. Bienstock

The use of alkalized alumina in removing sulfur dioxide from a coal-combustion flue gas at 625° F was investigated on a pilot plant scale. The absorber was 26 feet long and 1.6 inches ED. Counter-current gas-solids flow at gas velocities of 8 to 15 ft/sec in the presence and absence of baffles, as well as solids entrainment at gas velocities of 20 to 23 ft/sec with solids recycle, were employed. The spent absorbent as regenerated as fixed bed with the reducing gases--reformed natural .7.7d hydrogen. Of absorption-regeneration were successful completed using the alkalized alumina rolled into spherical granules 10 to 16 mesh. There was no loss in activity of absorbent toward SO2 with a modest attrition equivalent to 0.l percent of the solids feed. Supporting studies were conducted on the effect of the sodium content in the absorbent, the composition of the reducing gas, thermal treatment to increase absorbent hardness, and removal of absorbed chlorine from the absorbent. A mathematical model was formulated to describe the removal of SO2 by alkalized aluminum from fixed and falling beds.

Jan 1, 1967

By L. C. George

The Bureau of Mines measured vapor pressures of selected mixtures in the binary system SnCla-ZnC12 by the static pressure method. Equations expressing the vapor pressure) and the heat and free energy of vaporization) as functions of temperature were developed by numerical analysis based on the sigma-plot method. It was found that the vapor pressure of any SnCl2-ZnCl2 mixture) at any temperature within the range of this investigation) could be accurately calculated from the derived values for the heat and free energy of vaporization for the mixture, with a probable error of 0.01 cm Hg or less.

Jan 1, 1967

By R. L. Andrews

The Bureau of Mines investigated means of electrodepositing iridium to form thick coatings suitable for the protection of such metals as tungsten and molybdenum, which oxidize rapidly at high temperatures. Using a fused sodium cyanide bath, thick, adherent, and coherent deposits of iridium up to 15 mils thick were plated on tungsten and molybdenum substrates at 600° C and current densities of 10 to 100 ma/cm2. Limited oxidation testing of molybdenum encapsulated with pure iridium indicates that the coating may offer protection to approximately l,000° C in flowing air, but that at higher temperatures, the volatility of its oxide limits use of pure iridium. Alloy coatings of iridium with platinum, palladium, and rhodium up to 4 mils thick were formed from a fused sodium cyanide electrolyte; because their oxides are less volatile, these alloys may protect substrates at higher temperatures. Deposits made from aqueous electrolytes either had very low rates of deposition or were highly stressed and cracked when heavy deposits were made.

Jan 1, 1967

By Manuel Gomez

Published experimental coke data from a pilot plant slot-type oven were examined by statistical regression analysis. Quantitative relationships were found to exist between the coking rate, bulk density, and fine grinding of the coal, sole-oven expansion, volatile matter, moisture, ash, and carbon con-tent of the coal and coke parameters indicative of size and strength. Regression equations developed from coke data were shown to yield computed values that were in good agreement with experimental results for 11 coke properties. Prediction equations developed were evaluated with an independent set of data. Present results indicate that the variables cited undergo much interaction and the sum of these interactions determines coke size and strength.

Jan 1, 1967

By Jr. Driscoll

The thermoelectric properties of yttrium monoarsenide, yttrium monoanti-monide) and ternary materials from the Y-As-Se and Y-Sb-Te systems were investigated by the Bureau of Mines from room temperature to 1,000° C. The maximum calculated figure of merit for yttrium monoarsenide and yttrium monoantimonide was 2 x 10-5 ° C-1. YAs and YSb were semimetallic conductors with low Seebeck coefficients and electrical resistivities. The values of the Seebeck coefficient and electrical resistivity of the Y-As-Se and Y-Sb-Te materials were between those of the yttrium selenides and tellurides and of YAs and YSb, respectively. The maximum power factor calculated for the Y-As-Se materials was 2 X 10-5 watt/cm ° C2 which yielded an estimated figure of merit of 6 X 10-4 0 C-1. Most of the Y-As-Se compounds had high Seebeck coefficients and moderately low electrical resistivities. The Y-Sb-Te materials were degenerate semiconductors with power factors of 6 X 10-8 watt/cm ° C2.

Jan 1, 1967

By Theodore Kessler

The purpose of this Bureau of Mines investigation was to determine what new organic compounds or high concentrations of a particular organic species can be formed by exposure of coal derivatives to ultrasonic energy. Tetralin, l-methylnaphthalene, and pyridine were used as model compounds. Gaseous and solid reaction products resulting from the ultrasonic irradiation of these coal derivatives were determined using mass spectrometry. Products from the irradiation of tetralin were studied as a function of time, atmosphere, and sample size. The sonolysis (chemical reactions produced by ultrasonic energy) of tetralin and l-methylnaphthalene produced C2H2, HCN, CH4, H2, CO, and CO2, depending upon the experimental conditions. The ultrasonic irradiation of tetralin also produced diacetylene under certain experimental conditions. The cleavage of organic chemical bonds by ultrasonic cavitation in the absence of water was also observed in this study.

Jan 1, 1967

By James H. Russell

The Bureau of Mines used a statistical approach to evaluate the effects of temperature, current density, and composition of the electrolyte on the purity of boron prepared by electrolysis of a fused mixture of boric oxide in potassium fluoborate. The quadratic equation which best fits the data was calculated for a temperature of 650° to 850° C, a cathode current density of 40 to 1,150 amp/ft2,and a boric oxide content of 0.3 to 7.1 molal. The best products, better than 95 percent boron, were obtained when the current density was less than 2 amp/ft2 and the boric oxide content was less than 2 molal.

Jan 1, 1967

By Webster S. Anderson

The design, development, and testing of hydraulic props to provide a lightweight, high strength, recoverable unit is described. Modifications in design incorporating threaded components resulted in the development of a lightweight hydraulic prop fabricated from aluminum alloy tubing. This new design facilitates interchange and replacement of component parts, and the physical properties of the material are not changed as they are when welding is required. The new prop is 65,000 pounds and has a maximum load capacity of a lower weight-to-load capacity ratio than the hydraulic props now available.

Jan 1, 1967

By J. J. Demeter

A tube-wall reactor with a Raney nickel catalyst deposited on the outer wall of the tube by flame spraying is effective in the practically complete conversion of 3H2+1CO synthesis gas to a high-Btu gas (methane) at an hourly space velocity of 7,000 volumes of gas (NTP) per hour per volume of annular volume. Partially reacted synthesis gas containing an appreciable amount of methane can also be treated in this reactor to increase the heating value to over 900 Btu per cubic foot. Excellent heat removal through the metal wall to a coolant and temperature control were obtained. The heat transfer co-efficient from the catalyst to the coolant was about 275 Btu per hour per square foot per ° F. Synthesis tests were conducted with tubes 1.2 inches in ad by 6 inches long, and 1.3 inches in od by 36 inches long. When operating at a synthesis gas rate of 100 to 120 scfh per square foot of catalyst-coated tube, catalyst life was long enough to realize a catalyst cost for the raw Raney nickel alloy of about 0.3 cent per 1,000 cubic feet of pipeline gas (900 to 950 Btu per scf). Gas recycling at ratios of 1:1 to 3:1 was effective in increasing conversion and in extending the life of the catalyst to about 16 weeks. In cost and in operating characteristics the tube-wall reactor compares favorably with the fluidized-bed and hot-gas-recycle reactor systems for the synthesis of high-Btu gas from H2+CO.

Jan 1, 1967

By J. P. Morris

The Bureau of Mines investigated the mechanics of fuming of iron-carbon melts during top-blowing with oxygen. Melts weighing 45 lb were prepared in an induction furnace and blown with oxygen by means of water-cooled lances. The rate of fuming was measured and correlated with the operating variables. The data showed that the primary cause of fuming was a boil at the bath surface in the impingement zone of the oxygen jet. Nucleation of the carbon monoxide bubbles producing the boil was apparently brought about by the precipitation of an oxide phase. The actual fuming mechanism involved partial oxidation and vaporization of bubble films and fine metal spray generated by the bursting of the bubbles. Bubbles that formed outside the impingement zone produced little fume. The distribution of trace elements between the metal and fume strongly indicated that the fume contained fine spray particles as well as particles that had condensed from vapor. The rate of fuming was found to be proportional to the carbon content of the metal) the concentration of oxygen in the jet) and the bath temperature) provided that a continuous boil occurred. In the absence of a boil) very little fume was produced.

Jan 1, 1967