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By T. N. Rushton

Rate minima are encountered in the reduction of magnetite with hydrogen. In a certain temperature zone, the reaction rate decreases with rise in temperature. This is inexplicable by classical kinetic theories; neither is a transition in reduction mechanism suitable for interpreting the observed behavior, This anomaly can be fully explained by hypothesizing two species of chemisorbed hydrogen with different adsorption coefficients and activation energies for adsorption. Competition between two energetic states of adsorption occurs with temperature rise, with the low energy state predominating below the anomalous temperature zone and the high energy state above it. The presence of two possible adsorption sites appears to be characteristic for oxidic adsorbents.

Jan 1, 1968

By Wesley T. Holmes

This report describes the first phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected slag compositions in the titania-alumina-silica-calcia-magnesia system. Both the melting-holding-quenching method and the hot-stage microscope method were used in the tests. Liquidus temperatures of slags studied ranged from 1,217° to 1,667° C. The lowest liquidus temperature of the slags occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. Liquidus temperatures were also lowered when Si02 was substituted for Ti02 plus Al2O3 when CaO and MgO levels were held constant. Improved methods for the measurement of liquidus temperatures on very small samples are described.

Jan 1, 1968

By T. A. Sullivan

Refining in a molten salt electrolyte was investigated as a means of recovering nickel containing less than 1 percent and preferably less than 0.2 percent cobalt from nickel products containing up to 5 percent cobalt. Electrolytic separation of nick and cobalt was accomplished in a molten KCl-LiCl-NiCl2 electrolyte. Nickel containing less than 0.10 percent cobalt was routinely prepared. Factors that influenced the transfer of cobalt to the refined product were the nickel concentration of the electrolyte, the cobalt concentration of the electrolyte, the ratio of nickel to cobalt in the electrolyte, and cathode current densities. A method of recovering the cobalt from the electrolyte was developed. The possibility of preparing high-purity nickel by this process was shown, as well as the preparation of various cobalt-nickel-tungsten alloys.

Jan 1, 1968

By Wesley T. Holmes

This report describes the second phase of an investigation aimed at obtaining a wider knowledge of the problems involved in smelting titaniferous magnetites. Liquidus temperature measurements were made on selected synthetic slag compositions in the Ti02 -A1203 -FeO-Si02 -CaO-MgO system. Both the hot-stage microscope and the strip furnace (melting-holding-quenching technique) were used during test procedure to determine the effects of CaO, MgO, and SiO2 on the liquidus temperature of slags. The liquidus temperatures of slags studied ranged from 1,241° to 1,900° C. The lowest liquidus temperature for each Ti02 plus A1203 plus FeO weight-percent generally occurred when the difference between CaO plus MgO and Si02 was less than 12 weight-percent. In this investigation substitution of either CaO or MgO for SiO2 and MgO for CaO raised the liquidus temperature of more than 50 percent of the reported base slags when Ti02, A1203, and FeO contents were held constant. The results of this investigation may serve as guidelines for determining flux requirements in smelting a wide variety of titaniferous magnetite concentrates or ores.

Jan 1, 1968

By Charles S. Allbright

To develop a method for predicting the stability of a fuel during long-term storage from rapid aging tests at 200° F, the Bureau of Mines determined the stabilities of three gasoline base stocks and an alkylate blending stock in both sealed storage and aerated storage at 110° F for periods extending to 32 weeks. Stabilities of samples containing gasoline-additive compounds were compared by aging, using two methods--rapid aging in a bomb at 200° F for intervals up to 16 hours and storage at 110° F. The additives used were an uninhibited tetraethyllead motor mix, N,N'-di-sec-buty1-p-phenylenediamine and 2,6-di-tert-butyl-4-methylpheno1. Results were related by graphs that enable predictions of gum and sediment formation during storage from data obtained in bomb tests. A premium-gasoline base stock and the alkylate proved to be stable, but the two regular-grade gasoline base stocks were found to be unstable. Addition of the diamine antioxidant improved the stability of both of the regular gasoline base stocks, while the phenol antioxidant improved only one of them. The presence of the tetraethyllead decreased the storage stability of all four fuels, both with respect to formation of gum and precipitation of inorganic sediment. The rapid test at 200° F appears to offer promise as a basis for a method of predicting gasoline stability in long-term 110° F storage.

Jan 1, 1968

By R. G. Peluso

Methods and results of studies to determine friction and shock losses encountered in auxiliary face ventilation systems utilizing flexible, spiral-reinforced ventilation tubing are presented. The results, tabulated in graphic form, simplify fan selection and enable mine operators to design adequate auxiliary ventilation systems. Problem illustrates the use of graphs.

Jan 1, 1968

By G. A. Brady

Seven samples of Pennsylvania anthracite from the Bottom Ross bed were analyzed and tested to obtain data on cleaning characteristics, proximate and ultimate analyses, specific gravity, grindability, heating value, and ash softening temperature. Ash content of the samples varied irregularly from 9.0 to 34.4 percent, the range being narrowed to an upper limit of 14.8 percent ash by removing impurities dense enough to sink in a medium with a specific gravity of 1.90. Ash content of the sink material with specific gravity greater than 1.90 ranged from 56.4 to 80.4 percent; corresponding specific gravities were 2.095 to 2.534. Volatile matter contents were indicated to be higher for the ash-forming minerals than for the pure coal substance in the various specific gravity fractions of a given sample. Specific gravities of anthracites with compa¬rable ash contents but from different locations in the bed varied as much as 0.06. The grindability index increased significantly with increasing ash con¬tent of specific gravity fractions from all the samples.

Jan 1, 1968

By Edward W. Parsons

The transverse force developed by expansion-shell rock-bolt anchors on the wall of a drill hole as the bolt is tensioned was measured by the Bureau of Mines using a device specially designed and fabricated for attachment to a universal testing machine. Load cells equipped with electrical-resistance strain gages provided the data from which the transverse force, in pounds, was calculated. Seven different expansion-shell anchors were tested, and the ratio of transverse force to bolt-tension load was found to range between 0.98 and 1.94 to 1.0. The drag load appeared to be the major cause of the transverse-force variation, but the relative effects of individual factors that affected the ratio between the transverse force and the bolt tension were not determined.

Jan 1, 1968

By R. L. de Beauchamp

A preliminary investigation was made of the extraction of chromium from ferrochromium by low-temperature chlorination in the 3400 to 5250 C range. The objective was to devise a method for separating chromium from iron in high-carbon ferrochromium produced from domestic chromite concentrates. The majority of iron was removed as a volatile chloride; chromium was contained in the residue as a nonvolatile chloride, which was separated from carbon and unattacked ferrochromium by dissolution. A small rotary chlorination apparatus was designed, built, and used for the chlorination tests, and samples of commercial-grade high-and low-carbon ferrochromiums were chlorinated for comparison of chlorination characteristics. Low-temperature chlorination of three types of ferrochromium resulted in the removal of 81.9 to 91.6 percent of the iron content as sublimed FeC13. Recovery of chromium in a leach solution of the reactor product varied from 82.4 to 93.1 percent.

Jan 1, 1968

By L. A. Neumeier

Sound experimental ingots of zinc alloys for use as rolling slabs were cast with a specially constructed, semicontinuous casting machine. Nominal alloy compositions of Zn-1.0 percent Cu, Zn-0.12 and 0.36 percent Ti, and Zn-1.0 percent Cu-0.03 to 0.36 percent Ti were cast. This Bureau of Mines study was conducted to evaluate the suitability of the casting procedure for providing stock for rolling into sheet. Microscopic examination of ingot sections revealed structures in which grain size varied from the outer to center ingot zones. Columnar grains present in the center zone of the Zn-1.0 percent Cu ingot were absent in the titanium-containing ingots. The ingots with titanium displayed a finer grain size and eutectic structure in the center ingot zone than in the outer zone; the transition in grain size between the two zones was quite abrupt in some ingots. The overall grain size of the titanium-containing ingots was finer than that of alloys cast by more conventional methods. Chemical analysis revealed that compositional segregation is not a significant factor in the formation of the ingot structure. Microstructural studies of small ingots of similar alloys solidified at slow, fast, and intermediate rates confirmed that the ingot structure in the semicontinuous-cast ingots is related to cooling rate, which is, in turn, related to the particular casting machine design and the influx of cooling water on the withdrawing ingots. Microstructures of thin sheet hot-rolled from slabs of the semicontinuous-cast ingots demonstrated that the ingot structure does not preclude the rolling of sheet having a uniform microstructure. Results of hardness surveys of the semicontinuous-cast ingots demonstrated that copper and titanium exert essentially additive hardening effects in these cast alloys.

Jan 1, 1968

By R. S. Fowkes

Jetstream pressure distributions and coal cutting rates were determined for a number of nozzles and under different operating conditions. The jetstrearn pressure distribution data were fitted to an assumed curvilinear equation by the utilization of a numerical least-squares technique with the aid of a digital computer. Subsequent manipulation of the approximation equation showed that the total force of the jetstream, rather than its maximum pressure or total kinetic energy per unit Lime, was the most significant quantity affecting the coal cutting rate. A shorter method for assessing the ability of a nozzle to cut coal was found.

Jan 1, 1968

By R. J. Leary

This investigation was conducted to determine the effects of various rare-earth metal addition practices upon the macrostructure and the pattern of sulfur distribution in steel ingots. Heats of plain carbon steel were melted in a 1-ton, basic electric-arc furnace. Melts were treated with mixtures of rare-earth silicides, aluminum, and cryolite either in the furnace before tap or in the ladle after tap to determine the effects of this form of rare-earth treatment upon ingot macrostructure. Steels thus treated with rare earths in the furnace were characteristically free of the gross subsurface nonmetallics which typically result from conventional rare-earth treatments. Steel treated in the ladle showed only a few such nonmetallics, and practical techniques were developed for eliminating most of these. Results showed that furnace deoxidation was controlled by the concentration ratio of rare earths: aluminum. During casting, deoxidation was controlled by the concentration of rare earths. Oxygen contents equivalent to vacuum ladle degassing resulted from air-melt furnace treatments with the rare-earth mixtures described. Rare earths in steel inhibited the onset of equiaxed grain formation during ingot freezing, and also virtually prevented interdendritic segregation of sulfides.

Jan 1, 1968

By Clarence O. Babcock

Model pillars of limestone, marble, sandstone, and granite having length to diameter ratios of 3:1, 2:1, 1:1, and 0.5:1 were broken in axial compression to determine whether lateral end constraint affected the breaking strength. Steel rings bonded to the ends of the model pillars with epoxy provided, during the loading cycle, a lateral end constraint of about 17 to 30 percent of the average axial stress. The effect of this constraint was to increase the breaking strength of the rock as compared to cylindrical pillars without constraint. The percentage increase in breaking strength varied with rock type and increased as the length to diameter ratio decreased. The maximum increase in breaking strength was 35 percent for marble pillars having a length to diameter ratio of 0.5:1. A theory was developed which relates the expected constraint to the physical properties of the ring and rock.

Jan 1, 1968

By Manuel Gomez

Coking time was investigated as a function of coal properties, carbonization parameters, and the interactions between these variables. The results indicate that coal properties and carbonization conditions interact to influence the coking time, and these interactions may be determined quantitatively. Prediction equations were developed and used to simulate the effects of bulk density, flue temperature, and oven width on coking times for coals having a wide range of properties. The data presented provide additional information on the carbonization process to permit the coke oven operator to maintain closer control of coke production and coke uniformity.

Jan 1, 1968

By J. Vance Batty

Two methods were devised and evaluated for quantitatively measuring the amount of oleic acid on flotation products and in flotation waters. One method involved use of an organic solvent to remove carbon-l4-tagged oleic acid from mineral surfaces and flotation water phases with subsequent radio-metric analysis of the extracts. Studies showed this method to be slow and subject to large variations in accuracy and reproducibility. In the second procedure, tagged oleic acid was measured directly on the surfaces of dried mineral products. Oleic acid in the water phase was determined by adsorbing it on fine mineral, drying, and radiometric counting. Quantitative analysis of oleic acid on flotation products from bench-scale flotation tests with synthetic mixtures of ore minerals and quartz and with natural ores showed this method to be fast, accurate, and reproducible.

Jan 1, 1968

By Frank G. Horino

This report describes an instrument designed by the Bureau of Mines for quantitatively identifying texture of rock surfaces produced by grinding or extremely rough surfaces beyond the range of commercial surface measuring instruments. The transducer for the instrument is a linear variable differential transformer that converts mechanical motion caused by surface roughness, waviness, and lay to an electrical output. The electrical output is recorded graphically as an X-Y plot of the line traversed on the rock surface. Details of the synthesized device and its calibration are given. The sensitivity of the unit is 2 percent of the scale setting of the amplifier. The horizontal scale is adaptable from ¼ inch to 15 inches of specimen length with a sensitivity of 0.01 inch if a 10 to 1 magnification is used and 0.1 inch if a 1 to 1 magnification is used.

Jan 1, 1968

By R. V. Mrazek

The heat of formation of vanadium trichloride was determined at 298.15° K. Measurements were made in a solution calorimeter in which an aqueous hydrochloric acid-potassium dichromate solvent was employed. Data are presented for the heats of solution of vanadium trichloride and the vanadium trioxide "backup" compound, and for appropriate dilution reactions needed to preserve stoichiometry. The resulting heat of formation of vanadium trichioride (VCI3) at 298.15° K was found to be ?H°298.15° K = -138.89 ±0.37 kcal/g mole.

Jan 1, 1968

By Perry N. Halstead

This report describes two goniometers that, by simple manipulation, can be used to ascertain the attitude of a joint, vein, or fracture plane observed on the planar projection of a borehole photograph taken with an NX borehole camera of the type developed by the U.S. Army Corps of Engineers. One goniometer was designed to interpret photographs taken in vertical drill holes and the other for photographs taken in inclined drill holes. In practice, several measurements are made on each photograph with the goniometer. These data are then substituted into mathematical equations, which are derived in this report and the attitudes of fracture planes are determined.

Jan 1, 1968

By M. R. Geer

The Bureau of Mines examined the washability data for 25 Appalachian coals requiring low-density washing to reduce sulfur content to 1 percent, using the distribution-curve method. The purpose was to estimate how closely theoretical sulfur values could be approached, what yields of washed coal could be expected, and the recovery efficiencies that might be achieved. Assuming that the run-of-mine coal would be crushed to 3/8 inch and cleaned in dense-medium cyclones, the calculations indicate that theoretical sulfur contents could be approached closely when cleaning at a specific gravity of separation as low as 1.30. With coals that have favorable specific gravity compositions the recovery efficiency anticipated for cleaning at 1.30 specific gravity is surprisingly high. Similar calculations for cleaning with concentrating tables at intermediate specific gravities indicated that theoretical sulfur contents at 1.50 specific gravity could be approached closely with some coals but not with others. The calculations suggest that operating a table at a specific gravity of separation much lower than about 1.50 probably would be unsatisfactory with most coals.

Jan 1, 1968

By Philip C. Tully

These modifications to the Redlich-Kwong equations for pure hydrogen and neon were developed after an unsuccessful attempt to generalize a modification technique previously developed for helium. New coefficients of the B terms were developed by minimizing the residuals. No changes were made in the coefficients of the A terms. For normal hydrogen, B was changed to [0.08063Tc PcT] for temperatures from 980 to 423° K and pressures up to 1,050 atm. The average deviation in Z was 0.36 percent with maximum deviations less than 1 percent for all but a few low-temperature points. For neon, B was changed to [PCT 0.1025T], for temperatures from 120° to 973° K and pressures up to 1,500 atm. The average deviation in Z was 0.34 percent with maximum deviations less than 1 percent for all but a few high-pressure and low-temperature points. Efforts to attain a lower temperature range to comparable accuracy with this type of modification were unsuccessful. In the range of applicability, these equations should be used with caution when calculating derived thermodynamic functions, such as the isobaric specific heat.

Jan 1, 1968