Search Documents

By W. S. Sanner

Anthracite was used extensively as a fuel in iron metallurgy from 1840 to 1880. In 1874, 226 of the 680 blast furnaces in the United States were operating on anthracite and producing almost one-half of the Nation's pig iron. However, by 1890, railroad expansion, the development of western iron-ore reserves, and the growing use of coke decreased the importance of anthracite as a metallurgical fuel. As a result, the last blast furnace designed exclusively for anthracite use was built in 1891. Because of the increased energy requirements of our expanding national economy, the abnormally high demands during national emergencies, and the proximity of anthracite deposits to eastern steel-producing areas, interest has grown in again using anthracite in iron metallurgy. Estimates of anthracite reserves indicate a 300-yr. supply at a production rate of 30 million tons per year. These large reserves dictate the development of an adequate technology for the use of anthracite by the metallurgical industry.

Jan 1, 1961

By Donald W. Mitchell

Studies were made in the Bureau of Mines Experimental coal mine to evaluate the effectiveness of a few extinguishing agents and techniques for controlling a fire on a simulated mining machine. The investigation showed that water containing an alkali-metal salt or a surface-active (wetting) agent was more effective than water alone. For close attack, fog applications was the most effective technique studied; high rates of agent application controlled the fire more quickly than low rates. The ability to control the fire increased as the distance of attack decreased. Dry powders controlled the fire when applied by shovel but not when applied airborne by rock-dust distributor or by hand fire extinguishers. Dry alkali-metal salt powders (potassium and sodium bicarbonates and sodium tetraborate) quenched the fire more readily than limestone dust. In each instance the finer powder, the greater its effectiveness. In an open ventilated entry, smoke and hot gases backed against the air currents. An airspeed of 230 feet per minute was required to permit approach to within 10 feet of the fire. At lower airspeeds, approach could be made by extending the brattice across the bottom two-thirds of the entry, by pushing the smoke ahead with water sprays, or by discharging dust from a rock-dust distributor. In a dead-end entry, the fire was approached to within 30 feet by coursing fresh air along an airtight line brattice; however, it was safer, easier, and less time-consuming to attack the fire from a fresh-air base 100 feet away with a solid stream or by high-expansion foam; the latter method was more effective.

Jan 1, 1961

By Martin H. Stanczyk

The direct dissolution of a typical zinc sulfide flotation concentrate by elevated temperature and pressure leaching was investigated. The concentrate assayed about 55 percent Zn, 32 percent S, 6 percent Fe, and 1 percent Pb and contained minor quantities of copper and precious metals. The influence of various factors on the dissolution of the zinc in acidic and ammoniacal pulps when using oxygen as the oxidant was determined. The tests revealed that the sphalerite was difficult to oxidize. Complete dissolution of the mineral required vigorous and intimate nixing of the gaseous, liquid, and sold phases. The addition of pyrite or sulfuric acid to water slurries of the concentrate was required to obtain a high zinc extraction when leaching under acidic conditions. The quantity of pyrite and acid used was about 0.125 and 0.25 pound, respectively, per pound of zinc sulfide contained in the leach charge. In tests with acid, about 96 percent of the zinc was extracted from the concentrate in 1 hour at 200° C. when the oxygen partial pressure was 75 pounds per square inch gage or higher. Leaching with a continuous flow of air as the oxidant gave results that were almost as good as those obtained when oxygen was used, In tests with air fed through the autoclave at 320 liters per hour, 95 percent of the zinc was dissolved in 1 hour, Acid leach solutions assaying approximately 58 grams Zn per liter and containing Fe, Ni, Cr, and Cu impurities were produced in the better tests. The leached residue consisted essentially of red iron oxide together with substantially all of the lead and precious metals.

Jan 1, 1961

By J. B. Gayle

Although heated circuits frequently have been employed in the conditioning stases of certain flotation processes, particularly the flotation of fluorite, the control of temperature is not generally considered economically feasible for the flotation of coal. This viewpoint, although widely held, can neither be substantiated nor refuted by reference to published data. Some evidence is available, however, that temperature is an important variable in the floatability of coal as well as other minerals. For example, Gayle and Swelley4 found that contact angles for coal and related substances were definitely dependent on temperature. Bailey and Whalan5 showed that changes in pulp temperature may exert a pronounced influence on recoveries of coal in batch flotation tests. The present laboratory-scale investigation was undertaken to obtain information about the effects of changes in pulp temperature on coal flotation recovery and also on the selectivity of separation possible using different reagents. The results indicated that flotation recoveries were markedly affected by temperature variations when certain reagents, particularly simple aliphatic alcohols, were used. For other reagents, particularly kerosine, flotation recoveries were substantially independent of variations in pulp temperature. Release-analysis results indicated that temperature variations did not greatly affect the selectivity of separation possible with the reagents tested.

Jan 1, 1961

By W. M. Dressel

The objective of the research reported in this publication of the Federal Bureau of Mines was to devise a mineral dressing procedure that would concentrate zinc silicate minerals from certain deposits in southwestern Missouri. The best flotation results were obtained by batch laboratory flotation using sulfidizing agents and ethoxylated cocoamine. The flotation concentrate contained 70 percent of the zinc at a grade of 47.8 percent. Gravity concentration tests showed that 55 percent of the zinc could be recovered at a grade of 48.3 percent.

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 Mah Alla D.

Previously existing heat-of-formation values for the oxides of vanadium were rudimentary. They were subject to uncertainties of 1 to 5 kilocalories per gram-atom of contained oxygen. This fact has been the only adverse influence on the accuracy of thermodynamic calculations involving these substances, as the requisite entropy and high-temperature heat-content data are known with reasonable accuracy. This report presents new heat-of-formation data for four oxides of vanadium (VO, V203, V02, and V205), obtained by combustion calorimetry. It is believed that the uncertainties have been reduced to 0.1 to 0.3 kilocalorie per gram-atom of contained oxygen. The new heat-of-formation data were combined with existing entropy and high-temperature heat-content values to obtain free energies of formation of the four oxides at temperatures up to 2,000° K.

Jan 1, 1961

By S. L. May

Procedures for separating columbium and tantalum have been developed by the Bureau of Mines as part of a broad research program on the utilization of low-grade ores of columbium and tantalum, Columbium and tantalum compounds of greater than 99 percent purity have been obtained by application of the solvent extraction separation system: Hydrofluoric acid-sulfuric acid-methyl iso-butyl ketone. This system is unique in that it not only separates columbium from tantalum, but also separates these two metals from other metallic impurities. The system is effective for separating the metals irrespective of the tantalum and columbium ratio of the starting materials. Investigations in which the spent feed obtained from the initial coextraction step was recycled to the system indicated that efficiency was increased, and cost was reduced without impairing product purity. Continuous tests demonstrated that this solvent extraction system could be used in large-scale equipment without loss in efficiency or in purity of products. The separation of columbium and tantalum has been difficult because of the similarity in their chemical bahavior. Many methods have been proposed for separating these two elements, but most methods either did not achieve satisfactory separation or were tedious and time consuming. The Marignac process (3, 4)4 developed in 1866 was the only method used commercially until recently. This separation procedure is based on the difference in solubility in aqueous solution of potassium tantalum fluoride and potassium columbium oxyfluoride. Current commercial practice appears to favor solvent extraction as a method for separating tantalum from columbium (1). Several efficient methods for separating columbium from tantalum by solvent extraction (2, 9, 8) were reported earlier from this laboratory.

Jan 1, 1961

By R. M. Becker

As part of the Bureau of Mines program for examining the Nation's iron and titanium resources, magnetic, gravity, and geologic surveys were made to permit an estimate of the extent and magnitude of the Iron Mountain, Colorado, titaniferous magnetite deposit. Gabbro is the dominant rock type of the area. Within the gabbro are lenses of titaniferous magnetite, 5 to 25 feet wide and as much as several hundred feet long. These lenses comprise a zone which has scattered occurrences of magnetite for 2,200 feet. To the west, the gabbro grades into a strip of pyroxenite that in turn borders a large monzonite mass. A wedgelike broadening of the pyroxenite with depth accompanied by little or no increase in the titaniferous magnetite is considered a reasonable interpretation of the field data. The iron deposits appear to be limited and discontinuous.

Jan 1, 1961

By A. N. Fried

With the growing importance of fluid injection in recent years, the petroleum industry has been investigating and field- testing a variety of new methods designed to modify the physical properties of reservoir oil to improve the efficiency of gas and water injection. These procedures include condensing-gas drive, LPG (liquefied petroleum gas) injection, alcohol-slug process, high-pressure-gas displacement, detergent-solution flooding, and in situ combustion (30, 37).3 A new and different method to increase the effectiveness of gas and water injection has been tested by the Bureau of Mines, Consideration of both fundamental and practical factors that operate to limit the oil recovery attain- able by conventional oil-displacement mechanisms led to the concept of a displacement mechanism called the foam-drive method. This report describes the experimental study that tested this concept in the laboratory.

Jan 1, 1961

By E. Morrice

This report of the Federal Bureau of Mines presents a laboratory procedure, with the requisite equipment, for electrowinning ingot (liquid) cerium metal from a fused-fluoride bath, the metal purity being about 99.9 percent. Physicochemical studies, including bath properties and electrochemistry, are included, with a speculative model of the mechanisms involved. An historical review of the methods used for electrowinning misch metals and yttrim-group metals, as well as individual rare-earth metals, is presented. The electrolytic preparation of metal from fused salt and nonaqueous media is summarized, along with the unsuccessful attempts at depositing the metals from aqueous solutions.

Jan 1, 1961

By Richard Havens

A flotation procedure was devised by the Federal Bureau of Mines for beneficiating Mount Wheeler, Nev., beryllium ores that contain the beryllium minerals bertrandite and phenacite in a complex association with calcite, fluorspar, mica, quartz, and other accessory minerals, The method also has proven to be effective in trials on ore from the Lake George, Colo., area. Samples used in most of the research ranged from 0.49 to 0.73 percent BeO. Beryllium mineralization varied from two-thirds bertrandite to all phenacite. An unusually high grade sample containing 5 percent BeO as phenacite was floated on a batch basis to prepare concentrate for utilization studies. The beryllium minerals were floated from undeslimed pulps at natural pH using sodium fluoride and sodium hexametaphosphate (HMP), as modifiers, and a fatty acid-fuel oil combination as the collector. Key factors were the use of a minimum of about 4 pounds of sodium fluoride and between 2 and 4 pounds of HMP per ton of ore. Efficacy of the HMP was related to the grind, mineralogical composition, corollary reagents, and type and time of conditioning. Addition of the fluoride, HMP, and collector in that order, followed by appropriate conditioning after each addition, was essential for satisfactory flotation.

Jan 1, 1961

By Bernard Porter

The solubility of UO2 was determined at 1,250° C. in ternary melts of UF4 and BaF2 with CaF2, LiF, and SrF2. The solubility of Ce02 was measured at 800° and 850° C. in a solution of CeF3, BaF2, and LiF. The amount of La203 which dissolves at 950° C. in a binary mixture of LiF and LaF3 and a ternary of LiF, LaF3, and BaF2 was also measured. In each case, the amount of soluble oxide was mound to be less than 5 weight-percent. A procedure was developed for filtering fused, oxide-saturated fluoride melts in order to obtain a representative sample for chemical analysis. The oxide content of the samples was determined by an inert-gas fusion procedure.

Jan 1, 1961

By T. T. Campbell

This report traces the development of techniques for the preparation of high-purity rare-earth metals. Rare-earth metals, excepting samarium, europium, and ytterbium, were prepared by converting their oxides to anhydrous chlorides or fluorides and reducing the rare-earth halides with active metals such as lithium or calcium. High-purity, anhydrous rare-earth chlorides were prepared by dissolving the rare-earth oxides in hydrochloric acid to form hydrated chlorides and by subsequently dehydrating the hydrated salts in the presence of ammonium chloride at temperatures ranging from 70° to 360° C. while under reduced pressure (50 microns to 1 inch Hg). The chlorides were also prepared by direct chlorination of rare-earth oxide-carbon mixtures. Reaction efficiencies in excess of 95 percent were obtained by either method; however, purer chlorides were prepared by the aqueous ammonium chloride conversion method. Purification of yttrium chloride by high-temperature vacuum distillation proved to be an effective method of separating, oxygen-bearing compounds from the chloride. Yttrium metal prepared from purified chloride contained significantly smaller amounts of oxygen (990 p.p.m. oxygen in yttrium metal prepared from raw chloride and 200 p.p.m. in that prepared from distilled chloride).

Jan 1, 1961

By Robert H. Merrill

Measurement of the deformation of a borehole in rock subjected to a change in applied stress can be used to calculate the magnitude and direction of the applied stress, provided a satisfactory deformation-applied stress relationship exists , In this investigation by the Bureau of Mines the deformation of a bore- hole in a rock model subjected to a known applied stress was compared with the theoretical deformation of a hole in an elastic, isotropic plate and was found to be in good agreement. Hence, this relationship can be used to calculate the applied stress on a borehole from borehole deformation measurements.

Jan 1, 1961

By K. E. Tame

A resume of the history and state of the art of physical beneficiation of uranium ores is presented along with a detailed description of research on concentration of uranium ores by attrition grinding. The information on flotation, gravity concentration, electronic sorting, and selective grinding was gathered to complement the study of attrition grinding methods. Both dry and wet grinding procedures were investigated as potential methods of upgrading a variety of ore types, ranging in grade from 0.02 to 0.42 percent U308. A Mardun4 disintegrator that employs high-speed rotating paddles in a cylindrical shell lined with interrupter bars was used in most of the dry grinding studies. Attrition scrubbing devices, which impart a violent mixing or attritioning action to ore pulps, and cylindrical mills, employing rods or punchings as grinding media, were used in the wet grinding tests.

Jan 1, 1961

By Harry R. Nicholls

A simple economical method has been developed for determining the in situ longitudinal and shear velocities in rock from which its elastic constants can be calculated. By detonating small charges of high explosives in shallow drill holes near a free surface, both longitudinal and shear waves were generated simultaneously. Accelerometers and velocity gages mounted to the rock surface were used to record the arrival time for both waves over travel path lengths from 50 to 450 feet, Measurements were made in two rock types. From the arrival time measurements, the longitudinal and shear wave velocities were calculated. From these velocities and the density of the rock, the elastic constants were calculated. The dynamic elastic constants of drill core samples of the two rock types were determined in the laboratory by the resonant-frequency method, The lab- oratory and in situ elastic constants are compared and significant differences noted. In general, there is less spread in the in situ data than in the laboratory data, and Poisson's ratio does not fall outside the theoretical limits for the in situ data as is often the case for laboratory-determined elastic constants.

Jan 1, 1961

By T. N. McVay

The Bureau of Mines has developed a field test for detecting the presence of columbium in a variety of minerals containing the clement. The test consists of fusing the mineral or rock powder with potassium pyrosulfate in a porcelain crucible, digesting the melt with hot dilute hydrochloric acid to release the columbium oxide (Cb205), and subsequently reducing the columbium oxide to a lower oxide by adding tin, which gives a blue color to the contents of the crucible. The method will detect 1 percent of contained columbium oxide (Cb205) in a mineral sample provided no tungsten is present. If a mineral containing appreciable titanium is test,-!d in the same manner, the solution in the crucible becomes violet. In the presence of columbium, titanium at first causes a violet coloration of the solution, which after a few minutes is masked by the stronger blue of the reduced columbium oxide. Although tantalum oxide (Ta205) does not interfere with the columbium test, tungsten gives a blue color that is indistinguishable from the color obtained with columbium. A simple method is available to detect the presence of columbium in the absence of tungsten, but when the presence of tungsten is suspected, the sample must be subjected to somewhat more elaborate chemical tests to determine the presence or absence of columbium. Although these latter tests can be made in the field, several steps are involved that arc best performed in the laboratory with simple equipment.

Jan 1, 1962

By R. V. Higgins

Many contributions to methods of forecasting the performance of waterfloods of a five-spot pattern have been made by investigators. In most of these forecasting methods, a previously selected sweep efficiency is used, and other simplifying assumptions are employed to obtain the objective. In this paper the calculated oil recoveries from several five-spot single- and multiple-layer stratified reservoirs were made with a minimum of assumptions, and because of the techniques used, no previously selected sweep efficiency was required. As a result, the accuracy of the forecast is increased. Permeability curves and continuously changing saturation gradients are used in every section of the pattern. By means of a potentiometric model, the flood pattern is divided into channels, the centers of which are the streamlines. The channels are divided into cells. As flood water enters, the permeability and saturation of each cell change with time. In this study the production from multiple-sand layers of different absolute permeability but with the same relative permeability-saturation relations are combined. The results are shown for a single- and 10-layer reservoir with a permeability variation of 0.60. The oil rate, water-oil ratio, and recovery are shown as functions of time for a 2- and 20-centipoise oil starting in primary phase and after fill-up.

Jan 1, 1962

By Wesley Holmes

Concentrating, nodulizing, and smelting studies were conducted at the Albany Metallurgy Research Center of the Bureau of Mines to determine whether (1) western iron ores of the type found in the Carter Greek deposit near Dillon, Mont., could be utilized; (2) concentrates of acceptable grade with good iron recovery could be attained by wet-magnetic beneficiation; (3) nodulized concentrates could be smelted with reductants readily available in Montana; (4) iron concentrates could be smelted without prior agglomeration; and (5) high-purity iron could be produced directly from high-grade concentrates, Three small samples and two tonnage samples from the Carter Creek deposit were uniform in chemical composition, and their iron content averaged about 31 percent. They were found to be banded gneisses, and magnetite was the principal iron-bearing mineral.

Jan 1, 1962