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By P. C. Good

Tungsten metal in fused form and of high purity was prepared by reducing tungstic oxide with redistilled calcium metal in a heavy-walled sealed reactor. Alloys of tungsten with vanadium, molybdenum) chromium, columbium, and tantalum were prepared by coreduction of mixed metal oxides in the same manner. This work was undertaken by the Bureau of Mines to investigate new approaches for preparing tungsten and its alloys in high-purity form. The standard method of producing tungsten metal has been the reduction of tungstic oxides by hydrogen. The resulting metal powder is compacted, sintered, and fabricated by powder metallurgy methods. Long experience in this field has resulted in the development of a technology that (by careful control of the variables such as metal composition, particle size, and sinterng technique) is well adapted to producing wire and the small shapes usually prepared from tungsten metal.

Jan 1, 1961

By C. P. Mabie

This report summarizes studies by the Bureau of Mines in developing a simple method for estimating the phosphorus pentoxide (P205) content of finely ground sedimentary phosphate ores and beneficiated products. The method used involved leaching, filtration, and precipitation. The Bureau found that measurement of the volume of ammonium phosphomolybdate precipitate obtained from samples containing 16.8 to 37.7 percent P205 and the use of an appropriate calibration curve permitted estimates of percentage of P205 content accurate within ± 1.1 to ± 2.6 percent, respectively, at the 95-percent confidence limits. Incidental to mineral dressing and petrographic investigations of western phosphate ores in 1959, the Bureau of Mines undertook development of a simple process-control method for rapid on-the-spot evaluation of phosphate-mineral recovery. Because of the fine-grained and obscure character of western phosphate ores, chemical, rather than microscopic or petrographic, techniques were investigated. The described method involves acid decomposition of the ore or product, filtration, addition of ammonium molybdate reagent to the filtrate, and centrifuging and measuring the volume of yellow ammonium phosphomolybdate precipitate produced.

Jan 1, 1961

By John P. Capp

The feasibility of simultaneously burning several paths through a coalbed to develop a multiple path underground gasification system was investigated by the Bureau of Mines during two experiments, Boreholes were drilled through the overburden and into the coal and arranged in a circle approximately 50 feet from a central borehole. In the first experiment, in an area which had previously been hydraulically fractured,5 air was injected at the center borehole. The coal was ignited at the other boreholes and the fire fronts traveled toward the center, counter to the flow of air, to backward burn paths through the coalbed. Two paths were linked during the first 5 days of operation. The outlets of these two paths were throttled and air pressure was increased to maintain the flow of air, but no other linkages were made. Fourteen days after the two linkages these two paths were opened and gasification was carried on for 10 days, but with only moderate success. In an effort to overcome operating difficulties air was injected at the peripheral boreholes, and the gases were drawn off at the center borehole. Reversed flow operations continued for 12 days and two more paths linked. The heating value of the gas generally was higher than 100 British thermal units per standard cubic foot (B.t.u. per std. c.f.). Because only four of seven paths linked, however, the entire system could not be evaluated with respect to product-gas output and recovery of energy.

Jan 1, 1961

By E. R. Palowitch

This report stems from a study by the Bureau of Mines of the possibility of reducing coal filter-cake moisture by applying radiant heat directly to the filter cake while under vacuum during the drying phase of the filter cycle. One disk of a 4-foot-diameter vacuum filter was equipped with gas-fired radiant-heat generators and the effect of radiant heating on the moisture content of a variety of filter cakes was studied. The results of this investigation show that this process can best be described as a filter aid capable of increasing the effectiveness of conventional filtration approximately 6 percentage points of moisture. The operating cost of removing water by this method is somewhat lower than the average operating cost of thermal drying and is considerably cheaper when the total cost is considered. Removal of water from coal that has been wet-cleaned is an important part of the overall coal preparation process. Water is a contaminant, and it is foolish to wash coal to reduce its ash content and add inert water in the process. In some instances the removal of water is actually more important than the removal of ash-forming minerals; its weight adds to the cost of transportation, and its evaporation during burning or carbonizing absorbs useful heat. Fine coal that contains more than about 10 percent moisture is notoriously difficult to handle. A problem thus exists for which there are sound practical and economic reasons to seek a solution.

Jan 1, 1961

By Donald F. Smith

This report describes the construction and calibration of two ice calorimeters and includes results of high-temperature heat-content measurements, made by the Federal Bureau of Mines, on rubidium fluoride, hafnium tetrafluoride, cesium chloride, and cesium iodide. The heats and entropies of fusion of rubidium fluoride, cesium chloride, and cesium iodide have been calculated at their respective melting points using equations derived from the experimental heat-content data. Hafnium tetrafluoride did not melt within the range of temperatures investigated. Heat and entropy of transition of cesium chloride from the alpha to the beta form were also determined. INTRODUCTION Free-energy data usually afford the cheapest and quickest means of determining the feasibility of experimentally untested reactions. For known reactions, free-energy data show the variation of the equilibrium constant with temperature and make it possible to calculate, without experiment, the maximum ratio of product to raw material for a given chemical process.

Jan 1, 1961

By M. E. Tyrrell

Despits its high melting point (2,135° C.), resistance to attack by molten metals, and its hardness (8), spinel (MgO?Al203) synthesized by the fusion of alumina (Al 2 0.) and magnesia (MgO) is not used on a large scale as a commercial furnace lining, mainly because of the prohibitive cost. This investigation by the Federal Bureau of Mines was prompted by the possibility of producing synthetic spinel from inexpensive raw materials by methods outlined in U.S. Patent 2,029,773, "Process for Obtaining Products Containing Spinets," dated February 4, 1936. In this patent Ture B. Haglund described a process for recovering crystalline spinels from melts in the system Mg0?Al203-2CaO-SiO2, a system well suited to the use of starting materials such as dolomite CaMg(C03)2, olivine [2(Mg?Fe)0.Si02], and bauxite (Al203?2H20) which are abundant in the southeastern United States. Compositions, ranging from a low content in the eutectic mixture of 35 percent spinal and 65 percent dicalcium silicate (2 CaO?SiO2) to a high of 75 percent spinel and 25 percent dicalcium silicate, were fused in electric furnaces of the arc-resistance and internal-resistance types. So long as members of the system were in proper chemical balance, "dusting" slags could be produced over the entire range of spinel concentration.

Jan 1, 1961

By T. A. Sullivan

The work described in this report was undertaken to evaluate and develop techniques for determining the oxygen content of titanium and titanium alloys. Early investigations of volatilization techniques involving halogenation were unsuccessful. Later efforts were concentrated on evaluating vacuum fusion and inert-gas fusion techniques. Two vacuum fusion methods and an inert-gas fusion method were found to be satisfactory in the 0.02 to 1.00 pct., oxygen range. These methods are described in detail. The coefficient of variation by any of the three methods is approximately 5 pct, While the main portion of this paper is devoted to the vacuum and inert-gas fusion methods, a resume of other suggested methods for analyzing titanium for oxygen also is given. INTRODUCTION The Federal Bureau of Nines has conducted research on titanium metal since 1938. This research included development of the Kroll process for the production of titanium (2)4, various sodium reduction processes for making titanium metal and lower valent titanium chloride-sodium chloride mixtures (17), and a fused salt electrolytic process for Me production of high-purity titanium metal and the recovery of titanium by electrorefining from off-grade materials (20).

Jan 1, 1961

By Scott W. Hazen

In recent years many mining companies have recognized that their chance for continued economic survival depends on the adaptation of technological advances in their operations. Increased productivity through new developments in mining methods and improvements in equipment has made mining and processing of lower grade ores possible. Cost analysis has produced accurate data on the costs for development, production, and processing of ore. All of these changes and cost studies have shown the necessity for increased accuracy in determining the grade of ore. Methods of estimating grade in a mineral deposit have not kept pace with the technological advances in the other areas. The same methods are in use today as in the past. Experience and judgment are major criteria of accuracy and the results are highly subjective. In 1953, as part of its research program to develop a better understanding of fundamentals of mining technology, the Federal Bureau of Mines began a sampling method research project at its Denver Mining Research Center. The basic objective of the project is to investigate sampling methods and to study the adaptation of the techniques of statistical analysis to mine sampling.

Jan 1, 1961

By W. L. Schmidt

The effect of a water-repellent film in sandstone cores on the effective permeability-saturation relationship was investigated as part of a cooperative research program between the Bureau of Mines and the American Gas Association. The repellent film was formed by the reaction of methyltrichlorosilane3 with the connate water in the core. Other researchers have reported on the use of silicone chemicals to alter the flow characteristics of porous media (1-3, 5-7, 9, 10).4 The previous studies, however, dealt almost entirely with oil-water or oil-gas systems and not with water-gas systems. The primary purpose of this study was to determine the feasibility of using silane to retard the influx of water into natural-gas storage wells and to determine the necessary requirements for achieving this result. The success or failure of silane treatment as a remedial measure depends on its effect on gas-production rate and attendant water production.

Jan 1, 1961

By Charles W. Huggins

Electron diffraction and electron microscopy were used to determine the unit cell parameters of garnierite [(Ni,Mg)3 Si2O5 (OH)4] and to examine its crystal habit. Bundles of ribbons, many less than 200 A. in cross section, make up the bulk specimen of the garnierite Electron diffraction revealed the unit cell to be monoclinic. Unit cell parameters were: a, 5.33 A,; b, 9.23 A.; c, 14.96 A.; and ß, 94°441.

Jan 1, 1961

By R. F. Stewart

A sedimentation method involving the use of the Palo-Travis apparatus was found satisfactory for rapid determination of the size distribution of coal particles ranging from 10 microns in diameter to those passing an 840-micron opening (20-mesh sieve), The method is most useful for comparing the size distributions of samples of pulverized coal where the actual size of the particles is not required and is applicable to sieve and subsieve sizes of a wide variety of coals and chars that can be wetted and are heavier than water. An analysis, including all calculations, can be completed in 1/2 to 10 hours, depending on the time required for the finely divided coal to settle. A typical analysis requires about an hour, making this a rapid, precise method for routine size-distribution analysis of powdered coals. When used with coal particles smaller than 400 microns, the method is precise within 15 microns for wide variations in test conditions and within 5 microns for identical test conditions. The precision decreases as particle size increases, becoming unsatisfactory for particles larger than 400 microns (40-mesh). For precision within 15 microns, the samples must be equal in weight. Greater precision is obtained with 4-gram samples, but samples as small as l gram may be used.

Jan 1, 1961

By Joseph A. Sutton

This study was undertaken by the Bureau of Mines to determine whether the sulfur-oxidizing bacterium Thiobacillus thiooxidans could use sulfur compounds to produce sulfuric acid in sufficient quantities to leach valuable metals from low-grade ores. The results of extended tests indicated that the bacterium is capable of extracting appreciable amounts of copper and cobalt from ore and mineral samples when sulfur is available in a state that can be readily assimilated by the organisms. Under the conditions of these tests, this organism was not able to assimilate and oxidize the sulfur as it occurred in the ores and minerals. Ores containing copper minerals in the silicate, carbonate, and oxide forms, in the presence of elemental sulfur, were more susceptible to bacterial action than ores containing copper minerals in the sulfide form. Thiobacillus thiooxidans remained active on elemental sulfur in the presence of some of the ores which were tested, but could not tolerate others. Therefore, strains of the bacterium were progressively adjusted to increasing concentrations (0.5 to 10 grams) of the individual ores until they could remain active on 10-gram portions of all ores being tested.

Jan 1, 1961

By K. K. Kershner

Nickel having a purity of more than 99.99 percent with reference to metallic impurities was electrodeposited at the Rolla Metallurgy Research Center of the Federal Bureau of Mines. The production of high-purity nickel is in keeping with the current trend in technologies for producing metals with lower and lower percentages of impurities. To understand more fully the role to be played by nickel by itself and as a component in many alloys, the element must be in a state of high purity. Procedures are outlined for purifying nickel solutions by precipitating and filtering off impurities. Details are given for using the purified solutions as electrolytes in depositing high-purity nickel. The elecneleposited nickel contained 0.0005 to 0.002 percent each of cobalt, copper, aid iron together with spectrographically detectable traces of aluminum, magnesium, and silicon. The deposits were smooth and dense; the crystalline structure was typical of an electrodeposited metal. Some preliminary experiments for purifying nickel solutions by liquid-liquid extraction are also described in this report. Tests of this type were limited since more encouraging results were obtained by other methods of purification.

Jan 1, 1961

By D. Bienstock

A high-B.t.u, gas can be synthesized by the catalytic methanation of a mixture of 2.5 to 3 parts of hydrogen to 1 part of carbon monoxide, obtained in the gasification of coal, using a steel catalyst followed by Raney nickel in a hot-gas-recycle system. Conversion of 99 percent of the H2+CO yields a fuel gas with a heating value of 983 to 1130 B.t.u. per cubic foot containing 78 to 96 percent methane, no carbon monoxide, and very small amounts of unsaturated hydrocarbons. With the steel catalyst alone, conversions were 85 to 90 percent, giving a fuel gas of 810 to 868 B.t.u, per cubic foot, or 847 to 975 B.t.u. on a C02-free basis. INTRODUCTION In 1948 the U.S, marketed production of natural gas was 5.15 trillion cubic feet; by 1958 it had reached 11.0 trillion cubic feet, a rate of growth of 8 percent annually. 4 5 Although demand is expected to increase less rapidly, by 1966 it may reach 16 trillion cubic feet, based on an estimated 4.7 percent annual increase.6

Jan 1, 1961

By L. J. Kane

Several processes being developed by the Federal Bureau of Mines to provide new and more efficient uses for coal require practical methods for removing dust from hot gases. Filters provide such means. The efficiency of filters made of aluminum silicate fibers and porous stainless steel was determined. The results obtained with the fibers were previously reported.5 In this investigation tests were made with three porosities of stainless steel filter material (grades C, D, and E) at a gas flow of 1,000 std. c.f.h./sq. ft. of filter, temperatures of 75° and 1,000° F., and dust loadings (as represented by cumulative dust fed) of 100, 1,000, and 10,000 gr./sq. ft. of filter. Pressure drop during the runs ranged from 0.1 to 21 in. of mercury, and dust removal from 25 to 99.93 pct. Filters having the finest pores gave the greatest pressure drop and percentage of dust removal; however, their dust-holding capacity was slightly lower. Usually, their ability to remove a higher percentage of dust at the same pressure drop more than compensated for the slightly lower dust-holding capacity. With increase in temperature, for the same weight rate of flow of gas, the pressure drop increased and the percentage of dust removal decreased. The effect of temperature was probably due to the accompanying change in the linear velocity and viscosity of the gas.

Jan 1, 1961

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 L. R. Fisher

The purpose of this investigation was twofold: (1) To devise a rapid method for determining quantitatively the porphyrin-carboxylic acid content of a particular crude-oil porphyrin aggregate, and (2) to isolate porphyrins in the crystalline state from crude-oil porphyrin aggregates. The first purpose was accomplished by applying adsorption chromatography. In fulfillment of the second aim three different crystalline porphyries were isolated by methods which involved both adsorption chromatography and fractionation of benzene solutions with hydrochloric acid of varying strength. The three porphyrins had etio, rhodo-, and phyllo-type absorption spectra, respectively. INTRODUCTION Many samples of petroleum have, as interesting minor constituents, chemical compounds known as metalloporphyrins. Their presence in crude oil and other bituminous materials was first discovered by Treibs a quarter century ago. Much experimental work has been done on metalloporphyrins because of their importance to the petroleum industry. They have a deleterious effect on refining catalysts. The ash resulting from the burning of heavy fuel oil is very reactive, We to the presence of metallic constituents, particularly vanadium. In oil-fired gas turbines, the ash may build up on the blades, causing imbalance of the rotors and, in addition, severe corrosion. In industrial boilers, the ash residue is responsible for severe damage to boiler tubes and to the refractory brickwork (15).4 Through study of the chemical constitution of the various metalloporphyrins found in petroleum, much can be learned concerning the origin, migration, and history of crude oils.

Jan 1, 1961

By J. E. Miller

This paper reports experimental determinations by the Bureau of Mines of compressibility factors to 4,000 pounds per square inch absolute (p.s.i.a.) for helium at temperatures from -10° to 130° F. and for 16 helium-nitrogen mixtures at 70° F. This information is needed for computing accurate discharge volumes and is necessary for determining an average-density value for use in orifice-meter formulas. In thermodynamic calculations, several functions of the compressibility factor with pressure and temperature are required. The data in the original publications (6, 8)5 of this study have been reexamined and have been given a more comprehensive treatment. The recalculated compressibility factors are higher by approximately 0.2 percent because in the earlier work a linear relationship between the compressibility factor of helium and pressure was assumed.

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 Stephan Stecura

One of the principal objectives of the Bureau of Mines program for development of superrefractory ceramic materials is to obtain fundamental data on the physical properties of refractory oxides. Elements of particular interest to research workers in the Bureau include groups III and IV of the Periodic Table and the rare-earth group. This report contains thermal expansion and phase inversion measurements on oxides of scandium, yttrium, lanthanum and 12 lanthanide series elements (promethium and terbium omitted) up to 1,350°C, made by high-temperature X-ray diffractometer techniques. Thermal expansion values were calculated from unit cell dimensions measured at selected temperatures; with anisotropic oxides expansion was determined parallel to each major crystallographic axis. The combined random and systematic errors in the thermal expansion values are considered to be less than 3 percent of the total expansion at 500° C, and approximately 2 percent at 1,000° C, No difference in expansion coefficients was observed between heating and cooling cycles for oxides that did not undergo phase inversion. Tabular data of linear expansion, in percent, linear expansion coefficients, and graphical presentation of linear expansion as a function of temperature are presented.

Jan 1, 1961