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By W. M. Merritts

A joint investigation by the Bureau of Mines and the Christopher Coal Co. at the Humphrey No. 7 mine, operating in the Pittsburgh coalbed in northern West Virginia, was undertaken to gain more insight concerning the hazardous emission of methane gas in mining, This report describes the equipment, procedure, and results. Horizontal bleeder holes drilled in the faces drained large quantities of methane, eliminating downtime of mining equipment. Also, larger quantities of methane were removed by forcing 14 to 25 g.p.m. water at 25 to 200 p.s.i. 5 pressure into the bleeder holes, In one infusion test a fluorescein dye was added to the infusion water; in later mining operations, the infusion water was traced for a distance of 1,500 feet. With vacuum pump applied to the horizontal hole the gas-flow rate increased, and the methane content decreased.

Jan 1, 1962

By Leonard Obert

This report describes a gage which, when used with my procedure for producing strain relief, will measure the resulting borehole deformation, From the borehole deformation the magnitude and direction of the principal stresses in a plane normal to the axis of the borehole can be calculated. The design considerations, mechanical construction, sensitivity, and stability of the gage are discussed. INTRODUCTION During the past two decades an increasing mount of consideration has been given to the problem of measuring and evaluating stress in rock around underground openings. Several investigators have made theoretical and model studies of the stress and (or) strain concentrations around simulated mine openings or in structural members, such as mine pillars or immediate roof. Other investigators have developed gages for directly or indirectly measuring stress or strain, and a number of reports present the results of measurements made with these gages. Because various methods and instruments have been developed, factors involved in this type of measurement will be briefly considered.

Jan 1, 1962

By Clark F. Grain

These investigations were undertaken as part of the Bureau of Mines program for the development and evaluation of high temperature nonmetallic materials. This report consists of thermal expansion and phase inversion measurements by high-temperature X-ray diffractometry on the principal oxides of beryllium (BeO), calcium (CaO), titanium (TiO2 ), zirconium (ZrO2 ), hafnium (HfO2), and thorium (ThO2); all were high-purity commercially available oxides. Thermal expansion values were calculated from unit cell dimensions measured at selected temperatures. Expansion was determined parallel to each major crystallographic axis for the anisotropic oxides: BeO, TOi2, ZrC2, and HfO2. 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 hysteresis in the expansion curves was noted between heating and cooling cycles. The Bureau's values were compared with published expansion measurements obtained by X-ray diffraction, dilatometric, interferometric, and telemicroscopic techniques. For anisotropic oxides, average linear expansion values were calculated from the volume expansion.

Jan 1, 1962

By Charles B. Kenahan

Vanadium is subject to only light corrosion in phosphoric acid at temperatures up to 60° C. and has a moderate corrosion rate in this acid at 100° C. It is relatively corrosion resistant in sulfuric and hydrochloric acids up to 60° C, but corrodes rapidly at 100° C. It corrodes rapidly in dilute nitric acid at 35° C. Vanadium is almost inert in 10-percent solutions of formic, acetic, lactic, tartaric, and citric acids; in 9-percent oxalic acid it corrodes slowly up to 60° C. and rapidly at 100° C. Vanadium is resistant to corrosion in substitute ocean water, tapwater, and in 3-percent sodium chloride and 10-percent sodium hydroxide solutions. It is readily attacked, however, by 20-percent ferric chloride, 20-percent cupric chloride and 5-percent mercuric chloride solutions. Vanadium is protected by contact with magnesium, aluminum, and steel SAE 4130 in substitute ocean water, by magnesium and aluminum in 3-percent sodium chloride solution, and by magnesium in tapwater. Vanadium protects copper in substitute ocean water. When vanadium and stainless steel are coupled in sulfuric acid solutions, both metals are usually unaffected by contact, whereas the corrosion rate of titanium in sulfuric acid is greatly reduced by contact with vanadium.

Jan 1, 1962

By Joseph M. Kuchta

The limits of flammability and minimum autoignition temperature of a fuel are important elements in assessing fire and explosion hazards that may exist when using or handling the fuel. The limits of flammability define the range of compositions of the fuel gas or vapor mixed with an oxidant through which a flame, initiated by an outside energy source such as an electrical spark, can propagate. The minimum autoignition temperature (M.A.I.T.) is the lowest temperature at which the fuel vapors ignite spontaneously in a specified medium; in this case the ignition energy is supplied by the heat content of tae environment. This temperature is also referred to as S.I.T. value by some authors. Because the autoignition of a fuel also depends on the time interval during which the fuel is subjected to heat, ignition delays are significant. Ignition delay is defined here as the total time elapsed between the introduction of the liquid fuel into the oxidizing atmosphere and the appearance of a flame. This time interval includes both the physical and chemical processes leading to ignition. The ignition delay is usually maximum at the M.A.I.T, and decreases as the temperature of the system is increased. The flash point and the fire point are also useful in assessing the fire and explosion hazards of a fuel. The flash point is the lowest temperature at which saturated, flammable fuel vapor-air mixtures are formed at atmospheric pressure and, therefore, it is essentially the lower limit of flammability

Jan 1, 1962

By J. R. Nettle

The development of a process for upgrading offgrade titanium metal by electrorefining in molten salt led to an investigation of the electrotransfer characteristics of selected metals when alloyed with the titanium to be refined. Previous tests on seven binary titanium alloys showed that the degree of transfer of the alloying constituent depends on the constituent and on the operating procedurese.5 This report describes tests on electrorefining ternary mixtures of titanium with selected metallic elements. Ten alloys were prepared from high purity titanium and 2-1/2 percent of each of the metal pairs selected from the same elements used in the binary study; manganese, vanadium, chromium, zirconium, tin, molybdenum, aluminum. Operating variables were similar to those investigated in the binary alloy study that gave minimum alloy metal transfer. The data presented indicate the transfer characteristics of the various metals and combinations tested relative to each other.

Jan 1, 1962

By W. T. Abel

The rate of the steam-carbon reaction, which is of fundamental importance to coal gasification, was determined by passing steam over graphite specimens suspended in an electrically heated tube. The measurements were made at 1,900° to 2,400° F. and at steam-feed rates of 0.1 to 2.0 moles of steam per mole of carbon per minute. At the maximum steam-feed rate, the reaction rate of carbon ranged from 0.4 percent per minute at 1,900° F. to 7 percent per minute at 2,400° F. Up to about 2,200° F., the steam-feed rate had only a slight effect; above this temperature, it limited the reaction velocity when the final mole fraction of steam in the reaction products was much less than 1.

Jan 1, 1962

By R. S. Warfield

Following World War II, the rapid increase in both military and civilian activity in the area served by the Alaska Railroad stimulated interest in the availability of local sources of nonmetallic minerals that might be used for building materials. Except for abundant sand and gravel and some pumice, the construction industry of the area depended entirely on high-cost imports for building materials of mineral origin. Because continued rapid growth was anticipated, development and use of local sources of such materials was advocated by both military and civil authorities to reduce the high costs of con¬struction and bolster the unstable economy of the area. The U.S. Department of the Interior began a program On included examining the numerous deposits of nonmetallic minerals accessible to the Alaska Railroad to determine their possible use as raw materials for the construction industry. Preliminary field investigations were made by the Geological Survey. The more promising deposits were subsequently examined and sampled by Bureau of Mines engineers, and the samples were subjected to the laboratory tests necessary to indicate the chemical and physical characteristics of the raw materials or their products. Such field and laboratory investigations were conducted on clay, shale, argillite, limestone, gypsum, and pumice taken from various parts of the area. In initial phasees of the work, done irate 1948 through 1952, many of the deposits examined were suitable for proctoring building materials. Results of the work completed during that period have been published in a Bureau of Mines report3 giving general information and detailed data on more than 35 deposits that were investigated.

Jan 1, 1962

By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

By Philip E. Niebuhr

A procedure, which can be performed in the field by nonanalytical personnel, is given for sensitive spot tests for detecting tellurium or selenium. The expressed need of a field test for detecting small amounts of tellurium, which may be accompanied by relatively large amounts of selenium, has led to the development of this method. Tellurium search has been impeded by the lack of a satisfactory test from the standpoint of sensitivity and specificity. A quantitative laboratory method exists, but it is expensive and relatively laborious. Several other qualitative tests are known, but they require unstable solutions, which must be freshly prepared for use, and a greater variety of laboratory equipment. The particular advantages of the test described are its simplicity and the stability of the reagents required, there-fore is is well adapted for field use. Also, this test was found to be of practical use in the analytical laboratory when screening samples, thereby reducing analytical costs. The roughly quantitative interpretation of the results can save time by indicating the approximate size of the sample taken for a quantitative determination.

Jan 1, 1962

By W. J. Boone

The Bureau of Mines has programmed for publication a series of Reports of Investigations of studies it has undertaken on low-temperature phase equilibria of several helium-bearing natural gases. This report is the second of a series of papers of the same general title; it is anticipated that additional reports of this series will be published. The advent of a helium conservation program and the prospect of production of helium by private industry, make it especially desirable to publish these data. This report describes phase equilibria related to a natural gas that is processed for helium at the Bureau's Exell Helium Plant (located about 35 miles north of Amarillo, Tex.). Carbon dioxide and water in the gas were removed before making the study; hence the data obtained are representative of the gas stream immediately after similar preliminary treatment in the plant process. Phase equilibrium data were obtained for conditions from -50° to -275° F. and from 100 to 500 p.s.i.a. Analyses of samples were made as follows: For a given run at a selected temperature and pressure, samples of the vapor and liquid phases were analyzed by mass spectrometer, and an additional sample of the liquid phase was analyzed for helium by means of special apparatus (7). 4

Jan 1, 1962

By Willard L. Hunter

The research described in this Bureau of Minus report was conducted to improve the chromium-iron ratio of offgrade chromite. Two methods were used: (1) Iron was selectively reduced from chromite by carbothermic reduction in an electric-arc furnace, and (2) a mixture of carbon, chromite, and sometimes fluorspar was chlorinated to remove a substantial part of the iron. Chromite concentrate from the Mouat deposit in Montana and from northern California was used in the test work. Chromium-bearing slag and chromite that had been beneficiated by a roast-leach process were each smelted to produce high-carbon ferrochromium. Iron was selectively reduced in a laboratory-scale., electric-arc furnace. Carbon additions to the smelting charges varied from 40 to 100 percent of the stoichiometric requirement, and slag basicities were varied from 0.4 to 1.0 chromium-iron ratios of more than 4:1 were obtained with 89 percent recovery of chromium in a chromium-bearing slag.

Jan 1, 1962

By M. R. Geer

All the coal lands in Alaska are publicly owned, and the Federal Government is the principal consumer of coal. Therefore the Government has long been concerned with the wise utilization of the coal reserves of Alaska as well as with the availability of coals meeting the specifications for use in various Government installations. Coal preparation plays a key role in both of these areas of interest. The proper choice and operation of coal-washing equipment permits the mining of inferior deposits, minimizes waste of coal in preparation, and assures a prepared product of the best quality obtainable from the raw coal. Thus, from time to time, the Bureau of Mines has made washability examinations on most of the coals mined in Alaska. Generally, these examinations were made when new mines or new beds were opened, when construction of new preparation plants was being considered, or when the operation of existing plants could be improved by better knowledge of the raw coal. The purpose of this report is to bring together all the washability data available on the coals of the Matanuska Valley and Beluga River fields. The pattern of energy development for the rapidly growing Anchorage area is not clear at this time. Formerly coal was the only fuel available for large-scale space heating and power generation. More recently both oil and natural gas have entered the market, and several hydroelectric projects have been completed. Additional major hydroelectric projects are being considered. The role that will be played by coal in this competitive energy market is uncertain. However I if coal is the fuel used in future power plants or industrial installations, the information contained in this report will be useful in indicating the quality of the coals that can be supplied and in selecting proper preparation techniques.

Jan 1, 1962

By M. D. Schlesinger

Experimental data for coal hydrogenation are presented to show that when a vehicle oil produced from coal is present, coal is hydrogenated to the same high conversion whether molybdenum catalyst is impregnated on the coal or intimately mixed with the slurry. Differences in product distribution could be related to the severity of operating conditions. No minimum mixing time was established, but 2 hours was sufficient. Longer periods of mixing, to 14.75 hours, had no effect on the results. The hydrogenation conditions were in the pressure range of 8,500 to 10,000 p,s,i. at 400° to 500° C. Most of the experiments were made in duplicate. The results were obtained with molybdenum concentrations of 0.01, 0.1, and 1 percent. Al the mentioned pressure range and a time at temperature of 15 to 60 minutes, coal conversions higher than 98 percent were obtained.

Jan 1, 1962

By Raymond W. Hiteshue

Experiments were conducted al temperatures of 480° to 800° C. and hydrogen pressure of 6,000 p.s.i.g. to determine the effect of coal residence time on the conversion of a high-volatile bituminous C coal to liquid and gaseous products when using a semicontinuous apparatus designed fur rapid heating and cooling of reactants. The objective of the studies at high temperatures was to determine if appreciable quantities of coal could be converted to gaseous hydrocarbons and low-boiling liquid hydrocarbons. Experiments at lower temperatures were designed to indicate shifts in product distribution with respect to temperature and to learn more about the general mechanism of the reaction when using close control of coal residence time. One percent molybdenum, based on m.a.f. (moisture-and ash-free) coal, was used throughout this investigation. At 800° C., 6,000 p.s.i.g., and "zero" residence time) the yield of gaseous hydrocarbons was about 38 percent and the yield of oil about 4.5 percent, based on m.a.f. coal. With IS minutes residence time, under the same conditions, the yield of gaseous hydrocarbons was approximately 80 percent with no increase in yield of oil. Apparently at 800° C., and hydrogen pressure of 6,000 p.s.i.g. coal was rapidly carbonized to char with expulsion of volatiles. Char was then slowly hydrogenated to gaseous hydrocarbons without production of oil.

Jan 1, 1962

By J. R. Welty

High-temperature thermodynamic data have, in recent years, become increasingly important for the extractive metallurgist. The extraction of metals from their ores previously was based on trial and error methods, involving hours of testing and often costly equipment fabrication. Using thermodynamic data it is frequently possible to predict the feasibility of a proposed metallurgical process as well as the optimum operating conditions for the process with reasonable accuracy. Such predictions can save consider-able tim~ and expense. Widespread use of thermodynamic analyses has been handicapped by lack of dependable experimental data. Investigators, notably K. K. Kelley (4)4. have devoted many years to determining and compiling such data. These investigators, although prolific in their production of thermodynamic values, have been unable to meet all the needs of industry and other branches of science. This becomes obvious when one considers the aeronautical and nuclear fields, in which previously unimportant, therefore uninvestigated, substances have become of prime importance.

Jan 1, 1962

By Louis P. Domingues

As part of a study on high-temperature ceramic materials, the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of yttrium, lanthanum, and cerium were analyzed thermogravimetrically. The temperature ranged from room temperature to 1,500° C. Each salt was decomposed by heating at a rate of 2.5° C. per minute, and some of the salts were subjected to additional rates of 5° C. per minute or 10° C. per minute. The decomposition sequences have been identified, and the temperatures of formation of intermediate compounds and of the oxides have been determined. The minimum oxide formation temperature of a given lanthanum salt exceeds that for the similar salt of yttrium, and both exceed that for the same salt of cerium except for one cerium carbonate. Variation of the heating rate indicates a thermal lag in the materials and produces the shift of formation temperatures to higher values and loss of resolution in the weight-loss distribution as the heating rate increases.

Jan 1, 1962

By Robert K. Koch

Laboratory-scale studies on defluorination of natural and synthetic fluorspars by pyrohydrolysis at 1,500° C. were made to determine the feasibility of developing a process for producing hydrogen fluoride from siliceous fluorspars. It was found that the reaction (at 1,500° C.) is not promising for process development, even though a silica-free offgas can be generated. The primary difficulty is the low hydrogen fluoride content of the offgases; an HF content of 6 percent was the best achieved. Previous research by the Bureau of Mines has demonstrated that offgases averaging 27 percent hydrogen fluoride can be produced under carefully controlled conditions at 1,280° C. The lower temperature process is a better method for production of HF. However, charges in which the CaF to Si02 mole ratio varied from 0.4 to 2 could be processed with similar results. Also, combined alumina and ferric oxide contents up to 25 mole-percent did not noticeably alter the rate of defluorination. Therefore, virtually any natural siliceous fluorspar would respond in essentially the same manner when exposed to water vapor at 1,500° C.

Jan 1, 1962

By W. A. McKinney

The segregation process consists of heating crushed oxidized or mixed oxide-sulfide copper are with a copper-volatilizing salt and carbonaceous material at about 750° C. to produce metallic copper which is recovered from the furnace calcines by conventional sulfide flotation. The Bureau of Mines made a number of bench-scale laboratory tests on two copper ores to determine the relative merits of using halogen salts, potassium chlorate, or various salt mixtures as volatilizing agents in segregation of the copper. Laboratory investigation of typical siliceous and calcareous oxidized ores revealed that sodium chloride was a better segregating agent than the other salts. Calcium chloride, magnesium chloride, sodium fluoride, or potassium chlorate gave nearly as good segregation as the sodium chloride on the siliceous ore. Segregation of the calcareous ore with calcium chloride was nearly as good as that obtained with sodium chloride, but inferior segregation resulted when magnesium chloride, sodium bromide, or potassium chlorate was employed. The use of sodium bromide or sodium iodide on the siliceous ore, and of sodium fluoride or sodium iodide on the calcareous are, gave appreciably poorer segregation than sodium chloride or the other salts. Other tests of the ores, using mixtures of sodium chloride and the other halogen salts or potassium chlorate, gave segregation approaching that obtained with sodium chloride.

Jan 1, 1962

By K. E. Tame

The Bureau of Mines is studying possible modifications in conventional uranium ore-processing steps to confine and permit controlled disposal of radioactive wastes. A potential method of minimizing pollution from radio-active nuclides, principally radium 226, in uranium mill waste streams is to reuse the waste solutions within the mill. Such reuse of waste solution in the Kerr-McGee Shiprock-type process was investigated in the laboratory. The Shiprock mill employs a two-stage acid-leaching process for dissolution of the uranium, countercurrent decantation for liquid-solid separation and washing, and organophosphorus solvent extraction for recovery of the uranium and vanadium from solution. The simulated use of barren raffinate instead of fresh water in the mill circuit was carried through a laboratory campaign of 28 interlocked leaching, washing, and solvent extraction cycles. About 99 percent of the uranium and 91 percent of the vanadium were dissolved from the are, Washing efficiency in the thickener circuit averaged about 99.5 percent when the pulp was washed with enough barren raffinate and makeup water to recover 2.5 tons of pregnant solution per ton of ore. The only solution discarded was that contained in the washed and thickened leach residue. A buildup of salts due to recycling of solutions did not adversely affect operation of the washing circuit.

Jan 1, 1962