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By W. R. Huff

This report describes the development and operation by the Bureau of Mines of a pilot plant designed for using high-volatile A bituminous coal-in-water suspensions as a source of preheated coal and superheated steam in the pressure gasification of coal with oxygen. Figure 1 on page 2 is a block diagram of the integrated gasification process, in which a total of 70 tons of coal was fed from slurry and gasified. The present work included (1) development of equipment and methods both for mixing pulverized coal and water to produce slurry and for pumping and metering the slurry at gasification pressure; (2) development of equipment for heating the flowing slurry and, because slurry that can be pumped produces more steam than is necessary as a gasification reactant, developing equipment for removing and metering the excess steam; and (3) demonstration of the process under actual gasifier operating conditions, at a coal rate of about 800 pounds per hour and gasification pressures in the range 100 to 300 pounds per square inch gage. By using the forced-convection principle, a flow of slurry made from a caking, high-volatile A bituminous coal can be continuously heated to 600° F. in a coil-type heater. The flow rate and concentration of the slurry and the temperature gradient along the length of the heating coil must be closely controlled. In a radiant-type heater, involuntary reductions in flow rate, even momentary, can lead to coking and plugging of the heater coil.

Jan 1, 1961

By William D. Riley

In order to evaluate the corrosion resistance of zirconium in mineral extraction processes, such as a clay-hydrochloric acid leaching process for extracting alumina, the Bureau of Mines conducted corrosion studies in HCl-AlC13-FeC13 environments. A series of weight loss and electrochemical tests were conducted at 25° and 65° C in aluminum chloride (AlC13) plus hydrochloric acid (HCl) solutions containing 0 to 1,000 ppm ferric ion. It was determined that zirconium, which normally exists in a passive state in chloride-containing solutions, undergoes pitting attack in solutions containing more than 100 ppm of ferric ion. It is also shown that an oxide film prepared in air at high temperature offers protection in acid solutions containing levels of ferric ion from 300 to 1,000 ppm.

Jan 1, 1981

By E. Wittenau

This paper describing the concentrator practice of the Copper Queen Branch of the Phelps Dodge Corporation at Bisbee, Ariz., is one of a series of papers on milling methods and costs being prepared by the United States Bureau of Mines. The Copper Queen Concentrator treats 4,000 tons of copper ore daily by preferential flotation, whereby the copper sulphides are floated and considerable iron pyrite is depressed. During 1929 the heads to the concentrator averaged 2.15 per pent of copper, the recovery was 91.32 per cent of the total copper, and the concentrates produced contained 12.92 per cent of copper.

Jan 1, 1931

By Mackenzie Burnett

The Brattice Window Method was used to measure the leakage rates of a total of 42 ventilation stoppings in 8 hardrock mines. Various types of stopping construction were evaluated. The following types are listed in order of decreasing effectiveness: 1) Cinder block, 2) Timber and mortar, 3) Timber and polyurethane foam, and 4) Timber and brattice material. There are slight differences in the effectiveness of the first three types, while the timber and brattice type is substantially inferior to the others. The repeatability of the Brattice Window Method was found to vary with physical conditions in the mine such as stopping location with respect to intersections, regularity of drift cross section, and the presence of hardware such as air and water pipes, timber sets and wire mesh. The Brattice Window Method is viewed primarily as a tool for estimating and comparing stopping leakages for the purpose of determining where repair efforts should be concentrated. A laboratory test program resulted in the derivation of several "rules of thumb" for employing the Brattice Window Method, which will aid in securing accurate and repeatable data.

Jan 1, 1979

By E. E. Harton

Bureau of Mines Information Circular 16, Bibliography of Investment and Operating Costs for Chemical and Petroleum Plants, was published in October 1949 as an aid in making estimates of investment and operating costs of processes for manufacturing synthetic liquid fuels. Development of such processes by the Bureau of Mines was authorized by Public Law 290, 78th Congress. This bibliography included refer¬ences to and abstracts of publications appearing from 1930 to September 1948 on all processes in general use in the petroleum refining and chemical industries. Publications in this field have been numerous since compilation of the above bibliography, and the present report was prepared to cover the field from September 1948 through June 1952.3/

Jan 1, 1955

By Arden D. Fugate

This work was conducted to determine a feasible process for converting siliceous fluoride offgases to a commercially usable product. The offgases were generated by pyrohydrolytic defluorination of low-grade fluorspar in a gas-fired rotary kiln, and fluorine was collected as a hydrofluoric-fluosilicic acid. A silicon-free fluoride solution for further processing was then produced by neutralizing the acidic scrubber solution with anhydrous ammonia, silicon being separated as orthosilicic acid. Ninety to ninety-nine percent of the fluorine originally present remained in solution as ammonium fluoride. Silicon was also separated from synthetic fluosilicic acids, having F-to-Si weight ratios ranging from 3.50 to 14.3. The solutions below a ratio of 4.06, the F-to-Si ratio of H2SiF6, containing dissolved silicon were desiliconized as completely as those containing less than the stoichiometric quantity of silicon. An electrolytic-grade cryolite was recovered from the ammonium fluoride solution by reacting with either sodium aluminate or alumina trihydrate and sodium hydroxide. A product containing 97 to 100 percent of the fluorine, represented by Na3A1F6, was recovered, and 94 to 99 percent of the theoretical yield was realized.

Jan 1, 1963

By W. W. Weller

Low-temperature heat capacities of scandium sesquioxide (Sc203) and a mixture of cerium sesquioxide (Ce203) and cerium dioxide (CeO2) were measured over the temperature range from 50° to 298° K. The entropy of scandium sesquioxide at 298.15° K was evaluated directly as S°298.15 = 18.4 ± 0.1 cal/deg mole. That of cerium sesquioxide was extracted by combining the heat-capacity data for the mixture with those for pure cerium dioxide; the result was S298.15 36.0 ± 1.0 cal/deg mole.

Jan 1, 1963

By J. M. Stuve

Low-temperature heat capacities and the enthalpy of formation were deter-mined calorimetrically by the Bureau of Mines for CuO?CuS04. The derived standard entropy (S°298.15) was 40.36±0.04 cal/deg-mole, and the enthalpy of formation (?H°f) was -219.l±0.3 kcal/g-mole. A large thermal anomaly was observed in the heat capacity of CuO?CuS04 at 20±0.1 K. Gibbs energy of formation data are tabulated up to 1,200 K. Construction details of a precision low-temperature adiabatic calorimeter capable of determining heat capacities of solids in the temperature range 5 to 320 K are given. A calibrated miniature germanium resistance thermometer was incorporated into the calorimeter to extend the range of accurate measurements below 15 K. High-resistance dc heater windings were used throughout the cryostat to reduce heat conduction of inner connecting wires.

Jan 1, 1975

By Verne E. Hooker

The Bureau of Mines conducted a preliminary investigation to determine the state of stress in crystalline rock outcrops near Atlanta, Ga. The secondary principal stresses in a horizontal plane near the surface are compressive and are 500 to 3,000 psi. The maximum compressive stress is northeast-southwest in the Stone Mountain-Lithonia district but changes to northwest-southeast near Douglasville. The elastic constants were determined from data obtained by static and dynamic laboratory methods and in situ velocity measurements. Results show Young's modulus to be dependent upon both stress level and anisotropy in the rock. Average secant moduli obtained from triaxial tests were used to compute the applied stress from borehole deformation measurements.

Jan 1, 1966

By S. H. Ash

Unusual mining conditions prevail in the State of Washington because the majority of the coal seams lie on extra steep dips, and the roof and floor of the seams are of such a character as to require an excessive amount of timber- ing. The seams as a rule give off a considerable amount of methane, which makes good ventilation imperative. Due to physical conditions, supervision is costly and travel about the workings is difficult. Because of the facts stated, the accident rate has been above the average, and for some time considerable thought has been given the idea of making promotion of safety in and about the mines a responsibility to be shared equally by the employees and the management. With this idea in mind the legislature of the State of Washington, turing March, 1927, passed laws providing that safety committees be selected to function at the coal mines of the State and at the same time recognizing the fact that first-aid education is an integral part of any safety movement; legislation was passed making it mandatory to have all persons in and about the ines trained in first-aid administration. The provisions of the State mining law3 are as follows: "In every mine a general safety committee shall be selected, composed of the mine superintendent or manager of mines, one man selected by the employees or any association of employees in or around said mine, and a third member selected by these two. "The general safety committee shall elect one of the members to act as chairman and one to act as secretary. The duties of the chairman shall be to preside at all meetings of the general safety committee, enforce its rules and regulations and see that its business is conducted in a prompt and business-like manner. The secretary shall keep an accurate written record of the proceedings of all meetings, conduct its correspondence and post notices of regular and special meetings and other matters pertaining to safety. The duties of the general safety committee shall be to investigate all serious and fatal accidents; make bi-monthly.

Jun 1, 1930

By Ralph H. Espach

In the spring of 1943, when it was evident that the Tensleep sandstone in the Elk Basin field, Wyoming and Montana, held a large reserve of petroleum, Bureau of Mines engineers obtained samples of oil from the bottom of nine wells and analyzed them for such physical characteristics as the volumes of gas in solution, saturation pressures or bubble points, shrinkage in volume caused by the release of gas from solution, expansion of the oil with decrease in pressure, and other related properties. The composition of the gas in solution in the oil was studied. The pressures and temperatures existing in the reservoir and the productivity characteristics of the oil wells were determined. The data obtained indicate that the oil in the Tensleep reservoir of the Elk Basin field has unusually varying physical characteristics, such as a saturation pressure of 1,250 pounds per square inch absolute and 490 cubic feet of gas in solution in a barrel of oil at the crest of the structure, and a saturation pressure of 530 pounds per square inch absolute and 134 cubic feet of gas in solution in a barrel of oil low on the flanks. The hydrogen sulfide content of the 6a r; in solution in the oil varies from 18 percent for oil on the crest to 5 percent for oil low on the flanks of the structure. Of even greater significance is the fact that these and other variable characteristics of the reservoir oil are related to the position of oil in the structure. Many geologists and petroleum engineers have considered all the oil in a petroleum reservoir to have uniform physical characteristics and that equilibrium conditions prevailed in all underground accumulations of oil and gas. That such is not always so is borne out by the results of the study made by the writers.

Jan 1, 1951

By R. W. Huber

Three arc-melted ingots, two of a titanium-7 percent manganese alloy and the third of unalloyed titanium, were forged and rolled into 3/4-inch plate; comparative data were obtained on these processes. The finished plate, part of which was used by the Naval Bureau of Ordnance, was tested for mechanical and other properties. These properties were correlated with sponge purity, forging technique, rolling temperature, and cooling rate from the rolling temperature. For the alloy material, transformation data were obtained, and their age-hardening characteristics were studied. The temperature-impact relationship was established for rolled sections from all three ingots. INTRODUCTION Arc-melted ingots of unalloyed titanium and a titanium-manganese alloy were fabricated into plate under closely controlled conditions by personnel of the Metals and Alloys Section, Physical Metallurgy Branch, Bureau of Mines, College Park, Md. This program was cosponsored by the Naval Bureau of Ordnance. Bureau of Mines interest lay in correlating the processing procedures with the mechanical properties of the finished plate.

Jan 1, 1955

By John W. Kopp

Stemming is used in blasting operations to help contain explosive gases as long as possible. Stemming can reduce airblast, improve fragmentation, and reduce the chances of hot explosive gases igniting methane and dust explosions in underground mines. Stemming is required in underground coal mines but is generally not used in underground metal and nonmetal mines. Some underground metal and nonmetal mines are classified as gassy and can require special blasting procedures such as the use of stemming to minsure the safety of miners. The types and amounts of stemming material that are desirable in underground metal and nonmetal mine blasting to ensure good or improved fragmentation while containing the hot gases are largely unknown. This Bureau of Mines research examined the effectiveness of differing lengths of stemming by measuring stemming ejection times as related to burden movement. With properly stemmed blasts, stemming is contained until some burden movement has occurred. Test blasts at two surface limestone quarries were evaluated using high-speed photography. For the conditions of these tests, a stemming length of at least 26 charge diameters was found to prevent premature stemming ejection. In tests with stemming lengths of 16 charge diameters, the stemming was effective but there was early venting of hot gases through fractures in the rock. Further testing with other rock types, hole diameters, explosive types, and stemming materials as they affect incendivity is recommended.

Jan 1, 1987

By Joseph A. DeCarlo

For the first time the Bureau of Mines is combining, in one report, comprehensive tabulations on both beehive and slot-type ovens. This publication presents statistical data on the number and capacity of all such coke ovens in the United States on December 31, 1957. Combining data on both types of ovens should prove helpful to those interested in keeping abreast of the latest changes in carbonizing capacity, particularly since the coke has similar properties and uses. Annual reports furnished to the Bureau of Mines by coke-oven operators shared that 78 oven-coke plants were operating in 22 States on December 31, 1957. This was a decline of one plant from December 31, 1956, as the Republic Steel Corp. took the ovens at Canton, Ohio, out of production on December 17, 1957, for dismantling and rebuilding in 1958. Total oven-coke capacity was 80,299,400 tons in 1957.

Jan 1, 1958

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By A. R. Taylor

This report describes the design, construction, and operation of a low temperature adiabatic calorimeter for measuring heat capacities of solids or liquids from 60° to 300° K. A brief discussion of the basic theory involved in chemical thermodynamics and the problems involved in obtaining accurate experimental data is presented. The operation of the calorimeter was tested by measuring the heat capacity of a sample of benzoic acid obtained from the National Bureau of Standards over a temperature range of 60° to 300° K. The measured heat capacity values of the benzoic acid compared favorably with similar values obtained by the Bureau of Standards, the maximum deviation being 0.5 percent. THEORY A brief discussion of the basic theory involved in chemical thermodynamics will illustrate the applications of heat capacity data and the problems involved in obtaining accurate experimental data.

Jan 1, 1962

By R. S. Fowkes

The Bureau of Mines constructed a fully automated pilot plant facility to study the hydraulic transportation of solids through a lock hopper feeder system. An equation for the energy requirements to transport coarse solids hydraulically proved applicable to this system. Optimum velocities were obtained for limestone, mine refuse, and bituminous coal. The experimental data, calculations, and graphs show the effect of velocity, specific gravity, and solids concentration on head loss and power requirements. Other data were obtained and evaluated to determine the effect of particle size on head loss. Results also are given for (a) tests using friction reducing polymers; (b) tests using seven test sections of steel alloy pipe to determine their wear characteristics; (c) tests to determine spatial segregation of moving particles; and (d) tests to determine the effect of shape, size, and specific gravity on particle velocity in a horizontal pipeline. The lock hopper feeder system was found practical for continuous hydraulic transportation of the material types and size ranges tested.

Jan 1, 1969

By M. J. Kovalik

The effect of oxidation by air at temperatures ranging from 200° to 390° C on the change of chemical and physical properties of Pittsburgh-bed coal was studied as a function of processing time and temperature. The goal was to prepare a nonagglomerating fuel from a strongly coking coal for use in continuous carbonizing processes and in fixed-bed gasifiers. The oxidized coal was carbonized in a bench-scale apparatus, and the coke strength was evaluated in a Roga tumbler. Strength of the coke was progressively reduced with time of oxidation until the coking power of the coal was apparently destroyed. Time requirements to obtain an essentially nonagglomerating product were inversely related to processing temperature. Gaseous products released from the coal during oxidation reduced the yield of the desired nonagglomerating product, which decreased with time of oxidation at constant temperature and with increase in processing temperature at equal time. Oxidation at a temperature slightly above the lower limit of the plastic temperature range of Pittsburgh-bed coal was most effective because of the short processing time required and moderate processing losses.

Jan 1, 1963

By Joseph A. Sutton, John D. Corrick

The chemistry involved in the microbial dissolution of iron and copper from such sulfide minerals as pyrite, chalcopyrite, chalcocite, cove11ite, and bornite is described. The chemical criteria used to evaluate the activity of microorganisms on these minerals were changes in pH, ferric iron produced, and oxygen consumption. In a series of experiments in which a ferrous sulfate nutrient solution was percolated over small portions of the above-mentioned copper sulfide minerals for 56 days, the iron-oxidizing bacteria Ferrobaci11us ferrooxidans and Thiobaci11us ferrooxidans were capable of bringing about the dissolution of 23.7 percent of the copper from chalcocite, 56.3 percent of the copper from cove11ite, and 29.8 percent of the copper from bornite by the microbial production of ferric sulfate which reacted with these minerals. Laboratory tests have demonstrated that pure strains of the iron-oxidizing bacteria act as catalysts to the ferrous iron being oxidized by the Oxygen of a system containing pyrite and chalcopyrite. In a series of experiments during which nutrient solution was percolated over pyrite for 70 days, the ferric iron produced by the iron-oxidizing bacteria was 112 to 120 times greater than that produced atmospherically.

Jan 1, 1964

This final report summarizes the effort on a very aggressively scheduled and demanding development program undertaken by Westinghouse for the U.S. Bureau of Mines under Contract No. H0101262. The objective of this program was to produce hardware and test it to determine the efficacy of certain concepts of Coal Mine Rescue and Survival as established by the request for proposal and the study performed for the U.S. Bureau of Mines by the National Academy of Engineering (NAE). (These are stated in paragraph 1. 1 for reference.) In carrying out this program, Westinghouse provided specific hardware designs in consonance with the objectives of the concepts outlined in the NAE study final report. Though this contract did not require producing final design hardware ready for introduction to the coal mining community, components of the CMR&SS - as delivered - have some value in disaster situations and are to be kept on standby alert. Additional design and production development is required and should be undertaken on most of the subsystems and components before they can be used in the competitive coal mining community.

Jan 1, 1971