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By W. A. Stickney, J. W. Town

Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .Batch and continuous - circuit flotation , leaching , precipitation , and electrodeposition studies were made by the Bureau of Mines to determine optimum conditions for treatment of complex mercury - antimony sulfide and mercury- arsenic sulfide ores and concentrates . On the Red Devil ore sample over 95 percent of both the mercury and antimony sulfides were recovered in a flotation concentrate containing 35.6 percent mercury and 21.0 percent antimony . By selective flotation a mercury concentrate containing 71.0 percent mercury and 2.9 percent antimony was obtained with a mercury recovery of 90.4 percent . Leaching results show that , with 150 grams per liter of sodium sulfide and 50 grams per liter of sodium hydroxide , 95 to 99 percent of the mercury , antimony , and arsenic sulfides could be extracted from the concentrates treated . Sodium hydroxide reagent consumption was based on the sulfides generated in the dissolution of the sulfide minerals and on the method of metal recovery used . Selective leaching of the antimony and arsenic sulfides with potassium sulfide dissolved more than 95 percent of either of these two sulfides and 0.5 to 5 percent of the mercury sulfide present . Methods for recovering mercury and antimony from solution were electrodeposition of mercury followed by electrodeposition of antimony , aluminum precipitation of both mercury and antimony , or antimony precipitation of mercury followed by antimony electrodeposition . The method used in recovering the mercury depended on the mercury- antimony content of the solution being treated .

Jan 1, 1964

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

A series of economic evaluations of processes for producing metallurgicalgrade alumina from low- grade aluminous materials is being conducted by the Bureau of Mines to determine the relative processing costs . The two processes considered in this evaluation are concerned with the recovery of alumina from clay through the formation of ammonium alum . In the first process , dehydrated clay is leached with ammonium bisulfate solution ; in the second process , clay is baked with ammonium sulfate and then leached with water containing a small quantity of sulfuric acid . After the alumina is dissolved by either of these methods , the iron is reduced to the ferrous state to avoid crystallization of ferric sulfate with the alum . The recovery of pure alum requires two crystallization steps . The alum crystals are then redissolved and precipitated with ammonia to produce alumina hydrate , which is calcined to a - alumina . These evaluations are based on published work , and the proposed plants are designed for a capacity of 1,000 tons of alumina per day . The estimated operating cost per ton of alumina for the bisulfate leaching process is $ 117.06 , and for the sulfate baking process , $ 109.26 . Using a Marshall and Stevens chemical equipment index basis of 240.0 , the estimated fixed capital costs , in the same order , are $ 158 million and $ 146 million . Under current economic conditions , these two processes are not competitive with the Bayer process for the production of alumina from bauxite . Since small improvements will not reduce costs sufficiently to approach competitive costs , future research work with these processes should be confined to areas likely to result in major cost reductions .

Jan 1, 1965

By John Nagy

Dust explosion data obtained in laboratory studies by the Bureau of Mines are presented for activated carbon, asphalt, charcoal, carbon black, coal, coke, gilsonite, graphite, lignite, miscellaneous carbons, pitch, tunnel dust, and mixtures of these materials with other ingredients. The explosion hazard is shown to increase as the volatile content of the dusts increases.

Jan 1, 1965

By Robert M. Becker

This report (part 3 of a five-part series) presents computer programs for evaluating moments and moment relationships of the generalized probability distributions extended or developed in parts I and 2. The principal program is for evaluating the first three moments and moment relationships of the compound-multinomial distribution for finite as well as for infinite populations. This is the generalized distribution for sampling to some amount of items per sample. Another program is for evaluating the first four moments, the moments of the mean, and the moment relationships of the multinomial and generalized hypergeometric distributions. This is a general moment program in sampling to some number of items per sample or for sampling to some number of samples. This program will accept either ungrouped data, frequency data, or probability data.

Jan 1, 1965

By Jr. Frank Parrish

This report describes the performance of 17 selected water-injection projects producing from Pennsylvanian-and Permian-age reservoirs. Illustrations depict reservoir structure and thickness, and production and injection history. A selected bibliography of publications pertaining to area oil recovery and geology is included. Tabulations of field and reservoir data reveal marked differences in the projects. Increased oil recovery resulted from injecting water in most cases; however, seven projects recovered less oil than the operators anticipated. Oil recovery by water injection ranged from 0.2 to 262 bbl per acre ft, or 0.1 to 22.5 pct of the initial stock-tank oil in place. Major reasons suggested for poor performance include: (1) Adverse directional horizontal permeability, (2) channeling of injected water through fractures or zones of high permeability, and (3) lack of containment of injected water. One 330-foot-deep project is among the first successful shallow water-floods in north Texas. Another project is the first successful Canyon sand-stone waterflood reported in the area. Previous gas injection in two Cisco sandstone projects did not prevent the reservoirs from responding favorably to waterflooding.

Jan 1, 1965

By A. J. Forney

Recent experiments used catalysts of plate assemblies in synthesizing high-Btu gas and gasoline indirectly from coal. A gas with a heating value of 925 to 943 Bt-: per cubic foot has been prod u la the hot-gas-recycle pilot plant from synthesis gas (3H2+100) with lathe turnings used as catalyst in the first reactor, and assemblies of parallel sprayed plats of nickel in the second. Solid plates made of Raney nickel, and steel and aluminum plates sprayed with Raney nickel or nickel oxide were tested. Those catalysts had very low resistance to gas flow; 90 percent lower than nickel granules used in previous experiments. In a single stage of synthesis thee nickel plates were only partially successful. Although the heating values of the product gas ranged from 856 to 941 Btu per cubic foot, the carbon monoxide content of he gas was above 0.1 percent. Both steel and wrought turnings were tested in single-stage synthesis, but the conversion of hydrogen and carbon monoxide was too low to attain the desired heating value of 900 Btu per cubic foot in the product gas. Assemblies of plates thermally sprayed with fusel iron were tried in an experiment to make gasoline. A gasoline yield of 52 percent (of the hydro¬carbons produced) was obtained using a 1H2-10O feed These sprayed assemblies were in service for 1,500 hours, the longest that this type of catalyst has been used. When a second reactor containing Raney nickel catalyst was added in series with the first reactor, complete utilization of the feed gas was obtained because in addition to the liquid product, a high-Btu gas with a heating value of 800 Btu per cubic foot was made.

Jan 1, 1965

By John W. Buch

Hydraulic cutting tests made on samples of Pennsylvania anthracite (3,700 psi and 260 gpm) were promising enough for the Bureau to establish a full scale experiment in an anthracite mine. Water pressure and quantity for mining anthracite were arbitrarily established at 5,000 psi and 300 gpm (1,000 hp). For full-volume flow, hydraulic pressure is controlled by orifice size with the displacement pump. The hydraulic jumbo was designed for maneuvering on pitches from 0° to 20° in any direction and for a coalbed ranging in thickness from 10 feet 6 inches to 15 feet. All motions of the jumbo are by oil hydraulics. Jet flow is controlled (start-stop) at the face, through an interlocked pushbutton system. One button is in the operator's cab; one, at the pump station; and one (a safety shutoff), near the mining face. To December 1962, 7,400 tons of bed material had been mined at an average rate of 0.800 ton per minute, with an average power requirement of 14.125 kilowatt-hours per ton. In January 1963, the objective was changed from an engineering-development basis to a research basis--to determine, ultimately, the most efficient level of operating characteristics for maximum response, as measured by mining-out rate. This research phase of the project is not yet complete, but conclusions, and the method of arriving at them, will be made the subject of another Bureau publication. It should be noted that as of December 1963 nearly 13,000 tons of bed material had been mined, at rates as high as 1. 3 tons per minute for a complete face advance.

Jan 1, 1965

By C. C. Popoff

This report reviews the phosphate deposits, mines, and industry, and prospects in 10 districts covering most of the Montana phosphate field. These districts are discussed individually, and an evaluation of the resources and potential of each is presented. Phosphate rock produced from underground mines in the Garrison district is shipped to Canada for processing to fertilizers, utilized locally for production of animal feed supplement, and pulverized and sold for direct application to the soil. Production from the Melrose district is shipped to Silver Bow and processed to elemental phosphorus. The Maxville-Philipsburg district is destined to become a major producer with the development of the Douglas Creek mine and beneficiation plant by Montana Phosphate Products Co. Montana ranks fourth after Florida, Tennessee, and Idaho in total annual production in the United States. Production him increased from about 60,000 long tons of acid-grade phosphate rock in 1940 to more than 660,000 tons of acid-, beneficiation-, and furnace-grade ore in 1961. Montana has the second largest potential resources in the Western field; in the area south of Butte there are approximately 1.2 billion tons of phosphate rock (+18 to +31 pct P2O5) available above and within 100 feet below entry level; and in the northern part of the field there are about 67.6 million tons available above entry level. In contrast to Idaho, most of the phosphate deposits in Montana are best suited to underground mining.

Jan 1, 1965

By Robert M. Becker

Particle mixtures were sampled in the laboratory, using ordinary sampling procedures, to determine whether or not the compound-multinomial probability distribution and other developments of part 2 agreed with experimental results. The objective was accomplished by the Bureau of Mines by comparing the moments and moment relationships of the appropriate probability models with their corresponding experimental values over a fairly wide range. The overall agreement between the corresponding theoretical and experimental values is both good and complete. The results demonstrate that sampling to a constant amount, such as weight, of items per sample is not the same, in general, as sampling to some constant number of items per sample. The results seem to confirm all the developments of part 2 and the application of the compound-multinomial function to bulk sampling.

Jan 1, 1965

By K. C. Dean

This report is the first of a series concerned with processes for producing magnesium. These reports will evaluate metallothermic, carbothermic , and electrolytic production methods, and will furnish a cost basis for comparing the processes. Areas deemed most promising for future research will be delineated for each procedure. This report presents briefly the history of the metallothermic process, and describes the operations of the Defense Plant Corp. (DPC) plants that employed the process. A hypothetical plant designed to produce 12,000 tons of magnesium per year, using ferrosilicon as a reductant, is described, and raw materials, energy, and major equipment requirements are estimated. Several process modifications are suggested for future research.

Jan 1, 1965

By J. L. Eakin

A method was developed by the Bureau of Mines in the laboratory and in the field to relieve capillary waterblocks in gas wells. Impaired gas permeability was improved by this inexpensive chemical treatment which lowers the surface tension of the water held in the capillaries of the formation. Effectiveness of the alcohol-surfactant treatment was tested with a variety of chemicals and with sandstone cores cut from rocks having relatively low permeability. Field tests on 20 gas-producing and storage wells demonstrated the effectiveness and limitations of the method. The productive capacity of some wells was doubled by the treatment. The final test was evaluated by the neutron logging technique for measuring changes in apparent liquid saturation. Maximum apparent liquid saturation was reduced by 52 percent; gas production rate increased from 2.3 to 3.5 MMcfd (million cubic feet per day).

Jan 1, 1965

By Raymond L. Lowrie

Coal deposits in the Boulder-Weld County coalfield in Colorado are analyzed in relation to economic factors governing the growth, stability, and competitive potential of the coal industry. Recoverable reserves, estimated to be 571 million tons, are discussed in detail, particularly those in the Erie and Frederick Quadrangles. Geology of the coal measures, quantity and quality of water resources, and chemical and physical properties of the coal are described. Coal production factors, including mining techniques and equipment, labor requirements, transportation facilities and rates, and markets, are considered for coal's position in competition with alternate fuels. Growth of the fuels market, through increasing thermal-electric power generation in the Denver Metropolitan Area, will stimulate coal production in Colorado. Reserves of the contiguous Boulder-Weld coalfield, if mined in a sustained, year-round, high-tonnage operation, could be used to supply much of that fuel demand.

Jan 1, 1966

By Alla D. Mah

Compilation of data on materials of metallurgical interest is one of the important activities of the Berkeley Thermodynamics Laboratory of the Bureau of Mines. Recent renewed interest in metallurgy of vanadium renders the present compilation a timely guide for experimentation to improve present methods or to develop better methods of extractive metallurgy. Thermodynamic data for vanadium and its inorganic compounds have been critically surveyed, selected, and compiled into one convenient reference from which information can be readily obtained for evaluating heat balances, determining trends, and establishing limits of metallurgical processes. By indicating the direction of experimentation, this report enables the saving of time, effort, and expense which would otherwise be necessary for trial and error experimentation. Much of the data has been obtained experimentally at the Berkeley laboratory. Other data were collected through an extensive survey of worldwide literature through April 1965. Estimates were made when no data were avail-able. Data on the vanadium halides was sparse, and the results derived from existing data were at times divergent. Some of the selected values for the halides may need modification as more or better experimental data become available.

Jan 1, 1966

By R. W. Van Dolah

An attempt has been made in this investigation to define the conditions under which ammonium nitrate (AN) might detonate as a result of involvement in fire. The initiation of detonation by shocks derived from explosives or from projectile impact was investigated as a function of temperature and charge diameter. A new technique was devised to investigate the burning of raw and contaminated AN under pressure. No transition, to detonation in AN was obtained in the burning experiments. The critical diameter for detonation of fertilizer-grade AN was found to be quite small when the AN was at temperatures just below melting point; this indicates that initiation of detonation may be less difficult at elevated temperatures but such initiation by gas-phase detonation was shown to be unlikely. Transition from burning to detonation was obtained with AN intimately mixed with fuels that included polyethyl-ene, paper, and fuel oil when these were contained in vessels with restricted vents. However, the experimental results supported by an analytical study indicate that the initiation of detonation in AN from fire exposure in normal storage and from transportation incidents is quite improbable. The detonation of AN in recent incidents more likely may have resulted from the effects of adjacent explosions.

Jan 1, 1966

By Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

Jan 1, 1966

By Harry R. Nicholls

Preliminary tests on presplitting rock in the presence of an in situ static stress field were undertaken to study the influence of a horizontal static stress field on the creation of a vertical presplit fracture plane. These tests indicated that it is easier to fracture the rock parallel to the in situ maximum compressive stress than in other directions. Instrumented shots indicate that the interaction of stress waves generated by the detonating charges is probably responsible for starting tensile fractures between shotholes and that expanding gases may propagate these initial cracks by a wedging action. The hole spacing for presplitting appears to be equal to the half wavelength of the stress wave. However, wider hole spacing appears feasible if the initial fracture is started by closer hole spacing.

Jan 1, 1966

By R. F. Kendall

Only a limited number of mass and infrared reference spectra of high purity unsaturated hydrocarbons and oxygenates are presently available in the literature. To aid Bureau of Mines research programs requiring such references, 64 mass spectra and 70 infrared spectra were obtained and are reported. The individual compounds, acquired from commercial sources, were purified by preparatory gas chromatography. Purity determinations were made using a combination of analytical gas chromatography, microhydrogenation, and catalytic deoxygenation. These spectra will aid spectroscopists in the identification of compounds of the types reported.

Jan 1, 1966

By D. A. Elkins

This report is the second of a series of three that will evaluate, in order, the metallothermic, carbothermic, and electrolytic methods of magnesium production. The historical development of the carbothermic process is outlined. Production costs varying from 38.9 to 21.8 cents per pound of magnesium are estimated for different versions of the process. Additional suggested process modifications are listed. The technical and economic potential of the different versions are compared. Areas deemed most promising for future research on the process are delineated.

Jan 1, 1967

By J. M. Singer

Methods are proposed for predicting concentrations of nitrogen oxides and carbon monoxide in the combustion gases of flames, specifically of lean, stoichiometric, and rich propane-air flames. Calculations are based on kinetic and thermodynamic theory. These theoretical data are compared with concentrations observed experimentally downstream of flat grid-type burner flames (approximately 25,000 Btu/hr) that were used to simulate gas appliances such as water and space heaters. Air pollutant concentrations are also computed for (1) flames chemically perturbed by recycling flue gases into the primary fuel-air mixtures; (2) flames thermally perturbed by cooling the burned gases at different rates; and (3) flames perturbed by combination of these two effects. In general, experimental and computed concentrations agree to within a factor of 2 to 7 with the experimental values always being higher than the theoretical. The theoretical analysis indicates that cooling the primary flame by recycling cold flue gases (with and without excess air) reduces the relative emission of nitric oxide and increases emission of carbon monoxide if the flame stoichiometry does not radically change. Cooling rates of about 5,500° to 10,000° R/sec starting at about 3,500° R generally suffice to prevent nitric oxide concentrations in lean flames from increasing much above the initial values at the combustion zone; these same cooling rates do not prevent oxidation of most of the initial carbon monoxide.

Jan 1, 1967

By Jack L. Henry

The monocarbide region of the ternary system U-C-O has been investigated at 1,700° C as the first phase of a more extensive study of a portion of the four-component system U-C-O-N. An area bounded by the following compositional limits in atomic percent was studied: U, 44 to 55; C, 30 to 60; 0, 0.2 to 20. Compacts composed of mixtures of uranium, graphite, and uranium dioxide powders were sintered at 1,700° C under an equilibrium pressure of carbon monoxide to produce uranium oxycarbide specimens having a variety of compositions. Sintered specimens were evaluated by X-ray, chemical analysis, and ceramographic techniques. Solid-solution boundaries and phase relations have been established, and the effects of composition on the lattice parameter as well as the decomposition pressure have been investigated. Oxygen can be substituted for carbon in stoichiometric uranium monocarbide to the extent of about 17 atomic percent at 1,700° C. The composition range of the oxycarbide solid solution extends from about 48 to 51 atomic percent uranium in the low oxygen region. Above 10 atomic percent oxygen the composition range narrows to less than 1 atomic percent uranium. Carbon monoxide exists as a gaseous phase in equilibrium with all compositions which contain oxygen. Five separate phase fields were found bounding the solid-solution area. Other phases within this portion of the system include uranium, uranium dioxide, uranium dicarbide, and uranium sesquicarbide. Decomposition pressures of oxycarbide compositions at 1,700° C have been found to vary from a few microns for stoichiometric and uranium-rich compositions to 35 torr for carbon-oxygen-rich specimens. Lattice parameters were found to depend upon the U to C + 0 ratio as well upon the extent of substitution of oxygen into the stoichiometric monocarbide lattice.

Jan 1, 1967