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By A. R. Rule

A flotation process was developed by the Bureau of Mines for separation of carbonate and phosphate minerals occurring in unaltered phosphate ores of the Phosphoria formation. The process involves depression of phosphate minerals with fluosilicic acid and flotation of carbonate minerals with fatty acid emulsions. In individual laboratory tests, selective removal of carbonates was achieved with phosphate recoveries ranging from 60 to 80 pct P205. In continuous-circuit testing, sizing and separate treatment of coarse and fine fractions was necessary to achieve 65-pct P205 recovery. Concentrate grade ranged from 26 to 33 pct P205. The flotation tailings containing primarily carbonate and phosphate minerals is a potential fertilizer material. When reacted with H3P04, concentrated superphosphate containing approximately 40 pct available P205 was obtained.

Jan 1, 1974

By A. R. Rule

This report describes preliminary studies by the Bureau of Mines to develop a procedure for extracting the fluorine from low-grade fluorspar ores in which the CaF2 particles are finely locked in the calcite matrix. A combination of flotation beneficiation and pyrohydrolysis is applied to recover and to liberate the fluorine. Flotation of a finely locked high-calcite fluorspar ore containing only 11.7 pct CaF2 recovered over 92 pct of the fluorspar at a grade of 51 to 52 pct CaF2. Pyrohydrolysis of the flotation concentrate liberated nearly 90 pct of the fluorine as aqueous HF. By this procedure over 80 pct of the fluorine contained in the original ore was extracted.

Jan 1, 1974

By R. B. Schluter

The objective of this Bureau of Mines investigation was to determine the effects of adding manganese compounds and ores to iron ore pellets. Manganese dioxide, carbonate, sulfate and chloride, plus six manganiferous ores from the Minnesota Cuyuna Range were tested as additives to increase the manganese content of iron ore pellets. One to 5 percent manganese, as a compound or ore, was added to five magnetite concentrates and one hematite concentrate. These concentrates were ballad, indurated (1,300° C), and tested for reducibility. Manganese sulfate and chloride were unsatisfactory additives causing cracking and degradation of the pellets during reduction. Manganese dioxide, carbonate, and the ores were satisfactory additives. The additives increased pellet compression strengths with a corresponding loss of reducibility, as compared to the pellets without manganese additions. The changes in compression strengths and reducibility were caused by the formation of Jacobite spinel and slag within the pellets. However, when the induration temperature was lowered from 1,300° to 1,200° C the reducibility and compression strengths were comparable to the pellets without manganese additions indurated at 1,300° C.

Jan 1, 1974

By Phillip N. Yasnowsky

The thrust of this Bureau of Mines report is to relate the size of automobiles to the price of gasoline, and the use of minerals in automobile manufacture to the size of automobiles. Only one of the many plausible scenarios of public reaction to higher gasoline prices, a switch to economy size automobiles, is developed. No account is taken of other potential impacts such as improvements in public transportation or increased occupancy per vehicle. Furthermore, a gasoline price increase is the only incentive to the greater utilization of economy cars that is considered. A gasoline price increase to $0.60 per gallon would reduce the amount of minerals required to produce the automobiles sold in the United States by an estimated 15 percent. Gasoline prices of $0.80 and $1 per gallon would cause declines in mineral requirements for U.S. automobile sales estimated at 26 percent and 35 percent, respectively.

Jan 1, 1974

By Andrew A. Cochran

Laboratory-scale research was conducted by the Bureau of Mines to develop a new process for treating electroplating and other wastes. Various acid and alkaline cyanide wastes were combined under controlled conditions to neutralize the wastes and to almost completely precipitate the metals and cyanides. The metals were subsequently recovered for recycling; the cyanides can also be easily recycled. The process was successfully used to treat the major types of electroplating and etching wastes, containing Cd, Cr, Cu, Ni, and Zn, and to treat both concentrated and dilute wastes. The economic aspects of treating concentrated electroplating, etching, and anodizing wastes are especially attractive because of the low cost of mixing two wastes, the high value of the recovered metals, and the simplicity of the recovery procedures. The filtrates from the waste-plus-waste step were relatively harmless compared with the original wastes and met Public Health Service standards for free cyanide content. Free cyanide ions were not detected in most of the filtrates; the limit of detection was 0.03 ppm. Only small amounts of HCN were produced during the neutralization; the HCN was collected and neutralized.

Jan 1, 1974

By Harold E. Marr

Energy dispersion X-ray analysis was evaluated for possible application in the secondary metals industries for the rapid analysis and identification of copper-base alloys. Laboratory investigations of standard brass and bronze samples indicate that X-ray methods are capable of separating standard alloys into 10 general classes with analytical times of less than 3 seconds per sample for clean, flat samples. A radioactive source of americium 241 with a secondary fluorescer was used as an excitation source, and a lithium-drifted silicon semiconductor detector was utilized for energy discrimination of X-rays.

Jan 1, 1974

By C. B. Daellenbach

A prototype particulate size analyzer system was developed that would rapidly determine size distributions of homogeneous and two-mineral materials in the 74-micrometer (200-mesh) to 7-micrometer size range. The system sizes particles in a series of hydrocyclone elutriation steps and senses the weight of the five sized fractions by nuclear attenuation techniques. Size distribution of materials was determined from experimentally developed mathematical relationships that existed between particulate weight and the measured transmittance of gamma rays from an Americium-241 source. In the developmental phases, size distributions of three minerals (quartz, magnetite, and hematite) and a laboratory prepared two-mineral mixture of quartz and magnetite were accurately determined by the prototype system. In later stages of the investigation, semiconcentrates, an intermediate magnetic product from a taconite plant, were evaluated. Using 25-gram feed samples of this industrial material, the analyzer system was found to predict weight percentages for individual size fractions with an accuracy of ±0.85 percent or better at a 95-percent confidence level.

Jan 1, 1974

By R. R. Schehl

The Bureau of Mines analyzed the structure of a high-grade metallurgical coke, carbonized at different temperatures in the range 500° to 1,000° C, through X-ray diffraction studies. Growth in the crystallite size with increasing coking temperature was calculated from profile analysis and compared with values obtained from the radial distribution function. The carbonization temperature appeared to have little influence upon the stack height, whereas the layer diameters more than doubled in size between 500° and 1,000° C. These results are comparable to those obtained from other studies of poorer quality cokes.

Jan 1, 1974

By Verne E. Hooker

This Bureau of Mines report summarizes the results of modifications in the borehole deformation gage design and subsequent changes in the overcoring techniques. Modifications in the borehole deformation gage have greatly improved the creep characteristics and enhanced the versatility of the gage. In situ field tests in competent rock near St. Cloud, Minn., provided sufficient data to compare the reliability between gages and new techniques in obtaining good engineering estimates of stresses. Near-surface horizontal stresses at the test sites are compressive and biaxial in nature.

Jan 1, 1974

By K. C. Dean

Fine-sized mineral wastes discarded by ore milling plants require stabilization to prevent air and water pollution. Stabilization has been attained by physical, chemical, vegetative, and combination procedures. Vegetative reclamation is preferred to physical and chemical stabilization but is diffi¬cult to achieve because the wastes are sterile, contain deleterious inorganic salts, and lack the essential nutrients and physical characteristics required for sustaining vegetative growth. Methods now have been developed for attain¬ing vegetative growth on all but excessively acidic, basic, or saline tailings at costs ranging from $120 to $650 per acre. The cost for stabilizing tail¬ings requiring more intensive treatment techniques may range upward to $1,750 per acre. This report summarizes procedures developed by the Bureau of Mines and industry for vegetating amenable tailings, lists costs for the various processes, and suggests procedures that may be applicable for stabilizing saline and pyrite-containing tailings. Ridged planting beds, drip irrigation, and deep-furrow planting techniques are suggested for stabilizing saline wastes. A combination of mill tailings and sewage sludge can be used for pro¬ducing synthetic soils, and layers of sewage sludge buried under a layer of tailings offer promise of inhibiting acid formation from oxidation of sulfides in mineral wastes.

Jan 1, 1974

By Laurance L. Oden

The Bureau of Mines conducted corrosion tests of 18 commercial alloys in H3 P04 -phosphate rock or A1,03 slurry, in 10 pct HF, and in 25 pct H2 SiF6 to simulate three environments anticipated in a Bureau process to extract fluoride values from phosphate rock. Small alloy coupons were rotated in duplicate tests at 4.4 to 21 fps in the slurry at 170° C to determine rates of erosion-corrosion. At 4.4 fps the lowest rates, in mils penetration per year (mpy), were measured for Hastelloy C-276 (<20), Hastelloy B (30), and Inconel 625 (150);the rates increased at 21 fps to 55 mpy, 45 mpy, and 1,000 mpy, respectively. The corrosion rate for all alloys exceeded 40 mpy in either the equilibrium vapor or liquid phases of aqueous solutions containing 10 pct HF or 25 pct H2SiF6 at 100° C. Uniform corrosion in 10 pct HF at 50° C was observed only for Inconel 625 (22 mpy), Hastelloy C-276 (43 mpy), and Illium 98 (17 mpy). Inconel 625 (0.75 mpy), Hastelloy C-276 (1.3 mpy), Illium 98 (1.7 mpy), and Incoloy 825 (0.45 mpy) were attacked uniformly in 25 pct H2SiF6 at 50° C.

Jan 1, 1974

By John E. Kelley

A method for measuring the spark-shower radiance of metals when abraded on a grinding wheel was developed by the Bureau of Mines for evaluating the sparking tendency of metals. The radiance was measured in units of emissive power per solid angle per area of the detector. Over 100 metals were tested and rated relative to commercially pure iron. The metals tested included elemental metals, iron binary and ternary alloys, iron-carbon ternary alloys, commercial steels, nonferrous alloys, and a few hard-metal compounds. Some alloys were synthesized; others were obtained commercially. Alloys that possessed good strength properties were emphasized for selection. The results indicate that the spark-shower radiance of plain carbon steels and carbon alloy steels was greater than that of pure iron. Certain elements, particularly vanadium and chromium, reduced the sparking tendency of iron. Stainless steels and particularly nickel alloys displayed low spark-shower radiance. Some metallic elements had much lower radiance than iron; others, much greater. Plain carbon steels, heat treated to a variety of hardnesses, gave radiance values that generally increased with increasing hardness. The effect on sparking tendency of an increase in hardness of an alloy steel was studied. The sparking tendency increased with an increase in hardness to a maximum, then decreased with a further increase in hardness.

Jan 1, 1974

By L. E. Schultze

[The Bureau of Mines conducted bench-scale studies to develop techniques for stripping tetravalent cerium from tri-n-butyl phosphate solutions. Experiments were conducted in a constant-temperature bath using beakers and mechanical stirring. Ninety-five pct of the cerium was stripped from a 50-pct tri-n-butyl phosphate 50-pct kerosene solution containing 0.18 M cerium in 15 minutes at 50° C using 0.11 M aqueous formaldehyde.]

Jan 1, 1974

By R. V. Subramanian

This project financed by the Bureau of Mines investigated the use of polymers to achieve rock bonding and reinforce coal mine structures for better or permanent ground support. Support was achieved by pumping the polymers into the rock interstices to bond the mass together for increased structural competence. Holes were drilled in the mine roof, after which the polymers were injected at about 100 psi to permeate the cracks. Initial laboratory work indicated that of all the resin systems tested, the epoxy resins could most likely be modified to be suitable for rock injection. This was confirmed when several potentially suitable resin systems underwent intensive evaluation. In a series of three field tests, two conducted in a copper mine with coal mine-type shale and the third in a coal mine, it was shown that the polymers penetrated cracks less than 0.005 inch wide. The fast-setting epoxy systems, cured out in thin films under mine conditions, produced a bond exceeding the strength of the uncracked virgin rock.

Jan 1, 1974

By C. M. McCulloch

The natural vertical fracture system in bituminous coalbeds is called cleat. Cleat orientation commonly controls the direction of mining with major development paralleling the face cleat. Previous researchers have categorized the origin of cleat as endogenetic, relating the origin of cleat to compaction and coalification, and exogenetic, relating the origin of cleat to tectonic forces. In the coalbeds studied for this report it was found that tectonic forces were the controlling factor of cleat formation. Face cleats were formed as extension fractures during structural deformation, and butt cleats, as release fractures during erosion and uplift. The face cleat of the Pittsburgh coalbed rotates from N 80° W in north-western West Virginia to N 57° W in southwestern Pennsylvania; the face cleat maintains a perpendicular orientation to the shifting axial trend of local structures. Cleat orientation in other bituminous coalbeds in Virginia, Utah, Oklahoma, and Central Pennsylvania showed a similar relationship to local structure. Directional permeability of coal is directly related to cleat. Holes drilled perpendicular to the face cleat yield from 2.5 to 10 times the amount of gas released as compared with holes drilled perpendicular to the butt cleat.

Jan 1, 1974

By Carlon S. Land

The Bureau of Mines investigated the influence of a free gas saturation on oil recovery by water drive. A digital computer was used to calculate the combined oil recovery from solution-gas drive to various states of depletion. Results of these calculations are compared and optimum conditions for the maximum oil recovery are found for various fluid-rock systems. For most of the fluid-rock systems, the calculations show an optimum gas saturation other than zero. Using fluid and rock properties as parameters, graphs are plotted showing the optimum gas saturation and increase in oil recovery brought about by the gas saturation. The effects of fluid properties and relative permeability on the optimum gas saturation are seen in these graphs. The graphs can be used as guides in connection with other considerations in determining the optimum time to start a waterflood. They should also be helpful in determining the MER of a water-drive reservoir. The effects of compressibility and solubility of the trapped gas saturation are investigated for select cases using a backward difference scheme to solve the partial differential equation of three-phase flow. From these calculations, it is observed that some benefit of a gas saturation remains for injection pressures up to 1.5 times the original bubble-point pressure.

Jan 1, 1974

By H. V. Makar

The Bureau of Mines successfully demonstrated, on a pilot plant scale, a sodium sulfate (Na2S04) refining process for removal of copper from molten ferrous scrap. Previous tests established technical feasibility on a bench scale for achieving low copper concentrations and determining the principal factors controlling process efficiency. The pilot plant study involved a 1-ton arc furnace for melting ferrous scrap and a 1-1/2-ton treatment ladle. Results of these tests showed that copper removals obtained in laboratory tests (approximately 40 relative percent copper removal with 10 weight-percent surface addition of sodium sulfate) could be achieved on the pilot plant scale when excess carbon was added with the sodium sulfate compacts. Data were obtained on temperature losses and carbon consumption related to Na2SO4 treatment.

Jan 1, 1974

The Bureau of Mines has successfully used sulfur hexafluoride (SF6) as a tracer gas to measure mine air flows under conditions where conventional methods have failed. SF6 was employed experimentally to measure accurately recirculation of return into intake air caused by leakage through an old stoped area, to check for potential leakage from an adjacent mine, to trace 10,000 cfm of "lost" air from an intake airway, and to measure transit air time through uranium mines. It proved useful as a means of accurately measuring airflow volumes in airways of large cross section and very low flow velocity, and in determining the recirculation resulting from underground cooling plants.

Jan 1, 1974

By John L. Reuss

A laboratory study was conducted by the Bureau of Mines to investigate the technical feasibility of decomposing hydrous magnesium chlorides by using a steam pyrohydrolysis technique. This procedure consisted of injecting steam into the atmosphere of a decomposition furnace containing samples of hydrous magnesium chloride and determining the rate of hydrolysis by measuring the rate of chloride evolution. The variables investigated were temperature, amount of water vapor in the decomposition atmosphere, and hydration stage of magnesium chloride. The application of steam was shown to accelerate both the rate and completeness of magnesium chloride decomposition reactions. For example, when magnesium chloride hexahydrate is exposed to a furnace temperature of 600&apos; C in an air atmosphere for 20 minutes, the decomposition is 37 percent. Under identical conditions in a steam atmosphere, the decomposition is in excess of 70 percent. The magnesium oxide produced by the steam pyrohydrolysis of magnesium chloride dihydrate at 800° C contained 98 percent magnesium oxide. Based on magnesium oxide composition, this is equivalent to that of burned magnesite produced at temperatures in excess of 1,300° C. To demonstrate the quality of the product on a practical basis, metal reduction tests have shown it to be equivalent to reagent-grade magnesium oxide as a carbothermic reduction feed material.

Jan 1, 1974

By M. L. Whisman

The Bureau of Mines developed and tested in the laboratory several innovative techniques for reclaiming used lubricating oil. These processes included percolation through both chemically treated clay and ion-exchange resins, distillation through batch and continuous wiped-wall vacuum apparatus, treatment with solvent extraction systems, and chemical removal of impurities with chelating agents. In each treatment, the criteria of evaluation was oil recovery and reduction of acidic and metallic components. Both vacuum distillation and solvent treatment ranked high in their abilities to remove acidic and metallic components of the used oil with good oil recoveries. A combination of the two techniques gave the best overall results in terms of quality evaluations made by established bench tests. The methods were not ranked according to economic practicablity.

Jan 1, 1974