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By Franklin B. W. Woodbury

The Bureau of Mines, as part of its goal of helping maintain an adequate supply of minerals to meet national economic and strategic A needs, is evaluating alternative technologies to treat oxidized taconites. Since process control is an essential element in the application of these process technologies, research was performed on a prototype monitoring system utilizing a Californium-252 (252-Cf) neutron source and a thermal neutron capture-gamma ray spectra analysis method to measure the amount of iron and percent solids in process slurries. The prototype system was used to monitor the concentrate and tailing streams in a 900-lb/hr flotation pilot plant during continuous around-the-clock tests. The iron content of the process slurries was determined by measuring the total peak areas under the capture spectrum peaks at 7.626-7.632 MeV, the associated escape peaks at 7.136-7.122 and 6.626-6.612 MeV, and the iron doublets at 4.900 and 4.998 MeV. A potential method for determining the percent solids in process slurries using the 2.22 MeV hydrogen capture peak is discussed. Results of this work demonstrate a potential method for providing process control parameters using the data from thermal neutron capture-gamma ray reactions.

Jan 1, 1980

By T. O. Llewellyn

The Bureau of Mines conducted batch-?scale tests on a sample of parphyry copper mill tailings as part of a study to determine the feasibility of rutile recovery from this source. The tailings that were tested contained 0.75 percent titanium dioxide (Ti02), with about two-thirds of the Ti02 values occurring as rutile. Mineralogical studies indicated that about one-half of the Ti02 content could be considered recoverable. Beneficiation studies of the tailings showed that best flotation results were obtained when sulfides and carbonates were removed by bulk flotation prior to rutile flotation. Rutile flotation was most effective when a petroleum sulfonate collector was used in an acid circuit. From this basic method of flotation, two alternative procedures were developed. The first procedure was to size and grind the tailings to minus 200 mesh; deslime the total pulp; and then float the sulfides, carbonates, and rutile. The second procedure was the same, except that it did not include sizing and grinding. Flotation of the sized and ground tailings yielded rutile concentrates containing 43.1 percent Ti02 and 75.7 percent of the recoverable Ti02. Rutile concentrates floated from the tailings that were deslimed but not ground contained only 34.7 percent Ti02 and 69.4 percent of the recoverable Ti02.

Jan 1, 1980

By H. R. Beard

The Bureau of Mines investigated the absorption of radium and thorium from waste uranium leach liquor by clays and other materials. This work was conducted in support of the Bureau's goal of minimizing the environmental conflicts, impacts, and occupational hazards associated with mining and milling operations. Tailing and soil samples from New Mexico were evaluated for their potential to absorb radium and thorium from tailing liquors. Absorption ranged from 0 to 97 pct for radium and 0 to 60 pct for thorium. Some samples that readily absorbed radium were contacted with various salt solutions that could be present in tailing solutions to determine whether desorption would be a potential problem. The desorption of radium ranged from 0 to 75 pct. An alpha spectrometric method was used to determine the radium and thorium concentrations in the solutions and solids.

Jan 1, 1980

By E. L. Litchfield

Four short-term studies of practical ignition problems were undertaken and completed during the course of the Bureau of Mines project "Development of Specifications for Intrinsically Safe Equipment." Conclusions were as follows: (1) the most easily ignitible mixture of propane-air in a PTB break flash apparatus is approximately 5.2 percent propane; (2) miniature lamp bulbs to be used in intrinsically safe circuits are about as incendive to coal dust-air as to methane-air and should be tested in gas mixtures containing about 7.0 to 7.5 percent methane; (3) the sodium amalgam contained in high-pressure sodium lamps does not present an ignition hazard for coal dust or methane, where the lamps contain no more than 30 milligrams of amal-gam; (4) the maximum allowable surface temperature of permissible electrical enclosures should remain at 150° C despite efforts by industry groups to raise the value to 200° C.

Jan 1, 1980

By W. D. Riley

The U.S. Department of the Interior, Bureau of Mines, has been conducting minerals recovery research in support of the nation's geothermal program since 1974. The Bureau's program of laboratory and field studies has focused on determining the materials of construction for geothermal resource recovery plants and an the recovery of mineral values from the geobrines. An analytical program has been conducted at the Avondale Research Center to determine the chemical constituents of some high- and low-salinity geobrines found in the Imperial, Valley of California. Data are reported for the early stages of brine production of femur geothermal wells--the low-salinity, medium-enthalpy brines from the East Mesa Known Geothermal Resource Area (KGRA), Mesa 6-1 and 6-2, and the high-salinity, high-enthalpy brine from the Salton Sea KGRA, Magmamax 1 and Woolsey 1. The reported results indicate the importance of the operating and engineering history, the operating parameters during sampling, and the method of sampling in order to evaluate the chemical analyses.

Jan 1, 1980

By B. W. Jong

As part of the Bureau of Mines program to develop substitute or improved performance refractory materials for metallurgical applications, the Tuscaloosa Research Center has evaluated the effect of additives on sintering and strength properties of aialon (silicon aluminum oxynitride) compositions fabricated by a conventional powder metallurgy technique. Additions of Y203, Gd203, CeO2, MgO, ZrO2, ZrSiO4, and MgA12O4 to a sialon composition containing 70 pct ß-Si3N4 + 30 pct a-A1203 increased sintered densities by as much as 50 pct over densities of undoped material. The studies also indicated that sintered densities reached a maximum between 20 and 30 mole-pct a-A1203 when a series of sialon compositions of a-Si3N4, having 6.7 to 57.9 pet a-Al203, were doped with Y203, Gd2O3, and MgO. In studies to establish the effect of the crystalline phase of the silicon nitride and alumina used, tests were made using a- and ß-Si3N4 and a- and ?-A12 03 as starting materials. The tests indicated that when using an addition of 5 wt-pct Y203, best results were obtained with a sialon composed of 74.4 mole-pct a-Si304 and 25.6 mole-pct ?-A1203. In other tests made with this sialon composition MOR values of 28,120 and 29,500 psi at 25° C, and 23,520 and 16,850 psi at 1,400° C, were obtained when doping with 5 wt-pct ZrSiO4 and ZrO2, respectively.

Jan 1, 1980

By Steven J. Page

The Bureau of Mines used fiber-laden air to test two identical fibrous aerosol monitors (FAM) in order to establish the FAM-optical count correlation. The FAM is a unique instrument developed by GCA Corp. (GCA) to measure real-time fibrous aerosol concentrations. It will also respond to particulates that have sufficient shape irregularities to possess fiber characteristics such as the 3:1 length: diameter (L:D) aspect ratio. Results of the Bureau's laboratory tests showed that the FAM response is linearly correlated to concentration data obtained using the optical membrane filter count technique approved by the National Institute for Occupational Safety and Health (NIOSH), U.S. Department of Health, Education, and Welfare. A plot of the FAM-optical count correlation showed that FAM concentration readings are generally well within ±25 pct of the optical membrane filter count. Initial tests to estimate the best ratio control setting of the FAM for 5-µm fiber-length discrimination were performed using one instrument only (the ratio control setting determines the minimum threshold fiber length that will be detected by the FAM). The estimated setting was then used to correlate both FAM units. The result was a 65 pct difference in correlation between the two units. It appears that the major factor responsible for this difference was the internal adjustment of the photomultiplier detector sensitivity for each of the two FAM units.

Jan 1, 1980

By J. R. Cobble

As part of the Federal Bureau of Mines project to develop new or improved materials for metallurgical furnace applications, the Tuscaloosa (Ala.) Research Center has conducted research to develop a reproducible laboratory test for evaluating the resistance of refractories to molten slags. Tests were conducted with a slag representative of slag used to produce mineral wool. A rotating cylindrical furnace was lined with the brick being tested, and it was operated at temperatures up to 1,660° C for periods ranging from 8 to 32 hours. The effects of such variables as slag temperature, rotational velocity, charge rate, and contact time on refractory erosion were determined. The research demonstrated the reproducibility of the test procedure developed.

Jan 1, 1980

By Martin Hertzberg

The concept of limit burning velocities, formulated in an earlier Bureau of Mines report (RI 8127), is applied to the problem of flame propagation through tubes of finite size. The limit burning velocity for conductive-convective wall-loss quenching (process b) is (Su)b = [aPe,] where the proper choice of critical Peclet constant, Pe, is determined mainly by the ratio of contact-perimeter loss area to flame-zone cross sectional area. This ratio of loss area to propagation area relates to the shape of the flame front and its control by buoyancy and by boundary conditions. The comparison of (Su)b with previously defined limit velocities for systems mixed by natural convection allows one to assess the influence of tube dimensions and boundary constraints on the "true" or earthly limits for the three directions of propagation. The flame quenching caused by inert powders is shown to be similarly described in terms of a limit burning velocity, (Su)?b. The tube's surface-to-volume ratio (~1/ro) is simply replaced by the powder's surface area per unit volume of the flammable mixture. Thermal loss quenching by these "internal walls" occurs at a critical Peclet constant somewhat higher than that observed for tubes, and the problem is complicated by the finite heat capacities of the powders and particle lag effects in the flame front.

Jan 1, 1980

By J. S. Dunning

One Federal Bureau of Mines research goal, to minimize requirements for domestically scarce mineral commodities through conservation and substitution, can be accomplished by utilizing more abundant elements such as iron, molybdenum, and titanium. An example of this research is the study of precipitation-hardening, iron-base alloys containing molybdenum and titanium, as substitutes for the high-tonnage stainless steels that are high in imported nickel and chromium. The precipitation hardened iron-base alloys are strengthened by a dispersion of the ternary Laves phase, Fe2 (Mo, Ti). Aluminum and chromium additions changed the solid solubility limits of molybdenum and titanium in a-iron and affected the composition of precipitating phases. A baseline composition of Fe-7Mo-2Ti was selected to study the effects of aluminum and chromium additions on the precipitation-hardening mechanism and microstructure and was also used in studies of mechanical properties and oxidation resistance. The study yielded workable, precipitation-hardening alloys, with elevated temperature strengths equivalent to or superior to types 304 and 316 stainless steels. Chromium and aluminum additions in combination were more effective in providing oxidation resistance than either addition was alone.

Jan 1, 1980

By J. M. Gomes

The Bureau of Mines has investigated the occurrence and recovery of by-product heavy minerals from sand and gravel operations as a means of assessing the Nation's resources. Sand samples from 63 locations in central and southern California were treated to yield heavy-mineral concentrates. The mineral compositions of the concentrates were characterized by chemical and mineralogical examinations. Additional large quantities of concentrates were prepared from selected deposits that contained significant quantities. Beneficiation studies were performed on these concentrates to recover individual mineral products. Gold was recovered by amalgamation; platinum-group metals and radioactive minerals by flotation; magnetite, ilmenite, and chromite by magnetic and high-tension separation techniques.

Jan 1, 1980

By H. O. McDonald

Solutions containing Cr6+ and sulfuric acid are used in a number of surface-finishing operations. Substantial quantities of chromium and copper are lost and pollution problems are created when the spent solutions are discarded. To minimize the undesirable environmental effects while improving secondary resource recovery technology, the Bureau of Mines is conducting research to detoxify and recover metals from these solutions. Spent etchants are treated to remove copper and reduce Cr6+ to Cr 3+ in an electrolytic cell. The anodes and cathodes are granulated coke. The spent solution is continuously pumped through the electrodes. Hexavalent chromium is reduced to trivalent chromium, and copper is recovered at the cathode. Reoxidation of Cr3+ at the anode was not observed. The removal and recovery of copper reduction of Cr6+ lessen chemical demand and increase efficiency in waste in treatment operations associated with the use of these solutions.

Jan 1, 1980

By Robert P. Vinson, John C. LaScola, Fred N. Kissell, Edward D. Thimon

The face ventilation measurement method developed by the Bureau of Mines involves releasing a small volume of tracer gas (SF6) on the off-curtain side of the working face at the start of the mining cycle. At the same time, gas bottle samples are taken in the immediate return airway. The gas samples are analyzed, and a curve is drawn of SF6 concentration versus time. From this curve, the percentage of gas removed per time is calculated. A curve showing a high percentage of the tracer gas removed in a short period would represent a well-ventilated face. The face ventilation measurement method was tested in a full-scale mine entry model. Subsequently it was used underground to evaluate the spray-fan ventilation system and in an MSHA test facility to test machine-mounted scrubbers. The method was shown to be a simple and effective way of evaluating face ventilation systems.

Jan 1, 1980

By J. M. Kuchta

The chemical and thermal criteria used for predicting the spontaneous combustion hazard are briefly reviewed and data are presented to characterize the gas desorptions and self-heating tendencies of 29 U.S. coals. Closed vessel desorption experiments showed that CO, CO2, and CH4 are the main gases evolved and that the CO, CO/?O2 index, and 02 absorption rate increase with decreasing rank and increasing oxygen content of the coal. In this Bureau of Mines report, the effects of temperature, moisture, and other variables are discussed together with the application of the data to the complex conditions encountered in a mining environment. An important finding is that the presence of CO alone in a mine is not necessarily an indication of a self-heating reaction of the coal. Based upon experiments conducted in an adiabatic-type calorimeter, the self-heating temperatures of lignite and subbituminous coals can be as low as 30° C, whereas the bituminous coals require a temperature of about 60° C or more. The self-heating hazard is greatest when the coals are dried and exposed to a high humidity condition, apparently as a result of the "heat-of-wetting." Generally, the hazard is greatest with the western coals of the United States.

Jan 1, 1980

By W. H. Eddy

The Bureau of Mines used several laboratory batch flotation schemes combined with magnetic separation to investigate the feasibility of recovering potash feldspar and glass sands from molybdenite tailings. Four molybdenite tailings or prospective tailings were used as test samples. Feldspar concentrates containing from 10.7 pct to 12.0 pct K2O were recovered from three of the four samples. The alkali content of the fourth sample met the grade for a mixed feldspar. All the feldspar concentrates contained iron in excess of the 0.10-pct-Fe203 specification for most uses. Electron-beam microprobe examination of the feldspar concentrates showed the presence of an iron-bearing potash feldspar in quantities that were excessive with respect to most iron specifications. However, a high-quality glass sand was produced from all of the samples.

Jan 1, 1980

By J. A. Eisele

The Bureau of Mines conducted bench-scale cyclic tests to determine the composition of recycled leach liquor in the Bureau?s proposed clay/HCl leach/ HCl sparge process for producing Al203 from clay. The data developed from these tests make it possible to synthesize leach liquors for predetermined steady-state operating conditions when conducting large-scale crystallization tests. The results of two sparge tests were compared. One was a 20-cycle test with a 36-pct-HCl concentration in the mother liquor; the other was a 10-cycle test with a 26-pct-HCl concentration in the mother liquor. The effect of impurity concentrations in the leach liquor on the purity of aluminum chloride (AlCl30?6H20) crystals was determined, but there was poor correlation between this data and results that have been obtained from miniplant-scale work.

Jan 1, 1980

By D. Harry Chambers

The Bureau of Mines, through a memorandum of agreement with the Department of Defense, conducted research to recover silver from aircraft scrap. Silver was recovered by an electrolytic method from stainless steel honeycomb sections separated from the aircraft. These sections had been constructed by sandwiching a stainless steel honeycomb core between stainless steel sheets and then brazing the assembly with a silver alloy. Over 300 pounds of silver was used in the B-58 bomber, concentrated in certain honeycomb sections of the aircraft. Following shredding of the aircraft parts, an average of 95 percent (ranging 67 to 100 percent) of the silver was recovered in a single electro-refining step. After the electrorefined product was magnetically cleaned, purity of the recovered silver was greater than 99.3 percent.

Jan 1, 1980

By Robert F. Chaiken

A novel approach to eliminating environmental and public safety hazards that are associated with fires in abandoned coal mines and waste banks involves the use of in situ combustion technology developed by the Federal Bureau of Mines to accelerate the burning of the wasted coals in place. This technology would be used under exhaust ventilation control conditions that would allow for total management of the hot gases produced. Combustion stoichiometries would be optimized to minimize unburnt combustibles and to maximize the heat content of the gas products, which will be exhausted at one or more fan locations. When necessary, scrubber systems would be employed to remove air pollutants, such as sulfur dioxide; heat utilization systems (process heat, steam, and electricity) would also be employed to offset operational costs. Ultimately, complete burnout would solve the fire and acid water formation problems of the abandoned coal mine or waste bank. Pertinent technical data for burnout control are derived and discussed in terms of the important material and operational parameters. In general, it is believed feasible to operate a burnout system in an existing abandoned mine or waste bank fire at thermal power levels in the range of 10 to 100 Mw, and at exhaust gas temperatures of 1,000° C (1,830° F).

Jan 1, 1980

By Robert D. Schmidt

This Bureau of Mines report describes the development and application of a computer model for simulating the hydrological activity associated with in situ leaching. The model is intended to provide uranium resource developers with a description of the flow behavior of leachants and ground water during the development, production, and restoration phases of a leaching operation involving an arbitrary pattern of injection and recovery wells. Different aquifer environments are modeled, using a closed-form solution to the partial differential equation that describes three-dimensional changes in piezometric head as a result of pumping from leachant injection and recovery wells. The computer program can model a maximum of, 50 arbitarily located wells. Numerical techniques involving difference quotients and Taylor expansions about time points are used to derive time, velocity, areal sweep, and fluid volume parameters associated with leaching hydraulics. These parameters are output by the program in graphic and tabular formats. Other numeric methods insure that the program running time is minimized without significantly affect-ing the accuracy of results.

Jan 1, 1980

By R. F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Bureau of Mines has developed a general method for preparing solutions from a wide range of metal and mineral samples for chemical analysis. The development of the method from current knowledge of vessel material, pressure dissolution techniques, and the fluoride-boric acid reaction is given. The method uses 7 ml of a mixture of HC1-HNO3-HF acids in a ratio of 3.5:2:1.5 sealed in plastic bottles that act as pressure vessels when heated in a boiling water bath. A final volume of 100 ml is obtained by the addition of 93 ml of a 1. 5-pct H3BO3 solution to the bottles, which are reheated; precipitated fluorides as well as sample residue are dissolved by the fluoride-boric acid reaction. A copper slag and a steelmaking slag treated using this method were analyzed by atomic absorption spectroscopy yielding values for Si, Mg, Ca, AI, Fe, Mn, Na, As, Pb, Sb, and Zn very close to certified values with an average relative standard deviation of 2.13 pct. The low cost, reduction in preparation time, ease and safety of sample handling, conservation of reagents, and ability to dissolve volatile materials without loss make this method superior to traditional wet digestion techniques for many materials, and ideal for use with atomic absorption, and optical emission or X-ray emission spectroscopy.

Jan 1, 1980