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By J. Bennetts

As part of its mission to develop technology that will help increase the supply of critical and strategic minerals from domestic resources, the Bureau of Mines has investigated methods for beneficiating platinum-group metal ores from the Stillwater complex, Montana. This report presents the result of a bench-scale study employing froth flotation to recover a sulfide concentrate containing platinum-palladium values from a mineralized gabbro. Best results were obtained with a flotation scheme utilizing a mercaptobenzothiazone collector and sulfuric acid. Rougher concentrates containing approximately 11 oz Pt-Pd/ton and 90 pct of the metal values in the ore were obtained. Subsequently, cleaner concentrates containing approximately 26 oz Pt-Pd/ton and between 80 to 85 pct of the Pt-Pd values in the ore were prepared.

Jan 1, 1980

As part of the Bureau of Mines subactivity in secondary resource recovery and to expand the Nation's mineral base, the Tuscaloosa Research Center made characterization and preliminary beneficiation studies of the waste residues from various coal-conversion processes: from pilot plant tests of the Synthane process for coal gasification, the Synthoil process for coal liquefaction, and the solvent-refined coal (SRC) process for sulfur removal from coal. Those coal conversion processes selected for this study were based on the availability of pilot plant samples. Physical, chemical, and mineralogical examinations of the wastes made to determine the mineral content prior to physical beneficiation tests indicated that in addition to significant quantities of carbon, some trace elements offer potential for concentration.

Jan 1, 1980

The Bureau of Mines, U.S. Department of the Interior, devised a flotation technique for upgrading chromite in chromium ores and gravity concentrates. The technique consisted of cationic flotation of chromite from a slime-free pulp acidified to pH 2.5 or lower using H2S04 modifier. Flotation results showed that ore containing serpentine as the primary gangue mineral was more amenable to concentration by this technique than ore containing the readily floatable olivine as the primary gangue mineral. Rougher flotation of a chromite ore containing abundant serpertine increased the grade form 19 to 41 percent Cra03 at a chromite recovery of 89.6 percent. Rougher flotation of ore containing abundant olivine upgraded the chromite from 23.4 to 29.6 percent Cr203 at a recovery of 89.4 percent. The technique was also applied to chromite gravity concentrates to further upgrade chromite and to reject silicates. Flotation of a gravity concentrate containing 40.9 percent Cr203 and 4.4 percent SiO2 recovered 90 percent of the chromite in cleaner products containing 44.9 percent Cr203 and 0.63 percent Si02. The combined recovery by gravity and flotation was 87 percent. An economic evaluation of this technique will be undertaken to deter-mine its feasibility for commercial use.

Jan 1, 1980

By J. P. Hansen

In order to help assure an adequate domestic supply of minerals essential to the Nation's economy and and security by developing more efficient minerals extraction technologies, the Bureau of Mines Tuscaloosa Research Center examined the application of autogenous microgrinding to calcium carbonate minerals. Treatment of minus 8-mesh Alabama marble resulted in a product 80 pct minus 5 micrometers (µm) at a power consumption of 70 to 80 kwhr/ton, This study shows that coarse particles of calcium carbonate minerals are effective as the grinding media for the autogenous attrition grinding of these minerals. The minus 8- plus 30-mesh fraction is an effective grinding medium (sand) for particles smaller than 30 mesh. A 40-pct-solids slurry and a sand: marble ratio of 2.5 appeared to be near optimum. For residence times above 13 minutes, products were greater than 80 pet minus 5 µm and greater than 54 pct minus 2 µm. Power consumption was uniformly low, ranging from 50 to 100 kwhr/ton of product depending upon the feed rate. One marble sample from Georgia was shown to be the most persistent grinding medium, with losses of less than half those of the other materials tested.

Jan 1, 1980

By F. X. McCawley

The Bureau of Mines, in pursuing its goal of extending the life span of strategic materials, conducted field corrosion studies at the East Mesa Known Geothermal Resources Area (KGRA) in the Imperial Valley, Calif., to determine the optimum materials of construction for use in geothermal mineral energy resource recovery plants. These studies included characterization of geothermal environments and in situ corrosion testing. The corrosion resistance of 10 alloys exposed to 5 brine and steam process environments was evaluated using the low-salinity, high-temperature brine from geothermal well Mesa 6-1. Of these alloys, Hastelloy C-276, Hastelloy S, Incone1 625, titanium-2nickel, and 316 L stainless steel had excellent resistance to corrosion in all of the process environments; E-Brite 26-1 and 430 stainless steel had fair resistance. Although general corrosion rates for 4130 steel and 1020 carbon steel were substantially higher than those of the other iron-base alloys, these two alloys could prove useful in low-salinity process environments because of their low cost. Aluminum alloy 5005 was the least corrosion resistant alloy and pitted severely. Scales formed on all of the alloys in every process environment. Calcite, aragonite, and an amorphous silicate were the major components of the scales.

Jan 1, 1980

By H. D. Jacobs

The Federal Bureau of Mines, as part of a program to insure future raw material needs for the iron and steel industry, undertook research to beneficiate the oxidized taconites from the western Mesabi range in Minnesota. The data presented were obtained by applying the Bureau-developed selective-flocculation/cationic-flotation process to the second of three oxidized taconite samples. These three samples are representative of an estimated 10 billion tons of ore analyzing 30 to 40 pct iron. The experimental work was performed in a 900-lb/hr pilot plant. Treating the ore sample (36.1 pct Fe) with the Bureau's process produced commercially acceptable concentrates averaging 63.5 pct Fe and 4.3 pct SiO2, with an average iron recovery of 84.6 pct.

Jan 1, 1980

By Mark S. Stagg

Blast-induced ground vibrations from surface coal mine, quarry, and construction blasting were measured and analyzed for frequency content and duration characteristics. Eighteen commercially available ground vibration measurement systems were evaluated in the field and laboratory for linearity, accuracy, and crosstalk. Buried, surface, and sandbagged transducer placement methods were compared, along with peak and vector-sum measurements. The recommended minimum frequency ranges for ground vibration instrumentation are 2 to 150 Hz for coal mine and quarry blasting, and 5 to 200 Hz for construction and excavation blasting. When higher or lower frequency vibrations are possible, as in construction blasting or for a quarry shot close to a residence, care should be taken to insure proper choices of instrumentation and vibration criteria. Several instruments operating in these ranges are available, and all but one of the seismographs tested fell within ±3-dB accuracy limits (+41 pct, -29 pct). Waveform recordings of all three ground vibration components are recommended as the peak amplitude and frequency may vary among the three. Peak or vector-sum readings are adequate if only amplitude levels are desired. The soil density matched box should be anchored or buried, particularly for high-frequency, high-amplitude construction blasting.

Jan 1, 1980

The Bureau of Mines studied blast-produced ground vibration from surface mining to assess its damage and annoyance potential, and to determine safe levels and appropriate measurement techniques. Direct measurements were made of ground-vibration-produced structure responses and damage in 76 homes for 219 production blasts. These results were combined with damage data from nine other blasting studies, including the three analyzed previously for Bureau of Mines Bulletin 656. Save levels of ground vibration from blasting range from 0.5 to 2.0 in/sec peak particle velocity for residential-type structures. The damage threshold values are functions of the frequencies of the vibration transmitted into the residences and the types of construction. Particularly serious are the low-frequency vibrations that exist in soft foundation materials and/or result from long blast-to-residence distances. These vibrations produce not only structure resonances (4 to 12 Hz for whole structures and 10 to 25 Hz for mid walls) but also excessive levels of displacement and strain. Threshold damage was defined as the occurrence of cosmetic damage; that is, the most superficial interior cracking of the type that develops in all homes independent of blasting. Homes with plastered interior walls are more susceptible to blast-produced cracking then modern gypsum wallboard; the latter are adequately protected by a minimum particle velocity of approximately 0.75 in/ sec for frequencies below 40 Hz. Structure response amplification factors were measured; typical values were 1.5 for structures as a whole (racking) and 4 for midwalls, at their respective resonance frequencies. For blast vibrations above 40 Hz, all amplification factors for frame residential structures were less than unity. The human response and annoyance problem from ground vibration is aggravated by wall rattling, secondary noises, and the presence of airblast. Approximately 5 to 10 pct of the neighbors will judge peak particle velocity levels of 0.5 to 0.75 in/sec as "less than acceptable" (i.e., unacceptable) based on direct reactions to the vibration. Even lower levels cause psychological response problems, and thus social, economic, and public relations factors become critical for continued blasting.

Jan 1, 1980

By Virgil J. Stachura

The Bureau of Mines has investigated techniques and instrumentation that measure accurately the airblast overpressures from surface mine blasting. The results include equivalencies between broadband research instrumentation and commercially available impulse precision sound levels meters measuring: root-mean-square, peak, fast, slow, impulse, A and C weighting, C-weighted sound exposure level (CSEL), and "linear" (flat) response. These values were obtained from field measurements and broadband FM tape recordings of production blasts at area and contour coal mines, limestones quarries, and iron mines. Frequency response was determined for 14 commercial systems.

Jan 1, 1981

By R. B. Schluter

The Bureau of Mines investigated the flotation responses of two copper-nickel ore samples from the Duluth Complex with the objective of recovering bulk sulfide concentrates. One of the ores studied was taken from a test pit; the other was taken from a test shaft. The samples were quite similar except that the pit sample analyzed 0.35 pct Cu and 0.11 pct Ni and the shaft sample analyzed 0.69 pct Cu and 0.14 pct Ni. Flotation responses were studied in both laboratory and pilot plant tests. Pilot plant flotation responses were similar for both samples resulting in grades of 12.2 pct Cu and 2.5 pct Ni for the pit sample and 12.2 pct Cu and 2.1 pct Ni for the shaft sample. Weight recoveries were 2.5 pct for the pit sample and 5.2 pct for the shaft sample. Copper and nickel recoveries for the pit sample were 87 and 62 pct, respectively, and 92 and 73 pct for the shaft sample. Both concentrates contained small but significant values of cobalt and precious metals. Cobalt recoveries were low--less than 40 pct for both concentrates. Precious metals contents of the concentrates were 1.59 oz/ton for the pit sample and 0.99 oz/ton for the shaft sample. Silver was the predominant precious metal by weight, but platinum and palladium represented the highest values.

Jan 1, 1980

By K. R. Farley

A simplified method for the atomic absorption determination of antimony is described. Samples are dissolved in hydrobromic acid and diluted to volume with water. Solutions can be ready for analysis in about 10 minutes and are stable for at least 24 hours. The spectral line at 231 nanometers is used, and there is no effect on absorption resulting .from the presence of any concentration of HBr. Absorbance is linear with antimony concentrations up to 120 micrograms per milliliter. Sensitivity is 1.48 micrograms per milliliter per 0.0044 absorbance. Relative errors on National Bureau of Standards Standard Reference Materials were 3 percent or less, and relative standard deviations on 12 determinations of each of three flue dust samples were 4 percent or less (95-percent confidence limit).

Jan 1, 1980

By R. H. Nafziger

The Bureau of Mines evaluated 18 domestic titaniferous materials with widely varying compositions, mineralogy, and physical properties in electric-arc furnaces, Techniques were devised to recover both the titanium and iron values contained in these materials so that the reliance of the United States on foreign sources of higher grade ilmenites and rutile might be decreased. Most of the tested titaniferous materials responded well to lower grade or byproduct reductants, such as bituminous coals, charcoal, and coke breeze. Sufficient slag fluidity was realized by maintaining from 8 to 12 wt-pct iron in the slags; no contaminating fluidizers were required. Fluid slags containing up to 79, 70, and 54 wt-pct Ti02 were realized from east coast ilmenites, a rock ilmenite, and a titaniferous magnetite ore, respectively. A carbon-lined furnace shell is recommended for minimum slag contamination. Good results also were obtained during extended submerged-arc furnace tests.

Jan 1, 1980

By Steven J. Page

Responding to the increasing concern for dust control in metal and nonmetal mining, the Bureau of Mines investigated typical dust reduction efficiencies of wet bar cutter machines as they are presently being used in salt mines. Wet bar techniques have previously been used in coal mines, achieving dust reduction efficiencies ranging from 11 to 60 pct. Two different wet bar techniques, namely, the front spray and the water trickle, have been studied as they are currently being used in two salt mines. Preliminary results show that the dust reduction efficiencies have a large variation (0 to 66 pct), as is the case for wet bars used in coal. However, whereas wet bars in coal required 3 to 4 gpm water consumption, wet bars in salt obtained similar efficiencies with only 0.1 to 0.4 gpm. The most reliable data obtained during this study show that the front spray system consistently performs at efficiencies between 41 and 66 pct, with an average of 54 pct. The results indicate that, although wet bar cutter techniques in salt mines are a relatively simple and inexpensive means of dust control with a minimum of water consumption, further investigation should be performed to fully evaluate and optimize wet bar cutter dust reduction efficiencies.

Jan 1, 1980

By Nicholas Kyriazi

It is of interest to know how to obtain as high an absorption efficiency as possible from a CO2-absorption canister used in closed-circuit breathing apparatus. In this study the Bureau of Mines found that varying the bed depth and the cross-sectional area of a canister changes its absorption characteristics. In tests using four ,1 rectangular, variable-depth canisters with different cross-sectional areas, the Bureau found that, given a constant weight of the chemical absorbent, LiOH, and a constant COa input, the canisters with a greater cross-sectional area reached C02 levels of 0.5 volume-percent in the effluent gas sooner than did the canisters with a greater bed depth. However, resistance to flow through the canister increases with bed depth, and a trade-off is inevitable. It was anticipated that the efficiency of a canister would increase with increasing intergranular air space approaching the tidal volume of the breathing waveform and then level off at some point under 100 percent. This postulation was partially substantiated. Cylindrical and radial canisters were also tested and compared. It appears that shape is not as important a factor in absorption efficiency as bed depth, since neither canister differed significantly from the rectangular canisters with regard to absorption efficiency values.

Jan 1, 1980

By J. E. Pahlman

As part of its effort to reduce the need for strategic minerals through conservation and to reduce the capital and energy requirements of mineral processing, the Bureau of Mines has investigated a method for preparing ferrochromium alloys containing less than 2 percent carbon. This method will conserve chromium and should reduce the capital and energy requirements for chromite reduction. Reduced products containing less than 2 wt-pct C and as low as 0.01 wt-pct C were obtained by reacting pellets of chromite and carbonaceous reductant mixtures at pressures of 0.1 to 1 torr and temperatures of 1,230° to 1,320° C. The extent of reduction increased with increased temperature and decreased pressure; however, operating conditions were limited due to the onset of significant chromium vaporization at higher temperatures and lower pressures. Foundry coke, anthracite, and carbon black were found to be supe¬rior to graphite as reductants. The reduction of chromite to metallics was found to proceed via the carbide intermediates (Fe,Cr)7C3 and (Fe,Cr)23C6, No evidence of carbide intermediates Fe3C or Cr3C2 was found. Buttons of ferrochrome alloys were made by melting a mixture of reduced products with CaO and Si02 at 1,700° C for 20 minutes in an induction furnace,

Jan 1, 1980

By W. P. Diamond, J. R. Levine

The explosion hazard of methane-air mixtures has become an increasingly serious mine planning problem, and an advance assessment of methane gas potential can therefore be essential for a safe and economic mine development pro- gram. As part of its coal mine health and safety program, the Bureau of Mines has developed a simple, inexpensive test to measure the methane content of coal samples obtained from exploration cores. The gas content of coal per unit weight as determined by the direct method test can be used as a basis for a preliminary estimate of mine ventilation requirements, and to determine if degasification of the coalbed in advance of mining should be considered. Since the Bureau began measuring the gas content of coal samples in 1972, experience has led to equipment and procedural changes, the most significant of which has been the development of a ball mill for crushing the coal sample to release the residual gas at the end of the desorption test period. This revised procedure replaces the crushing box and graphical methods described in earlier Bureau publications. The results of 583 direct method tests are summarized in tabular form. These results include data on the gas content of 125 coalbeds in 15 States.

Jan 1, 1980

By W. P. Diamond

The explosion hazard of methane-air mixtures has become an increasingly serious mine planning problem, and an advance assessment of methane gas potential can therefore be essential for a safe and economic mine development program. As part of its coal mine health and safety program, the Bureau of Mines has developed a simple, inexpensive test to measure the methane content of coal samples obtained from exploration cores. The gas content of coal per unit weight as determined by the direct method test can be used as a basis for a preliminary estimate of mine ventilation requirements, and to determine if degasification of the coalbed in advance of mining should be considered. Since the Bureau began measuring the gas content of coal samples in 1972, experience has led to equipment and procedural changes, the most significant of which has been the development of a ball mill for crushing the coal sample to release the residual gas at the end of the desorption test period. This revised procedure replaces the crushing box and graphical methods described in earlier Bureau publications. The results of 583 direct method tests are summarized in tabular form. These results include data on the gas content of 125 coalbeds in 15 States.

Jan 1, 1980

By Philip Thompson

The Bureau of Mines investigated a selective flocculation-flotation technique to remove insoluble slimes from low-grade potash ore in a continous 45-kilogram-per-hour (100-pound-per-hour) process investigation unit (PIU). This research is part of the Bureau's program to improve resource recovery from low-grade ores. Results showed that 84 percent of the insoluble slimes were removed from an ore containing 5.5 percent water-insolubles and 14 percent K20 using a Bureau-developed, cationic flocculant-glycol ester-diesel oil reagent. Subsequent potash flotation recovered 75 percent of the potash in a cleaner concentrate assaying 56 percent K20. Concentrate leaching upgraded the product to market specifications of 60 percent K2O. An economic evaluation by the Bureau suggested that the rate of return on investment, after taxes, should be about 20 percent for such an enterprise.

Jan 1, 1980

By Theodore Christos

The Bureau of Mines sponsored an investigation of the thermal oxidative degradation characteristics of certain solvents and hydraulic fluids used in underground mining operations. The following halogenated solvents were studied in view of their usefulness and their flame retardant property: tetrachloroethylene, C12C = CC12; 1, 1, 2-trichloroethane, CIH2CCHC12: and trichloroethylene, C12C = CHC1. The hydraulic fluids studied were representative of five groups approved by the Mine Safety and Health Administration for underground operation, namely: glycol-water solutions, mineral oil-water emulsions, synthetics other than phosphate esters, synthetic phosphate esters, and mixtures of phosphate esters with mineral oils and other ingredients. It was observed that the partially halogenated solvents present a greater potential toxic hazard than the fully halogenated materials, due not only to the easy production of hydrogen chloride but also to their ease of oxidation leading to the formation of phosgene and carbon monoxide. The pure phosphate esters exhibited the best thermal oxidative stability of the five groups of hydraulic fluids tested. A fluid containing phosphate esters mixed with mineral oils and other unidentified ingredients appeared to be the most hazardous On the basis that it produced very toxic acrolein and phosphine.

Jan 1, 1980

By S. E. Khalafalla

In support of its goal to maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines has investigated a novel hydrometallurgical system with sulfur dioxide. Differential leaching with dissolved SO2 of manganese, nickel, and cobalt from their hydrous oxides was found to be very rapid and efficient--almost instantaneous and quantitative. In this method a given weight of mixed oxides previously ground to minus 200-mesh is slurried with a leach solution containing a specified quantity of dissolved SO2 for 10 minutes at room temperature and ambient pressure. An empirical leaching parameter, R, is defined as the ratio of the number of SO2 moles in the leaching solution to the weight of the metal oxide charge. Plots of the variation of metal extraction with the ratio R generate a series of sigmoidal-shaped curves, each of which is characteristic of a specific metal extraction. A threshold value of R is required to initiate the leaching of a given metal from the mixed oxides. Once this threshold is reached, the metal recovery can increase to more than 95 pct in very short times. For increasing values of R, the extractability of various metals by SO2 follows the order: Mn > Ni > Co >> Fe, Al, Cu. Differences in the threshold R values permit a variety of metal separations to be made simply by adjusting the quantity of SO2 in the contacting solution. Success in this leaching system depends upon comminuting the sea nodules to less than 0.149 mm (100-mesh). Above this critical size, leaching is slowed due to the inaccessibility of inner particle reacting groups to the SO2 leaching agent. This results in nonselective extraction and less extraction of preferred metal values. At or below 0.149 mm, leaching by SO, is possible with all its attributes of selectivity, sensitivity, and rapidity. Leaching with HC1 solutions of the same pH level as dissolved SO2 yielded mixed, slow, and incomplete metal extractions. This observation rules out any interpretation based on hydrogen ion as the leaching agent. The leaching curves resemble the complexometric titration curves of heavy metals with specific coordination species.

Jan 1, 1981