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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 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 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

A preliminary study was conducted by the Bureau of Mines to determine the effect of humidity on salt mine airborne dust levels. Results showed less dust where the humidity was elevated. Dust reductions appeared to be dependent on the equilibrium between humidity and salt.

Jan 1, 1980

The Bureau of Mines conducted large-scale laboratory copper ore leaching tests to enable improving copper recovery from large dump-leaching operations. This was done by comparing leaching progress when copper was recovered from recycled leach liquor either by cementation or by solvent extraction. Copper was leached from 7-ton ore samples at room temperature using pH 2 ferric sulfate solutions. With are samples containing 11 percent minus 0.5-inch fines, no marked advantage in using either of the copper recovery methods was evident after 416 days of leaching. With ore containing 32 percent minus 0.5-inch fines, solvent extraction of copper was advantageous in that 60 percent of the copper was extracted after 568 days, whereas only 48 percent of the copper was extracted when cementation was used. Less acid was consumed during leaching when solvent extraction, rather than cementation, was used for copper recovery. Iron, contributed by cementation with scrap iron, plugged the ore bed containing 32 percent fines.

Jan 1, 1981

By M. J. Sapko

A moderately scaled apparatus was developed by the Bureau of Mines to determine the fire resistance characteristics of mine conveyor belts and similar type materials. The design of the apparatus was based upon data obtained in full-scale fire tests and features a radiant panel to preheat the belt and a methane-oxygen ribbon burner to ignite the sample under ventilating condi¬tions in a rectangular duct. The test method overcomes the limitations of existing laboratory-scale methods and provides a measure of both ignitability and flammability in quantitative terms. Flame propagation depended upon such variables as air velocity, ignitor heat flux, and belt width and height in the test chamber. Data are presented for nine belt materials and fire resistance ratings are proposed in terms of the flame spread rate, heat release rate, and the critical ignitor heat flux. The ratings discriminate between the fire hazard posed by different fire-resistant belts and tend to be in reasonable agreement with those obtained in full-scale fire tests.

Jan 1, 1981

By L. A. Haas

The Bureau of Mines conducted bench-scale leaching tests with recycled spent copper electrolytes and copper-nickel mattes produced from the Minnesota Duluth Complex concentrates. This report describes the first stage of an overall two-stage leach operation. The objective of this research was to determine the matte-leach technology required to convert spent copper electrolyte into an enriched nickel liquor suitable for a nickel refinery and there-fore essentially free of copper, iron, and sulfuric acid. The experimental variables investigated were matte composition, particle size, spent electrolyte content, pulp concentration, oxygenation, temperature, and time. The time required to produce an enriched purified nickel liquor decreased with increasing pulp concentration, temperature, and oxygenation, but increased with increasing particle size and electrolyte copper and acid content. Nickel-rich (about 50 g/l) liquors at a pH of about 4 and containing less than 1 g/l of copper and iron were produced at 70° C by leaching minus 325-mesh low-iron (less than 5 pct) matte for 8 hours with spent electrolyte containing 22.4 g/l Cu, 28.9 g/l Ni, less than 0.1 g/l Fe, and 50 g/l H2S04 at a pulp concentration of 1 kg of matte per liter of spent electrolyteo Varying the nickel content of the spent electrolyte from 11 to 101 g/l appeared to have no appreciable influence on the matte leaching characteristics.

Jan 1, 1981

By C. F. Davidson

The Bureau of Mines studied the extraction of lithium from lithium-containing clays by chlorination with hydrogen chloride (HC1). In bench-scale laboratory investigations, HC1-H20 mixtures were used to selectively chlorinate lithium, but not calcium or magnesium, in lithium-containing clays. The addition of calcium carbonate to the clay was found to improve the lithium recovery. Reaction conditions found to affect the lithium recovery were ratio of clay to carbonate, reaction temperature, and HC1 concentration. The best conditions for selective chlorination of the lithium were 2:1 clay-carbonate, 750° C, and 20 wt-pct HC1. The experimental results and trends in lithium extraction are explained using thermodynamic relationships.

Jan 1, 1981

By S. D. Hill

To help insure the continued viability of the minerals and materials sector of the U.S. economy, the Bureau of Mines is conducting research and disseminating technology that will result in more efficient minerals extraction. As part of this effort, a process is being investigated that involves an aqueous chlorine-oxygen leaching procedure to treat complex sulfide concentrates to produce ZnCl2. Subsequent fused-salt electrolysis of the ZnCI2 produces high-purity zinc metal. Previous reports described preliminary, small-scale research on the chlorine-oxygen leaching system and fused-salt electrolysis of ZnCl2. This report discusses the details of design, construction, and longterm, continuous operation of both monopolar and bipolar fused-salt cells. The effects of temperature, electrode gap, current density, electrolyte composition, and electrode configuration on current efficiency and energy consumption were determined for a ZnCl2-KC1-NaCl electrolyte system. Zinc metal was produced at the rate of about 50 lb/day in a monopolar cell which was operated continuously for 60 days with current efficiencies from 85.8 to 98.6 pct and an average power consumption of 2.1 kwhr/lb. Bipolar cells with several different electrode configurations were operated for 90 days. A current efficiency of about 70 pct and power consumption of about 1.7 kwhr/lb of zinc were achieved using a three-electrode-pair, bipolar assembly with a chlorine gas lift pump to circulate electrolyte.

Jan 1, 1981

By M. J. Ferrante

High-temperature enthalpy and X-ray powder diffraction studies were con-ducted on aluminum sulfide (Al2S3) as part of the Bureau of Mines effort to provide new data for the advancement of mineral technology consistent with environmental preservation and energy conservation. Relative enthalpies were measured with a copper-block calorimeter from 298.15 to 879 K. Tabulated values are listed for heat capacity, entropy, Gibbs energy functions, and relative enthalpies between 298.15 and 900 K. Enthalpies were also given in the form of an equation and combined with published data to calculate standard enthalpies of formation and Gibbs energies of formation for reactions of crystalline aluminum with crystalline, liquid, and gaseous diatomic sulfur. The hexagonal, rhombohedral, and cubic phases of Al2S3 were identified by X-ray powder diffraction studies, and the indexed powder diffraction patterns of these phases are given. The hexagonal phase was stable to about 852 K and was partially converted to the rhombohedral form at 879 K.

Jan 1, 1981