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By David E. Siskind

The Bureau of Mines studied airblast from surface mining to assess its damage and annoyance potential, and to determine safe levels and appropriate measurement techniques. Research results obtained from direct measurements of airblast-produced structure responses, damage, and analysis of instrument characteristics were combined with studies of sonic booms and human response to transient overpressures. Safe levels of airblast were found to be 134 dBL (0.1 Hz), 133 dBL (2 Hz), 129 dBL (6 Hz), and 105 dB C-slow. These four air-blast levels and measurement methods are equivalent in terms of structure response, and anyone could be used as a safe-level criterion. Of the four methods, only the 0.1-Hz high-pass linear method accurately measures the total airblast energy present; however, the other three were found to adequately quantify the structure response and also represent techniques that are readily available to industry. Where a single airblast measuring system must he used, the 2-Hz linear peak response is the best overall compromise. The human response and annoyance problem from airblast is probably caused primarily by wall rattling and the resulting secondary noises. Although these will not entirely be precluded by the recommended levels, they are low enough to preclude damage to residential structures and any possible human injury over the long term.

Jan 1, 1980

By G. R. Palmer

Using a fluidized, countercurrent multiple-compartment ion-exchange (MCIX) column previously developed by the Bureau of Mines, Bureau researchers have successfully extracted uranium from a simulated acidic in situ leach liquor that contained 150 ppm U30s? This successful demonstration of the MCIX system is reported, and the effects of varying the operating conditions on the performance of the system are also examined. Operating the MCIX system with a flow rate of 15 gpm/ft2 and an aqueous-to-resin flow ratio of 200:1, more than 90 percent of the uranium Has extracted, and a resin containing approximately 28 grams U308 per liter was produced. The absorption column used to investigate the operating variables was approximately 18 feet long with a 2-inch ID and was divided into compartments that were 1 foot long.

Jan 1, 1980

By R. E. Simpson

Beginning in 1972, fully grouted resin bolts were used in underground mines. An estimated 20 million resin bolts will be installed in 1980 owing to their apparent support improvement in most roof-bolt applications. Inorganic cements were tested to replace the resin at a lower cost while retaining the advantages of a grouted bolt. Although other inorganic materials were considered, all but portland and gypsum cements were rejected for reasons of availability, performance, or cost. Portland and gypsum-type cements were tested by the Bureau of Mines to select a fast-hardening, low-cost material that would anchor a roof bolt adequately to meet safety standards. An alpha-gypsum cement, accelerated with potassium sulfate, was selected as the best material because it had adequate pull strength at a desired set time of less than 5 minutes and was readily available.

Jan 1, 1980

By G. W. Elger

The Bureau of Mines conducted laboratory and larger scale studies on samples of domestic perovskite and ilmenite ore concentrates to devise a procedure for recovering TiC from these ores. From the concentrates, mixtures of titanium and calcium carbides were produced. The carbides were then ground and reacted with water. This reaction decomposed the CaC2 to acetylene and hydrated lime and simultaneously liberated the TiC. Using a combination of elutriation and gravity-separation techniques to separate the hydrated lime, approximately 93 pct of the titanium was subsequently recovered as purified carbide containing 54 to 70 pct titanium with CaO content as low as 0,6 pct. This combination of techniques can be used to separate more than 90 pct of the CaO from the TiC. Therefore, this carbiding procedure is a viable method for treating titaniferous materials, including perovskite, that contain more than 20 pct CaO. Tests made in a static-bed reactor showed that for the reaction of TiC with elemental chlorine to produce titanium tetrachloride (TiCI4), a temperature of at least 940° F is desirable to achieve a suitable extraction of titanium in a laboratory chlorination reactor. In fluidized-bed tests at 840° F, 98 pct of the titanium contained in TiC was extracted.

Jan 1, 1980

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 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 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 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 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 E. R. Cole

This Bureau of Mines investigation was prompted by the need forr a stable anode for electrowinning metals, particularly zinc and copper, from acid solutions. The polarization behavior of Pb-Ag (1 pct Ag) anodes in H2SO4 and fluoride solutions was determined as the first step in the development of such an anode. A Luggin capillary, dc power supply, high-impedance voltmeter, and other equipment standard to an electrochemical laboratory were used in this study. It was determined that during polarization, a relatively hard, stable coating of Pb02 was formed on the surface of the lead-silver anode and the rate of formation of this coating was considerably enhanced by the presence of fluoride ions in solution. Subsequent investigations at the Bureau of Mines Rolla Research Center resulted in the development of a Pb02-coated titanium (Pb02-Ti) anode. Results of this effort were presented in Bureau of Mines Report of Investigations 8111. Additional data resulting from extensive testing of the Pb02-Ti anodes, as well as process improvements and innovations, are included in this report. The anodes were considered generally unsatisfactory for zinc electrowinning because of lower conductivity, higher oxygen overvoltages, and shorter in-cell life as compared with the Pb-Ag anodes now being used in industry. However, the PbO2-Ti anodes were used successfully to oxidize waste chromium solutions and to electrowin copper.

Jan 1, 1981

By Philip C. Good

The Bureau of Mines investigated the feasibility of utilizing low-grade phosphatic shale as a feed for phosphoric acid production. Present practice in the phosphate mining operations of southeastern Idaho is to remove and either stockpile or waste low-grade phosphatic shales as the high-grade phosphate beds are selectively mined. Acid digestion studies were performed on uncalcined shale and on shale calcined to remove free carbon to determine phosphoric acid quality, yield, and amenability to filtration. The untreated shale, containing 21.4 pct P205, was digested with sulfuric acid in a single-tank reactor to yield phosporic acid and gypsum residue. Although 96 pct P205 recovery was attained in digesting uncalcined shale, only the calcined product gave satisfactory filtration rates. Calcined shale yielded phosphoric acid recovery of about 93 pct of the contained P205. It was higher in impurities than commercially prepared acid derived from high-grade western phosphate rock. An acid filtration rate of 745 lb P205/ft2/day was attained. This value is lower than the rate of 900 lb P205/ft that is generally considered to be acceptable in industrial production of phosphoric acid from high-grade phosphate rock.

Jan 1, 1981

By I. Liebman

The Bureau of Mines conducted experiments on coal dust explosion suppression. The investigation took place on a beltway in the double-entry of the Bureau's Experimental Mine. Using conditions that simulate those in a working mine, the investigation showed that a coal dust explosion can be readily initiated in a conveyor belt entry. Also, the explosion can spread into adjacent entries through opened crosscuts (stopping destroyed by explosion) to propagate for long distances even though the adjacent entries are rock dusted in compliance with regulations. Passive water barriers (water-filled tubs) were found to be effective in suppressing explosions on a beltway; however, barrier efficiency was reduced by opened crosscuts. The study indicated that the beltway barrier should be the distributed type consisting of continuous rows of water-filled tubs covering long distances along the entry. A plan is outlined for the installation of a water barrier system in a working coal mine for the protection of a beltway.

Jan 1, 1981

By W. N. Marchant

The Bureau of Mines performed chemical research to elaborate details of sulfur chemistry pertaining to the citrate flue gas desulfurization process in which sulfur dioxide (SO2), absorbed (as bisulfite ion) in a buffered sodium citrate solution, is reduced by hydrogen sulfide (H2S) according to the overall reaction 2H2S + HSO3 + H+ ? 3S + 3H20. The rate-limiting step in the process was shown to be the reduction by H2S of thiosulfate (S2031-) that is formed as an intermediate. Pseudo first-order kinetic measurements were made at room temperature to retard the reaction sufficiently that adequate analysis was possible. These measurements showed the rates of the following net processes to be -d [S02]/dt (pH 4.5) = (0.409±0.050)min-1 [S02]; d [S2032-]/dt (pH 4.5) = (0.199±0.017)min-1 [S02]; -d [S2032-]/dt (pH 4.0) = (0.0437±0.0265)min-1 [S2032-]~1; -dH2S/dt (pH 3.9) = (21.6±3.0) mmoles/min-atm [H2S]g1.4, where [H2S]g is the partial pressure of H2S in the gas phase, in atmospheres, and the rate describes the consumption of H2S, in millimoles per minute; d[S]/dt (pH 4.0) = (38.0±3.4)min-1 [H2S]1, where [H2S] is the concentration of H2S in solution. Hydrogen ion consumption during the slow phase of regeneration was shown to occur at (2.1±0.5) times he rate of thiosulfate consumption, which is interpreted as evidence for the following as the rate-limiting reaction: 2H2S + S2032- + 2H+ ? 4S + 3H20 A scheme consisting of five sequential general reactions is proposed to account for sulfur formation.

Jan 1, 1981

By E. D. Calvert

The Bureau of Mines, in its effort to promote greater utilization of domestically abundant materials, conducted reasearch on an alternate mold material that has commercial potential for titanium investment casting. Using variations of the conventional lost wax molding process, investment shell molds were formed entirely of fused, calcia-stabilized Zr02 and a Zr02-forming binder. Optimization of binder/slurry properties', stucco grain size and dis¬tribution, and curing practices resulted in a structurally sound investment shell that was distortion free and thermally stable. Small titanium castings, weighing up to 10 pounds, were prepared in unheated molds by both static and centrifugal casting techniques. Microstruc¬tural examination of the castings revealed that mold fill and surface quality were enhanced by centrifugal casting, although good results also were obtained from the statically poured molds. Microstructural and electron microprobe examinations showed that excessive, brittle case formation could be avoided by curing the dried shell molds in air for at least 2 hours at 1,400° C. Increasing curing temperature and time above these levels yielded added bene¬fits. Molds fired in vacuum at 1,500° C for 4 hours yielded castings essen¬tially free of case formation. The tensile properties of as-cast test specimens (no surface conditioning performed) id the chemical composition of representative metal samples showed that castings produced were comparable to Grades C-1 and C-2 unalloyed titanium This indicated that no sifnificant degradation of metal properties resulted from mold/metal interaction.

Jan 1, 1981

By Kenneth L. Cashdollar

This report describes three types of optical dust probes that have been designed, built, and tested by the Bureau of Mines. Each of the probes measures dust cloud concentrations by the attentuation of light. The first is a single-path-length probe, the second is a double-path-length probe, and the third is a single-path-length probe that employs jets of air to keep the windows of the light source and detector free from dust coating. The theory of operation and the calibration procedures for each of the probes are described. The results of the Bureaus laboratory, mine, and field tests of the probes are also reported.

Jan 1, 1981

By R. A. Bloomfield

This report summarizes Bureau of Mines contract research on the disposal of retorted oil shale. A data base has been developed describing the physical-chemical properties, geotechnical engineering properties, and natural cementation characteristics of spent shale. Results of field compaction tests and seepage pond tests are presented, along with results of a partially saturated finite element seepage model used to predict infiltration and seepage rates. Preliminary engineering analyses are presented for underground disposal systems, which include material transport methods, and for a surface disposal system, which includes stability analyses.

Jan 1, 1981