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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 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 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 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

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 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 V. R. Spironello

The Bureau of Mines is conducting studies of the slags related to ferrous technology to evaluate acceptable substitutes for the auxiliary flux, mineral fluorspar, in foundry operations. This work is directed toward the Bureau's goal of minimizing the Nation's dependence on scarce and critical minerals Comparative basic practice cupola (18-inch-ID) trials were made to evaluate a waste material called "used potlining," which contains significant levels of fluorine, sodium, and aluminum in various compounds. Used potlining is recovered from alumina reduction cells after its useful life, and was supplied by the Aluminum Co. of America (Alcoa) to the Bureau for evaluation. The material in the lump and pelletized form (with limestone) provided extremely fluid slags based on visual observation during cupola operation. No adverse effects were found on cupola performance, metal and slag chemistry, the environment, or mechanical properties of the castings produced. Fluorine recovery in the slag was equal to, or higher than, that of fluorspar; fluorine losses to the scrubber water and solids were lower. The acidity of the scrubber Hater was somewhat neutralized. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag and visual inspection. The recovery of sodium in the slag, presumably as the oxide, significantly increased slag fluidity, suggesting that less than equivalent fluorine may be required. There was no contamination of the gray iron by the aluminum from the used potlining. Used potlining was completely satisfactory as a substitute for fluorspar in cupola ironmelting.

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 S. E. Khalafalla

The Bureau of Mines has used colloidal solutions of magnetite in a magnetic field to segregate nonmagnetic materials such as nonferrous scrap metals and to concentrate precious minerals. Conventional magnetic separation relies on the inherent magnetic susceptibility of the material to be separated and may be designated as magnetic separation of the first kind the medium of separation rather than the separated particles are made magnetizable, a new system of gravity separation results. In this new magnetic separation of the second kind, a magnetic fluid rather than air or water acts as the separation medium. The same force that attracts magnetic objects in separations of the first kind also attracts the entire separation medium in separations of the second kind, thereby creating a reactionary force of equal magnitude in the opposite direction. This force, sometimes called the levitation force, can be made to segregate nonmagnetic particles in a flowing stream according to their specific gravity. The technique has been applied to segregate nonferrous metals from automobile and appliance shredders and mixed scraps. The system has also been used to upgrade diamondiferous jig concentrates from certain river gravels in order to facilitate the sorting and recovery of their diamond content.

Jan 1, 1981

By N. I. Jayaraman

High-pressure shrouded sprays were first tested on a bench to determine air-moving capability and dust collection efficiency. The bench-scale tests indicated that at 500 psi and above, the dust collection efficiency, when sampled downstream of a water eliminator, was about 99 pet for two types of nozzles. However, for the same water flow, the induced airflow was about three times greater in one type than in another. Since the only difference in the nozzles was the spray angle, this factor was important in air movement through a shrouded spray. Full-scale model mine tests were then conducted to determine the reduction in dust concentration behind the line curtain and at the operator position produced by high-pressure sprays in a shroud. The shroud was mounted on top of the boom of a model continuous miner, and high-pressure (greater than 500 psi) sprays were installed inside the shroud. The inlet of dusty air to the shroud was open toward the face and the outlet toward the exhaust line curtain. The high-pressure sprays were compared with conventional sprays mounted at the head of the continuous miner and directing water toward the face. The difference at the operator position (opposite side of brattice) was significant in that, under certain conditions, with conventional sprays an increase in respirable dust concentration of 471 pet was noticed compared with dry operation due to rollback from face. High-pressure shrouded sprays, on the other hand, decreased the dust concentrations at the operator position (opposite side of brattice) by 28.2 pct.

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 Arne Landsberg

The Bureau of Mines has undertaken research to elucidate the chemistry involved in the efficient recovery and control of minor elements in base metal smelting operations. These elements should be effectively recovered not only because they have commercial value, but also because of their potential hazard to workers' health and the environment, if they are not controlled during processing. Cadmium, a minor metal in zinc ores, is the subject of this report. The roasting step of the complex zinc-smelting process was chosen for investigation because of the high potential for removing cadmium by volatilization during this primary stage. Commercial roaster feed materials were used to determine the sequence of reactions and the effect of these reactions on the volatilization of cadmium. Electron microprobe examination of both the commercial roaster product and oxidized sulfide solid solutions prepared in the laboratory showed that oxidized iron was of prime importance in preventing cadmium volatilization. The mechanism by which iron prevents cadmium volatilization is proposed, and a preheating technique is recommended for more effectively recovering cadmium prior to roasting.

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