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By B. D. Nash

The Bureau of Mines continued its research into the recovery of fluorine by the phosphoric acid acidulation defluorination of phosphate rock concentrates. A small process development unit with a capacity of about 10 kilo-grams of charge per hour was operated, and concentrates from both Idaho and Florida were processed. Over 80 percent of the fluorine was evolved and recovered as a dilute fluosilicic acid solution. Phosphate extraction from the concentrates always exceeded 98 percent. The fluorine was converted to a synthetic fluorspar product (3CaFa?SiOa) suitable for use as a slag conditioner in electric furnace steelmaking operations.

Jan 1, 1977

By Martin Hertzberg

The early and reliable detection of the self-heating of combustible substances in mines is of considerable importance to the mining community. This Bureau of Mines report describes the results of a variety of studies of incipient combustion and its detection. Heated samples of coal, wood, and various polymers were used to evaluate the relative sensitivities of several types of detectors. The laboratory results indicate that submicrometer particulate detection is the most universal and sensitive method. Carbon monoxide detection was as sensitive as submicrometer particulate detection for pyrolyzing coal but was relatively insensitive to pyrolyzing wood or plastics. The conventional type of ionization smoke detector was the least sensitive for coal and of intermediate sensitivity for wood and plastics. Self-heating experiments with Pittsburgh seam coal piles of varying particle sizes gave ignition temperatures of 170° C for 4-to 7-µm dust, which increased monotonically with particle size. The measured heating rates were compared with data from an adiabatic calorimeter to obtain preexponential rate constants. The preexponential rate constants varied linearly with the surface area per unit mass of sample as would be expected for heterogeneous surface oxidation. The propagation behavior of ignition waves and the overall self-heating appears to depend critically on the magnitude of the convective flows induced, which counteract the depletion of oxygen in the void spaces of the pile. Classical theories of thermal ignition require substantial modification to be applied reliably to such cases.

Jan 1, 1977

By Arne Landsberg

The Bureau of Mines measured the vapor pressure of FeC12 , FeBr2, FeI2, Sb, Bi, Cd, Mg, Pb, FeC13 , and VCl2 using the Knudsen-and torsion-effusion methods, and on FeC13 -NaC1 mixtures, Au2Cl6, and MgNi2 using only the Knudsen method. Apparent vapor pressures calculated from the experimental data vary with orifice size and method of determination. Reaction with residual oxygen in the instruments was noted to have an effect on the iron halide data. Vapor pressure curves plotted as log P versus 1/T (where P is pressure and T is absolute temperature) for one substance using several orifice sizes tended to converge at a single point when extrapolated beyond the experimental region. All of the data, except those of VC12, agree with previously published results. The importance of comparing effusion measurements with those obtained by other methods and the variations encountered with various orifice sizes are discussed.

Jan 1, 1977

By R. K. Koch

The Bureau of Mines developed a zircon sand molding process for static casting of small titanium or zirconium shapes. Castings with unfinished weights up to 3.5 kg (7.7 lb) were produced in an inductoslag furnace and castings up to 7 kg (15.4 lb) were poured in a consumable electrode skull-casting furnace. Molds and cores were made by ram-molding, foundry-grade zircon sand (AFS gfn 93 to 95) bonded by grade D waterglass and tempered with water. Molds and cores were cured either at 250° C (482° F) or 900° C (1,652° F). Castings from the higher temperature molds broke cleanly from the sand while the lower temperature molds produced castings that had to be cleaned by sand-blasting. However, low-temperature cured molds and cores have a number of advantages as follows: (1) A faster, less energy-consuming curing cycle is used; (2) expended cores are water soluble which greatly facilitates core removal; and (3) enough of the binder in crushed expended molds is reactivated by temper water so that the molding mix can be reused five times without any fresh binder additions and up to twenty times without exceeding a total cumulative binder addition of 52 ml/kg dry sand. Crushed used molds that had been cured at 900° C had no detectable binding strength when mixed only with temper water. A large number of oxide and silicate mold washes were studied for improved casting integrity. The most effective wash found for zirconium or titanium casting was monoclinic zirconia (325 mesh).

Jan 1, 1977

By L. W. Higley

Particulates generated in electric furnace (EF) steelmaking constitute approximately 1 to 2 pct of the charge. This flue dust is a rich source of zinc (values are substantially higher than in ore), but although there are several processes for recovering the metal, none are considered economic in the United States. This report reviews extraction technology and presents results of Bureau of Mines reduction-volatilization tests on pelletized EF dusts which achieved high recoveries of zinc. The data are sufficiently encouraging to warrant consideration of EF dusts as raw material for primary zinc smelters.

Jan 1, 1977

By Stephen A. Hare, O&apos

The melting, casting, and welding of the Raney nickel alloy (42 pct Ni-58 pct A1), a methanation catalyst useful in coal gasification, were investigated. Melting was done in graphite crucibles by heating aluminum and adding nickel using a cryolite slag cover. Casting conditions were found to be optimum when the melt temperature ranged from 1,125° to 1,200° C and the mold temperature ranged from ambient to 250° C. Suitable mold materials were found to be quartz, heat-resistant glassware, olivine, and zircon. Welding of the alloy can be accomplished using tungsten inert gas process. Tensile strength of the alloy, in the as-cast condition, was found to be 2,000 1b/sq in with an impact strength of less than 1 ft-1b. The coefficient of thermal expansion was determined to be 18.4 x 10-6/° C after heat treatment.

Jan 1, 1977

By D. L. Paulson

The Bureau of Mines is investigating pyrometallurgica1 and" chemical methods to recover valuable constituents from metallurgical dusts and slags. Under this program a technique was developed to recover iron from molten copper smelting furnace slags by carbon injection. Slags from gas-fired reverberatory and electric copper smelting furnaces were treated in an 800-kva electric-arc furnace by injecting coke breeze into the bottom of the molten bath. Over 95 pct of the iron and over 90 pct of the copper contained in the smelting furnace slags were recovered, while up to 85 pct of the carbon injected into the system was utilized. It is anticipated that the metal product containing approximately 95 wt-pct iron and 2 wt-pct copper will be a satisfactory medium for recovering copper by cementation.

Jan 1, 1977

By P. W. Jeran, M. C. Irani, D. H. Lawhead

The Beckley mine is one of five new mines in a heretofore unmined portion of the Beckley coalbed. The remoteness of these new mines from prior mining and their greater overburden preclude applying methane emission experience obtained in the old mines. Four sections of the Beckley mine were monitored. The data gathered show that variations in methane emission cannot be explained by variations in coal production. Although overburdens varied by as much as 30 pct, no correlation with methane emissions could be determined. The rib emissions increase with increased length of rib from a section advancing into virgin coal and do not decline over a prolonged idle period (32 days) whereas some decline has been measured for a section not mining into virgin coal. The indication is that degasification prior to mining will reduce the hazard of methane emissions in this area of the Beckley coalbed.

Jan 1, 1977

By P. W. Jeran

The Beckley mine is one of five new mines in a heretofore unmined portion of the Beckley coalbed. The remoteness of these new mines from prior mining and their greater overburden preclude applying methane emission experience obtained in the old mines. Four sections of the Beckley mine were monitored. The data gathered show that variations in methane emission cannot be explained by variations in coal production. Although overburdens varied by as much as 30 pct, no correlation with methane emissions could be determined. The rib emissions increase with increased length of rib from a section advancing into virgin coal and do not decline over a prolonged idle period (32 days) whereas some decline has been measured for a section not mining into virgin coal. The indication is that degasification prior to mining will reduce the hazard of methane emissions in this area of the Beckley coalbed.

Jan 1, 1977

By M. J. Sapko

The Bureau of Mines conducted laboratory-scale flammability experiments to investigate the possible use of water spray systems for inerting or quenching mine-gas ignitions, such as those encountered at the working face of a coal mine. The inerting results for premixed methane-air-water mixtures indicated that water droplets of less than 10 µm tend to be as effective as the vapor. Water requirements for inerting such mixtures were much smaller than those for quenching the sustained flame propagation by the application of water sprays. The minimum water mass concentration for quenching methane-air flames increased linearly with increasing droplet diameter (surface weighted mean) and decreased with increasing spray temperature, whereas the droplet surface area required per unit volume was essentially constant for a given gas mixture composition. Data extrapolations indicated that a quenching system may be feasible for the longwall mining application.

Jan 1, 1977

By Jack E. Fraley

Because of their noncombustibility, silicate and magnesium oxycements are desirable for sealing shale in underground coal mines. In this Bureau of Mines investigation, cement samples were cured and tested (nonstandard tests) for submersion to note resistance to dissolution (breaking into parts), which is an important property for a coating. Nonappreciable dissolution during 1 week of submersion was set for passing the test. Over half of the coatings passed the test.

Jan 1, 1977

By R. R. Backer

The Bureau of Mines investigated the typical physical and chemical properties of coal waste materials from the western part of the United States. The results are compared, in so far as possible, with the properties of waste materials from eastern coal operations. The authors found a disparity of mines and preparation plants among western U.S. coal operations and dissimilarities with typical operations in the East. The relatively cleaner product from the predominance of surface mining and the occurrence of thicker seams in the West reduces the amount of coal preparation required and the size of the waste piles. Because of the abundance of land available for waste disposal, many of the piles are low and extended over large areas. New concepts relating statistical shear strength data to liquifaction potential are presented. The somewhat limited data indicates that western coal sludge is coarser with higher permeabilities and shear strengths than the eastern deposits.

Jan 1, 1977

By W. P. Diamond, B. M. Bench, C. M. McCulloch

This Bureau of Mines report describes photolineaments obtained from stereoscopic examination of vertical aerial photographs and by the Ronchi grating study of aerial photoindex sheets. The photolineaments are compared with the trends of oriented fracture systems procured by measuring the compass direction of joints in bedrock. The relative reliability of the methods is shown, and the results are presented in graphical, tabular, and written form. Analyses of field measurements of strikes of bedrock joints in the project area indicate for the most part two intersecting sets of major joints oriented N 76° W - N 15° E, and N 57° W - N 27° E. The analyses of lineaments determined by stereoscopic examination of aerial photographs show dominant trends of lineament zones of weakness to be an average of N 65° W - N 20°E. Analysis of lineaments found by Ronchi grid viewing of aerial photoindex sheets indicate dominant trends of N 70° W - N 27° E. The three methods give similar findings and verify the work of previous authors. The Ronchi grid method is a useful guide, but it cannot be substituted for the two more painstaking methods.

Jan 1, 1977

By B. M. Bench

This Bureau of Mines report describes photo lineaments obtained from stereoscopic examination of vertical aerial photographs and by the Ronchi grating study of aerial photoindex sheets. The photolineaments are compared with the trends of oriented fracture systems procured by measuring the compass direction of joints in bedrock. The relative reliability of the methods is shown, and the results are presented in graphical, tabular, and written form. Analyses of field measurements of strikes of bedrock joints in the project area indicate for the most part two intersecting sets of major joints oriented N 76° W -N 15° E, and N 57° W -N 27° E. The analyses of lineaments determined by stereoscopic examination of aerial photographs show dominant trends of lineament zones of weakness to be an average of N 65° W -N 20° E. Analysis of lineaments found by Ronchi grid viewing of aerial photoindex sheets indicate dominant trends of N 70° W -N 27° E. The three methods give similar findings and verify the work of previous authors. The Ronchi grid method is a useful guide, but it cannot be substituted for the two more painstaking methods.

Jan 1, 1977

By P. G. Barnard

Losses of alloying metals in furnace flue dusts, grinding swarfs, and mill scale produced during the manufacture of stainless steel are substantial. About 25 million lb Cr, 8.7 million lb Ni, and 150,000 lb Mo and other critical metals can be made available annually for recycling by a process developed by the Bureau of Mines. Stainless steel wastes pelletized with a portland cement binder were reduced in a small electric-arc furnace by a two-stage process to produce a recyclable alloy containing Cr, Ni, Mn, and Fe. The initial reduction was with carbon; the second, with ferrosilicon. Results are compared with previously reported laboratory induction melting tests. A 2,000-lb demonstration test of the process in a commercial electric-arc furnace is also described. Data are also presented on three 1,500-lb tests made using various slag conditions in the electric-arc furnace. Recoveries up to 99 pct of the Fe, Cr, and Ni contents of stainless steel wastes were obtained in using the process.

Jan 1, 1977

By J. H. Maysilles

The Bureau of Mines is examining a variety of low-grade uranium ores because projections indicate that an appreciable percentage of future U.S. uranium production will be derived from resources containing 0.01 to 0.1 percent U308. One possible source is represented by a granitic material from Wyoming; the available samples contained 0.06 and 0.12 percent U308. Tests were conducted to explore the general leaching characteristics of this potential resource. The material responded to both acidic and alkaline leaching techniques. Conventional acid leaching extracted 93 percent of the uranium in 18 hours; the required acid addition was 50 to 100 pounds of H2S04 per ton of ore, and the oxidant addition was 3 pounds of NaCl03 per ton of ore. The acid consumption continues after maximum uranium recovery has been reached; this effect may complicate heap or in situ leaching with acidic solutions. Some variation in reagent requirements was noted between the two ore samples. Conventional carbonate leaching with strong solutions at 85° C extracted 94 percent of the uranium in 24 hours. These granitic materials also showed some response to dilute carbonate solutions, and the results suggest that the material may be chemically amenable to heap or in situ leaching with dilute carbonate solutions.

Jan 1, 1977

By Robert A. Bruce

A motion transducer based on coherent mixing of laser light backscattered from rough surfaces is evaluated in terms of sensitivity, bandwidth and range. Tests made with a prototype composed of a 4-mw HeNe laser, a silicon avalanche photodiode, and a 15-cm aperture telescope demonstrate that remote measurements with reasonable bandwidth and accuracy are feasible at distances up to 100 meters.

Jan 1, 1977

By Robert F. Chaiken

A quasi-steady-burning channel model is used in this Bureau of Mines study to describe the conductive heat loss from an in situ coal combustor to the surrounding rock strata. The calculated heat losses are significantly greater than those previously estimated, but are still very acceptable from the viewpoint of energy recovery. Approximately 80% to 90% of the heat of combustion of the coal should appear as sensible heat of the gaseous exhaust, with exhaust temperatures in the range of 1,000° to 1,200° C. The effects of burning stoichiometry and channel size on the heat loss are also discussed in terms of the model. Such effects are shown to be compatible with an in situ combustion process even in thin seams. However, these results depend on gas leakage and adverse roof falls not being important factors in deter-mining the heat loss mechanism.

Jan 1, 1977

By Joan C. Biordi

In this research by the Bureau of Mines, slightly lean CH4-O2-Ar flames at 0.042 atm with and without small amounts of the inhibitor CF3Br were probed using molecular beam and mass spectrometric techniques. Ratios of product concentrations to reactant concentrations were formed and compared with the equilibrium constant for seven reactions--(l) H+O2 = OH+O, (2) O+H2 = OH+H, (3) OH+H2 = H2O+H, (4) OH+OH = H2O+O, (5) CO+OH = CO2+H, (6) Br+HBr = Br2+H, and (7) H+HBr =H2+Br--to determine to what extent they may be considered balanced in various regions of the flame. With the possible exception of reaction 4, none of the reactions are completely balanced until maximum flame temperature is reached. Once the reactions become equilibrated, their balance is maintained as the temperature and radical concentrations falloff in the secondary reaction zone. Reaction 7, in inhibited flames, is balanced at relatively low temperatures, comparable to reaction 4. Reaction 6 was found not to balance in either the secondary or primary reaction zones. Radical decay in the secondary reaction zone was analyzed using the pool-decay concept. The important recombination reactions were judged to be H+OH+M~H2O+M, and H+O2+M?HO2+M. A rate coefficient of 2x1016 cm6 mole-2 sec-1 is calculated for M = the burnt gas mixture of Ar, HaO, CO2, and 5x1015 cm6 mole-a sec-1 is calculated for M = Ar (both for T = 1,750±150 K).

Jan 1, 1977

By Aarne Visnapuu

Pneumatic chipping, scaling, and grinding can expose the tool operator to noise levels in the range 90 to 120 dbA. In most chipping and scaling operations, casting resonance is the primary source of noise, followed by air exhaust, and machine and chisel resonance. In grinding, the air-exhaust noise predominates. The Bureau of Mines has shown that noise from these operations can be reduced by up to 15 dbA. Workpiece resonance was reduced by sand or other damping methods; tool resonance, by internal damping; and chisel resonance, by constrained-layer treatment. Mufflers reduced air-exhaust noise, and an acoustically treated booth was effective in containing noise around the work area without increasing operator exposure.

Jan 1, 1977