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By S. C. Schaefer

Thermodynamic properties of indium oxide (In203) have been studied with a high-temperature galvanic cell employing stabilized zirconia electrolytes. In the temperature range 790° to 1,230° K the free-energy change for the cell reaction 21n(1) + 3Cu20(c) = In203(c) + 6Cu(c) together with the standard free energy of formation of cuprous oxide gives the standard free energy of formation of indium oxide from the elements as ?Gf° = -218.78 + 75.34 X 10-3T ±0.7 kcal/mole. A third-law analysis yields the standard enthalpy of formation: ?Hf°298.15 = -221.5 kcal/mole.

Jan 1, 1971

By J. A. Lamonica

The Bureau of Mines conducted an environmental noise survey to determine the noise levels to which underground coal mine employees are exposed, to evaluate noise survey techniques and equipment, and to compare noise exposures using two criteria, Walsh-Healey and CHABA, for determining allowable exposures that were under consideration for the Federal Coal Mine Health and Safety Act of 1969- Time study techniques and Bureau-approved standard sound level meters were employed. The shift exposures of 20 percent of the miners studied were in excess of the safe standards established by both criteria. The shift exposures calculated using the Walsh-Healey criteria were greater than those calculated using the CHABA criteria owing to the intermittent nature of the exposure. Ultimately the CHABA criteria were rejected, and the Walsh-Healey criteria were adopted.

Jan 1, 1971

By I. L. Nichols

The inplace cyanidation leaching of gold from placer deposits is a potential method for treating gravels too deeply buried and too low in gold content to be processed economically by conventional dredging methods. Laboratory experiments were made to evaluate those placer cyanidation factors adaptable to small-scale studies. The variables investigated included gold particle size and location in sand beds, cyanide solution flow rate, and cyanide solution strength as factors affecting gold solubility rates. The solution flow rate, in turn, was influenced by variables such as bed slope, solution head pressure, and sand size, and the effects of these factors were studied. Free gold, minus 150-mesh and finer in size, is rapidly dissolved by dilute cyanide solutions from mixtures of gold and silica sand prepared to simulate placer deposits. About 94 percent of minus 325-mesh free gold was extracted in 5 hours from silica sand mixtures, and 94 percent extraction of minus 150-mesh gold was obtained in 21 hours with 0.1 percent NaCN solutions. Moving solutions were almost twice as effective in leaching free gold from silica sand mixtures than stagnant solutions.

Jan 1, 1971

By H. R. Appell

The Bureau of Mines is experimentally converting cellulose, the chief constituent of organic solid waste, to a low-sulfur oil, All types of cellulosic wastes, including urban refuse, agricultural wastes, sewage sludge, wood, lignin, and bovine manure, have been converted to oil by reaction with carbon monoxide and water at temperatures of 350° to 400° C and pressures near 4,000 psig, and in the presence of various catalysts and solvents, Cellulose conversions of 90 percent and better (corresponding to oil yields of 40 to 50 percent) have been obtained. A continuous reactor for use at maximum conditions up to 500° C and 5,000 psig has been operated successfully, Using sucrose as a feedstock, operation in this system has permitted a simplified and preliminary chemical study of the conversion process. Oil yields of over 30 percent have been obtained with this unit.

Jan 1, 1971

By Manuel Gomez

Dehydrogenation factors, proximate analysis, and ultimate analysis were examined as predictors of the low-temperature -carbonization properties of coals varying in rank from lignite through anthracite. All factors studied contributed to reduction in variance of the sample populations investigated. Response surface regression models based on variables from proximate and ultimate analyses of coal were constructed for eight low-temperature carbonization assay product and gas component Fields. These models were tested with independent samples that included drill cores, sized fractions, petrographic fractions, and run-of-mine coal. The models developed were used to predict low-temperature carbonization yields or coals from major fields of Wyoming. This information was cast in the form of contour plots describing the potential low-temperature carbonization product yields of Wyoming coals and the properties of the resultant char or coke. The variables used as input v the models may be measured and collected during exploration; thus, the carbonization properties of a seam can be determined in advance of mining. The information presented in this report is useful in that it broadens the deciionmaking base for management when either mine locations or coal conversicl plant sites, or both, are being considered.

Jan 1, 1971

By V. E. Edlund

Laboratory batch flotation tests were conducted on copper converter slags to evaluate the relative merits of recovering copper from slow-cooled versus water-quenched slags. Three slags containing 1.6, 5.0, and 6.6 percent copper were used. More than 90 percent of the copper was recovered in a rougher concentrate leaving a 0.2- to 0.3-percent copper tailings when treating slow-cooled slag. Lower recoveries and higher copper tailings ranging from 0,5 to 0.6 percent copper were obtained from quenched slag. Grindability studies were made on the respective heat-treated slags. Quenched slags proved more difficult to grind than slow-cooled slags. Cost studies showed that (1) the cost of slow cooling and crushing off-sets any advantages of higher copper recoveries from slow-cooled slag, and (2) water-quenched slag, which requires no crushing preparatory to grinding, could be treated more economically. Costs based on processing 1,000 tons of slag per day would be $1.85 per ton for quenched slag versus $2.37 per ton for slow-cooled slag.

Jan 1, 1971

By V. E. Edlund

Laboratory batch flotation tests were conducted on copper converter slags to evaluate the relative merits of recovering copper from slow-cooled versus water-quenched slags. Three slags containing 1.6, 5.0, and 6.6 percent copper were used. More than 90 percent of the copper was recovered in a rougher concentrate leaving a 0.2- to 0.3-percent copper tailings when treating slow-cooled slag. Lower recoveries and higher copper tailings ranging from 0.5 to 0.6 percent copper were obtained from quenched slag. Grindability studies were made on the respective heat-treated slags. Quenched slags proved more difficult to grind than slow-cooled slags. Cost studies showed that quenched slags can be treated at slightly lower cost than slow-cooled slags. However, the cost advantage of processing quenched slags is more than offset by the higher copper recoveries obtained from slow-cooled slags.

Jan 1, 1971

By D. A. Wilson

A cyclic leaching process was developed for selectively leaching and recovering cadmium from nickel-cadmium scrap battery waste. The six major steps in the process are the following: (1) washing the plates to remove KOH electrolyte, (2) roasting at 550° to 600° C to oxidize metallic cadmium and decompose cadmium and nickel salts, (3) leaching with an ammonium nitrate solution, (4) precipitation of the leached cadmium from solution as cadmium carbonate using CO2 gas, (5) removal of CO2 from the lixiviator by adjusting to pH 4.5, heating, and evacuating the system, and (6) removal of small amounts of leached nickel from the lixiviator using a solvent extraction technique. The regenerated lixiviator is then recycled to leach additional plates. Cadmium extraction was 94 percent and the cadmium carbonate product contained 0.14 percent nickel and 0.12 percent cobalt impurity. The leached plates were smelted to a high nickel-low iron alloy with no detectable amounts of cadmium.

Jan 1, 1971

By R. A. Vik

The influence of thermal treatments on the grindability of low-grade hematitic iron ores from Michigan and Minnesota was examined in bench-scale tests. Treatment factors were roasting temperature, roasting atmosphere, and ore cooling conditions. Bond ball mill grindability and work indices were used as response indicators in evaluating the condition of the ore. Of the three treatment factors evaluated, roasting atmosphere, which brought about the con version of iron oxides to magnetite, had the most significant effect; roasting temperature had the next most important effect; and cooling condition had the least effect. Optimum grindability was obtained with reduced-quenched products of both ores at 650° C, near the alpha-beta phase transformation of quartz.

Jan 1, 1971

By F. G. Horino

The Bureau of Mines conducted compressive strength tests on model pillars of selected rock types with each pillar containing a critically oriented plane of weakness. The objective of these tests was to determine if a significant increase in the strength of the model pillar could be obtained by either (1) installing tensioned rock bolts through the pillar and normal to the plane of weakness, or (2) wrapping tensioned steel wire ropes around the pillar at uniformly spaced intervals along the pillar. Equations based on Coulomb's failure criterion are developed to predict uniaxial compressive strength of model pillars that are either rock-bolted or wire-roped. Laboratory compressive strength tests on unbolted and bolted model pillars of sandstone, marble, Indiana limestone, and oil shale containing a plane of weakness oriented at 45° showed that the bolted pillars are stronger than the unbolted pillars by 84, 31, 52, and 28 pct, respectively. Laboratory compres-sive strength tests on nonroped and roped model pillars of Texas limestone, sandstone, and granite containing planes of weakness showed that the roped pillars were stronger than the nonroped pillars by factors ranging from 1.01 to 2.41, depending upon the angle of the plane of weakness and the rock type. Rocks with a low Young's modulus benefited most by the wire-roping technique.

Jan 1, 1971

By T. T. Campbell

Studies were conducted by the Bureau of Mines to develop a process for preparing thorium-magnesium master alloys or pure thorium metal by magnesium reduction of thorium tetrachloride in a semicontinuous reactor. Thorium tetrachloride was prepared in a fluidized-bed reactor by chlorination of thorium oxide or thorium oxalate. Conditions were established for producing a suitable thorium oxide feed for a fluidized-bed reactor. Thorium tetra-chloride was purified by vacuum sublimation and subsequently reduced by magnesium in a semicontinuous reactor to form thorium-magnesium alloys. Relatively pure thorium was produced by removing magnesium from the alloys by vacuum sublimation. Close to 100 percent of the thorium fed into the reactor was recovered either as metal (~93 percent) or as thorium oxide (~7 percent). The oxide can be recycled directly into the process.

Jan 1, 1971

By R. L. Rough

Photoelastic, wire resistance, and borehole-deformation gages were used to measure the in situ strains when an outcropping Black Hand Sandstone Formation in Hocking State Forest, Hocking County, Ohio, was overcored to stress-relieve the surrounding sandstone. Strains transmitted to the photo-elastic gage did not produce isochromatic patterns suitable for quantitative analysis. Strain readings from the wire resistance gage indicated tensile-strain loading during overcoring; readings from the strain-gage bridges in the borehole-deformation gage indicated compressive-strain relaxation during overcoring. The magnitude and orientation of the computed stress fields obtained from both gages were comparable when the corresponding tensile and compressive elastic moduli were applied. Stresses computed from deformation and resistance gages at depths to 5 feet showed the maximum stresses to range from 1.042 to 2.121 times greater than the minimum stresses. The bearings of principal stresses calculated from the deformation gage readings varied between N 61° E and N 83° E; the wire resistance strain gage bearing computations varied between N 68° E and N 82° E. Measurements of in situ strain in sandstone were shown to have promise but to require further development in field technique that could likely be achieved through experience.

Jan 1, 1971

By P. R. Tisot

Structural response and/or deformation was determined for each of four different grade Green River oil shales (27.0-, 34.5-, 45.5-, and 63.5-gal/ton) as they were heated in an inert atmosphere, under constant compressive stress, from ambient to subretorting temperatures; that is, below those required for rapid pyrolysis of the organic matter. Small cores and small columns of confined fragments comprised the test specimens, which were heated, in a specially designed microunit, at a uniform rate either to 725° or to 825° F under three different stress levels, 80, 200, and 325 psi. Structural response of some cores was observed as they were heated in a stress-free environment. The obtained stress-strain-time-temperature relationships provide information regarding the oil shale's yield temperature, yield stress, rate of compressive strain, loss of mechanical strength, and nature of structural deformation. Effects of structural deformation on induced permeability in small columns of fragments are presented. Results indicate that underground retorting of Green River oil shale may be seriously impaired through loss of induced permeability brought about by structural deformation of rich oil shale under the influence of heat and compressive stress.

Jan 1, 1971

By William G. Pariseau

A small displacement-small strain finite element technique utilizing the constant strain triangle and incremental constitutive equations for elastic-plastic media that are nonhardening and obey a Coulomb yield condition has been applied to the analysis of gravity flow initiation in a V-shaped hopper containing a powder under lunar environmental conditions. Three methods of loading were examined. Of the three, the method of computing the initial state of stress in a filled hopper prior to drawdown by adding material to the hopper layer-by-layer is superior (as expected). Results of the analysis of a typical hopper problem show that the initial state of stress, the elastic moduli, and the strength parameters have an important influence on material response subsequent to the opening of the hopper outlet.

Jan 1, 1971

By John M. Gomes

The Bureau of Mines investigated two techniques for removing CaO from scheelite (CaW04) prior to electrolysis. In the first technique, a crude tungstic oxide (WO3) containing 0.15-percent lime (CaO) was prepared by digesting scheelite concentrates in hot hydrochloric acid. This oxide was used as cell feed to produce tungsten of 99.9-percent purity. The second technique used a high-temperature, two-phase separation, resulting in extraction of 99 percent of the WO3 in the halide-tungstate phase, while 90 percent of the CaO was retained in the silicate phase. Tungsten of 99.9-percent purity was deposited from the halide-tungstate melt after B203 and NaPO3 were added to form an electrolyte. The two methods were compared with a previously developed technique of depositing tungsten from scheelite concentrate fed directly to the electrolytic cell.

Jan 1, 1971

By D. W. Mitchell

This Bureau of Mines report summarizes experience and past research on methods for sealing abandoned areas of a coal mine and areas from which the pillars have been wholly or partially extracted. The Federal Coal Mine Health and Safety Act of 1969 requires that such areas be ventilated or sealed with explosion-proof bulkheads, but the present study indicates that bulkheads alone cannot isolate areas in a coal mine in which methane and other dangerous gases have accumulated. Gas-air exchanges between sealed and open areas must be controlled.

Jan 1, 1971

By Benton L. Tibbetts

Comprehensive geophysical measurements were made in the Tertiary Channel gravel deposits of Badger Hill, Calif., with the refraction seismograph, gravimeter, and well logging equipment, to develop a three-dimensional physical model of the gold-bearing gravels. Tests were also made of the applicability of magnetometer and electrical resistivity techniques. Results of 14 seismic profiles revealed four distinct layers with velocities of 1,600 ft/sec for loose gravel, 5,900 ft/sec for compact gravel, 8,600 ft/sec for cemented, blue gravel, and 15,500 ft/sec for bedrock. The depth to bedrock along the middle of the channel varied from a minimum of 100 feet in the hydraulically mined pit area to a maximum of about 300 feet in the upper bench area immediately south of the pit. These geophysical methods revealed that 40 percent of the drill holes necessary to delineate the deposit could be eliminated, at a cost saving of at least 30 percent.

Jan 1, 1971

By L. B. Pankratz

Low-temperature heat capacities, high-temperature enthalpy increments, and the enthalpy of formation at 298° K were determined calorimetrically for vanadium subnitride (VN0.465). The low-temperature investigation gave S°298.15 = 6.379 ±0.005 cal/deg mole, and a combustion calorimeter investiga¬tion provided ?Hf°298.15 = -31.80 ±0.60 kcal/mole. The two quantities were combined with the high-temperature data to give standard values of enthalpies of formation and free energies of formation above 298° K. These and related thermodynamic functions were tabulated to 1,800° K. Similar data are included in the range of 298° to 1,600° K for the mononitride, VN.

Jan 1, 1971

By Larman J. Heath

Liquid incendiaries were burned within the interstices of several different types of sandstone cores to determine the technical feasibility of increasing sandstone permeability by this method. Fuel-oxidant mixtures were tested in 186 cores; six cores exploded when ignited. In virtually all instances, the explosion completely pulverized the sandstone cores. In addition n those cores damaged by explosions, 24 cores were fractured so severely that permeability tests were impossible. Although combustion gener¬ally increased the permeability, specific mixtures at given pressures were inconsistent in their ignition and burning behavior. Tests indicated that the heat of burning incendiaries significantly increased sandstone permeability. The improved permeability ratios were usually less than 2, but one was 10.3. Permeability alteration by other in situ methods was not as effective as that by flame propagation.

Jan 1, 1971

The Bureau of Mines has long been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts, the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions1 issued by the Bureau of Mines, and the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. The Government, with the exception of the Tennessee Valley Authority, purchased approximately 5.5 million tons of coal in fiscal year 1971. In connection with these purchases, the Bureau analyzed 4,366 samples. These are published (table 1) for the use of Government officials and the public. Such analyses of delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1972