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By Donald R. Corson

The Bureau of Mines is conducting research on the effects of various established and potential soil-stabilization additives to hydraulic backfill. This initial phase is an evaluation of the effect of inclusion of varying amounts of Portland cement and combinations of cement and a dispersant on the bearing strength of backfill. Results of unconfined compression tests are given for over 200 sample cylinders incorporating a fill material with cement or cement and dispersant. Inclusion of a minor amount of dispersant (0.2 percent by weight) is found to yield a significant increase in strength for 20-to-1 and leaner sand-cement mixes. An apparent optimum concentration of dispersant exists beyond which no further increase in strength is achieved. A dispersant-cement ratio of l.8- to-1 yielded a strength increase of 515 percent over the strength of untreated 40-to-l sand-cement mixes.

Jan 1, 1966

By S. E. Khalafallo

The Bureau of Mines investigated the kinetics of reduction of wustite and magnetite with carbon monoxide. A mechanism was postulated wherein the interaction between gaseous and absorbed carbon monoxide appears to be the rate-determining process. This mechanism fully accounts for the experimental rate equation JL.h relates th velocity of reduction to the pressure of the reducing gas at constant temperature. It also explains the variability of the heat of activation of the reduction process with the state of aggregation of the oxide material. The integrated rate equation is in perfect agreement with the experimental reduction-time curves.

Jan 1, 1966

By H. J. Heinen

The Bureau of Milts studied repetitive batch electrowinning of molybdenum from molybdic oxide ) to determine the effects upon the electrolyte life, purity of metal product , and overall cell performance. The electrolyte consisted of 54.0 weight-percent sodium tetraborate (Na2B407), 23.6 weight-percent sodium chloride (NaC1), 14.9 weight-percent sodium fluoride (NaF), and 7.5 weight-percent Mo03. The feed materials were pure and technical-grade Mo03. Electrolysis was conducted at l,000° C in a graphite cell in an atmosphere of air and carbon oxides. Electrolyte degradation did not occur during repetitive winning of molybdenum from pure Mo03 in an 8-day (5,400-ampere-hour) period of operation. Electrowon metal contained <0.1 percent total impurities. The electrode configuration is a key factor in the direct conversion of technical-grade Mo03 to metal by repetitive cyclic electrolysis. The best configuration found was a cathodic crucible and a central anode. Metal purity of 99.8 percent and a current efficiency of 91 percent were maintained until the combined impurity buildup the electrolyte reached 4.7 percent silicon, l.0 percent aluminum, and 0.6 percent iron. One pound of molybdenum was produced per 1.5 pounds of solvent salts employed. About 25 percent of the initial NaCl and NaF contents of the electrolyte were lost owing to volatilization and crucible penetration.

Jan 1, 1966

By Donald W. Mitchell

Certification tests for urethane-foam systems and techniques for apply-ing foam safely in mines are described. Fire hazard from foam exists if flame propagates beyond the ignition source or penetrates the foam. Foam that passes the certification tests can be applied on stoppings, continuous sections of ribs of relatively wide passageways (with no foam on the roof), short sections of roof such as overcasts, roof cavities, and intersections (with no foam on the ribs), and between buntons on one wall of a shaft. Foam on the ribs and adjoining roof presents a fire hazard. Stoppings covered with foam passing the certification tests are resistant to penetration of heat, flame, and smoke than similar stopping without foam. Flame propagation can be arrested by water sprays. Spontaneous ignition of foam can be prevented.

Jan 1, 1966

By Jr. Karr

The Bureau of Mines studied the influence of carbonization method, temperature, and carrier gas on the composition of eight different low-temperature tars produced from a Colorado subbituminous coal. A fluidized bed was compared with an entrained bed, temperature was varied from 500° C to 650° C, and external heating using recycle gas as the carrier gas was compared with internal heating using oxygen-containing gas. The entrained bed yielded significantly more m-cresol and m-ethylphenol, indicating that thermodynamic equilibrium was more nearly approached in the system. Increasing the temperature greatly increased the yield of benzenes and naphthalenes, while paraffins, olefins, and total tar acids were reduced. Using oxygen in the carrier gas decreased the yield of low-boiling phenols and increased that of paraffins and olefins at 650° C.

Jan 1, 1966

By Elton L. Litchfield

The techniques for direct initiation of detonation, developed by the Bureau of Mines, have been applied to gaseous mixtures of oxygen with methane, &apos;thane, propane, butane, or hexane. An exploding wire was used as the initiation source to determine minimum stored electrical energies required to effect detonation of mixtures between one-half and two times the stoichiometric fuel ratios. Detonations were obtained in the most easily initiated mixtures of ethane, propane, butane, and hexane for initiation energies between 24 and 33 joules at 1 atm and 28-43 joules at 0.5 atm initial pressure. Methane mixtures, at 1 atm, were not observed to detonate when initiated with up to 484 joules.

Jan 1, 1966

By R. O. Dannenberg

This Bureau of Mines report describes the results of research to develop a process for recovering additional beryllium from a commercial mill waste product, fluoferrate leach residue. Forty-five percent of the total beryllium in the leach residue was recovered in a beryllia product assaying over 98 pct Be0 by a process comprising (1) leaching with 1 N sulfuric acid, (2) adjusting the acidity of the leach liquor to pH 2, (3) extracting the beryllium with di-2-ethylhexyl phosphoric acid (EHPA), (4) stripping the loaded extract with sodium hydroxide solution, (5) boiling the sodium beryllate strip solution to precipitate beryllium hydroxide, and (6) calcining the beryllium hydroxide. Calculated reagent requirements per pound of Be° recovered by a proposed flowsheet were 28.1 lb sulfuric acid, 0.04 lb flocculent, 0.15 lb EHPA, 0.06 lb isodecanol (IDA), 0.22 gal kerosine, and 6.3 lb sodium hydroxide.

Jan 1, 1966

By C. L. Klingman

The Bureau of Mines tested eight commercially available, activated charcoals experimentally to compare the following characteristics: capacity for adsorption of nitrogen at 77° K and 170 atmospheres&apos; pressure, surface area, carbon tetrachloride adsorption capacity, hardness, and density. The nitrogen adsorption test was devised to simulate plant conditions occurring in the final step of purification in Bureau helium faciliti.es. The remaining tests were patterned after empirical acceptance tests that are widely used throughout the adsorbent industry. Surface area and carbon tetrachloride adsorption correlated well with nitrogen adsorption. The samples with low density generally had better adsorption qualities than those of higher density. The carbon tetrachloride test appeared to be the most practical for selecting a charcoal to be purchased, but an attrition, or hardness test should also be run to be sure the charcoal will not crumble in use.

Jan 1, 1966

By Stephen D. Hill

The Bureau of Mines devised and constructed a modified Knudsen effusion apparatus, permitting a constant measure of the weight of effusing vapor, to determine the equilibrium vapor pressure of metal halides at temperatures up to 1,200° K and over the pressure range 10-5 to 10-2 torr. The reliability of the apparatus was established by determining the vapor pressure of potassium chloride. After correcting for partial dimerization of the vapor, data obtained on solid KCl between 750° and 950° K can be expressed by the following equation:

Jan 1, 1966

By Jr. Norman

The Bureau of Mines investigated the thermoelectric properties of yttrium selenides and tellurides from room temperature to 900° C. X-ray crystallographic data were determined for the yttrium-selenium and yttrium-tellurium compounds that were orthorhombic with a cubic substructure. The yttrium selenides and tellurides exhibited semimetallic to insulator conduction properties with figures of merit of 10-9 to 10-4 °C-1. The mono-selenide and monotelluride behavior was partially degenerate; unsatisfied bonds were the source of the large number of charge carriers. The higher stoichiometry selenide compounds were intrinsic semiconductors) but with high electrical resistivities. A critical defect or impurity ionization energy for carrier activation appeared to exist in the majority of telluride compounds. Mobility and energy band determinations are required to interpret completely the observed effects in most of the compounds studied.

Jan 1, 1966

By J. G. Donaldson

Binary alloys of molybdenum and tungsten were prepared by the Bureau of Mines in laboratory-scale experiments by hydrogen reduction of their vaporized hexafluorides. Near-optimum deposition parameters were determined, and the nature of the deposited alloys was investigated. Dense, homogeneous alloys were codeposited between 650° and 750° C with a reduction efficiency of more than 75 percent. The alloy composition was uniform when the hydrogen ratio in the gas feed mixture did not exceed 3 times the stoichiometric requirement. Regulating the proportions of the metal hexafluorides in the gas feed provided a large degree of control over the composition of the deposit. Hardness of the deposits varied directly with the proportion of excess hydro,,,, in the gas feed and with the weight-percent of tungsten in the alloy. Hardness was not affected by deposition temperature over the range 650° to 750° C for specimens of similar composition. Extreme brittleness and unsuitable physical shapes of the alloys prevented tensile strength measurements.

Jan 1, 1966

By J. V. Batty

The Bureau of Mines devised techniques involving the use of beta-and gamma-ray-emitting radioisotopes and successfully adapted these techniques to the density of mineralized flotation froths) the rate of flow of finely ground ore pulps) and the residence time of pulps in processing circuits. Specifically, the water and mineral loads of flotation froths were continuously measured by determining the proportion of a constant-strength beam of beta rays that was absorbed by the froth column. Continuous measurement of the rate of flow of an ore pulp was accomplished by measuring the changing width of a free-falling stream of the pulp with a collimated beam of beta rays. The residence time of solids in conditioning and resin-in-pulp circuits was accurately measured by following the progress through these circuits of a portion of the pulp that had been tagged with the gamma-emitting Ag110 radioisotope.

Jan 1, 1966

By A. A. Cochran

Bureau of MinesThe Bureau of Mines studied the development of practical methods for recovering manganese from the extensive domestic resources of low-grade ores and open hearth slags. A one-step operation was developed on a laboratory scale in which manganese and iron compounds are treated with chlorine, volatilized, and separated by selective condensation. Manganese recoveries of 90 to nearly 100 percent were obtained from 9 of the most important domestic ores. Analyses of the manganese chloride product indicated that it was suit-able for aqueous electrolysis with little additional purification. A complete, integrated process that provides for the recovery and recycling of chlorine is proposed. This process appears to have distinct advantages over previously proposed manganese recovery processes, and, in sharp contrast to leaching procedures, it is applicable to practically any manganese-bearing material.

Jan 1, 1967

By Verne E. Hooker

The Bureau of Mines conducted a preliminary investigation to determine the state of stress in crystalline rock outcrops near Atlanta, Ga. The secondary principal stresses in a horizontal plane near the surface are compressive and are 500 to 3,000 psi. The maximum compressive stress is northeast-southwest in the Stone Mountain-Lithonia district but changes to northwest-southeast near Douglasville. The elastic constants were determined from data obtained by static and dynamic laboratory methods and in situ velocity measurements. Results show Young&apos;s modulus to be dependent upon both stress level and anisotropy in the rock. Average secant moduli obtained from triaxial tests were used to compute the applied stress from borehole deformation measurements.

Jan 1, 1966

By L. B. Pankratzt

The heat capacity of dimo1ybdenum carbide (Mo2C) was measured from 51° to 298° K, and the entropy at 298.15° K was evaluated. Heat content measurements above 298.15° It were conducted for dimolybdenum carbide (M0caY) and monotantalum carbide (TaC). The results were combined with known heats of formation and the 298.15° K entropy for TaC to obtain values of the heat and free energy of formation from 298.15° K to 1,400° K for MoaC and from 298.15°K to 1,800° K for TaC.

Jan 1, 1966

By Webster S. Anderson

Bureau of Mines planer mining tests on the phosphate bed of the Douglas mine, near Drummond, Mont., indicated that a competent bed with a Mohs&apos; scale hardness of 3 to 4 cannot be mined economically with the planer. Although planer mining was feasible where the bed was fractured enough for a 4-inch depth of cut to be consistently maintained, the depth of cut in the competent beds at the Douglas mine did not exceed 0.5 inch. Average production rates were 0.15 ton per minute and 9 tons per man-shift.

Jan 1, 1966

By E. J. Kloos

The Bureau of Mines devised a new machine-test method for measuring carbon dioxide inspired by a wearer of self-contained breathing apparatus. The new method compares favorably in speed and precision with standard man-tests in which the apparatus is tested while actually worn, and is scheduled for use in future approval tests for facepiece carbon dioxide &apos;measurements. However, man-tests will still be used to measure the efficiency of the carbon dioxide sorbent materials in closed-circuit breathing apparatus.

Jan 1, 1966

By Larmon J. Heath

The Bureau of Mines explored the use of air or natural gas for recovering additional oil from natural water-drive reservoirs with little or no original gas saturation. Engineering and production data for a field in the Mid-Continent area, results of limited laboratory experiments, and data shown in the literature were considered. Injecting air into a water-coned well could seriously damage the well. Injecting natural gas into the watered-out zone could improve the producing water-oil ratio. In the reservoir studied, oil recovery can be increased by injecting natural gas to decrease water-oil ratios. Laboratory tests on a core from the field show an increase in oil recovery of 7.6 percent of the original oil in place as a result of increasing the free gas saturation. This recovery could amount to as much as an additional 6 million barrels of oil from this field.

Jan 1, 1966

By C. Ortuglio

The Bureau of Mines developed equations to determine the relationship of yields and products obtained from BM-AGA carbonization in 13-and l8-inch-diameter retorts. The developed equations indicate that results of carbonization in l8-inch-diameter retorts can be predicted from results obtained with l3-inch-diameter retorts.

Jan 1, 1966

By D. E. Wolfson

Twenty-two samples of West Virginia coals were carbonized at 9000 C by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Eighteen samples represented the Coa1burg, No. 2 Gas, No. 2 Gas and Peerless, Powellton, Eagle, Big Eagle, Lower Eagle, Sewell, Fire Creek, and Pocahontas No.6 beds in Fayette County, and four samples represented the Sewell and Fire Creek beds in Greenbrier County. Expansion characteristics of the majority of samples were determined in the Bureau of Mines sole-heated oven. Chemical analyses were determined for all coals. The coals in Fayette County are high-volatile A, medium-volatile, and low-volatile in rank, and the Greenbrier coals are medium-volatile in rank. Most of the coals are chemically suitable for metallurgical coking. All coke strength indices are within acceptable limits for metallurgical coking coals. All the high-volatile A coals contracted and the medium-and low-volatile coals expanded in the sole-heated oven expansion test.

Jan 1, 1966