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By H. Leitch

In laboratory experiments, the Bureau of Mines investigated melting, quenching, and sulfuric acid leaching of alumina from mixtures of albite and anorthite, and from anorthosites containing 26 to 32 percent alumina. Variations in pouring temperature, quenching and leaching conditions, were studied with respect to the extraction of alumina and impurities. Virtually all of the alumina was dissolved by leaching melted and quenched California anorthosite in boiling 16-percent sulfuric acid solutions for 15 to 30 minutes. The leach solutions were readily separable from the solid residue by conventional thickening and filtration techniques. Only 2 to 5 grams of SiO2, Fe2O3, or CaO dissolved per 100 grams of alumina. The quantity of SiOz in solution varied inversely with the duration of the leach and with the concentration of the H2SO4 solution used. Melted and quenched Wyoming and Minnesota anorthosites with SiO2:CaO weight ratios of 4.3 and 3.2, respectively, were less amenable to sulfuric acid leaching than California anorthosite with an SiO2:CaO weight ratio of 5.3. However, excellent results were obtained on the Wyoming and Minnesota anorthosites by the addition of SiO2 to these materials before melting, in quantities sufficient to adjust the SiO2:CaO weight ratios of the furnace charges to between 4 and 6.

Jan 1, 1966

By Wilbert T. Malenka

In its search for a highly productive mining system for anthracite beds pitching from 100 to 200, where conventional mobile equipment cannot be used) the Bureau initiated a longwall project by introducing a shearer drum cutter loader of European origin. Because of the undulating nature of the roof and floor and changing bed thicknesses, the machine proved inflexible and extra work was required in lifting bottom coal and blasting top coal.

Jan 1, 1966

By Galen G. Waddell

Dilation and contraction of the rock surrounding horizontal access open-ings of a deep mine were analyzed during stope advance to determine what type of measurements, made with relatively inexpensive instrumentation, would best reflect the rock behavior. A variety of instruments, mostly mechanical extensometers, were used. Detailed descriptions are given of Down-the-hole extensometers, floating rockbolt clusters, transit surveys, and other instruments and measuring techniques. Although all of the radial-deformation-rate graphs illustrated useful rock behavior data, the most informative graphs were compiled from data procured with the radial extensometers that penetrated, to various depths, the rock around the access openings. An analysis is given of measurement data on the rock around lateral drifts and across and adjacent to the nearly vertical vein of the Star mine, Burke, Idaho. Several useful relationships were found between the rock deformation rate and the stoping process. Information was produced on the elastic state of rock around an underground opening, effectiveness of stope support, rheology of rock, zone of influence around stopes, effectiveness of rockbolts, axis of maximum strain in a plane perpendicular to the long axis of the lateral, and other phenomena. This information could be of particular value in determining location, design, and support of underground openings.

Jan 1, 1966

By H. E. Perlee

Autoignition temperatures and limits of flammability of nine halogenated hydrocarbons in atmospheres of air, oxygen, and nitrogen tetroxide were measured in a modified standard autoignition apparatus and limit-of-flammability apparatus previously developed at the Bureau of Nines. Of the nine halogenated hydrocarbons investigates--bromochloromethane, bromotrifluoromethane, bromochlorodifluoromethane, 1,1,2-trichlorotrifluoroethane, 1-bromo-l-chloro-2,2,2-trifluoroethane, dibromodifluoromethane, l,2-dibromo-1,1,2,2-tetrafluoro-ethane, 1,1,1,3,3-pentachlorotrifluoropropane, and l-bromo-2,4-dichloro-1,1,2, 3,3,4-hexafluorobutane--two formed flammable mixtures with nitrogen tetroxide and six with oxygen; none formed flammable mixtures with air. Three of the halogenated hydrocarbons formed no flammable zones with any of the three oxidizing atmospheres. For those halogenated hydrocarbons that supported combustion in oxygen atmospheres, explosion pressures developed during constant-volume burning of mixtures near the middle of the flammable zone were observed to range from about 6 psig for dibromodifluoromethane to 158 psig for 1-bromo-1-chloro-2,2,2-trifluoroethane. In all cases, the calculated burning velocities of these mixtures were less than 8 in/sec.

Jan 1, 1966

By L. J. E. Hofer

The Bureau of Mines determined rates of adsorption and desorption of methane as a function of particle size and temperature, using coals from the Pocahontas No.3 seam (lvb) from the Bishop mine of western Virginia, and the Pittsburgh seam (hvab) from the Pursglove No. 15 mine of northern West Virginia. For a given coal sample and temperature, the rate curves for adsorption and desorption are essentially the same when expressed on a fractional approach to equilibrium basis. The rates of adsorption and desorption increased eightfold as the particle size was decreased from 6-8 to 270-325 mesh per inch. The adsorption process appears to be diffusion controlled. Rate of sorption processes increased with increasing temperature; however, the amount adsorbed at equilibrium decreased.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted petrographic classification and flotation studies to determine if acid-grade concentrates could be obtained from individual and composite samples from the Meade Peak member of the Phosphoria Formation, Idaho. The petrographic studies were made to determine the effect of compositional features on concentration of phosphates. The ore grade, ovule size, and clay content were the main features affecting grade and recovery of phosphate. Flotation results on roasted ore with a tall oil emulsion scheme showed that beds containing over 10 percent P2O5 could be beneficiated and composited with the two high-grade beds to produce a composite concentrate containing 31.9 percent 05 at 84.3 percent recovery. Treatment of these intermediate-grade phosphate beds by flotation increased ore reserves over 200 percent and increased the ore-to-waste ratio in the ore zone from 1:5.7 to 1:0.27.

Jan 1, 1966

By R. F. Abernethy

A modified Unterzaucher method was applied to the direct determination of oxygen in coal. Coal samples were pyrolyzed in a nitrogen atmosphere, and the gaseous oxygen compounds liberated were converted to carbon monoxide by a platinized-carbon catalyst at 9000 C. After passing over heated copper and through a tube containing soda-asbestos and magnesium perchlorate, the purified carbon monoxide was oxidized to carbon dioxide by iodine pentoxide--liberating an equivalent amount of iodine. The iodine was titrated with 0.02 ~ sodium thiosulfate; in a few tests the weight of carbon dioxide produced was determined. Direct oxygen determinations of coal included organic oxygen from the coal substance, plus a small quantity of inorganic oxygen derived principally from carbonate minerals and from combined water of silicates in the mineral matter. The influence of mineral matter on the direct oxygen determination was investigated by testing (1) untreated coal, (2) demineralized coal from which most of the mineral matter except pyrite was removed by treatment with hydrofluoric and hydrochloric acids, and (3) coal samples treated with dilute hydrochloric acid.

Jan 1, 1966

By R. L. Benner

The Bureau of Mines investigated the ZnO-Fe2O3-Fe3O4 system at 1,000°, 1,300°, and 1,400° C, with oxygen pressures between 1.0 and lx10-4 atmospheres. The results, divided into the thermodynamic properties as related to the spinel structure, and the thermodynamic properties as related to zinc concentrate roasting, were used to calculate the activities of ZnO, Fe2O4, and Fe3O4 within the spinel solid solution region of the ternary system, and the pseudo-binary activities of ZnFe2O4 and Fe304. The activities of both systems show large positive deviations from Raoult's Law, especially at high Fe3O4 concentrations. The free energies, the enthalpies, and the entropies of mixing for the binary system were calculated from the binary activities, and the entropies of mixing were compared with two statistical models, one representing an ideal solution, and one representing the mixing of a normal with an inverse spinel. The binary entropy of mixing seemed to be better represented by the latter statistical model, indicating that the tetrahedral and octahedral cations of the reactants tend to remain in the product, even at the high temperatures of the study. This comparison also indicated that the cations of the components are the major contributing factors to the thermodynamic properties.

Jan 1, 1966

By Willard L. Hunter

The Bureau of Mines studied the effect of temperature upon the reduction of chromite by carbon and the relative reducibility of chromites as a function of their composition. Ferric oxide was also studied to provide comparative data. Pellets weighing approximately 1 gram and containing 70 percent ferric oxide, chromic oxide, or chromite and 30 percent graphite were subjected to closely controlled temperatures under a flow of argon for 15 minutes. The amount of CO and CO2 evolved was measured, and the reduced sample was analyzed by X-ray diffraction techniques. The reduction of Fe2O3 was studied over a temperature range of 600° to 1,400° C, while the reduction of Cr2O5 and chromite was conducted from 9000 to 1,621° C. The temperature above which appreciable reduction of Cr203 by graphite took place was 1,125° C. The temperature at which significant reduction started for three of the four chromite samples was approximately the same, indicating that there was concurrent reduction of iron and chromium oxides in the chromite mineral rather than selective reduction of iron oxides followed by reduction of chromic oxide. Rhodesian chromite appeared to dissociate at a lower temperature with concurrent reduction of iron. Based on the temperature at Which chromite was 50 percent reduced in 15 minutes, Transvaal chromite reduced most easily, followed by Mouat, then by Kampersian, and finally by Rhodesian DFC material. Statistical analysis of test results indicated that the ferric iron content of chromites affects their reduction behavior more than any other constituent.

Jan 1, 1966

By H. C. Fuller

Submerged combustion and inverse solubility methods were investigated as promising alternative means for crystallizing manganese sulfate from solutions produced by leaching manganese ores with either sulfuric acid or sulfur dioxide. Evaporation of water from typical manganese sulfate solutions by sub-merged combustion techniques enabled production of a slurry containing 32 to 39 pct MnSO4.H2O crystals suspended in a saturated solution of manganese sulfate. Such a slurry required further processing by thickening or filtration and drying to produce crystals of MnSO4.H2O. In a second approach, semicontinuous processing of manganese sulfate solu¬tions by thermal crystallization under pressure effected a recovery of 94.5 pct of the MnSO4.H2O as dry free-flowing crystals. Treatment of a solution containing about 100 grams manganese per liter at 189° C, produced a "barren" solution containing only 1.9 grams manganese per liter. Calculations made on comparable manganese sulfate solutions show that the heat requirement of the thermal crystallization method was about one-third to one-fourth that of the submerged combustion method.

Jan 1, 1966

By Alton B. Cook

A material balance equation was derived for calculating (1) the initial oil volume and (2) the relationship of average reservoir pressure to net gas in storage in reservoirs used for natural gas storage operations. The equation is also applicable to secondary-recovery operations where reservoirs are completely repressured and gas cycled. Using this equation minimized two probable sources of appreciable error in conventional material balance calculations: inaccurate measuring of and accounting for produced gas, and differences between true reservoir pressure and average reservoir pressures as derived from bottom-hole pressure measurements. A new procedure is presented for calculating water encroachment. By solving the conventional material balance equation and the derived equation for gas storage simultaneously, the values for initial oil in place and net water encroachment can both be determined.

Jan 1, 1966

By M. M. Fine

This Bureau of Mines report describes the theory, experimental procedures, and the results obtained to date in the development of the Bureau's process for magnetically roasting iron ores using scrap iron as a means of reduction. Since magnetic separation is an operational step common to magnetic taconite plants, the preliminary research studies emphasized only the novel magnetic roasting step. The studies included the use of automobile scrap, ferrous reductants such as borings and turnings, and prereduced pellets. Technical feasibility of the process was demonstrated both on a bench- and pilot-scale. Quality magnetic concentrates with recoveries of over 90 percent were obtained from a direct shipping ore containing 59.5 percent Fe and from fine grained semitaconites with about 30 percent Fe.

Jan 1, 1966

By Robert S. Warfield

Eight samples of high-volatile bituminous coal, each large enough for a study of its coking properties by the Bureau of Mines, were obtained from a location along the Kukpowruk River, Arctic Northwestern Alaska. Bench scale and pilot plant carbonization studies with several patterns of coal blending were conducted. The data from these tests were compared to data from similar tests on a coking blend used by the Kaiser Steel Corporation at Fontana, Calif. The majority of the samples representing the 20-foot seam was found to have significant coking properties, and produced coke approaching metallurgical quality when blended with selected coking coals. Although oxidation effects were evident in the samples representing upper portions of the seam, it appears that the whole seam could be used.

Jan 1, 1966

By R. L. Benner

A compound stability diagram was constructed by the Bureau of Mines for the Zn-Fe-S-O system to show the phases that should be thermodynamically stable at various temperatures, oxygen pressures, and SO2 pressures. The diagram was demonstrated to have good qualitative value for predicting stable phases that may, in turn, be related to the recovery of zinc in the leaching phase of the electrolytic zinc process. The study showed that roasting temperature is the most Significant variable in preventing roaster formation of zinc ferrite, which is directly related to subsequent extraction of zinc in the leaching step.

Jan 1, 1966

By Lippe D. Sadwin

A high-speed streak camera method for making equation of state measurements (shock and particle velocities) on samples of rock under dynamic load conditions is described. Experimental data are given for tests on 12 samples representing 5 rock types. Analysis of these data shows that the method is practical and that good reproducibility of results can be obtained. The pressure range covered in the tests was from 1 to 50 kilobars.

Jan 1, 1966

By R. W. Van Dolah

An attempt has been made in this investigation to define the conditions under which ammonium nitrate (AN) might detonate as a result of involvement in fire. The initiation of detonation by shocks derived from explosives or from projectile impact was investigated as a function of temperature and charge diameter. A new technique was devised to investigate the burning of raw and contaminated AN under pressure. No transition, to detonation in AN was obtained in the burning experiments. The critical diameter for detonation of fertilizer-grade AN was found to be quite small when the AN was at temperatures just below melting point; this indicates that initiation of detonation may be less difficult at elevated temperatures but such initiation by gas-phase detonation was shown to be unlikely. Transition from burning to detonation was obtained with AN intimately mixed with fuels that included polyethyl-ene, paper, and fuel oil when these were contained in vessels with restricted vents. However, the experimental results supported by an analytical study indicate that the initiation of detonation in AN from fire exposure in normal storage and from transportation incidents is quite improbable. The detonation of AN in recent incidents more likely may have resulted from the effects of adjacent explosions.

Jan 1, 1966

By P. L. Weston

The Bureau of Mines used high-temperature reduction roasting, magnetic separation, acid-leaching, and autoclave precipitation processes to recover iron and manganese from brown Cuyana range ores of Minnesota. Wet magnetic separation concentrated over 90 percent of the iron in 3 of 4 ores as high grade products analyzing 74 to 85 percent iron, 2.5 to 6 percent manganese, and 3 to 10 percent SiO2. The nonmagnetic fractions were leached with dilute sulfuric acid extracting 83 to 93 percent of the contained manganese and small amounts of iron. The leach solutions contained Mn-to-Fe and Mn-to-SiO2 ratios favorable enough for possible consumption in metallurgical mane operations. Exceptionally pure Mn solutions were achieved by pressure precipitation of the remaining iron in an autoclave followed by lime precipitation of silica and alumina.

Jan 1, 1966

By James Paone

The Bureau of Mines made drillability studies with impregnated diamond bits in the laboratory on 7 rock types and in the field on 21 different rock types. Results indicate that drill parameters of rotational speed, thrust, and torque must produce sufficient applied forces to induce stress levels that cause continuous failure in rock to achieve efficient penetration rates. Higher rotational speeds appear to be more effective in drilling relatively harder rocks, although the increased speed causes more bit wear; increases in thrust result in higher drilling rates but not linearly; and up to a critical value a linear relation exists between torque and penetration rate for a specific rock type. Penetration rates with impregnated bits show a trend similar to that obtained with surface-set bits for rock under 25,000 psi compressive strength.

Jan 1, 1966

By R. Barany

The heats of the glass-crystal transformation of nepheline (Na0.7794K0.2206AlSiO4) and wollastonite (CaSiO3) and the heat of formation of nepheline at 298.15° K were determined by solution calorimetry. For the glass-crystal transformations, the heat values were -9.0 ± 0.3 kcal/mole for nepheline and -8.1 ± 0.2 kcal/mole for wollastonite. The heat of formation of nepheline was -34.8 ± 0.6 kcal/mole from the oxides and -501.0 ± 0.5 kcal/mole from the elements.

Jan 1, 1966

By P. C. Good

Work was done to determine conditions necessary for efficient electrodeposition of aluminum from fused chloride electrolytes. Aluminum was deposited from a molten chloride salt electrolyte over a temperature range of 150° to 750° C. At lower temperatures in a heat-resistant glass cell, aluminum was deposited on stainless steel and on aluminum cathodes. The deposit was recovered in the form of light, feathery dendrites that could not be consolidated. At 750° C, molten aluminum was deposited at cathode current efficiencies as high as 90 to 100 percent on titanium diboride cathodes and in molten aluminum cathodes. Nitride-bonded silicon carbide was the best cell material, although porcelain was also used. The electrolyte consisted of a mixture of sodium and potassium chlorides in 1 to 1 mole ratio, containing aluminum chloride in concentrations ranging from 2 to 30 weight-percent in cells holding up to 1,000 grams of electrolyte. Generally favorable results were attained in studies made at temperatures greater than the melting point of aluminum.

Jan 1, 1966