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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'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 L. B. Pankratzt

The heat content above 298.15° K of ferroelectric lithium columbate (LiCbO3) was measured to 1,770° K. The Curie temperature was determined to be 1,450° K, the melting point 1,540° K, and the heat of fusion 16.94 kcal/mole. Heat content and entropy increments have been tabulated for the temperature range from i98.15° to 1,800° K. Heat contents are also given in equation form.

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' 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 Jerry W. Ramsey

The Bureau of Mines studied two Pennsylvania anthracites using low-temperature carbon dioxide adsorption. A modified form of the Brunauer-Emmett-Teller equation was used to calculate specific surface areas. Two mesh sizes of each anthracite were used to determine how gamma irradiation at 106 and 108 rads, both in vacuum and in the presence of air, affected the carbon dioxide surface areas. Results show that anthracites have a system of pores that are essentially all interconnected rather than isolated; that anthracites differ from one another in specific surface, which may correlate with density; and that irradiation in vacuum has no discernible effect on specific surface of anthracite, but irradiation in air does produce changes in specific surface.

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 '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 R. L. Crosby

Microscopical and X-ray diffraction techniques were used to identify two intermediate phases in that part of the solid region of the magnesium-cerium system between and Mg3Ce. Previous literature had reported only one intermediate phase for this region, 1)12t chemical analysis determined the approximate composition of the two compounds to be Mg23Ce2 and Mg17Ce2. The range in composition of the two intermediate phases was found to be limited to less than 0.3 atomic percent cerium. The study did not determine the crystal structure of Mg17Ce2, but that of Mg23Ce2 is tetragonal with a = 10.33 A and c = 19.51 A.

Jan 1, 1966

By Jr. Hazen

Relationships that may exist between assays and sample interval lengths when using unequal sample intervals in mine sampling have been investigated as part of the larger research problem of adapting statistical methods to the analysis of weighted average grades. The theoretical relationship between the amount of difference in the weighted and unweighted average grade of ore and the size of the correlation coefficient between assay value and sample interval length was found to be linear. Numerous examples of actual field sample and assay data, which have been obtained by using unequal sample intervals, are documented, and the differences between weighted and unweighted average grades of ore and the correlation coefficients between assays and sample interval lengths have been computed and plotted on graphs. Differences between these actual field data and the expected theoretical linear relationship are examined. It is hypothesized that the use of unequal sample intervals in mine sampling is, in fact, stratified sampling in a statistical context. The sampler establishes stratification by selecting unequal sample intervals on the basis of differences in lithology, changes in rock type, characteristics of mineralization, or differences in metal content. Statistically} methods currently used in mine sampling, involving unequal sample intervals, fail to consider differences in the inherent variances in grade of ore within the various strata established by using unequal sample intervals. Consequently the strata are sampled with different precision. This difference in precision of sampling between strata may account for much of the deviation between the plotted points representing actual field sampling data and the theoretical linear relationship between the amount of the difference between weighted and unweighted average grade of ore and the size of correlation coefficient between assays and sample interval lengths.

Jan 1, 1966

By Jr. Sharkey

The Bureau of Mines investigated gases from flash and laser irradiation of Pittsburgh seam (hvab) coal to determine the action of high temperatures on coal. Temperatures in excess of l,000° C were reached with both types of irradiation. Craters about 300 microns in diameter were produced in the coal with millisecond pulses from the laser unit rated at 1.7 joules' output. Gaseous products from laser and flash irradiations in vacuum contained 21 and 8 percent acetylene, respectively. Diacetylene, vinylacetylene, and other products to molecular weight 130 were indicated in the mass spectrum of the gas from the laser study. Single experiments were also conducted in which the laser energy, particle size of the coal, and atmosphere were varied. The results indicated that the distributions of products obtained from the flash and laser irradiations of coal were different from that produced in high-temperature carbonization.

Jan 1, 1966

By Richard C. Ballance

Fly ash from four sources and in certain proportions was shown to assist chemical coagulation of turbid water and settling of chemically induced floc. Fly ash reduced the time required to form the first visible floc, promoted more uniform flocs about 2 mm in diameter, and increased the mean settling rate of floc particles. Also, the addition of fly ash produced denser sludges than those obtained with alum alone. Final turbidities were independent of fly ash particle size and carbon content. Optimum proportions of fly ash additive are given.

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

By R. Barany

The heats of formation of seven substances were determined by solution calorimetry. At 298.15° K, the heat of formation of lithium sulfate from lithium, rhombic sulfur, and oxygen was -343.1 ± 0.7 kcal/mole, and the heat of formation of lithium sulfate monohydrate from lithium, rhombic sulfur, oxy-gen, and hydrogen was -414.3 ± 0.7 kcal/mo1e. For the silicates, the heats of formation at 298.15° K from the elements were kaliophilite, -503.8 ± 0.5 kcal/mole; leucite, -721.6 ± 0,8 kcal/mole; eucryptite, -505,2 ± 0.6 kcal/mole; alpha-spodumene, -727.9 ± 0.9 kcal/mole; and beta-spodumene, -721.1 ± 0.9 kcal/mole. The corresponding heats of formation at 298.15° K from the constituent oxides were kaliophilite, -42.7 ± 1.1 kca1/mole; leucite, -42.8 ± 1.1 kcal/mole; eucryptite, -16.1 ± 0.7 kcal/mole; alpha-spodumene, -21.0 ± 0.7 kcal/mo1e; and beta-spodumene, -14.3 ± 0.7 kcal/mo1e.

Jan 1, 1966

By A. W. Deurbrouck

The Bureau of Mines analyzed 13 samples collected from three Randolph County coalbeds. The Peerless and Sewell bed samples were generally of metallurgical quality as received from the mines or could be easily upgraded. How-ever, the Lower Kittanning coa1bed samples proved to be quite inimical to upgrading to metallurgical quality.

Jan 1, 1966

By E. K. Kleespies

The Bureau of Mines demonstrated a technique for electrowinning titanium from titanium nitride and titanium dioxide. Titanium-nickel-copper metal solutions containing 26 to 61 weight-percent titanium were prepared by electrolyzing titanium nitride in molten mixtures of potassium fluotitanate) and sodium chloride or barium chloride and depositing titanium on nickel-copper cathodes. A titanium-nickel alloy was prepared by electrolyzing titanium dioxide in an electrolyte of potassium fluotitanate) sodium fluoride) and calcium fluoride and depositing titanium on solid nickel cathodes. This alloy contained 21 weight-percent titanium and had a combined oxygen-carbon content of less than 0.1 weight-percent. A compartmented cell confined the oxide feed near the anode and inhibited oxygen contamination of the metal.

Jan 1, 1966

By Richard F. Link

A statistical technique, useful to analyze assay and other data characterized by location in three dimensions, is described in this Bureau of Mines report. If present, trends in the data are defined for the purposes of improving ore estimation, predicting ore beyond existing workings, and aiding geological interpretation. The technique is to fit linear and quadratic polynomial equations to the data through the statistical method of regression analysis. The fitted linear equations have the geometric form of hyperplanes; the fitted quadratic equations have the geometric form of ellipsoids or elliptic hyperboloids of one or two sheets. To visualize these three-dimensional forms, contour maps of a series of plane sections through the fitted surfaces are plotted. Both the fitting of the polynomial equations and the plotting of the con-tour maps are done by electronic computer to facilitate calculations and to obtain accurate results. Computer programs are described in appendixes. Methods employed are illustrated by an example analysis) based on data from a part of the Fresnillo mine) Zacatecas, Mexico.

Jan 1, 1966

By Robert K. Koch

The Bureau of Mines investigated separating HF from HF-SiF4-H2O mixtures by passing the mixed gases through a sodium fluoride slurry in an airlift scrubber and forming a mixed precipitate of NaHF2 and Na2SiF6. The oven-dried precipitate was thermally dissociated in two stages. The first stage was carried out at 400° C and dissociated NaHF2 to NaF and HF. Condensation and analysis of the evolved HF proved it to be 97 to 99 weight-percent HF containing 0.79 to 0.99 weight-percent H2O and 10 to 93 ppm silicon. The second stage was carried out at 700° C and dissociated Na2SiF6 to NaF (for recycle) and SiF4. The quantity of HF recovered from gaseous HF-H2O-air mixtures decreased with increasing relative H2O concentrations. Air was beneficial when scrubbing extremely dilute wet HF gases. At HF partial pressures of 0.24 and 0.013 mm Hg in the scrubber entrance gases, HF partial pressures of 6.2 x 10-4 and 9 x 10-6 mm Hg were obtained, respectively, in the scrubber exit gases. Scrubber efficiencies were 99.7 and 99.3 percent.

Jan 1, 1966

By Oliver Q. Leone

Electrorefining tests using titanium-nitrogen alloys as anode material showed that no significant quantity of nitrogen was transferred to the cathode deposit. The nitrogen of the anode remained in the scale, and the titanium-nitrogen alloy was anodically insoluble in the electrolyte when the nitrogen content was 11 weight-percent.

Jan 1, 1966