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By Jr. Blake

This work was done to determine the technical feasibility of using the Pedersen process to produce cell-grade alumina and an iron byproduct from the high-silica and titania bauxites of the Pacific Northwest. Smelting of these bauxites with lime and coke at about 1,750° C in an electric arc furnace produced calcium aluminate slags in which at least 80 percent of the alumina was leachable by sodium carbonate solution. After a lime-desilication of the sodium aluminate leach liquors, neutralization of these solutions with carbon dioxide resulted in precipitation of an alumina hydrate of sufficient purity for calcination to cell-grade alumina. Recoveries of byproduct iron averaged over 90 percent; however, the iron contained about 1 percent phosphorous and would require additional refining. Additional small scale tests on these slags showed the following: (1) Titania had little effect on leachability if sufficient additional lime was added to form calcium titanate (CaO.TiO 2); (2) a slag containing about 14 percent silica required a slower cooling rate than one containing 7 percent silica for formation of high percentages of soluble aluminates; and (3) high-silica slags leached better at room temperature for long periods than at 65° C for shorter periods, but low-silica slags leached well by either method.

Jan 1, 1967

By R. F. Waters

Laboratory-scale selective volatilization methods developed by the Bureau of Mines to recover germanium and gallium concentrates from coal fly ash and phosphorus furnace flue dust are summarized. In the better experiments between 85 and 98 percent of the germanium was recovered as the lower oxide and as sulfides, and between 75 and 97 percent of the gallium was recovered as the lower oxide and as the trichloride. Grades of the condensates were inconsistent and varied between a few tenths of a percent and 8 percent, depending on the method used. In the primary extractions of germanium alone the degree of enrichment surpassed 100 to 1, and for gallium the best ratio was 30 to 1. Upgrading of condensates by vaporization retreatment and by leaching and precipitation is discussed. An appreciable degree of mechanical preconcentration by attrition scrubbing and elutriation was possible on two fly ash samples.

Jan 1, 1967

By J. F. Shultz

The Bureau of Mines investigated the hydrogenation of carbon monoxide and carbon dioxide over Raney nickel catalyst and nitrided fused-iron catalyst using both a single-pass and a recycle system. Activation energy over Raney nickel catalyst is 29 to 32 kcal/mole for synthesis from either CO or CO2, Pressure dependence of the gas conversion is to the 0.3 power for synthesis from CO and to the 0.5 power for synthesis from CO2. Nitrided fused-iron catalysts were tested using high recycle rates and 3H2+lCO, 2H2+lCO, and 1H2+lCO feed gas at 21.4 atmospheres absolute pressure. The relative usage of hydrogen (moles H2 consumed per moles Ha+CO consumed) was larger than in corresponding single-pass tests, and the relative usage of hydrogen approached the feed gas ratio monotonically as conversion increased. Activation energy was found to be 12 or 13 kcal/mole fresh feed gases of 3H2+lCO or 2H2+lCO. For single-pass operation the activation energy under the same conditions was 19 to 21 kcal/mole.

Jan 1, 1967

By G. G. Campbell

The Bureau of Mines in cooperation with Quaker State Refining Corp. conducted two underground-combustion oil-recovery experiments in the Venango Second sandstone in the Reno pool, Foster-Rena-Oil City field, Sugar Creek Township) Venango County, Pa.) to determine the applicability of the process for reservoirs producing Pennsylvania-grade paraffin-base crude oil. Tests were terminated when analyses of produced gas showed that a self-sustaining combustion front did not exist. It was thought that insufficient fuel had been deposited in the formation. Laboratory retort tests made after the second field test was concluded showed that crude oil from the Reno area would deposit enough fuel to support combustion if air flux, temperature, and time were maintained within defined limits.

Jan 1, 1967

By John R. Dudo

The Bureau of Mines Morgantown Petroleum Research Laboratory, with the cooperation of the Penn York Oil Company, cored the Dewdrop, Bradford Third, Lewis Run, and Sartwell sands in the Sartwell oilfield, McKean County, Pa. This report contains a review of the geology and depositional history of the field and an evaluation of the feasibility of secondary recovery of oil from the Bradford Third and Sartwell sands by waterflood or gas drive. Core analysis, geologic data, and electrical and radioactivity logs were used to evaluate the reservoir characteristics. Reservoir geometry, rock properties, fluid characteristics and saturations, and relative permeability-saturation relationships were used to assess the floodability of these two sands. The results of this study indicate that between 53,000 and 61,000 barrels of oil can be recovered by water or gas injection. The success of a waterflood or gas drive will depend on the field injection rates of the reservoirs comprising this oilfield. Following an economic evaluation, additional field work is recommended to further test the floodability of the reservoir.

Jan 1, 1967

By W. A. Calhoun

Progress made in a second and final metallurgical investigation made by the Bureau of Mines of near-surface Hawaiian bauxitic deposits from Kauai, Maui, and Hawaii Islands, and on a deeper deposit from Kauai, is reported. Previously reported Al2O3 extractions were increased by modifying conventional processes to fit the ore being tested. Increases in Al2O3 extraction were: Kauai, from 82.8 to 95.4 percent; Maui, 85.5 to 94.1 percent; and Hawaii, from 79.5 to 86.4 percent. Use of a "caustic-reduction sinter, leaching, and magnetic separation process" for Al2O3 extraction also produced an iron concentrate of commercial grade, except for titanium content. No successful method was developed for the recovery of a satisfactory titanium concentrate.

Jan 1, 1967

By A. F. Baker

The Bureau of Mines conducted pressure-drop studies in a 4-foot-diameter simulated blast furnace shaft to compare anthracite metallurgical briquets with coke and formcoke. The test materials were used alone, layered, and in mixed burdens of commercial fuel-to-ore ratios. Anthracite briquets had a higher pressure drop per foot than furnace coke, but they had a lower pressure drop per foot than formcoke. This appears to be due to packing and shape, as well as to particle size. The superficial air velocities at which beds of briquets and furnace coke disrupted were about the same. However, if briquets of the shapes and sizes tested are substituted for furnace coke in commercial metallurgical furnaces, higher blowing pressures will be required to deliver comparable amounts of air. Test burdens with more than 5 percent material smaller than 1/4-inch diameter showed significant increases in resistance to airflow.

Jan 1, 1967

By D. A. Elkins

This report is the second of a series of three that will evaluate, in order, the metallothermic, carbothermic, and electrolytic methods of magnesium production. The historical development of the carbothermic process is outlined. Production costs varying from 38.9 to 21.8 cents per pound of magnesium are estimated for different versions of the process. Additional suggested process modifications are listed. The technical and economic potential of the different versions are compared. Areas deemed most promising for future research on the process are delineated.

Jan 1, 1967

By R. L. Grant

The Bureau of Mines developed two new gap-sensitivity methods for explosives, and especially permissible explosives, to overcome certain disadvantages of the present routine half-cartridge method. The revised methods are based on the statistical up-and-down method and give more useful measurements of the 50-percent' gap values than the nonstatistical routine method. The new methods use full cartridges and incorporate certain physical improvements such as the use of cardboard tubes for containing the explosives and coal dust gaps to simulate actual mining conditions. A total of 60 samples of permissible explosives were evaluated simultaneously with the 2 improved methods and with the half-cartridge method

Jan 1, 1967

By W. S. Landers

Nine high-volatile bituminous Utah coals were carbonized singly and in blends with low-and medium-volatile bituminous coals. Of the 9 coals, 2 are in commercial use as the base coals in blends that produce industrially accept-able metallurgical coke, while 7 are regarded as weakly coking and are not used commercially in coking blends. The carbonization tests were made in a la-inch diameter, cylindrical retort, using 50-pound charges. Sunnyside coal blended with autogenous char generally produced larger and stronger coke than was yielded by straight Sunnyside coal. The volatile matter of the char and the concentration of the char in the blend appear to be important parameters influencing coke size and strength. A blend of 10 per-cent autogenous char of 7.2-percent volatile matter with Sunnyside coal yielded coke that was larger, stronger, and of higher apparent specific gravity than coke produced from an industrial coke oven blend consisting of 15 percent medium-volatile coal and 85 percent Sunnyside coal.

Jan 1, 1967

By R. A. Guereco

Accurate measurements of physical dimensions of a section of stainless steel capillary tubing are presented and used to develop two final working equations for an absolute gas viscosimeter. The effects of pressure and temperature on these dimensions are considered. The internal surface finish and nonuniformity of the capillary bore are discussed, as well as entrance, kinetic energy, gas slippage, and gas compressibility correction factors.

Jan 1, 1967

By Robert E. Barieau

General expressions for evaluating various thermodynamic properties applicable to the van der Waals equation of state have been derived. These formulas were subsequently used to evaluate various thermodynamic functions in the two-phase region. The results indicate that, for a van der Waals fluid, there is a finite discontinuity in the second derivative of the vapor pressure curve, in the second derivative of the chemical potential or Gibbs free energy at the critical point, and in the heat capacity at constant volume measured at the critical density. Numerical values are tabulated and graphs are presented for all functions calculated.

Jan 1, 1967

By T. Kessler

The purpose of this investigation was to evaluate the application of a spark-source mass spectrograph equipped with a spinning-electrode system for the study of various high-molecular-weight materials derived from coal. Conclusions from the investigation of anthracene, phenanthrene, chrysene, coronene, truxene, a coal-tar pitch (800 to 850 C softening point), and anthracene-chrysene synthetic mixtures follow: 1. Simplified mass spectra of anthracene, phenanthrene, chrysene, coronene, and truxene, from which the molecular weights were easily determined, were obtained by the spinning-electrode system. 2. Eight structural types having molecular weights from 178 to 252 corresponding to compounds previously observed in an electron impact mass spectrum of a coal-tar pitch sample were affirmed by this technique. 3. Mass spectra obtained from synthetic mixtures of anthracene and chrysene demonstrated that the technique is applicable for semiquantitative analysis.

Jan 1, 1967

By O. Terichow

A pendulum sclerometer designed by the Bureau of Mines is described. Its method of operation is given, along with the results of tests made on representative mineral samples of Mohs' hardness scale to determine the applicability of the device for research on rock testing. The sclerometer hardness values obtained from the tests indicated that reproducibility and accuracy were good. A quantitative comparison of the pendulum hardness values with microhardness and surface energy values published by other investigators showed good agreement on minerals with Mohs' hardness numbers of 2 to 9.

Jan 1, 1967

By W. H. Eddy

The Bureau of Mines conducted laboratory batch flotation tests and continuous pilot plant flotation tests on a complex calcareous fluorspar ore from Cave-in-Rock, Ill., to determine the technical feasibility of producing commercial-grade concentrates by the sodium fluoride-calcium lignin sulfonate-fatty acid method of concentrating fluorspar previously developed by the Bureau. The continuous flotation tests, treating about 150 pounds of ore per hour, produced fluorspar concentrates assaying 96.4 percent CaF2; 90 percent of the fluorspar was recovered.

Jan 1, 1967

By Joseph M. Singer

Having established that sodium chloride reduces the incendivity of explosives, the Bureau of Mines studied the effect of sodium nitrate in reducing ignition hazards. Gallery experiments showed that sodium nitrate reduced the incendivity of certain explosives to 8 percent natural gas in air but increased their incendivity to coal dust predispersed in air. Laboratory experiments using hot jets from explosions of stoichiometric mixtures of methane-oxygen-nitrogen showed that both sodium chloride and sodium nitrate reduced the incendivity to methane, to mixtures of coal dust and methane) and to coal dust. The difference between the gallery and laboratory results with respect to coal dust is attributed to temperature-time effects.

Jan 1, 1967

By Jr. Hazen

Two statistical techniques, the mean-square-successive-difference test and correlation, are used to investigate the problem of assigning an area of influence to an assay. Data from five hydrothermal deposits, Climax molybdenum, Cebolla Creek titaniferous iron, San Manuel copper, Piedra Hueca copper, and Butte copper, are studied. Two groupings of the assays are used for the mean-square-successive-difference tests. One group involves an increasing sample volume by reaveraging assays to represent a longer sample intervals, the other by regrouping assays to represent longer sample intervals without a change in sample volume.

Jan 1, 1967

By L. A. Neumeier

A refinement of the tungsten-cobalt phase diagram is presented for compositions to 85 at. pct cobalt and for temperatures to the solidus. Preparation of alloys by powder metallurgy methods is described, and the results of studies made by a combination of techniques involving microscopy, X-ray diffraction, thermal analysis, and dilatometry are discussed. The existence of u-W6Co7 is confirmed (rhombohedral D85 structure). The W6Co7 phase forms periectically at 1,685'115° C by reaction of liquid with primary W; the peritectic melt is at 71 at. pct cobalt. The homogeneity range of u-W6Co7 extends to both sides of the ideal stoichiometric ratio, through a compositional range of about 5 at. pct. The compositional limits for u-W6Co7 vary slightly below 1,471°±5° C, the temperature of the eutectic reaction forming u-W6Co7 plus a. The eutectic composition is at 79 at, pct cobalt. The existence of WCo3 is confirmed (hexagonal D019 structure). WCo3 forms peritectoidally at 1,093°±5° C by reaction between a and u-W6Co7 and exists over a narrow homogeneity range of 0.5 to 0.6 at. pct. The solid solubility of cobalt in tungsten is low (maximum 0,9 at, pct cobalt) and results in contraction of the tungsten lattice. Tungsten is extensively soluble in a-Co at higher temperatures; the a-Co lattice is expanded by the presence of tungsten in solid solution. There was no indication of the formation of a o-phase nor of any intermediate phases other than WeCo7 and WCo3. The WeCo7 and WCo3 phases are compared with similar phases in other systems.

Jan 1, 1967

By E. Morrice

High-purity neodymium, praseodymium, and didymium (a cerium-free mixture of light rare-earth elements) were prepared by electrolysis of the oxides in a medium consisting of the respective rare-earth fluorides and lithium fluoride. The metals were electrodeposited in the liquid state and collected as nodules on a skull of frozen electrolyte. Cells were operated from 1,000° to 1,100° C. The requisite temperature was maintained by passing alternating and direct currents through the bath. Graphite was used for the anodes and tungsten for the cathode. The metal products contained <0.02 percent each carbon and oxygen and <0.025 percent tungsten as major impurities. Analysis of typical didymium metal nodules showed an approximately twofold enrichment in neodymium and praseodymium over their respective concentrations in the cell feed. The lanthanum content of the metal was about one-half its content in the oxide.

Jan 1, 1967

By J. M. Singer

Methods are proposed for predicting concentrations of nitrogen oxides and carbon monoxide in the combustion gases of flames, specifically of lean, stoichiometric, and rich propane-air flames. Calculations are based on kinetic and thermodynamic theory. These theoretical data are compared with concentrations observed experimentally downstream of flat grid-type burner flames (approximately 25,000 Btu/hr) that were used to simulate gas appliances such as water and space heaters. Air pollutant concentrations are also computed for (1) flames chemically perturbed by recycling flue gases into the primary fuel-air mixtures; (2) flames thermally perturbed by cooling the burned gases at different rates; and (3) flames perturbed by combination of these two effects. In general, experimental and computed concentrations agree to within a factor of 2 to 7 with the experimental values always being higher than the theoretical. The theoretical analysis indicates that cooling the primary flame by recycling cold flue gases (with and without excess air) reduces the relative emission of nitric oxide and increases emission of carbon monoxide if the flame stoichiometry does not radically change. Cooling rates of about 5,500° to 10,000° R/sec starting at about 3,500° R generally suffice to prevent nitric oxide concentrations in lean flames from increasing much above the initial values at the combustion zone; these same cooling rates do not prevent oxidation of most of the initial carbon monoxide.

Jan 1, 1967