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By A. L. Service

In 1965 the Western phosphate industry ranked third after Florida and Tennessee in total mine and marketable production of phosphate rock and phosphate rock products. It has become an important regional industry and, since the close of World War II, it has become important in the national phosphate economy. This report includes an evaluation of the trends and outlook for the Western phosphate industry through 1975 as part of the Bureau's program to determine the rate at which the Nation's mineral resources are being utilized. The first part of this report is concerned with the relationship between the Western phosphate industry and that of the United States and the world. It describes the principal phosphate deposits and discusses production, export, and import of phosphate rock and marketable products. The second part of the report is concerned with the Western phosphate industry and discusses trends and outlook through 1975. Projections for the utilization of phosphate rock, phosphate fertilizers, and elemental phosphorus have been developed and extended through 1975 in an effort to provide data and information pertaining to the rate of depletion of the Nation's phosphate resources.

Jan 1, 1967

By Lowell Stroud

Ten natural gases containing from 0.023 to 8.4 percent helium were investigated. In seven high-helium samples, the isotopic abundance of Ne21 was greater than in the atmosphere, being supplemented by 33 to 85 percent of "excess" or "radiogenic" Ne21. The ratio of He4/Ne21(rad) in these gases was evaluated and found to vary between 2.9 x 107 and 5.9 x 107 , a factor of approximately 2. Argon concentrations were determined by the isotope dilution method. The isotopic ratios of Ar40/Ar36 in the high-helium gases were from 5 to 75 times the atmospheric value, with the Ar40 being about 80 to 99 percent radiogenic in nature. The ratios of He4/Ar40(rad) in all 10 gases were evaluated and found to range from 4 to 18. The isotopic ratio of N14/N15 in four of the high-helium gases was essentially the same as in the atmosphere; in three cases it was approximately 5 percent higher than the atmospheric value of 272.0. The genesis of nitrogen and the relationship of nitrogen to helium in natural gases were reviewed and are discussed in terms of a theory for the concurrent generation of nitrogen, helium, radiogenic neon 21, and petroleum (hydrocarbon gases and liquids).

Jan 1, 1967

By Adrian J. Mathias

This report presents the results of an investigation of a mine production-scheduling model and a critical path analysis for long-range mine planning. An example is given to illustrate how these techniques might be used to plan long-range development and production scheduling for a large underground mine. The model, based on estimated ore block grades and tonnages, and on designed mine development layout, simulates mining of ore blocks in a sequence necessary to fulfill mill requirements for ore tonnage and grade evaluation within pre-established system restrictions. Simulated production schedules are obtained as output from the model. These production schedules are then incorporated into a critical path analysis to determine the sequence for the long-range development work so as to fulfill the production schedules and thereby meet the ore grade and tonnage requirements of the mill.

Jan 1, 1967

By Charles B. Kenahan

The effects of ultrasonic radiation on the electrodeposition of copper-zinc, copper-cadmium, and copper-tin alloys from cyanide baths were investigated by the Bureau of Mines at frequencies of 18.5 and 38 kilocycles per second, and at acoustic intensities up to 0.5 watt per cm3. Significant changes occurred in the composition of the deposited alloys; some of these deposits were brighter, harder, more adherent, or of finer grain size than nonirradiated deposits. The irradiated deposits were also smoother and less porous, and they afforded better corrosion protection for the substrate metal in sodium chloride solution. The limiting current densities of the cyanide baths were increased by the application of ultrasonics. Anode and cathode current efficiencies also were increased, and cell voltages were lowered; the relationship of these effects to current density is discussed. Electrode potential measurements showed significant depolarization effects at both electrodes during ultrasonic irradiation. The resulting decrease in cell voltage was due chiefly to depolarization at the anode, and the anode became less passive.

Jan 1, 1967

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 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 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 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 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 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 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 A. Gene Collins

The Bureau of Mines undertook research to determine the bromide and iodide content of Mississippi and Alabama oilfield waters of the Tertiary and Cretaceous Period to determine genetic relationships of the ions, to determine their origin, and to determine their genetic relation to petroleum. The 280 samples were analyzed after a pretreatment to remove interferences. The iodide was oxidized to iodate and was titrated with thiosulfate. The bromide was oxidized to bromate and was determined iodometrically. A computer was used to calculate the correlation coefficients of iodide to bromide and to other ions. The other ions are sodium plus potassium, calcium, magnesium, chloride, bicarbonate, and sulfate. The mineral content of the samples ranged from 52 to 1,760 mg/l for bromide and from 2 to 65 mg/l for iodide. The mean bromide-to-chloride and iodide-to-chloride ratios were 0.0065 and 0.0002. The correlation coefficient matrix and linear plots indicated a definite bromide-to-calcium relationship for the brines investigated.

Jan 1, 1967

By Charles S. Allbright

This report describes hydrogenation of petroleum distillate fuels in bench scale equipment and the effects of hydrogenation on the storage stability and the composition of the fuels. Two distillate fuels were hydrogenated in laboratory equipment using a commercially available cobalt molybdate catalyst. Reactor temperatures were varied from 600° to 850° F and pressures from 100 to 600 psig. Product fuels were analyzed by ASTM, Bureau of Mines, mass, and infrared methods. Hydrogenation of a catalytically cracked fuel from Oklahoma crude oil significantly improved the storage stability, reducing insoluble gum formed during 9 months of storage at 110° F from 19.0 to 1.3 mg per 100 ml fuel, average. Conversion of the olefins to other hydrocarbon types varied with the temperature of hydrogenation--at 700° to 850° F the conversion was mainly to aromatics, at 650° F about 50:50 to saturates and aromatics, at 600° F principally to saturates. Processing a fuel composed of a mixture of virgin distillate and catalytically cracked stock, both from Illinois crude, at 700° F and 200 psig effected marked improvement in stability; the buildup of insoluble gum in storage was lowered from 18.3 to less than 1 mg per 100 ml fuel.

Jan 1, 1967

By E. G. King

The Bureau of Mines made experimental determinations of the heats of formation of forsterite and chrysotile at 298.15° K. The heat capacities of two polymorphs of serpentine, chrysotile and antigorite, were measured over the temperature range from 50° to 298° K and the entropies at 298.15° K were evaluated. The heat content of antigorite above 298.15° K was measured to 850° K. These thermochemical data were combined with other pertinent data to give heat and free energy of formation values at high temperatures. Free energy values are given for the reaction, forsterite + water = brucite + serpentine at different temperatures and pressures.

Jan 1, 1967

By V. R. Miller

The Bureau of Mines investigated methods for testing the tensile and sheer strength of cast specimens of bulk solder and of soldered joints in order to increase the strength and extend the useful temperature range of soft solders. A spread-area test for determining the wettability of solder on copper surfaces was developed. Mannitol was used as a flux in spread tests to control spreading and to avoid plating, etching, and other side effects of regular fluxes. Data on commercial and high-purity solders obtained by these methods show more consistency than those reported by others from similar tests.

Jan 1, 1967