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By B. J. Dalton

The Bureau of Mines Helium Research Center has developed a computer program for solving two-phase equilibria data for binary mixtures and for evaluating thermodynamic functions of interest, including all critical points. This computer program was used to calculate equilibrium points on the PVTu surface for the helium-nitrogen system as predicted by the Van der Waals equation of state. Numerical values are tabulated and illustrations are presented for 1,279 equilibrium points and for quantities needed to construct Ponchon diagrams. Equilibrium ratios as a function of pressure at constant temperature and of temperature at constant pressure-are also shown graphically. In addition, saturated partial molal volume and partial molal enthalpy data are given. It is shown that the Van der Waals helium-nitrogen system exhibits retro-grade condensation of the second type for liquid helium concentrations of about 0.07 mole fraction or less and pressures below about 45 atm. It is also shown that the critical point is at a -maximum value of pressure (at constant temperature) and of temperature (at constant pressure).

Jan 1, 1971

By Raymond M. Stateham

Microseismic noise rates and slope movements were measured in an unstable area along the north wall of the Tripp-Veteran pit, Kennecott Copper Corp., Ruth, Nev. Low-noise, wide-band microseismic geophones were located at various points in the wall, and the change in distance across open fractures, resulting from instability, was determined by repeated measurements between fixed points set on each side of the fractures. The microseismic noise rate increased and decreased with corresponding increases and decreases in the rate at which the fractures opened. The microseismic noise rates and changes in width of the fractures show excellent agreement, and the two types of measurements complement each other in monitoring the progress of pit wall failure.

Jan 1, 1971

By P. T. Brooks

Mineral nodules from the ocean floor represent a vast potential source of manganese, nickel, cobalt, and copper. Process development studies to devise methods for recovering these metals were conducted by the Bureau of Mines using two types of nodules--relatively low-grade calcareous nodules from the Atlantic Ocean and higher grade siliceous nodules from the Pacific Ocean. Ammoniacal carbonate leaching of reduced nodules appeared to have the best potential for processing the calcareous nodules, but the method proved to be impractical for recovering manganese. Extraction of 90 percent or better of the nickel, cobalt, and copper showed the technique to be attractive for recovery of these metals. The siliceous nodules appeared amenable to a process that starts with either a sulfur dioxide leach or a sulfation roast followed by a water leach to dissolve the soluble sulfates.

Jan 1, 1971

By F. P. Haver

Because of increasing concern with air pollution, the Bureau of Mines has developed a hydrometallurgical procedure to obtain elemental sulfur from chalcopyrite (CuFeS2) by means of the following reaction: CuFeS2 + 3FeCl3 ? CuCl + 4FeCl2 + 2S. Under optimum conditions, 99.6 percent of the copper and 71.6 percent of the iron were extracted in 2 hours from a typical mill concentrate containing 75 percent CuFeS2 and 15 percent pyrite (FeS2). At the same time, 68.2 percent of the sulfur in the concentrate was oxidized to the elemental form. The leach was highly selective; gangue minerals, including pyrite, were not attacked, thus accounting for the relatively low recoveries of iron and sulfur. To obtain these results, the concentrate was ground to 98.9 percent minus 325 mesh, and 300 grams was treated with 1 liter of boiling ferric chloride (FeCl3) solution. The FeC13/CuFeS2 ratio was 2.7. Cement copper containing 99.9 percent copper was recovered from the leach solution by cementation on sponge iron. Excess iron, dissolved during leaching and cementation, was removed from the stripped solution by crystallization. Ferrous chloride (FeCl2?4H2O), obtained as a byproduct, was converted to high-purity ferric oxide (Fe203) and HCI by an oxidizing roast. The hydrochloric acid was then electrolyzed to obtain chlorine, which was used to regenerate the leach solution. The leach residue, which contained ~50 weight-percent elemental sulfur, was treated with an organic solvent to recover the sulfur and cyanided to reclaim gold and silver.

Jan 1, 1971

By F. E. Joyce

The Bureau of Mines studied copper-nickel minerals (mainly sulfides) of the Duluth Gabbro Complex in north-eastern Minnesota to determine their response to selective high-temperature sulfatization techniques. The gabbro, containing 0.44 percent copper and 0.13 percent nickel, was ground to minus 325 mesh and sulfatized in a heated, rotating, stainless steel bench-scale retort. Tests demonstrated that over 95 percent of the copper and 80 percent of the nickel can be converted to water-soluble sulfates, depending upon the roasting conditions employed. Yield equations were developed using regression analysis for predicting the extraction of copper and nickel between the temperature limits of 520° to 670° C, the roasting time limits of 3 to 7 hours, and S02 limits of 10 to 40 percent in S02-air mixtures.

Jan 1, 1971

By Hillary W. St. Clair

This report describes an experimental method for determining parameters for the rate of reaction of CO2 with solid carbon. The method involves the simulation of a flow reactor by a mathematical model based on a hypothetical multistage reactor which permits calculation of the analyses of effluent gas and carbon consumed as functions of the flow rate and duration of the reaction. The method is applied to experimental data on the reaction of coke with CO2 in fluidized-bed and fixed-bed flow reactors. A method is described whereby two parameters may be determined simultaneously. The method involves a reiterative procedure that finds the values of the parameters that minimize the sum of squares of deviation between calculated and observed analyses of the effluent gas.

Jan 1, 1971

By C. Daniel Kealy

Finite-element,, mathematical models that solve LaPlace's and Richard's equations numerically were used to locate the phreatic surface within tailings pond embankments and to define the subsurface flow of water from the pond. Both must be known to design structurally and environmentally safe tailings dams. The permeability distribution within and beneath the embankment, the fluid potential values upgradient and downgradient from the embankment, and the geometry and elevation of an approximately impermeable layer at some depth beneath the embankment were used as computer inputs in analyzing over a dozen finite-element models of tailings dams varying structurally from simple to complex. Results predicted with the finite-element model were confirmed with measurements in a laboratory model of a tailings pond and in the field. Of particular importance to the design of safe slopes, all data indicated that the phreatic surface within a tailings dam is concave upward, a configuration opposite that in most earth dams. The close correlation between predicted and experimental values confirmed the practicability of using the finite-element technique to design safe tailings dams.

Jan 1, 1971

By C. Kenneth Eilerts

A method is described for controlling instability in finite-difference computations of liquid saturation near the borehole of a recovery well. Differences of pressure-and saturation-dependent variables are indexed offcenter, upstream and downstream alternately, to provide a stabilizing average. It was found that size of the time step could be increased by a factor of 4 without loss of numerical stability. Finite differences of the variables occur in a variety of relative numerical sizes and combinations. Those relationships of the differences that contribute to instability may be identified by the computing program in which they occur and modified to assist convergence of the computations and execution of the partial differential equations of liquid and gas flow.

Jan 1, 1971

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions2 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made, Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated the properties of zinc alloys containing 25 to 40 wt pet Al and 0 to 0.7 pet Mg. Microstructures, hardness, and tensile properties were evaluated for material as extruded at 285° C, solution treated at 300° to 400° C, and subsequently aged at 100° to 200° C. The alloys without magnesium are characterized by low hardness and strength with high tensile elongation and reduction in area. It was verified that magnesium effectively retards the Zn-Al eutectoid transformation below 275° C and markedly increases hardness and strength with decreases in ductility. Solution treating at 350° C results in large grain sizes and gross embrittlement. Subsequent aging of the Zn-Al-Mg alloys at 200° C restores ductility substantially and stabilizes the structures, but strengths are considerably reduced. Combined strength and ductility properties are better for the as-extruded condition than for any heat-treated condition. There is usually little advantage in overall tensile properties from increasing magnesium above 0.1 pct.

Jan 1, 1971

By L. M. Adams

Experiments in reclaiming acidic surface-mined coal lands with raw fly ash from bituminous-coal-fired powerplants were conducted by the Bureau of Mines at two sites in northern West Virginia. Plots at both sites were treated with varying tonnages of fly ash from three area powerplants and were planted with a variety of grasses, legumes, trees, and shrubs. Eight grasses and seven legumes were investigated. Greatest promise for growth under harsh soil conditions was shown by Kentucky 31 fescue, rye and red top grasses, and birdsfoot trefoil, a legume. Survival of trees and shrubs was negligible. Addition of fly ash to the spoil increased the pH to a range tolerable to some types of plant growth, improved the texture of the soil, and increased the available water of the resulting mixture.

Jan 1, 1971

By John Nagy

Data from experiments and literature on gas and dust explosions in closed vessels are presented to show the effects of the vessel size and shape; the initial pressure, temperature, and turbulence; and the fuel-air ratio and the strength of ignition source on pressure and rate of pressure rise. An attempt is made to correlate some of these parameters with an elementary mathematical model. Analyses of data on 17 vessels--spherical, cubical, cylindrical, and rectilinear in shape--ranging from 0,018 to 905 cubic feet in volume were made. Although the study was initiated to provide information primarily on dust-explosion phenomena, some data were obtained for gas explosions so that the factor of initial turbulence caused by the pneumatic blast used to disperse dust could be evaluated. The mathematical interpretation of the explosion phenomena was in general accord with the experimental data, and correlation was obtained for several factors affecting explosion development. Neither vessel size nor shape affected maximum pressure (when heat loss was neglected). The rate of pres-sure rise decreased as vessel size increased, and the rate was proportional to the ratio of the surface area of the vessel to its volume. Induced initial turbulence markedly increased the rate of pressure rise and slightly increased the maximum pressure. Changes in initial pressure produced proportional changes in maximum pressure and rate of pressure rise. Initial temperature and maximum pressure were inversely related, but initial temperature had little effect on the maximum rate of pressure rise. Comparative experiments showed no appreciable difference in explosion development of gas and dust fuels. The vessels and experimental work are described, and all data are given in tables. The mathematical model will facilitate extrapolation from laboratory to industrial conditions and will allow comparison of results obtained in different laboratories.

Jan 1, 1971

By Foster Fraas

Calculations based on data related to the electrostatic precipitator illustrate the variation in the electric forces on a particle with change in position in the ionized field. The feeble forces in some separators are explained by the low field intensity at midpoint locations between the electrodes. When the particles are in contact with the exterior surface of a rotating cylindrical electrode, a high field intensity at the electrode surface combined with the image charge results in large electric forces. The permissible feed velocity increases as the square root of the electrode diameter, providing high values in efficiency and feed rate capacity, particularly in surface-to-mass ratio separations such as are encountered in secondary materials recycling operations.

Jan 1, 1971

By Richard N. Spencer

This report describes investigations of the economic merits of multiple zone mining and beneficiation versus selective mining of altered Western phosphate rock. The same deposit was considered in both instances and it was assumed that the grade of selectively mined ore was comparable to the grade of the concentrate from beneficiation. The beneficiating scheme used for the investigation was one proved by small continuous circuit operation. All economic factors were found to favor multiple zone mining plus beneficiation. Capital requirements and production costs were lower, and production life of the deposit was extended 4.5 times. The concentrate from beneficiation would be a uniform high-quality feed for acidulation and would be low in stable metallic oxide (R203) content. Such a feed would permit improved plant operating control, and the low R203 would promote more rapid filtration and minimize sludge formation in the phosphoric acid. With the proposed treatment, the concentrate produced by flotation from this deposit would cost about 1.5 times as much per ton as the concentrate produced by classification sizing. Therefore, inclusion of a flotation step in treatment schemes requires an economic analysis for each ore deposit.

Jan 1, 1971

By Aarne Visnapuu

Dissociation and vaporization of gold chlorides and bromides were investigated by a static pressure method and by Knudsen cell mass spectrometer. Two distinct chlorine and three distinct bromine pressure-temperature relation-ships were observed for the respective salts. The chlorine pressures are attributed to the dissociation of Au2Cl6 and Au2C12, and the bromine pressures to the dissociation of Au2Br6, Au2Br4, and AU2Br2, These pressure-temperature relationships were used to calculate dissociation pressure equations, enthalpies, and entropies of dissociation for each salt. Mass analysis of the vapors over AU2Cls between 83° and 152° C confirmed the existence of gaseous AU2C16. Ionization potential of this molecule is 11.0±0.1 ev and enthalpy of vaporization is 28.l±2.0 kcal/mole. Mass analysis of the vapors over the gold bromides detected only Bra in the temperature range 15°-150° C.

Jan 1, 1971

By D. S. Burgess

A commercially available Halon 1301 extinguisher has been evaluated as part of an explosion-suppression system for use in coal mines. Studies were made both of the dispersion pattern of the Halon 1301 at an initial pressure of 280 psig, and of the efficacy of this suppressant against 9.5 percent methane-air flames. These flames were quenched successfully only when the suppressant was applied before the fireball diameter exceeded 18 inches.

Jan 1, 1971

By A. F. Baker

Laboratory flotation of synthetic coal-pyrite mixtures and high-pyritic-sulfur coal indicated that ferric chloride (FeCl3), aluminum chloride (AIC13), chromium chloride (CrCl3), and cupric sulfate (CuSO4) are potential pyrite depressants. For each metal salt there appeared to be a range of pH values and optimum concentration for selectively depressing pyrite in coal flotation. Pyrite was depressed in the pH range from 4.5 to 7.0 with ferric chloride, from 5.8 to 7.0 with aluminum chloride, from 6.4 to 7.1 with chromium chloride, and from 6.4 to 7.4 with cupric sulfate. Best separation of pyrite from coal was achieved in flotation solutions containing from 2 X 10-5 to 5 x 10-5 mole/ liter of each salt. In solutions containing excess salt concentrations, coal was also depressed. These Bureau of Mines tests demonstrated on a laboratory scale that, in solutions containing 4 X 10-5 mole/liter ferric chloride and from 1 x 10-4 to 2 x 10-4 mole/liter sodium hydroxide, the pyritic sulfur content of a Lower Freeport bed coal sample could be reduced from about 2.51 percent to less than 0.60 percent with recoveries of over 83 percent. The depression of pyrite appears to be due to the adsorption of positively charged colloidal metal hydroxide at the pyrite-solution interface. This hypothesis is supported by zeta potential determinations which showed that suspended coal and pyrite particles in solutions containing metal salts are positively charged in the pH range where depression occurs.

Jan 1, 1971

By W. K. Sawyer

Resistivity, porosity, permeability, and saturation data were obtained on core samples from the Big Injun, Clinton, Gordon, Bradford Second and Third, and Venango Second oil sands and formation factor-porosity relationships were derived using the general form of Archie's equation F = aø-m, where F is the formation factor, ø is the porosity, and a and m are constants that depend on characteristics of the rock. It was found that a and m varied significantly between sands, as did the exponent in the Archie relation I = Sw-n, where I is the resistivity index and S, is the water saturation. The average exponent, n, determined from all data was 50 percent greater at residual oil saturation than at residual water saturation. Samples from each sand exhibited differences in directional resistivity and/or permeability. The Bradford Third sand data showed correlation between resistivity and permeability anisotropy.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated the properties and anisotropy in properties of rolled Zn-Ti and Zn-1.0 wt pct Cu-Ti alloys containing up to 0.36 wt pct Ti. Finish rolling was at varied temperatures to total reductions as high as 92 pct. Alloy properties are very sensitive to various combinations of composition, rolling temperature, and reduction. Properly rolled Zn-1.0 Cu-Ti alloys are superior in strength to Zn-Ti alloys. Conditions are described that lead to best tensile properties. Creep resistance for Zn-Ti alloys decreases with increased rolling temperature when finish rolled to 92-pct total reduction: but not when finish rolled to 33- or 67-pct reduction. Creep resistance for 7n-1.0 Cu-Ti alloys improves with increased rolling temperature to about 480° F. Heavily cold-rolled Zn-1.0 Cu-Ti alloys have fine grain sizes and poor hardness, tensile, and creep properties, but high ductility. Thermal expansivity is markedly affected by the copper addition. Data show the anisotropy of tensile, creep, and thermal expansivity properties. Large idiomorphic crystallites of TiZn15 appear in both Zn-Ti and Zn-Cu-Ti alloys when more than about 0.2 pct Ti is present. A new Zn-Cu-Ti intermediate phase was also identified. Empirical equations are presented relating creep rates with major process variables.

Jan 1, 1971

By B. Dimitriades

Data on smog-forming reactivities of exhaust aldehydes are scarce. Such data were obtained by irradiating in a smog chamber typical exhaust aldehydes, individually and in exhaustlike mixtures. Observed reactivity manifestations were rate of nitrogen dioxide formation (RNO2) and yields of oxidant, peroxyacetyl nitrate, and formaldehyde. Results showed that exhaust aldehydes vary widely in reactivity. Formaldehyde showed high RNO2 reactivity but low oxidant yield; benzaldehyde, [m]-, and [p]-tolualdehyde were totally unreactive when irradiated individually; [o]-tolualdehyde was reactive. In mixtures, benzaldehyde manifested reactivity in terms of peroxybenzoyl nitrate yield. Exhaust aldehydes as a group are judged to be as reactive as the exhaust olefin group. The importance of the aldehyde contribution to exhaust reactivity and methods for assessing such contribution are discussed.

Jan 1, 1971