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By Oleg Terichow

The Bureau of Mines studied the penetration of a slender cylindrical tube into a sand bed, simulating seafloor material under the application of a static load. The factorial experimental design was based on three factors: tube diameter, geometry of penetrating bit, and seawater saturation of sand, all of which were found to be significant in influencing the depth of penetration. The geometry of the penetrating bit, or shoe, is of major significance in the mechanics of penetration and should be considered the most important factor for additional study. Linear regression analyses of the load-penetration data show that the relationship is linear.

Jan 1, 1970

By Roy F. Abernethy

This report describes a method developed by the Bureau of Mines for the determination of beryllium in coal ash. Samples are put into solution by standard wet chemical procedures. Interfering elements are complexed with Na2EDTA, and the beryllium is separated by extraction of its acetyl acetone complex with chloroform or carbon tetrachloride. Final determination is made with Beryllon II.

Jan 1, 1970

By E. F. Ferrell

Electrowon molybdenum powders and a commercial hydrogen-reduced powder, all with different minor impurities, were investigated by the Bureau of Mines with respect to inherent properties, to fabrication techniques, and to proper-ties of the fabricated sheet. Compared with the commercial hydrogen-reduced powder, the electrowon powders had a larger particle size, a greater flow rate, a higher apparent density, and a lower oxygen content. Sheet materials prepared from the two types of powders showed similar mechanical properties, under the same conditions of heat treatments, except for low-temperature ductility. Yield strengths varied with carbon content, heat treatment, and test temperature.

Jan 1, 1970

By Alfred E. Schwaneke

A versatile torsion creep tester was instrumented with electromechanical and servomechanical components to operate automatically and unattended, producing digital printed outputs. The apparatus uses an electrical system for applying torsional stresses, and a unique angular transducer as a null detector operating a servocontrolled strain measuring system with the digital readout. The tester is designed to measure the creep in single-crystal or polycrystalline zinc, zinc alloys, magnesium, magnesium alloys, or other metals and alloys. Applied stresses may be varied from zero up to 2,000 psi in the outermost fibers of a 1/8-inch-diameter, 4-inch-long specimen. Strain readings to 0.001 degree, equivalent to a strain of 2.73 X 10-7, may be made automatically from one every 5 seconds to one per month. The apparatus has provisions for programed temperature control and special atmospheres or vacuum operation. A discussion of applications of the system to other mechanical testing apparatus is included.

Jan 1, 1970

By J. Grumer

The Bureau of Mines, under the sponsorship of the Space Nuclear Propulsion Office, conducted a laboratory-scale hydrogen safety study which determined several combustion characteristics of hydrogen diffusion flames. Experiments show that ambient air may enter the top of a hydrogen flare stack when the hydrogen flow is low. A new concept, supported by photographic evidence, predicts that diffusion flames burning in air on a wide, upright pipe (stack) and fed with slow, upward flows of buoyant gas will induce a downward flow of air along the walls of the pipe that can support combustion within the pipe. Predicted flamedip limits agree roughly with experimental values determined on 6-, 12-, and 18-inch-diameter stacks and increase with increasing stack diameter. Measurements were made of the limiting flow at which a hydrogen diffusion flame blows out in still air. By means of an empirical application of the critical boundary 8 velocity gradient concept, these data lead to a blowout limit of about 10 reciprocal seconds for a hydrogen diffusion flame. Burning rates of large hydrogen diffusion flames ranging from about 0.03 to 1 ft/sec were used to predict approximate flame heights on flare stacks. Temperatures of larger hydrogen diffusion flames up to about 3,600° F were observed, but the most representative value appears to be about 2,600° F. It was found that crosswinds do not strip significant amounts of unburned hydrogen from its diffusion flame and that water-cooled flare stacks are not likely to be damaged when flame is blown back into them by opposing winds.

Jan 1, 1970

By I. D. Shah

The Bureau of Mines investigated the sequence of principal chemical reactions taking place during the roasting of covellite (CuS). Practically all covellite is converted to digenite (Cul.SS) before oxidation to Cu20 begins. Part of the Cu2O is then converted to CuO, which in turn forms CuS04 through CuO?CuS04 as an intermediary. CuS04 and CuO'CuS04 decompose at 600° to 700° C to yield CuO and S03 (g) as final products. An overall mechanism is proposed for chemical reactions occurring at different interfaces of partially oxidized CuS pellets.

Jan 1, 1970

By J. E. Murphy

Purification of samarium metal by sublimation and by vaporization from a low-melting metal flux, at the same temperature, were compared. Vaporization proved more effective for removing impurities such as magnesium, calcium, and manganese. Recovery of samarium, however, is more rapid by sublimation because of its constant rate of distillation.

Jan 1, 1970

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 R. L. Wise

Heat content studies were conducted on burned shale, spent shale, and three grades of raw oil shale from the Green River Formation. Corrections were made for product enthalpies. The results were compared with previous work, indicating good agreement below retorting temperatures, but some differences at retorting temperatures. A general equation was developed relating heat content to oil-shale grade and temperature.

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 K. C. Strebig

The effect of some organic additives in diamond drilling of quartzite was investigated in the laboratory with a drill instrumented to measure the rate of penetration, the thrust, and the torque and to record each as a function of the distance drilled. A statistical plan was followed throughout the investigation, and an equation representing the bit performance was derived from the mathematical theory of reliability. The coefficient of friction in drilling increased with the use of additives, although the wear coefficient decreased. The decrease in wear associated with an increase in energy per unit volume consumed and the increase in penetration rate resulted in a net decrease in the cost per foot of drilling. A hypothesis explaining the effects achieved with the additives is given.

Jan 1, 1971

By Richard F. Link

The principal procedures for the statistical analysis of gold assay and other trace-element data depend on applying either the normal frequency distribution or the lognormal frequency distribution. The consequences of applying both methods are examined through reference to example data from United States and South African gold mines. It is concluded that for estimation of average grades, except for certain data with a very high coefficient of variation (ratio of standard deviation to mean), use of the lognormal distribution is ordinarily undesirable because bias may be introduced and little efficiency can be gained. However, if biased average grades can be tolerated, as in the examination of data from surveys in exploration geochemistry, use of the log-normal distribution may be desirable. Various statistical analyses are detailed, and the tables presented to implement the analyses are more complete than those previously published.

Jan 1, 1971

By E. J. White

Data from oil well logs and core analyses were used to quantitatively evaluate formation porosity and water saturation of heterogeneous carbonates and to study the pore geometry and performance characteristics of cores from these formations. Logs and cores from the Madison limestone from 233 wells in three fields in the Williston basin were used in the investigation. A comparison of log and core analyses shows that log porosities are consistently larger than core porosities, and the differences are correlatable with core porosity ranges. Water saturations from logs are usually smaller than the corresponding core saturations by summation of fluids, but the difference is attributable to mud filtrate invasion into the cores during drilling. Petrophysical studies show that the low permeabilities and high residual water saturations in these reservoir rocks are due to their fine crystalline texture and complex pore geometry (heterogeneity). It is concluded that both log and core analyses must be used for reliable evaluation of these carbonate formations.

Jan 1, 1971

By A. R. Taylor

Using solution calorimetry, the following heats of reaction were determined: (1) NaCN(c) + 1/Cu20(c) + 129H20(l) ? CuCN(c) + NaOH?128.5H2O ?H = -13.44±0.10 kcal/mole, (2) HCN(2) + NaOH?128.5H20 ? NaCN(c) + 129.5H20(l) ? = -2.52±0.02 kcal/mole. From these reactions, the heats of formation for CuCN(c) and HCN(2) were calculated to be 22.7±0.4 kcal/mole and 24.9±0.4 kcal/mole, respectively. Reaction 2 was made to check the consistency of literature values for heats of formation of HCN and NaCN. Adiabatic calorimetric measurements between 10° and 400° K showed the entropy and heat capacity of CuCN(c) to be 21.51±0.06 eu and 14.58±0.04 cal/mole deg, respectively, at 298° K. A broad anomaly in the heat capacity was found in the temperature range 285°-320° K. The heat of transition associated with this anomaly was less than 1 cal/mole, the sensitivity of the measurements.

Jan 1, 1971

By David P. Lindroth

The heat content above 25.0° C up to 1,000° C was measured for six rock types: St. Cloud Gray Granodiorite, Holston Limestone, Sioux Quartzite, Rockville Quartz Monzonite, Salem Limestone, and the basalt at Dresser, Wis. The calorimetric data were obtained with an isothermal jacket-copper block calorimeter. The experimental heat content data for each rock type are presented, along with specific heat data obtained from the temperature derivative of the heat content. For the six rock types the maximum deviations of the specific heats at a given temperature were within 10 percent below 575° C and within 34 percent above 5750°C. The increase in the values of specific heat range from a minimum of 13 percent for the basalt at Dresser, Wis. (temperature range, 100° to 1,000° C) to a maximum of 46 percent for Holston Limestone (temperature range, 100° to 870° C).

Jan 1, 1971