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By R. J. Heemstra

A method was developed for calibrating photographic emulsions and retrieving working curves for emission spectrography. The values obtained from a digital readout or a recorder chart of a comparator-microphotometer are converted to light intensity values using an emulsion characteristic curve derived from a quartic polynomial preliminary curve. The characteristic curve, consisting of Seidel transform versus the logarithm of intensity, is split into two cubic polynomials at the zero value of the transform, resulting in eight emulsion calibration coefficients. These methods allow use of the calibration curves even at very small and very high intensities, thus extending the range of analysis. Use of a small computer allows rapid calculations. A computer program was written to formulate, code, and file each working curve along with its statistical error. Proper coding of the input data permits the direct printout of the concentration of the elements under investigation.

Jan 1, 1970

By D. S. Burgess

An investigation of the hazard of spillage of liquefied natural gas (LNG) onto water is described. About 2,000 gallons of LNG were consumed in various tests. The initial vaporization rate of LNG following spillage was found to be 0.037 lb/ft2 sec; when the spill was confined, this vaporization rate was moderated after about 20 seconds by the growth of an ice layer on the water surface; when the spill was unconfined, a coherent ice floe was not observed and the vaporization rate was essentially time independent. The maximum diameter (in feet) of the spreading LNG pool was found to be given by 6.25 Wo 1/3, where Wo is the weight of LNG in pounds, Downwind of a natural gas source, time-averaged methane concentrations were given in good approximation by standard air pollution equations. However, peak concentrations were as much as twentyfold higher than average, adding an additional factor to the assessment of hazard. The effect of layering by the cold vaporized natural gas was similar to the effect of a temperature inversion on normal gases in the atmosphere. Small-scale explosions were observed on pouring LNG onto a water surface; no single explanation seems pertinent to all of the incidents observed.

Jan 1, 1970

By Frank G. Horino

This report presents a method of utilizing the Coulomb strength criteria for estimating the strength and stability of pillars and pit slopes containing planes of weakness. It is assumed that the Coulomb theory, as a special case of the Mohr envelope, is a satisfactory first approximation of failure in uniaxial compression or triaxial loading with low lateral loads. Accepting this assumption for brittle materials, an expression for the strength decrease of rock pillars containing a plane of weakness or fracture at any angle of orientation is derived. As few as six samples (three solid cores and three fractured cores at a failure-oriented angle) are required for testing uniaxially and triaxially to statistically determine the coefficients of friction and the shear strengths of both the solid rock and the fracture plane and the range of failure angles of the fracture plane. Interpretation of the data shows that the mean normal stress and maximum shear stress technique of analyzing the data is superior for solid core and that shear and normal stress values using angles of failure should be used for fractured specimens with failure-oriented angles. Plots of either the strength or strength ratios against fracture angles obtained from oriented drill core samples give a useful first approximation of strength decrease due to fracture. Using the same test conditions for both fractured and unfractured material increases the validity of the tests.

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 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 John P. Hansen

Batches of red or brown iron ore concentrates, weighing 100 or 200 grams, were reduced with gaseous reductants in a laboratory-sized fluidized-bed reactor. Using a loss of weight technique, the rates of reduction were measured and the effects of temperature, gas consumption, and gas flow rates were determined. Below about 725° C the rate of reduction was controlled by the chemical reaction at the reduction interface having an activation energy of about 10 kcal/g mole. Above about 725° C the rate of reduction appeared to be controlled by the flow of the gaseous reductant and therefore to be directly proportional to the flow rate. Above 725° C, hydrogen reduced the iron ore much faster than carbon monoxide. In gas mixtures, carbon monoxide or nitrogen reduced the hydrogen partial pressure and lowered the reaction rate proportionally. When present in large concentrations, carbon monoxide had a serious inhibiting effect on the reduction rate, probably owing to carburization and sintering of the reduced iron.

Jan 1, 1970

By Henry M. Harris

The roll forming of oxide powders was studied in a Bureau of Mines investigation to find the conditions and parameters required to make satisfactory ceramic strip. High-quality porous or dense alumina, zirconia, and porcelain shapes were made by sintering strip roll-formed at room temperature from powders containing minor amounts of binder and water. Strips with thicknesses of 0.04 to 0.08 inch and bulk densities from 40 to 90 percent of theoretical densities were made. The parameters most important to formability were particle size, condition of the powders, and roll gap. Other factors affecting quality were speed and surface condition of the rolls, amount and type of binder, water content, and sintering conditions. Ceramic strip was formed at rates up to 78 feet/minute, which is 13 to 23 times faster than reported by previous investigators, and forming was done in a simple and inexpensive roll unit. Reshaping the strip was possible by cutting, grinding, shearing, and stamping. The following innovations were developed that allow roll processing not normally possible with ceramic powders: (1) Fine-sized powders were made into strip by preparing these as partially sintered granules; (2) thick strip was formed by pressure feeding powders into the rolls; (3) flexible strip was made using a rubber-base bonding agent; (4) corrugated strip was formed on shaped rolls; and (5) porcelain strip was densified and reduced in thickness by rerolling while hot.

Jan 1, 1970

By H. J. Heinen

Malononitrile [CH2(CN)2J, which forms a carbanion in basic solutions, was investigated as a potential leachant for gold and was shown to be an effective extractant in alkaline pulps. Malononitrile was comparable to equal molar quantities of sodium cyanide (NaCN) in leaching gold from an oxide ore and yielded 10 to 20 percent higher recovery in leaching a refractory carbonaceous ore, although dissolution was slower with malononitrile than with cyanide. Complete recovery of the gold from the pregnant solutions was achieved by coprecipitation with a lead salt on zinc dust; the leachant was shown to be capable of regeneration and recycling a limited number of times. Addition of an anion-exchange resin to the carbonaceous pulp containing malononitri1e increased gold recovery from 67 to 95 percent. Some malononitrile derivatives were also shown to be gold solvents.

Jan 1, 1970

By Albert W. Deurbrouck

This Bureau of Mines report describes the washability characteristics of 13 coalbed samples collected in Colorado. Such data are needed to evaluate the quality of the coals of the West, where most of our low-sulfur-content coal reserves are found. Of the 13 samples included in this report, 11 had a total sulfur content of 1 percent or less. All of the samples contained low percentages of ash or could be readily washed to a desirable ash level with minimal loss of yield. The coals ranged in rank from high-volatile A bituminous to subbituminous B; nine of the samples were high-volatile C bituminous. The coalbeds ranged in thickness from 6 to 26 feet; the average was about 8 feet.

Jan 1, 1970

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 Paul Biggs

This Bureau of Mines report provides information on 138 waterflood projects in Wyoming. Injection was in 25 producing zones and 65 fields. Specific data presented include field location, discovery and development, water supply and injection, oil and water production, estimates of oil in place, and oil recoveries by primary and secondary methods. The 138 projects studied will, if successful, recover about 800 million barrels of secondary oil. Almost all of the injection water is from deep water wells.

Jan 1, 1970

By J. R. Ross

Recovery of uranium from slightly alkaline mine water, available in the Ambrosia Lake district of New Mexico, was studied using countercurrent ion exchange columns developed by the Bureau of Mines. Approximately 5 million gallons of mine water containing 9 to 12 ppm U308 was treated by ion exchange using a 14-inch-diameter absorption column composed of five or six compartments each 4 feet deep. Uranium recoveries averaged in excess of 98 percent at solution flows ranging from 15 to 25 gallons per square foot per minute and resin loadings up to 3.6 pounds of U.08 per cubic foot. In subsequent tests, loaded resin was continuously eluted in a countercurrent elution column with a diameter of 4 inches and containing a bed of resin 9 feet deep. The resin was eluted to a residual loading of less than 0.06 pound of U305 per cubic foot, at a resin-retention time of 224 minutes, using only 1.9 volumes of 1.1 M NaCl-0.05 M NaHCO3 solution per volume of resin. Compared with existing ion exchange practices for recovering uranium from mine waters in the Ambrosia Lake district of New Mexico, use of these improved ion exchange contactors would reduce ion exchange resin requirements at least 70 percent and allow further substantial reductions in capital and operating costs.

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 J. D. Marchant

Solid-state electrotransport of impurities in cerium, lanthanum, and praseodymium, using a pulsed current, was investigated. The results were compared with those of using a steady current. Impurities that showed appreciable movement with the pulsed current, but not with the steady current, were as follows: Molybdenum and oxygen in cerium, aluminum, iron, and molybdenum in lanthanum. The use of a pulsed current enhances the practical application of solid-state electrotransport to remove a wider variety of impurities from the host metals.

Jan 1, 1971

By K. P. V. Lei

An electrochemical process was developed for the preparation of vanadium from vanadium carbide. Commercially available vanadium carbide (V2C) was used as the starting material. Vanadium was obtained by electrolysis of the V2C in a BaCl2-KCl-NaCI-VCl2 electrolyte at 670° C using a helium-atmosphere, molten-salt electrolytic cell. Vanadium products were recovered with purities high as 99.6 percent. Current efficiencies of 87 percent and vanadium recoveries of 84 percent were attained. The cathode products were amenable to electrorefining to high-purity vanadium of 99.96-percent purity.

Jan 1, 1971