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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 Garrett R. Hyde

Sintered yttria and sintered dysprosia can be used to make single-component thermistors having typical thermistor geometries and operable in the temperature range 500° to 1,200° C. However, at these temperatures, instability of platinum electrodes can contribute a slight aging effect if the thermistor is kept near 1,200° C for long periods. Typical characteristics at 500° C for an yttria disk thermistor 12 mm in diameter and 2 mm thick are a resistance of 12.4 megohms and a temperature coefficient of resistance of -3.8 percent per degree C. Typical characteristics at 500° C for a dysprosia thermistor of the same dimensions are a resistance of 1.84 kohms and a temperature coefficient of resistance of -1.6 percent per degree C.

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 Roy L. Wilfong

Surface area measurements were conducted on cadmium sulfide powders following thermal treatments at temperatures up to 500° C and treatment times up to 1 week. Thermal treatments at temperatures up to 300° C produced no significant changes in the surface area of the powders even after 1 week of exposure. At 500° C some decomposition of the cadmium sulfide occurred.

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 James J. Olson

The Bureau of Mines recorded both particle accelerations and velocities from one-stick and production blasts at Eagle-Picher Industries' Shullsburg mine, Shullsburg, Wis., to test the effectiveness of square root scaling in grouping underground blast vibrations and to determine the effects of rock type and mine geometry on blast vibrations. Although the charge weights of subsequent delay periods sometimes exceeded the charge weight of the zero-delay period, both acceleration and velocity records showed that the zero-delay portion of the Shullsburg production blasts produced the highest vibration amplitudes. Because of the restricted range of charge weights in the Shullsburg experiments, no statistical determination of an appropriate scaling factor could be made. However, the square root scaled peak particle velocity data from the Shullsburg production blasts grouped well within the approximate band-width of vibration data obtained by the Bureau from quarry blasts in many different rock types. This indicates that scaling by some factor, perhaps the square root or cube root of the charge weight, may be an effective way to group and study vibration data from underground blasts. Further research is needed to determine which scaling factor is best for underground blasting.

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 Kenneth H. Johnston

Information on oil and water production, volume of water injected, core analyses, and well completion data was collected on 28 Red Fork sand water-flood projects for comparison and evaluation of results. An average water injection efficiency of 35 percent, an average water-injected to oil-produced ratio of 16.8:1, and an average loss outside the flood pattern of approximately 45 percent of the injected fluid resulted in an oil recovery to January 1, 1969, of only 5.6 percent of the pore volume, or 9.1 percent of the initial stock-tank oil in place. The principal causes of poor oil recovery from these projects are the losses of large quantities of injection water from the flood patterns through oriented, natural fracture systems or zones of high permeability and excessive channeling of injection fluids from input wells to oil wells. For more efficient operation and a higher percentage of oil recovery from the Red Fork sand and other low-permeability-sand waterflood projects, directional orientation of both induced-and natural-fracture systems should be determined during early development. The success of a low-permeability-sand waterflood project depends to a large extent upon the orientation of the injection wells with the fracture system.

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 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 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 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 E. E. Remmenga

Often a collection of analytical data, which should reasonably be expected to follow the normal distribution, contains too many extreme values, which the experimenter is inclined to eliminate according to some arbitrary procedure. The stepwise computer procedure described for this purpose is similar to many other truncation procedures; however, because truncation of a basically normal distribution causes a downward bias in the estimated variance, this procedure provides a graphical method to compensate for the bias.

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