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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 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 M. J. Ferrante

The Bureau of Mines investigated the applicability of the freeze-drying technique for preparing dispersion-strengthened tungsten powders suitable for conversion by powder metallurgy into materials which might have improved high-temperature strength. Extruded rods from compacts of tungsten-5 vol pct thoria had at 1,650° C a tensile strength of 30,300 psi and a 10-hour stress-rupture strength of 12,700 psi, These are slightly below those measured for swaged rods of commercial tungsten-3.7 vol pct thoria. Only those tungsten-thoria dispersions containing a stoichiometric deficiency of oxygen yielded a significant strengthening effect. A low-melting eutectic formed in extruded tungsten dispersions containing either zirconia or yttria, which caused a lowering of the tensile strengths. These tensile strengths were only slightly higher than strengths of elemental tungsten made from commercial powder having a particle size of 2.4 microns (Fisher subsieve). Sheet made from this commercial tungsten had a slightly higher tensile strength than tungsten made by freeze drying, but the freeze-dried tungsten sheet had a lower recrystallization temperature, a lower ductile-to-brittle transition temperature, and a higher purity.

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 Robert M. Doerr

The research objective was to determine the effect of aluminum alloy additions on the oxidation behavior of cobalt-nickel alloys. Thirty high-purity alloys were reacted with 02 at 0.5 atm at 1,351°, 1,389°, and 1,429° K in a volumetric apparatus for about 300 min. The alloy compositions consisted of Co-Ni master alloys (0, 22, 50, 70, 91, and 100 wt pct Ni) with aluminum additions of about 0, 1, 2, 4, and 8 wt pet. Large early deviations from, or changes in, the parabolic rate constant were encountered, but in most cases, the reaction rate declined approximately in accordance with the parabolic rate law. A sharp peak in the parabolic oxidation rate constant was observed for specimens containing a to 22 percent nickel and 1 to 2 percent aluminum at 1,351° K, and the rate constants for these compositions were lower at the higher temperatures. Specimens containing 8 percent aluminum reacted far more slowly than did any of the others.

Jan 1, 1971

By Vance G. Leak

Leaching of manganese from low-grade Minnesota ores was studied over the temperature range 25° to 225° C at atmospheric and elevated pressures to demonstrate that good recoveries of manganese could be achieved from unroasted ores using reagents available nearby. Various combinations of ore, pyrite, lignite derivatives, and sulfuric acid were tested on a small scale. Pyrite alone required the highest temperature to effect a good extraction, but the combination of pyrite, lignite char, and sulfuric acid solubilized 99 percent of the manganese after 30 minutes of reaction at 75° C.

Jan 1, 1971

By Galen G. Waddell

This report describes a method of measuring and analyzing the initial deformation which occurs in the medium surrounding a mine accessway as the opening is created. Discussed are (1) the hypothesis upon which the research is based; (2) the in situ rock-deformation measuring equipment developed; (3) the field tests, consisting of measuring the deformation of the medium around two 4-foot-diameter raise bores as the boring progressed; and (4) a finite-element technique to correlate theoretical with experimental results, using elastic theory. Described also are the raise-bore operation and performance. The instrumentation developed proved to have the sensitivity and resolution necessary to measure rock deformation around a full-scale raise bore during excavation. Tests show the relationships of rock deformation to progress of the raise boring and to time. The initial deformation of the opening appeared to be elastic. Using the deformation records and an estimated field stress, the modulus of elasticity was determined for the rock mass. In addition, the importance of this type of measurement in assessing support-problem areas is discussed.

Jan 1, 1971

By Murray Jacobson

A method for determining airborne trona dust concentrations using a midget impinger was developed. During sampling, the trona dust, composed of sodium carbonate and bicarbonate, dissolves in the collecting medium (water). Resulting solutions are then titrated using 0.1 [N] hydrochloric acid solution. The mass concentration of the trona sample is determined from a calibration curve relating the volume of acid required for neutralizing a collected sample to the mass of the dust. Test results obtained using this method are equivalent to those obtained using a gravimetric sampling method.

Jan 1, 1971

By E. G. Davis

This report summarizes an investigation to determine the occurrence and recoverability of heavy minerals in sand and gravel operations in the Southeastern United States. A total of 61 samples from 34 sand and gravel operations in Alabama, Georgia, South Carolina, and North Carolina were studied. Heavy minerals, in amounts ranging from 3 to 400 pounds per ton, were found in all of the samples. Eighty percent of the samples contained 20 to 40 pounds per ton of heavy min¬eral. Valuable heavy minerals, in order of decreasing amounts, were ilmenite, kyanite, zircon, rutile, and monazite. Large-scale concentration tests were made on five samples from four major producers. Gravity concentration by Humphreys spirals and tables resulted in bulk heavy mineral concentrates that graded from 82 to 98 percent total heavy minerals. Mineral recoveries ranged, in percent, as follows: Ilmenite 60 to 95; zircon 96 to 100; kyanite 37 to 77; rutile 89 to 100; and monazite 96 to 100. Separation studies on the gravity concentrates showed they would respond to high-tension and high-intensity magnetic separation techniques to produce individual mineral concentrates. The recovery of each individual mineral from fractionation of the heavy mineral gravity concentrates, in percent, was: Ilmenite 77 to 94; rutile 41 to 68; kyanite 62 to 79; zircon 49 to 83; and rare-earth products, monazite and xenotime, 42 to 96. The grade of each mineral concentrate was: Ilmenite 51.1 to 68.7 percent Ti02; rutile 93.7 to 94.3 percent Ti02; kyanite 55 percent A1203; zircon 58 to 61 percent Zr02; and rare-earth products containing 73.8 to 90.8 percent monazite and 4.8 to 12.7 percent xenotime.

Jan 1, 1971

By Robert Blickensderfer

Tungsten alloys with high-temperature strength properties, comparable to the best of alloys recently developed by others, were produced by a new process called here the oxyreaction process. The process involved additions of a powder of a reactive metal compound, ZrN, ZrW2, or HfW2, to a base metal powder, tungsten, which contained some oxygen. The powders were blended, compacted, sintered, and extruded. During sintering, diffusion and internal oxidation occurred to produce reactive-metal oxide particles and solid solutions. A dispersion of oxide particles could be precipitated by heat treating. The oxyreaction process circumvents many of the agglomerating and coarsening problems encountered in the current methods for dispersing a stable oxide in a metal. Oxyreaction strengthening results from solid-solution strengthening and from dispersion strengthening produced by the reactive metal and its oxides. At a test temperature of 1,650° C, the alloys prepared from WW, had tensile strengths up to 70,000 psi and stress-rupture lives up to 142 hr at 10,000 psi stress; the alloys prepared from ZrN powders had tensile strengths up to 80,000 psi and stress-rupture lives up to 27 hr at 10,000 psi stress. Tensile strengthening in the alloys was attributed to Zr in solid solution or to Zr-O-W structures too small to be observed in an electron microscope replica. Stress-rupture life was attributed to a dispersion of submicron Zr02 particles which precipitated and grew to 0.05-to 0.2-micron size during the test. Tensile strengthening and stress-rupture life were dependent upon both the zirconium and oxygen contents with the maximum occurring at roughly 0.9 atomic pot Zr and 0.9 atomic pot 0. Studies of the details of the oxyreaction process were made on the W-ZrW2 alloys and three general steps were determined: (1) The reaction of 0 in tungsten powder with ZrW2 to form relatively large Zr02 particles; (2) the dissolution of remaining ZrW2 into the W matrix and partial internal oxidation to form ultrafine but sparse zirconium oxide particles and possibly to establish Zr-O-W structures; (3) the development of ultrafine Zr02 particles during high-temperature aging.

Jan 1, 1971

By P. G. Pigott

This Bureau of Mines laboratory research demonstrated that building bricks meeting ASTM specification C62-66 for grades SW and MW of FBS-type bricks can be produced from waste copper mill tailings. Waste tailings from accumulations at Magna, Utah, Anaconda, Mont., and Hayden, Miami, and San Manuel, Ariz., were dry-pressed into bricks, and the products were tested in accordance with ASTM Designation C67-66 on sampling, and testing of brick. An evaluation derived from pilot-plant production of similar brick at the Coal Research Bureau of West Virginia University indicated the production cost to be about $34 per 1,000 bricks. Utilization of such mill tailings on a commercial scale would eliminate the need for digging new pits for brick raw material production, conserve natural resources, and simultaneously remove potential sources of air pollution.

Jan 1, 1971

By J. A. Lamonica

The Bureau of Mines conducted an environmental noise survey to determine the noise levels to which underground coal mine employees are exposed, to evaluate noise survey techniques and equipment, and to compare noise exposures using two criteria, Walsh-Healey and CHABA, for determining allowable exposures that were under consideration for the Federal Coal Mine Health and Safety Act of 1969- Time study techniques and Bureau-approved standard sound level meters were employed. The shift exposures of 20 percent of the miners studied were in excess of the safe standards established by both criteria. The shift exposures calculated using the Walsh-Healey criteria were greater than those calculated using the CHABA criteria owing to the intermittent nature of the exposure. Ultimately the CHABA criteria were rejected, and the Walsh-Healey criteria were adopted.

Jan 1, 1971

By I. L. Nichols

The inplace cyanidation leaching of gold from placer deposits is a potential method for treating gravels too deeply buried and too low in gold content to be processed economically by conventional dredging methods. Laboratory experiments were made to evaluate those placer cyanidation factors adaptable to small-scale studies. The variables investigated included gold particle size and location in sand beds, cyanide solution flow rate, and cyanide solution strength as factors affecting gold solubility rates. The solution flow rate, in turn, was influenced by variables such as bed slope, solution head pressure, and sand size, and the effects of these factors were studied. Free gold, minus 150-mesh and finer in size, is rapidly dissolved by dilute cyanide solutions from mixtures of gold and silica sand prepared to simulate placer deposits. About 94 percent of minus 325-mesh free gold was extracted in 5 hours from silica sand mixtures, and 94 percent extraction of minus 150-mesh gold was obtained in 21 hours with 0.1 percent NaCN solutions. Moving solutions were almost twice as effective in leaching free gold from silica sand mixtures than stagnant solutions.

Jan 1, 1971

By H. R. Appell

The Bureau of Mines is experimentally converting cellulose, the chief constituent of organic solid waste, to a low-sulfur oil, All types of cellulosic wastes, including urban refuse, agricultural wastes, sewage sludge, wood, lignin, and bovine manure, have been converted to oil by reaction with carbon monoxide and water at temperatures of 350° to 400° C and pressures near 4,000 psig, and in the presence of various catalysts and solvents, Cellulose conversions of 90 percent and better (corresponding to oil yields of 40 to 50 percent) have been obtained. A continuous reactor for use at maximum conditions up to 500° C and 5,000 psig has been operated successfully, Using sucrose as a feedstock, operation in this system has permitted a simplified and preliminary chemical study of the conversion process. Oil yields of over 30 percent have been obtained with this unit.

Jan 1, 1971

By D. A. Wilson

A cyclic leaching process was developed for selectively leaching and recovering cadmium from nickel-cadmium scrap battery waste. The six major steps in the process are the following: (1) washing the plates to remove KOH electrolyte, (2) roasting at 550° to 600° C to oxidize metallic cadmium and decompose cadmium and nickel salts, (3) leaching with an ammonium nitrate solution, (4) precipitation of the leached cadmium from solution as cadmium carbonate using CO2 gas, (5) removal of CO2 from the lixiviator by adjusting to pH 4.5, heating, and evacuating the system, and (6) removal of small amounts of leached nickel from the lixiviator using a solvent extraction technique. The regenerated lixiviator is then recycled to leach additional plates. Cadmium extraction was 94 percent and the cadmium carbonate product contained 0.14 percent nickel and 0.12 percent cobalt impurity. The leached plates were smelted to a high nickel-low iron alloy with no detectable amounts of cadmium.

Jan 1, 1971

By R. A. Vik

The influence of thermal treatments on the grindability of low-grade hematitic iron ores from Michigan and Minnesota was examined in bench-scale tests. Treatment factors were roasting temperature, roasting atmosphere, and ore cooling conditions. Bond ball mill grindability and work indices were used as response indicators in evaluating the condition of the ore. Of the three treatment factors evaluated, roasting atmosphere, which brought about the con version of iron oxides to magnetite, had the most significant effect; roasting temperature had the next most important effect; and cooling condition had the least effect. Optimum grindability was obtained with reduced-quenched products of both ores at 650° C, near the alpha-beta phase transformation of quartz.

Jan 1, 1971

By R. L. Rough

Photoelastic, wire resistance, and borehole-deformation gages were used to measure the in situ strains when an outcropping Black Hand Sandstone Formation in Hocking State Forest, Hocking County, Ohio, was overcored to stress-relieve the surrounding sandstone. Strains transmitted to the photo-elastic gage did not produce isochromatic patterns suitable for quantitative analysis. Strain readings from the wire resistance gage indicated tensile-strain loading during overcoring; readings from the strain-gage bridges in the borehole-deformation gage indicated compressive-strain relaxation during overcoring. The magnitude and orientation of the computed stress fields obtained from both gages were comparable when the corresponding tensile and compressive elastic moduli were applied. Stresses computed from deformation and resistance gages at depths to 5 feet showed the maximum stresses to range from 1.042 to 2.121 times greater than the minimum stresses. The bearings of principal stresses calculated from the deformation gage readings varied between N 61° E and N 83° E; the wire resistance strain gage bearing computations varied between N 68° E and N 82° E. Measurements of in situ strain in sandstone were shown to have promise but to require further development in field technique that could likely be achieved through experience.

Jan 1, 1971

By P. R. Tisot

Structural response and/or deformation was determined for each of four different grade Green River oil shales (27.0-, 34.5-, 45.5-, and 63.5-gal/ton) as they were heated in an inert atmosphere, under constant compressive stress, from ambient to subretorting temperatures; that is, below those required for rapid pyrolysis of the organic matter. Small cores and small columns of confined fragments comprised the test specimens, which were heated, in a specially designed microunit, at a uniform rate either to 725° or to 825° F under three different stress levels, 80, 200, and 325 psi. Structural response of some cores was observed as they were heated in a stress-free environment. The obtained stress-strain-time-temperature relationships provide information regarding the oil shale's yield temperature, yield stress, rate of compressive strain, loss of mechanical strength, and nature of structural deformation. Effects of structural deformation on induced permeability in small columns of fragments are presented. Results indicate that underground retorting of Green River oil shale may be seriously impaired through loss of induced permeability brought about by structural deformation of rich oil shale under the influence of heat and compressive stress.

Jan 1, 1971