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By K. C. Dean

Fine-sized mineral wastes discarded by ore milling plants require stabilization to prevent air and water pollution. Stabilization has been attained by physical, chemical, vegetative, and combination procedures. Vegetative reclamation is preferred to physical and chemical stabilization but is diffi¬cult to achieve because the wastes are sterile, contain deleterious inorganic salts, and lack the essential nutrients and physical characteristics required for sustaining vegetative growth. Methods now have been developed for attain¬ing vegetative growth on all but excessively acidic, basic, or saline tailings at costs ranging from $120 to $650 per acre. The cost for stabilizing tail¬ings requiring more intensive treatment techniques may range upward to $1,750 per acre. This report summarizes procedures developed by the Bureau of Mines and industry for vegetating amenable tailings, lists costs for the various processes, and suggests procedures that may be applicable for stabilizing saline and pyrite-containing tailings. Ridged planting beds, drip irrigation, and deep-furrow planting techniques are suggested for stabilizing saline wastes. A combination of mill tailings and sewage sludge can be used for pro¬ducing synthetic soils, and layers of sewage sludge buried under a layer of tailings offer promise of inhibiting acid formation from oxidation of sulfides in mineral wastes.

Jan 1, 1974

By Laurance L. Oden

The Bureau of Mines conducted corrosion tests of 18 commercial alloys in H3 P04 -phosphate rock or A1,03 slurry, in 10 pct HF, and in 25 pct H2 SiF6 to simulate three environments anticipated in a Bureau process to extract fluoride values from phosphate rock. Small alloy coupons were rotated in duplicate tests at 4.4 to 21 fps in the slurry at 170° C to determine rates of erosion-corrosion. At 4.4 fps the lowest rates, in mils penetration per year (mpy), were measured for Hastelloy C-276 (<20), Hastelloy B (30), and Inconel 625 (150);the rates increased at 21 fps to 55 mpy, 45 mpy, and 1,000 mpy, respectively. The corrosion rate for all alloys exceeded 40 mpy in either the equilibrium vapor or liquid phases of aqueous solutions containing 10 pct HF or 25 pct H2SiF6 at 100° C. Uniform corrosion in 10 pct HF at 50° C was observed only for Inconel 625 (22 mpy), Hastelloy C-276 (43 mpy), and Illium 98 (17 mpy). Inconel 625 (0.75 mpy), Hastelloy C-276 (1.3 mpy), Illium 98 (1.7 mpy), and Incoloy 825 (0.45 mpy) were attacked uniformly in 25 pct H2SiF6 at 50° C.

Jan 1, 1974

By John E. Kelley

A method for measuring the spark-shower radiance of metals when abraded on a grinding wheel was developed by the Bureau of Mines for evaluating the sparking tendency of metals. The radiance was measured in units of emissive power per solid angle per area of the detector. Over 100 metals were tested and rated relative to commercially pure iron. The metals tested included elemental metals, iron binary and ternary alloys, iron-carbon ternary alloys, commercial steels, nonferrous alloys, and a few hard-metal compounds. Some alloys were synthesized; others were obtained commercially. Alloys that possessed good strength properties were emphasized for selection. The results indicate that the spark-shower radiance of plain carbon steels and carbon alloy steels was greater than that of pure iron. Certain elements, particularly vanadium and chromium, reduced the sparking tendency of iron. Stainless steels and particularly nickel alloys displayed low spark-shower radiance. Some metallic elements had much lower radiance than iron; others, much greater. Plain carbon steels, heat treated to a variety of hardnesses, gave radiance values that generally increased with increasing hardness. The effect on sparking tendency of an increase in hardness of an alloy steel was studied. The sparking tendency increased with an increase in hardness to a maximum, then decreased with a further increase in hardness.

Jan 1, 1974

By L. E. Schultze

[The Bureau of Mines conducted bench-scale studies to develop techniques for stripping tetravalent cerium from tri-n-butyl phosphate solutions. Experiments were conducted in a constant-temperature bath using beakers and mechanical stirring. Ninety-five pct of the cerium was stripped from a 50-pct tri-n-butyl phosphate 50-pct kerosene solution containing 0.18 M cerium in 15 minutes at 50° C using 0.11 M aqueous formaldehyde.]

Jan 1, 1974

By H. V. Makar

The Bureau of Mines successfully demonstrated, on a pilot plant scale, a sodium sulfate (Na2S04) refining process for removal of copper from molten ferrous scrap. Previous tests established technical feasibility on a bench scale for achieving low copper concentrations and determining the principal factors controlling process efficiency. The pilot plant study involved a 1-ton arc furnace for melting ferrous scrap and a 1-1/2-ton treatment ladle. Results of these tests showed that copper removals obtained in laboratory tests (approximately 40 relative percent copper removal with 10 weight-percent surface addition of sodium sulfate) could be achieved on the pilot plant scale when excess carbon was added with the sodium sulfate compacts. Data were obtained on temperature losses and carbon consumption related to Na2SO4 treatment.

Jan 1, 1974

By Russell E. Griffin

Dielectric constants and dissipation factors were measured by the Bureau of Mines for 13 simulated lunar rocks over the 20-to 100-megahertz frequency range by means of the susceptance-variation method. Measurements were made at room temperature and normal atmospheric pressure. Results are presented and some comparison is made with data reported by others. The rocks used include a broad range of physical characteristics and chemical compositions from the large areas of volcanism in Oregon and northern California, and two nonvolcanic types. These rocks make up a suite of rock standards used by a group of laboratories engaged in lunar research. The data presented will add to the basic scientific and engineering knowledge needed to utilize extra-terrestrial mineral resources for support of future space missions.

Jan 1, 1974

The Bureau of Mines has successfully used sulfur hexafluoride (SF6) as a tracer gas to measure mine air flows under conditions where conventional methods have failed. SF6 was employed experimentally to measure accurately recirculation of return into intake air caused by leakage through an old stoped area, to check for potential leakage from an adjacent mine, to trace 10,000 cfm of "lost" air from an intake airway, and to measure transit air time through uranium mines. It proved useful as a means of accurately measuring airflow volumes in airways of large cross section and very low flow velocity, and in determining the recirculation resulting from underground cooling plants.

Jan 1, 1974

By I. A. Jacobson

In a closely controlled laboratory retorting system for oil shale, a relationship was developed by the Bureau of Mines between the temperature in the retort and the weight ratio of ethylene to ethane in the gases produced. Reciprocal temperature was shown to be directly proportional to the log ([ethylene]/[ethane]). From this relationship a number, called retorting index, was developed. The retorting index has the dimension of temperature, but its magnitude depends on both temperature and residence time for the reactants in the heated zone in the oil-shale retort. The slopes of the lines relating reciprocal temperature and the logarithm of the ethylene-ethane ratios are nearly constant for each of the retorting processes for which data have been presented. The retorting index should be a valuable tool to control the operation of oil-shale retorts, either aboveground or in situ. If an optimum operating condition can be established, the maintenance of the optimum or the departure from it should be easily monitored by use of the index.

Jan 1, 1974

By J. J. Cummins

The Bureau of Mines heated at 150° to 350° C for 0.5 to 360. days Green River oil shale that had been previously extracted by benzene to provide information on in situ processing conditions, to determine the effect of low-temperature heating on the unconverted kerogen, and to determine the composition of benzene-soluble thermal products. The methods used in determining the composition of the soluble thermal products consisted of fractionation of the soluble material, elemental analysis of the soluble products, fractionation of the polar resins by ion-exchange chromatography, gas chromatographic analysis of [n]-alkanes3 and mass spectral analysis of the branched plus cyclic alkanes and aromatic oils. The methods used to determine the effect of low-temperature heating on the unconverted kerogen remaining in the oil shale heated residues consisted of carbon-hydrogen analysis, volatile material determination, carbon residue determination, and oxidation rate determination. In general, it was concluded that significant increases in the degradation of kerogen to oil occurred between the temperature range of 250° to 350° C; that the composition of the soluble products depends upon the temperature at which they are formed; and that the [n]-alkanes are pyrolytically degraded from the kerogen structure. In particular, the 250° C heating temperature is beneficial to the formation of branched plus cyclic alkanes. Also, the heated and unconverted oil shale kerogen and the soluble thermal products become more aromatic as the temperature increases from 150° to 350° C.

Jan 1, 1974

By M. L. Whisman

The Bureau of Mines developed and tested in the laboratory several innovative techniques for reclaiming used lubricating oil. These processes included percolation through both chemically treated clay and ion-exchange resins, distillation through batch and continuous wiped-wall vacuum apparatus, treatment with solvent extraction systems, and chemical removal of impurities with chelating agents. In each treatment, the criteria of evaluation was oil recovery and reduction of acidic and metallic components. Both vacuum distillation and solvent treatment ranked high in their abilities to remove acidic and metallic components of the used oil with good oil recoveries. A combination of the two techniques gave the best overall results in terms of quality evaluations made by established bench tests. The methods were not ranked according to economic practicablity.

Jan 1, 1974

By J. J. Drost

The feasibility of basic oxygen furnace (BOF) offgas heat recuperation by preheating scrap was investigated on a pilot plant scale by the Bureau of Mines. In this study, offgases generated during the oxygen blowing of a molten pig iron and scrap charge were passed through a static bed of shredded auto scrap. Scrap quantities varying from 100 to 180 pounds and representing from 22 to 40 percent of the 450-pound BOF metallic charge were preheated in this manner. Average scrap bed temperatures of 1,650° F for 100 pounds of scrap and 1,150° F for 180 pounds of scrap have been achieved during the blows. As compared to cold scrap used in the normal BOF practice, it was found that by preheating scrap, usage could be increased by 43 percent. The thermal energy recovered by this preheating method can account for up to 44 percent of the energy necessary to melt the scrap.

Jan 1, 1974

By P. T. Brooks

A process for extracting 69 percent of the vanadium from weathered Nevada dolomitic shale containing about 1 percent V205 was developed on a laboratory scale by the Bureau of Mines. The process essentially is comprised of salt roasting, leaching with dilute sulfuric acid, solvent extraction, and precipitation of vanadium as ammonium metavanadate. Carbonaceous unweathered shale was less amenable to treatment. A preliminary cost estimate for mining and processing 1,500 tons per day of weathered shale indicated a production cost of about 1 dollar per lb of V205. Considering recent sales at nearly $1. 75 per lb of contained V205, larger scale testing to obtain more definitive process design and evaluation data may be warranted.

Jan 1, 1974

By Jack L. Henry

A laboratory and a pilot-plant-scale investigation has been conducted by the Bureau of Mines to examine possible sources of nitride defects in the production of magnesium-reduced titanium sponge. The production of alpha-stabilized nitride inclusions in hot-rolled titanium plate from air contamination of sponge during its manufacture has been experimentally demonstrated. Magnesium-reduced sponge prepared from air-contaminated magnesium or when contaminated by an air leak during reduction, vacuum distillation, or inert gas sweep, shows very large variations in nitrogen content. Refractory nitrides, delta TiN and epsilon Ti2N have been identified in this sponge. The highest incidence of inclusions resulted from sponge that was reduced by air-contaminated magnesium and from sponge subjected to air contamination during the vacuum distillation cycle and during helium sweep. Air contamination of sponge during the reduction cycle was not nearly as effective in producing inclusions. Tests showed that color and texture may not be reliable criteria for locating defects during sponge inspection. Maintenance of good vacuum-tight integrity, filtration of molten magnesium prior to charging into the reduction retort, and mechanical attrition of sponge to pulverize and disperse nitrides are suggested as practices to lower inclusion incidence in commercial titanium ingots.

Jan 1, 1974

By Jack L. Henry

The Bureau of Mines conducted seven pioneering experiments in a 12-inch-diameter Kroll reduction reactor to examine the feasibility of coreducing the chlorides of Ti, AI, and V to produce a homogeneous titanium alloy sponge. The coreduction studies proceeded in a normal manner, and the yields of sponge were comparable with those of pure titanium sponge made in the same reactor. Vanadium concentration was very uniform throughout the sponge cake when VC14 in solution in TiCl4 was fed into the molten magnesium. More difficulty was encountered in feeding solid VCl2 and AIC13. Vanadium and aluminum concentration in the sponge was not uniform, and mechanical difficulties were experienced with the small-scale screw feeder. Although the sponge varied in composition from region to region, the ingots prepared from it were uniform in composition.

Jan 1, 1974

By Russell R. McLellan

As part of an effort to develop new or improved placer mining technology in the Tertiary gold-bearing channel gravel of northern California, the Bureau of Mines conducted investigations at the old Badger Hill placer mine in Nevada County, Calif., to collect data and information regarding drilling and sampling methods and deposit characteristics. Sampling studies involved the collection and processing of 400 tons of large-and small-volume samples from drill holes, underground workings, surface pits, and blasthole rounds. A total of 355 samples averaging 2,296 pounds per sample provided reasonably accurate data for analysis of the gold distribution. These studies indicated that the bulk of the gold is within 40 feet of bedrock in stacked, lenticular zones of cemented gravel that are largely confined to the relatively narrow, meandering course of the deepest portion of the bedrock channel. Drilling studies involved the testing of truck-mounted rotary, buckett and vibratory drills, none of which proved to be a completely versatile tool for sampling quickly and reliably both consolidated and unconsolidated gravel..

Jan 1, 1974

By Mark I. Copeland

This study was conducted by the Bureau of Mines to determine the effect of steel reheating practices in burning natural gas on the amount of silicon required to prevent the formation of copper on steels containing up to 1 wt-pct Cu. Formation of copper, which causes surface hot shortness, was readily prevented by as little as 0.3 wt-pct Si and by 2 vol-pct excess oxygen in the furnace atmosphere when reheating steels containing up to 0.8 wt-pct Cu. Up to 0.8 wt-pct Si content and careful control of reheating conditions were necessary for steels containing 1 wt-pct Cu. Best conditions for these steels were reheating to 2,200° F (1,205° C) in burning gases containing 2 vol-pct excess oxygen, and then to higher temperatures in gases of 6 vol-pct excess oxygen. Slag and mold wash were not detrimental on steels reheated for 8 hr by a soaking-pit-type furnace schedule, but they were problematical on steels heated for 2 hr by a pusher-type furnace schedule. The effect of silicon contents on scaling rates also was determined.

Jan 1, 1974

By J. M. Stuve

Low-temperature adiabatic heat-capacity determinations were made by the Bureau of Mines in the temperature range from 5 to 300 K for the two crystalline modifications of zinc sulfide, sphalerite (ß) and wurtzite (a). The entropy at 298.15 K of sphalerite was evaluated as l4.02±0.04 cal/deg mole and wurtzite, l4.06±0.04 cal/deg mole.

Jan 1, 1974

By C. Melvin Lepper

The Bureau of Mines has developed an improved earth resistivity field system which employs a novel technique for obtaining null measurements. The instrument is designed to operate reliably in high-noise environments such as those found in the vicinity of operating mines. The system consists of a low-frequency transmitter, a sensitive receiver and an external battery pack, each in its own case to provide protection from the elements. The receiver and transmitter units have self-contained recharge-able batteries to supply power to the circuitry and separate built-in battery chargers that operate on standard 115 Vac power. The system is portable and simple to operate. Measurement accuracy, reliability, and dynamic range are superior to most commercially available equipment even though less time and effort is required to make null readings. Unlike some commercial systems, long integration times are not required to enhance signal-to-noise ratio in areas of high background noise.

Jan 1, 1974

By F. W. Wood

The Bureau of Mines has sought clarification of the Ti-TiN system by studying the phases formed by diffusion reactions between titanium and titanium nitride. Reaction couples were prepared by embedding pockets of TiN powder in arc-melted buttons of titanium. Specimens were vacuum annealed at nominal temperatures of 800°, 950°, 1,200°, and 1,500° C. Metallographically mounted cross sections from reacted specimens and from some that were not annealed were examined optically, with an electron microprobe, with an election microscope, and by X-ray diffraction. Each annealed specimen contained a segregated core primarily of d-phase material, an ?-phase diffusion layer, an a-phase diffusion layer, and host metal. On the basis of corresponding microprobe analyses, and considering results of certain other research, a new phase diagram is proposed. It contains no qualitative innovations, only quantitative adjustments. Results were also analyzed from the viewpoint of diffusion behavior. Diffusion coefficients calculated for the ? phase were sufficiently scattered that the parameters are very tentative. Nevertheless, the diffusion behavior reported is in reasonable agreement with one of two prior studies if it is assumed that the earlier investigators were mistaken in their identification of the nitride phase in which the diffusion occurred.

Jan 1, 1974

By H. G. Lucas

A feeder screw supplied at constant pressure by a hopper-orifice arrangement was developed for feeding solids in size ranges up to several hundred micrometers at constant flow rates. Performance of the feeder was evaluated by measuring the flow rates obtained with 3-to 7-micrometer coal ash, 70 percent through 200-mesh coal, and minus 325-plus 400-mesh coal ash. Constant feed rates within a few percent of set values were achieved for half-hour periods for the larger particles and for 5-minute periods for the finer particles. Suggestions are given for feedstock preparation and feeder operation for optimum performance.

Jan 1, 1974