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By H. W. Leavenworth

Research was conducted by the Bureau of Mines to develop a technique to grow metallic fibers from a sulfide mineral. In this research, chalcopyrite (CuFeS2) was made sulfur deficient, and the remaining sulfur partitioned to the iron in the mineral to liberate metallic copper, or to the copper to liberate metallic iron. The metals formed on the surface as fibers and in the interior as spherical particles. Fiber growth is very fast. Lengths of 3 to 4 cm form in a matter of minutes, and the diameter of individual fibers is less than 1 µm. The mechanism of fiber growth is explained, and the reactions are reversible as predicted. Copper fibers can be made to grow from the surface at 400° C or to dissolve back onto the solid surface and be replaced by iron fibers at 625° C. Growth and dissolution can also be controlled to form copper/iron duplex fibers.

Jan 1, 1974

By H. E. Perlee

Mathematical expressions are derived for the histories of the pressure, flame radius, mass fraction burned, and burned and unburned gas temperatures associated with a spherical flame propagating concentrically in a spherical vessel. The equations are solved numerically for a 9.5 pct CH4/air mixture using the best available information for the burning velocity, expansion ratio, and specific heat ratio. Calculated histories are in complete accord with experimental measurements. The accuracy of calculated histories is determined relative to errors in the system parameters, and it is found that 10 pct errors in either the burning velocity or the expansion ratio results in a 40-pct error in the pressure history. A 10-pct error in either burned or unburned specific heat ratio results in a 22-pct error &apos;in the pressure history. It was further established that the usual assumption of constant specific heat ratio is unacceptable, but equating the burned and unburned specific heat ratios result in no apparent error in the histories. The cubic law (P = Kt3 + Po) is derived and discussed, and it is found that the law is valid only during the early period (P<2 atm) of flame growth.

Jan 1, 1974

By David L. Veith

Caustic scrubbing followed by silica flotation with cationic ether primary amine proved effective in upgrading commercial magnetic concentrates to supergrade products containing 2 percent SiO2, or less. Samples representing 41 million long tons per year of commercial magnetic concentrates from the Lake Superior region were tested by the Bureau of Mines. Bench-scale and pilot plant research indicated an estimated potential of 32 million long tons per year of superconcentrates to be available. Two pilot plant investigations yielded superconcentrates containing 1.1 and 1.9 percent SiO2 that were derived from commercial concentrates containing 7.0 and 4.2 percent SiO2, respectively. Corresponding iron recoveries were 90 and 93 percent at reagent costs of just over 33 cents per long ton of superconcentrates produced. Additional sources evaluated on a bench scale resulted in iron recoveries of 72 to 95 percent in products containing 1.7 to 2.0 percent Si02. Although reagent cost ranged up to 60 cents per long ton of superconcentrate, it is probable that these costs would be reduced in plant applications where benefits are derived from material and reagent recycle.

Jan 1, 1974

By C. C. Hwang

The Bureau of Mines formulated a method for calculating the concentration of entrained dust from a dust deposit by a turbulent gas stream. In particular, a diffusion equation is used to calculate dust concentrations in a channel following an explosion. Dust leaving the channel walls was treated as originating from stationary or moving, and single or multiple material sources. Formulas and sample computations for various types of dust sources in circular and rectangular channels are given, based on experimental entrainment rates. The analysis predicts the dust concentration as a function of time and channel space. The results appear to agree with the physical characteristics of explosion-driven dust dispersion in a O.6-m-diameter, 50-m-long explosion tunnel. The analysis is also applied to simultaneous and consecutive dispersion of coal and rock dust from simulated coal mine surfaces (walls, floor, roof, and ribs).

Jan 1, 1974

By G. J. Conroy

This Bureau of Mines study was initiated to determine whether or not a large-scale investigation of 400-Hz applications in coal mines was justified as a means of increasing safety in operations due to size and weight reductions in portable and other mining machinery. Potential uses for 400-Hz power in mining operations are explored, and cost and size comparisons with 60-Hz systems are made. The use of variable-frequency motor drive is suggested for conveyors. The conclusion was reached that there is no significant potential safety increase due to a general size and weight reduction, as the fact of such general reduction cannot be demonstrated.

Jan 1, 1974

By Gordon E. Fletcher

This Bureau of Mines report outlines the atomic absorption analysis of oilfield brines for barium, calcium, copper, iron, lead lithium, magnesium, manganese, potassium, sodium, strontium, and zinc, using the method of additions. The advantages of using atomic absorption are discussed. The method of additions was chosen to overcome large matrix interferences usually found in brines; techniques of overcoming chemical, ionization, and background interferences are also described. The method was used to analyze several hundred oilfield brines and found to be rapid and reasonably accurate. A solvent extraction method was used to concentrate lead, copper, zinc, and iron in low-level samples.

Jan 1, 1974

By A. R. Rule

A flotation process was developed by the Bureau of Mines for separation of carbonate and phosphate minerals occurring in unaltered phosphate ores of the Phosphoria formation. The process involves depression of phosphate minerals with fluosilicic acid and flotation of carbonate minerals with fatty acid emulsions. In individual laboratory tests, selective removal of carbonates was achieved with phosphate recoveries ranging from 60 to 80 pct P205. In continuous-circuit testing, sizing and separate treatment of coarse and fine fractions was necessary to achieve 65-pct P205 recovery. Concentrate grade ranged from 26 to 33 pct P205. The flotation tailings containing primarily carbonate and phosphate minerals is a potential fertilizer material. When reacted with H3P04, concentrated superphosphate containing approximately 40 pct available P205 was obtained.

Jan 1, 1974

By C. H. Elder

An analysis of the geologic structure of an area of Buchanan County, Va., was made by the Bureau of Mines using imagery from an airborne AN/APQ-97 side-looking radar system to evaluate that mapping technique for delineating structural features that may cause mining problems. Side-looking airborne radar (SLAR) was found to be a useful remote sensing tool for geologic structural analysis, Fault and joint systems identified by lineaments and linear patterns in the imagery were verified by surface and in-mine observations. Little Paw Paw fault was extended 10 miles by SLAR lineament analysis. A 22-mile fault, here named the Bishop-Bradshaw Creek fault, was mapped by lineament analysis and verified by observation of the fault on the Bishop Coal Co. mine map and on offset patterns of commercial gas production along the fault and surface observation of lineament along the fault. Three major super-imposed joint sets and several fault or fractured zones were identified by SLAR lineament analysis, showing more complex structure than earlier mapping indicated. SLAR imagery accurately delineated structural features that are known to affect gas migration and accumulation and that weaken the rock forming the immediate roof to mine workings, causing mining problems and potentially hazardous environment in the mines.

Jan 1, 1974

By R. B. Schluter

The objective of this Bureau of Mines investigation was to determine the effects of adding manganese compounds and ores to iron ore pellets. Manganese dioxide, carbonate, sulfate and chloride, plus six manganiferous ores from the Minnesota Cuyuna Range were tested as additives to increase the manganese content of iron ore pellets. One to 5 percent manganese, as a compound or ore, was added to five magnetite concentrates and one hematite concentrate. These concentrates were ballad, indurated (1,300° C), and tested for reducibility. Manganese sulfate and chloride were unsatisfactory additives causing cracking and degradation of the pellets during reduction. Manganese dioxide, carbonate, and the ores were satisfactory additives. The additives increased pellet compression strengths with a corresponding loss of reducibility, as compared to the pellets without manganese additions. The changes in compression strengths and reducibility were caused by the formation of Jacobite spinel and slag within the pellets. However, when the induration temperature was lowered from 1,300° to 1,200° C the reducibility and compression strengths were comparable to the pellets without manganese additions indurated at 1,300° C.

Jan 1, 1974

By P. B. Lorenz

Wettability measurements and laboratory waterflood tests were compared under a wide variety of conditions. Experiments were conducted with synthetic and natural crude oils, treated and untreated outcrop and oilfield sandstone cores, and synthetic brines with and without caustic, detergent, or phosphate additives. Measurements were made on equilibrated and unequilibrated systems at 77° and 150° F. Wettability was evaluated by the Bureau of Mines method from capillary pressure curves determined with a centrifuge. The waterflood data were fitted by empirical curves; the parameters of the curves characterize primary and subordinate production and also give the ultimate oil recovery. Results showed that wettability measurements at 77° F were useful predictors of recovery efficiency in waterflood tests run at both temperatures. Oil recovery in the early stages of waterflooding increased with increasing water wettability; however, the ultimate recovery was highest at a slightly oil-wet condition. The oil displaced at highest speed in the centrifuge was correlated with ultimate recovery in waterflood tests. Chemical additives to the brine sometimes lowered wettability and also sometimes improved waterflood recovery, but wettability and recovery were not correlated with additives present. The effect of additives on recovery in waterflooding was best seen in water-oil ratio curves.

Jan 1, 1974

By Andrew A. Cochran

Laboratory-scale research was conducted by the Bureau of Mines to develop a new process for treating electroplating and other wastes. Various acid and alkaline cyanide wastes were combined under controlled conditions to neutralize the wastes and to almost completely precipitate the metals and cyanides. The metals were subsequently recovered for recycling; the cyanides can also be easily recycled. The process was successfully used to treat the major types of electroplating and etching wastes, containing Cd, Cr, Cu, Ni, and Zn, and to treat both concentrated and dilute wastes. The economic aspects of treating concentrated electroplating, etching, and anodizing wastes are especially attractive because of the low cost of mixing two wastes, the high value of the recovered metals, and the simplicity of the recovery procedures. The filtrates from the waste-plus-waste step were relatively harmless compared with the original wastes and met Public Health Service standards for free cyanide content. Free cyanide ions were not detected in most of the filtrates; the limit of detection was 0.03 ppm. Only small amounts of HCN were produced during the neutralization; the HCN was collected and neutralized.

Jan 1, 1974

By Harold E. Marr

Energy dispersion X-ray analysis was evaluated for possible application in the secondary metals industries for the rapid analysis and identification of copper-base alloys. Laboratory investigations of standard brass and bronze samples indicate that X-ray methods are capable of separating standard alloys into 10 general classes with analytical times of less than 3 seconds per sample for clean, flat samples. A radioactive source of americium 241 with a secondary fluorescer was used as an excitation source, and a lithium-drifted silicon semiconductor detector was utilized for energy discrimination of X-rays.

Jan 1, 1974

By Everett A. Sondreal

Material and energy balances for stockpiled lignite were calculated by computer simulation techniques to determine the occurrence of spontaneous heating. Data on properties of lignite which affect spontaneous heating were required. In some cases, best values from reported data were utilized; in other cases, new data were developed. These include specific studies on the rate and conditions that influence oxidation, heat of oxidation, heat of wetting, specific heat, thermal conductivity, and permeability of stockpiles to air. These data are presented and discussed in detail for possible application to other studies. Results of computer simulations confirm past field experience on the storage of lignite containing as-mined moisture, and predict a greater risk of heat occurrence in stockpiles of dried lignite where experience is lacking. Successful storage was predicted for dried lignite of 20 pct moisture content, if it were cooled after drying and compacted to an interparticle void fraction of 9 pct (bulk density of 67 lb/cu ft) compared to 10 pet void fraction (72 lb/cu ft) for as-mined lignite.

Jan 1, 1974

By R. R. Schehl

The Bureau of Mines analyzed the structure of a high-grade metallurgical coke, carbonized at different temperatures in the range 500° to 1,000° C, through X-ray diffraction studies. Growth in the crystallite size with increasing coking temperature was calculated from profile analysis and compared with values obtained from the radial distribution function. The carbonization temperature appeared to have little influence upon the stack height, whereas the layer diameters more than doubled in size between 500° and 1,000° C. These results are comparable to those obtained from other studies of poorer quality cokes.

Jan 1, 1974

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 F. M. Carlson

Comparisons are made between the results of the Buckley-Leverett and Kern solutions, which describe immiscible displacement of oil by gas in a linear system and the results obtained from a less restrictive numerical model. This model takes into account the effect of compressibility of the oil and gas and the effect of allowing changes in the amount of gas in solution in the oil. These effects are best exemplified by imposing large pressure drops across the system. With these large pressure drops, comparison of the model solution with the Buckley-Leverett solution reveals that the Buckley-Leverett solution provides estimates of recoveries at breakthrough of the gas that are too low. In contrast to the model, the Kern solution predicts breakthrough recoveries that are too high. A modification to the Kern solution is presented to facilitate more accurate predictions of recovery at gas breakthrough for gas injection at pressures higher than the saturation pressure of the oil.

Jan 1, 1974

By R. H. Sprute

This report describes Bureau of Mines laboratory test results in electro-kinetic dewatering and consolidation of metal-mine mill tailings from five mines in the Coeur d&apos;Alene, Idaho, district. Classified (coarse) tailings, slimes, and unclassified material were separately tested. Tailings were placed in 0.3 ft3 plexiglass models, and dc potential was applied until dewatering ceased. Time-oriented measurements of water removal, changes in resistivity, and power consumption were recorded during the dewatering process. Moisture content and density of the dewatered material at test end indicated the method to be generally effective for all materials examined, but best results were achieved with well-mixed unclassified tailings.

Jan 1, 1974

By David E. Siskind

The Bureau of Mines has studied the fracturing produced in the vicinity of large-diameter blastholes in Lithonia granite. Cores were taken from the vicinity of AN-FO production blasts and examined using a total of seven laboratory and field measurement techniques to delineate zones of damage and evaluate the effectiveness of the seven diagnostic tests for fracture-state determination. Laboratory measurements of acoustic pulse velocity, porosity, permeability, compressive strength, and Young&apos;s modulus indicated the extent of fracturing with the acoustic techniques providing the best means of distinguishing between fractured and unfractured core. A severely fractured zone was found to extend approximately 25 inches (64 cm) from the center of the 6-l/2-inch blastholes, equivalent to 8 blast-hole radii. A second zone, characterized by a lesser degree of fracturing extended from 25 to 45 inches (64 to 114 cm) or 8-to l4-blasthole radii. Beyond 45 inches (114 cm) the rock was undamaged.

Jan 1, 1974

By D. J. MacDonald

Wettability measurements and laboratory waterflood tests were compared under a wide variety of conditions. Experiments were conducted with synthetic and natural crude oils, treated and untreated outcrop and oilfield sandstone cores, and synthetic brines with and without caustic, detergent, or phosphate additives. Measurements were made on equilibrated and unequilibrated systems at 77° and 150° F. Wettability was evaluated by the Bureau of Mines method from capillary pressure curves determined with a centrifuge. The waterflood data were fitted by empirical curves; the parameters of the curves characterize primary and subordinate production and also give the ultimate oil recovery. Results showed that wettability measurements at 77° F were useful predictors of recovery efficiency in waterflood tests run at both temperatures. Oil recovery in the early stages of waterflooding increased with increasing water wettability; however, the ultimate recovery was highest at a slightly oil-wet condition. The oil displaced at highest speed in the centrifuge was correlated with ultimate recovery in waterflood tests. Chemical additives to the brine sometimes lowered wettability and also sometimes improved waterflood recovery, but wettability and recovery were not correlated with additives present. The effect of additives on recovery in waterflooding was best seen in water-oil ratio curves.

Jan 1, 1974