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By Ernest A. Curth

The Bureau of Mines studied pressure changes in coal pillars by using encapsulated hydraulic pressure cells to measure relative changes in stress developed during mining. The data indicate that (1) abutment stresses were detected when the pillar line is within 42 to 100 feet, (2) vertical pressure increases as coal is mined in the pillars, (3) at first pressure is higher at the edge of the pillar than in the core, but as mining progresses, the higher pressure is measured in the core of the stump, and (4) in the two instances where lateral pressures were measured, they remained lower than the vertical pressures during pillar extraction. The data also indicate that the mean vertical pressure increase, 6P, in a pillar is roughly related to the percent of pillar extracted, A, by the empirical parabolic equation

Jan 1, 1967

By E. J. Murphy

The Bureau of Mines developed a fast, reliable modification of the Griess-Ilosvay procedure suitable for field analysis for NO2 in the fumes from explosives. Known concentrations of NO2-air mixtures were analyzed for the nitrous acid or nitrite formed in the reaction with three Griess-Ilosvay-type reagents by diazotizing and coupling. Comparison was made of the Rider-Mellon, Saltzman, and Patty-Petty procedures; the three procedures are in agreement if sufficient time of contact between NO2 and the reagents is allowed. In experiments to obtain an accurate factor for converting NO2 to nitrite, overnight contact was allowed in order to be sure conversion was complete. The factor was found to be 75 percent with a standard deviation of ±3.2. Low and erratic results were found using either the Saltzman or Patty-Petty reagents as absorbing liquids unless several hours' contact was allowed. If dilute NaOH solution was used as the absorbing liquid instead of a Griess-Ilosvay-type reagent, 92 percent of the overnight conversion factor was found after a 3-minute shaking time and a la-minute standby time. The Saltzman reagent was preferable for fieldwork with the dilute NaOH solution as the absorbent because of its easy application, rapid reaction, and intense color even at low NOB concentrations.

Jan 1, 1967

By W. H. Eddy

The Bureau of Mines made small-scale continuous tests and large-scale commercial plant tests of a calcareous fluorspar ore near Cave-In-Rock, Ill., to determine if the application of the lignin-fluoride process of fluorspar flotation would be industrially feasible for treatment of fluorspar ores, and also to compare the lignin-fluoride process with the quebracho process, which is the method currently used for concentrating calcareous fluorspar ores. The small-scale continuous tests yielded fluorspar concentrates analyzing 93.6 percent CaF2 with a recovery of 87.6 percent of the total fluorspar in the ore. In large-scale commercial plant tests, a fluorspar concentrate analyzing 93.3 percent CaF2 with a recovery of 78.0 percent was produced by the quebracho method. About 86.0 percent of the fluorspar was recovered in a metallurgical-grade fluorspar concentrate from the lignin-fluoride circuit which analyzed 89.9 percent CaF2? with a much simpler flowsheet than that in the current commercial application.

Jan 1, 1967

By D. K. Deardorff

The purpose of this work was to investigate the hafnium-carbon phase diagram. Alloys used to study this system were prepared from high-purity components by both consumable-and nonconsumable-electrode arc melting. Data for the diagram were obtained on the alloys by metallography, optical pyrometry, thermal analysis, heat treatment, and X-ray diffraction. The data indicate that a carbide compound occurs over considerable range of composition, and that one of each of the following types of reactions occurs in the hafnium-carbon system: Peritectoid, peritectic, and eutectic. The maximum melting temperature of hafnium carbide is 3,840° C at 49 to 50 atomic percent carbon, and the composition range of hafnium carbide at temperatures of 2,150° to 2,380° C is from 37.0 to 48.5 atomic percent carbon. The hafnium a-S transformation temperature is raised on alloying with carbon from 1,750° to 1,890° C, where a peritectoid reaction isotherm occurs. Alloying hafnium with carbon increases the hafnium melting temperature from 2,190° to 2,250° C, at which temperature a peritectic reaction occurs. Hafnium carbide and carbon react at 3,055° C to form a eutectic of 68.3 atomic percent carbon.

Jan 1, 1967

By F. A. Skirvin

Purification techniques were investigated for removing low-level metallic impurities from tungsten hexachloride. These techniques included distillation) fused-salt scrubbing) zone refining) and adsorption. Fractional distillation of tungsten hexachloride was found to be an effective purification method. The impurity levels of molybdenum) iron) nickel) copper) magnesium) and manganese were reduced to provide a tungsten halide sample which contained a total of less than 10 ppm detectable metallic impurities. Purification by fused-salt scrubbing of tungsten hexachloride in a lithium chloride-potassium chloride eutectic produced a hexachloride product which was of approximately the same quality as that obtained by distillation. Zone refining and adsorption did not appear to be as effective as distillation or fused-salt scrubbing.

Jan 1, 1967

By J. B. Zink

The Bureau of Mines developed a spectrochemical method to determine six constituents in coal ash in the following concentration ranges: silica 9 to 63 percent, alumina 7.5 to 35 percent, ferric oxide 2 to 30 percent, calcium oxide 1 to 29 percent, magnesium oxide 0.5 to 6 percent, and titanium oxide 0.5 to 4 percent. Samples of coal ash are fused with a mixture of lithium tetraborate and vanadium pentoxide. The resulting beads are crushed, mixed with powdered graphite, and briquetted. The pellets are analyzed spectrographically, using controlled high-voltage spark excitation. Vanadium serves as the internal standard. Effects due to matrix variations are minimized by fusion with lithium tetraborate. Intensity ratios of selected analytical lines are determined photometrically, Concentrations are read from analytical curves, prepared from synthetic standards, relating log intensity ratios to log concentration. A combustion procedure is used to determine sulfur tri-oxide. The method is most useful when large numbers of coal ashes must be analyzed but a high degree of accuracy is not essential.

Jan 1, 1967

By Elton L. Litchfield, Milton L. Weiss

Studies were made on the projectile impact sensitivity of explosives by subjecting explosive samples to the impact of metal projectiles fired from a 0.50- caliber gun . The projectiles , in the form of right cylinders , made plane surface to plane surface contact with the explosives . Pressures in the explosive were investigated with an expendable pressure transducer in some instances . The physical model of the projectile - explosive interaction describes , in principle , the duration of the peak shock pressure in terms of the projectile and explosive geometry and the steady- state penetration of the explosive . Of the explosives studied , liquid hydrogen- solid oxygen and liquid oxygen - solid or liquid hydrocarbon fuel were the most shock sensitive ( requiring an initiating shock of about 1.0 kb or 987 atmospheres pressure ) ; cast TNT was the least sensitive ( requiring an initiating shock of more than 110 kb pressure ) . Measurements of pressure in the explosive showed some moderate space resolution by the transducer and gave pressure distributions in agreement with expectations from the model of the shock processes . The appearance of the recovered projectiles and the calculated initiation shock pressures suggest that the solid explosives were initiated directly to high- order detonation , whereas the liquid explosives were probably initiated to low- order detonation-- with a subsequent , later transition to high- order detonation .

Jan 1, 1965

By Maurice Deul

A special short-term research project was initiated to develop plant design parameters for treating mine waters to yield an effluent acceptable for discharge into streams and a sludge amenable to effective and economic disposal. Neutralization was investigated to provide simple and direct treatment of ferruginous acid waters using lime; coarse limestone, and limestone followed by lime. Limestone treatment was accomplished using a small cement mixer as a simple reactor to provide abrasive agitation of limestone and mine water. Results from tests with nine mine waters encompassing a wide range of iron and acid concentrations showed that coarse limestone, one of the cheapest neutralizing agents known, is potentially useful for treating mine water discharges. However, process variables must be defined more completely before the practical applications and limitations of the process can be fully established. In all the tests a pH of >7.2 was obtained ultimately with limestone. Reaction time to reduce the iron content below 7 ppm in the water was dependent on the original ferrous iron concentration. For waters with high ferrous iron content, treatment with limestone followed by lime rapidly produced an acceptable treated water, Sludges with good settling and handling characteristics resulted when limestone was used for neutralization either alone or with subsequent treatment. Reaction rates are expressed graphically as pH change and iron depletion curves; characteristic solids settling curves are shown. The temperature dependency of ferrous iron oxidation was verified.

Jan 1, 1967

By Renpei Yoda

An investigation was conducted to develop columbium alloys with e1evated-temperature strengths higher than those exhibited by more common commercial columbium alloys, and attention was given to improving the oxidation resistance and ease of fabrication. Additions of carbon, aluminum, and chromium were made to some columbium-base alloys, and their effects on workability, recrystallization, oxidation resistance, and mechanical properties at elevated temperatures were explored. The additions were made to take advantage of (1) solid solution strengthening, and (2) precipitation hardening. Three alloys displayed good high-temperature properties with relatively good oxidation resistance at 1,000° C, and tensile strengths from 26,000 to 32,200 psi at 1,400° C. When the properties of these alloys were compared with those of commercial alloys, B-66 and FS-85 (1),4 the outcome was favor-able for the alloys studied in this investigation.

Jan 1, 1967

By W. S. Sanner

Seven samples were analyzed from the major reserves of the Bottom Red Ash bed, Northern anthracite field. The data show variations in thickness and geo-logic structure and in the amount of coal that can be recovered. Recovery of market-grade (less than 17 percent ash) coal is high for all samples, ranging from 76 tp 95 percent in the 3-1/4-by 9/16-inch sizes. The occurrence of coal containing less than 5 percent ash varies from 19.5 to as much as 57.5 percent. Crushing the coarse sizes to minus 9/16 inch increased recovery of market-grade coal in six of seven bed samples. Crushing released sufficient impurities to cause substantial increases in yield of coal containing less than 5 percent ash for all samples. Analyses of the float coal indicate that the quality of coal is comparable for all samples.

Jan 1, 1967

By Manuel Gomez

Low-temperature carbonization product yields for 129 coals representative of 12 Utah coalfields were estimated, using regression equations developed from heating value and proximate and ultimate analysis data. It was shown that yields of char, tar plus light oil, water of decomposition, and gas, as well as the gas volume and the heating value of the gas, could be predicted with reasonable accuracy. Published and experimental results from eight Utah coals carbonized at selected temperatures in the 4500 to 1,000° C range were used to determine the effect of temperature on product yields. Carbonization temperature, heating value) oxygen, and volatile matter of coal appear to be the principal variables influencing carbonization product yields. Data presented show that the heating value and the residual volatile matter in low-temperature char may be predicted using relationships developed from proximate analysis data for 220 coals.

Jan 1, 1967

By L. F. Heising

Ten composite samples of Mesabi Range nonmagnetic taconite from the Hibbing, Minn., area were evaluated by flotation and by reduction roasting-magnetic separation to determine their potential as a future source of iron are. Only one of the composites yielded concentrates that could be considered marketable, using as a criterion a 10-to-1 iron-to-silica ratio. Cursory petrographic examinations of all 10 composited samples and a detailed mineralogical study on 1 sample suggest that unfavorable mineralogical associations between iron and gangue minerals are responsible for their poor beneficiation characteristics.

Jan 1, 1967

By Karl-Heinz Frohne

This report presents the findings of a study of a portion of the Clover-Rush Run oilfield located in Roane County, W. Va. The study was made to investigate the possibilities of secondary oil recovery in the Big Injun sandstone underlying the William Kaufman lease. Reservoir properties, original reserves, and primary oil recovery are also presented. The investigation is based on a core analysis and related laboratory tests, well records, field production data, and subsurface information from the Kaufman property. A theoretical primary oil recovery of 9.7 percent of original oil in place is predicted for the reservoir. A waterflood performance prediction of a hypothetical pilot area was made by use of a computer. The prediction showed that, based on laboratory oil water relative permeability curves, the water-injection time needed to initiate oil production is excessive and that the stabilized water-injection and corresponding oil-production rates are very low. This precludes waterflooding the reservoir on an economic basis. A prediction for secondary oil recovery by gas injection was attempted but could not be completed because essential reservoir data were not available. In July 1965, the lease operator initiated, and is currently conducting, a gas-injection program, but there had been no increase in oil production up to November 1966.

Jan 1, 1967

By J. W. Town

Studies were made by the Bureau of Mines to determine the influence of textural features on the beneficiation of phosphate minerals (pellets) from selected bed and composite samples representing different rock types of the Western Phosphoria Formation. The particle size of the samples was reduced by attrition grinding to minus 20-, 28-, or 48-mesh depending on ore grade and gangue matrix. Sizing of the ground material showed that the phosphate pellets would concentrate in the plus 200-, 270-, or 325-mesh size fractions sufficiently so that the phosphate content was above the 31.5 :cent P2O5 required for acidulation. The phosphate content of essentially pure phosphate pellets was shown to range from 33 to 39 percent P2O5. Microscopic identification of the particles in each size fraction showed that the phosphate was either in the pellet form and readily liberated or so intimately associated with the gangue matrix that size reduction necessary Co obtain liberation was impractical.

Jan 1, 1967

By Glenn E. Johnson

The Bureau of Mines investigated the production of hydrogen cyanide by reacting powdered coal (minus 300 mesh) with ammonia at 1,250° C in a bench-scale study. Both metallic and ceramic reactors were used. Yields up to 0.7 cu ft of hydrogen cyanide per cubic foot of ammonia consumed r- obtained. The resulting ammonia conversion of about 75 volume-percent approximates conversion obtained commercially in processes utilizing natural gas and platinum catalysts. The coals that had higher volatile-matter contents gave the best yields of hydrogen cyanide. Allowing the coal to adsorb ammonia before reaction resulted in increased yields of hydrogen cyanide. Cost studies for a plant with a 40-million-pound-per-year capacity indi-cate that hydrogen cyanide can be profitably coproduced with carbon black, from coal and ammonia, at the current market price of hydrogen cyanide (11.5 cents/lb). These figures are based on heating the reactor electrically. If a cheaper heating method were devised the economics of the process would be more favorable.

Jan 1, 1967

By R. A. Guereca

The Bureau of Mines conducted an analysis to determine criteria for steady-state, laminar flow boundary conditions for a coiled-tube gas viscosimeter by comparing experimental data from a thick-walled, stainless steel capillary in a horizontal, straight-tube condition, with similar data taken after the same capillary was formed into a helix. Overlapping volumetric f10wrates and pressure drops are covered for both configurations at pressure levels of 28, 225, and 1,000 psia at 3000 K. Friction factor, Reynolds number, and Dean number correlation plots show conditions where the coi1ed-tube flow deviates from straight-tube flow. The coiled-tube data indicate departure from Poiseui11e steady-state laminar flow at a Reynolds number close to 390 and a Dean number of about 15. Below these conditions and consistent with the data reported, Dean's circulation appears negligible. For the particular coil used, a conservative upper limit of 10 is chosen for the Dean number corresponding to an upper limit of about 250 for the Reynolds number.

Jan 1, 1967

By William R. Hardwick

Present information indicates that a copper deposit can be safely fractured with a nuclear explosive and the copper successfully recovered by the in-situ leaching method. The process is not yet at the stage where it can be presented t ) the mining industry as a technique proven in all its aspects, but it is a method with high success potential. Unknown factors must be evaluated by a full-scale test before the economics or the extent of the use of the method by the mining industry can be predicted. Preliminary calculations indicate that the cost of fracturing a copper deposit nuclear explosives may range from l.8 to 55.2 cents per ton or in some case: less than a cent per pound of recoverable copper. Copper may be recovered at less cost than by conventional methods. Deposits with 4 pounds of recoverable copper may be economic and production from a deposit may begin in less than half the time required for conventional methods.

Jan 1, 1967

By Robert W. Ageton

Optimal planning for mining the deep, lead-zinc-silver deposits of the Coeur d'Alene mining district, Shoshone County, Idaho, could be facilitated by a knowledge of the magnitude and direction of the pressure acting in the virgin rock. The distribution of primary stresses should be considered in order to prevent possibly destructive mining-induced stress concentrations. This particular investigation was concerned with determining stress in a zone 4,000 feet below the surface and known to be ender stress concentrations due to mining operations. Disking of the stress-relief cores obtained in a vertical down hole permitted qualitative evaluation from visual observations; the results indicate that a high lateral stress existed at the time the measurements were made. Stress-ellipsoid determinations gave a compressive principal stress of -13,000 psi oriented about N 45° W and nearly horizontal, a compressive principal stress of -11,000 psi oriented about S 45° W and abut 60° off the vertical pointing away from the vein, and a compressive principal stress -5 -7,000 psi oriented N 45° E and about 60° off the vertical, pointing toward the vein. Subsequent to the overcoring stress-relief drilling, a rock burst occurred about 100 feet northwest of the test site.

Jan 1, 1967

By Robert M. Doerr

The purpose of the investigation was to determine the oxidation behavior of selected tungsten-cobalt alloys. Specimens of Wand W-Co containing 0.7, 1.7, 3.4, and 9.7 weight-percent Co were subjected to pure 02 at 1,000° and 1,100° K, and specimens of W-Co containing 29.8 weight-percent Co, at 1,100° K. Reaction kinetics were determined volumetrically. For specimens other than those containing 29.8 percent Co, the reactions proceeded at about a constant rate at either temperature, indicating the formation of a scale of constant protectivity; the reaction rates were essentially independent of the Co concentration. The scales on these alloy specimens consisted principally of WO3 and CoWO4. Specimens of a 29.8 weight-percent Co alloy, consisting primarily of the W6CO7 phase, oxidized with only slight deviations from the parabolic rate law at 1,100° K. The protective scale on these specimens consisted chiefly of Co3O4, CoW04, and W1 8°49; Co3O4 was outermost, and the W18O49 was adjacent to the alloy. The results suggest that the Co-rich outer scale inhibited the inward transport of 0 to an extent sufficient to greatly limit the amount of the nonprotective WO3 formed, so that protective W18O49 formed instead.

Jan 1, 1967

By Richard N. Spencer

Electric-furnace smelting for simultaneous recovery of zinc spelter and lead bullion from complex lead-zinc sinter was investigated. Reduction of lead and zinc was satisfactory. Condensation of lead and zinc vapor to pyrophoric metal powder in a water-cooled, shock-condensing system produced excellent recoveries. Metal-splash condensation to produce zinc spelter was unsatisfactory. Special smelting experiments differentiated the effects of several smelting parameters on zinc metal recovery. The principal cause for unsatisfactory zinc metal recovery was transfer of iron to the condenser and subsequent degradation of zinc in a mixture composed of lead and an iron-zinc intermetallic compound. Limitations of the process were determined. Slag-resistance open-bath electric smelting of complex lead-zinc sinter is not considered feasible.

Jan 1, 1967