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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 John Nagy

Data from experiments and literature on gas and dust explosions in closed vessels are presented to show the effects of the vessel size and shape; the initial pressure, temperature, and turbulence; and the fuel-air ratio and the strength of ignition source on pressure and rate of pressure rise. An attempt is made to correlate some of these parameters with an elementary mathematical model. Analyses of data on 17 vessels--spherical, cubical, cylindrical, and rectilinear in shape--ranging from 0,018 to 905 cubic feet in volume were made. Although the study was initiated to provide information primarily on dust-explosion phenomena, some data were obtained for gas explosions so that the factor of initial turbulence caused by the pneumatic blast used to disperse dust could be evaluated. The mathematical interpretation of the explosion phenomena was in general accord with the experimental data, and correlation was obtained for several factors affecting explosion development. Neither vessel size nor shape affected maximum pressure (when heat loss was neglected). The rate of pres-sure rise decreased as vessel size increased, and the rate was proportional to the ratio of the surface area of the vessel to its volume. Induced initial turbulence markedly increased the rate of pressure rise and slightly increased the maximum pressure. Changes in initial pressure produced proportional changes in maximum pressure and rate of pressure rise. Initial temperature and maximum pressure were inversely related, but initial temperature had little effect on the maximum rate of pressure rise. Comparative experiments showed no appreciable difference in explosion development of gas and dust fuels. The vessels and experimental work are described, and all data are given in tables. The mathematical model will facilitate extrapolation from laboratory to industrial conditions and will allow comparison of results obtained in different laboratories.

Jan 1, 1971

By George S. Koch

Several methods of calculating ore grades by diamond-drill sampling in the Homestake mine, Lead, S. Dak., have been evaluated by statistical analyses of assay data. The natural distribution of gold particles, partly masked through sampling and assaying procedures, is probably lognormal. As a consequence of the gold particles being clustered rather than randomly distributed within the ore bodies, (1) more mine samples are needed to obtain a specified precision of mean grade than the number predicted by the standard-error-of-the-mean law; (2) the variance of gold values is not inversely proportional to sample volume, and, therefore, small-diameter drill core yields samples nearly as good as larger diameter core; and (3) sampling at 5-foot intervals provides nearly as good results as sampling at shorter intervals.

Jan 1, 1971

By Aarne Visnapuu

Dissociation and vaporization of gold chlorides and bromides were investigated by a static pressure method and by Knudsen cell mass spectrometer. Two distinct chlorine and three distinct bromine pressure-temperature relation-ships were observed for the respective salts. The chlorine pressures are attributed to the dissociation of Au2Cl6 and Au2C12, and the bromine pressures to the dissociation of Au2Br6, Au2Br4, and AU2Br2, These pressure-temperature relationships were used to calculate dissociation pressure equations, enthalpies, and entropies of dissociation for each salt. Mass analysis of the vapors over AU2Cls between 83° and 152° C confirmed the existence of gaseous AU2C16. Ionization potential of this molecule is 11.0±0.1 ev and enthalpy of vaporization is 28.l±2.0 kcal/mole. Mass analysis of the vapors over the gold bromides detected only Bra in the temperature range 15°-150° C.

Jan 1, 1971

By D. S. Burgess

A commercially available Halon 1301 extinguisher has been evaluated as part of an explosion-suppression system for use in coal mines. Studies were made both of the dispersion pattern of the Halon 1301 at an initial pressure of 280 psig, and of the efficacy of this suppressant against 9.5 percent methane-air flames. These flames were quenched successfully only when the suppressant was applied before the fireball diameter exceeded 18 inches.

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 W. K. Sawyer

Resistivity, porosity, permeability, and saturation data were obtained on core samples from the Big Injun, Clinton, Gordon, Bradford Second and Third, and Venango Second oil sands and formation factor-porosity relationships were derived using the general form of Archie's equation F = aø-m, where F is the formation factor, ø is the porosity, and a and m are constants that depend on characteristics of the rock. It was found that a and m varied significantly between sands, as did the exponent in the Archie relation I = Sw-n, where I is the resistivity index and S, is the water saturation. The average exponent, n, determined from all data was 50 percent greater at residual oil saturation than at residual water saturation. Samples from each sand exhibited differences in directional resistivity and/or permeability. The Bradford Third sand data showed correlation between resistivity and permeability anisotropy.

Jan 1, 1971

By Martin H. Stanczyk

Freezing to dewater typical Florida phosphate rock slime as demonstrated in laboratory tests appeared to have potential commercial use because of indicated moderate energy requirements, good compaction of dewatered solids, and effective recovery of usable water. After freezing, thawing, decanting, and filtering, batch freezing of gallon-size 13.7 percent solids slime samples yielded 42 percent solids products. Cationic amine, used as a process additive, yielded 46.8 percent solids product with significant filter area reduction. Semicontinuous 8 stage freezing tests also produced thickened slimes. Cooling and freezing 13.7 percent solids slime from 30° to minus 10° C required removal of 183 Btu per pound of slime; Carnot cycle calculation indicated that the theoretical minimum energy to transfer this heat was 27.8 Btu per pound. To produce 1 ton of 44 percent solids slime from 13.7 percent sol-ids slime, the calculated theoretical energy required for cooling and freezing was 52.3 kilowatt-hours. During the research heat capacity and heat of fusion data were determined for the slime at various percent solids.

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 R. E. Meaker

Electrical conductivities and densities of molten fluoride systems were measured as functions of the melt temperature and composition. For any given mixture, the two properties change linearly with temperature. Three alkali metal fluorides were selected as solvents for melts of the type LiF-, NaF-, and KF-MFx, where M is a metal selected from the alkali metal or alkaline earth groups, or from the lanthanide or actinide series of elements, and x = 1-4. Heats of activation for conductance were calculated from the experimental data and varied from 2.3 to 9.2 kcal/mole at 1,000° C. Some relation between position in the phase diagram and the conductivity changes was suggested.

Jan 1, 1971

By W. F. Marshall

This report describes exhaust-emission data from 10 diesel engines: six 4-cycle, direct-injection, naturally aspirated engines; two 4-cycle, direct-injection, turbocharged engines; one 4-cycle, precombustion-chamber, turbo-charged engine; and one 2-cycle, direct-injection engine. These engines were tested over a 3-year period (1968-70). Lowest emissions were obtained with a precombustion-chamber engine. Emissions from the 2-cycle, direct-injection engine fell within the range of emission rates for the 4-cycle, naturally aspirated, direct-injection engines. Excluding the precombustion-chamber engine and excepting one of the 4-cycle, naturally aspirated engines, carbon monoxide emission rates were about the same for all engines tested. Test data on smoke, odor, and emissions of hydrocarbons, oxides of nitro-gen, carbon monoxide, and aldehydes are given.

Jan 1, 1971

By R. F. Abernethy

A small-scale method was developed for determining the free-swelling index of coal samples of limited quantity, especially the macerals. Results of a series of tests using a 0.3-gram sample correlated well with those by the standard method using a 1-gram sample. The standard and small-scale methods are modified to give unrestricted swelling for those coals having swelling index numbers above 7.

Jan 1, 1971

By J. M. Stuve

Calorimetric determinations of the low-temperature heat capacities, standard enthalpy of formation, and high-temperature enthalpies were made of (Na20)4 ?Fe20,(c). The resulting values of entropy (S°), enthalpy of formation (?Hf°), and free energy of formation (?Gf°) at 298.15° K are 104.676 cal/deg mole, -656.2 ±.kcal/mole, and -603.4 A kcal/mole, respectively. Tabulations of Cp°, S°, - (G°-H°298)/T, H°-H°298, ?Hf°, ?Gf°, and log Kf are given to 1,200° K.

Jan 1, 1971

In 1962 and 1963, two in situ combustion pilot tests were conducted in the shallow Second Venango sand near Reno, Pa. Because of poor oxygen utilization and lack of production response, both tests were considered failures and were terminated. The area was then relatively inactive until late 1966, when a development well drilled near the 1963 test site had surprisingly good production in what was considered to be a pressure-depleted reservoir. Other wells drilled in and around the old thermal pilot areas also came in as good oil producers. This report presents a study of the increased oil production from the Second Venango sand in the Reno area, and the apparent connection of the present production response and the old thermal pilot tests. Apparently combustion occurred in the Second Venango sand after the 1962 and 1963 experiments were terminated and, supported by large volumes of air left in the reservoir after the 1963 test, generated carbon dioxide which helped repressure the formation. This field evidence of combustion warrants another pilot experiment to further explore the use of properly designed in situ combustion techniques in increasing production from the Second Venango sand.

Jan 1, 1971

By L. A. Neumeier

The Bureau of Mines evaluated creep and other properties of extruded Zn-30 pct-AI alloys containing 0 to 0.7 pct Mg. The alloys were extruded both above and below the Zn-Al eutectoid temperature of 275° C. Creep behavior is defined for the alloys as extruded and after various heat treatments. Tensile properties, hardness, thermal expansivity, impact resistance, and microstructures are given. The alloys, either with or without magnesium, required substantially less pressure for extrusion near 275° C than at higher or lower temperatures. The alloys containing magnesium exhibited significantly greater hardness, tensile strength, and creep resistance, but much lower ductility than the 2n-30 pct Al alloy. The properties were very sensitive to the processing conditions.

Jan 1, 1971

By Robert E. Wood

[The temperature dependency of the low-density thermal conductivity coefficients, ?°T, of nitrogen, 100° to 1,200° K, is correlated with the Keyes' equation, ?T ½ -1 -12/T) WT = aT+ bT 10 The equation ?T,P = ?°T +a[ ]ß represented 509 experimental higher V pressure thermal conductivities in the temperature range 131.2° to 973.15° K for pressures to 500 atmospheres, with a mean absolute deviation of 2.35 percent. This equation was used to compute thermal conductivities of gaseous nitrogen for 47 pressures, 1 to 240 atmospheres, and 110 temperatures, 133° to 740° K, which are common to conditions encountered in Bureau of Mines helium purification processes. Isobaric heat capacities, CP, and viscosities, ?T,P, from previous work were combined with the present thermal conductivities, ?T,P, to compute Prandl1 numbers, C?T P / ?T ,P, of nitrogen. Tabular values of Prandtl num¬bers are presented for 49 pressures, 1 to 240 atmospheres, and 75 temperatures, 133° to 740° K. Estimated uncertainties are ±5 percent in the tabulated thermal conductivities and ±15 percent for the computed Prandtl numbers. However, the uncertainty may rise to ±10 percent for thermal conductivities and to ±30 percent for Prandtl numbers as the critical conditions of nitrogen are approached.]

Jan 1, 1971

By Lester J. Crow

A preliminary survey was performed to investigate the impregnation of relatively weak, porous volcanic tuff and a relatively strong, dense sandstone with five different monomers. Increases in compressive strengths by factors of 2 to 5, and elastic moduli by factors of 2 to 3.5, are reported for natural rocks (tuff., sandstone, dacite), which were impregnated with five monomers (methyl methacrylate; chlorostyrene; 40 percent TMPTMA-60 percent styrene; 40 percent TMPTMA-60 percent chlorostyrene; 60 percent polyester-40 percent styrene); polymerization took place after monomers were forced into the rock. Impregnation was performed (1) by pressurizing rock specimens from one end, or (2) by a vacuum-soak operation. Polymerization was accomplished by either radiation or chemical initiation techniques. Strength improvement is dependent on (1) the type of monomer used, (2) the amount of polymer incorporated into the rock, and (3) the degree of water saturation of the rock. Water saturation strongly reduced the effectiveness of the method for the polymer systems tested. The more viscous monomers (for example, 60 percent polyester-40 percent styrene) were more effective in displacing the water from the rock, and compressive strengths of wet rock were doubled with these systems. Water saturations ranging from 25 to 100 percent of maximum saturation gave essentially identical results. Further tests on other types of mine rock; including shale and coal, are planned. Water-compatible polymer systems should be developed, or present systems should be suitably modified. For application to tunnel stabilization, design studies evaluating the improvement in rock strength and its influence on the support system are also recommended.

Jan 1, 1971

By A. W. Maynard

Simple chemical spot tests for the identification of major alloying elements in aluminum-base alloys are described. The tests are suitable for use by nontechnical personnel working outside a laboratory. Tests for zinc, copper, manganese, and magnesium employ electrographic sampling methods and sample papers. Use of electrographic sampling in a test for magnesium in aluminum is made possible by using glass fiber filter paper. Differentiations between magnesium and magnesium-silicon alloys of aluminum and between aluminum-base and magnesium-base alloys are made by direct chemical solution tests. Description of a device for obtaining reliable electrographic samples is included. A sequence of testing for identification by alloy groups is given.

Jan 1, 1971

By R. D. Groves

Techniques were developed for preparing metallurgical-grade copper powder from industrially produced cement copper. Flotation was used for rejecting discrete gangue particles, acid leaching to remove residual iron and aluminum, hydrogen reduction to eliminate oxygen, sintering to consolidate the fine-sized copper, and grinding to obtain copper powder. Powders prepared from six different cement copper samples contained, in percent, 98.5 to 99.0 Cu, 0.10 to 0.05 Fe, 0.10 to 0.08 insoluble material and the remaining individual impurities less than 0.15 percent. The apparent density, flow characteristics, and other physical properties were suitable for powder metallurgy applications. An economic evaluation showed that this process was economically feasible. Processing costs appeared modest when considering that copper powder commands a price normally about 17.5 cents per pound over that of electrolytic copper.

Jan 1, 1971

By S. C. Schaefer

Thermodynamic properties of indium oxide (In203) have been studied with a high-temperature galvanic cell employing stabilized zirconia electrolytes. In the temperature range 790° to 1,230° K the free-energy change for the cell reaction 21n(1) + 3Cu20(c) = In203(c) + 6Cu(c) together with the standard free energy of formation of cuprous oxide gives the standard free energy of formation of indium oxide from the elements as ?Gf° = -218.78 + 75.34 X 10-3T ±0.7 kcal/mole. A third-law analysis yields the standard enthalpy of formation: ?Hf°298.15 = -221.5 kcal/mole.

Jan 1, 1971