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By Joseph L. Condon

Fifteen shots of three explosives with charge weights of 0.52, 1.1, 3.1, and 5.1 kilograms were fired in a pond to study the seismic effects of detonating explosives in water. Shock pressures and bubble periods were measured with pressure transducers in the water. Vibrations were measured on land in three orthogonal directions with particle velocity gages. Statistical tests indicated that a charge weight exponent of 0.43 best scaled the data. While shock pressures and bubble periods showed considerable differences in explosive performances, the amplitudes of ground vibrations showed less difference, and one prediction equation was therefore derived to estimate vibration amplitudes from all the explosives.

Jan 1, 1970

By H. R. Babitzke

As part of a continuing project to develop refractory metal alloys for high-temperature structural applications, the Bureau of Mines applied solid solution and precipitation strengthening techniques to improve the properties of columbium alloys. The purpose was to investigate the effects of hafnium, tungsten, and boron on the formability, strength, and oxidation resistance of columbium. The experiment was of factorial design with two replications which called for 72 ingots of 36 basic compositions, weighing 150 grams each. Hafnium, tungsten, and boron were evaluated at 3, 3, and 4 levels, respectively. Values of alloy content are all in atomic percent. The highest strength observed was 29,000 psi at 1,200° C for alloys Cb-15Hf (No. 3), Cb-7.5Hf-5W-2B (No. 14), and Cb-15Hf-5W-2B (No. 15). At 1,200° C, the ternary alloy Cb-15Hf-5W (No. 6) which has shown good properties in previous Bureau of Mines investigations was the most resistant to oxidation For boron additions, the alloys oxidized more readily with increasing amounts of this element. The fabricability of the alloys high in boron became increasingly difficult, resulting in an inadequate number of alloys required for a complete statistical analysis for all the tests. As a result of the decrease in ductility, an insufficient quantity of tensile samples were available for a proper analysis for the high-temperature strength data.

Jan 1, 1970

The Bureau of Mines performed cratering experiments in a homogeneous granite to test scaling laws for charge weights of 0.00476, 0.0220, 0.0900, 0.304, and 1.03 lb. Agreement among the data was best when empirical scaling exponents greater than one-third were assumed. Although the analysis showed that the best empirical scaling exponents were 0.37 for crater volume, 0.38 for crater radius, and 0.39 scaling for crater depth, all three crater dimensions could be scaled with a 0.38 scaling exponent.

Jan 1, 1970

By K. Thirumalai

This study forms a part of Bureau of Mines continuing research on thermal fragmentation of rocks. The potential of internal heating techniques for rock fragmentation is discussed. A concept of rock fragmentation with rapid inter¬nal heating of a localized inner volume of rock is advanced The energy required for rock fragmentation is made available by creating a required vol¬ume of localized heating. The fragmentation of rock using the proposed method is analyzed and qualitatively compared with the results of experiments with Charcoal granite, Dresser basalt, and Sioux Quartzite. High frequency dielec¬tric heating below 100 MHz is used in the study as an example to examine the working of the concept. The selection of operating conditions for the experi¬mental heating is explained. Fragmentation of Charcoal granite and Dresser basalt test rock blocks is achieved for localized heating below 550° C. The heated volume required for fragmentation is observed to be less than 2 percent of the test block volume and the electrical energy consumption is in the order of 3.5 to 6 5 kwhr/m3 The method offers a possibility for in situ fragmenta¬tion of rocks, favorable for internal heating. The method is highly dependent on rock properties governing internal heat generation The efficiency of dielectric heating in the experimental study is observed to increase with increasing dielectric loss of the rock material, ranging from about 10 percent in Sioux. Quartzite to about 50 percent in Dresses basalt

Jan 1, 1970

By W. S. Sanner

Pyrolysis (destructive distillation) techniques developed at the Bureau of Mines to determine the yield and quality of the products from coal were used to convert municipal (household) and industrial refuse into potentially useful solids, liquids, and gases without adding to environmental pollution. The tests demonstrated that a ton of municipal refuse can be converted into 154 to 424 pounds of solid residue, 0.5 to 6 gallons of tar, 1 to 4 gallons of light oil, 97 to 133 gallons of liquor, 16 to 32 pounds of ammonium sulfate, and 7,380 to 18,058 cubic feet of gas. A ton of industrial refuse, consisting of paper, rags, and cardboard, can be converted to 618 to 838 pounds of residue, 1.5 to 3 gallons of light oil, 68 to 75 gallons of liquor, 12 to 23 pounds of ammonium sulfate, and 9,270 to 14,065 cubic feet of gas. The energy from the gas is more than sufficient to provide the heat for the pyrolysis.

Jan 1, 1970

By Donald R. Johnson

Apparatus providing simultaneous differential thermal analysis, thermo-gravimetry, and evolved gas analysis, has been developed by the Bureau of Mines specifically for thermal study of oil shale and other solid, natural fuels. The apparatus is described in detail, and simultaneous analyses on a single sample of an oil shale mineral, nahcolite, and a thermal analysis demonstration compound, calcium oxalate monohydrate, are presented to demonstrate the instrument's capabilities.

Jan 1, 1970

By Harold A. Watson

A method for measuring leakage of vapors into a chemical-cartridge half-mask facepiece during simulated use is described. The respirator, fitted with high efficiency cartridges, is worn in a dichlorodifluoromethane (CC12F2)--air test mixture while a series of timed activities (facial movements, varied breathing, exercise, etc.) is performed. Complementing other tightness tests, this method is useful particularly for studying face fit and the effect of facial movements on leakage. The concentration of CC12F2 within the facepiece is monitored continuously to observe the immediate effect of physical activity on leakage. A composite sample is collected simultaneously in a plastic bag as a measure of average leakage during the 18-minute test period. Leakage, reported as percent, is calculated from the concentrations of CC12F2 within the facepiece and in the test atmosphere.

Jan 1, 1970

By Fred Leighton

The Bureau of Mines has developed rock noise source location techniques that may be used to obtain precise and practical source locations from micro-seismic field data. These techniques enable one to monitor all or any part of a rock structure and map progressive stress buildup or rock movement. Thus, the microseismic method of determining instability in rock structures is becoming an invaluable engineering tool for the mining or civil engineer engaged in rock excavation and construction.

Jan 1, 1970

By Basil Dimitriades

The roles of hydrocarbons and nitrogen oxides in smog formation were investigated by the Bureau of Mines. Samples of automobile exhaust with varying HC and NOx levels were irradiated in a smog chamber under conditions that resulted in smog levels similar to those observed in the atmosphere. Results were used to define the patterns that describe the dependence of a number of smog manifestations on HC and on NOx. Using these dependence data and some simplifying assumptions, estimates were made of the ranges within which HC and NOx must lie in order to obtain specified levels of air quality.

Jan 1, 1970

By Laurance L. Oden

The Bureau of Mines is developing melting data for binary combinations of the alkaline earth fluorides and yttria to facilitate the formulation of slag compositions. The present report deals with the CaF2-Y203 system for which solidus and liquidus temperatures and solid solubilities were determined. The information is presented as the phase diagram. All specimen compositions were blended from high-purity materials and encapsulated in Mo or Pt20Rh prior toheat treatment. Liquidus temperatures were determined by ceramographic examination of heat-treated and quenched specimens. Solidus temperatures were determined by differential thermal analysis and by electron microprobe analysis of quenched specimens. Terminal solid solubilities were derived by parametric methods. The peritectic system was found to be pseudobinary due to the formation of yttrium oxyfluoride at temperatures near the liquidus. The peritectic point occurs at 7 mole pct Y203 and 1,438° ± 5°C. The terminal solid solubility of Y203 in CaF2 decreases from 7 mole pct at 1,438° C to 1 mole pct at 1,100° C, and the solubility of CaF2 in Y203 decreases from 9.5 to 7 mole pct over the same temperature interval.

Jan 1, 1970

By John R. Zelonka

Models made by encasing strain-gage networks in epoxy are described and evaluated. With this technique relatively complex models can be constructed in which any number of gages can be located and alined precisely. Although the gages are an integral part of the model matrix, they create no important mechanical or thermal stresses. Model construction techniques and experimental data proved reproducible and reliable. In addition, the sGlution obtained with these models to the problem of the state of stress around a circular hole in a plate subject to a plane stress condition was in agreement with theoretical, photoelastic, and finite-element solutions.

Jan 1, 1970

By Frank G. Horino

This report presents a method of utilizing the Coulomb strength criteria for estimating the strength and stability of pillars and pit slopes containing planes of weakness. It is assumed that the Coulomb theory, as a special case of the Mohr envelope, is a satisfactory first approximation of failure in uniaxial compression or triaxial loading with low lateral loads. Accepting this assumption for brittle materials, an expression for the strength decrease of rock pillars containing a plane of weakness or fracture at any angle of orientation is derived. As few as six samples (three solid cores and three fractured cores at a failure-oriented angle) are required for testing uniaxially and triaxially to statistically determine the coefficients of friction and the shear strengths of both the solid rock and the fracture plane and the range of failure angles of the fracture plane. Interpretation of the data shows that the mean normal stress and maximum shear stress technique of analyzing the data is superior for solid core and that shear and normal stress values using angles of failure should be used for fractured specimens with failure-oriented angles. Plots of either the strength or strength ratios against fracture angles obtained from oriented drill core samples give a useful first approximation of strength decrease due to fracture. Using the same test conditions for both fractured and unfractured material increases the validity of the tests.

Jan 1, 1970

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 K. P. V. Lei

An electrochemical process was developed for the preparation of vanadium from vanadium carbide. Commercially available vanadium carbide (V2C) was used as the starting material. Vanadium was obtained by electrolysis of the V2C in a BaCl2-KCl-NaCI-VCl2 electrolyte at 670° C using a helium-atmosphere, molten-salt electrolytic cell. Vanadium products were recovered with purities high as 99.6 percent. Current efficiencies of 87 percent and vanadium recoveries of 84 percent were attained. The cathode products were amenable to electrorefining to high-purity vanadium of 99.96-percent purity.

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