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By Robert C. Johnson

Single crystal whiskers of ZrO2 and TiO2 were grown by solution and crystallization of these oxides in molten baths. Mixtures of Na2B407 and LiC1 were the most suitable growth media for zirconia. Sodium borate alone and Na2CO3 plus SiO2 were best suited for titania. The solubilities of zirconia and titania in molten sodium borate were determined, Whether zirconia whiskers were dendritic or nondendritic depended on the temperature used. The best single crystal whiskers were grown below 1,100° C. Titania whiskers always grew as single crystals. The tensile strengths of zirconia and titania whiskers were about 15,000 psi and 50,000 psi, respectively. Modulus of rupture was about 49,000 psi for zirconia whiskers and 75,000 psi for titania whiskers. Chemical analyses showed the zirconia and titania whiskers to be pure. The zirconia and titania whiskers were shown by X-ray analysis to be, respectively, baddeleyite and rutile.

Jan 1, 1965

By W. W. Weller

Heat capacity measurements of anhydrous cobalt sulfate (CoSO4), copper sulfate (CuSO4), nickel sulfate (NiSO4), and zinc sulfate (ZnSO4) were conducted over the temperature range 51° to 298° K. The results were used to evaluate the following entropies at 298.15° K (cal/deg mole): CoSO4, 28.1; CuSO4, 26.8; NiSO4, 24.8; and ZnSO4, 26.4. Entropies were combined with heats of formation to give free energies of formation.

Jan 1, 1965

By J. E. Miller

Primary standard gas mixtures were developed for more accurate calibration of analytical instruments at the Bureau of Mines Helium Research Center and for calibration of analytical instruments used in the helium conservation program. A 10-kg-capacity balance is used to weigh a 4-kg metal cylinder filled to high pressure (1,800 psi maximum) with the component gases of the desired mixture. At 1,800 psi, a cylinder contains about 60 g of helium, or 420 g of nitrogen. An accuracy of ±0.05 mole-percent or better is claimed for each component in the mixtures.

Jan 1, 1965

By Thomas A. Morgan

The distribution of stress adjacent to each of 25 mine openings was determined by the borehole stress-relief method in the FMC Corp. Westvaco trona mine at Westvaco, Wyo. The purpose of the stress determinations was twofold: First, to study the effect on these distributions of various factors such as opening shape, stress level, and loading history; and second, to estimate the distribution of stresses adjacent to extensive high-extraction (85 to 100 percent) areas. Stress distributions in areas of low average stress correspond closely to the theoretical distributions based on elastic theory. However, in areas of high average stress, the stress distributions are of a type associated with plastic failure. The stresses adjacent to a mined-out area supported by remnant pillars were significantly higher than the stresses adjacent to another area in which the remnant pillars were removed.

Jan 1, 1965

By Arnold B. Hubbard

Automatic control instruments were utilized by the Bureau of Mines for routine assays of large numbers of oil shale samples and other bituminous materials. The standard Fischer assay method was automated by automatically controlling the heating cycles of a battery of 12 electric heaters with electronic controllers and programmers. The condensers were cooled with a modified automatically controlled refrigeration bath. The complete assembly consisted of 12 retort units, necessary control instruments, and the refrigeration bath. This equipment was capable of producing more consistent results than those previously obtained with the gas-heated retorts and of increasing the output of assays substantially with no increase in operating personnel.

Jan 1, 1965

By Robert C. Ellman

The Bureau of Mines investigated the factors that cause agglomeration of lignite by freezing during winter shipment and sought methods to avoid it. Tests showed that lignite may be freezeproofed by removal of the relatively small quantity of moisture involved in forming the frost crystals which cement particles together, or by controlling the crystal characteristics. Adding dried lignite fines proved to be an effective and superior freezeproofing method. Commercial adoption of this method has been successful.

Jan 1, 1965

By D. E. Fogelson

In a factorial experiment, blasting caps were detonated in three sizes of shotholes in mortar with three types of stemming--dry sand, wet sand, and hydrostone. Free-surface displacement pulses were recorded with a capacitive-displacement gage at a distance of 15 inches. The effects of decoupling and the type of stemming on the amplitude and the duration of the displacement pulse were determined. Both the amplitude and the duration of the displacement pulse were significantly decreased by increasing the decoupling, but they were little affected by the type of stemming.

Jan 1, 1965

By Larry A. Haas

The Bureau of Mines constructed a torsion effusion apparatus to measure the equilibrium vapor pressure of pure metals, alloys, and compounds at temperatures up to 1,500° K. The reliability of the apparatus was established by determining the vapor pressure of silver. The data obtained on solid and liquid silver in the temperature range 1,200° to 1,500° K can be expressed by the following equations:

Jan 1, 1965

By George C. Price

The Bureau of Mines conducted this study in the Roslyn No.5 coalbed in the State of Washington to determine the feasibility of mining hydraulically the portion of the coalbed that was steeply pitching. All of the experimental mining was done while advancing raises and rooms. A Bureau-developed hydraulic mining machine was used successfully in the pitching coalbed. It consisted of a remotely controlled monitor mounted on a self-advancing roof support unit of the type commonly used for roof support in longwall mining systems. The coal cutting rates averaged 0.73 and 0.54 ton per minute in raise and room mining, respectively, while using water volumes up to 230 gpm at a pressure of 4,000 psig. Productivity averaged 4.7 and 5.2 tons per man-shift for raise and room mining, respectively, compared with 7.5 and 8.5 tons per man-shift, respectively, by conventional hand mining methods.

Jan 1, 1965

By R. Barany

The heats of formation of anhydrous ferric sulfate and anhydrous indium sulfate were determined by solution calorimetry. At 298.15° K the heats of formation from the metal, rhombic sulfur, and oxygen were -615.6 ±O.7 kcal/mole for ferric sulfate and -649.6 ±O.6 kcal/mole for indium sulfate. Heats of decomposition at 298.15° K are given for the reaction that forms metal oxide, sulfur dioxide, and oxygen) and for the reaction that forms the metal oxide and sulfur trioxide.

Jan 1, 1965

By John W. Thatcher

A demountable X-ray tube vacuum spectrograph was designed by the Bureau of Mines for the determination of long-wavelength X-ray spectra from the light elements. This instrument was operated for both secondary and combined primary-secondary excitation of the aluminum K-series. There was an increased analytical sensitivity for elements in period 3, and an indication that with improved X-ray tubes or direct election excitation of the sample, X-ray determination of elements in period 2 is also possible.

Jan 1, 1965

By Gilbert M. Farrior

The electrical resistivity the coefficient of electrical resistivity the Hall coefficient, and the absolute thermoelectric power were determined in this Bureau of Mines investigation for nine compositions of the TiB2-CrB2 sub-system. The numerical values of the electrical resistivity and the thermo-electric power were greater for the intermediate compositions than for the end members. The absolute values of the Hall coefficients and the coefficients of electrical resistivity were less for the intermediate compositions than for the end members. The electrical resistivities and Hall coefficients were about the order of magnitude of most metals--from 34 to 202 microhm-cm and from about 0 to -23.3 X 10-4 cuP/coulomb. The thermoelectric power was somewhat greater than that of most metals--up to 15.6 microvolts per 0 C.

Jan 1, 1965

By H. P. LeVan

Research was conducted to examine the feasibility of extracting manganese from Georgia umber ore by a three-stage continuous sulfuric acid-ferrous sulfate pickle liquor leaching process. A continuous cyclic process for treating the umber was operated successfully, using a synthetic solution simulating a ferrous sulfate fortified anolyte solution discharged from a manganese electrolytic cell as the leaching medium. Leaching efficiency based on removal of the manganese from the ore ranged from 83 to 89 percent for all systems tested.

Jan 1, 1965

By Martin H. Stanczyk

The Bureau of Mines studied continuous closed-circuit attrition grinding of a coarse commercial filler-grade kaolin to produce paper-coating-grade clay having a particle size analysis of at least 70 percent minus 2-micron equivalent spherical diameter (esd). The coarse clay, containing about 12 percent minus 2-micron-esd material, was ground in a Bureau-developed 10-inch-diameter attrition grinder in closed circuit with a 5-foot-diameter bowl classifier. In the best test, a finished product containing 82.7 percent minus 2-micron-esd material was obtained when grinding 20 pounds of raw clay per hour at percent solids with a 100-percent circulating load. Energy consumption was about 341 kilowatt-hours per ton of clay feed, or 487 kilowatt-hours per ton of minus 2-micron-esd material produced. Closed-circuit grinding gave some-what greater particle size reduction and lower energy consumption than either batch or continuous open-circuit grinding.

Jan 1, 1965

By Jerry B. F. Champlin

NIOSHAn accelerated testing procedure developed by the Bureau of Mines for evaluating commercially available corrosion inhibitors is described. Ultra-sonic agitation of the corrodent solutions and the hot-finished mild steel test coupons was used to evaluate the effects of several variables on the effectiveness of two corrosion inhibitors. Small changes in the weight of the test coupons in both controlled and inhibited corrodents, before and after exposure, affected the precision and accuracy of the results. Minute amounts of oxygen in the systems were found to be causing the relatively large deviations in the corrosion developed in the controlled tests. Microscopic examination of the test coupons revealed that both surface preparation and internal strains resulting from fabrication methods materially affect corrosion behavior.

Jan 1, 1965

By S. E. Khalafalla

The Bureau of Mines investigated variations in the activation energy for the carbon monoxide reduction of magnetite and ferrous oxide with respect to the state of aggregation of the oxide material. Reduction phenomena can only be satisfactorily explained by including an adsorption step in the reduction process. Summation of the values of the exothermic heat of chemisorption and the variable apparent activation energy for reduction yields a nearly constant value of about 50 kcal for either ferrous oxide or magnetite regardless of whether they are aggregated in pelletized form or coarsely crystalline particles.

Jan 1, 1965

By Edward W. Parsons

The explosive-expansion center-hole anchor was designed and developed for the specific purpose of use as a component of an instrument system that measures differential ground movement within a small drill hole in rock. Such anchors should have an unobstructed center hole, should be installed without a twisting action which could tangle connecting wires, and should be capable of being installed at depths in excess of 100 feet. The anchor has a thick-walled center tube and a thin-walled outer tube. Low-energy detonating cord, wrapped around the center tube and detonated with a mild end primer, expands the outer tube to produce anchorage. The explosive-expansion center-hole anchor can be installed easily in drill holes of any inclination but cannot be installed under water. Centering of the anchor is critical with regard to its subsequent holding power. The anchor is safe to make and handle.

Jan 1, 1965

By Albert W. Deurbrouck

Twelve samples from six Barbour County coal beds were analyzed for this report. The samples collected were generally high sulfur content coals, frequently exceeding 3 percent in the raw-coal sample. Many of them could not be upgraded to acceptable metallurgical standards even by rigorous preparation procedures. The production of coal in the county in 1963 amounted to almost 3 million tons of which 44 percent was mechanically cleaned.

Jan 1, 1965

By L. B. Pankratz

Heat contents, measured above 298.15° K, and derived entropy increments are presented in tabular and equation form for the two crystalline forms of zinc sulfide (sphalerite and wurtzite) and for four solid solutions of iron and zinc sulfides having the compositions Zno.,,6Fe0.302S, Zno.750Fe0.250S, Zno.650Fe0.3505, and Zno.498Feo.502S.

Jan 1, 1965

By Henry M. Harris

The Bureau of Mines investigated a glass containing approximately 17 percent lithia and 83 percent silica to establish a method of devitrifying cast and rolled shapes. Glass shapes with high strength were made by melting, forming, and rapid cooling of the composition, and the shapes subsequently were converted to a crystalline condition by heat treatment. The best devitrification schedule included rapid cooling of the glass to below 300° C, followed by reheating at a rate of 50° to 400° C per hour, depending on the size of the shape, followed by a of 60 to 70 hours at 500° C and another period of 15 hours at 800° C. attempts to use faster heating rates or slow cooling to accomplish devitrification in deformation of the shapes. The crystalline shapes had flexural strengths that averaged over 33,000 psi, achieved with an annealing time of 60 to 70 hours at 500° C.

Jan 1, 1965