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By W. E. Anable

The Bureau of Mines studied the purification of commercially available yttrium by melting it in a 100-kw electron-beam furnace. Button-scale melts were made to determine the ultimate purification that could be attained by melting yttrium at 1,733° to 1,770° C at low pressure (0.05 to 0.1 micron) for 1 to 120 minutes. In addition, numerous melts were made to study the effect of doping yttrium with carbon, 17 selected metallic additions, and 3 compounds. Except for nickel and zirconium, the metallic impurities in yttrium were lowered significantly on extended treatment; silicon was lowered only slightly. The nonmetallic impurities} oxygen, nitrogen, and carbon, were not lowered except on short exposures. In isolated instances, the oxygen content was lowered from 5,860 ppm to about 5,000 ppm. In most instances the carbon con-tent was lowered from 545 to about 220 ppm in 20 minutes and then increased again. It was concluded that yttrium cannot be purified by direct heating or by the doping technique employed.

Jan 1, 1965

By J. D. Spagnola

The Bureau of Mines conducted research to obtain comparative data on the extent of reduction of galena and sphalerite with molecular hydrogen and with hydrogen from the thermal cracking of ammonia and methane at various time intervals. Galena reductions of 95 to 99 percent were obtained with H2 and with decomposed NH3 while reductions of 70 to 80 percent were obtained with cracked CH4? Sphalerite reductions of 99 percent were obtained at 1,000° C with Hz and with decomposed NBs; however, complete volatilization of the free zinc from the remaining concentrate and the subsequent recombination of zinc and sulfur vapors resulted. A promoted iron catalyst brought about a decrease of 100° C in the temperature required for complete decomposition of ammonia. It was found that H2S retards NB3 decomposition and that nitrogen retards the reduction of galena by H2? A mixture of N2 and He in about the same ratio as that obtained by the thermal cracking of NBs gave about 15 percent less reduction of galena than was obtained with decomposed NB3; this indicates that a portion of the hydrogen obtained by NBs decomposition is in an active form.

Jan 1, 1965

By Alla D. Mah

The heat of combustion of TaC0.996 was determined by oxygen bomb calorimetry to be -302.8 ±0.4 kcal/mole. The corresponding heat of formation of TaC0.996 is -35.4 ±0.5 kcal/mole, and the calculated heat of formation of TaC1.00 is -35.5 ±0.5 kcal/mole.

Jan 1, 1965

By A. R. Taylor Jr.

The heat capacities of a-quartz form beryllium fluoride were measured at approximately 3° intervals from 8° to 300° K., using an adiabatic calorimeter. At 298.15° K the heat capacity and entropy were 12.39 cal/deg mole and 12.75 ±0.04 eu respectively. Enthalpy measurements were made with an ice calorimeter at approximately 30° intervals on the quartz and glassy forms of beryllium fluoride between 300° and 1,200° K. A melting point of 825° K and an 0,-8 type transition at 500° K with a heat effect of 75 ca1/mole were deter-mined from the enthalpy data for the quartz-type sample. Beryllium fluoride glass crystallized spontaneously into the quartz modification at 500° K. The heat of the reaction BeF2 (a-quartz) .... BeF2 (glass) was found to be 1,125 ±16 cal/mole at 298° K by solution calorimetry. This value, when corrected to 273° K, was used to correct for the heat absorbed by the formation of glassy BeF2 when the sample was dropped into the ice calorimeter from temperatures above the melting point. Using corrected enthalpy measurements, the heat of fusion was determined to be 1.13 kcal/mole at 825° K.

Jan 1, 1965

By Albert W. Deurbrouck

This report describes the preparation characteristics of 23 coal samples collected from nine of the more significant coalbeds of Fayette County, W. Va. In 1963 almost 5.4 million tons of medium to high volatile B coals of excellent quality for metallurgical and steam markets were produced in Fayette County. Of the 23 coal samples collected 11 would require some upgrading to pro-vide metallurgical quality products, 11 were acceptable as received, and 1 was a noncaking coal. Cleaning these coals to metallurgical standards would require only the removal of the sink 1.58 specific gravity material which would be quite easy as very little near-separating-gravity material was present at this gravity.

Jan 1, 1965

By R. L. Solmer

During 1959-61, the Bureau of Mines investigated the strain and deformation induced in rock and concrete linings around mine openings by retreat panel caving at the Climax Molybdenum mine. Two concrete-lined slusher drifts on the Phillipson level of the mine were instrumented with both electrical strain gages and extensometers. Changes in strain and deformation were recorded over an 18-month period during the undercutting and caving of the mining panel. General agreement was found between the strain and deformation measurements and the hypothesis that the vertical component of the stress field on the openings is almost completely removed by undercutting. This phenomenon is a possible explanation for the structural failures that occur in the slusher drifts during the undercutting cycle.

Jan 1, 1965

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 Norman G. Foster

The mass spectra of 14 previously unreported alkylthiophenes are pre-sented. Low ionization voltage data of selected compounds from these 14 and 23 previously reported alkylthiophenes are presented and discussed for their value in supporting fragmentation mechanisms analytical correlations. A comparison with and corroboration of earlier correlations is made. Additional correlations concerning detection of side chain branching and the detection of ethyl-alkyl and propyl-alkylthiophenes are made. A discussion of the possible fragmentation routes and mechanism of fragmentation is given. Speculative structures are inferred s out some of the ions and hence this work provides a basis for suggesting fation mechanisms for the alkylthiophenes according to modern theories ass spectrometry. Verification of these mechanisms must await the availability of isotopically labeled molecules which are labeled in specific lotions that permit the definition of the paths of frag-mentation. Some suggestions for further work to generalize on the correlations and studies made to this point are presented.

Jan 1, 1965

By Jr. Smith

The equilibrium compositions of product gases for mixtures of air with methane, propane, or ethylene at and around flame temperatures are reported. For each hydrocarbon, compositions are given for five fuel-to-air ratios--two lean, two rich, and one stoichiometric--at five pressures, from 1 to 20 atmospheres, and at an ambient temperature of 25° C.

Jan 1, 1965

By R. L. Crosby

A part of the liquidus of the magnesium-zirconium system was determined by chemical analysis of suction samples taken from the melt in the approximate temperature range of 850° to 1,450° C. The melt was prepared in a furnace pressurized with an inert gas. The average zirconium value in weight-percent of the liquidus composition at each sampling temperature was 0.96 at 867° C, 1.40 at 1,062° C, 2.05 at 1,262° C, and 2.96 at 1,402° C. The equilibrium solid phase was zirconium.

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 P. L. Woolf

Two blast furnaces, one a. commercial furnace and the other the Bureau of Mines experimental furnace, were successfully operated with extremely low slag volumes. The lowest slag rate obtained on the industrial furnace was 335 pounds per ton of metal. Using the same burden materials a 245-pound slag volume was achieved on the furnace. The coke rate saving and increase in productivity resulting from lowered slag rates are discussed as well as the factors limiting a low slag practice.

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

Vanadium, molybdenum, and a titanium-10 percent vanadium alloy were evaluated for their susceptibility to stress corrosion cracking in a number of corrodents. Tests were conducted utilizing conventional U-bend techniques with subsequent evaluation in a pneumatic constant-load apparatus. Vanadium and molybdenum were generally resistant to stress corrosion cracking in the media studied. U-bend specimens of vanadium showed evidence of stress corrosion cracking in 6 li hydrochloric and 18 li sulfuric acids; however, tensile stress specimens exposed to these solutions did not exhibit stress cracking. Similar results were obtained when U-bend specimens of molybdenum were immersed in 10 percent formic acid. Titanium-10 percent vanadium alloy was susceptible to stress corrosion cracking in 10-percent (2.85 li) hydrochloric acid solution. Heat treating the alloy greatly reduced its corrosion rate and its susceptibility to stress cor-rosion cracking in this medium.

Jan 1, 1965

By Philip G. Burkhalter

Total yield and backscattered electron coefficients were measured in this Bureau of Mines study in an microanalyzer as a function of atomic number and of primary crier: ;y in the 15- to 35-kilovolt range. The electron coefficients were obtained indirectly from measurements of the specimen electron current and the primary beam current collected in a Faraday cage and were measured with a precision better than 0.5 percent. Secondary electron emission was suppressed with opposing potential applied to a screen grid surrounding the specimen. The values of the backscattered electron coefficients agreed with published values within 5 percent.

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