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By Herbert R. Babitzke

The purpose of this investigation was to optimize the high-temperature properties of columbium and tantalum. Columbium and tantalum were combined with selected alloying elements to achieve solid solution and dispersion strengthening. Fifty-six alloys were evaluated to determine their formability, hardness, strength at elevated temperatures, and oxidation resistance. The following six alloys showed high-temperature strength: [Cb-15Hf-5W-2Zr-4Al-4Ti-2N Cb-15Hf -5W-5Zr Cb-15.3Ti-4.1Zr-13.7Hf Ta-20Hf-4Al Ta-30Hf-4Al Ta-20Hf-5W-4Al] At 1,200° C, the columbium alloys had strength values of 40,000 psi or greater, and the tantalum alloys had strength values from 50,000 to 58,000 psi. For a 2-hour test period at 1,000° C, weight gains of only 9 and 8 mg/cm2, respectively, were observed on oxidation testing of two alloys, Cb-15Hf-5W-2Zr-4Al-4Ti-2N and Ta-20Hf-5W-4Al.

Jan 1, 1968

By A. R. Taylor

Using solution calorimetry, the following heats of reaction were determined: (1) NaCN(c) + 1/Cu20(c) + 129H20(l) ? CuCN(c) + NaOH?128.5H2O ?H = -13.44±0.10 kcal/mole, (2) HCN(2) + NaOH?128.5H20 ? NaCN(c) + 129.5H20(l) ? = -2.52±0.02 kcal/mole. From these reactions, the heats of formation for CuCN(c) and HCN(2) were calculated to be 22.7±0.4 kcal/mole and 24.9±0.4 kcal/mole, respectively. Reaction 2 was made to check the consistency of literature values for heats of formation of HCN and NaCN. Adiabatic calorimetric measurements between 10° and 400° K showed the entropy and heat capacity of CuCN(c) to be 21.51±0.06 eu and 14.58±0.04 cal/mole deg, respectively, at 298° K. A broad anomaly in the heat capacity was found in the temperature range 285°-320° K. The heat of transition associated with this anomaly was less than 1 cal/mole, the sensitivity of the measurements.

Jan 1, 1971

By R. B. Anderson

As a part of a Bureau of Mines program on the conversion of coal to liquid and gaseous fuels, the kinetics of the Fischer-Tropsch synthesis on iron catalysts was investigated. Nitrided catalysts were studied at 21.4 atmospheres using feed gases ranging from 2H2+1CO to 0.25H2+1CO, and at 7.8 to 21.4 atmospheres using 1H2+1CO gas. The overall apparent activation energy increased with increasing carbon monoxide content of the feed gas from 19.5 kcal/mole for 2H2+1CO to 23.7 for 0.7H2+1CO. The rate of synthesis with 1H2+1CO feed increased linearly with operating pressure from 7.8 to 21.4 atmospheres. A semifundamental rate equation of the form [r=a'PH2 0.6pco 0.4- ?r0.5PH200.5] was shown to fit the data satisfactorily. The relative usage of hydrogen to carbon monoxide decreased with increasing conversion, passed a minimum, and then increased. Apparently water is the principal primary product and carbon dioxide is produced by subsequent water-gas shift reaction. In another group of experiments water, carbon dioxide, argon, and methane were added to 1H2+1CO feed to a nitrided iron catalyst. Argon and methane were only diluents. Carbon dioxide was a slight inhibitor and water vapor was a strong inhibitor to the rate of synthesis. Water accelerated the water-gas shift and usually increased methane production. Important factors of catalyst geometry in determining rate were found to be particle size and extent of reduction. Apparently the active portion of the catalyst is confined to a layer of 0.01 to 0.02 cm from the external surface of particles. A special solution was made of differential equations relating re¬action at the catalyst surface to diffusion in pores of the catalyst for spherical particles with an active layer surrounding an inert core. The equation derived expressed the experimental data reasonably well. Diffusivities determined by this equation varied from 3 to 24X10-6 cm2/sec; these values are of the same magnitude as observed for the diffusion of gases in liquid. The appendix presents a group of synthesis experiments at pressures of 21.4 to 103 atmospheres. In this range the rate of synthesis on nitrided iron catalysts increased with pressure to the 0.74 to 0.84 power.

Jan 1, 1964

By S. C. Schaefer

The Bureau of Mines investigated tIle standard Gibbs energies of formation, 8Gfo, for MllF2 (manganese difluoride) and CoF2 (cobalt difluo-ride). High-temperature galvanic cells employing CaF2 (calcium diflu-oride) as the solid electrolyte were used to measure the open-circuit potentials for the cell reactions ?

Jan 1, 1985

By J. J. Lukasko

The U.S. Bureau of Mines developed an alternative electrochemical process for the production of calcium metal. The current industrial practice is costly, complex, and inefficient. The Bureau method involved electrowinning of a calcium-tin alloy followed by electrorefining to produce calcium metal. In the electrowinning cell, CaCI2 was fed to a KCI2-CaCI2 electrolyte. The calcium was electrowon at 6500 C into the pure molten tin cathode until the cathode contained 7.5 wt pct Ca. Current efficiency for electrowinning averaged over 90 pct. The resulting calcium-tin alloy served as the anode for the electrorefming cell, which employed a [CaC~-CaF2] fused salt as the electrolyte. Calcium metal was electrorefmed at 8500 C with a current efficiency of 85 pct based on calcium metal recovered. The calcium metal analyzed 99.2 pct, which is purer than commercially produced calcium.

Jan 1, 1990

By Stephan Stecura

Crystallographic modifications and kinetics of solid-state phase trans-formations were determined for five rare-earth" sesquioxides--La2O3, Nd2O3, Sm2O3, Eu2O3, and Gd2O3. Oxides used for crystal modification studies were prepared by thermal decomposition of the following high-purity salts of the five rare-earth elements--carbonates, chlorides, fluorides, nitrates, oxalates, and sulfates. X-ray diffraction patterns of the cubic and hexagonal oxides were indexed by a graphical method and patterns of the monoclinic oxides by Ito's method. The kinetics of crystallographic transformation were determined by high-temperature X-ray diffractometry. The kinetic data were interpreted using a shrinking sphere model. All of the transformations followed first order kinetics. Activation energies were calculated by application of the Arrhenius equation. These solid-state phase inversions were concluded to occur by a reconstructive transformation mechanism.

Jan 1, 1965

By John E. Miller

Supercompressibility factors, Fpv, were derived from experimental compressibility data for five helium-nitrogen mixtures containing from 50 to 100 pct helium. These Fpv values are required as volumetric correction factors for or if ice meter measurement of "crude helium" (helium-nitrogen) purchased by the Government in a program of helium conservation. Although compressibility measurements were made by the Burnett method (2)3 - for pressures from 100 to 3,400 psia and temperatures from 40° to 100° F, Fpv values were needed only for pressures from 400 to 2,000 psia. Consequently, values at increments of 2° F, 2 pct helium, and 10 psia were tabulated only for the required pressure range. Values for pressures outside this range can be calculated from information shown in the tables. Values for the second, third, and fourth coefficients in the equation Z = 1 + BP + CP2 + DP3 are also included.

Jan 1, 1963

By A. A. Berk

In the course of a study of the formation of external deposits on tubes in water-tube boilers it became desirable to determine the sulfur dioxide (SO2) and sulfur trioxide (SO3) in the Due gases. Determinations made by the A.S.M.E. method for SO2 and SO3 in gaseous products of combustion did not give accurate results. It was found that minute quantities of copper, present in the flue gases from the coal in use, caused oxidation of sulfite in the absorption bottle and that the carbon dioxide (CO2) in the flue gases caused high values for SO2. The A.S.M.E. test procedure was revised to prevent oxidation of sulfite in the absorption bottle and to allow for the effect of CO2; subsequent analyses of flue gases produced reliable results. The revised procedure is described.

Jan 1, 1950

By A. Salmoni, E. K. Gillin, T. Eger, A. Cann, P. Vi, M. Hunt

Kittusamy (Kittusamy & Buchholz, 2004) state that there have been few studies conducted to assess exposure to whole-body vibration (WBV) in the construction industry. They suggest that there is very little reliable data from the construction industry that characterizes exposure levels to various hazards including WBV or the health outcomes from such exposure and that there is a need for more exposure data. In a recent exploratory study of heavy construction equipment Cann (Cann, Salmoni, Vi, & Eger, 2003) looked at vibration levels for 14 different types of construction equipment. Eight of the 14 pieces of equipment tested exposed operators to levels of WBV that exceeded the recommended limits for an 8-hour period when comparing the measured VDV to the ISO 2631-1 standards. The purpose of the present research was not only to test a larger number of scrapers but also to investigate scraper operator exposure to whole body vibration (WBV) separately for each task. Methods 33 scrapers were evaluated for WBV in a variety of residential and road construction projects. Testing equipment consisted of triaxial accelerometers that allowed vibration data collection in all three orthogonal axes, with the x-axis positioned to measure vibration in the anterior-posterior direction, the y-axis in the medial-lateral direction, and the z-axis in the vertical direction. Root mean square accelerations (aRMS), vibration dose value (VDV), crest factor, and maximum transient vibration values (MTVV) were derived from this software and exported to an Excel™ spreadsheet for later data analysis. Test sessions for each piece of equipment lasted for approximately 20 minutes until at least three work cycles had been completed. Tasks included: idling while waiting for a bulldozer to push the scraper through the scraping phase, scraping, traveling loaded with dirt, dumping and traveling empty. Results Task breakdown by time reveals 25% of the work cycle was spent traveling fully loaded with dirt, 19% dumping, 21% traveling unloaded, 17% idling and 18% scraping. Calculation of aRMS vector sums gave values of 2.55 m/s2 during loaded transport, 2.46 m/s2 during dumping, 2.31 m/s2 during unloaded travel, 0.55 m/s2 during idling and 1.46 m/s2 during scraping (see Table 1). The highest acceleration values recorded were found in the z-axis during fully loaded transport reaching an average aRMS over three work cycles of 2.55 m/s2.

Jan 6, 2006

By Edward A. McClatchie

A novel nondispersive electro-optical gas analyzer has been designed, fabricated and tested. The instrument is based on a pressure modulated absorption technique. Key features of this new gas analyzer technique include long-term zero and calibration stability. The technique was investigated for the gases carbon dioxide (CO2), carbon monoxide (CO), methane (CH4) and nitrogen dioxide (NO2). The delivered analyzer was capable of measuring the three species CO, CO2 and NO2. It is a compact (300 cu in) package, is battery powered and weighs 15 lbs. Some thirty readings of each gas may be made on a single battery charge.

Jan 1, 1980

By W. W. Adams

Every man-hour of work performed in and about the coal mines of the United States had a 2-percent heavier death load from accidents in 1938 than in 1937. This is an unorthodox way of stating that the death rate per million man-hours of exposure or employment was 2 percent higher in 1938 than in 1937, increasing from 1.74 to 1.78. Thus the average miner had a 2-percent greater chance of being killed in 1938 than he had in 1937. The average quantity of coal resulting from 1 man-hour of work increased 3.6 percent -from 0.615 ton in 1937 to 0.637 ton in 1938. The production of the average ton of coal was accompanied by a slightly smaller loss of life in 1938 than in 1937, the accident rate being 2.793 per million tons in 1938 compared with 2.833 in 1937.

Jan 1, 1941

By Bertrand L. Johnson

Pure talc is a hydrous magnesium silicate (Mg3Si4010(OH)2). Pyrophyllite, although it resemble: talc in certain physical properties and uses, is a hydrous aluminum silicate (Al2Si4010(OH)2) - like kaolin, except that kaolin has a somewhat different composition (Al2Si205(OH)4) and structure. Soapstone can be considered essentially an impure talc grid when pulverized is used for many of the same purposes as talc. Massive, compact varieties of talc often are called steatite. PROPERTIES Talc and pyrophyllite are characterizes; by their softness (hardness on Mohs' scale, 1) their greasy feel, pearly luster, white color, and perfect basal cleavage. They have similar crystal structures, and this similarity explains the close resemblance of the two minerals in physical acid chemical properties. Talc is a good electrical insulator, resists the action of most acids and alkalies, and has an exceptional heat-retaining capacity. Its specific gravity is about 2.7.

Jan 1, 1939

By E. D. Gardner

About five minutes after 3 o'clock on Thanksgiving morning, November 24, 1927, smoke was discovered coming up No. 2 shaft of the Magma Copper Co.'s mine at Superior, Pinal County, Arizona. Of the 49 men in the mine at the time, 42 were able to make their way to the outside unassisted, but 7 perished. Six bodies were recovered, and the seventh, that of an Apache Indian cage-tender at No. 2 shaft, is thought to be in the caved section between the 1,600 and 2,250 foot levels A second and independent fire broke, out in No. 1 shift about 2 a.m., November 27, burning .out the shaft timbers from the surface to the 200-foot level and destroying the surface fan and structures. About 20 men were underground fighting the fire in No. 2 shaft, but all were safely withdrawn, aril the fire in No. 1 haft was quickly controlled.

Jan 1, 1928

By P. C. Good

The Bureau of Mines conducted a laboratory investigation of a sinter-leach method to recover aluminum and fluorine from waste carbon potlining residues from secondary cryolite recovery operations in aluminum reduction plants. After removal of carbon by burning, the residue was sintered at 900° to 1,100° C with silica and N2CO3, then crushed and leached with dilute NaOH solution, dilute Na2C03 solution, water, or water containing residual Na2O which remained in the sinter after reaction and decomposition of Na2CO3. Over 90 percent of the contained aluminum and up to 87 percent of the contained fluorine were extracted from this waste product in the form of a mixed alkaline solution. Treatment of the alkaline solution with CO2 yielded a white precipitate containing 89 percent of the original aluminum and 61 percent of the original fluorine as a mixture of synthetic cryolite and alumina, together with a variable excess of soda.

Jan 1, 1969

By Arne Landsberg

The Bureau of Mines measured the vapor pressure of FeC12 , FeBr2, FeI2, Sb, Bi, Cd, Mg, Pb, FeC13 , and VCl2 using the Knudsen-and torsion-effusion methods, and on FeC13 -NaC1 mixtures, Au2Cl6, and MgNi2 using only the Knudsen method. Apparent vapor pressures calculated from the experimental data vary with orifice size and method of determination. Reaction with residual oxygen in the instruments was noted to have an effect on the iron halide data. Vapor pressure curves plotted as log P versus 1/T (where P is pressure and T is absolute temperature) for one substance using several orifice sizes tended to converge at a single point when extrapolated beyond the experimental region. All of the data, except those of VC12, agree with previously published results. The importance of comparing effusion measurements with those obtained by other methods and the variations encountered with various orifice sizes are discussed.

Jan 1, 1977

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 Laurance L. Oden

The Bureau of Mines is developing nickel catalysts for converting synthesis gas derived from coal to synthetic natural gas. The present report describes the relationship between the composition of aluminum-nickel alloys in the composition range NiAl3 to Ni2Al3 equilibrated at 840° C and the properties of catalysts obtained from them. Methanation activity was determined in the temperature range of 300° to 360° C in a flowing gas stream containing 1 pct CO, 8 pct H2, and the remainder He. One part per million of H2S was added to the gas stream at 400° C to evaluate the susceptibility of catalysts to sulfur poisoning. The total surface area was measured by the adsorption of nitrogen at liquid nitrogen temperature, and the active surface area was measured by the adsorption of hydrogen at room temperature. Total surface area and active surface area were found to increase with increasing proportion of aluminum-saturated Ni2Al3 in the precursor alloy, but methanation activity and resistance to poisoning by H2S were nearly constant. However, the methanation activity of the catalyst prepared from stoichiometric Ni2Al3 was less than half that of the other catalysts.

Jan 1, 1978

By Richard G. Sandberg

The Bureau of Mins, U.S. Department of the Interior, is investigating a hydrometallurgical procedure to conserve cobalt, nickel, and copper by recovering the metals from the matte byproducts of smelting Missouri lead ores. For want of adequate processing technology the mattes are now either unmarketable or marginally so. The procedure involves leaching with manganese dioxide and sulfuric acid to obtain copper, nickel, cobalt, lead, and manganese sulfates, and elemental sulfur as expressed by the following reaction: MS + MnO2 + 2H2SO4 ? MSO4 + MnS04 + S° + 2H2O, where M = Cu, Ni, Co, and Pb. The leach solutions, containing near theoretical amounts of sulfuric acid and manganese dioxide at 85° to 100° C, convert up to 98 pct of the cobalt, nickel, and copper in the mattes to sulfates in less than 2 hr. As they are formed, the cobalt, nickel, and copper sulfates are dissolved leaving a residue of lead sulfate, lead, sulfur, and gangue. The soluble metals are recovered from the leach solutions by caustic and sulfide precipitation, and the residue returned to the smelter for lead recovery. The manganese can be reclaimed from the spent leach liquor as manganese oxide and recycled to leaching.

Jan 1, 1979

By Charles W. Huggins

The Bureau of Mines investigated palygorskite, a natural asbestiform material, to accumulate knowledge that might serve as a foundation for future synthesis of a similar material. Unit cell, chemical analysis, DTA, TGA, optical constants, and electron microscopy data were obtained. Selected palygorskite samples of bettor than 97-percent purity were used to obtain this information. Chemical analysis revealed the following formula: (OH2)4 (OH)2 Ca0.01Fe0.02K0 .c3Mg2.10A12.00Si7.93020.3.91 H2O. The optical constants for sodium light are a = 1.522; S = 1.530; ?=1.533; biaxially (-). The following orthorhomibic unit cell constants were determined: ao = 12.690 A, Z = 2, bo = 17.857 A, Dx = 2.327. co = 5.207 A, Identical diffraction patterns resulted from the three palygorskite samples that were studied. X-ray, chemical, DTA, TGA, and optical data were compared with literature values for similar fibrous materials. X-ray diffraction lines were indexed. Several electron micrographs were made to compare the structures of palygorskite and attapulgite with that of chrysotile. The micrographs revealed extremely short laths for attapulgite, very long flexible laths for palygorskite, and tubular structure for chrysotile.

Jan 1, 1962

By E. G. King

Sodium-aluminum and calcium-aluminum silicates are important rock-forming minerals. While many of them are of only theoretical interest, several are of practical importance--as ceramic raw materials and as potential future sources of aluminum. Heretofore, thermodynamic data for these minerals were incomplete; and in many instances missing data were difficult to estimate reliably. This has seriously hampered thermodynamic calculations pertaining both to the natural formations of these minerals and to their decomposition in sintering and fluxing reactions. This paper reports the results of the Federal Bureau of Mines measurements of low-temperature heat capacities of four crystalline silicate minerals--dehydrated analcite (NaAlSi2O6), hexagonal anorthite (CaA12 Si208), lawsonite (Ca2Al2Si2080?2H20), and leonhardite (Ca2Al4Si8C24?7H2O). It augments previous similar measurements of related minerals, which were summarized recently.4 The measured heat-capacity data were used to derive entropy values for the four minerals at 298.15° K. Some relations between these entropy values and those of other similar minerals were discussed. These relations illustrate the difficulty of estimating entropy values of tertiary (or higher) silicates.

Jan 1, 1961