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By J. M. Stuve

Heat of solution measurements of high-purity neodymium metal and neodymium trichloride (NdCls) in 4.360 molal hydrochloric acid (HCI) were used to determine the standard heat of formation (6EPr) of NdCls? From solution data obtained, the heat of formation of NdCls (c) was computed as -248,970 ±260 cal/mole at 298.150 K.

Jan 1, 1965

By Glenn L. Cook

Correlations between mass spectra and molecular structures of 186 organic sulfur compounds are discussed. The olefinic ions, the alkyl ions, the CnE2n+1 ions, the m/e 61 ions, and the m/e 35 ions in the spectra of thiols are related to molecular structure. In the spectra of sulfides, the olefinic ions, the m/e 61 ions, the m/e 35 ions, the CnH2n+1S+ ions, and the CnH2n+1SH+ ions are correlated with molecular structure. For disu1fides, the correlations relate HSSF+& and RSSH+ ions to molecular structure. Base peaks of alkylthiophenes are correlated to their molecular structures. Some unimolecular reactions of sulfur compounds in the mass spectrometer are considered. A cyclic intermediate is suggested for the reaction which produces m/e 47, CH3S+, and m/e 48, CH4S+, ions in the spectra of sulfides. An expanded ring is suggested as a possible intermediate in the reactions of thiophenes. Heats of formation of sulfur-containing ions and their appearance potentials are presented in tabular form. Ionization potentials for sulfur-containing radicals and molecules are also given. Discussion of the spectra, tabulated in the appendixes, provides an insight into the relationship of the molecular structure of a compound to the mass-to-charge ratios and the intensities of the ions in its mass spectrum. Correlations of the mass spectra with molecular structures are empirically developed by observing regularities in the spectra of the reference compounds. Correlations extend the usefulness of mass spectra because they can be employed to determine the molecular structure of an unknown compound.

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 Wilbur I. Duvall

A linear array of shot and gage holes 30 feet deep in a granite outcrop was used to compare the size and shape of radial strain pulses produced in the rock when short cylindrical charges of cast composition B were detonated axially or at one end. The axially detonated charges produced radial strain pulses that had shorter rise times and larger peak strain than the strain pulses produced by end detonated charges.

Jan 1, 1965

By Lippe D. Sadwin

This report describes a high-speed streak camera technique for measuring the lateral shock pressure generated by a cylindrical explosive charge detonated from one end. Experimental data show that the magnitude of the lateral pressure is approximately 50 percent that of the pressure generated from the terminal end of the charge for three explosives studied.

Jan 1, 1965

By d&apos, D. V. Andrea

Nine rock properties were determined for rocks coming from 49 locations and having a wide range of compressive strengths. Plots of the nine rock properties versus each other were prepared. A stepwise multiple linear regression analysis was performed to obtain several equations for predicting compressive strength. Both linear and curvilinear relationships were assumed between compressive strength and the other rock properties. The prediction equations had multiple correlation coefficients ranging from 0.947 for an equation with 1 variable (point load tensile strength) to 0.986 for an equation with 25 variables. Of the properties tested only point load tensile strength could be used alone to estimate compressive strength with fair accuracy.

Jan 1, 1965

By Leonard Obert

This Bur of Mines investigation considers the deformational behavior (creep) of pillars made from three quasi-plastic rocks--salt, trona, and potash ore. The first phase of this study considers the design of a model pillar suitable for creep tests; in the second phase, six model pillars prepared from salt from two sources, from trona, and from potash ore. The pillars in each group were subjected to a different but constant axial stress, and the axial strain was measured for 1,000 hours.

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 J. M. Stuve

Calorimetric data for the dissolution of scandium sesquioxide and scandium trichloride in 4.360 molal hydrochloric acid were used to evaluate the standard heat of formation of ScCl3(c). The heat of reaction for Sc(c) + 1.5Cl2(g) = ScCl3(c) at 298.15° K was computed as -225,440 ±340 cal/mole.

Jan 1, 1965

By W. R. Huff

Yield stress and plastic viscosity values, determined from shear rate-shear stress relationships, were found to be a linear function of coal concentration for coal-water slurries containing 40, 45, 50, and 55 weight-percent of powdered coal. In the laminar region, the flow is described by an equation derived from the fact that the square root of the shear stress varied linearily with the square root of the shear rate. In the turbulent region, the friction factor was found to be inversely proportional to the velocity to the 0.12 power.

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 J. G. Walters

Analyses of light oils produced from the fluidized carbonization of coal at 485°, 550°, 600°, and 660° C are presented. Tar vapors from 485 C fluidized carbonization were thermally treated at 600°, 700°, and .800° C, and the analyses of light oils produced by this treatment are also presented. Procedures were developed for analysis of coal carbonization light oil by gas chromatography to permit a more definitive analysis than can be obtained by the conventional distillation procedure. An increase in low-boiling olefins, benzene, and toluene, a decrease in low-boiling paraffins, and little change in the remainder of the aromatics was observed with increased temperature of carbonization.

Jan 1, 1965

By Edward M. Kawenski

Tests were made in the Bureau of Mines Experimental Coal Mine on stop-pings similar to those used in operating coal mines to obtain information on air leakage through the face and the rupture strength of a stopping subjected to a pressure differential. Block stoppings were made from cinder, slag, and gravel aggregates with and without mortared joints and coatings. Sheet stop-pings were uncoated brattice cloth and nylon or brattice cloth and expanded metal-lath coated with asphalt, latex, mortar, or rigid urethane foam. Limited data were obtained on air through stoppings subjected to simulated roof convergence and to shock forces created by the firing of an adjacent charge of explosive. The pressure differential required to rupture stoppings was determined. shows that coating the face of a stopping effectively reduces ail: leakage. Block stoppings, particularly those with mortared joints, are most resistant to pressure and shock forces than are sheet stop-pings. Where ground movement is a factor, sheet stoppings leak less air than block stoppings.

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

By J. P. Hansen

Wustite beds were reduced with carbon monoxide and mixtures of hydrogen and nitrogen in the temperature range 900° to 1,300° C to determine the effect of temperature, gas flow, and surface area on the rate of reduction to iron. The composition of the gas stream as it passed through the wustite bed was continuously measured with infrared absorption cells and heated-wire methods. The change in composition was used to calculate the reaction rates. Arrhenius plots of the data give heats of activation of 34 kcal for particles using CO, 27 kcal for particles using H2, 24 kcal for pellets using C8, and 6 kcal for pellets using H2. The velocity of reduction is dependent on the area of reacting interface and the driving potential of the gas (reducing gas concentration minus equilibrium concentration) as well as the exponential temperature effect. The reaction rate was independent of the gas velocity over the range of conditions studied.

Jan 1, 1965

By J. G. Donaldson

Cobalt-tungsten binary deposits were formed in laboratory experiments by hydrogen reduction of the anhydrous mixed vapors of cobaltous chloride and tungsten hexachloride. The materials were sublimed in seperately heated zones of reaction tube and were transported in a stream of purified helium into the deposition section of the tube where the chloride gases were reduced to metal by a countercurrent flow of hydrogen. Heattreating of the near stoichiometric binary metallic deposits converted nearly all to the intermetallic compound Co3W, however, small quantities of both cobalt and tungsten remained. Mechanical tests showed that the tensile strength of heat-treated 75 percent cobalt-25 percent tungsten deposits was twice as high as that of similarly treated deposits of cobalt.

Jan 1, 1965

By John D. Corrick

The environmental and nutritional characteristics necessary for maximum copper extraction from a low-grade ore by Ferrobacillus ferrooxidans have been explored as have many of the limiting parameters. Criteria considered were oxygen consumption, copper extracted, soluble copper concentration, temperature, pH, particle size, nutrients, and other inorganic salt concentrations. A set of environmental and nutritional conditions were developed for E. ferrooxidans Which supported cell reproduction and maximum microbial oxidation of a low-grade copper sulfide ore. Percolator tests conducted under these optimum conditions resulted in an 18 percent increase in the quantity of copper microbially extracted over that extracted under conditions considered to be standard. Manometric tests determined those extremes of environmental conditions and nutritional factors Which were detrimental to the extraction of copper by E. ferrooxidans.

Jan 1, 1965

By W. L. Acherman

Molybdenum, tungsten, and vanadium were found by the Bureau of Mines to possess generally superior chemical and galvanic corrosion properties in many aqueous corrosive media at temperatures up to the boiling point. The corrosion resistance of vanadium in certain solutions was further improved by alloying it with such metals as columbium, tantalum, and titanium. was susceptible to a type of crevice corrosion in mercuric chloride solutions, but no other instances of crevice corrosion were encountered. With few exceptions, molybdenum, tungsten, and vanadium were not adversely affected when coupled with dissimilar metals in galvanic corrosion experiments; in some cases one or both members of a couple were protected by contact. When exposed to aqueous ammonia spray at 60° C, all three metals were attacked, but they were moderately resistant in spray environments of substitute ocean water and ammonium dihydrogen phosphate.

Jan 1, 1966

By E. A. Loria

The Bureau of Mines analyzed the effects of oxygen, nitrogen, and carbon on the tensile properties of electrorefined vanadium in terms of the Petch equation. The effects of the different impurities and grain sizes on the yield and flow stress between 2730 and 770 K were studied. For specimens of like composition, the values of the Petch parameters 01 and ky obtained by two different methods, extrapolation and grain size, were nearly the same. For high-purity electrorefined vanadium, the 01 value at 2730 K was 10,300 psi (5,150 psi shear). The 01 values for this metal at 1950 and 2730 K were lower by factors of 3 to 4 than for three less pure samples of commercial vanadium metal of equivalent grain size. Nitrogen was more effective than oxygen in increasing 01' the increase being about twice as much for the same impurity level. Carbon produced a slight increase in 01 up to 0.024 percent and then a gradual decrease in 01 to 0.11 percent, the maximum carbon content studied. The corresponding ky values followed the same trend in regard to oxygen and nitrogen additions, whereas the addition of carbon produced no variations at either temperature. Dislocations in vanadium are anchored by carbon, oxygen, and nitrogen with increasing firmness in that order. The high purity of electrorefined vanadium was confirmed by low yield stress and high ductility throughout the low temperature range. The metal also exhibited profuse twinning with high ductility at 1230 and 770 K. The effective surface energy for fracture, y, was found to lie between 3.3 and 3.6 x 1()4 erg cm-2?

Jan 1, 1966