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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 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 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 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 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

By P. L. Woolf

An investigation was conducted to evaluate the use of a formcoke as the total fuel in the Bureau of Mines experimental blast furnace. The formcoke performed very satisfactorily, and comparisons made with a metallurgical coke showed that the performance with the formcoke was somewhat superior under the experimental conditions used.

Jan 1, 1966

By A. W. Deurbrouck

Four samples of Pittsburgh-bed coal, of various size consist and ash content were dewatered in a pilot-size vacuum-disk filter partially enclosed with a steam jacket. Steam fed at 2.5 to 12.5 pounds per minute reduced the moisture content of the filter cakes from 2.8 to 13.8 percentage points more than normal vacuum dewatering. Approximately 1.5 pounds of steam was required to remove 1 pound of water.

Jan 1, 1966

By R. T. Sorensen

Research and testing in a small scale equivalent of a commercial flota-tion plant was completed on four low-grade, iron-bearing materials from the western Mesabi range. Closed circuit-flotation of calcium-activated silica with fatty acid collector developed data for comparison with the batch process and highlighted problems not evident from previous bench testing. The four ore samples contained from 27 to 39 percent Fe and were equally represented by nonmagnetic taconite and semitaconite type materials. Iron concentrates containing 6.0 percent, or less, SiO2 were made 5, all four samples. Of the two material types, the semitaconite was the ore amenable to treatment, yielding iron recoveries of about 90 percent as cc pared with 70 to 80 percent for the other. Pilot plant tests showed that concentrate grade made in batch tests could be duplicated in the closed circuit and demonstrated that the amount of recoverable middling iron varied considerably between ore samples. The continuous tests also showed that water temperature strongly influenced results in the treatment of one ore but apparently was of indifferent consequence in another. Progress in thickening and filtration of flotation concentrates was made through introduction of tapioca flour to serve the dual role of iron mineral depressant and flocculant.

Jan 1, 1966

By Jr. Jacobson

Thermal reactions of l-methylpyrrole, l-butylpyrrole, and l-isopropyl-pyrrole were investigated by a flow method in the temperature range of 4500 to 5750 C. Those of I-butylpyrrole and l-isopropylpyrrole were also investigated in the 3400 to 4000 C range in a static system. The I-substituted pyrroles isomerize by an irreversible reaction to 2-substituted pyrroles. A reversible isomerization reaction shifted the alkyl group from the 2-to the 3-position on the pyrrole ring. All of the isomerization reactions are homogeneous, unimolecular, nonchain, first-order reactions having similar mechanisms and transition states. There is decomposition and cleavage of the longer alkyl side chain when it is in either the 2-or 3-position giving, as products, pyrrole, 2-and 3-methylpyrrole, 2-and 3-ethylpyrrole, pyridines, and hydrocarbons. The decomposition reactions appear to be by free-radical mechanisms. Pyridine homologs are formed by the expansion of the alkylpyrrole: butylpyrrole produces pyridine, and isopropylpyrrole produces 3-methylpyridine. Approximate Arrhenius equations are given for the formation of the decomposition products.

Jan 1, 1966

By W. H. Oppelt

Two exploratory gasification tests of limited duration were made at Dorsten, Germany, with strongly coking Pittsburgh-bed coal in a fixed-bed pressure gasifier. To reduce the coking potential of the Arkwright coal, ash refuse from the gasification of Dorsten (Leopold) coal was added to pre-pare coal-ash mixtures which contained nominal 20 and 30 percent ash. Major adjustments in principal process variables at the beginning of the tests resulted in wide fluctuations in the rate of gas production, gas offtake temperature, and carbon dioxide concentration in the gas. Because a higher steam-to-oxygen ratio was used in the tests than was customarily employed for routine operation, gas production was lower, and steam and oxygen consumption was higher. After operating conditions had been improved, the results of a 12~-hour-long test with addition of sufficient ash refuse to obtain a nominal 30 percent ash concentration indicated that operation is feasible with this coal mixture using a fixed-bed pressure gasifier equipped with a rotating coal distributor and stirrer.

Jan 1, 1966

By Foster Fraas

A separator for minerals of low magnetic susceptibility and fine particle size in a water suspension is described. A ring-shaped matrix of ferromagnetic fragments rotating so as to pass successively through magnetic-field and field-free regions provides for the separation. Application is illustrated in the separation of hematite and ilmenite from quartz.

Jan 1, 1966

By J. P. Morris

A diphenyl ether calorimeter for measuring high-temperature heat contents of ferrous alloys and iron-and steelmaking slags was constructed and calibrated with specimens of molybdenum, alumina, and platinum that were heated to temperatures ranging from 1,720° to 1,875° K. The standard deviation of the calibration measurements was 0.37 percent. By measurements of the enthalpy of delta and liquid iron, the heat of fusion of iron was found to be 3,298 ±100 cal per mole.

Jan 1, 1966

By R. W. Dalzell

The performance characteristics, efficiency, and operating pressure of jute line-brattice systems were studied under varying underground conditions; various fabric grades and installation methods were used. The test results indicate that line-brattice system efficiency is dependent upon the method of ventilation the method of installation, porosity of fabric, and size of tight rib area.

Jan 1, 1966