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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 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. 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 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 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

By E. G. Davis

The Bureau of Mines made laboratory-scale experiments to examine the technical possibilities of reclaiming manganese from slags produced by oxygen lancing of high-manganese pig iron. Ferromanganese was added to molten pig iron to yield a 4-to 5-percent manganese hot metal, which simulated a product obtainable from the blast furnace. This was injected with oxygen to reduce the metal to 1 percent or less manganese and form a slag containing about 40 percent manganese. The molten slag was water-quenched, treated with H2SO4) roasted at 660° C, and water-leached to give soluble manganese and iron sulfates. The sulfates were precipitated as hydroxides, converted to the oxide form, and smelted to produce a standard ferromanganese containing 74.6 percent Mn and 0.01 percent P. As an alternate method of manganese recovery, a manganese cell feed was prepared from the leach solutions and electrolytic manganese was produced. Direct smelting of the high-manganese slag resulted in 74.2 ferromanganese meeting ASTM specifications except for phosphorus content. The high phosphorus content of the metal and high slag-to-metal ratio obtained made this approach unattractive.

Jan 1, 1966

By James S. Browning

Research by the Bureau of Mines demonstrated that organic heavy liquid adhering to or adsorbed on fine mineral particles can be effectively removed by a novel method embracing pulping or displacement washing with hot water alone or in combination with a detergent. Displacement washing with steam alone or in combination with a detergent also was effective for removing the heavy liquid. In tests of sized minus 48-plus 200-mesh mineral charges, both the hot water washing with detergents and detergent steaming effectively reduced the heavy liquid losses on the particles to about 0.2 pound per ton of mineral or less. Centrifuging of the wash solutions permitted an almost complete recovery of heavy liquid from the solution as a pure heavy liquid product.

Jan 1, 1966

By Louis A. Panek

Determining the change of stress in rock based on measurements of the deformation of a drill hole is a procedure that is increasing in popularity. A closely related procedure involves the applicat10n of this principle to determine the existing stresses in a rock medium, by cutting free (core drilling) an annulus containing the drill hole. In this Bureau of Mines report, expressions are derived from which one can calculate the stress ellipsoid--the three-dimensional change of stress, or the existing three-dimensional stress field, as the case may be. Study of these equations shows that the stress components in three dimensions can be determined by measurements in only two drill holes, and yields general principles that are useful in planning an efficient program of drilling and measurement. Procedures are given for calculating the least squares estimates of the stress components and their standard errors, and for evaluating or comparing calculated values by means of standard statistical inferences.

Jan 1, 1966

By John J. Mulligan

The Bureau of Mines investigated the tin deposits of the Cape Mountain area during July and August 1962 to test the effectiveness of detrital-cover sampling in permafrost areas as a relatively cheap and simple means of guiding mine development and exploration. Results indicate that systematic detrita1-cover sampling can be used effectively to delineate obscure deposits with sufficient accuracy to permit sampling with a minimum of trenching or drilling. Extensions of known outcroppings were traced in sufficient detail to guide lode sampling and several previously unknown tin-bearing lodes were found and sampled. Lode sampling was limited to the minimum needed to establish the reliability of detrital-cover sampling results. The results of previous lode and placer investigations are summarized and detrital-cover sampling methods and results are described in detail.

Jan 1, 1966

By W. L. Falke

This Bureau of Mines report illustrates critical path planning and scheduling techniques as applied to typical mining operations. Detailed examples of arrow diagramming and computer oriented applications of critical path methods are given. Program Evaluation and Review Technique (PERT) is discussed briefly in comparison to the Critical Path Method (CPM).

Jan 1, 1966

By H. Leitch

In laboratory experiments, the Bureau of Mines investigated melting, quenching, and sulfuric acid leaching of alumina from mixtures of albite and anorthite, and from anorthosites containing 26 to 32 percent alumina. Variations in pouring temperature, quenching and leaching conditions, were studied with respect to the extraction of alumina and impurities. Virtually all of the alumina was dissolved by leaching melted and quenched California anorthosite in boiling 16-percent sulfuric acid solutions for 15 to 30 minutes. The leach solutions were readily separable from the solid residue by conventional thickening and filtration techniques. Only 2 to 5 grams of SiO2, Fe2O3, or CaO dissolved per 100 grams of alumina. The quantity of SiOz in solution varied inversely with the duration of the leach and with the concentration of the H2SO4 solution used. Melted and quenched Wyoming and Minnesota anorthosites with SiO2:CaO weight ratios of 4.3 and 3.2, respectively, were less amenable to sulfuric acid leaching than California anorthosite with an SiO2:CaO weight ratio of 5.3. However, excellent results were obtained on the Wyoming and Minnesota anorthosites by the addition of SiO2 to these materials before melting, in quantities sufficient to adjust the SiO2:CaO weight ratios of the furnace charges to between 4 and 6.

Jan 1, 1966

By Wilbert T. Malenka

In its search for a highly productive mining system for anthracite beds pitching from 100 to 200, where conventional mobile equipment cannot be used) the Bureau initiated a longwall project by introducing a shearer drum cutter loader of European origin. Because of the undulating nature of the roof and floor and changing bed thicknesses, the machine proved inflexible and extra work was required in lifting bottom coal and blasting top coal.

Jan 1, 1966