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By J. G. Donaldson

The Bureau of Mines investigated the formation of boron and boron-carbide coatings by vapor-phase reactions. Optimum parameters were determined for hydrogen reduction of boron trichloride and for the fonnation of boron-carbide coatings on graphite by reaction with the depositing boron. At 1,300° C, about 85 percent of the boron was deposited. Tungsten substrates did not react with the boron deposit; other substrates reacted to various extents. The hydrogen reduction of boron tribromide was briefly investigated. Boron carbide was deposited at 1,300° C by adding methane to the boron trichloride-hydrogen feed gas. The chemical composition of the vapor-deposited boron carbide approximated B4C. A method of etching B4C was developed to study its microstructure. When boron was deposited on graphite at 1,500° C, very hard, uniform, strongly adherent coatings of B4C were formed that might be useful in rocket nozzle applications.

Jan 1, 1968

By Sabri Ergun

Previous studies of magnetic separation of pyrite from coals have been reviewed critically. Magnetic susceptibilities of United States coals of differing rank have been measured. The effects of crushing, magnetic mixing, drying, weathering, and heat treatment on the enhancement of the magnetism of pyrite have been analyzed. The importance of size distribution of pyrite in the coal and the necessity of crushing to liberate the pyrite has been discussed. It has been found that the inherent susceptibilities of the carbonaceous, mineral-free portions of coals (? -0.5 X 10-6 in cgs units) and of relatively pure pyrite isolated from coals (? -0.3 X 10-6) do not permit efficient separation of pyrite from coal; the average susceptibility of the magnetic fraction of coal must be raised to 3 X 10-6. Friction forces encountered in crushing sedimentary pyrite embedded in coal do not increase its susceptibility. Subsequent weathering or heat treatment below 400° C leads to the formation of iron sulfate and hence increases the effective paramagnetism of pyrite. Ferromagnetic compounds of iron are not formed in significant quantities at temperatures below 400° C. The degree of liberation and apparent susceptibility of pyrite are the most important parameters in its separation. It is concluded that effective beneficiation of coals can be achieved by magnetic separation. A sufficient increase in the susceptibility can be achieved by converting less than 0.1 percent of pyrite into ferromagnetic compounds of iron. Such conversions occur only at temperatures >500° C. An investigation of the dielectric properties of coals and pyrite in the frequency range 0.1 to 60 Mhz indicates that the imaginary dielectric constant of the pyrite is about 100 times larger than that of coal. Exploratory experiments indicate that pyrite can be selectively heated to temperatures above 500° C without appreciable rise in the temperature of coal. It appears that dielectric heating of coals in the Ghz frequency range is the most feasible method of enhancing the paramagnetism of pyrite.

Jan 1, 1968

By J. L. Walter

Tungsten ingots with and without small amounts of aluminum, silicon, and potassium were prepared by conventional powder-metallurgy techniques and hot-rolled to 0.001-in.-thick sheet. The ingots were rolled three different ways: I) initially cross-rolled, then straight-rolled; 2) straight-rolled, and 3) straig-ht-rolled, then cross-rolled. Total reductions were 99.8 pct. Samples of the sheet were annealed, in vacuo, at temperatures from 1200" to 2200°C. Substructures and textures were determined by transmission electron microscopy and X-ray diffraction. The doping agents were found to form particles of mullite (Al,Si,O,,) which, on rolling., appear to form strings of particles aligned parallel to the rolling direction. These strings of purticles are associated with an increase in the recrystal-lizution temperature from 1400°C for undoped sheet ThE addition of small amounts of aluminum, silicon, and potassium to tungsten has a profound effect on the grain structure of drawn and recrystallized wire.'" The grains generally do not occupy the entire cross section of the wire and have lengths many times the wire diameter. The grain boundaries are, in general, nearly parallel to the wire axis and have long ''fingers" projecting one into the other as may be seen in Fig. 1, a longitudinal section of recrystallized doped wire. When unsuitable additions or no additions are made or the wire is not sufficiently reduced during draw- to 2000°C for doped sheet. The particles also limit lateral grain growth while allowing growth parallel to the rolling direction. This results in the formation by primary re crystallization of large highly elongated grains of specific preferred orientation. The undoped sheet recrystallized to small equiaxed gains. The preferred orientations of the large grains were determined from axis density plots to be (113) (691). (0i3) (362), (116) (304) types for the initially cross-rolled then straight rolled material. These orientations are similar to the orientations of the large elongated grains in doped and heavily drawn tungsten wire. The nucleation of the large grains appears to occur by recovery of certain of the polygonized regions of specific orientation, followed by strain-induced boundary migration.

Jan 1, 1968

By J. C. Draper

This subject was introduced last April in a paper presented in Birmingham, Alabama, by James E. Elkin, General Superintendent of Duquesne's Coal Department. This paper will cover some of the same data and in addition it will update and further describe our experience. Our Portal No. 3 was started in June 1965 with battery tractor-trailer face haulage. This mine is operating in the Sewickley seam in Dunkard Township, Greene County, in Southwestern Pennsylvania as shown on Fig. 1. The Warwick group of mines fronts on the Monongahela River and extends westward for some ten miles as shown on Fig. 2.

Jan 1, 1968

By M. Boucraut

The authors investigate the influence of the basicity index CaO / Si02 on the sintering properties of hematite ore mixtures. The experimentation was performed with three different mixtures of ores from Tazadit, Nimba, Mano-River, Itabira, Marcona, Goa, Mapawa and Cassinga. Increasing the basicity index CaO / Si02 between 0.1 and 3, chiefly through limestone admixture makes possible to reduce the thermal consumption of sintering and to improve the physical and chemical properties of the sinter. In the case of a plant using hematite ores, it seems interesting to produce an hyperbasic sinter and to complete the blast furnace burden with calibrated ore or acid pellets.

Jan 1, 1968

Sphalerites from Devonian cassiterite-sulphide deposits and Pb-Zn-Ag fissure veins have similar ranges of Cd contents, but the average Cd and Fe contents could indicate a small initial difference in availability of Cd between the Zeehan-Renison Bell district and the Mt. Bischoff-Waratah district. Sphalerites from banded Pb-Zn deposits (Rosebery and Hercules) are characterized by low Cd content which is a world-wide feature of such deposits in exIrusive rocks, and may indicaIe a genetic relationship between ore deposition and vulcanism.

Jan 1, 1968

By Robert K. Linn

The New ldria Mining District is in the southern part of the Diablo mountains of the California Coast Range, 140 miles southeast of San Francisco. The district, noted primarily for quicksilver, also has become important recently as a producer of short-fiber chrysotile asbestos. Between 1853 and 1966, the New Idria district produced 568,092 flasks of quicksilver valued at about $55,600,000, 99 per cent of which was recovered from one deposit, the New Idria mine. In 1944, the district was ranked third in all-time production of North American quicksilver districts, and, since that time, the New Idria mine produced an additional 129,045 flasks, placing the district and the New Idria mine second in all-time production. The major structure of the region is the northwest-trending Coalinga anticline consisting of an asymmetric dome of sedimentary beds ranging in age from Jurassic to Quaternary and marked at its northwest end by an oval body of sheared serpentine 14 miles long by 4 miles wide. The serpentine core, rimmed by Franciscan sandstone of probable Jurassic age, was uplifted in stages between Jurassic and Quaternary time and was intruded along a ring of faults into beds of the Panoche Formation of upper Cretaceous age. The core of serpentine and Franciscan rocks is the locus of about 20 quicksilver mines that rim the faultbounded core and lie within the serpentine mass. The host rock of the most productive deposits is altered Panoche shale and sandstone that lies intermittently along the perimeter of the core. Deposits of the New Idria group of mines and those of a few other small mines lie along the northeast contact in the footwall of the New ldria thrust fault, and a few others occur on steep normal faults around the south and southwest. The chief ore mineral in all quicksilver mines is cinnabar, but minor amounts of metacinnabar and native mercury are found in some of the mines. Ore shoots were deposited in fracture zones and stockworks in altered Panoche shale and sandstone and in definite fissure veins in Franciscan sandstone. Rocks made highly amenable to fracturing by hydrothermal alteration were fractured extensively by late faults. The resulting fracture zones, located along the late faults and at changes in strike or dip of the hanging wall or footwall, are the principal controls of most ore shoots. The largest and richest ore shoots are those of the New Idria mine. The major ore bodies occur in fractured shale and sandstone beneath the New ldria thrust fault at its junction with major tear faults.

Jan 1, 1968

By Irving Wender

This report describes Bureau of Mines experiments and reviews the work of others on the exposure of coal and coal-derived products to gamma rays and some other types of radiation. Results are presented on tests of three bituminous coals and a lignite that had been pulverized to minus 200-mesh particles and exposed to 1,000 megaroentgens of gamma irradiation from spent-fuel elements of a nuclear reactor. Of about 20 chemical and physical tests in Bureau work, only mass spectrometry of gases evolved during vacuum pyrolysis of the coals to 450° C gave results indicating differences in the irradiated and unirradiated samples. Mass-spectral distribution curves for CO and CO2 evolution showed fewer irregularities (reversals of curvature) for irradiated coals; thus, mass spectrometry appears to be the most sensitive method for determining radio-induced changes in coal. It is concluded that coal is not significantly altered by gamma irradiation owing to the resistivity of its highly condensed ring structure. High-level gamma irradiation, therefore, is unlikely to prove advantageous in coal processing and utilization. Specially treated coals, because of resistivity of coal to radiation damage, may be useful as an absorbent in processing radioactive wastes.

Jan 1, 1968

"Developing markets for western metallurgical coal have continued to stimulate considerable exploration activity in the Rocky Mountain foothills and to influence major segments of a wide-ranging carbonization R&D pro-gram. Adjunct studies have included expanded petrographie investigations.Coal preparation has• been principally directed toward utilization of prepared small coal and was, like much of the year's combustion work, strongly influenced by concern over atmospheric pollution. Particular attention has been given to desulphurization and to the suppression of pollutants in combustion systems.In the area of non-fuel utilization of coal, interest has centered on plant nutrients and on a series of coal-based carbons which, inter alia, possess utility as filtration media.Other projects included the development of improved sampling and analytical methods, investigations into the effect of storage on coal proper-ties and R&D in solids pipelining. In addition, a significant volume of basic 'uncommitted' research has been maintained."

Jan 1, 1968

Jan 1, 1968

By Thomas M. Larimer

Prior to April, 1961, the coal charge to Clairtonts coke oven batteries was 3" x 0" mine waslied coal having approximately 6.0% to 7.0% moisture. Even at this size and moisture content, the arching, rat-holing and hang-up was excessive and the effective live storage of coal was only 60% to 70% of the rated capacity of the coal bunkers, depending upon the moisture of the coal. In addition, many production delays were encountered in the time and methods required to fill the larry cars. The need for an improved metallurgical coke led to the introduction of pulverized coal to a portion of the plant in 196 1. When the full potential of the pulverizing equipment was realized, we were able to serve seven batteries in our second unit of batteries with pulverized coal through two coal bunkers. The discharge hoppers of these bunkers were equipped with air vibrators to assist the flow of pulverized coal into the larry cars. The vibrators were helpful in this respect but required considerable maintenance and caused damage to the bin plates.

Jan 1, 1968

Jan 1, 1968

By Roy A. Anderson, Roger H. McConnel

The Metaline district from 1906 through 1965 has produced nearly 16 million tons of ore yielding 400,808 tons of zinc and 178,062 tons of lead. The sediments, ranging from Precambrian into the Devonian, are schist, phyllite, conglomerate, greenstone, quartzite, limestone, dolomite, and carbonaceous slates. Quartz monzonite and granodiorite of the Cretaceous(?) Kaniksu batholith are exposed over a large area beginning a few miles south of the district. There is minor Tertiary conglomerate and basalt. Abundant glacial deposits obscure much of the bedrock. Northeasterly trending folds, having steep to overturned northwesterly limbs, and thrust faults, striking northeasterly and dipping southeasterly, characterize the deformation of the Precambrian and Paleozoic rocks. Recent drilling indicates that the Slate Creek fault, too, is also a southeasterly dipping thrust fault. This new evidence suggests that the Valley Block, like the other major structural blocks, may in part be a thrust plate rather than a graben, and that thus the district may have greater structural unity with the surrounding region than has heretofore been apparent. The Cambrian Metaline Formation of limestone and dolomite contains essentially all the lead-zinc mineralization. Most of the ore mined to date has come from a carbonaceous and irregularly siliceous breccia of sedimentary and diagenetic origin, locally called the "Josephine Horizon," that makes up the top few to 200 feet of the formation. The Josephine Unit is a breccia of gray limestone, coarse light gray dolomite, very thin-bedded, dark gray siliceous dolomite, and "zebra rock" believed to be of algal origin, embedded in a matrix of black dolomite or black jasperoid or some mixture of these two. The jaspcroid fragments and irregular blobs embedded in the black dolomite matrix and the jasperoid laminae in the very thin-bedded dark gray dolomite suggest that jasperoid was formed at the same time as the breccia matrix and as the laminated dolomite. So too, the marked tendency of sphalerite and galena to be disseminated mainly in the dark breccia matrix and their tendency to be most abundant in the jasperoid laminae of the very thin-bedded dark gray dolomite, even where the mineralized and laminated dolomite is fragmented and engulfed in black dolomite breccia matrix, suggests that in these ha bits the sulfides also were deposited contemporaneously with the sediments. Yet very commonly, veins and vague veinlets and patches of white quartz, usually carrying rather coarse sphalerite and sometimes galena crosscut all rock types. These contradictory relationships throughout the Josephine Unit suggest that both the black jasperoid and the sulfides were original constituents of the Josephine Unit but that, locally, they later were remobilized and deposited as white quartz and coarser grained sulfides. Possibly, at least in part, this "metamorphism" is one of the effects produced during or shortly after the intrusion of the Kaniksu batholith.

Jan 1, 1968

By Philip C. Good

Red mud residue from Bayer process treatment of Jamaican bauxite was dewatered in batch and in continuous centrifuges. Solids content of the residue was increased from its original value of 20 to 25 percent to about 40 percent by centrifuging. Clear effluent amounting to approximately 40 percent of the slurry liquid was recovered containing dissolved alumina and soda values for potential recycle to the alumina plant" Addition of a chemical flocculant to the centrifuge increased capacity by about 35 percent. Manufacturer's estimate of large-scale equipment requirements, based on data collected in this investigation, was that a proposed installation for dewatering 16,000 tons per day of Jamaican red mud would require twenty-two 24-by 60-inch solid-bowl-type centrifuges. Cost analysis of a proposed installation, based on a Jamaican red mud tonnage of 16,000 per day, is included also.

Jan 1, 1968

By Nathaniel Arbiter

A fully-instrumented driving mechanism has been constructed to study the power, aerating and solid suspension characteristics of several laboratory flotation machines. Machines operating over normal flotation speed ranges give constant power numbers in liquid' systems indicating that they operate under fully baffled turbulent flow conditions. Owing to lack of geometrical scaling, power numbers for different sizes of cells of the same make are different. Even larger differences occur between cells of different manufactures. For a given impeller, varying the tank size did not significantly affect the power consumption. Tank geometry and baffling has a slight effect on power consumption with shrouded impellers. For a given impeller speed, suspension height decreases while power increases with increasing mass of solids in suspension. While power consumption is hardly affected by particle size and clearance between the impeller and tank bottom, the suspension height significantly increases as clearance increases and as particle size decreases. Aeration was found to affect not only power but also the suspension characteristics of the machine. For closely sized particles drastic sedimentation occurred when a critical value of the air flow number was exceeded. The critical air flow number decreased with increasing particle size. This effect was less marked with a wide particle size range. The self-aerating capacity of flotation machines increases with cell size at a given speed for the same impeller-shroud system, but decreases in the presence of frother and solids. Equations have been established for correlating all of the studied variables. Data taken from the literature were also correlated with these equations.

Jan 1, 1968

By Richard Thomas Newcomb

The trend towards proportionately rising volumes of surface mining through- out the world and especially in the United States has led some observers to predict that the future of underground mining is quite limited. Certainly, the simple extrapolation of current trends1 gives evidence of a compelling sort for the hypothesis that technological progress is proceeding at a faster pace in surface than in underground mining. This paper attempts to examine the basis for these predictions by searching the historical record on differential rates of productivity as these are observed in iron ore and coal mining. In recent years economists have discussed "technology gaps" among industries or segments of the same industry, by which they mean that mechanisms for invention and its diffusion are faulty or retarded in such a way that feasible cost-cutting innovations are not applied or developed, even though technicians regard them as practical.2

Jan 1, 1968

Resonance re-emission from nickel vapour affords a convenient method for isolating the resonance lines at 3415A, 3515A, and 3524A. The vapour is generated by cathodic sputtering and is illuminated by light from a nickel atomic spectral lamp. The resonance lines thus isolated can be usefully employed for absorption measurements on mineral samples where the nickel concentration is too high for measurements with the more sensitive line at 2320A. A spectrophotometer employing a resonance lamp as monochromator possesses several advantages where a great number of determinations are made under routine conditions. The wavelength setting is stable under even the most rigorous conditions and with the provision for automatic setting of full scale deflection the instrument requires virtually no adjustment. The instrument has been used under routine conditions for the determination of nickel (in the range O· 05-2 per cent) in mineral samples.

Jan 1, 1968

By Gerald W. Elger

To determine the feasibility of removing nonferrous metal impurities from automobile scrap by thermal treatment in a rotary kiln, the Bureau of Mines conducted four series of tests with synthetic scrap mixtures heated at various temperatures under oxidizing and reducing conditions. The treated scrap mixtures were melted in an electric-arc furnace and cast into small ingots for impurity evaluation. Analyses showed that the ingots were essentially free of residual metal impurities except for copper. Test data indicated that in an oxidizing atmosphere the percentage of copper removed increased with treatment temperature. Percent of copper removed in a reducing atmosphere was found not to be temperature dependent. A significant finding was that copper was embrittled under some of the operating conditions and was mechanically removed by fragmentation.

Jan 1, 1968

By H. J. Gluiskoter

The chlorine content of the coals in the Illinois Basin ranges from 0.00% to more than 0.60%. The chlorine content of the Herrin (No. 6) Coal has been mapped on a regional scale and, in general, increases with the depth of the coal. The depth-chlorine correlation exists because the coal is in apparent equilibrium with the composition of the ground water associated with it, and the salinity of the ground water generally increases with depth. At least part of the chlorine can be easily removed from the coal in the laboratory. In a natural weathering experiment, chlorine values decreased markedly during an 8-week period. Results to date indicate that none of the coals studied has a sufficiently high chlorine content to make it unusable in high-temperature steam boilers, although special steps may be necessary in the preparation or utilization of some of the highest chlorine coals. Investigations into the occurrence and distribution of chlorine in Illinois coals have been in progress at the Illinois State Geological Survey for over 35 years. Since 1948, chlorine analyses of face channel samples and of drill core samples of coal have been made routinely. The increased interest in chlorine and alkalies in coal in the U.S. followed that in Europe, where power plants during World War II were called upon to produce at higher levels than previously and with less down time for maintenance. Higher steam temperatures were reached, resulting in increases in the amount of fouling of external heating surfaces and in corrosion of boiler tubes when high chlorine coals were used. Early studies of the problem showed that coals with high chlorine content were more likely than those low in chlorine to cause difficulties in installations fired with powdered fuel. Crossleyl reported that the first rule of thumb developed for British coals was that coals considered to be high in chlorine (more than 0.30%) caused the most trouble, those intermediate in chlorine content (0.15% to 0.30%) were less likely to cause difficulties and those low in chlorine (less than 0.15%) generally were not associated with alkali bonded deposits and corrosion. However, this relatively simple picture was not adequate to characterize the difficulties that could be expected during the utilization of a large number of coals and Crossley1 developed another scheme for assessing the chances of superheater corrosion. This scheme took into consideration the observation that coals high in sulfur as well as chlorine are more likely to cause corrosion and fouling than coals low in sulfur and high in chlorine. Crossley also considered the ash content. When two coals had the same chlorine and sulfur contents, the one with the greater amount of ash would be the less likely to cause difficulties. Knowing only the amount of chlorine in a coal obviously will not give all the answers. Indeed, the significance of the chlorine content has been much discussed and it has been suggested that perhaps the total alkalies are a better indicator of possible troubles. The observation that the deposits that form

Jan 1, 1968

Jan 1, 1968