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Jan 1, 1961

By M. R. Geer

The use of the cyclone as a dense-medium cleaning device was first described by Driessen6/ in 1945, after development of the process in the Netherlands during the German occupation of World War II. A pilot plant was built in the Netherlands soon thereafter, and the first commercial plant was built in 1948. By 1958, 18 plants were operating or under construction.7/ Thus, economic factors in Europe, where the high cost of coal places a premium on efficient cleaning, dictated rapid adoption of the cyclone. American reception of the process differed. The Bureau of Mines presented the results of its own small-scale cyclone experiments in 1946;8/ showing a sharp separation between coal and impurity; adoption by industry now is taking place. There is now much greater emphasis on the efficient cleaning of fine coal, and the first American cyclone plant has begun operating; others are planned or under construction. With the present interest in improved treatment of fine coal, the Bureau of Mines felt that additional performance data on the cyclone would be helpful to industry. Therefore, a complete, open-circuit pilot plant was built to make cleaning trials on American coals covering a wide range of washability characteristics. Five raw coals and one middling product were included in the investigation, and each was cleaned at several densities; 17 cleaning trials are reported.

Jan 1, 1961

By J. W. MacDonald

PROPERTY AND PRODUCTION: Around 100 Million Tons of Recoverable Coal are available from the approximate 10,000 acres allocated to the mine. Over 1300 acres of surface land holdings extend well beyond the limits required for plant site, storage tracks, water supply reservoir, settling ponds and waste disposal. COAL: Extensive core drilled testing confirmed the early indicated high quality of the #6 Seam Washability data show less than four percent of the' coal seam required removal to provide a superior product for the available market. PREPARATION PANT DESIGN: The limited needs enabled Preparation Plant Design to meet the requirements without inclusion of novel equipment. The simplified needs afforded ample opportunity for considering increased automation where advantage or economy was antioipated. Plant design included protection of opportunity for pre-drying in advance of air cleaning the fine coal and accommodations for addition of Dense Media separating equipment in event warranted or required by future market changes. Protection is also afforded for addition of Raw Coal Storage accommodations in event warranted. Figure I shows the Preparation Plant Flow Sheet.

Jan 1, 1961

THE Michipicoten area, one of numerous iron-bearing "Archean" segments in the Shield, contains two main types of iron formation, a normal Keewatin-type, consisting of interbanded chert, siliceous magnetite and jasper, and, gradational to this, a carbonate-sulphide type which contains large de-posits of siderite and pyrite. The carbonate-sulphide type of iron formation bears a direct and intimate relationship to the volcanic development of the area; it there-by affords some insight into genetic problems of Archeanron formation in general. The purpose of this pa-per is to summarize the geological setting of Michipicoten iron formations and to briefly review genetic aspects of recent work in the area. GENERAL GEOLOGY in largely by assorted volcanics and sediments of the Michipicoten series and younger, regional granite masses. (Fig. 1). The Michipicoten series comprises a thick assemblage of mixed flows and pyroclastics together with elastic sediments and banded iron formations. The volcanics belong to the Andesite-Rhyolite Association, and characters-

Jan 1, 1961

By H. W. Manley

SULPHUR, like the minerals of coal, iron and petroleum, is one of the essential materials in our modern expanding industrial civilization. Before discussing the salient features of the production of sulphur from the Canadian sour gas, it seems appropriate to outline the historical past and probable future utilization of sulphur. The ancient Greek writer Homer spoke of its "pest-averting sulphur" and the "divine purifying fumigation". Ancient alchemists found sulphur to be a fascinating and baffling material. The discovery of gun powder in the year of 1250, and its application to the art of war a, century later, made sulphur an important commodity in the progress of mankind. The initial manufacture of sulphuric acid in the year of 1736 by the Englishman Joshua Ward, established the basis of a chemical industry that today utilizes 80 per cent of the consumption of elemental sulphur. Commercial production of the chemical soda ash ( N a2C03) discovered in 1787 by the famous Leblanc Process, in-creased international demand for the element sulphur and marks the birthday of the Sicilian sulphur industry.

Jan 1, 1961

By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By W. A. Tiller, D. H. Lane

A simple zone melting technique for investigating the effect of ultrasonic irradiation upon ingot solidification is described. The effect of i) ultrasonic power level, ii) freezing velocity, iii) constant or variable frequency, iv) direction of irradiation, and v) transducer-cozlpling bar joint upon the grain size of type 316 stainless steel have been investigated. The results of this study support the postulate that the ultrasonic vibrations increase the nucleation probability in the layer of liquid adjacent to the freezing interface. In the first paper of this series,l the possible mechanisms whereby ingot structure may be altered by irradiating a solidifying melt with ultrasonic vibrations have been discussed. A new technique for efficiently introducing the ultrasonic energy into the solid-liquid interface region was presented and applied to ingot preparation by the consumable-electrode arc-melting technique. The experimental results support the postulate that the ultrasonic vibrations may refine the ingot structure by increasing the nucleation probability in the zone of liquid adjacent to the solid-liquid interface. The present paper describes the application of the same technique to a relatively simple laboratory-scale zone-melting apparatus. This apparatus is found to be well suited to the detailed study of ultrasonic technology in this area and allows one to determine, in particular, the minimum ultrasonic power level needed to produce a certain grain size in a particular material. The results of this study support the nucleation mechanism for grain refinement, but do not provide any deeper insight into the specific nucleation mechanism responsible for the effect. EXPERIMENT The apparatus used in these experiments is shown in Fig. 1 and illustrated schematically in Fig. 2. The material to be studied, type 316 stainless steel, was in the form of a 3/4-in. sq bar 30 in. long. This bar was placed in a square open-topped mold with open ends made from high-purity graphite coated with a flame-sprayed Al2O3, skin. Surrounding the crucible was a molybdenum susceptor with 3/8-in. diam holes spaced at 1-in. intervals along its length to serve as sight ports. A tapered transducer horn was brazed to one end of the specimen. The entire assemblage was enclosed in a quartz tube, the transducer itself projecting out one end and resting in a cooling tank. A vacuum seal between the coupling bar and the end plate enclosed one end. A similar plate and seal enclosed the other end. The system is gas tight and can be operated under vacuum or an inert atmosphere. For these experiments, flowing argon at 15 in. of Hg pressure was used. The heat source for melting the stainless steel specimen was a 2-in. long 3-kc induction coil placed around the quartz tube; this source heated the susceptor, inductively melting about a 3-in. zone of the sample by radiation. To move the molten zone at a specified rate, the induction coil was moved down the tube at this rate with the aid of a simple pulling device. Thus, the sample could be irradiated at varying ultrasonic frequencies and power levels and could be solidified at varying rates. The power input to the transducer was measured using a "John Fluke Model 120 VAW-Meter." 1 The power delivered to the interface region is probably only about 50 pct of that measured on the VAW-meter. In a typical run, when the ultrasonic power was turned on, the interface of the molten zone closest

Jan 1, 1961

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By C. N. Adams

The purpose of this investigation was to evaluate the physical and mechanical properties of high-purity titanium made by two processes. Sodium-reduced metal with 58 Brinell hardness number (B.h.n.) and electrorefined metal with 60 B.h.n. and 70 B.h.n. were used. Titanium of these hardness levels did not work-harden excessively, and beyond 40 percent cold work the hardening effect was not great. Rapid softening occurred when the metal was annealed at temperature between 300° and 600° C. Full annealing, as determined by property and microstructure studies, was accomplished after 30 minutes at 700° C. A recrystallization diagram is presented which is based on determinations of annealed grain size as a function of rolling reduction and annealing time. For reductions of less than 20 percent, exaggerated grain growth occurred during annealing; for reductions greater than 20 percent, the variation in grain size for each annealing temperature was minor.

Jan 1, 1961

By K. K. Kershner

The purpose of this research by the Federal Bureau of Mines was to investigate the recovery of tin from mine-run ores and low-grade concentrates. Over 95 percent of the total tin in such materials was volatilized to tin chlorides at temperatures ranging from 520° to 565° C. Gaseous mixtures of hydrogen and hydrogen chloride were used for reducing cassiterite to stannous oxide and for converting this compound to tin chlorides. The chlorides were swept from the reaction zone of an oscillating kiln by a rapid flow of reactant gases and collected in a condensing system. Losses of tin that occur in current metallurgical processing were prevented. Approximately the same time of treatment was required for minus 35-mesh mine-run ores and low-grade concentrates. In a continuous process, the circulating gases would require some enrichment.

Jan 1, 1961

By Dr. Ralph W. Edie

The limestone reef reservoir at Swan Hills consists essentially of a "buildup" of successively smaller atoll-like layers. Precipitation of calcium carbonate within the lagoonal area of each layer essentially kept pace with growth of the outer organic lattice. Within the reef mass, six de-positional environments characterized by specific suites of fossils (or fossil fragments) and associated limestone textures are recognized as follows: ( 1) Aerated moderately agitated water of normal marine salinity (widespread shelf or submerged reef-built platform). Thamnopora-type corals, Amphipora, "pancake" stroma-toporoids, crinoids, articulate bra-chiopods, rare rugose cup corals, and ostracods occurs in light gray-buff skeletal microgranular limestone of low permeability. (2) Semi-stagnant quiet water of normal marine salinity (leeward side of reef). Crinoids, articulate brachio-pods, rare thamnopora-type corals, Amphipora, pancake and bulbous stromatoporoids, rugose cup corals, ostracods and gastropods occur in impermeable dark brown argillaceous skeletal calcilutite with thin black bituminous shale beds and rare dark chert nodules.

Jan 1, 1961

By H. D. Kline

This publication describes mining and milling methods and costs at the Madison mine of National Lead Co., St. Louis Smelting & Refining Division, in the Fredericktown district of southeast Missouri and is one of a series prepared by the Federal Bureau of Mines on methods, practices, and costs of mining and milling throughout the United States. The are bodies of the Madison mine are known for the complexity and diversity of their are minerals. Sulfides of copper, nickel, and cobalt occur in commercial quantities with lead sulfide, which is the most valuable metallic mineral in are bodies of the Bonne Terre formation in southeast Missouri. Several attempts were made by various operators to mine the complex ores and separate the sulfide minerals before 1927 when National Lead Co. became interested in the Fredericktown district. Operating then as the St. Louis Smelting & Refining Co., the company began mining and milling ores from the Madison mine in 1944 and has operated continuously since then. A recently built refinery produces copper, nickel, and cobalt metal from a concentrate containing iron sulphides and small quantities of copper, nickel, and cobalt sulphides.

Jan 1, 1961

A spectrographic procedure applicable to the semiquantitative determination of 29 elements in tungsten is presented. The method is designed to give estimates of impurity concentrations up to 500 p.p.m. Limits of detectability range from 0.3 p.p.m. for the more sensitive elements to 100 p.p.m. for the less sensitive ones. Tungsten metal samples varying in particle size from minus 300-to 30-mesh are excited in the presence of 5 percent germanium with a direct current arc. Germanium acts to stabilize the arc, minimizes the volatilization of tungsten, and serves as an efficient carrier to sweep impurities from the tungsten into the excitation zone. Curves are presented that show the volatilization behavior of germanium, tungsten, and impurities in tungsten at different concentration levels. Data obtained were used as guides in establishing the method of analysis. In the absence of established reliable analytical procedures for determining many impurities in tungsten in the parts per million concentration range, the spectrographic method described here should prove to be helpful in evaluating high-purity tungsten.

Jan 1, 1961

By W. S. Sanner

Anthracite was used extensively as a fuel in iron metallurgy from 1840 to 1880. In 1874, 226 of the 680 blast furnaces in the United States were operating on anthracite and producing almost one-half of the Nation's pig iron. However, by 1890, railroad expansion, the development of western iron-ore reserves, and the growing use of coke decreased the importance of anthracite as a metallurgical fuel. As a result, the last blast furnace designed exclusively for anthracite use was built in 1891. Because of the increased energy requirements of our expanding national economy, the abnormally high demands during national emergencies, and the proximity of anthracite deposits to eastern steel-producing areas, interest has grown in again using anthracite in iron metallurgy. Estimates of anthracite reserves indicate a 300-yr. supply at a production rate of 30 million tons per year. These large reserves dictate the development of an adequate technology for the use of anthracite by the metallurgical industry.

Jan 1, 1961

The paper outlines the development of a solvent extraction process for the recovery of scandium, yttrium, thorium, and heavy lanthanides from waste sulphate liquor at the Port Pirie uranium treatment plant. A summary is given of known solvents for these elements, including the recently developed alkyl-phosphoric acid esters which are applicable to sulphate solutions.A kerosene solution of di- (2'-ethylhexyl) phosphoric acid (EHPA) has been suggested by some workers as a suitable solvent for fractionation of the lanthanides. Experimental work with this solvent showed that it could be used for initial recovery of the above elements from low concentrations in the complex sulphate liquor. In particular, scandium could be recovered as a high grade product by extraction with 0·lM EHPA, followed by a purification strip with 9N sulphuric acid, and final stripping of scandium with sodium hydroxide solution.To enable alkaline stripping to be used successfully, the kerosene solution of the reagent was modified by the addition of a small proportion of nonanol. Experimental work included laboratory scale batch tests and small pilot scale continuous tests.A proposed extension of the process for the separate recovery of individual heavy lanthanides, yttrium, and thorium is described.INTRODUCTIONAt the Port Pirie uranium treatment plant of the South Australian Government, large volumes of "barren liquor", free from 'uranium, are at present run to waste. This "barren liquor" results from sulphuric acid leaching of Radium,Hill uranium concentrate, followed by separation of solid residues and removal of uranium from the clear solution by ion exchange. The mineral davidite, from which the uranium is derived, contains other potentially valuable components, notably vanadium, chromium, thorium, yttrium, scandium, and the lanthanides. These constituents are...

Jan 1, 1961

Present roof bolting practices in the collieries of Australian Iron and Steel Pty. Ltd. are outlined. Roof support has been improved since introducing roof bolts and it is hoped to increase the reliability of the bolts still further.Expansion-shell, and split and wedge roof bolts five to eight feet long are placed by "Atlas Falcon" and "Fletcher" roof bolters. Both anchorage and tightening have presented some problems.Good panel supervision is required if systematic roof bolting is to be properly co-ordinated with coal production without unnecessary delay to either. Successful roof bolting can only be the product of conscientious men and supervisors who are all convinced of its value. A rigid operational code should be established early and maintained.INTRODUCTIONRoof bolting is a method of support which is permanent and reduces or eliminates the need for other support; The method was pioneered in America and was first experimentally investigated in Australian collieries at Elrington in 1949 (McKensey, 1953). Pneumatic installation methods were employed. Subsequently, a method of using standard hand-held electric coal drills was developed at John Darling Colliery (Horseman, 1954). Pneumatic roof bolting equipment was first operated in the collieries of Australian Ironand Steel Pty. Ltd (A.I. &. S.) in 1951. Since then various hydraulically operated mobile machines have been installed in Australian collieries and these, together with improved pneumatic equipment, form the two present basic methods of placing ,roof bolts. Roof bolt anchorage is achieved by either split and wedge or expansion-shell bolts.The two broad types of roof bolting are 1. consolidation of strata, and 2. suspension support.

Jan 1, 1961

By J. T. McCartney

Thin sections of coal have been prepared for many years either by cutting on a microtome (1,2)5 or by grinding and polishing (2,1). Specimens of most coals had to be demineralized in hydrofluoric acid and softened in caustic solutions before they could be successfully cut with a conventional microtome. Some lignites could be cut without pretreatment. Jeffrey (1) obtained sections from coals of all ranks, although long and tedious pretreatment was required for anthracite. His sections were less than 1 cm.2 in area (probably much less for high rank coals) and about 5 microns thick. Thiessen (2) also cut sections of softened coals, mostly of low rank. His sections were a few square millimeters in area and about 3 microns thick. However, Thiessen preferred ground and polished sections for detailed studies because they were larger and had not been chemically attacked by softening media. He prepared ground sections as large as 4 cm.2 in area and usually 5 to 10 microns thick. Thousands of such sections, covering complete column samples of many coal beds, were studied for a number of years (4). With the development of the electron microscope and increased interest in quantitative optical studies of coals, a need for much thinner sections arose. However, no suitable technique for preparing such sections was known until Fernández-Morán developed a diamond knife for cutting ultrathin sections of hard materials (5). Workers at the Centre d'Etudes et Recherches de Charbonnages de France applied this new tool to the cutting of coal sections and have recently described their technique to the Burg, of Mines. Using their methods, with some modifications, researchers of the Bureau of Mines have succeeded in cutting ultrathin sections of coals ranging in rank from lignite to

Jan 1, 1961

By R. J. Leary

Significant improvements in surface conditions or mechanical properties of steels have been attributed by several investigators to ladle additions of small quantities of rare-earth metals or their oxides. To investigate systematically these effects in wrought and in cast plain carbon and alloy mechanical steels containing approximately 0.35 percent carbon, heats of four representative compositions were melted by the Bureau of Mines in a 4-ton open-hearth furnace. Each heat was cast into three sets of ingots to exemplify respectively, treatments with (1) rare-earth metals, (2) rare-earth metal oxides, and (3) an untreated set as a control. The development of melting, casting and rolling practices is described and discussed. Lance injection of oxygen shortly after melt raised the temperature of the metal immediately as much as 500° F., principally because mechanical agitation exposed the high-carbon metal to the flame and furnace root. An exceptional degree of superheat in the metal at the termination of the refining period was attributed to oxygen injection during the refining period. Bath temperatures higher than industrial practice were permitted by the all-basic furnace lining. Rates of carbon elimination as high as 0.036 percent carbon per minute were achieved by oxygen injections.

Jan 1, 1961

By James E. Mauser

This report deals with the investigation of a continuous process for producing pure zirconium. It covers the construction, operation, and maintenance of the semicontinuous reactor. The report covers a study of test variables, such as reactor temperature and reluctant charge weights, and evaluates the results, such as billet metal hardness, residual billet salt content, and suitability of a purified billet as a consumable electrode for arc melting. The purpose of this project was to develop an inexpensive and continuous process for producing pure zirconium. The process developed, termed the semicontinuous reactor process, produced billets of compacted zirconium sponge. The metal was produced by reducing zirconium tetrachloride with sodium and magnesium beneath molten byproduct salt. Hydraulic rams at each end of a vertical reaction tube compacted the sponge and ejected it as a billet. These billets were purified by heat under vacuum to remove entrapped salt. The goal was to utilize the purified billet directly as a consumable electrode for arc melting.

Jan 1, 1961

By Jr. J. L. Ryon.

Experimentation with ammonium nitrate-fuel oil mixtures at three underground salt mines revealed its excellent applications at those properties. The author relates the present blasting practice used at these mines by the Intemzational Salt Co. The International Salt Company is presently performing blasting operations with a pneumatically -placed ammonium nitrate-fuel oil mixture at three rock salt mines, and plans its use in the near future at its new Cleveland mine. Use of ammonium nitrate is saving the company approximately $250,000 annually. With rapidly increasing operating expenses and increasing competitive pressure resulting in lower prices, savings such as those realized through the use of ammonium nitrate are vitally important. ORIGINAL INVESTIGATION AND EXPERIMENTAL ACTIVITIES The three mines presently involved are located at Detroit, Mich.; Avery Island, La.; and Retsof, N. Y. Initial experiments were conducted at the Detroit mine where a detailed investigation was carried on to determine the significance of the static electricity factor when blowing ammonium nitrate into drill holes in which millisecond delay electric blasting caps had been placed. Although the information developed at the Detroit mine was passed along to the other mines, each mine independently pursued its own course of inves- tigation. This fact, plus the differing mining conditions, resulted in slightly different operational procedures at each mine. Some of the varying statistical data are shown in Table I, and data common to all three International Salt Company mines are shown in Table 11. BLASTING PROCEDURE AT THE DETROIT MINE This mine has been using the ammonium nitrate-fuel oil mixture for more than two years on a full time production basis and represents the successful detonation of several hundred thousand holes. Results have been excellent and the blasting cost has been reduced many times. The actual operation at Detroit consists of adding the fuel oil to the bags of ammonium nitrate by means of a portable fuel oil tank complete with hose, nozzle, and metering device. The bags of the ammonium nitrate-fuel oil mixture are transported to the working face from the oiling area by means of a jeep-drawn trailer. At the face, the ammonium nitrate is placed on the elevating platform of a powder-load ing rig which consists of a pneumatically-tired, large fork-lift truck with a fully insulated elevating platform constructed on the forks. The placement of the dynamite primer and the pneumatic placement of the ammonium nitrate is a two-man operation. First, one cartridge of the primer is placed in each hole on the line of holes which can be reached from the loading rig platform. The plastic hose is then inserted into the hole and pushes the primer to the back of the hole. The proper charge of ammonium nitrate is then placed in the pneumatic placement machine and,

Jan 1, 1961