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By James A. Whelan

The Bureau of Mines sponsored research studies of variables in rotary drilling, done in the Department of Mineral Engineering, University of Minnesota. By studying carefully controlled drilling with good instrumentation, it was hoped to obtain a better understanding of rock failure during drilling and of the stresses in drill bits during drilling. Experimental procedures and equipment are described. From these studies it was concluded that 1. Thrust requirements, other things being equal, are proportional to the total length of cutting edge in the bit. 2. Data from penetrating a wedge into rock under thrust only are not directly applicable to rotary drilling. 3, In rotary drilling the initial wear on a bit greatly decreases penetration rate under any given set of conditions; however, after initial wear the effect of wear on penetration rate is reduced. 4. An increase in rotary speed increases the overall penetration rate but decreases the penetration per revolution. 5. An increase in thrust increases the overall penetration rate and the penetration per revolution. 6, Torque on a drill bit is proportional to both penetration rate and bit diameter. 7. For small-diameter holes full-hole drilling will save both drilling time and energy compared with pilot drilling followed by reaming; for large-diameter holes pilot drilling-reaming is advantageous in both respects,

Jan 1, 1962

Spectrochemical methods were developed to determine beryllium in the concentration range 0.0015 to 4.0 percent in siliceous mineral beneficiation products. Two methods are described. They are (1) a fusion-pellet-spark procedure (spark method) and (2) a sustaining alternating-current arc procedure (arc method). In the spark method the sample is fused with lithium tetra-borate and vanadium pentoxide. The resulting bead is crushed, mixed with powdered graphite, and briquetted. This is analyzed spectrographically using controlled high-voltage spark excitation. In the arc method the sample is diluted with germanium metal, graphite, and vanadium pentoxide. Weighed charges are packed into cupped graphite electrodes and subjected to excitation with a sustaining alternating-current arc. Vanadium serves as internal standard for both methods. Effects due to matrix variations in samples and standards are eliminated either by fusion with lithium tetraborate in the spark method or by dilution with germanium and graphite in the arc method. Beryllium determinations show deviations from accepted chemical values of approximately 5 and 8 percent for the spark and arc methods, respectively. Analyses can be made more rapidly by the arc procedure with a sacrifice in precision and accuracy. Either method can be applied to the determination of beryllium in silicate rocks.

Jan 1, 1962

By Frank A. Peters

This Bureau of Mines report is the second of a series of process evaluations planned to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. Included in these evaluations are recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The processes considered in this report are designed to extract alumina as aluminum chloride from calcined clay with 20 percent hydrochloric acid and to remove the silica residue by filtration. Iron is removed by one of the following processes: Isopropyl ether extraction, in which iron chloride is extracted before decomposing the aluminum chloride; gas precipitation, in which the aluminum chloride is precipitated with hydrogen chloride while leaving the iron chloride in solution; gas precipitation-isopropyl ether extraction, in which the aluminum chloride from precipitation is extracted with isopropyl ether, if necessary; caustic purification, in which a crude alumina is produced and then purified by a modified Bayer operation; or sinter purification, in which a crude alumina is produced and then purified by a lime-soda sinter operation. For plants producing 1,000 tons of alumina a day the estimated operating costs per ton of alumina are: [Isopropyl ether extraction process $ 65.09 Gas precipitation process 89.04 Gas precipitation-isopropyl ether extraction process 119.65 Caustic purification process 73.79 Sinter purification process 80.47] The estimated fixed capital costs per annual ton for these plants on a Marshall and Stevens chemical equipment basis of 240.0 are: [Isopropyl ether extraction process $229.03 Gas precipitation process 287.16 Gas precipitation-isopropyl ether extraction process 356.59 Caustic purification process 266.48 Sinter purification process 279.13]

Jan 1, 1962

By C. H. Riggs

This report describes the development, oil recovery, and potentialities of productive formations in the Hall-Gurney field, Russell County, Kans. It is presented as part of a general program to aid and promote increased recovery from petroleum reservoirs. The report is based on studies of well logs, drill cuttings, and oil-and water-production histories of individual wells and leases. The geological interpretations follow closely those in published literature with only slight local modifications. Oil and water analyses, made at a Bureau of Mines research center, were supplemented by many analyses obtained from oil-producing and service companies. The Hall-Gurney field, in south central Russell County, Kans., (fig. 1) was discovered in 1931 but was not developed extensively until 1941. By 1960 the rate of oil production from the field had declined to the extent that many wells were abandoned. In some areas natural productive forces have effected good recovery. However, in other areas inefficient waterflooding, both natural and accidental, has adversely affected recovery potentialities.

Jan 1, 1963

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Nicholas County, W. Va. It is one in a series describing coals suitable for producing metallurgical coke, either as mined or after beneficiation. Almost 5 million tons of coal were produced in Nicholas County, W. Va., in 1960, of which over 2.6 million tons were cleaned in eight preparation plants. It has been estimated that over 6 billion tons remained in the county as of December 31, 1960, in beds 12 inches and more thick.

Jan 1, 1962

By Louis A. Panek

Tests of mine-roof models in a centrifuge show that the suspension effect due to bolting a horizontally bedded mine roof with frictionless surfaces of contact between beds depends principally on the number of bolted beds and their relative flexural rigidities, provided that sufficient bolt tension is exerted to prevent strata separations at the bolt locations. Strata separations tend to occur in the unbolted roof mainly because the beds have unequal thicknesses. "Suspension effect" refers to the transfer of part of the weight of weaker or thinner beds to the flexurally more rigid beds by roof bolts or by any other means. The factors investigated were number of beds in the bolted unit, bed thickness, modulus of elasticity of beds, length of bolts, spacing of bolts across and along the opening, bolt load, and intensity of roof load. The general principles of behavior of the bolted roof beds are explained by an approximate theory. Model test data are used to validate the theory and to obtain an expression for the "suspension efficiency". As the suspension effect actually observed in the models is smaller than that predicted by the approximate theory, the suspension efficiency in general is less than unity. Mathematical expressions are obtained for (1) the change in roof bending stress due to the suspension effect, which is needed for design of a roof-bolting system, (2) the change of roof deflection due to the suspension effect, which may be useful for evaluating the effectiveness of a roof-bolting system, and (3) the bolt load or pre-load that is required to achieve the desired reinforcing effect.

Jan 1, 1962

By Lowell Stroud

This report is the third in a series presenting equilibrium vapor-liquid data for helium-bearing natural gases. The first two reports contained phase data for the gases processed for helium at the Bureau of Mines Amarillo and Exell, Tex., helium plants. The present report offers similar information for a lower-helium-content (0.75 mole-percent) natural gas to be processed in the Department of the Interior's long-range helium-conservation program. A windowed-cell apparatus was used to obtain 218 samples of equilibrium vapor and liquid phases at 73 experimental conditions ranging in temperature from -100° F to -275° F and in pressure from 100 to 500 psi. From the phase data, the condensation characteristics, helium solubility, and equilibrium-vaporization-coefficient data for helium, nitrogen, and methane were evaluated. The effect of using a. preliminary hydrocarbon trap upon the subsequent vapor-liquid compositions is reported. A brief comment regarding the composition effect of passing the gas through a gasoline-removal unit is also included.

Jan 1, 1963

By H. E. Peterson

This report revises an earlier publication by the Bureau of Mines on tungsten analytical procedures and expands the coverage by including appropriate procedures for the critical impurity elements that commonly occur in tungsten ores and concentrates (13).3 The basic methods described are not original, but many of the modifications to improve reliability and sensitivity were developed by the Bureau. Gravimetric and colorimetric methods currently used for the determination of tungsten in ores, mill tailings, and concentrates are described. Colorimetric procedures are preferred for low concentrations of tungsten, whereas either procedure is satisfactory for moderate concentrations. Conversely, a gravimetric method is preferred for the determination of tungsten in concentrates.

Jan 1, 1963

By R. O. Dannenberg

Exploratory research was conducted to ascertain the feasibility of recovering beryllium from Spor Mountain, Utah, ore by the sodium fluosilicate (Na2SiF6) method used industrially for processing beryl. Na2SiF6 requirements to form water-soluble salts of beryllium were determined for three different samples--two clayey ores containing 0.6 and 1.3 pct BeO, respectively, and a calcareous ore containing 0.6 pct BeO. The ores were sintered with Na2SiF6 at 750° C for 3 hours. About 80 pct of the beryllium was rendered water soluble by sintering the 0.6-pct BeO ores with 30 and 40 lb Na2SiF6 per lb BeO contained in clayey and calcareous ores, respectively. The higher grade 1.3-pct BeO clayey ore required only 20 lb Na2SiF6 per lb BeO to solubilize over 80 pet of the beryllium. As the 0.6-pct BeO clayey ore was possibly the most representative of the deposit as presently delineated, leach liquor prepared from this sample was treated to recover beryllium salts. About 60 pet of the beryllium contained in the ore was recovered as beryllium hydroxide, which then was calcined to yield a 99-pct BeO final product by means of the following operations: (1) Sintering with Na2SiF2, (2) leaching with water, (3) precipitating crude Be(OH)2 by adding NaOH, (4) filtering to separate the hydroxide from the NaF solution, (5) redissolving the crude Be(OH)2 in excess NaOH, (6) filtering to reject caustic-insoluble impurities, and finally (7) boiling the Na2BeO2 filtrate from (8) to precipitate pure Be(OH)2. Reagent consumption was 49 lb Na2SiF6 per lb BeO recovered and 17 lb NaOH per lb BeO.

Jan 1, 1963

By A. R. Taylor

Low-temperature heat capacities of cesium chloride (7° - 300° K) and cesium iodide (13° - 300°K) were measured with an adiabatic calorimeter. The heat-capacity measurements were analyzed graphically to determine smooth values of heat capacity, entropy, enthalpy function, and free-energy function at 10° K intervals and at 273.15° and 298.15° K.

Jan 1, 1963

By P. T. Brooks

The selective recovery of nickel and cobalt from impure raw materials is being investigated by the Bureau of Mines as part of a program to develop improved procedures for preparation of pure metals. A combination solvent extraction-electrolytic process has been developed in the laboratory that enables preparation of high-quality nickel and cobalt from nickel oxide containing, in percent, 76 nickel, 0.8 cobalt, 0.5 magnesium, 0.2 iron, and lesser quantities of copper, zinc, and other metals. The oxide was smelted, using carbon as reductant, and cast into anodes. These anodes subsequently were dissolved in diaphragm-type electrolytic cells. Nickel and cobalt were deposited separately from appropriate electrolytes, concurrent with dissolution of the impure anodes. Anolyte containing nickel and cobalt in the form of chlorides and sulfates was treated for removal of impurities and separation of nickel and cobalt. First, iron and aluminum were removed as hydroxides by adding nickel hydroxide to raise the pH of the anolyte from 2.3 to 4.5. Next, the pH was adjusted to 2 by adding hydrochloric acid, and the solution was treated by solvent extraction to separate nickel and cobalt.

Jan 1, 1963

By Charles Prasky

This report describes and appraises recent progress in the development of a differential sulfatizing process for recovering a ferrograde manganese oxide from low-grade manganiferous ferruginous materials in the Cuyuna range. Individual process steps were carried out successfully using a 20-inch-diameter shaft for continuous countercurrent sulfatization of the manganese, a multiple-compartment rotary drum for leaching the water-soluble manganese sulfate, a submerged-combustion evaporator for the recovery of monohydrate crystals of manganese sulfate, and a shaft furnace for the thermal decomposition of sulfate crystals for production of a ferrograde manganese oxide and a sulfur dioxide gas suitable for sulfatization of fresh are. Of the two general kinds of Cuyuna manganiferous materials--the carbonate slates and the oxidized ores--only the slates were studied at pilot scale.

Jan 1, 1963

By M. M. Wong

Electrolysis of titanium carbide and a material consisting of titanium, carbon, nitrogen, and oxygen as soluble anodes in Used electrolytes was investigated by the Bureau of Mines for the preparation of crude titanium metal. Tests made in all-chloride electrolytes showed only a low recovery of titanium as well as a substantial volatilization of titanium trichloride (TiC13) when present in the electrolyte. Electrolysis at 750° to 850° C in a mixture containing 85 percent NaC1-15 percent potassium floutitanate (K2TiF6) yielded as high as 91 percent recovery of titanium from titanium carbide and 62 percent recovery of titanium from the titanium-carbon-nitrogen-oxygen material. Problems associated with the preparation of crude metal by fused-salt electrolysis are discussed. The crude metals produced from both anode materials were electrorefined in a sodium chloride-titanium chloride (NaCl-TiC12) electrolyte, and ductile titanium metal was obtained.

Jan 1, 1963

By T. A. Henrie

A technique was devised for measuring the rate of chemical reactions between reactive metals and molten-salt mixtures at high temperatures. The rate of the heterogeneous reaction between high-purity titanium metal and titanium trichloride in molten sodium chloride was determined. The reaction is surface-controlled, and the heat of activation is 8.29 kilocalories per mole TiC13. An active site or reaction nuclei is created by adsorbing a TiC13 molecule at the metal surface. Reaction of the second TiC13 species forms an activated complex that decomposes into three TiC12 molecules.

Jan 1, 1963

By James H. Gary

Data regarding the composition and physical properties of Florida land-pebble phosphate-waste slime are presented, and the feasibility of dewatering and beneficiating the slime by several different methods is discussed. Chemical analyses, electron micrographs, and X-ray diffraction data showed that principal constituents of the slime included quartz, attapulgite, and flaorapatite. Viscosity of the slime changed with pH; thixotropic, Newtonian, and rheopectic states were observed as the pH increased. Use of various flocculating agents was not effective in improving thickening properties of the slime. Dewatering tests using pressure filtration showed that temperature influenced the filtration rate more than pressure; the filtration rate at 165° C was tenfold that at room temperature. Selective flotation of the slime, using two different processes, gave promising results. About 25 pct of the phosphate was recovered in a concentrate assaying 31 pct P205, Other tests demonstrated that the slime could be successfully fractionated at 20-microns using a hydrocyclone. In hydrometallurgical tests about 80 pct of the phosphorus and alumina were chemically extracted from the slime using sulfuric acid. Limited bacteriological studies made of the slime showed that several types of microorganisms were present and grew in the material despite the presence of fluorine-bearing minerals.

Jan 1, 1963

By G. T. Krempasky

In an attempt to develop a suitable precast concrete support for underground use, two different models (1955 and 1958) of a five-piece concrete set were designed, fabricated, and tested under adverse loading conditions. Model 1955 was designed to withstand an ultimate, uniformly distributed, vertical load equivalent to what a three-piece, 12- by 12-inch wood set of intermediate-grade Douglas fir would withstand. A design figure of 138,000 pounds for the vertical load was used on both the 1955 and 1958 models. In addition, the 1958 model was designed to withstand a uniform horizontal load of 7,000 pounds per foot and additional concentrated-point loading. The step- by-step design of each model is presented in the appendixes. A series of five destruction tests was conducted underground on the 1955 model, and results of the tests showed that the type and method of blocking were of major significance.

Jan 1, 1963

By William C. Miller

This report describes investigations by the Bureau of Mines designed to establish the noise level and spectrum of various types of pneumatic rock drills and to furnish information that would be useful in conducting sound measurements in mining environments and in reducing the noise generated in pneumatic drilling. These investigations show that (1) the noise generated by the drills in the frequencies below 100 cps is caused by the impact of the piston and drill steel, in the frequency range between 100 and 2,000 cps by the exhausting of air from the ports, and in the frequencies above 2,000 cps by the resonant frequencies of steel drill parts and of drill steel; (2) satisfactory instruments and instrumentation systems are available for field and laboratory measurements; (3) reliable sound measurements can be made in mining environments; and (4) devices can be developed that will abate the noise.

Jan 1, 1963

By W. E. Robinson

Samples of raw oil shale and kerogen concentrates were oxidized by alkaline potassium permanganate, air, nitric acid, oxygen, and ozone to obtain information about the chemical structure of organic kerogen in oil shale. In one test, oil shale and oil-shale products were oxidized exhaustively with alkaline potassium permanganate, and the distribution of the organic carbon in the final oxidation products was determined. Comparing results of this oxidation with those obtained from other carbonaceous materials and known compounds gave information about the structure of kerogen. Alkaline potassium permanganate oxidation also was used partly to degrade kerogen into soluble products for characterization purposes. Structures present in these degradation products were indicative of type structures originally present in the kerogen. Nitric acid, oxygen, and ozone were used also for partly degrading kerogen to soluble oxidation products. Carbon-balance oxidation tests using alkaline potassium permanganate showed that Colorado oil-shale kerogen differs from many other carbonaceous materials such as coal and kerogens from other areas. Composition of the degradation products indicated that Colorado oil-shale kerogen is predominantly cycloparaffinic and saturated heterocyclic structures with some long-chain paraffinic and aromatic structures present. The ring systems may be connected through short carbon chains or bridges containing oxygen, nitrogen, and sulfur.

Jan 1, 1963

By M. E. Hawkins

Mineral analyses and electrical resistivity measurements of 324 representative samples of oilfield brines from 24 oil-productive counties in Mississippi and Alabama are presented in tabular form. Results of the mineral analyses, which include calcium, magnesium, carbonates, bicarbonates, sulfates, chlorides, sodium, and barium (with strontium if present), are reported in milligrams per liter. Electrical resistivity measurements in ohm-meter2 per meter at 75° F are reported in ohm-meters in the tables. Chemical analyses of formation waters are helpful to operators having water problems associated with petroleum recovery; electrical resistivity values are helpful in making interpretations from electric logs.

Jan 1, 1963

By David J. Kusler

A gravimetric method for the determination of carbon dioxide, carbon monoxide, hydrogen, methane, and oxygen in blast furnace top gas is described. Nitrogen may be determined directly by volume measurement or by difference. The method is direct, permits continuous as sampling, and provides an averaged analysis over a selected range of sampling intervals from 1/2 to 24 hr or more. Neither expensive equipment nor specialized personnel are required. The method is suitable for routine analysis, and the results compare favorably with those obtained by established methods.

Jan 1, 1963