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By M. J. Ferrante

Enthalpy and entropy increments above 298.15° K were determined for cop-per sulfate between 298° and 1,000° K and for copper oxysulfate between 2980 and 1,146° K by the method of copper-block drop calorimetry. Enthalpies, entropies, and heat capacities are tabulated for both compounds. In addition, free-energy functions are tabulated for the sulfate. Equations representing the enthalpies are given for each compound.

Jan 1, 1972

By R. L. Hopkins

Fifteen alkyl cycloalkyl sulfides and three dicycloalkyl sulfides were synthesized to provide reference compounds in the search for these classes of sulfur compounds in crude oils. In synthesizing sulfides by alkaline alkylation the order in which the reactants were added was shown to determine the yield and purity of the product.

Jan 1, 1966

By G. E. MeGlelland

During the 1970?s, the Bureau of Mines investigated a particle agglomeration technique for improving the flow of leaching solution through heaps of clayey or crushed, low-grade gold-silver ores. This technology has been adopted on a broad scale by the precious-metal-processing industry. This report presents information on the application of agglomeration technology to finely ground precious-metal-bearing tailings. Two commercial operations that have benefited from agglomeration technology are discussed. The technology is cost effective because of decreased leach times and improved precious metal recoveries.

Jan 1, 1985

By J. M. Oestreich

Supercritical water (sew) Is being tested for commercial use 1n several organic extraction systems but little work has been done on the extraction of metals from minerals. This lack of information prompted Bureau of Hines (BOM) research into the sew treatment of minerals. As a result, this research project is intended to serve mainly as a starting point for further experimentation. A simple flow-through reactor was built out of high pressure tubing and used to treat minerals with SCU at 400? C and 3500 to 7000 psi. The research produced four main conclusions: (1) carbonates of copper, iron, and lead convert to oxides; (2) most iron minerals showed alteration to oxides with some iron dissolution; (3) valuable trace elements including nickel, chromium, and others leached to some extent from sea minerals along with some calcium, iron, silicon, and sulfur; and (4) treatment of sulfides extracted elemental sulfur and resulted in several alteration reactions, though with the exception of cinnabar and the iron bearing minerals, the metals in sulfides were mainly insoluble. Surface alterations on many of the minerals show significant changes have occurred in the minerals even when only minor extractions were detected. These surface effects may be very important when used in conjunction with flotation processes since the sew treatment may selectively enhance or suppress a mineral's floatability.

Jan 1, 1989

By F. R. McDonald

The proton NMR spectra of 32 pyridines in two solvents, carbon tetrachloride and benzene-d6, are presented. The chemical-shift and differential-shift values are correlated with the substitutent position and with the solvent media. The ring protons and the protons on alkyl substituents are tabulated. The paramagnetic shift of the protons adjacent to the nitrogen is discussed, and a proposed structure for the pyridine-benzene complex that is consistent with the observed anomalous paramagnetic shift is presented. The utility of the data in the identification of pyridine compounds found in shale-oil naphtha is demonstrated.

Jan 1, 1971

By Margaret R. Egan

This Bureau of Mines report presents results from experimental studies on wood crib fires in an intermediate-scale fire tunnel. Gas concentrations, smoke particle characteristics, heat release rates, and ventilation rates were determined. These measurements form a data base for wood, which can be used with previous analyses for coal and future studies of other mine combustibles, to comprehend the potential hazards of these materials in underground mine fires. A knowledge of the combustion products emitted from these materials will benefit fire detection and control. Results show the changes in burning rate and heat release rate produced by different crib configurations and ventilation rates. Also included are the effects that the burning rate has on smoke characteristics and gas production.

Jan 1, 1986

By Alla D. Mah

Compilation of data on materials of metallurgical interest is one of the important activities of the Berkeley Thermodynamics Laboratory of the Bureau of Mines. Recent renewed interest in metallurgy of vanadium renders the present compilation a timely guide for experimentation to improve present methods or to develop better methods of extractive metallurgy. Thermodynamic data for vanadium and its inorganic compounds have been critically surveyed, selected, and compiled into one convenient reference from which information can be readily obtained for evaluating heat balances, determining trends, and establishing limits of metallurgical processes. By indicating the direction of experimentation, this report enables the saving of time, effort, and expense which would otherwise be necessary for trial and error experimentation. Much of the data has been obtained experimentally at the Berkeley laboratory. Other data were collected through an extensive survey of worldwide literature through April 1965. Estimates were made when no data were avail-able. Data on the vanadium halides was sparse, and the results derived from existing data were at times divergent. Some of the selected values for the halides may need modification as more or better experimental data become available.

Jan 1, 1966

By Earle S. Burnett

Rotating piston deadweight gages have been used for many years for measurement of pressure to several hundred atmospheres. They have been calibrated by comparison of fluid pressures produced by various loads bearing on the piston bases, as measured by corresponding heights of balancing columns of mercury. When expressed in appropriate units, these ratios of column heights to piston loads are called piston constants. Experimental arrangements and procedures for their determination are presented in this paper, followed by a discussion of their significance and of their subsequent applications.

Jan 1, 1966

By John Nagy

The effect of low percentages of methane (0 to 5 pet.) in an air atmosphere on spark initiated explosions of coal dust was investigated. With low dust concentrations (0.1 to 0.4 oz./cu, ft.), small amounts of methane increase the explosion pressure; with larger dust concentrations (0.5 to 2.0 oz./cu. ft.), small amounts of methane decrease the explosion pressure. The rate of pressure rise of a coal dust explosion increases with increase in methane concentration; about 3 to 4 pct. further addition of methane yields a decrease in the rate of pressure rise. Convection currents created by the air or gas blast used to disperse dust produce an increase in explosion pressure and rate of pressure rise. The minimum explosive concentration of the coal dust decreases about linearly as the concentration of methane increases from 0 to 5 pct. The explosion pressure increases linearly as the initial pressure within the chamber increases. Similarities between coal dust and methane explosions are indicated, INTRODUCTION During coal mining, methane occluded in coal or adjoining strata is liberated into the mine atmosphere,4 Normally, the methane is diluted and swept away by the ventilating air. Under some conditions, through accidental disruption of the ventilation system, sudden outburst, or because insufficient fresh air is supplied to a working place, low percentages of methane may be present during mining operations. If it is permitted to accumulate, methane itself presents an explosion hazard; its limits of explosibility arc approximately 5 and 15 pct. The effect of low percentages of methane on the explosibility of coal dust was studied to provide a broader understanding of the hazards of ignition and explosion and thus to facilitate development of control

Jan 1, 1961

By Jacqueline A. McClaskey

The U.S. Bureau of Mines Information and Analysis Directorate collects worldwide data on virtually every commercially important non fuel mineral commodity. These data form the base for tracking and assessing the health of the minerals sector of the U.S. economy. The Bureau's data collection activity was instituted by the 47th Congress in an appropriations act of August 7, 1882 (22 Stat. 329), which placed the collection of mineral statistics on an annual basis. The most recent authority for the U.S. Bureau of Mines survey activity is the National Materials and Minerals Policy, Research and Development Act of 1980 (Public Law 96-479, 96th Congress). This act strengthens protection for proprietary data provided to the U.S. Department of the Interior by persons or firms engaged in any phase of mineral or mineral-material production or consumption.

Jan 1, 1993

By A. Visnapuu

The Bureau of Mines has upgraded high-iron domestic chromite concentrates by a carbonyl process. The upgraded chromite concentrates show as much as 10 wt pct higher Cr203 content and up to a threefold in-crease in the Cr:Fe ratio, compared with the starting concentrates. The high-iron chromites were first reduced to convert the iron oxides to the metal, and then treated with CO at elevated pressures and low temperatures to convert part of the metallic iron fraction to iron pentacarbonyl. Carbonylation was accelerated by the addition of H2S in small quantities. The iron pentacarbonyl was extricated from the con-centrate in the pressure reactor during carbonylation by a CO sweep through a pressure-reducing valve and passed through a decomposer at atmospheric pressure to convert it back to iron metal and CO. CO pres-sure, temperature, promoter trends, and other factors enhancing iron pentacarbonyl formation are presented.

Jan 1, 1985

By Kenneth G. Skinner, Hewitt Wilson, Thomas L. Hurst

Although chromite deposits occur in California , Oregon, Washington, Montana, Wyoming , Pennsylvania, Maryland , New Mexico , North Carolina, Alaska, and the Phillippine Islands , less than 1 percent of the ore used in the United States is obtained from these deposits . Most of the ore in peacetime has been supplied by imports from South Africa, New Caledonia, Turkey, and Cuba . The mineral chromite , the most important chromium ore , is an isometric spinel with an ideal composition of FeO Cr2O3 , but commercial chromite has the variable composition (Fe , Mg) Oʻ (Cr , Al , Fe) 203. Chromite has a black color , a specific gravity of 4.4 , and a hardness of 5.5 . In thin section the color is reddish -brown to black . Chromite occurs in dunite and pyroxenitic ultrabasic rocks , which are composed of iron- magnesium silicate minerals such as olivine , saxonite , serpentine , and enstatite . These are also the gangue minerals . Com mercial ore occurs at random in the country rock in kidney- or lens - shaped deposits , which have no apparent relationship to each other . Stringers , veins , and bands often cut the country rock without regard either to fracture or to other deposits . Some beach sands , such as those in southern Oregon, contain chromite .

Mar 1, 1943

By T. M. Barczak

One of the primary goals of Bureau of Mines research is to reduce the cost of coal mining by improving the efficiency of longwall supports. One method of achieving this goal is the optimization of stress distribution within the support structure, resulting in a lower overall weight, more fully stressed shield. However, before stress optimization can be initiated, load conditions must be defined that cause maximum stress in the various support components. A finite-element model of a longwall shield was used to identify these critical load conditions. These load conditions were then evaluated in the Bureau's mine roof simulator (MRS) by instrumentation of a longwall shield and measurement of strains in each of the shield components. The critical (canopy-base contact) load conditions were identified that can cause structural failure at less than rated shield (hydraulic yield) capacity. Comparisons were made between full-contact and partial-contact load conditions. Other parameters investigated included the stiffness of the contact material, changes in shield geometry, rate of load application, and effects of horizontal constraint. Conclusions were drawn regarding the structural integrity of the major shield components and potential for stress optimization.

Jan 1, 1987

By Wallace W. Roepke

Four bit designs, two conical and two radial, were tested in coal against a 60° conical reference bit to obtain data on orthogonal cutting forces and primary respirable dust generation. One conical and one radial design were modified by the Bureau of Mines for these tests. Results were mixed: One radial bit used substantially lower overall cutting forces and specific energy than the other bits and was the only cutter lower on energy and most forces than the standard 60° bit. How-ever, it generated more specific and total dust than any other bit. The four bits were also tested for incendivity, with a 90° plumb-bob bit as the reference. The frictional ignition tests were designed to simulate both trimming top rock and cutting such rock during advance on-sump. Results of these tests were also mixed. The radial bits were substantially less incendive than the reference bit and caused no ignitions in either top trimming or sump modes. Only the modified mushroom-tipped conical bit caused ignitions. Bits similar to this modified design should not be used on drum-type miners in gassy mine areas; in-stead, the other types of bits tested should be used to reduce ignition potential to a minimum.

Jan 1, 1983

By GEORGE S. POPE

This bulletin is the third of a series a showing the results of ment purchases of coal according to specifications as to its quality and giving typical forms of proposals for supplying coal and general information relating to government coal purchases . Numerous calls for authentic information concerning the purchase of coal according to its heat value attest a growing interest in the subject. Many of the commodities of life have long been purchased according to specifications requiring chemical or physical tests , or both, to determine whether the material delivered meets the requirements , the price to be paid depending on the results of the tests . Until recent years coal consumers purchased coal merely on the statement of the dealer as to its quality , relying on his integrity and on the reputation of the mine or district from which the coal was obtained. It is surprising that the important question whether value was being received for the money expended was not sooner seriously considered . The purchase of coal by specification is an important step toward the conservation of our national mineral resources , for it results in an increased use of the lower grades of coal. The poorer coals find a market by competing with the better grades , not as to the price per ton but as to the cost of an equal number of heat units. This paper gives in detail the results of government purchases of coal for the fiscal year 1908–9 and the list of contracts with abstracts of specifications for the fiscal year 1909–10 , and summarizes the information on this subject obtained by the Survey. It is hoped that this information will promote a better understanding of the specification method of purchasing coal and furnish data valuable alike to coal dealers and coal consumers , so that equitable contracts can be more readily made.

Jan 1, 1910

By F. P. Haver

A method to recover copper and elemental sulfur from chalcopyrite concen¬trate, using a ferric chloride leach, CuFeS2 + 3FeCl3 ? CuCl + 4FeCl2 + 2S, was reported by the Federal Bureau of Mines in 1971 (Report of Investigations 7474). Since that time, additional work has been done to improve certain steps in the procedure; that is, the recovery of sulfur from the leach residue, the recovery of copper and iron from the leach solution, and the regeneration of the leach solution. It was determined that over 99 pct of the elemental sulfur in the leach residue could be extracted at ambient temperature with an ammonium sulfide solution. Heating the pregnant solution precipitated crystals of rhombic sulfur (99.5 pct purity) and liberated ammonia and hydrogen sulfide for recycle. Copper with a purity in excess of 99 pct was obtained from the leach solution by electrolysis, using a diaphragm cell, with an energy requirement of less than 0.7 kW-hr/lb. Metal was deposited as a weakly adherent powder that could be easily dislodged from the cathode and withdrawn continuously from the cell in the form of a slurry. During electrolysis, part of the Fe(II) was oxidized to Fe (III) at the anode so there was no chlorine evolution. The leach solution was regenerated by direct oxidation of the spent electrolyte with air or oxygen in a turboaerator at 80° C. This precipitated the iron dissolved during leaching in an easily filterable form, Fe203.xH20, and converted the remaining Fe(II) to Fe(III).

Jan 1, 1975

By A. Gene Collins

The Bureau of Mines undertook research to determine the bromide and iodide content of Mississippi and Alabama oilfield waters of the Tertiary and Cretaceous Period to determine genetic relationships of the ions, to determine their origin, and to determine their genetic relation to petroleum. The 280 samples were analyzed after a pretreatment to remove interferences. The iodide was oxidized to iodate and was titrated with thiosulfate. The bromide was oxidized to bromate and was determined iodometrically. A computer was used to calculate the correlation coefficients of iodide to bromide and to other ions. The other ions are sodium plus potassium, calcium, magnesium, chloride, bicarbonate, and sulfate. The mineral content of the samples ranged from 52 to 1,760 mg/l for bromide and from 2 to 65 mg/l for iodide. The mean bromide-to-chloride and iodide-to-chloride ratios were 0.0065 and 0.0002. The correlation coefficient matrix and linear plots indicated a definite bromide-to-calcium relationship for the brines investigated.

Jan 1, 1967

By L. B. Pankratz

The Bureau of Mines measured heat capacities of alpha and beta spodumene (LiAlSi2O5) and of beta eucryptite (LiAlSiO4) over the temperature range 51° to 298° K. The entropies at 298° K were found to be 30.9 ± 0.2 cal/deg mole for alpha spodumene, 36.9 ± 0.3 cal/deg mole for beta spodumene, and 24.8±0.2 cal/deg mole for beta eucryptite. High-temperature heat content measurements above 298° K were conducted for the same compounds. Measurements were made to 1,150° K for alpha spodumene, 1,600° K for beta spodumene, and 1,470° K for beta eucryptite. Tables of heats and free energies of formation are given from the elements and from the constituent oxides.

Jan 1, 1967

By K. Zipf, Z. T. Bieniawski

"An extensive mixed-mode fracture toughness testing programme was conducted on coal from three coal fields. A special mixed-mode testing fixture for coal and other geologic materials was developed together with reliable specimen preparation procedures. Dynamic modulus measurements made on each of the 116 fracture toughness specimens showed that these coals exhibit certain degrees of anisotropy. The fracture toughness testing programme systematically varied the loading rate, specimen orientation and fracture loading mode. Loading rate did not significantly effect the fracture toughness over the quasi-static range tested. Orientation did have a significant effect on measured fracture toughness. In the coals tested, the divider orientation and arrester orientation had higher fracture toughness than the short transverse orientation. Data showed that one orientation could have almost twice the fracture toughness as another. The fracture toughness testing enabled certain evaluations of three mixed-mode fracture theories: maximum tangential stress, maximum energy release rate and strain energy density theory. Due to the extreme heterogeneity of the coals tested, definitive conclusions regarding the best mixed-mode fracture theory are not possible; however, data do tend to support the strain energy density theory. INTRODUCTIONThe major aim of this research is to ·develop a fundamental understanding of how fine· fragments of coal (respirable dust) are generated during a fracture process. In a related paper [l], a hypothesis was presented for the mechanism of fine fragment formation during a generic coal material/cutting tool interaction. In this hypothesis, fine fragments are created during coal material/cutting tool interactions that are best described as general mixed-mode fracture processes. Data are required on the mixed-mode fracture behaviour of coal, the physical character of the newly-created fracture surfaces and the character of the inherent flaw structure of the coal material. Accordingly, a test programme was designed that provided some information in each of these areas. The testing effort seeks to measure critical fracture toughness under mixed-mode loadings as a material parameter characterizing in part the tendency of various coals to generate undesirable quantities of fines and respirable dust."

Jan 1, 1990

By Agnes Y. Lee

The Bureau of Mines has developed an effective hydrometallurgical method to recover high-purity Pb metal and elemental S from concentrates. This low-temperature process eliminates S gases and Pb emissions, in contrast to the current high-temperature smelting technology. The method consists of (1) oxidative leaching with H202, Pb02, and waste fluosilicic acid at 95° C to produce a solution of PbSiF6 and a residue containing elemental S, (2) electrowinning the PbSiF6 solution at 35° C to produce 99.99 pct Pb metal and H2SiF6, and (3) solvent extraction to recover S, leaving a residue containing Cu, Ag, and other metal values. Spent electrolyte was recycled repeatedly, with impurity buildup controlled by controlling the leach parameters.

Jan 1, 1986