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By Richard G. Sandberg

Sphalerite concentrates prepared during processing of Missouri lead ores contain small percentages of cobalt and nickel which adversely affect zinc electrolysis. The Bureau of Mines has evaluated solvent extraction and precipitation techniques to remove and recover cobalt and nickel from zinc sulfate solution prior to zinc electrolysis. Prepared zinc sulfate solutions containing about 190 gpl of zinc and 50 ppm of both cobalt and nickel were treated using various combinations of complexing reagents, solvent, pH, concentration, time, and temperature. The following complexing reagents gave the best results: a-nitroso-ß-naphthol, ß-nitroso-a-naphthol, 1,2 cyclohexane dione dioxime (nioxime), di-2-pyridyl ketone oxime, and dimethylglyoxime. These reagents in suitable solvents lowered the cobalt and nickel levels to <0.1 ppm. Stripping the complexed reagents from the solvents was not possible except for nioxime. Direct addition of the appropriate reagent to the prepared zinc sulfate solution resulted in the precipitation of cobalt and nickel. Several possible flowsheets are presented for the removal and recovery of cobalt and nickel. Good zinc deposits were successfully electrowon from zinc sulfate solutions purified by solvent extraction and precipitation.

Jan 1, 1978

By F. P. Miknis

Previous studies at the Bureau of Mines have shown that broad-line nuclear magnetic resonance (NMR) techniques have potential applications for rapid evaluation of oil-shale deposits. In a continuation of this study the techniques of pulsed NMR have been applied in a similar manner. The basis for the pulsed NMR oil-shale assay method lies in the assumption that the free induction decay (FID) amplitude following a 90° pulse is proportional to the potential oil yield. This assumption was tested on two groups of oil-shale samples, numbering 141 and 263 samples, from two different oil-shale cores. For both groups of samples a small number were selected as calibration samples. Free induction decay amplitude measurements were made on the 141 and 263 samples. The best least-squares regression line was obtained for the calibration samples, and the oil yields of the remaining samples were calculated using the slopes and intercepts obtained in the regression analyses. The agreement between measured and calculated oil yields was good, the indexes of determination being 0.93 and 0.89 for the groups of 141 and 263 samples, respectively.

Jan 1, 1974

By Robert K. Koch

Laboratory-scale studies on defluorination of natural and synthetic fluorspars by pyrohydrolysis at 1,500° C. were made to determine the feasibility of developing a process for producing hydrogen fluoride from siliceous fluorspars. It was found that the reaction (at 1,500° C.) is not promising for process development, even though a silica-free offgas can be generated. The primary difficulty is the low hydrogen fluoride content of the offgases; an HF content of 6 percent was the best achieved. Previous research by the Bureau of Mines has demonstrated that offgases averaging 27 percent hydrogen fluoride can be produced under carefully controlled conditions at 1,280° C. The lower temperature process is a better method for production of HF. However, charges in which the CaF to Si02 mole ratio varied from 0.4 to 2 could be processed with similar results. Also, combined alumina and ferric oxide contents up to 25 mole-percent did not noticeably alter the rate of defluorination. Therefore, virtually any natural siliceous fluorspar would respond in essentially the same manner when exposed to water vapor at 1,500° C.

Jan 1, 1962

By C. M. McCulloch

As part of the Bureau of Mines methane control program, the Pittsburgh coalbed was studied in Washington and Green Counties, Pa., and in Marion and Monongalia Counties, W. Va., where this coalbed is now being mined at its greatest depth. The coalbed thickness appeared to be structurally controlled; the bed was generally thinner near the axes of anticlines and thicker near the axes of synclines. The overburden isopach shows a similar relationship. Most of the clay veins in coal occur in the synclinal troughs, generally under sandstone roof. Cleat orientations measured in 18 underground mines showed that face cleats are perpendicular to the axial trends of the folds, and the butt cleats are parallel to the axial trends, indicating structural control of the cleat. Measurement and analysis of surface joint orientations provide a method for predicting the cleat orientations of the coalbed, but linears measured from infrared photographs and photoindex sheets helped only to determine regional trends. The results of these investigations provide a geologic framework for rational planning for underground mine development to use the best available technology to cope with methane emissions, coalbed discontinuities, and related ground support problems.

Jan 1, 1975

By Leland A. Yerkes

Refining aluminum from crude aluminum alloys by the subhalide reaction was investigated to develop a method of producing aluminum by means other than electrolysis of its oxide. The best materials and design for the apparatus and also optimum operating conditions, including temperature, pressure, vapor flow rate, and composition of alloy charge were studied. In the subhalide process, aluminum-trihalide vapor reacts with aluminum in the alloy under high temperature and low pressure, forming volatile aluminum monohalide which reverts to aluminum metal and aluminum trihalide on cooling. The only halide used in this investigation was aluminum trichloride. The crude aluminum-silicon alloys used as the principal raw material contained from 21.9 to 36 percent aluminum, and significant quantities of iron and titanium. These alloys were produced by direct electric smelting of clays. Graphite tubing that was heated by an induction coil proved to be satisfactory material for the laboratory reactor chamber, Enclosed in an insulated glass or quartz pipe, the reactor was used in both vertical and horizontal positions with various baffle and tray arrangements for directing the trihalide vapor both over and through the alloy. Aluminum trichloride vapor was generated in the sublimer at one end of the glass pipe, passed into the reactor where contact was made with the crude alloy, and aluminum monochloride gas was formed. When the gaseous mixture of aluminum monochloride and unreacted tri-chloride passed out of the reactor and entered the condenser, the gases were cooled to 900° C. or less, causing the monochloride to disproportionate into aluminum and aluminum trichloride vapor. The aluminum was deposited on the condenser walls while the aluminum trichloride vapor was carried out of the condenser and into the opposite end of the glass pipe where it solidified on the cooled copper coils.

Jan 1, 1961

By W. P. Diamond, B. M. Bench, C. M. McCulloch, Maurice Deul

As part of the Bureau of Mines methane control program, the Pittsburgh coalbed was studied in Washington and Green Counties, Pa., and in Marion and Monongalia Counties, W. Va., where this coalbed is now being mined at its greatest depth. The coalbed thickness appeared to be structurally controlled; the bed was generally thinner near the axes of anticlines and thicker near the axes of synclines. The overburden isopach shows a similar relationship. Most of the clay veins in coal occur in the synclinal troughs, generally under sandstone roof. Cleat orientations measured in 18 underground mines showed that face cleats are perpendicular to the axial trends of the folds, and the butt cleats are parallel to the axial trends, indicating structural control of the cleat. Measurement and analysis of surface joint orientations provide a method for predicting the cleat orientations of the coalbed, but linears measured from infrared photographs and photoindex sheets helped only to determine regional trends. The results of these investigations provide a geologic framework for rational planning for underground mine development to use the best available technology to cope with methane emissions, coalbed discontinuities, and related ground support problems.

Jan 1, 1975

By James J. Olson

The Bureau of Mines recorded both particle accelerations and velocities from one-stick and production blasts at Eagle-Picher Industries&apos; Shullsburg mine, Shullsburg, Wis., to test the effectiveness of square root scaling in grouping underground blast vibrations and to determine the effects of rock type and mine geometry on blast vibrations. Although the charge weights of subsequent delay periods sometimes exceeded the charge weight of the zero-delay period, both acceleration and velocity records showed that the zero-delay portion of the Shullsburg production blasts produced the highest vibration amplitudes. Because of the restricted range of charge weights in the Shullsburg experiments, no statistical determination of an appropriate scaling factor could be made. However, the square root scaled peak particle velocity data from the Shullsburg production blasts grouped well within the approximate band-width of vibration data obtained by the Bureau from quarry blasts in many different rock types. This indicates that scaling by some factor, perhaps the square root or cube root of the charge weight, may be an effective way to group and study vibration data from underground blasts. Further research is needed to determine which scaling factor is best for underground blasting.

Jan 1, 1970

By Donna D. Harbuck

The Bureau of Mines has investigated a process to produce titanium powder directly from titanium salts. If successful, such a process could lower the cost and increase the use of titanium. In this study, K2TiF6, K2TiF3, and TiF3 were reduced with potassium in the temperature range of 650° to 750° C. Under certain conditions, titanium powder 1.6 to 3.3 microns in size was produced. After leaching the product with a 0.1M HCl solution, powder impurities as low as 0.04 pct potassium and 0.28 pct fluorine were obtained. However, oxygen levels of over 1 pct and the frequent formation of insoluble byproducts demonstrate the need for further research to make the powder suitable for powder metallurgy applications.

Jan 1, 2011

By J. P. Morris

A diphenyl ether calorimeter for measuring high-temperature heat contents of ferrous alloys and iron-and steelmaking slags was constructed and calibrated with specimens of molybdenum, alumina, and platinum that were heated to temperatures ranging from 1,720° to 1,875° K. The standard deviation of the calibration measurements was 0.37 percent. By measurements of the enthalpy of delta and liquid iron, the heat of fusion of iron was found to be 3,298 ±100 cal per mole.

Jan 1, 1966

By Edward F. Divers

Tills U.S. Bureau of Mines report briefly evaluates the advantages and disadvantages of basic dust control techniques presently used by U.S. coal preparation and mineral processing plants. These include ventilation, baghouse-type collectors, wet scrubbers, electrostatic precipitators, source control, sprays, good housekeeping, and personal protection devices. Two specific problems in these types of operations are also considered: dust collector system duct clogging, and control room dust control. Information provided in this report results from dust control research projects conducted by the Bureau at various coal preparation and mineral processing plants over the past decade to reduce workers&apos; dust exposure. These studies indicate that plant ventilation systems normally provide the most cost effective method for dust control. Baghouses and scrubbers were also effective in specific applications, and examples of each are given. In extreme dust conditions, personal protection devices, such as respirators or the dust helmet, can also be highly cost effective.

Jan 1, 1990

By J. K. Whyatt

Assuring ground control safety in many mining and tunneling projects depends, at least in part, on an understanding of in situ stress conditions that will be encountered. Yet it is rarely practical to conduct more than a very limited number of stress measurements. Stresses along the route of a proposed excavation are typically interpolated from available measurements, often assuming a linear variation of stress with depth (or elevation). However, projects where multiple stress measurements are conducted often report more complex variations of in situ stress, usually in apparent relationship to geologic structures. These structures often include lithologies of contrasting elastic properties. A method is proposed for estimating stresses in these cases by first back-calculating regional loads from available stress measurements and then modeling the distribution of stress throughout the rock mass. The method has been successfully applied to a set of in situ stress measurements from the Coeur d’Alene Mining District of northern Idaho, USA. Results provided new insights into district stress conditions and the distribution of rockburst hazards along mine drifts and between various mines. This success should transfer readily to suitable deep tunneling projects.

By Maria I. De Rosa

Combustible materials, when burned, produce toxic gases and smoke, which may vary dramatically from one material to another, with resultant different total toxicity and smoke obscuration levels. This U.S. Bureau of Mines report presents smoke property data acquired for a variety of mine combustibles and shows that there exists a correlation between the smoke properties, the relative toxicity, and the smoke obscuration levels of those combustibles tested. These correlations can be used to devise simple, standard tests for determining the toxic and smoke obscuration hazards of mine materials during fire.

Jan 1, 1989

By J. F. Messerly

The purity of three specially prepared samples of benzene was determined with an adiabatic, low-temperature calorimeter with automatic control of shield temperature. Extensive measurements were made on each sample to determine how variations in operating procedures affect melting-point and freezing-point as well as purity data obtained by the calorimetric method. Detailed results of the investigations are presented, and effects of different operating procedures are discussed, together with problems encountered in interpretating experimental results.

Jan 1, 1963

By C. H. Schack, A. O. Ipsen, H. G. Poole

"INTRODUCTION In the course of the investigation of manganese mineral occurrences in continental United States, the Bureau of Mines has collected several lots of ore from properties in the vicinity of Long Valley, Ariz. The ore occurs as irregular and random pockets in a brecciated zone. As only high-grade portions of the deposits obtained by selective mining would be acceptable as commercial-grade manganese ores, an investigation was made to determine amenability of the ores to concentration by ore-dressing methods. Several types of ores, differing in grade and mineral associations, were studied.Ores from the Vaiazza property are of special interest, owing to the successful application of silica flotation for their concentration. Ores from the Shroup and Conner-Hough properties are very similar but differ somewhat in their response to ore-dressing Method's. In all instances, the man¬ganese minerals are psilomelane and pyrolusite, with minor amounts of other manganese oxides. The country rook is a brecciated limestone; the diluent in the high-grade ore pockets is chiefly silica. The low-grade manganese ores are limestone replacements, and the chief gangue material, of course, is limestone."

Nov 1, 1947

By Dennis A. Long

Slip and fall accidents are a major cause of lost-time injuries associated with large mobile equipment in surface mines. An evaluation of the safety hazards associated with getting on and off large surface mining vehicles showed that most of the accidents occur at the point where personnel attempt to mount or dismount the machine at ground level. The major hazardous design conditions were identified as excessively flexible supports for lower steps or rungs, inappropriate ground-level-to-first-step distances, poor step designs, access designs that use vehicle components as steps or walkways, and inadequate hand- rail and guardrail designs, Additional hazards are introduced by the lack of proper maintenance of ladder hardware and the work practices of operators in carrying articles while mounting and dismounting the vehicle. This Bureau of Mines report describes the design and in-mine testing of improved access system for large mobile mining equipment.

Jan 1, 1984

By Lawrence G. Houk

Lithium is the lightest of all metals, but as it deteriorates rapidly in air it has no structural applications. Alloys of lithium that will float upon water can be made with other light metals, but these ultralight alloys are not useful in aircraft production or elsewhere at present. Alone or alloyed with alkaline earth meals, lithium acts as reining agent on molten metals, and as a minor constituent with other metals it imparts characteristic properties to the allay. Lithium compounds have somewhat wider application in commerce than either the metal or the alloys. They are used in the glass, ceramic, chemical, and air-conditioning industries and less extensively in the optical, pharmaceutical, electrical, and textile industries. The United States is the leading producer anti consumer of lithium ores and compounds and apparently has the largest known ore reserves. The value of lithium ores and primary chemical byproducts produced is relatively small, yet the lithium chemical industry yields products worth hundreds of thousands of dollars each year, owing partly to the high degree of purity demanded by the trade for most finished products and to the low combining weight of lithium. Fortunately, the low-grade ores can now be concentrated economically, and this fact, together with our extensive reserves, assures adequate supplies to meet any reasonable increase in demand. Lithium is listed as essential by both the American and British war agencies, and its military importance may be greatly enhanced.

Jan 1, 1942

By Russell E. Griffin

Dielectric constants and dissipation factors were measured for six rocks over the 20-to 100-megahertz frequency range by means of the susceptance-variation method. Results for both dry and moist specimens are presented and compared with data reported by others. Loss factors calculated from the data presented are important to the Bureau&apos;s study of rock fragmentation by means of dielectric heating.

Jan 1, 1967

By F. H. Nehl

Ion elutriation was used to extract silver cyanide complexes and free cyanide from aqueous streams containing up to 10 ppm silver and 5 ppm free cyanide. Screening tests selected nine of 350 different surfactants for further, larger scale experiments. The screening procedure used 0.1 g of each of the surfactants in 300 mL of synthetic wastewater. Air was sparged into the test cell at 50 cc/min. The foam was refluxed during the tests and was not sampled. Samples of the solution were taken at specified intervals and analyzed by wet chemical methods for free cyanide and by atomic absorption for silver content. The most effective surfactants lowered the silver and free cyanide concentrations to less than 0.5 ppm in 1 h or less. These surfactants were quaternary amine salts with one long chain (C12-C18) organic group and three methyl groups. Experiments using 3 L batches of wastewater or an ion elutriation cell continuously fed with solution draining from an inactive heap leach operation confirmed the results from the screening tests.

Jan 1, 2010

By T. E. Sterner

The Bureau of Mines investigated the use of a chromatographic gas analyzer in determining the concentration of combustion products in gas produced during field and laboratory thermal oil-recovery tests. Several parameters (carrier-gas flow, cell current, sample size, and temperature) known to affect quantitative analyses were studied using a commercially available dual-column, dual-detector chromatographic gas analyzer which had been modified to provide close control of these variables. The apparatus made possible a much closer control of air-and gas-injection rates and provided adequate data for performing material-balance calculations and for determining oxygen utilization during the laboratory and field combustion tests. The chromatographic analysis also aided materially in evaluating and measuring bypassing and gas travel times and in detecting high-permeability zones that were present in the reservoir.

Jan 1, 1965

By Van E. Shaw

Three comparatively simple, efficient, and rapid extraction methods for the dissolution of yttrium and rare-earth elements from a euxenite carbonate residue have been developed, using dilute sulfuric acid as the solvent. Extraction processes have resulted in yields of 98+ percent of the total rare-earth elements and yttrium contained in the residue and have given preliminary separation between the cerium-group and the yttrium-group rare-earth elements. Extraction procedures presented are: Procedure 1. -The recovery of total rare-earth elements and yttrium by a cold dilute sulfuric acid leach at a pH of 2.5. Procedure 2. -The recovery of yttrium and yttrium-group rare-earth elements by leaching with dilute sulfuric acid at 125° F. and a pH of 3.0, with subsequent recovery of the cerium-group rare-earth elements by a cold dilute sulfuric acid leach of the residue at a pH of 2.5. Procedure 3. -The recovery of the total rare-earth elements and yttrium by fractional leaching as in procedure 1, followed by boiling the sulfate solution, which precipitates the cerium-group rare-earth elements and leaves the yttrium-group rare-earth elements in solution.

Jan 1, 1959