Search Documents

By Charles Prasky

This report describes fluidized bed techniques employed by the Bureau of Mines at Minneapolis to differentially sulfatize the manganese in two samples of low-grade manganiferous ferruginous carbonate slates from the Cuyuna Range district, Minn. Suitable mechanics of operation were established. A space rate of 1.25 to 1.5 fps, a retention time of 3 to 3.5 hours, a temperature of 700° C, and a 10 percent sulfur dioxide gas in air were adequate for sulfatizing the slates by fluidization. Under these conditions the overflow product removal rate from the 4-inch-diameter reactor was 4 to 5 pounds per hour. The sulfur dioxide was used more efficiently in the two-stage treatment than in the single-stage treatment. However, approximately 80 percent of the manganese was converted to sulfate by either treatment.

Jan 1, 1963

By R. E. Mussier

This investigation was made to study new methods to prepare high-purity yttrium metal, Various methods were used to prepare pure intermediate compounds, primarily chlorides, bromides, and iodides, which were subsequently reduced to metal. The process found most suitable for the preparation of pure anhydrous yttrium chloride involved thermal dehydration of a mixture of hydrated yttrium chloride and ammonium chloride while under vacuum. Yttrium bromide and iodide were prepared most effectively by the direct halogenation of yttrim carbide. Yttrim carbide was obtained by reacting and melting yttrium oxide-carbon mixtures in a carbon-arc furnace. Yttrium halides were purified by vacuum distillation and reduced by alkali or alkaline-earth metals. Lithium and sodium proved to be the best reductants from the standpoint of yield (>95 pct) and purity (>99.8 pct) of the yttrium. The product of the reduction step was sponge metal, which was consolidated readily by conventional cold-mold, arc-melting procedure. The purest yttrium obtained in laboratory scale work was prepared by sodium reduction of yttrium chloride and contained only 125 pp oxygen; other impurities did not exceed 1,000 ppm. In larger scale tests yttrium containing only 800 to 1,000 ppm total impurities was obtained by lithium reduction of yttrium chloride. The tensile properties of high-purity yttrium were determined. Mechanical tests showed that yttrium can be forged, extruded, rolled, spot welded, and deep drawn.

Jan 1, 1963

By L. H. Adami

This paper reports the results of solution calorimetry conducted to obtain the heats of formation of crystalline FeS04?6.952H20 and FeS04?1.008H20, from. which values were derived for the stoichiometric compounds FeS04?H20 and FeS04?H20. Also included are derived values of the free energies of formation and dehydration. This work was undertaken primarily to fill a need for data for pure, easily obtainable ferrous compounds that are suitable for use as calorimetric intermediates, The ferrous sulfate hydrates meet the essential requirements for this use.

Jan 1, 1963

By G. W. Birge

Carbonizing properties of the principal coalbeds of Elk, Clarion, Jefferson, Clearfield, and Centre Counties, Pa,, are described in this Bureau of Mines report, Twenty-six samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, and Brookville beds, were carbonized by the Bureau of Mines--American Gas Association (BM-AM) method, and yields of products and physical properties of cokes were determined. Expansion or contraction of the majority of the samples was measured in the Bureau of Mines sole-heated oven. Chemical analyses, agglutinating values, and free-swelling indexes are given for all samples. In this area the coals generally are characterized by high sulfur and moderately high ash content, and their suitability for metallurgical use would depend largely upon satisfactory cleaning. The samples from Elk, Clarion, and Jefferson Counties were high-volatile A bituminous In rank, whereas, most samples from Clearfield County and all those from Centre County were of medium-volatile rank. Coals from Clarion County had dry, mineral- matter-free fixed-carbon contents ranging from 56.5 to 60.3 percent and were weakly coking. With the exception of two samples which contained excessive ash, the medium-volatile coals of Clearfield and Centre Counties were strongly coking and, as indicated by sole-oven expansion results, would require blending with lower rank coal to avoid oven damage.

Jan 1, 1963

By M. E. Tyrrell

Mixtures of zirconium diboride and iron, cobalt, and nickel were resistance sintered to high-density compacts using modified electric welding equipment. To evaluate the use of iron, cobalt, or nickel as binders for zirconium diboride, the sintered compacts were examined in polished section and tested for crushing strength, hardness, microhardness, oxidation rate, and resistance to mechanical shock. Each of the zirconium diboride-metal mixtures produced brittle cermets, but the hardness was generally satisfactory. The iron- and cobalt-bonded cermets exhibited rather poor oxidation resistance. Cobalt provided the least brittle bond, and nickel, the hardest and most resistant to oxidation. Iron tended to form chalky compacts with low resistance to mechanical shock.

Jan 1, 1963

By J. G. Donaldson

A bench-scale method for recovering lead and zinc from slimes and mill tailings from the Tri-State District of Missouri, Oklahoma, and Kansas was developed by the Bureau of Mines. Dilute hydrochloric acid, containing sodium chloride, and chlorine gas were used to decompose the mineral constituents. Lead was electrolyzed from the pregnant acid solution, and zinc was precipitated from the depleted electrolyte by neutralization with lime. Up to 98 percent of the lead was recovered in an impure lead electro- deposit assaying approximately 85 percent lead. Zinc recoveries up to 90 percent of the total were attained in a precipitate assaying approximately 40 percent zinc.

Jan 1, 1963

By C. O. Hawk

As an exploratory effort to produce useful products from coal by a new path, the Bureau has made a few experiments on the fast heating of finely ground coal particles by irradiation with a flash of high intensity light. The flash was produced by an electrical discharge at high voltage through a xenon-filled tube. The flashes lasted from 2 to 3 milliseconds. The reaction took place in small sample tubes, ½ inch-dimeter by 4 inches long, and with small amounts of coal (total amount charged 0.1 gram, probable effective amount not more than 20 milligrams). Average particle size of the coal, estimated on a numerical basis, was 20 microns. Temperatures reached were evidently quite high, because all products obtained in quantity were characteristic of high temperature pyrolysis. Apparently, conversion of the coal was extensive where isolated particles received the full benefit of a flash. It seems particularly significant that acetylene was present in appreciable amounts--comprising almost 3 percent of the total gaseous product in one case. This is good evidence of a short heating period to very high temperature (well above 1,000° C) followed by rapid quenching. Although the results are interesting, they do not suggest any immediate practical application.

Jan 1, 1963

By David Schlain

A small alumina reduction cell with a graphite crucible and boron nitride liner was developed by the Bureau of Mines as the initial phase of a study of the reactions which occur in the reduction of alumina by the Hall-Heroult process. Operating conditions in the cell such as temperature, time, current density, electrolyte composition, and electrode materials may be varied easily. Aluminum was produced in the cell at a current efficiency of about 75 percent and a cell voltage of 2.7 volts. Although the data are not wholly conclusive, the operation of the cell did not appear to be greatly affected by large changes in temperature, electrode spacing, current density, and alumina concentration in the electrolyte.

Jan 1, 1963

By C. M. McKinney

This report contains Bureau of Mines analyses of 291 samples of crude petroleum from the Gulf Coast Area of Louisiana and Texas. Included are 65 analyses from 51 Louisiana fields and 226 analyses from 216 Texas fields. Analyses from the Texas fields include 90 from 58 Upper Gulf Coast fields, 47 from 28 Middle Gulf Coast fields, and 89 from 40 Lower Gulf Coast fields. The analyses represent fields that produced 1,000 barrels or more per day during at least one of the years 19.57 through 1961, with the exception of 23 analyses from the Texas fields. The fields considered are listed by state and geographical groupings, with field names arranged alphabetically within each grouping. The tabulation also includes information concerning the geological sources of the samples. General characteristics of the crude oils and analytical and computed data determined from the analyses are summarized. Crude oil production data are given for the fields for 1960 and 1961 and are cumulative through 1961.

Jan 1, 1963

By Earle S. Burnett

This report outlines the experimental procedures for using a Burnett apparatus to obtain compressibility coefficients for multiphase, multicomponent fluid mixtures. The conventional Burnett method is described briefly whereby multiphase compressibility data can be obtained by first determining the compressibility factor, Z, as an isothermal function of pressure alone. Then starting at conditions of temperature and pressure where Z is known, the fluid is cooled at constant volume to some lower temperature at which the resulting pressure is measured, and a corresponding value of Z is obtained from a fundamental relationship between compressibility factors, pressures, and temperatures at constant volume. The isochoric treatment of the fluid, extended to still lower temperatures and along other isochors, eventually results in compressibility determinations for the whole two-phase system thus covered experimentally.

Jan 1, 1963

By Thomas L. McVay

Laboratory batch and pilot plant flotation tests were made to determine the feasibility of recovering commercial grade kyanite from a quartzite- kyanite rock from the Graves Mountain, Ga., deposit. Best results in laboratory and continuous tests were obtained using sodium carbonate for pH control, citric acid for quartz depression, and oleic acid as the kyanite collector. Over 80 percent of the kyanite was recovered in a concentrate analyzing 56.8 percent Al203 and 3.8 percent hydrochloric acid soluble Fe203. Subsequent treatment of the flotation concentrate by magnetic separation reduced the acid soluble Fe2O3 to 0.6 percent and increased the alumina content to 59.2 percent. Acid leaching of the concentrate gave a product analyzing 59.7 percent Al203 and about 0.1 percent Fe203. As a result of the beneficiation research, a commercial kyanite flotation plant was completed in September 1962 by private industry.

Jan 1, 1963

By A. F. Baker

Tests were conducted in commercial foundries to determine the suitability of calcined anthracite as a cupola fuel. The calcined anthracite performed satisfactorily at two of the three foundries where iron-melting tests were conducted. Performance at the third installation was unsatisfactory because metal temperatures deviated widely and, in general, were lower than is desirable for the type of castings being made.

Jan 1, 1963

By Wilbur I. Duvall

Twelve millisecond delayed blasts in four limestone quarries in Iowa were instrumented with arrays of vertical velocity gages to determine if the direction of propagation through the rock or the method of initiation of the blast had any effect upon the level of vibration. Two gage arrays approximately 90° apart were used to test the effect of direction of propagation. The vibrations from blasts initiated by three methods were recorded. Vibration records from these tests were analyzed for peak particle velocity as a function of distance from the blast. The data are shown to fit a power Law equation. Direction of propagation is shown to affect the value of the exponent n. The effect of charge size per delay interval on the level of vibration is removed from the data by scaling the travel distance by the square root of the charge weight per delay period. The method of initiating the blasts is shown to have a strong effect upon the level of vibration and the spread in the data from one shot to another.

Jan 1, 1963

By Earl L. Hastings

Although the principal market for diatomite in the United States is in the East,4 production of the material is presently restricted to the West, because the deposits are larger, mining costs are cheaper, and the quality of product is better than that obtained from other domestic deposits. However, Tallahatta diatomite, occurring in Choctaw and Clarke Counties, Ala., has a freight rate advantage, which should encourage competition for those market that are now being supplied with the purer diatomites from the western deposits. For this reason, diatomite occurrences in the Tallahatta formation were examined by the Bureau of Mines and physical properties of samples from the deposit were determined to obtain additional data for use by any potential producer who wished to evaluate the material for its commercial possibilities. In 1894 K. M. Cunningham5 found that the buhrstone formation (now known as the Tallahatta formation) contained "siliceous shells of marine diatoms, radiolaria and foraminifera, thus being rather of the nature of tripoli or diatomaceous earth than of a true clay." Cooke6 and Semmes7 also reported the Tallahatta formation to be composed principally of diatomaceous earth with accompanying beds of sand, clay, and sandstone.

Jan 1, 1963

By N. H. Coates

A small, special-purpose centrifugal compressor was developed to circulate 60 pounds per hour of helium at 1,000° F and 250 psig because standard, commercial units were not available. Performance characteristics of this compressor were determined at helium flows of 2,000 to 18,000 std cu ft per hour, pressures of 100 to 250 psig, and temperatures of 100° to 1,000° F. This range is 2 to 90 actual cu ft per minute. Several graphs show the adiabatic head developed by the compressor over this wide flow range at various combinations of temperature and pressure. A compressor performance map relates pressure ratio to mass flow, temperature, pressure, and speed. This map can be used to accurately predict compressor performance factors within the range of operating conditions covered by the experiments.

Jan 1, 1963

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 Michael Sokaski

A dense-medium cyclone pilot plant was built to clean 112-inch to 0 size coal. This pilot plant does not require the removal of the extremely fine material (usually minus 1/2-mm) from the feed, which is necessary in conventional dense-medium cyclone plants. The essential difference between conventional cyclone plants and the pilot plant is in the medium-recovery system. The latter uses a combination of sieve bend screens, classifying cones, and magnetic separators for medium recovery. Eight tests were run in the pilot plant at a feed rate of 5 tons per hour with four different raw coals and one crushed jig middling product. Sharp separations were obtained as indicated by an average error area of 27 and probable error of 0.047 for the 112-inch to 200-mesh size range. Magnetite loss averaged about 2.5 pounds per ton of feed. The influence of several factors on cleaning performance of the cyclone was investigated. The diameters of both the overflow and underflow orifices were found to be important for optimum cleaning performance, but these diameters could vary over a wide range without serious effect; however, if this range was exceeded, cleaning performance deteriorated. Better cleaning performance was obtained when the cyclone inlet pressure was increased from 9 psig to 13 psig. The size of the magnetite particles in the medium was found to have a substantial effect, and the best cleaning results were obtained with grade B magnetite. Demagnetizing the magnetite in an effort to decrease the effective particle size did not improve cyclone performance.

Jan 1, 1963

By H. E. Powell

This study was made to determine the capabilities and limitations of the hydrocyclone for separating quartz sand from impure clays, Optimum operating conditions for beneficiating typical subgrade clays were determined. Estimates are furnished for installation and direct operating costs of hydrocyclones in such separations. Laboratory models of commercial hydrocyclones were used to beneficiate a suite of fire clays including plastic, semiflint, and flint types, all of which were contaminated with quartz in amounts ranging from 3 to more than 62 percent. Results show that this technique is not limited to a single type of clay but is applicable to clays ranging from plastic through flint, Under proper conditions use of this technique will result in good separation of the sand and good recovery of a useful clay mineral concentrate. Rejection of quartz from the clays investigated ranged from a low of 82.4 percent with an alumina recovery of 71.2 percent to a high of 99.0 percent with an alumina recovery of 85.6 percent.

Jan 1, 1963

By Thomas M. Nasiatka

Tests with a high-pressure water jet were conducted in the steeply pitching Roslyn No. 5 bituminous coalbed in the Roslyn No. 9 mine, Roslyn, Wash., to determine the feasibility of extracting coal from pillars and from a solid coal face in development without drilling and blasting. During pillar mining, using a hand-held monitor, the best results were obtained with a 0.150-inch- diameter nozzle, a water pressure of 3,500 psi, and a flow rate of 38.5 gpm.3 The rate of mining and productivity were 0.74 ton per minute and 16.6 tons per man-shift, respectively. During development mining, using a monitor mounted on a roof jack, the best results were obtained with a 0.148-inch-diameter nozzle, a water pressure of 4,500 psi, and a flow rate of 40.0 gpm. In one section of the mine where the coal was relatively hard, the rate .of mining and productivity were 0.10 ton per minute and 5.7 tons per man-shift, respectively in another section of the mine where the coal was relatively soft, the rate of mining and productivity were 0.51 ton per minute and 8.3 tons per man-shift, respectively. The tests showed that hydraulic mining methods were more productive than conventional mining methods in pillar mining. In development the productivity of hydraulic mining depended primarily upon the coal hardness. Compared with conventional methods, hydraulic mining methods were less productive where the coal was relatively hard and equally as productive where the coal was relatively soft.

Jan 1, 1963

By Thomas E. Green

A combined solvent extract ion-spectrophotometric method for the determination of as little as 1 ppm of copper in tungsten metal or tungstic oxide has been developed and evaluated. Metallic samples are converted to tungstic oxide by treatment with hydrofluoric and nitric acids. The oxide is then dissolved in sodium hydroxide, and the copper is extracted as the colored neocuproine complex. Total elapsed time for the analysis is approximately 1-1/2 days; however, actual working time for a group of six or eight determinations is less than 4 hours. Precision at the 2-ppm level is better than 0.1 ppm.

Jan 1, 1963