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By A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By David J. Kusler

This report describes a primary or direct, continuously sampling, and automatically averaging gravimetric method for analyzing gaseous mixtures of carbon dioxide, carbon monoxide) hydrogen, and (by volume measurement) nitrogen. The gaseous mixture is analyzed by passing it at a controlled and definite rate through a system that permits carbon dioxide and water retained by appropriate absorbents to be determined and the residual-gas volume (essentially nitrogen) to be measured. The accuracy and dependability have been established by comparison with very carefully conducted Orsat analyses. The method was developed for, and has been satisfactorily applied to, the analysis of blast-furnace top gas. It permits relatively attention free operation, using simple and low-cost materials usually found as basic equipment in the analytical laboratory. It provides, over a wide range of time or sampling intervals (from less than 1 to over 24 hours), the average composition, in terms of volume-percent, for those components usually determined in blast-furnace gas, if (as is usual) the flow rate of gas from the blast furnace is essentially constant over a selected analysis interval. Oxygen and methane are not determined; but, since these gases are normally absent or present only in traces, their analysis is seldom required.

Jan 1, 1959

By W. E. Webb

This report describes a method the Bureau of Mines devised for measuring the dielectric constant and loss tangent of low-loss minerals at microwave frequencies. Determina-tion of these properties makes it possible to predict the effects of using microwave heating in potential mineral processing applications. The method uses a test cell and radio-frequency (RF) impedance analyzer with automated data acquisition and analysis. In this initial phase of microwave heating research, the Bureau measured dielectric constants and loss tangents at frequencies between 100 MHz and 1 GHz. The objective was to establish a reliable data base for use in predicting the effects of microwave heating on minerals. Comparison with previously measured data showed the Bureau's measurement method to be accurate to within ± 3 pct. This report describes the method and discusses the preliminary results of the Bureau's investigations. Typical comparative data are included.

Jan 1, 1986

By John M. Gomes

A two-phase molten halide-silicate technique for extracting tungstic oxide (WO3) from scheelite (CaW04) and wolframite [(Fe, Mn)W04] was investigated. The halide phase extracted over 99 percent of the was, whereas the lower silicate phase retained about 90 percent of the calcium, iron, or manganese oxides. The most efficient extraction and separation of tungsten from scheelite was accomplished at 1,080° C in a molten system containing, in mole-percent, 9 calcium tungstate (CaW04), 42 sodium chloride (NaCl), 28 sodium fluoride (NaF), 17 sodium metasilicate (Na2SiO3), and 4 alumina (Al2O3). Wolframite was also treated at 1,0800°C; the molten system contained, in mole-percent, 11 (Fe, Mn)W04, 74 NaCl, and 15 Na2 SiO3.

Jan 1, 1968

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 H. B. Salisbury

As a part of a research program designed to help minimize national requirements for new mineral commodities by maximizing recovery of metals from domestic secondary resources, the Bureau of Mines investigated the development of economic methods for recovering copper and associated metals from complex electronic scrap. Three types were selected for research: (1) multiple-pin plugs and connectors, (2) obsolete aircraft radio assemblies, and (3) the magnetic fraction of shredded electronic scrap furnished by the Bureau's Avondale Research Center. The plugs and connectors, after incineration to remove plastic components and melting, yielded a brittle ingot, as did the internal portion of the radio assemblies. The brittle ingots were ground to minus 35-mesh for processing, and the magnetic material was used in the as-received condition. A process using pretreated or raw scrap as a copper precipitant in various concentrations of acidulated copper sulfate solution was developed as a means of effecting an initial separation and upgrading in the form of high-grade cement copper containing all or most of the precious metals.

Jan 1, 1981

By H. M. Smith

Data from the Bureau of Mines routine method for the analysis of crude petroleum are used to characterize crude oils. Some data are used directly while other data are used to calculate the aromatic) naphthene) and paraffin contents of the distillation fractions and the correlation index of the paraffin-naphthene portion of the fractions. The calculated properties show significant differences in composition between crude oils. The methods of calculation and interpretation of data are explained and illustrated.

Jan 1, 1966

By Gary P. Sames

This U.S. Bureau of Mines study was conducted in eastern Kentucky drift mines as part of an ongoing research program to characterize the outcrop barrier zone. "Hillseams" were identified as the dominant geologic cause of roof instability unique to the outcrop barrier zone, with many roof fall injuries and fatalities attributed to them. Hillseam is the eastern Kentucky miners term for weather-enlarged tension joints that occur in shallow mine overburden where surface slopes are steep. Hillseams are most conspicuous within 200 ft laterally of a coalbed outcrop and under 300 ft or less of overburden. Hillseams form by stress relief, and therefore tend to parallel topographic contours and ridges. They can intersect at various angles, especially under the nose of a ridge, and create massive blocks or wedges of roof prone to failure. Examples of hillseams are described in both outcrop and in coal mine roof to establish their geologic character and contribution to roof failure.

Jan 1, 1989

By J. M. Stuve

Low-temperature heat capacities and the enthalpy of formation were deter-mined calorimetrically by the Bureau of Mines for CuO?CuS04. The derived standard entropy (S°298.15) was 40.36±0.04 cal/deg-mole, and the enthalpy of formation (?H°f) was -219.l±0.3 kcal/g-mole. A large thermal anomaly was observed in the heat capacity of CuO?CuS04 at 20±0.1 K. Gibbs energy of formation data are tabulated up to 1,200 K. Construction details of a precision low-temperature adiabatic calorimeter capable of determining heat capacities of solids in the temperature range 5 to 320 K are given. A calibrated miniature germanium resistance thermometer was incorporated into the calorimeter to extend the range of accurate measurements below 15 K. High-resistance dc heater windings were used throughout the cryostat to reduce heat conduction of inner connecting wires.

Jan 1, 1975

By R. E. Siemens

The Bureau of Mines sought to correlate the variation of structure-sensitive superconducting properties with microstructure in selected Cb-Hf alloys and to compare the experimental results with those predicted by the GLAG theory. Alloys in wire and rod form were evaluated by critical temperature, critical current, magnetization, resistivity measurements, and optical and electron microscopy. In the absence of an external magnetic field, the current carrying capacity of columbium was greatly reduced with addition of up to 85 wt pct Hf, but a large increase in Ic occurred for Cb-90 wt pct Hf. Favorable Ic-H behavior was observed in cold-drawn alloys containing 25 and 57 wt pct Hf. Correspondingly, a maximum in Tc occurred at 10-25 and 90 wt pct Hf. Four- or five-hour heat treatment at 600° C resulted in maximum Ic values and maximum hysteresis in magnetization. Dislocation pileup, polygonization, and fine precipitates, responsible for flux pinning, are listed in order of their effectiveness as pinning sites. Sites having an average separation of 1,500 to 3,000 A and a diameter of 1,000 A or less were most effective in influencing Ic-H and M-H behavior. The resistive critical fields increased smoothly to a maximum of 80 k0e between 60 and 65 wt pct Hf. Highfield, mixed state, reversible paramagnetism was observed in some alloys; however, the GLAG theory was in good agreement with experimental results for the majority of the composition range studied.

Jan 1, 1969

By Robert W. Geehan

The Bureau of Mines developed, by core drilling, the property of Nevada Scheelite, Inc., from October 5, 1943, to February 24, 1944. Claims of the corporation are near Rawhide in the northern portion of Mineral County, Nev. The purpose of the work was to determine possible reserves in the lateral and vertical extensions of a tactite zone which was being mined for scheelite. Production from this zone to January 1, 1944, was said to be 64,500 tons, with a recovery of 50,618 units of tungsten trioxide. The development work was done by the Bureau of Mines in cooperation with the U. S. Geological Survey and comprised a study of the geology, mapping the areas, and exploring the deposit by diamond drilling, trenching and sampling. Eleven holes were drilled for a total footage of 2,365 feet of holes.

Jan 1, 1950

By ALICE V. Petar

Thallium is one of the rare metals that has come into commercial use within recent years . Its comparative scarcity , combined with a resemblance to the common metal lead , have retarded the development of uses for thallium . Although production is still measured in pounds rather than in tons , it is now finding application in a number of fields . Perhaps the earliest commercial use of thallium was as a constituent of optical glass of higher refractive power than similar glasses containing lead . One of the later applications to attract attention was the use of the oxysulphide in a sensitive electrical device similar to the selenium cell . The " Thalofide " cell , which was patented in 1919 , constituted for a time the most important outlet for thallium. During the next few years the limited use of thallium and its salts in other fields was insufficient to absorb an annual production of a few hundred pounds , and the price dropped from $ 16 or $18 per pound in 1922 to $ 5 per pound in 1924 . Beginning in 1925 several new uses were developed , especially as a poison for rodents and ants , and as a result the demand for thallium increased sufficiently to cause a recovery in price to the present level of from $12 to $15 per pound .

Jun 1, 1931

By A. J. Forney

Recent experiments used catalysts of plate assemblies in synthesizing high-Btu gas and gasoline indirectly from coal. A gas with a heating value of 925 to 943 Bt-: per cubic foot has been prod u la the hot-gas-recycle pilot plant from synthesis gas (3H2+100) with lathe turnings used as catalyst in the first reactor, and assemblies of parallel sprayed plats of nickel in the second. Solid plates made of Raney nickel, and steel and aluminum plates sprayed with Raney nickel or nickel oxide were tested. Those catalysts had very low resistance to gas flow; 90 percent lower than nickel granules used in previous experiments. In a single stage of synthesis thee nickel plates were only partially successful. Although the heating values of the product gas ranged from 856 to 941 Btu per cubic foot, the carbon monoxide content of he gas was above 0.1 percent. Both steel and wrought turnings were tested in single-stage synthesis, but the conversion of hydrogen and carbon monoxide was too low to attain the desired heating value of 900 Btu per cubic foot in the product gas. Assemblies of plates thermally sprayed with fusel iron were tried in an experiment to make gasoline. A gasoline yield of 52 percent (of the hydro¬carbons produced) was obtained using a 1H2-10O feed These sprayed assemblies were in service for 1,500 hours, the longest that this type of catalyst has been used. When a second reactor containing Raney nickel catalyst was added in series with the first reactor, complete utilization of the feed gas was obtained because in addition to the liquid product, a high-Btu gas with a heating value of 800 Btu per cubic foot was made.

Jan 1, 1965

By Wm. O. Vanderburg

This report on the mining and milling of tungsten ores is the second part of a general study of the domestic tungsten industry. The first part, comprising general information on tungsten, has been printed as Bureau of Mines Information Circular 6821. The purpose of these papers is to increase efficiency in the mining, preparation, and utilization of the tungsten resources of the United States. The tungsten industry forms so small a part of the vast mining and metallurgical operations of the illation that private metallurgists have not had enough inducement to give special attention to the recovery of tungsten minerals from the ores, and many of the small companies are financially unable to undertake research work. A study of the milling of tungsten ores reveals that further improvement is possible, especially in the treatment of slimes. Recent experimental work by the Bureau shows that the flotation process is applicable to certain tungsten ores. The future of the tungsten industry it the United States depends to a great extent on utilization of the low-grade deposits of the contact-metamorphic type.

Jan 1, 1935

By Jr. Hill

Laboratory metallurgical treatments of three high-iron bauxite ores from Arkansas were conducted to determine the relative effectiveness of experimental methods for recovering alumina and a commercially acceptable iron concentrate. The standard for evaluating recoveries from experimental processes was the Al2O3 recovery from Bayer digests of the crude ores; recoveries from digestion of the three ores were 74.1, 87.4, and 88.7 percent. Flotation, magnetic separation, or various combinations of digestion, calcination, and reduction-sintering, leaching, and magnetic separation of leach residues failed to produce Al2O3 recoveries as high as the standard. A high-iron-bearing fraction, containing between 68 and 78 percent of the total iron, was produced in a three-phase treatment involving a caustic, lime reduction-sinter of the crude ore, water extraction of Al2O3 from the sinter, and magnetic separation of the leach residue.

Jan 1, 1967

By Richard D. Hagni

The character of phosphorous-bearing minerals in the Birmingham red Iron ores and iron-bearing minerals in the Eufaula bauxite deposits in Alabama has been Intensively studied by petrographic, ore microscopic, luminescent microscopic, scanning electron microscopic, electron microprobe, and x-ray diffraction techniques. A total of 15 types of phosphorous-bearing mineral grains have been recognized in Birmingham iron ores by their characteristic sizes, shapes, and distributions. Size measurements, modal analyses, and texture analyses have permitted an estimate of potential liberation of phosphorous from the iron ores by beneficiation to be 27% In areas of previous mining and 60% in areas of current iron reserves. Fine grinding, selective flocculation, and flotation may constitute the best beneficiation technique for future research. Hematite and goethite are the most important iron minerals in Eufaula ferruginous bauxites, but pyrite, marcasite, and siderite are Important iron minerals in some varieties of ferruginous bauxite, and lepidocrocite and ilmenite occur locally in minor quantities. Although simple screening will remove the coarsest iron-bearing grains, research on the utilization of high gradient magnetic separation to reduce the amounts of iron-bearing grains is recommended.

Jan 1, 1981

By H. S. Auvil

[Coals of low-volatile rank cannot be coked without admixing large proportions of high-volatile cod in the used type of byproduct-coke oven, because they expend excessively and. exert side thrust, which ruins the oven wells. Some medium-volatile coals also give trouble. Since high-rank coals produce a strong, blocky coke, it is desirable to have the rank as high as practicable, particularly in the manufacture of foundry coke. Accordingly, it has become the practice to mix or blend high-volatile shrinking coals with as much low-volatile coal as possible and still have a mixture that mill not deform the walls or cause difficulty in pushing the coke. Occasionally, the safe limit of low-volatile cool has been exceeded and ovens have been damaged. It is desirable, therefore, to have a reliable method of determining the expending tendencies of mixtures before they are charged into the ovens. Furthermore, coal changes somewhat in its properties as mining progresses, end therefore, mixtures found to be safe at one time may cease to be so subsequently, particularly if nearly the maximum allowable percentage of low-volatile coal is being used. ]

Jan 1, 1938

By G. S. Scott

The Bureau of Mines is engaged in research to assess the hazards associated with the handling, storage, and use of combustible gases, vapors, and. liquids encountered in mines and in industry. As a part of this general pro-gram, numerous limits of flammability and ignition temperatures are being investigated for a wide variety of combustible materials, and methods are being developed to minimize the explosion hazards of these combustibles. The Bureau receives numerous requests for information on the explosion hazards of specified combustible mixtures under various conditions of use. This information circular has been prepared to assist those who may have similar requests. Destined primarily for the layman with a limited technical knowledge of the subject, it considers rather briefly the numerous factors that enter into the general problem of gaseous explosions and their prevention.

Jan 1, 1951

By A. H. Beebe

This paper describing the operations of the Cresson mine of the Cresson Consolidated Gold Mining & Milling Co. at Cripple Creek, Colorado, is one of a series of papers on mining methods and costs being prepared by the United States Bureau of Mines. The Cresson has recently been the most, important mine in the Cripple Creed district. During 1932 and 1933 an average of 230 tons of new ore (excluding dump material) that averaged about $10 in gold was shipped daily; 150 to 175 men were employed. Stoping was by the shrinkage method exclusively. The ore was screened washed, and hand-sorted at the surface and shipped to the Golden Cycle mill at Colorado Springs for treatment. A considerable proportion of the production was made by lessees working under the so-called "split-check" system. The authors are indebted to the management of the Cresson Consolidated Gold Mining & Milling Co. for permission to publish this paper.

Jan 1, 1934

By James J. Dowd

The investigation to evaluate the reserves of coking coal is being made by the Bureau of Mines in three parts: (1) To estimate known (measured plus indicated) recoverable reserves of all coking coal, (2) to upgrade marginal coals through effective preparation, and (3) to study the carbonizing properties of coal and coal blends not now widely used for metallurgical coke making. This is the seventh of a series of reports giving the results of studies by counties under part (1) of the investigation. (See appendix.) This report covers Floyd County, KY., which comprises parts of the Paintsville, Prestonsburg, Harold, Hindman, and Pikeville quadrangles. (See fig. 1.) A base map for each bed in each quadrangle was made to the scale of 1 inch equals 1,200 feet. Maps of mines, locations of drill holes, bed and total coal thicknesses, and the outcrop of the bed were plotted on the maps. With all avail-able data plotted, isopach lines were drawn to limit areas of known unmined reserves in beds up to 14 inches thick, 14 to 28 inches thick, 28 to 42 inches thick, and over 42 inches thick. These areas of coal reserves also were divided into "measured" and "indicated" categories. All areas in each thickness range and in each category, mined-out areas, areas excluded from the estimate but which may contain reserves based only on geologic inference, and areas outside of the outcrop were measured by planimeter on the base maps. Estimates of total reserves 14 inches and more thick and maps for individual beds were prepared from these data.

Jan 1, 1951