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By F. W. Wessel

This report summarizes Bureau of Mines laboratory tests of four tungsten¬-bearing materials of various grades, The test work has demonstrated that the dry reaction between sodium carbonate and scheelite is best conducted at 900° C. or a few degrees less. The sodium carbonate requirement, in addition to the stoichiometric equivalent of the scheelite, is in some inverse relationship to the grade of tungsten in the ore. Residence time and particle size exert a definite but minor control on the reaction. Pressure-digestion tests on an impure concentrate indicate the technical feasibility of extraction by this process. INTRDUCTION Over 100 years ago Oxland discovered that tungstic oxide could be removed from wolframite and converted to a soluble form by reacting the mineral with a soluble alkaline salt at elevated temperatures. He patented this discovery, and this patent 4/ since has been the basis for most tungsten extraction. Much literature exists on this process and its modifications, and the characteristics and possibilities of the reaction are quite well defined.

Jan 1, 1956

By William B. Harper

Domestic sales of carbon black sustained the upward movement for the 4th consecutive year, reflecting the increased sales of motor vehicles during the same period. Sales of carbon black in the domestic market topped 2 billion pounds for the first time during 1965 and have more than doubled the output of 20 years earlier. By far the largest user of carbon black is the rubber industry. That use accounted for more than 94 percent of the carbon black consumption with the bulk of it being used in tire casings and tubes. Thus demand for carbon black is naturally sensitive to trends in the sales of passenger cars and other motor vehicles, Manufacturers of inks, paints, plastics, paper chemicals, and food are also important users of carbon black.

Jan 1, 1967

By R. Wiebe

During a recent investigation the authors were interested in determining: (1.) How many points were necessary to locate the deviation curve for copper-constantan thermocouples within an accuracy of about 0.05° C., used in connection with the "standard" thermocouple of L. H. Adams. (2.) Whether copper-constantan thermocouples showing considerable deviations from the "standard' were consistent throughout their calibration. (3.) How reliable the extrapolated portion is - that is, the interval between -183 and -220° C. of the "standard" thermocouple. It seems that a calibration between 0 and -193° C. can be made within the stated accuracy by determining experimentally the e.m.f. of the particular couple at -78.50°, the normal sublimation point of carbon dioxide, and at -182.97°, the normal boiling point of oxygen. Substituting the values found for the two fixed points in the simple quadratic. Equation

Jan 1, 1931

By Victor Kalcevic

A gas-flow retort for thermal processing of oil shale to recover shale oil was developed by the Bureau of Mines at its Oil-Shale Demonstration Plant, Rifle, Colo., from 1948 to 1952. The retort is a crossflow gas-to-broken-solids heat exchanger. The heating medium is the gas produced in the shale retorting process. The gas is heated in specially designed stoves outside the retort and recycled to the retort. Oil shale from the Mahogany ledge section of the Green River formation in northwestern Colorado was the material processed. Indicated maximum oil recoveries for 20-to 25-gallon-per-ton shale in a l2-inch-thick shale bed and a 20-inch bed are 96 and 91 weight-percent of Fischer assay, respectively. Heat requirements for maximum recovery are 600 to 750 B.t.u. per pound of shale. Properties of the recovered shale oil are affected slightly by shale-bed thickness and extent of retorting. Oil recovery from oil shales assaying over 30 gallons per ton is lower than that from leaner shales.

Jan 1, 1959

By Louis C. Brichta

The Kline tract ?3.nd the Frey tract are two separate properties situated in the Wentworth district on the easterly edge of the Tri-State zinc-lead region (fig. 1). The Kline tract is in the southwestern corner of Lawrence County, Mo., and the Frey tract, 1 1/2 miles west of the Kline, is in the northeastern part of Newton County, Mo. A bureau Of Mines drilling project embraced work on both properties, but the amount of work done on the Frey tract was comparatively small. At the time of the project the Kline tract was under lease to the Wentworth Mining & Milling Co. The Surprise Mining Co. held the lease on the Frey tract. Underground workings on the generally flat-bedded are deposits of the Kline property-covered an area of-about 15 acres. No total metal-production records are available. In 1942-1943 the mine, operated by the Wentworth Mining & Milling Co., produced at an average monthly rate of 83 tons of 60-percent zinc concentrate derived from mining and milling 1,700 to 2,100 tons of ore. At the end of that period no significant amount of reserve ore was in sight. The gravity-flotation mill on the property was operating at about one-sixth capacity.

Jan 1, 1949

By J. M. Gomes

The Bureau of Mines, as part of an effort to maximize minerals and metals recovery from domestic resources, has investigated the feasibility of recovering heavy minerals as byproducts from sand and gravel, placer gold, and industrial mineral operations in northern California. Sand samples from about 50 locations were treated by gravity separation to yield heavy-mineral concentrates (black sands). Mineral compositions of the concentrates were determined by chemical analysis and mineralogical examination. Individual zircon, ilmenite, magnetite, platinum-group metals, thoria, and silica products were prepared from heavy-mineral concentrates by selective separation using low-and high-intensity magnetic, high-tension, and flotation equipment.

Jan 1, 1979

By John J. Sammarco

The U.S. Bureau of Mines is conducting research into computer-assisted mining, which requires investigation of new techniques for development and application of computer-based technologies. Today's technology can require significant effort in software development, as has become evident in the early stages of this Bureau research. Technologies for software automation, such as computer-aided software engineering (CASE), are available. This report explores CASE, its general features, and its importance in software development. Information is presented to assist in selection and application of the variety of CASE tools and methods for automating various stages of software development. When evaluating CASE for use, it is important to examine tools that support an organization's existing methods of software development. Support for existing hardware platforms must also be examined. Merely selecting a "good" CASE tool does not insure success. Thorough evaluation of implementing CASE is also critical. Subjects to evaluate for CASE implementation include organization culture, support from management and end users, training resources, and pilot projects. Organizations that benefit the most from CASE evaluate CASE features with respect to their needs and they properly implement CASE.

Jan 1, 1990

By G. L. Cook

The design of a dual-inlet system for a Consolidated model 21-103C mass spectrometer is described in detail. The system permits both high-mass and low-mass samples to be run by using a single instrument. The difficulties of using a single instrument for both purposes are given and a method of minimizing these difficulties through the use of the present design is discussed, After examining the experience of five years of use, the conclusions are that the bimodal operation is practical and the low-mass analyses had nearly the same precision as before the modifications to the instrument were made. In 1951, O'Neal and Wier.5/ published the first description of the modifications made to a mass spectrometer so that the spectra of hydrocarbons with molecular weights up to 600 could be obtained. Further discussion of the equipment of O'Neal appeared in 1953.6/ Also, Brown, Melpolder, and Young7/ described a parallel inlet system designed to reduce sorption effects at room temperature.

Jan 1, 1960

By H. R. Batchelder

The Bureau of Mines Gas Synthesis Demonstration Plant at Louisiana, Mo., includes apparatus for the gasification of pulverized coal with oxygen and superheated steam. A pebble heater constructed by the Babcock & Wilcox Co. is used to superheat nominal 5-pound steam for the gasification process, usually to temperatures of 1,600° to 2,300° F. with flow rates of 1,400 to 2,300 pounds per hour. Heaters of this sort have been described. So far as is known, the Babcock & Wilcox Co. is the sole commercial manufacturer of equipment of this type. Units have been built with capacities above 18,000 pounds of steam per hour.

Jan 1, 1951

By A. L. Engel

This report is a compilation of results of preliminary concentration tests of nine manganese-ore samples in 1953-1954. Three samples were from Nevada and the other six from California. These samples represent marginal or low-grade ores from deposits that have been mined selectively in the past. The present interest lies chiefly in the possibilities of concentration of the remaining low-grade ores for economical exploitation. The treatment methods included gravity concentration and flotation in most cases. Results were sometimes unsatisfactory, particularly when the ore was too fine grained for liberation of the minerals within economical grinding range. The contaminating gangue minerals, such as quartz and iron oxides, were locked with the manganese to an extent that prevented separation of high-grade concentrates with satisfactory recovery. In cases where fairly good concentrates were made, it was at the expense of recovery, a condition typical of low-grade ores.

Jan 1, 1955

By Donald F. Reed

In the latter half of 1948 the Bureau of Mines investigated the Magnet Cove Rutile Co.'s prerty in northern Hot Spring County, Ark. This work was supplemental to the work done by the Bureau on the same property in 1945.2/ It was undertaken for the purpose of investigating the extent of the ore body toward the south and west and at depth and to obtain representative samples of the ore for metallurgical tests. For the latter purpose, the samples were so taken as to minimize alteration of the physical characteristics of the ore, these characteristics being determining factors in working out processes of bencficiation. During the investigation, 27 holes were drilled, 10 with a diamond-coro drill end 17 with churn-drill rigs using a Baker standard cable-tool core barrel. Drilling developed an extension of the ore deposit westward from the previously mined area but did not disclose the full depth of mineralization. Metallurgical tests to determine methods of beneficiating the ore and utilizing the resultant products are now in progress.

Dec 1, 1949

By H. R. Babitzke, H. Kato, M. D. Carver

A number of columbium and tantalum alloys were investigated to determine their suitability for use at elevated temperatures . Columbium-vanadium , tantalum-vanadium , and tantalum-hafnium alloys , and also columbium- 10 wt pct titanium alloys modified with additions of 0.1 to 2 mole pct ZrO2 , TiO2 , ZrB₂ , TiB , ZrC, or TiC were prepared and examined . Workability , tensile properties , and oxidation resistance were tested . Of the columbium alloys studied , the columbium- 12 at . pct vanadium exhibited the best properties ; it compared closely with the columbium- 10 at . pct vanadium alloy studied in a previous investigation.

Jan 1, 1964

By Hillary W. St. Clair

The reduction zone of the iron blast furnace is represented by a mathematical model of the chemical reactions and heat transfer that occurs between gas and solids during the deoxidation of iron oxide. The model consists of a set of equations and an algorithm whereby the equations may be solved to give the temperature and composition of gas and solids at any position in the reaction zone and at any time after a specified initial state. The model is applied to the special case in which ferric oxide is reduced by graphitic carbon and carbon monoxide produced by burning carbon in dry air. The rate of reduction, carbon consumption and maximum temperature are shown as functions of the temperature and rate of flow of the incoming reducing gas and external heat loss. The model of the reduction zone is the essential part of a general mathematical model for simulation of the iron blast furnace. The simulation model will serve as a research tool to be used in conjunction with an experimental or operating furnace. After the simulation model has been correlated with the real furnace, it is proposed that further experimentation be done mostly with the model. The real furnace will then be operated primarily to test and confirm the model.

Jan 1, 1967

By J. L. Shultz

The Bureau of Mines extended its investigation of methanation catalysts. The noble metals (platinum, palladium, ruthenium, rhodium, osmium) and rhenium), molybdenum, and tungsten were tested in hydrogenations of carbon monoxide and carbon dioxide at 21 atmospheres in a temperature range between 200° and 600° C. From the 8 metals studied) 25 catalysts represent 5 catalyst types were prepared and tested. The impregnated 0.5-percent-ruthenium catalyst proved to be the most active and versatile of all the catalysts produced. Tungsten and the noble metals other than ruthenium were low in activity and usually required temperatures above 500° C for appreciable production of hydrocarbons. Molybdenum was moderate in activity, but further improvement in molybdenum catalysts seems possible.

Jan 1, 1967

By Robert H. Peters

This U.S. Bureau of Mines report identifies the types of serious accidents that occur most frequently at small underground coal mines and describes the strategies that could help prevent these accidents. A wide variety of methods for improving safety are suggested, including improvements in the design of equipment, work procedures, work schedules, safety programs, and emergency response plans, as well as techniques for diagnosing the potential hazards associated with new technologies and work procedures. Some of the papers in this volume focus on preventing specific types of mining accidents--ones associated with materials handling (primarily back injuries), equipment maintenance, improper machine guarding, and ground failure during retreat mining. Although the recommendations in this volume are heavily influenced by research performed at underground coal mines in the Appalachian coalfields, most of the papers contain advice that is equally pertinent to almost any type of mine.

Jan 1, 1994

By H. M. Thorne

The oil-shale deposits of the Puertollano basin in the Spanish province of Ciudad Real appear to have been give little consideration in discussions of oil-shale resources throughout the world. A small, integrated oil-shale operation has been conducted at Puertollano since about 1922 by a French company, Sociedad Mimora y Metalurgica de Penarroya, hereinafter referred to as "Penarroya", but only within recent years have the potentialities of the Spanish oil-shale deposits been recognized. Empresa Nacional "Calvo Sotelo" do Combustibles y Lubricantes, hereinafter designated as "Calvo Sotelo," which was created in 1942 by the National Industrial Institute of Spain to produce liquid fuels from oil shales, has made marked progress in the design and construction of a complete oil-shale plant at Puertollano. Penarroya is mainly a coal-mining company, and the oil-shale operations were on a small scale of approximately 220 tons a day in October 1947. It is an integrated operation comprising oil-shale mining and retorting and shale-oil refining. Motor gasoline, Diesel fuel oil, light burner fuel oil, lubricants, paraffin wax, cresols, and ammonium sulfate are manufactured.

Jan 1, 1950

By R. J. Leary

Oxidation testing of copper-clad steel strip was performed in a muffle furnace to determine whether copper in contact with steel scrap could be removed by oxidation in an airstream at high temperatures. Substantially all of the copper was oxidized before any significant iron oxidation occurred. The rate of copper oxidation was not affected by contact with iron. Copper oxide scale separated spontaneously from the underlying metal during cooling. Results indicate the possibility of removing light-gage copper coatings and components from ferrous scrap by oxidation in an incineration process.

Jan 1, 1965

By Arne Landsberg

A study of the chlorination kinetics of germanium, silicon, iron, tungsten, molybdenum, columbium, and tantalum has been made to determine the effects of temperature, chlorine concentration, geometric surface area and gamma radiation. The reaction products were volatile at the temperatures used this making it possible to follow the reaction rates by weight loss of the solid. Chlorination rates of germanium, silicon, and iron were found to be directly proportional to chlorine concentration while the rates for tungsten, molybdenum, columbium, and tantalum were proportional to the 0.5 to 0.6 power of chlorine concentration. A good correlation of reaction rate and geometric surface areas was not obtained because the true surface area of the samples could not be measured. Intense gamma radiation had no effect on reaction rates. The Arrhenius activation energies determined over the temperatures used are as follows: Germanium, 27 kcal/mole (233°-241° C); silicon 33 kcaL/mole (375°-517° C); iron, cold rolled, 20 kcal/mGle (259°-325° C) annealed, 21 kcal/mole (293°-337° C); tungsten, 43 kcal/mole (617-776° C); molybdenum, 37 kcal/mole (445°-4910 C); columbium) 34 kcal/mole (229°?255° C); and tantalum, 29 kcal/mole (370°-449° C).

Jan 1, 1965

By H. R. Babitzke, H. Kato, R. E. Siemens, G. Asai

The purpose of this investigation was to develop a wide variety of columbium and tantalum alloys and to determine their suitability for use at elevated temperatures . Sixty - nine columbium and tantalum alloys were investigated . For this study , columbium was alloyed with two or more of the following : nium, tungsten , vanadium , titanium, and zirconium . Tantalum was alloyed with vanadium or hafnium, or hafnium and carbon . The fabricability was determined by an arbitrary procedure . Hardness measurements , elevated - temperature tensile properties , and oxidation- resistance studies were made . Of the alloys studied , Cb - 15 Hf - 5W, Cb - 15Hf - 5W- 10Ti , Cb - 15Hf - 10W- 10Ti , Cb - 10V - 5W, Ta - 30V , and Ta - 20 to 33Hf exhibited excellent high - temperature properties . These alloys were not only easy to fabricate , but they also had good oxidation resistance and excellent high- temperature strength .

Jan 1, 1964

By L. R. Fisher

The purpose of this investigation was twofold: (1) To devise a rapid method for determining quantitatively the porphyrin-carboxylic acid content of a particular crude-oil porphyrin aggregate, and (2) to isolate porphyrins in the crystalline state from crude-oil porphyrin aggregates. The first purpose was accomplished by applying adsorption chromatography. In fulfillment of the second aim three different crystalline porphyries were isolated by methods which involved both adsorption chromatography and fractionation of benzene solutions with hydrochloric acid of varying strength. The three porphyrins had etio, rhodo-, and phyllo-type absorption spectra, respectively. INTRODUCTION Many samples of petroleum have, as interesting minor constituents, chemical compounds known as metalloporphyrins. Their presence in crude oil and other bituminous materials was first discovered by Treibs a quarter century ago. Much experimental work has been done on metalloporphyrins because of their importance to the petroleum industry. They have a deleterious effect on refining catalysts. The ash resulting from the burning of heavy fuel oil is very reactive, We to the presence of metallic constituents, particularly vanadium. In oil-fired gas turbines, the ash may build up on the blades, causing imbalance of the rotors and, in addition, severe corrosion. In industrial boilers, the ash residue is responsible for severe damage to boiler tubes and to the refractory brickwork (15).4 Through study of the chemical constitution of the various metalloporphyrins found in petroleum, much can be learned concerning the origin, migration, and history of crude oils.

Jan 1, 1961