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By H. R. Shell

To obtain a better understanding of the crystallization of fluoride containing amphiboles from melts, an investigation of the range of stability between fluoramphi-boles and other minerals was conducted by the Bureau of Mines. This study has shown that the stability of fluoramphiboles is strongly influenced by both fluoride concentration and isomorphic replacement. Over 150 reactions were made with different compositions and reaction conditions. substitutions attempted and the phases that formed when the composition was crystallized by cooling from the melt are discussed. The attainment of equilibrium in these multicomponent systems is not claimed. Many ions that would be expected to enter the amphibole structure instead resulted in crystallization of phases other than amphibole. Those compositions that resulted in a high yield of acicular fluoramphibole by crystallization from the melts are shown in table 2. The fluoramphiboles obtained from melts typically had an acicular crystal habit and a hardness of 6 to 7 on the Mohs' scale. Although many had relatively high length to cross section ratios, none were fibrous; it was concluded that the possibility of synthesizing a fibrous fluoramphibole from a melt was low. However, many compositions can be crystallized into a tough, hard, impact-resistant mass of interlocking acicular crystals.

Jan 1, 1958

By F. W. Smith

To determine whether preheating coals before carbonization would improve the coking properties of the coals, particularly the weaker coking coals, 3 coals, 1 each from Illinois, Kentucky, and Pennsylvania, and a blend of the Illinois with a Pocahontas coal were preheated before testing for coking properties in the Bureau's BM-AGA pilot oven. The effects of preheating on the chemical and physical proper-ties of the coals and on the yields of carbonization products and strength of the coke produced from the preheated coals were determined, as were also the effects of bulk density, gaseous atmosphere, and residence time during preheating. Most benefit from preheating was found with weaker or oxidized coking coals, whereas the more strongly coking coals and blends showed little effect. Direct charging of preheated coal to the coke oven without cooling gave better coke, increased yield of tar, and decreased yield of gas. INTRODUCTION Although 94 percent of today's coal production comes from fields east of the Mississippi, the Eastern States have only about one-third of the Nation's recoverable reserves. West Virginia, which now produces more than any other State, has much smaller reserves than Utah, Colorado, and Wyoming.5/ However, the manufacture of iron and steel in Western States, which has increased greatly since World War I, is handicapped by the scarcity of high-grade coking coals, such as are plentiful in the Appalachian region. Unless a practical method of improving the cokemaking property of local coals is developed, ferrous metallurgical industries in the West must continue to use inferior coking coals and to pay high shipping charges for better coals.

Jan 1, 1958

By Irving Hartmann

At the 9th International Conference of Directors of Safety in Mines Research a paper6/ was presented describing the initial phases of research by the Safety in Mines Research Establishment at Buxton, England, on the remote control of timber fires with high-expansion foam plugs in a rock tunnel. The work received extensive publicity, and great interest was aroused by the implied possibility that the method might be used successfully to control coal-mine fires, which for various reasons cannot be approached and attacked by standard fire fighting measures and frequently require sealing extensive, valuable coal properties and lead to loss of production and coal reserves and occasionally loss of lives. To investigate the practicability of the foam-plug technique under American min¬ing conditions, with room-and-pillar-type extraction and multiple entries, the Bureau of Mines in 1957 began an investigation at its Experimental Coal Mine, Bruceton, Pa, In preparation for this work it was necessary to rehabilitate and reinforce an elliptical tunnel in the mine where studies had been made, many years ago, leading to development of a ventilation system used in the Holland Tunnels between New York and New Jersey, and in many other vehicular tunnels.

Jan 1, 1958

By R. E. Morgan

Two sizes of Pennsylvania anthracite were gasified in the new-type Lurgi pressure generator at the Dorsten, Germany, works of the Steinkohlengas, A. G. These tests demonstrated that Chestnut-size anthracite and a Rice-Buckwheat mixture containing 27 and 19 percent ash, respectively, could be gasified satisfactorily at an elevated pressure in a fixed bed with oxygen and steam. These coals were especially prepared to approximate a rough-cleaned coal and a washed and screened product. The operating data obtained from the two tests and materials requirements are summarized. A wide range of reactant ratios could not be tested, nor could optimum operating conditions be determined, as the generator was being used throughout the testing program, employing normal operating practices, to produce gas for the gas grid; and the most economical coal, steam, and oxygen ratios may not have been used. Comparative costs are presented of the raw materials required for producing a high-B.t.u. gas, based on the operational data obtained from these tests and, to some extent, on data extrapolated from laboratory experimentation. A flowsheet of a proposed process for producing a high-B.t.u. gas by Lurgi gasification, followed by methanation, is also included.

Jan 1, 1958

By P. M. Sullivan

Galvanizers' sal skimmings have been treated by two methods of leaching in attempts to produce preflux solutions suitable for use in galvanizing operations. Both water-leaching and acid-leaching procedures are effective, except in severely exhausted skimmings when water-leaching becomes impractical. A preliminary analysis of the skimmings is not required. Solutions in the recommended concentration range can be produced conveniently by control of pH, specific gravity, and chlorine content. A technician would require only a short period of training to be able to perform the operations described.

Jan 1, 1958

By R. T. Johansen

The adverse effects on waterflooding and well-completion methods of clay minerals indigenous to petroleum-production formations recently have received considerable attention. Knowledge of the types and amounts of clay minerals present would allow estimates of the response of such formations to injected or infiltrated water; however, the random distribution of clays in sedimentary formations makes direct evaluation of ?water sensitivity? desirable. A method for the direct evaluation of water sensitivity has been developed, based on measurement of water-vapor adsorption. Correlation of such data with the results of nitrogen-adsorption measurements provides valuable information on the content and properties of clay minerals in sedimentary rocks. The method is relatively simple and has the advantage that it may be used with small, irregularly shaped chips or shale-streaked samples, as well as with typical core samples. Methods previously employed required separating the clay from the rest of the reservoir-sample material and then performing a clay analysis either by X-ray diffraction, differential thermal analysis, liquid permeability, or a combination of these methods (2,3) .3/ This water-vapor-adsorption method requires measuring only a few points on the isotherm to tell whether or not the sample is water sensitive. The goal of these measurements is not to determine the type or amount of clay present, but what will be its sensitivity to flood water. This method gives a direct means of solving this problem.

Jan 1, 1958

By Charles B. Kenahan

The chemical and galvanic corrosion properties of commercially pure titanium, a titanium-manganese alloy, a titanium-aluminum-tin alloy, 2 titanium-copper alloys, and 2 titanium-aluminum alloys were studied. Tests were conducted in synthetic ocean water, tapwater, 1-percent sodium hydroxide, 5-percent ferric chloride, and 5-percent ammonium sulfate solutions, various concentrations of sulfuric and hydro-chloric acids, and 1-percent oxalic acid. All tests were carried out at 35° or 60° C., with a flow of air or helium. Dissimilar metals involved in galvanic-couples experiments were aluminum, magnesium, and stainless steel. Electrode-potential measurements on single (uncoupled) specimens were also measured. Commercially pure titanium and the titanium-base alloys were generally quite similar in their resistance to corrosion, whether alone or in. contact with a dissimilar metal. Contact with the titanium metals caused aluminum and magnesium to corrode by galvanic action. Coupling with stainless steel in sulfuric acid solutions decreased the normal corrosion rate of the titanium metals. Contact with aluminum in air-aerated oxalic acid and 0.1N sulfuric acid solutions resulted in cathodic corrosion of titanium and the titanium-base alloys; however, there were a few exceptions. The copper alloys showed better corrosion characteristics than titanium in certain sulfuric acid solutions but were more susceptible to chemical attack in some hydrochloric acid solutions.

Jan 1, 1958

By W. T. Wertman

A research program to aid development of better and more efficient methods for producing petroleum and increasing its ultimate recovery from underground formations is an integral part of the work of the Bureau of Mines on conservation of the Nation's natural resources. Economic, efficient production of recoverable oil and gas from a reservoir depends to a great extent upon the best and most accurate information that can be obtained from a study of the reservoir rock and its fluid contents. Information on oil and water saturation is pertinent and essential in wildcat, extension, and pool wells for good reservoir operations and prediction of performance. This report presents results of an investigation by the Bureau of Mines of core recovery and degree of drilling-fluid contamination occurring during cable-tool coring operations using oil-base mud. Representative core samples were obtained from 6 major oil-producing sands in 8 fields of West Virginia, Pennsylvania, and New York. Field-mixed, oil-base drilling mud was used for the first coring test, and lightweight, premixed oil-base mud, with an organic chloride tracer added, was used in coring eight other wells. Tracer analyses were made to determine contamination of core by drilling-fluid filtrate. Core analyses, including oil and water content and minimum interstitial water-saturation tests, were made on selected core samples to compare and evaluate water saturations determined by the two methods.

Jan 1, 1958

By Frank C. Morris

This report presents the results of a Bureau of Mines study to identify clays found in several petroleum-reservoir rocks in the Tejon-Grapevine area, Kern County, Calif., and to determine the effect of water sensitivity of the clays on the permeability of the reservoir rocks. The clays in the porous rocks were examined in detail, and the clay-mineral types were identified by differential thermal analysis, X-ray diffraction, and optical and dye-staining methods. Fresh-water damage to the permeability of the oil-reservoir rocks was indicated by a study of 125 core samples from productive formations. The study indicated that, although clays were generally less than 5 percent of the reservoir rocks, they swelled in water, particularly fresh water, and nearly blocked the flow channels through which oil flows to the well, effectively reducing the permeability of the formations. The average permeability of rock decreased from 1,600 millidarcys in air to 620 millidarcys in salt water and 120 millidarcys in fresh water. The dominant clays in the oil-bearing sandstones were members of the montmorillonite group. They were associated with smaller quantities of clays found to be in the mica or illite group. None of the cores appeared to contain clays of the kaolinite group. In the lower section of the J.V. sandstone indications of what appeared to be the mineral sepiolite were noted.

Jan 1, 1959

By L. C. Brichta

During a study of the Badger-Peacock area from October 1950 to June 1953, the Federal Geological Survey and the Federal Bureau of Mines completed nearly 98 miles of resistivity profiling and drilled 96 test holes aggregating 17,628 feet of bore, In addition, seismic profile measurements were made along 8 traverse lines for an aggregate length of about 16,600 feet. The geophysical surveys were conducted by the Geophysics Branch of the Geological Survey; the drilling was done by the Bureau of Mines. Electrical-resistivity measurements disclosed 21 low-resistivity anomalies and 1 high-resistivity anomaly. Correlation of the resistivity data with the geological information revealed by the drilling disclosed that the low-resistivity anomalies indicated either slumped shale deposits in limestone sinks or undisturbed deposits of shale lying in erosional depressions in the limestone. The high-resistivity anomaly indicated hard, undisturbed limestone at or near the surface.

Jan 1, 1958

By H. Kenworthy

The objective of this investigation was to evaluate the technical feasibility of smelting certain low-grade domestic iron ores in an electric furnace. Laboratory-scale experiments showed that a high recovery of iron in the form of pig iron can be obtained from east Texas ores containing less than 25 percent iron. The pig iron was amenable to standard-or electric-furnace-refining methods for producing steel. Car-bon, silicon, and phosphorus were the primary impurities removed in refining. Overall recoveries of iron as pig iron exceeded 95 percent, in contrast with commercial mineral-dressing recoveries on these particular ores of 50 percent of the iron as a 45-to 50-percent iron concentrate.

Jan 1, 1958

By E. C. Perkins

This report describes a ferric chloride trap, based on formation of a low-melting sodium chloride-ferric chloride mixture of near-eutectic composition, and its use in chlorination of impure titaniferous materials. The trap is placed in the hot gas stream between the chlorination reactor and the condenser. Virtually all of the iron is removed by the trap. The condensed titanium tetrachloride is free of suspended solids and contains only a trace of iron. Four examples are given of the use of the ferric chloride trap in chlorination of impure titaniferous materials. INTRODUCTION In the Kroll process, ductile titanium metal is produced by reducing titanium tetrachloride with magnesium metal.4/ In commercial practice, titanium tetrachloride is produced by chlorinating titaniferous materials in the presence of carbon.2/ In 1957 most producers were using rutile, and virtually all plants were designed for its use. About four-fifths of the domestic consumption of rutile was imported from Australia. The Bureau of Mines, under provisions of contract DMP-116 with the General Services Administration, studied electrosmelting of domestic ilmenites and titaniferous magnetites to produce high-titanium slags with pig iron as a byproduct. Under the same contract, chlorination studies also were being made of these slags. Smelting was done at the Northwest Electrodevelopment Experiment Station, Albany, Oreg., and chlorination at the Electrometallurgical Experiment Station, Boulder City, Nev.

Jan 1, 1958

By Leonard Obert

The various underground rooms in the Bureau of Mines Oil-Shale mine, Rifle, Colo., have been open for periods ranging from 3 to 5 years. During this time 3 roof falls have occurred; 1 was induced, and the other 2 were unintentional. The three roof falls are described in this report. Two causative factors are discussed -a time-dependent deterioration of the roof rock and an unfavorable system of jointing that occurred in the strata overlying the present roof horizon. Irrespective of cause, the operating life of any stoping area would have been short com-pared with the life of the roof (1 to 4 in the most unfavorable instance), if a high-production system of mining had been employed. The report is concluded with several recommendations that should be considered in planning future mining operations.

Jan 1, 1958

By R. P. Maloney

The Bureau of Mines conducted a reconnaissance of the less accessible parts of the Beluga River coalfield in August 1957 to determine, if possible, which areas were most favorable for developing large reserves of coal suitable for open-pit mining. Several outcrops of subbituminous coal were observed within an area about 30 miles long and 3 miles wide; neither the length nor the width of the coal-bearing area was delineated by the examination. Coal beds 30 feet thick or more outcrop at two places, and beds 5 to 20 feet thick or more outcrop fairly abundantly along the Beluga River and its tributaries The coal measures appear to occur in a series of folds. The overburden comprises glacial gravels and poorly cemented sandstones and ranges from 20 to 400 feet in depth. Few partings were seen in any of the coal beds. Samples ranged in calorific value from 6,240 to 8,246 B. t. u. on an as-received basis. Adequate water is available for stripping by hydraulic methods.

Jan 1, 1958

By M. M. Barr

Rapid expansion of the titanium-metal industry focused attention upon ilmenite as a possible substitute for the more expensive and less abundant rutile in producing titanium tetrachloride. Most of the rutile available for this use is imported. Preliminary studies were undertaken to determine the chlorination characteristics of high-titanium slags produced by electric-arc furnace smelting of alluvial Idaho ilmenite at the Federal Bureau of Mines Northwest Electrodevelopment Experiment Station, Albany, Oreg. Low silicon, calcium, and aluminum contents of the slags enhanced their potential value for chlorination.

Jan 1, 1958

By G. W. Birge

This report describes the carbonizing properties of the principal coal beds of McDowell County, W. Va. Coals from 14 coal beds were selected for study: Upper Cedar Grove, Middle Cedar Grove, Lower Cedar Grove, Eagle, Douglas, Iaeger, Sewell, Welch, Beckley, Fire Creek and Pocahontas Nos. 3, 4, 5, and 9. Selection was based upon estimated minable reserves. McDowell County coals rank either as high-volatile A, medium-volatile, or low-volatile bituminous coal, and this variation in rank is reflected in the wide diversity of the carbonization properties of the coals. All coals tested were either satisfactory as mined or could be upgraded to meet present chemical standards for metallurgical coke; the coals produced strong coke, as determined by ASTM shatter and tumbler tests.

Jan 1, 1958

By R. R. Wells

This report summarizes the results of laboratory investigations by the Alaska Mining Experiment Station, Juneau, to determine the practicability of treating cinnabar-stibnite ore by bulk flotation and controlled-atmosphere roasting of the concentrate. Ore from the Red Devil mine near Sleetmute, Alaska, was selected for testing; it is typical of ores widely distributed throughout the Kuskokwim River Basin. The material, consisting of stibnite and cinnabar in ankerite, dolomite, and quartz, assayed 1.55 percent Hg and 2.87 percent Sb. Continuous treatment of the ore in a laboratory flotation circuit recovered 95.7 percent of the mercury and 82.6 percent of the antimony in a concentrate that assayed 20.4 percent Hg and 34.6 percent Sb.

Jan 1, 1958

By T. E. Gray

This report describes the preparation characteristics of the three significant coal beds in Greene County, Pa. It is one of a series planned to determine which coals are suitable for the production of metallurgical coke, either as mined or after beneficiation. Over 12.5 million tons of coal was produced in Greene County in 1956, of which approximately 10 million tons was cleaned mechanically in 8 cleaning plants. The Bureau of Mines has estimated that 3.5 billion tons of recoverable coal remained in the county as of January 1, 1954.

Jan 1, 1958

By W. H. Ode

In 1949 the Coal Committee of the Economic Commission for Europe, Geneva, Switzerland, established a Classification Working Party, to develop an international system for classifying coal. This project was necessitated by the increased trade in coal among various nations following World War II. Although national classification systems existed, they had been developed to cover the characteristics of domestic coals without reference to coals of other countries. Different terms for describing similar or identical coals in each nation caused confusion in evaluating coals shipped in international trade. Experts from Austria, Belgium, Bulgaria, Czechoslovakia, Denmark, the Federal Republic of Germany, France, Greece, Hungary, Italy, the Netherlands, Poland, Sweden, the Union of Soviet Socialist Republics, East Germany, the United Kingdom, the United States of America, and Yugoslavia participated in various stages of the classification work. Walter A. Selvig was appointed by the Bureau of Mines as the technical expert to represent the United States because of his experience in developing and standardizing methods of analyzing and classifying American coals. He served on the Classification Working Party until his retirement from the Bureau of Mines early in 1956. Extensive laboratory work was done in connection with the classification studies at the Pittsburgh Experiment Station of the Bureau of Mines.

Jan 1, 1958

By K. K. Kelley

Synthetic fluorphlogopite mica (KMg3AlSi3010F2) is a relatively new product developed at the Norris (Tenn.) Station of the Bureau of Mines, Thermodynamic data have applications both in the production and use of this product, and the work described in this paper was undertaken to fill the need for such data. Measurements were made of the heat of formation at 298° K., the heat capacity between 50° and 298° K., the entropy at 298° K., and the heat-content and entropy increments between 298° K. and a maximum of 1,804° K. These basic data are combined to obtain heats and free energies of formation of the mica from the elements and from molecular constituents at temperatures ranging from 298° to 1,800° K. Minimum heat requirements to form melted mica from commonly used ingredients were calculated.

Jan 1, 1959