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By M. R. Geer

The cleaning of fine coal, particularly for metallurgical use, is receiving greater attention. An increase in the proportion of fine coal in the run-of-mine product has been created by changes in mining practice, and a concur-rent deterioration in the quality of the fines has occurred because of more widespread full-seam mining. These two factors, augmented by the depletion of premium beds of metallurgical coal in some areas and the resulting shift to "dirtier" beds, are providing the impetus for adoption of improved cleaning techniques. For example, froth flotation, which has been used for years in a few preparation plants, now is gaining more rapidly in acceptance. Similarly, the dense-medium cyclone, which is used widely in Europe for making difficult separations, recently has been introduced to the United States. Regardless of the cleaning process employed, the finer sizes of coal can be treated with maximum effectiveness only when they are removed from the run-of-mine product and treated separately. No present process can treat the full range of sizes together with complete effectiveness. Flotation is applicable only to the coal finer than a top size ranging between 14-and 48-mesh, and cyclones require removal of all material finer than 0.5 to 0.3 mm. from the feed. Thus, the trend toward more-effective cleaning of the fine coal imposes the attendant problem of fine screening. Whereas in the past there was little need to screen finer than about l/4-in., present developments indicate that fine screening will become increasingly prevalent.

Jan 1, 1960

By J. D. Ramsdell

The purpose of this investigation was to determine the effects of the impurities, oxygen, nitrogen, carbon, and iron (in low percentages) on the mechanical properties of electrolytic titanium. The strength and hardness of binary Ti-O, Ti-N, and Ti-C alloys are linear functions of alloy content in the composition range investigated. Compared to oxygen and carbon, nitro-gen is the most effective strengthener and hardener, followed by oxygen, then carbon. When the carbon concentration is above 0.10 percent, carbides are present, and strength and hardness are relatively unchanged. For equivalent hardness levels, Ti-Fe alloys are stronger than binary titanium alloys containing oxygen, nitrogen, or carbon. However, the strengthening is related to the presence of transformed beta in the structure.

Jan 1, 1960

By P. C. Good

To meet a growing need for thorium metal of high purity and amenability to fabrication, the Bureau of Mines devised a method for preparing thorium metal by the reduction of thorium tetrachloride. Thorium tetrachloride was prepared by chlorinating calcined thorium oxalate with carbon tetrachloride. The crude thorium tetrachloride, containing oxygen-bearing compounds, was purified by a double vacuum distillation at 800 to 900° C., and thorium metal was made in the form of a dense sponge by the reaction of metallic sodium or magnesium with thorium tetrachloride at 800° C. Vacuum arc melting was used to consolidate the sponge metal to ingot form for evaluation of its physical and chemical properties.

Jan 1, 1960

By James M. Stuckey

In a search for improved methods of upgrading tar obtained by low-temperature carbonization of coal, monoethanolamine (MEA) was found to be effective in extracting tar acids from coal tar distillates derived from a subbitunwous and a lignite coal. Patch extractions showed that both yield and purity of the extracted acids improved with increasing volume ratios of monoethanolamine to tar acid, varied from 1:4 to 8:1. Yield improved, but purity decreased as the concentration of monoethanolamine was changed from 30 to 70 volume-percent, and as the concentration of tar acid in distillate was increased ad from 14 to 45 percent. In a continuous countercurrent extraction employing a double solvent (monoethanolamine and hexane) approximately 80 percent of the tar acids was extracted from 170° to 350° C. tar distillate when using 1.6:1 volume ratios of amine:tar acids. Tar acids isolated from his extract, although of improved purity, contained appreciable quantities of neutral oils and some tar bases. Aqueous monoethanolamine was not effective for extracting the last 10 to 15 percent of tar acids in 170° to 350° C. distillate oil from lignite coal. The highest yield of isolated tar acids and the best recovery of monoethanolamine were obtained by diluting the extract with water and saturating with C02. Some losses of solvent were encountered when aqueous monoethanolamine solutions were heated through decomposition of the amine with the liberation of ammonia.

Jan 1, 1960

By George L. Gates

This report presents is an evaluation by the Federal Bureau of Mines of the effect of clay-water, brine, and oil-base drilling fluids on the productivity of test wells drilled on the Umiat anticline in U.S. Naval Petroleum Reserve No. 4 in northern Alaska. Eleven, wells were drilled on the Umiat structure as part of the U.S. Navy's extensive exploration of the Reserve during 1944-53 to determine the possibilities for oil production. The Federal Geological Survey cooperated in the exploration program and has published a comprehensive report3/ on the geology of the area and case histories of the wells. The re¬port also includes the results of special studies by the Bureau in connection with the drilling and coring of well 9 with oil-base mud in hole and was the source of much of the information used in preparing this publication. Of the eleven wells, four were drilled with rotary tools and water-base mud (one of the water-base muds was an oil-in-water emulsion mud), five were drilled with cable tools with brine in the hole, one was drilled with cable tools with brine in the hole and later reamed with rotary tools and crude oil, and one was drilled with rotary tools and oil-base mud. Although all of the wells penetrated sandstones that contained oil and gas, some were productive and others were not. The latter two wells, one completed with crude oil in the hole (with some added brine) and the other with oil-base mud, had the greatest productive capacities. The wells drilled with cable tools and brine in the hole had lower productive capacities. In contrast, two of three wells completed with rotary methods and fresh-water drilling mud and the well com¬pleted with rotary and emulsion mud were unproductive.

Jan 1, 1960

By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By A. D. Hahn

The Federal Bureau of Mines examined ilmenite-bearing sands in southern Texas as part of a program to discover sources of supply for the domestic titanium industry. Deposits were examined from May 1956 through January 1959 in the outcrops of sandstone beds in the Jackson group of Eocene formations in Lee, Burleson, Fayette, and Starr Counties on the Gulf Coastal Plain; in alluvial valley fill in Brewster County in southwest Texas; in the sand beaches of Matagorda Peninsula and the Galveston, Padre, and Brazos Islands--part of the offshore chain of barrier islands along the Texas coast; and in unconsolidated sediments in Willacy County on the Rio Grande delta in the southeast Texas.

Jan 1, 1961

By John P. Powell

A comprehensive study of the effects of hydraulically fracturing water-flood wells in Oklahoma has been made by the Federal Bureau of Mines. This report presents results of that study and an analysis of some of the factors governing the results of fracture treatment on waterflood properties. Originally, hydraulic fracturing was used to stimulate oil production from old wells producing by primary methods, and its application to water-flooding was regarded with skepticism by most producers. However, since 1953 the number of fracture treatments of both oil and input wells in waterfloods has increased steadily. Hydraulic-fracture treatments in waterfloods have generally been successful in stimulating production from oil wells and increasing the rate of injection into input wells. Hydraulic fracturing has enabled several producers to turn probable failures into economically successful projects.

Jan 1, 1961

By W. R. Huff

This report describes the development and operation by the Bureau of Mines of a pilot plant designed for using high-volatile A bituminous coal-in-water suspensions as a source of preheated coal and superheated steam in the pressure gasification of coal with oxygen. Figure 1 on page 2 is a block diagram of the integrated gasification process, in which a total of 70 tons of coal was fed from slurry and gasified. The present work included (1) development of equipment and methods both for mixing pulverized coal and water to produce slurry and for pumping and metering the slurry at gasification pressure; (2) development of equipment for heating the flowing slurry and, because slurry that can be pumped produces more steam than is necessary as a gasification reactant, developing equipment for removing and metering the excess steam; and (3) demonstration of the process under actual gasifier operating conditions, at a coal rate of about 800 pounds per hour and gasification pressures in the range 100 to 300 pounds per square inch gage. By using the forced-convection principle, a flow of slurry made from a caking, high-volatile A bituminous coal can be continuously heated to 600° F. in a coil-type heater. The flow rate and concentration of the slurry and the temperature gradient along the length of the heating coil must be closely controlled. In a radiant-type heater, involuntary reductions in flow rate, even momentary, can lead to coking and plugging of the heater coil.

Jan 1, 1961

By F. E. Block

The metallic reduction of vanadium chlorides was investigated by the Federal Bureau of Mines as a possible new route for preparing vanadium metal in an effort to develop a production process that would be adaptable to large-scale plant production and would yield metal of uniformly high quality. Vanadium tetrachloride was usually prepared by chlorinating vanadium pentoxide in the presence of carbon. Although oxygen-?free tetrachloride was difficult to prepare this way, it could be prepared by the direct chlorination of vanadium carbide. Lower valent vanadium trichloride was prepared by the thermal decomposition of vanadium tetrachloride. Vanadium dichloride was also prepared by the thermal disproportionation of vanadium trichloride.

Jan 1, 1961

By W. J. Wenger

Oil fields in the Powder River Basin of Wyoming have produced 731 million barrels of petroleum through 1959. Production in 1959 was 32 million barrels, the highest production since 1924. The record production was in 1923, when the Basin produced 38 million barrels of oil and the Salt Creek field, then at its peak, produced 35 million barrels. In this report, the characteristics of crude oils found in the Basin are used as a basis for determining the best re-fining uses for the oils and for predicting the characteristics of oils that may be discovered in the Basin in the future. Analyses of 108 oils sampled over a period of 30 years are presented Crude oils of two major types are produced from the Powder River Basin. One has a low sulfur content and occurs in younger formations, and the other has a high sulfur content and occurs in older formations. The oils with low sulfur contents are generally light colored and waxy, and may be either paraffinic or naphthenic. The oils with high sulfur contents are usually dark colored and asphaltic; only their low boiling fractions are paraffinic. Alteration appears to account for the anomalous properties of some oils found at shallow depths. Shapes and slopes of correlation index curves classify the oils into the same two groups as their sulfur contents, with gently sloping curves representing the low-sulfur oils and steep curves representing high-sulfur, asphaltic oils,

Jan 1, 1961

By P. G. Clites

A laboratory furnace was developed by the Federal Bureau of Mines for use in studying the interrelationships among variables associated with skull melting and casting high-temperature metals. Although additional work is necessary to determine the extent to which the information obtained by using this furnace can be extrapolated to larger furnaces of the same type, many casting characteristics of metals and alloys can be determined on equipment of this size. This furnace is a laboratory-size, consumable-electrode, skull-casting furnace equipped with a water-cooled copper ladle. The ladle, which is a tilt-pour or over-the-lip type, has a volume of approximately 30 cubic inches and provides up to 20 cubic inches of molten metal for castings. Castings of various reactive and refractory metals, including zirconium, titanium, hafnium, columbium, molybdenum, tantalum, and tungsten, have been produced. In addition, castings of iron, chromium, and copper have been made. The simplicity and versatility of the apparatus would make it useful to metallurgical laboratories preparing cast specimens.

Jan 1, 1961

By R. J. Gajan

As part of its research program on secondary metal refining, the Federal Bureau of Mines has developed a fast method for determining aluminum, iron, copper, cadmium, and lead in zinc-base alloys. The new method is intended for use by trained technicians in laboratories with inexpensive equipment. It can be used either in the analytical laboratories of the many small plants that are characteristic of the secondary metals industry or in laboratories engaged in basic research to improve refining processes. A complete analysis for the foregoing elements can be made in less than 3 hours from a single sample in solution. The method is especially helpful when a small amount of sample is available. Aluminum and iron are determined spectrophotometrically and the other elements polarographically. The new method is now being used for control analysis in metallurgical research, and the results compare favorably with previously used spectrographic methods. Luke and Braun4/ described a photometric method for the determination of aluminum in zinc diecasting alloys in which the aluminum was complexed with Aluminon reagent (ammonium salt of aurintricarboxylic acid), forming a red lake. An adaptation of this method was used for determining aluminum. Beers law is obeyed between 0.01 and 0.06 milligram of aluminum.

Jan 1, 1961

By G. V. Sullivan

This report summarizes the results of metallurgical investigations by the Federal Bureau of Mines of manganese oxide ore, averaging 23 to 25 percent manganese, stockpiled at the Butte-Philipsburg depot of General Services Administration (GSA). The oxide ores were stockpiled in two general classifications, straight oxide ore and mixed oxide-carbonate ore. Continuous-circuit flotation tests at the Albany (Oreg.) Metallurgy Research Center of the Bureau of Mines showed that each of these ore types could be concentrated by an oil-emulsion scheme to produce a concentrate that could be sintered to meet program specifications. About 88 percent of the manganese was recovered in the concentrate from the straight oxide sample, with the sintered concentrate containing 48 percent Mn. The sintered concentrate from the mixed oxide-carbonate sample contained 41 percent Mn with a recovery in the concentrate of 95 percent.

Jan 1, 1961

By James S. Browning

The purpose of this investigation was to develop a dependable and economic method for recovering spodumene and mica from pegmatites of the type found in Gaston County, N. C. Laboratory batch tests and continuous flotation tests were made by the Federal Bureau of Mines to determine the feasibility of treating the ore by flotation to recover high-grade spodumene and mica concentrates. The spodumene flotation circuit yielded concentrates containing 6.50 percent lithia (Li20), with an overall recovery of 81.8 percent of the lithia in the ore, The mica circuit yielded concentrates containing 97.5 percent mica, with a recovery of 82.5 percent of the mica in the spodumene tailing.

Jan 1, 1961

By M. R. Geer

The use of the cyclone as a dense-medium cleaning device was first described by Driessen6/ in 1945, after development of the process in the Netherlands during the German occupation of World War II. A pilot plant was built in the Netherlands soon thereafter, and the first commercial plant was built in 1948. By 1958, 18 plants were operating or under construction.7/ Thus, economic factors in Europe, where the high cost of coal places a premium on efficient cleaning, dictated rapid adoption of the cyclone. American reception of the process differed. The Bureau of Mines presented the results of its own small-scale cyclone experiments in 1946;8/ showing a sharp separation between coal and impurity; adoption by industry now is taking place. There is now much greater emphasis on the efficient cleaning of fine coal, and the first American cyclone plant has begun operating; others are planned or under construction. With the present interest in improved treatment of fine coal, the Bureau of Mines felt that additional performance data on the cyclone would be helpful to industry. Therefore, a complete, open-circuit pilot plant was built to make cleaning trials on American coals covering a wide range of washability characteristics. Five raw coals and one middling product were included in the investigation, and each was cleaned at several densities; 17 cleaning trials are reported.

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

By D. Bienstock

In connection with air-pollution studies, the Bureau of Mines is cooperating with the U.S. Public Health Service in investigating the use of solids for removing sulfur dioxide in concentrations of less than 0.5 percent from combustion and waste gases. Removal of sulfur dioxide at flue-gas tempera¬tures would no longer result in the cooling of scrubbed gas, which is inherent to liquid scrubbing processes used exclusively in industry today. Results are reported of extensive investigation, using metallic oxides as absorbents, adsorbents, and oxidation catalysts at 130° and 330° C. (temperatures at which flue gas may be treated in powerplant practice). The most active absorbents tested were the oxides of manganese, cobalt, copper, and alkalized alumina; 23 to 33 grams of sulfur dioxidn were removed by 100 grams of absorbent at 130° C., while scrubbing more than 90 percent of the sulfur dioxide from a simulated flue gas, and 19 to 61 grams of sulfur dioxide were removed at 330° C. A more detailed study is reported on absorption and regeneration, using manganese oxides and alkalized alumina. Adsorption of sulfur dioxide on activated carbons and molecular sieves at elevated temperatures is considerably less efficient than removal by absorption--a maximum of 7 to 8 grams of sulfur dioxide could be removed with 100 grams of adsorbent at 130° C. A potash-promoted vanadium pentoxide is effective in converting sulfur dioxide to trioxide; complete conversion in a simulated flue gas containing 0.35 percent sulfur dioxide was obtained at 365° C. Pilot-plant and cost studies are being made by the Bureau to determine the economic feasibility of removing on an industrial scale the sulfur dioxide present in gases in low concentrations.

Jan 1, 1961

By David M. Gullikson

As part of its program of petroleum production research the Federal Bureau of Mines has long been engaged in the study and development of systems of analysis of oilfield waters (8, 12, 20, 21, 22, 27, 30).21 However, many of the early chemical procedures developed by the Bureau and widely adopted by the petroleum industry are time consuming, and some are unreliable for determining certain constituents found in California oilfield waters. Because of the need for more rapid and more accurate methods having greater sensitivity with low concentrations of some constituents, a study has been made by the Bureau's Petroleum Research Laboratory at San Francisco, in developing new techniques and modifying previously published techniques for analyzing oilfield waters by flame spectrophotometric, potentiometric, and colorimetric methods. Test solutions were synthesized for testing the suitability and accuracy of the procedures, and the effect of interfering ions. These solutions contained known quantities of characteristic constituents of oilfield waters including sodium, magnesium, potassium, calcium, lithium, strontium, barium, sulfate, chloride, bromide, iodide, carbonate, bicarbonate and borates in a wide range of concentrations. The compositions of these synthetic brines are listed in table 22. Many California oilfield waters contain salts of petroleum-derived organic acids and several synthetic oilfield waters also were prepared to which large quantities of naphthenates or salts of petroleum acids were added.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961