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By David J. Kusler

This report describes a rapid, reliable, and relatively simple method developed by the Bureau of Mines Pyrometallurgy Laboratory at Bruceton, Pa., for determining lime (calcium oxide) and magnesia (magnesium oxide) in various materials containing these constituents in greater than trace amounts. Optionally, titania (titanium dioxide) may be determined for the same sample. The accuracy of the method, suitable for most purposes, is shown by comparing the Bureau results with those obtained by accepted procedures. The method has been applied satisfactorily to the routine analysis of blast-furnace slags, for which purpose it was primarily developed, and to other calcareous compositions. In the Pyrometallurgy Laboratory it has replaced the standard methods previously used to determine lime and magnesia, and has been in general use by that laboratory for the past several years. The analysis time, generally under 3 hours, is considerably less than required by standard methods.

Jan 1, 1960

By J. E. Wilson

A bench-scale expansion tester using 71 grams of coal was developed to determine the practicability of an apparatus of this size to investigate the effect of variables such as oxidation, blending, bulk density, inerts, size consist, petrographic differences, and rate of heating on the expanding properties of coal. The value of this tester is shown by the correlation that exists between its results and those of the larger scale sole-heated oven expansion apparatus used in commercial plants. From tests on 32 coals the standard error of estimate for predicting sole-oven results from bench-scale results is ± 5.3 percentage points. A standard deviation of the difference between pairs of tests in the latter apparatus of ± 2.1 percentage points was determined for 31 samples. In the sole-heated oven test the expansion of a coal at constant pressure is directly proportional to the dry coal bulk density. Tests in the bench-scale tester show a similar relationship between expansion and bulk density. When the blending ratios of high-and low-volatile coals are varied, similar changes in expansion are observed in both the sole-heated oven and the bench-scale tester. Therefore, the effect of other variables on expansion should be similar in the latter apparatus.

Jan 1, 1960

By Byron E. Blair

This report describes procedures for using a high-speed camera to study blasting phenomena. Both quantitative and qualitative information can be obtained, provided that proper interpretations of the projected two-dimensional images are made. Geometrical relationships between object and image displacements are given in terms of horizontal and vertical angles of the camera optic axis with respect to the quarry face. Correction factors are given for obtaining true object displacements from image displacements in the camera film plane. The time of initial rock movement also is considered, and the control-ling factors of camera speed, scale factor, minimum increment of projection measurement, etc., are evaluated in terms of minimum time intervals. The high-speed camera and associated equipment are described, and field measurements and laboratory data analysis techniques are outlined. An analysis of a typical high-speed motion picture is made, and the application of the necessary correction factors is illustrated.

Jan 1, 1960

By J. B. Gayle

The removal of coal particles from a slurry by flotation is made possible by the formation of stable aggregates with air bubbles of suitable sizes. The formation of such aggregates is theoretically possible only for certain favorable combinations of the solid-liquid-gas interfacial tensions. Because interfacial tensions involving solid phases are not conveniently measurable, a related variable, the contact angle, frequently is used as a measure of the floatability of various materials. Zero angles indicate nonfloatable substances, and large angles indicate substances having a high degree of floatability. During a study of contact angles for coal and substances related to coal in their similarity of response to various physical and chemical treatments, particularly flotation, carbonization, and oxidation, the reproducibility of replicate determinations taken within a 4-hour period was found to be much better than that for comparable results taken over a longer period of time. Consideration of possible causes for these differences led to an investigation of the effects of temperature variations on contact angles. References to literature revealed only a small amount of information, some of it apparently conflicting. Specifically, Sutherland and Wark4/ found that temperature variations "within limits" did not appreciably influence the angles measured for galena conditioned with potassium ethyl xanthate. On the other hand, McGlashan and McLeod5/ presented preliminary data showing that for sphalerite conditioned with potassium ethyl xanthate the angle is maximum at 25° to 35° C., depending on the pH of the system.

Jan 1, 1960

By J. D. Ramsdell

The study described in this report was undertaken to obtain information on the character and effect of antimony additions to titanium. The availability of high-purity, low-hardness titanium metal, resulting from fused-salt electrorefining techniques, permitted a reassessment and evaluation of the physical behavior of titanium-antimony alloys. Alloys, based on several grades of titanium containing up to 10 percent antimony, were arc-melted and processed to sheet by hot and cold rolling. Properties and characteristics were evaluated by hardness tests, hot and cold rollability, annealing treatments, metallographic examination, and tensile tests.

Jan 1, 1960

By W. J. Wenger

THIRTY-FOUR analyses of crude oils from the fields of the Four Corners Area of Arizona, Colorado, New Mexico, and Utah are presented and compared. The samples, taken from formations in four geological time periods, have high gravity and low-sulfur, -nitrogen, and -asphalt content. Generally, the oils are paraffinic in the low-boiling fractions, with increasing naphthenicity in the higher-boiling fractions. Oils from Cretaceous formations resemble other Cretaceous oils in the Rocky Mountains, but oils from Permian and Pennsylvania formations are unlike other oils of these ages in the Rooky Mountains. The differences in the oils are minor and cannot be used to distinguish between fields or between producing formations. With minimum special processing, the oils should yield large amounts of good-quality motor fuels. INTRODUCTION The only place in the United States where four States have a common junction is known as the Four Corners Area. This area (fig. 1) includes the northeast corner of Arizona, the southwest corner of Colorado, the northwest corner of New Mexico, and the southeast corner of Utah. It includes three major geological basins: The Black Mesa, the San Juan, and the Paradox. Major oil developments have occurred in both the San Juan and Paradox basins, but no discovery of commercial importance has been made in the Black Mesa basin.

Jan 1, 1960

By F. E. Block

This investigation was made as part of a larger program to develop basically new methods for preparing yttrium metal in high-purity form. It was performed under a cooperative agreement between the U.S. Atomic Energy Commission (AEC) and the Federal Bureau of Mines. Laboratory-scale tests were made to devise methods for preparing high-purity, anhydrous yttrium trichloride, for reducing the yttrium trichloride with sodium or lithium, and for consolidating the resulting yttrium sponge into ingots.

Jan 1, 1960

By P. C. Good

High-purity chromium was prepared in massive form by the electrolysis of chromium trioxide solution at high temperatures. The metal thus obtained, containing 50 to 150 p.p.m. of oxygen, 20 p.p.m. of nitrogen, and traces of metallic impurities, could be hot-worked to rod and sheet and drawn to wire ductile at room temperatures. Optimum concentrations and operating conditions were established for the deposition of chromium from chromic acid baths containing sulfate, fluoride, and silicofluoride ions. Current efficiencies of 13 percent were attained with baths containing sulfate ion, and efficiencies of 40 to 44 percent with baths containing fluoride and silicofluoride ions. Cation exchange resins were used for removing metallic impurities from chromic acid solutions containing sulfate ion; solutions containing fluoride and silicofluoride ions were purified by recrystallization.

Jan 1, 1960

By E. G. King

Strontium sulfide and barium sulfide occur as intermediates in commercial treatments of the impure natural sulfates to produce pure strontium and barium chemicals. Thermodynamic considerations involving these sulfides have been hampered by lack of basic data, such as the entropies at 298.15°K. This paper reports the results of heat capacity measurements of strontium sulfide and barium sulfide in the temperature range 50°-298°K. The entropies at 298.15°K. were derived from the heat capacity values. Free energies of formation at 298.15°k. were computed from the entropies and literature values of the heats of formation. Strontium sulfide and barium sulfide are thermo-dynamically less stable than calcium sulfide, but more stable than magnesium sulfide.

Jan 1, 1960

By J. D. Ramsdell

To obtain information on the effects of cobalt on microstructure and tensile properties of titanium-vanadium-cobalt alloys, the composition ranges of 4 to 16 percent vanadium with 1 to 4 percent cobalt have been studied. The beta phase was not completely retained with vanadium additions up to 16 weight-percent or in the same alloys containing up to 4 percent cobalt.

Jan 1, 1960

By J. B. Gayle

Oven widths for experimental and commercial slot-type ovens differ appreably in most instances; the experimental ovens usually ranging from 10 to 14 inches and the commercial units from 14 to 21 inches. Application of results obtained with experimental ovens to commercial practice thus requires major extrapolations. A critical survey of the literature indicated that sufficient information about the effects of variations in oven width on the carbonizing process is not available to permit such extrapolations to be made with any considerable degree of confidence.

Jan 1, 1960

By I. Iwasaki

In recent years the rapid depletion of high-grade iron ores and the demand by blast furnace operators for increasingly low-silica ores have stimulated interest in flotation studies of low-grade iron ores, such as wash-ore tailings and oxidized taconites. Four processes have been reported for the flotation separation of these iron ores--anionic and cationic collection of the iron oxides, cationic collection of siliceous gangue, and anionic collection of activated siliceous gangue (5).5/ The effectiveness of any one method, however, depends largely on the mineralogical composition and on the physical structure of the sample; hence, a comprehensive study of the floatability of the individual minerals occurring in these materials is essential. A review of the literature shows that the floatability of hematite and magnetite has been frequently investigated, whereas very little corresponding information is available for goethite, or for its more earthy form, limonite, both of which are abundant in the Mesabi and Cuyuna ores (19). The purpose of this investigation was to formulate general information on the floatability of goethite. Vacuum flotation, contact angle measurement, and simplified flotation tests using a modified Hallimond tube were used. The experimental results were correlated with the electrokinetic properties of goethite as determined by streaming potential measurement. The results were used to interpret the batch flotation tests made on an artificial mixture of quartz and goethite.

Jan 1, 1960

By J. W. Eckerd

This report describes an investigation of the technical feasibility of using a conventional commercial-size (10-ft. i.d.), rotating grate, dry-ash-removal type gas producer to make producer gas from chestnut-size bone anthracite. Test instruments were installed, and some minor changes were made in the equipment to handle the large quantities of materials expected. Extensive tests, lasting about 4 weeks, were planned, using 35 to 50 percent ash chestnut anthracite bone. However, operations were suspended after 8 days when it became apparent that to use this type of fuel satisfactorily substantial changes in equipment and operating procedures would be required. Nevertheless, enough data were obtained to indicate that gas could be produced continuously and routinely from bone coal in this type of producer whenever conditions justified the necessary development work.

Jan 1, 1960

By C. M. McKinney

Bureau of Mines routine crude-oil analyses of 42 samples from 37 fields in the major producing areas in Mexico are presented in this report. Table 1 includes information on the source and general characteristics of each sample. Table 2 gives a summary of analytical and computed data. A map (fig. 1) shows approximately where the samples were obtained. ACKNOWLEDGMENTS Grateful acknowledgment is made to Alfonso Barnetche, manager of production, and Ing. Francisco Inguanzo, assistant manager of production, both of Petroleos Mexicanos, who supplied the crude-oil samples and furnished information concerning their sources.

Jan 1, 1960

By D. C. Fleck

This report describes a method of using sodium for reducing titanium tetrachloride, developed at Boulder City, Nev., as part of the Federal Bureau of Mines effort to improve the extractive metallurgy of titanium. Finely divided titanium metal, titanium lower chlorides, or a mixture thereof was produced in a continuous operation at temperatures between 105° and 205° C. by the reaction of molten sodium and vaporized titanium tetra-chloride in an agitated bed of finely divided inert solids (powdered sodium chloride or the reaction products). Composition of the product was controlled by varying the relative quantities of sodium and titanium tetrachloride used. A description of the operations and analytical data of the reaction products are given.

Jan 1, 1960

By John D. Bardill

A cooperative project between the Bureau of Mines, Department of the Interior, and the Montana School of Mines, investigating results of hydraulic systems for transporting sand slurries for emplacement, was begun in August 1955. In such circumstances, the Bureau provides funds for a fellowship leading to a Master of Science degree as well as available instruments, tools, supplies and equipment. The School provides the ore-beneficiating laboratory with its equipment for use as a pilot plant. The success of a hydraulic backfilling method employing mill tailings depends largely upon the physical characteristics of the tailings. One of these characteristics is size distribution, especially in the finer size ranges. When being emplaced underground, almost impervious layers of slimes separate from some types of mill tailings containing a high percentage of slimes and settle on the top of the sand fill. These coatings may be so dense that the water in the slurry cannot percolate through them for proper drainage. Successive layers of fill in a stope, each with an impervious coating on top, sometimes build up a hydrostatic head, creating pressure on the bulkheads. This may cause breaks in the lining material, inducing sand runs and flooding the level and sumps below. Deleterious slimes flocculated and disseminated throughout the sands should help prevent the formation of impervious slime layers, increasing percolation and settling rates.

Jan 1, 1960

By J. S. Berber

Bastnasite is a natural fluocarbonate of the cerium group and affords an abundant and high-grade source of the lighter rare-earth elements. As part of a broad research program in rare-earth element technology, the Federal Bureau of Mines directed extensive experimental work to separating and purifying the rare-earth elements in bastnasite. By the use of a combination of techniques--classical chemical, ion exchange, and solvent extraction--the processing of a bastnasite concentrate to obtain the individual rare-earth elements, or groups of elements, was accomplished. A bastnasite concentrate, containing about 60 percent rare-earth oxides, was sulfated with concentrated sulfuric acid to eliminate the carbon dioxide, fluorine, and silica. Calcination at 1,200° F. made the gangue matter insoluble, thus permitting the separation of the soluble rare-earth sulfates. Essentially 100 percent of the rare-earth elements were recovered by this procedure. Since the rare-earth sulfate solution contained only trace amounts of nonrare-earth elements, subsequent separation procedures were simplified.

Jan 1, 1960

By Alla D. Mah

THERMODYNAMIC data for manganese and its inorganic compounds have not been critically surveyed since the work of Maier (31) 3 in 1934. At that time data were lacking or inadequate for many of the important metallurgical compounds. Experimental work, conducted during the intervening years, has supplied so many new thermodynamic values that it is again desirable to examine the available data and compile them into a single publication for handy reference. This paper consists of three main sections. The first summarizes the basic metallurgical thermodynamic data for manganese and its compounds, including heat capacities, entropies, heat contents, temperatures and heats of phase changes, vapor pressures, and heats and free energies of formation. All data available to May 1959 have been considered. The second section contains heats, free energies, equilibrium pressures, and equilibrium constants of reactions of manganese compounds, with special emphasis on metallurgical reactions. The third section supplies basic thermodynamic data for other elements and compounds encountered in metallurgical reactions of manganese, thus making it possible for the reader to conduct thermodynamic calculations without recourse to other literature.

Jan 1, 1960

By W. M. Nabors

As part of a program to promote conservation and efficient utilization of petroleum resources, Bureau of Mines engineers at the Morgantown (W. Va.) Petroleum Research Laboratory are studying secondary oil-recovery projects in the Appalachian region. The increasing demand for petroleum and its products and the increasing cost of exploratory drilling tend to emphasize the importance of improving the recovery of oil from known petroleum reserves. Published reports setting forth the pertinent facts of these operations may help others to profit by the experience. This report presents the results of a study of secondary-recovery methods used in West Virginia by the Piedmont Oil and Gas Co., the Ryan Oil Co., and Water floods , Inc., on their Roane County leases in the Walton and Clover Rush Run pools. The principal oil-producing horizon underlying the area studied is the Big Injun sand, at approximately 2,000 feet. The sand is often referred to as blanket sand because it underlies much of the State and is oil-productive in many localities. Most of the pools in the area were discovered during 1907 to 1910 and were similarly developed and operated.

Jan 1, 1960

By V. A. Nieberlein

This paper presents the results of research undertaken to recover titanium and columbium by low-temperature chlorination of low-grade columbium-bearing ilmenite concentrates, and to simultaneously remove chlorinated impurities from the volatile chlorides without resort to distillation. Coke-reduced ilmenite was chlorinated at 400° to 500° C., and the resulting TiC14 was free of most impurities before condensation. A heated purification column was used wherein various packing materials reacted chemically or physically with the impurities which passed through them in the vapor phase. A nearly water-white TiC14 product was obtained directly. The principal impurities in the titanium tetrachloride were: 0.02 percent Fe, 0.01 percent V, 0.05 percent A1, 0.04 percent Si, and 0.07 percent Cb. This is a less pure product than commercial TiC14. Most of the columbium was recovered as crude CbC15, requiring further refining.

Jan 1, 1960