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By H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960

By Joel N. Van Sant

The rapidly expanding economy of the West, with its growth of heavy industry, and increased steel production, is primarily responsible for the refractory clay industry's concern over the adequacy of the clay supply in States of the Great Plains and Rocky Mountains. Hence, the investigation by the Federal Bureau of Mines of the occurrence and use of refractory clays in North Dakota, South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona has been encouraged by the major consumers and producers of this commodity. The Wyoming investigation is a part of the national program devised to close gaps in the domestic supply of specific types of clays to determine their characteristics and properties and to provide information that will assist the refractory-clay industry. Forty-two locations of clay-bearing rock in 17 areas in Wyoming were examined (fig. 1). Location 3 was not examined during this survey. Its description was taken from an earlier report. Locations 20, 21, and 22 were previously reported but were, also, examined by the Bureau. No samples were collected from these locations because field examination indicated that the shales were not refractory grade. The Hulett, Aladdin, and Newcastle areas are discussed in the section on the Black Hills district; the other 14 areas are described separately.

Jan 1, 1961

By J. B. Gayle

The rate of oxidation of coals with nitric acid has been used by earlier investigators4 5 6/ for determining fusain and for studying petrographic composition. These workers accumulated considerable evidence indicating that, for coals ranging from lignite to low-volatile in rank, the method gives values for fusain that agree satisfactorily with those obtained by optical methods. One group5/even concluded that, when discrepancies are noted between results obtained by chemical and microscopic methods, the results based on the oxidation reaction are probably the more reliable. Unfortunately, after concluding that the method was valid, most of these workers apparently lost interest. As a result, no attempt to exploit or apply the method to problems of utilization has been reported. Recent studies of the influence of inert petrographic constituents on the properties of cokes made from various coals7/ have indicated a need for additional means of characterizing coals and blends used for carbonization.

Jan 1, 1960

By R. L. Montgomery

Heats of solution of yttrium chloride and oxide in hydrochloric acid were measured by Bureau of Mines researchers. Using the heat of combustion of yttrium mentioned in the literature, the Bureau calculated the heat of formation of yttrium chloride to be -239.16 + 0.50 kcal./mole. The Bureau experiments gave evidence that the heats of solution of yttrium chloride from the literature are mostly too low because of water and/or oxychloride impurities. Heat of combustion of yttrium (8)3/ and its heat of solution in hydrochloric acid (2, 14) have been measured. The earlier heat of solution measurement (2) is unreliable because of possible potassium contamination (4). Heat of solution of yttrium chloride has been measured by three researchers (3, 9, 15), who obtained widely different results. Spedding and Flynn (14) report the heat of formation of yttrium chloride as -232.69 kcal./mole from their solution studies. The present work was designed to check the reported heats of solution of yttrium chloride and to determine the heat of solution of yttrium oxide. The latter measurement would allow the results of solution and combustion data for yttrium to be intercompared.

Jan 1, 1960

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 E. G. King

Thermodynamic calculations involving the oxides of tungsten and molybdenum have been hampered by lack of accurate entropies and high temperature heat contents. This paper presents work by the Federal Bureau of Mines on new low-temperature heat-capacity data leading to the evaluation of the 298.15° K. entropies of tungsten dioxide and tungsten trioxide, as well as high-temperature heat contents (above 298.15° K.) of molybdenum dioxide, molybdenum tri-oxide, tungsten dioxide, and tungsten trioxide. Included are heats of fusion of the two trioxides. The heats of formation at 298.15° K. of these four oxides are tabulated as measured by Mah4 5/ of this laboratory. Included also are the 298.15° K. entropy of Mo02 measured by Kin 6/ of this laboratory, and that for Mo03 according to Kelley and King.7/ These basic data provide a consistent compilation from which to perform accurate thermodynamic calculations involving these compounds. No previous low-temperature- heat-capacity measurements have been reported for tungsten dioxide. Seltz, Dunkerley, and DeWitt8/ measured the low-temperature heat capacity of tungsten trioxide. The only previously-reported high-temperature heat-content measurements for any of the oxides were conducted by Cosgrove and Snyder,9/ who measured molybdenum trioxide to 1,300° K.

Jan 1, 1960

By W. M. Mark

This investigation was undertaken to develop methods to improve the quality of titanium sponge produced by the Bureau of Mines modification of the Kroll magnesium reduction process. Research revealed that by systematic elimination of detrimental impurities introduced with the raw materials and by improved handling and processing techniques, high-quality ductile titanium with a hardness of less than 110 B.h.n. (Brinell hardness number) can be produced consistently. This improvement was accomplished by helium (or argon) stripping of residual atmospheric and other dissolved gases from the titanic chloride, preliminary dehydration of crude titanium sponge, and careful regulation of the titanium tetrachloride (TiC14) feed rate to the reactors.

Jan 1, 1960

By J. P. Capp

This experiment, one of a series on underground gasification of coal, was an investigation by the Federal Bureau of Mines of hydraulic fracturing as a means of increasing the air acceptance of a coalbed to permit introducing combustion air and removing product gases. Specific objectives of the investigation included: (1) Fracturing a coalbed; (2) determining the distance the coal was physically affected; (3) ascertaining the effect of the fracture on air acceptance of the coalbed; and (4) gasifying the coal. The coal was fractured with a fluid consisting of 15,000 lb. of sand mixed with 10,000 gal. of fuel oil and 5,000 gal. of kerosine, injected at pressures up to 900 p.s.i.g. and rates up to 425 g.p.m. The oil served as the fracturing medium, and the sand as a propping agent to hold the fracture open. From the fracture point, (the place in the bed where the fluid was injected), the fracture extended 200 ft. or more along the face cleats, somewhat less along the butt. cleats, and was confined to the coalbed. At the fracture point, the bed accepted about 500 std. c.f.m. of air, which was an etghtyfold increase. Fracture effects were extensive, as airflow was noted from old mine workings and outcrops 600 to 800 ft. from the fracture point. It is probable the actual fracture was much less than 600 ft. and that normal coalbed permeability beyond the fracture limits was responsible for this flow. This indicated that effects of the fracture extended beyond the area of coal physically affected. Although no attempt was made to gasify coal more than 200 ft. away, these effects plus the natural permeability of the bed likely would permit combustion beyond the outer limit of the fracture. As these experiments continued for more than 2 years, and greater air acceptance due to the fracture was observed at the beginning of each test, it is apparent that the effects of the fracturing persist for a considerable time.

Jan 1, 1960

By R. M. Becker

THIS IS a progress report on a study of the application of statistical practice to mine and mineral sampling undertaken by the Federal Bureau of Mines to provide sound theoretical and practical data for use of the mineral engineering professions. One of the problems in mine sampling is determining the reliability of the results. For certain types of sampling data (random data) the reliability of the results can be stated mathematically. For other types of data there is no known means of quantitatively expressing reliability. In applying measures of reliability to a set of random data, some knowledge or assumption of the characteristics of the particular data is necessary. In many fields these characteristics are well known. However, in mining, where the data are in assays, these characteristics are not well known.

Jan 1, 1961

By R. L. Marovelli

ANTICIPATING the eventual use of the huge tonnages of nonmagnetic taconites of the Mesabi range of the United States, the Federal Bureau of Mines is classifying and evaluating these deposits in detail. This introductory report describes work begun in 1954 as part of a long-range program to sample, classify, and evaluate important occurrences of nonmagnetic taconite on the Mesabi, range. Included in this report are brief discussions of the geology, history, and potential of the Mesabi range district and mining industry, together with a more detailed presentation of the sampling and metallurgical evaluation of these nonmagnetic taconite deposits. A total of 898 field samples was collected. Most of these were taken in the region between Grand Rapids and Chisholm, Minn., but a few came from the area between Chisholm and Buhl, Minn. Of the total samples, 865 were from open pit bank faces where the greater vertical distances presented by the cherty members facilitated the taking of a large number of samples. Conversely, the narrow face presented by the slaty members confined and limited the areas from which samples were taken. In addition, 33 of the field samples were taken from rock dumps in order to determine, in a preliminary way, the characteristics of these materials.

Jan 1, 1961

By L. J. Kane

Chemical processes using coal often require economical removal of dust from high-temperature gases. Laboratory-scale investigations by the Federal Bureau of Mines have shown that an aluminum silicate fiber is suitable for filtering dust from gases at 1,800° F. The effects of the bulk density of the filter, rate of gas-flow, concentration of dust in the filter, fiber diameter, depth of filter, and concentration of dust in the feed gas on removal efficiency, pressure drop, and capacity of the filter to hold dust were studied. The laboratory filters were difficult to construct because the fibers were longer than the tube diameter. This caused irregular distribution of fiber that permitted dust-laden gases to leak through channels developed in the filter. Leaks also formed between the filter and the tube wall, but this was minimized by improved filter design. However, edge leaks and leaks through channels in the filter probably would be insignificant in properly constructed filters of industrial size. As the concentration of dust in the filter increased, the efficiency of the low-density filters decreased, contrary to expectations, probably because a higher percentage of the dust passed through channels that developed in the filter. The efficiency of high-density filters, however, increased with the concentration of dust in the filter. Results indicate that loosely packed filters would have a longer life than tightly packed filters at the expense of efficiency. As regeneration or replacement of stationary filters is difficult and expensive, loose filters would be best for filtering gases containing much dust. Gases containing little dust may be cleaned with tightly packed filters to obtain higher efficiency. For either type of filter, precleaning with cyclone separators or other means is advisable.

Jan 1, 1960

By Henry H. Ginsberg

The Federal Bureau of Mines made pilot plant investigations of the process requirements necessary to produce heavy fuel oil by the liquid-phase hydrogenation of bituminous coal. The investigation was carried out in three separate series of experiments. The first series studied the effect of temperature and contact time on product distribution at 3,500 p.s.i.g. and 420° to 480° C. in the presence of 0.1 wt.-pct../ stannous sulfide plus 0.05 wt.-pct. iodoform based on gross coal. As a result of increased contact times and temperatures, the conversion-6/ and yield of hydrocarbon gas increased, the viscosity of product oil decreased, and elimination of oxygen, nitrogen, and sulfur from coal increased. The yield of oil did not indicate any definite trend with changes in temperature and contact time. The yield of oil ranged from 76 to 85 pct. for Pittsburgh coal and from 60 to 85 pct. for Rock Springs coal. Asphaltenes in the product oil ranged from 17 to 38 pct. of the total oil for Pittsburgh coal and from 12 to 22 pct. for Rock Springs coal. Fuel oils meeting Bunker C or American Society for Testing Materials (ASTM) Grade 6 specifications were produced with Rock Springs coal at 0.2- to 1.0-hr. contact time and 440° to 480° C. and with Pittsburgh coal at 0.3- to 1.0-hr. contact time and 420° to 460° C. In the second series of experiments tin, nickel, iron, and zinc were evaluated as catalysts for the hydrogenation of Rock Springs coal to heavy fuel oil at 3,500 p.s.i.g. and 460° C. Using the apparent conversion of coal as criterion of catalyst activity, at a contact time of 0.45 hr. tin was the most effective catalyst; nickel and iron were nearly as effective, but the use of zinc resulted in much lower conversion. When the contact time was increased to 0.80 hr., the apparent conversion of coal was essentially the same for each of the catalysts. When the yield of oil boiling below 3550 C. was used as criterion of catalyst activity, at 0.45 hr. the order of activity was tin, iron, nickel, and zinc; at 0.80 hr. tin was far superior and the others were essentially equal. The product oils contained from 8 to 20 pct. asphaltenes.

Jan 1, 1960

By N. E. Hanna

As part of a program for improving, the safety of permissible explosives, the Federal Bureau of Mines has undertaken an investigation to establish the ability of sodium chloride to reduce the incendivity of permissible explosives to firedamp atmospheres. A motivating influence for this investigation has been the comparatively extensive experience of British and other European investigators, who used sodium chloride as a component of their permitted explosives (1, 5, 6 7).5/ In the United States research and development work of this type has been less extensive, although sodium chloride has been added to permissible explosives as a cooling agent (9) for many years. The results of the first phase of this investigation were presented in a previous paper (8), which established that adding up to 10 percent sodium chloride to permissible explosives reduces the likelihood of ignition of firedamp in the gallery test; however, the results were somewhat inconsistent, and the conclusions were qualified. Accordingly, the investigation was continued with a study of the effect of added sodium chloride as a function of the quantity added and of the particle size of the salt.

Jan 1, 1960

By S. L. Ausmus

The work covered in this report is a continuation of an earlier feasibility study by the Federal Bureau of Mines and points out improvements in the skull-melting method for casting reactive metals such as titanium, zirconium, and hafnium. Machined graphite molds with laminated sections can be reused many times. Large tube sections can be produced by spin casting. Graphite powder is the best expendable mold material, but binders for this use must be compounded carefully. The effects of current and furnace atmosphere on the dependent variables of the casting technique are shown. Because of developments in casting technology for titanium which eliminate the basic problems of melting and pouring the metal, opportunities for improvement in the method have increased. The mold material and gate and riser configurations require particular attention. The limits of application of the casting method have yet to be defined. New knowledge in anyone of these areas could result in marked improvements and simplifications in casting methods.

Jan 1, 1960

By Thomas J. Blalock

The volumetric determination of uranium according to the method of Sill and Peterson (6),3/ which uses cerate oxidimetry after the separation of interferences such as sulfides and cupferrates, has been used for some time by the Bureau of Mines and gives satisfactory results for many of the samples tested. However, in those instances where the uranium content did not exceed a few tenths of 1 percent and iron was present in the range of 10 to 40 percent (as Fe203),4/ the method was cumbersome and unreliable. The need for a more accurate procedure for the determination of small amounts of uranium in the presence of large amounts of iron, such as in shale or black sands, prompted this investigation. The Bureau desired that materials containing as little as 60 p.p.m. of uranium be assayed within reasonable limits of accuracy. One of the primary aims of this work has been to eliminate, as far as possible, the necessity for repeated cup ferron extractions.

Jan 1, 1960

By J. Croeni

The search for new alloys for application in the atomic energy field had prompted investigation of zirconium-rare earth metal alloys by the Federal Bureau of Mines. In this instance the zirconium-dysprosium system was investigated by melting point, thermal analysis, resistivity, X-ray and metallographic methods. Results indicate a single eutectic system with a peritectoid reaction occurring at 890° C. The eutectic isotherm extends from 30 to 95-percent dysprosium at 1,280° C. Eutectic composition is located at approximately 70 percent dysprosium. Solid solubility of dysprosium in both alpha and beta zirconium is extensive. The extent of solid solubility of zirconium in dysprosium has not been determined. Although zirconium rich alloys exhibit a significant increase in hardness, they can be cold worked extensively. These alloys also appear adaptable to solution heat treatment. Additional investigations concerning corrosion resistance and other mechanical properties are necessary for satisfactory evaluation of these alloys. The superior corrosion resistance of zirconium and the nuclear cross-section characteristics of the rare earth metals have stimulated alloy investigations using zirconium as a base metal. Alloys combining these characteristics present a possible substitute for hafnium as a control rod material. In this particular study dysprosium was chosen as the alloying element, and several series of alloys were used to establish the equilibrium diagram.

Jan 1, 1960

By H. L. Gibbs

Many factors contributed to the decision to build a radiochemical laboratory at the Salt Lake City Metallurgy Research Center to investigate the application of radioactive isotopes and chemical compounds in extractive metallurgy. These reasons included the notable success achieved in biological sciences with radioisotopes, the development of reliable instruments and methods for identifying the isotopes and measuring their activities, and the commercial availability of radioisotopes in a variety of forms and known activities. The paramount reason, however, was the realization that better methods were needed for guiding and quantifying research to resolve the complex extractive metallurgy problems under study at the Research Center. This is the first of a series of reports describing the application of radioisotopes and radioactivity techniques in extractive metallurgy. The report includes a discussion of licensing and safety requirements, a general description of the laboratory and the methods used, a definition of the nature and scope of the research program, and a synopsis of the more important problems studied. Subsequent reports will concern radioactive techniques for solving specific problems in mineral dressing, hydrometallurgy, and pyrometallurgy.

Jan 1, 1960

By W. A. Stickney

As part of a Bureau of Mines program to investigate recovery of manganese (Mn) from low-grade materials, laboratory studies were made of four samples of mill rejects: Three from Montana and one from Peru. These studies demonstrated that certain mill-waste products can be a potential source of manganese. Both manganese oxide and carbonate minerals were recovered by flotation in an acid circuit with a fuel oil-tall oil emulsion as collector. Sintering) required to prepare a physically acceptable product, also was used as a method of beneficiation. In addition to being low-grade, some of the samples presented problems of intimate mineral association and complex textures.

Jan 1, 1960

By W. A. Grosh

Records show that much of the lead produced in the Upper Mississippi Valley lead-zinc field was taken from natural openings along crevice systems at shallow horizons or at the surface. During the early history of the district, the shallow deposits were worked intensively; but in recent years the production of lead, except as a byproduct of deeper mining for zinc ores, has not been significant. Considering the methods of early mining, the character of mineralization, and the fact that galena can still be found on the surface of the old digging areas, it was reasoned that enough mineralization might remain on and above bedrock to permit, through the use of modern equipment and methods, economical re-treatment of surface material in the digging areas.

Jan 1, 1960

By I. L. Feld

This report describes an attrition-grinding process and equipment for grinding coarse kaolins to the 2-micron particle-size range. The research was undertaken by the Bureau of Mines to devise an acceptable method for converting coarse kaolins, such as paper-filler-grade clays, to paper-coating-grade clays, thereby increasing the value and extending the life of the southeastern paper-clay deposits. The attrition-grinding process is basically the intense agitation of a slurry composed of the material to be ground, a granular grinding medium, and a suspending fluid. This process gave better particle-size reduction than that obtained by several other grinding methods. Results of batch tests in 5-and 10-inch-diameter attrition grinders demonstrated that a coarse kaolin containing about 13 percent minus 2-micron, equivalent spherical diameter (e.s.d.) particles was readily ground to give a product with 88 percent minus 2-micron e.s.d. material. Power consumption was reasonable in view of the increased value of the ground material. Comparison of particle-size reduction with power-consumption data for the two units indicated that better performance was obtained with the larger machine.

Jan 1, 1960