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By W. T. Benson

The Bureau of Mines has undertaken investigations to examine selected deposits of beryllium throughout the United States. The beryllium deposit about 6 miles southeast of Lone Pine in the Owens Valley region of Inyo County, Calif., was among those selected for study. In 1960, field work was conducted on the Inyo Beryl claim to determine the extent and character of the beryl-bearing deposit. This report describes the work that was done. In the area investigated, the beryl occurs disseminated in granite and limestone and as stringers. Apparently, the stringers are related to nearby pegmatite dikes, inasmuch as some appear to contain fine-Grained pegmatite. Granitic rocks enclose most of the stringers, which occur as fracture fillings, ranging from thin seams to 4 inches in thickness. The stringers are of muscovite, quartz, albite, and beryl. Some also include epidote and fluorite. For the most part, they are widely spaced. Therefore, mining of substantial tonnages averaging better than 0.2 percent beryl does not appear feasible.

Jan 1, 1962

By E. D. Calvert

The objective of this research was to examine variations in melting and forging practice for four titanium-base alloys and to determine their effect on the resultant product. Of particular interest was the evaluation of the skull-casting technique. The data should serve as a guide to producers and consumers of titanium products. Physical properties of four titanium-base alloys in ingot form and in sheet form were evaluated and correlated, where possible, with variations in the melting and casting procedure. Consumable-electrode melting was used throughout, but arc current and furnace backfill pressure were varied, and ingots were formed both by melting directly into a water-cooled copper mold and by skull melting followed by pouring into a graphite mold. Alloying metal additions for the alloys tested were (1) 8 percent manganese, (2) 6 percent aluminum and 4 percent vanadium, (3) 6 percent molybdenum and 2 percent aluminum, and (4) 16 percent vanadium and 2.8 percent aluminum.

Jan 1, 1962

By Robert W. Van Dolah

On December 27, 1961, a fire and explosion destroyed the blasting agent mixing plant and an attached storage barn of the Whitaker-Atlas Supply Co., near Norton, Wise County, Va. Five residences, an office building, four trucks, and three automobiles were completely destroyed; a house trailer and several other trucks and automobiles were severely damaged; and other property damage, including much window breakage, occurred up to 3 miles or more airline distance away. Through the quick action of the fire marshal of the Norton Fire Department, Norton, Va., there were no fatalities and only five persons required hospitalization. This incident is of particular interest because of the widespread practice of mixing fuel oil (FO) with ammonium nitrate (AN) to prepare low-cost blasting agents, in many cases under conditions and circumstances not very different from those presented here. A representative of the Bureau of Mines Explosives Research Laboratory, Pittsburgh, Pa., and field representatives of the Bureau's Health and Safety Activities conducted the investigation. Information in this report was obtained from representatives of the Whitaker-Atlas Supply Co., the Norton fire marshal, and others who were on the scene either shortly before or after the incident occurred. Representatives of the Manufacturing Chemists' Association, the Institute of Makers of Explosives, and individual ammonium nitrate producers participated in the inquiries and investigations.

Jan 1, 1962

By M. R. Geer

All the coal lands in Alaska are publicly owned, and the Federal Government is the principal consumer of coal. Therefore the Government has long been concerned with the wise utilization of the coal reserves of Alaska as well as with the availability of coals meeting the specifications for use in various Government installations. Coal preparation plays a key role in both of these areas of interest. The proper choice and operation of coal-washing equipment permits the mining of inferior deposits, minimizes waste of coal in preparation, and assures a prepared product of the best quality obtainable from the raw coal. Thus, from time to time, the Bureau of Mines has made washability examinations on most of the coals mined in Alaska. Generally, these examinations were made when new mines or new beds were opened, when construction of new preparation plants was being considered, or when the operation of existing plants could be improved by better knowledge of the raw coal. The purpose of this report is to bring together all the washability data available on the coals of the Matanuska Valley and Beluga River fields. The pattern of energy development for the rapidly growing Anchorage area is not clear at this time. Formerly coal was the only fuel available for large-scale space heating and power generation. More recently both oil and natural gas have entered the market, and several hydroelectric projects have been completed. Additional major hydroelectric projects are being considered. The role that will be played by coal in this competitive energy market is uncertain. However I if coal is the fuel used in future power plants or industrial installations, the information contained in this report will be useful in indicating the quality of the coals that can be supplied and in selecting proper preparation techniques.

Jan 1, 1962

By Scott W. Hazen

This report describes the design, analysis, and results of a special experimental mine-sampling project conducted as part of the Bureau of Mines continuing program on sample-methods research. The experimental project was conducted at the Bureau?s Denver Mining Research Center and at the Climax molybdenum mine within the framework of a cooperative research agreement between the Bureau and Climax Molybdenum Co., Division of American Metals-Climax, Inc. The primary objective of the project was to investigate the interrelation-ship between sample volume, number of samples, the standard deviation of an assay distribution, and the precision required for an estimate of grade of ore, and to develop this interrelationship into a relatively simple method of application for use in mine sampling.

Jan 1, 1962

By Charles W. Huggins

A study of the high magnification of some inorganic fibers which are found in nature or produced in the laboratory, has been conducted with the electron microscope. This series of electron microqraphs shows the important morphological differences exhibited by potassium-lead silicate, lead-aluminum silicate, chrysotile, wollastonite, silicon nitride, potassium titanate, cobalt chrysotile, magnesio-fluor-richterite, fluor-richterite, refractory oxide fiber, silicon carbide, massive serpentine, and palygorskite. A ribbon or a thin lath 250-2500 A. wide is the structural form of potassium-lead silicate and lead-aluminum silicate. Chrysotile, cobalt chrysotile, and massive serpentine all have a tubular structure and a fairly uniform (150-300 A.) diameter. Wollastonite, potassium titanate, fluor-richterite, and magnesio-richterite crystals have a lath shape, and potassium titanate laths are laminated ribbons. Single fibers of silicon nitride and palygorskite are ribbons, and the silicon nitride sample contains many twins (branching fibers). Palyqorskite fibers are highly flexible and have cross-sectional measurements of 150-300 A. Silicon carbide fibers differ from other fibers because their structure consists of several different forms. The sample used in this study had, predominately, a margarite-type structure. The refractory oxide fiber lost, all its apparent fibrosity after being prepared for electron microscopic examination, and only irregular fragments are visible in the electron micrographs.

Jan 1, 1962

By G. E. Johnson

A bench-scale study was made of removing hydrogen sulfide from synthesis gas at elevated pressure by iron oxide impregnated on wood chips. The gas contained 0.02 to 0.06 percent oxygen. The removal of hydrogen sulfide by iron oxide impregnated on wood chips is more efficient at elevated pressure. At constant space velocity, longer periods of operation at 400 p.s.i.g. are possible before the exit gas reaches a given maximum concentration of hydrogen sulfide, compared with 200 p.s.i.g. or atmospheric pressure. In tests at room temperature, 60° C., and 100° C., the most effective removal of hydrogen sulfide was obtained at room temperature and the least effective at 100° C. Dry impregnated wood chips removed only about half as much hydrogen sulfide as chips wetted to a water content of 50 percent.

Jan 1, 1962

By A. D. Hahn

This report describes reconnaissance by the Bureau of Mines of titanium-bearing beach sands on Ship Island in the Gulf of Mexico off the south coast of Harrison County, Miss. The purpose was to determine the ilmenite, rutile, and associated heavy-mineral content of black-sand-bearing beach sands. The investigation was part of a survey of titanium resources of the United States. Ilmenite (FeTi03), an iron-titanium oxide, is the major titanium-bearing mineral consumed in the titanium pigment industry. Rutile (TiO2), titanium dioxide, is used mainly as a constituent in welding-rod coatings and in producing titanium metal. The major fieldwork was conducted during the first half of February 1961. Nine holes, totaling 220 feet of bore, from which 110 samples Her taken, were drilled at widely spaced intervals on the island.

Jan 1, 1962

By M. E. Tyrrell

Lightweight basic refractories suitable for use in some sections of the all-basic furnace were developed. Potential advantages of such refractories are lower weight, improved resistance to thermal shock, and less tendency to spall off the working face. Plant trials in positions not subject to heavy loading or severe erosion seem warranted. Forsterite (2MgO.SiO2), stabilized dolomite (2Ca0?SiO2 + MgO), and chrome-spinel [(Fe,Mg)0?(Cr,Al) 031 refractories were fabricated using bubbles as the principal component in the brick mixtures. Bubbles were blown from melts of the basic raw materials as they were tapped from a conducting-hearth arc-resistance furnace. The bubbles were graded, bonded with synthetic Forsterite plus mineralizers, dry-pressed, and fired to temperatures of 1,600° C. or over in a gas-fired kiln. Refractory properties of the bubble brick were compared with those of insulating refractories made by burning combustibles out or dense brick mixtures. Lightweight refractories fabricated of bubbles were one-third lighter in weight than dense bricks of like materials. Their mechanical strength was satisfactory, and their resistance to thermal shock was excellent. In tolerance to open-hearth slag and in resistance to thermal shock, the chrome-spinel bubble bricks wore the best of the refractories tested. Basic refractories of the insulating type were about 40 percent lighter in weight than dense commercial refractories, but they were mechanically weak and not suitable for superduty service.

Jan 1, 1962

By Alfred V. C. Meyer

A Blastcorder4 was calibrated on the Bureau of Mines shaking table in the frequency range of 12 to 40 c.p.s. and in the amplitude range' of 0.25 to 1.0 g. The results of this calibration study show that in the frequency range of 12 to 30 c.p.s. the average accuracy of the Blastcorder is approximately ± 0.1 g.

Jan 1, 1962

By Raymond W. Hiteshue

Experiments were conducted al temperatures of 480° to 800° C. and hydrogen pressure of 6,000 p.s.i.g. to determine the effect of coal residence time on the conversion of a high-volatile bituminous C coal to liquid and gaseous products when using a semicontinuous apparatus designed fur rapid heating and cooling of reactants. The objective of the studies at high temperatures was to determine if appreciable quantities of coal could be converted to gaseous hydrocarbons and low-boiling liquid hydrocarbons. Experiments at lower temperatures were designed to indicate shifts in product distribution with respect to temperature and to learn more about the general mechanism of the reaction when using close control of coal residence time. One percent molybdenum, based on m.a.f. (moisture-and ash-free) coal, was used throughout this investigation. At 800° C., 6,000 p.s.i.g., and "zero" residence time) the yield of gaseous hydrocarbons was about 38 percent and the yield of oil about 4.5 percent, based on m.a.f. coal. With IS minutes residence time, under the same conditions, the yield of gaseous hydrocarbons was approximately 80 percent with no increase in yield of oil. Apparently at 800° C., and hydrogen pressure of 6,000 p.s.i.g. coal was rapidly carbonized to char with expulsion of volatiles. Char was then slowly hydrogenated to gaseous hydrocarbons without production of oil.

Jan 1, 1962

By Louis P. Domingues

As part of a study on high-temperature ceramic materials, the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of yttrium, lanthanum, and cerium were analyzed thermogravimetrically. The temperature ranged from room temperature to 1,500° C. Each salt was decomposed by heating at a rate of 2.5° C. per minute, and some of the salts were subjected to additional rates of 5° C. per minute or 10° C. per minute. The decomposition sequences have been identified, and the temperatures of formation of intermediate compounds and of the oxides have been determined. The minimum oxide formation temperature of a given lanthanum salt exceeds that for the similar salt of yttrium, and both exceed that for the same salt of cerium except for one cerium carbonate. Variation of the heating rate indicates a thermal lag in the materials and produces the shift of formation temperatures to higher values and loss of resolution in the weight-loss distribution as the heating rate increases.

Jan 1, 1962

By Robert K. Koch

Laboratory-scale studies on defluorination of natural and synthetic fluorspars by pyrohydrolysis at 1,500° C. were made to determine the feasibility of developing a process for producing hydrogen fluoride from siliceous fluorspars. It was found that the reaction (at 1,500° C.) is not promising for process development, even though a silica-free offgas can be generated. The primary difficulty is the low hydrogen fluoride content of the offgases; an HF content of 6 percent was the best achieved. Previous research by the Bureau of Mines has demonstrated that offgases averaging 27 percent hydrogen fluoride can be produced under carefully controlled conditions at 1,280° C. The lower temperature process is a better method for production of HF. However, charges in which the CaF to Si02 mole ratio varied from 0.4 to 2 could be processed with similar results. Also, combined alumina and ferric oxide contents up to 25 mole-percent did not noticeably alter the rate of defluorination. Therefore, virtually any natural siliceous fluorspar would respond in essentially the same manner when exposed to water vapor at 1,500° C.

Jan 1, 1962

By L. B. Pankratz

Present-day interest in the rare-earth elements and their compounds, for both metallurgical and ceramic uses, makes it highly desirable to accumulate basic thermodynamic data that can be applied to theoretical considerations of the processing of these substances. Such data still are seriously lacking. This Bureau of Mines paper reports the results of high-temperature heat content measurements of the sesquioxides of four rare-earth elements--europium, gadolinium, neodymium, and samarium--and of the closely related element, yttrium. The temperature ranges covered by the measurements are as follows: Monoclinic Eu2O3, 298°-1,802° K. Cubic Eu203, 298°-1,350° K. Monoclinic Gd203, 298-1,802° K. Cubic Gd203, 298°-1,550° K. Hexagonal Nd203, 298°-1,795° K. Monoclinic Sm203 298°-1,798° K. Cubic Sm203, 298°-1,149° K. Cubic Y203, 298°-1,799° K.

Jan 1, 1962

By Alla D. Mah

The need for more and better basic thermodynamic data for the oxides of many of the rare metals is evident to anyone who attempts thermodynamic calculations involving these substances. In continuation of a Bureau of Mines program to meet this need, this paper reports new experimental values of the heats of formation at 298.15° K. of the hexagonal crystalline variety of germanium dioxide and germanium dioxide glass. The values were obtained by means of combustion calorimetry and sodium hydroxide-solution calorimetry. The calorimetric results also made possible the derivation of values for the heat and entropy of fusion of hexagonal germanium dioxide at its melting point. The newly measured data were combined with previously known entropy and high-temperature heat content values to obtain heats and free energies of formation of germanium dioxide (in the hexagonal crystalline, glassy, and liquid states) over the temperature range from 298.15° to 2,000° K.

Jan 1, 1962

By Robert F. Stewart

The oxidation of structural materials at high temperatures in gas-cooled systems can be greatly retarded by the addition of small amounts of hydrogen to the inert coolant. In experimental equipment for gasifying coal with heat transferred by helium, the oxidation of graphite and metals (molybdenum, tungsten, and certain stainless steels) by trace impurities in the coolant helium was virtually eliminated by adding 0.1 to 1.0 percent hydrogen. The reaction of hydrogen with praphite does not preclude its use to retard oxidation; at 2,400° F. only 0.2 pound of graphite per square foot per year is lost for each percent of hydrogen in the helium. The addition of hydrogen appeared to prevent the mass transfer of carbon often associated with oxidation of graphite, without causing noticeable embrittlement of stainless steels and molybdenum or other damaging effects. This method has been tested in precision gas-recycle systems and applied successfully for more than a year in a pilot-scale unit operating at 250 pounds per square inch gage and 2,400° F. It is now used routinely and can be applied to many gas-cooled systems operating at high temperatures.

Jan 1, 1962

By F. H. Gibson

In recent years physico-chemical techniques have been applied for rapid analysis of coal and coke ash as replacements for classical wet-chemical methods. Although the classical methods are accurate, they are time consuming because many chemical separations are necessary to complete an analysis, and they require skilled analysts for accurate work (12).4 For the past several years the Bureau of Mines has applied some of the newer physico-chemical techniques in its continued search for new and improved methods at analysis. The methods of analyzing coal and coke ash evolved from this work include spectrophotometric methods far SiO2, A120, , Fe203 , TiO2, and P2O5; chelatometric titration for CaO and MgO; and flame photometry for Na20 and K2O. The methods are rapid and direct, are suitable for analyzing a group of samples at the same time in production work, and dire results with almost the same accuracy as classical procedures. With the new methods, complete analyses in duplicate can be obtained at a rate of 2 to 3 times that of conventional methods.

Jan 1, 1962

By C. W. Dwiggins

This report describes the development, theory, and application of techniques and instruments for quantitatively determining nickel, vanadium, and iron in oils, using direct, X-ray emission spectrographic methods (5, 6).3 The methods developed apply to petroleum and other oils as well as some specific fractions of oils. The quantities of nickel, vanadium, and iron in various petroleums are of practical and theoretical interest. Even traces of nickel and vanadium may poison cracking catalysts, and X-ray methods have been used for determining nickel in such catalysts (7). At least parts of the nickel and vanadium occur as metal-porphyrin complexes, a fact which may have considerable bearing on knowledge of the origin of petroleum.

Jan 1, 1962

By E. G. King

As low-temperature heat-capacity and entropy data were available for only one sesquisulfide (cerium sesquisulfide), it appeared desirable to augment the information for this class of compounds by measuring the sulfides of antimony and indium. In addition a pressing need existed for data on indium sulfide to supplement vaporization studies in progress in the Department of Mineral Technology, University of California. This Bureau of Mines paper reports low-temperature heat-capacity measurements and entropy evaluations at 298.15° R. of antimony sesquisulfide of stoiehiometric composition (Sb2S3) and of indium sesquisulfide which was somewhat deficient in sulfur (In2S2.93). The data for the latter substance were adjusted to correspond to the stoichiome tric composition (In2S3 ) . Indium sesquisulfide has a lower entropy at 298.15' K, than either antimony sesquisulfide or cerium sesquisulfide, in line with the higher atomic density of the indium compound.

Jan 1, 1962

By Harry R. Nicholls

The objectives of this investigation were to determine the strain propagation laws for a strain pulse in salt and to compare the seismic effects from the detonation of different explosives in salt. The investigation showed that a strain propagation law of the type, e = K(R/W 1/3 ) n, and a strain energy propagation law of the type, Ea/W 1/3 = K(R/WI/3)b , are valid in salt. A change in the regression law coefficient, n , was noted with strain level. A similar change in b was inferred because strain energy is proportional to the square of strain amplitude. Particle velocity data may be used interchangeably with strain data under the test conditions.

Jan 1, 1962