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By W. T. Abel

The rate of the steam-carbon reaction, which is of fundamental importance to coal gasification, was determined by passing steam over graphite specimens suspended in an electrically heated tube. The measurements were made at 1,900° to 2,400° F. and at steam-feed rates of 0.1 to 2.0 moles of steam per mole of carbon per minute. At the maximum steam-feed rate, the reaction rate of carbon ranged from 0.4 percent per minute at 1,900° F. to 7 percent per minute at 2,400° F. Up to about 2,200° F., the steam-feed rate had only a slight effect; above this temperature, it limited the reaction velocity when the final mole fraction of steam in the reaction products was much less than 1.

Jan 1, 1962

By E. G. King

Heat of formation values for mercuric sulfide appear in all the comprehensive listings of thermodynamic data, but experimentally determined entropy values have been lacking. Consequently, all free energy calculations involving mercuric sulfide have been based upon estimated entropy values. This paper reports Bureau of Mines measurements of the low-temperature heat capacity of red mercuric sulfide (cinnabar) and the entropy value at 298.15° K. derived therefrom. The entropy value was combined with heat data to obtain free energy values for the formation of red mercuric sulfide from liquid or gaseous mercury and from rhombic or gaseous diatomic sulfur.

Jan 1, 1962

By W. A. Calhoun

This report gives results of metallurgical investigations performed by the Bureau of Mines on mineral samples taken during April 1959, from Hawaiian bauxite deposits on the islands of Kauai, Maui, and Hawaii. The bauxite samples were tested at the Bureau's Rolla Metallurgy Research Center, Rolla, Mo., to determine if alumina could be extracted. The results were encouraging. Extraction of the alumina by the American Bayer type digest of crude ore samples from Kauai, Maui, and Hawaii recovered 78.8, 73.1, and 70.0 percent, of the total alumina, respectively. These recoveries were increased to 82.8, 85.5, and 79.5 percent by modifying the treatment, which consisted essentially of calcination and weak caustic desilication to provide a residue. The residue was then treated with calcium oxide and digested in a strong caustic solution to extract the alumina.

Jan 1, 1962

By J. V. Batty

Radioisotopes of selenium (se78) and tellurium (Te123) were successfully employed by the Bureau of Mines as tracers in metallurgical research directed to developing improved methods for volatilizing these elements from low-tenor raw materials. Prior research, guided and controlled by conventional analytical methods, was seriously hampered by inconsistent selenium and tellurium analyses, by the slowness of the conventional chemical methods, and by the poor accountability of these volatile elements in test products. Methods were devised and evaluated for admixing the radioactive tracer with typical raw materials and then following the deportment of the selenium and tellurium by radiometric methods with occasional chemical analysis checks. These techniques were found unusually effective in (1) quantifying the completeness and the rate of volatilization of selenium and tellurium while heating the raw materials at different rates to different temperatures and (2) accurately tracing and quantifying the distribution of minute amounts of these volatile elements in the several products made by high-temperature treatment and in the several units comprising the experimental equipment.

Jan 1, 1962

By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

By Philip E. Niebuhr

A procedure, which can be performed in the field by nonanalytical personnel, is given for sensitive spot tests for detecting tellurium or selenium. The expressed need of a field test for detecting small amounts of tellurium, which may be accompanied by relatively large amounts of selenium, has led to the development of this method. Tellurium search has been impeded by the lack of a satisfactory test from the standpoint of sensitivity and specificity. A quantitative laboratory method exists, but it is expensive and relatively laborious. Several other qualitative tests are known, but they require unstable solutions, which must be freshly prepared for use, and a greater variety of laboratory equipment. The particular advantages of the test described are its simplicity and the stability of the reagents required, there-fore is is well adapted for field use. Also, this test was found to be of practical use in the analytical laboratory when screening samples, thereby reducing analytical costs. The roughly quantitative interpretation of the results can save time by indicating the approximate size of the sample taken for a quantitative determination.

Jan 1, 1962

By Joseph M. Singer

This research project had two main objectives: (1) To identify the smoke limits of gaseous fuel-air mixtures and (2) to obtain and evaluate basic chemical information on the formation of smoke in very rich flames near the smoke limit. Such information would do much to establish the circumstances for car-bon deposition in gas appliances and in other types of combustors. Based on tests with ethylene and propane, these studies showed the following: 1. Smoke limits are related to the yellow-tip limits of the fuel. Previous research established sufficient data to permit prediction of yellow-tip limits on gas burners using a wide variety of fuels. The present study of smoke limits deals only with ethylene-air flames, but the concept that was developed is probably applicable to other fuels.

Jan 1, 1962

By W. J. Boone

The Bureau of Mines has programmed for publication a series of Reports of Investigations of studies it has undertaken on low-temperature phase equilibria of several helium-bearing natural gases. This report is the second of a series of papers of the same general title; it is anticipated that additional reports of this series will be published. The advent of a helium conservation program and the prospect of production of helium by private industry, make it especially desirable to publish these data. This report describes phase equilibria related to a natural gas that is processed for helium at the Bureau's Exell Helium Plant (located about 35 miles north of Amarillo, Tex.). Carbon dioxide and water in the gas were removed before making the study; hence the data obtained are representative of the gas stream immediately after similar preliminary treatment in the plant process. Phase equilibrium data were obtained for conditions from -50° to -275° F. and from 100 to 500 p.s.i.a. Analyses of samples were made as follows: For a given run at a selected temperature and pressure, samples of the vapor and liquid phases were analyzed by mass spectrometer, and an additional sample of the liquid phase was analyzed for helium by means of special apparatus (7). 4

Jan 1, 1962

By David E. Fogelson

One model each of three different makes of portable displacement seismographs was calibrated on a shaking table capable of 5,000 pounds of force, Calibration tests were conducted in the frequency range of 5 to 200 c.p,s, and in the amplitude range of 0,002 to 0.05 inch peak-to-peak, The seismographs were tested under two mounting conditions: (1) The feet of the instrument were bolted to the shaking table, and (2) the feet were resting on emery cloth affixed to the table, The results of these tests show that, in the frequency range of 5 to 40 c.p,s, and for vibration levels less than 0.2 g, the magnification for all three instruments is constant with input level but varies slightly with frequency. For vibration levels greater than 0.4 g. and for frequencies greater than 40 c.p.s., the magnification of all three instruments shows large variations with frequency and amplitude of table motion.

Jan 1, 1962

By Willard L. Hunter

The research described in this Bureau of Minus report was conducted to improve the chromium-iron ratio of offgrade chromite. Two methods were used: (1) Iron was selectively reduced from chromite by carbothermic reduction in an electric-arc furnace, and (2) a mixture of carbon, chromite, and sometimes fluorspar was chlorinated to remove a substantial part of the iron. Chromite concentrate from the Mouat deposit in Montana and from northern California was used in the test work. Chromium-bearing slag and chromite that had been beneficiated by a roast-leach process were each smelted to produce high-carbon ferrochromium. Iron was selectively reduced in a laboratory-scale., electric-arc furnace. Carbon additions to the smelting charges varied from 40 to 100 percent of the stoichiometric requirement, and slag basicities were varied from 0.4 to 1.0 chromium-iron ratios of more than 4:1 were obtained with 89 percent recovery of chromium in a chromium-bearing slag.

Jan 1, 1962

By K. E. Tame

Pollution from radioactive nuclides, principally Ra226, in liquid waste from uranium mills can be minimized by reusing the waste solution within the mill. Such reuse of waste solution in the Vitro Chemical Co.-type process was investigated in the laboratory. Vitro employs an acid leaching process for dissolution of the uranium, countercurrent decantation for liquid-solid separation and washing, and amine solvent extraction for recovery of the uranium from solution. The simulated reuse of barren raffinate in the mill circuit was carried through two separate laboratory campaigns of 29 and 31 cycles. Conventional chloride stripping of the amine was employed in the first campaign, whereas nitrate stripping was used in the second campaign. Dissolution of uranium from the are in the acid leaching circuit averaged 96 percent. Washing efficiencies of 98 to 99 percent were attained by using 4 volume tons of combined raffinate and makeup water per ton of ore. Uranium recovery from the pregnant solution using a 5-percent solution of amine LA-1 in kerosine ranged from 99.3 to 99.9 percent.

Jan 1, 1962

By J. Burlin Johnson

In small-scale blasting experiments conducted in the Bureau of Mines laboratory, small charges were used to produce craters in blocks of concrete mortar. The results are compared with larger scale experiments of other research workers, and the comparison demonstrates the similarity of the results obtained and indicates that small-scale blasting should be a useful tool for predicting large-scale blasting effects. INTRODUCTION The purpose at this investigation was to conduct blasting experiments in mortar in the laboratory and then, by comparing the results with those from larger scale field blasts in rock to determine to what extent, if any, the laboratory results resemble those in the field. The work described herein was the initial phase of a project aimed at evaluating small-scale blasting as a tool for use in improving blasting techniques. It is evident from the stand-point of control and cost that small-scale blasting would be valuable in the study of rock fragmentation by blasting in mines and quarries, if the extrapolation is valid.

Jan 1, 1962

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 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