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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 Sarkis G. Ampian

The Bureau of Mines has developed a method for identifying fine particles of beryl in mineral samples by preferentially staining the beryl grains. The sample is first subjected to a heated sodium hydroxide solution to etch the beryl particles, which are subsequently stained an intense blue color in a boiling alkaline solution of quinalizarin. Positive identification of beryl grains permits quantitative analyses by microscopic techniques. INTRODUCTION Beryl, a beryllium aluminum Silicate, is the principal ore mineral of beryllium. The only known commercial concentrations of this mineral are found in pegmatite dikes of granitic composition. Normally beryl is associated with muscovite mica, quartz, and the sodium-and potassium-bearing feldspars (orthoclase, microcline, and albite). Other beryllium-bearing minerals which are found occasionally in minor amounts with beryl are phenacite, a beryllium silicate, and chrysoberyl, a beryllium aluminate.

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 John J. Mulligan

Lead-silver deposits in the Omilak area, on the western slopes of the Darby Mountains, Seward Peninsula, Alaska, were investigated by the Bureau of Mines, during the 1953 and 1954 field seasons, as a part of the U.S. Department of Interior's continuing program for the development of Alaska's resources. The Omilak area was the scene of early day prospecting and mining activity. The Omilak mine, which operated from 1881 to 1890, was the second producing lode mine in Alaska; the first was a small gold mine near Sitka. Several hundred tons of ore were produced at the Omilak mina; as an indication of grade, 41 tons shipped from Omilak in 1889 contained 75 percent lead and 142 ounces of silver per ton. A prominent, nearby occurrence of lead-silver minerals, found but not explored during this period, has since become known as the Foster prospect. Subsequent exploration of this prospect revealed an abundance of massive galena occurring on an outcrop and as float scattered through limestone talus. Evidence of lead deposition, together with the generally high silver content of lead ores previously shipped from the district, indicated that deposits might be found which would be commercially valuable even in this remote area. To investigate the possibility, the Bureau of Mines made a reconnaissance of the Omilak area and did bulldozer trenching, diamond core drilling, and sampling at the roster prospect. Data resulting from the investigation are presented in detail in this report and are summarized in the following paragraphs.

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 M. D. Schlesinger

Experimental data for coal hydrogenation are presented to show that when a vehicle oil produced from coal is present, coal is hydrogenated to the same high conversion whether molybdenum catalyst is impregnated on the coal or intimately mixed with the slurry. Differences in product distribution could be related to the severity of operating conditions. No minimum mixing time was established, but 2 hours was sufficient. Longer periods of mixing, to 14.75 hours, had no effect on the results. The hydrogenation conditions were in the pressure range of 8,500 to 10,000 p,s,i. at 400° to 500° C. Most of the experiments were made in duplicate. The results were obtained with molybdenum concentrations of 0.01, 0.1, and 1 percent. Al the mentioned pressure range and a time at temperature of 15 to 60 minutes, coal conversions higher than 98 percent were obtained.

Jan 1, 1962

By Paul S. Lewis

The Bureau of Mines hydrogenated coals of different rank that had been irradiated with either x-rays or gamma rays. Lignite, high-volatile A and C bituminous, and low-volatile bituminous coals were exposed to l billion roent¬gens of gamma-ray radiation; specimens of high-volatile A and C bituminous coals from other sources received 6 million roentgens of X-ray radiation. Irradiated and unirradiated control specimens of those coals were hydrogenated in autoclave experiments at (6,000-p.s.i. final pressure and 400° C. with retention times of 15, 30, or 60 minutes depending on the coal rank and catalytic treatment. Comparison of results from irradiated specimens with those from the control experiments showed that the radiation had no beneficial effect on the coal. High-volatile C bituminous coal may have been affected by radiation more than the other coals. One billion roentgens appeared to reduce the amount of coal converted to liquids and gases by about 10 pct., and 6 million roentgens reduced it by about 6 pct. then catalyzed with tin. In all other cases, the conversion of irradiated coal was either reduced by as much as 4 pct. or was essentially the sank as that obtained with unirradiated coal. Irradiation during hydrogenation nay be effective for increasing the reactivity of coal and should be investigated; further work with coals irradiated prier to hydrogenation is not recommended.

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