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By R. Barany

This report contains the results of experimental work conducted by the Bureau of Mines to obtain the heats of formation at 298.15° K. of analcite, dehydrated analcite, lawsonite, anorthite, hexagonal anorthite, and leonhardite. Thermodynamic data for these minerals have applications in ceramics, extractive metallurgy, and particularly in geochemistry. Except for data on anorthite, no previous similar data existed. The present results will be a substantial aid in deriving the temperature-pressure-equilibrium relationships among these minerals. The heats of formation were determined by solution calorimetry, with hydrofluoric acid as the reaction medium. The results were expressed both in terms of the constituent oxides and in terms of the constituent elements. The heat of formation data were combined with related entropy values to obtain the free energies of formation at 298.15° K.

Jan 1, 1962

By A. Gene Collins

During recent years the interest in trace and minor constituents of oil-field water, petroleum, and their associated reservoir rocks has increased. The metals copper, nickel, lead, manganese, iron, zinc, and cadmium are not determined routinely in oilfield brine analyses. Determination of these metals and subsequent correlation of these data should yield information to aid 1n the interpretation of the origin of different waters. The methods of analyzing oilfield waters have several potential applications: (1) Aiding in the search for petroleum; (2) identifying sources of intrusive brines; (3) controlling corrosion; (4) controlling produced water; increasing knowledge of the geology of subsurface formations; (5) identifying incompatible waters in waterflooding operations; (6) increasing the knowledge of the flow of oil, gas, and water in underground formations; and (7) aiding in the identification and location of valuable mineral reserves. Some brines contain enough valuable minerals to be recovered commercially.

Jan 1, 1962

By Gerald W. Elger

This report compares the quality of zirconium metal prepared by batch reduction of zirconium tetrachloride by (1) sodium, (2) magnesium, and (3) mixtures of sodium and magnesium. Criteria for quality are based on chemical analyses and hardness testing of zirconium arc-melted from sponge. The best quality zirconium with respect to low oxygen content and hardness numbers was prepared by reaction of zirconium tetrachloride with a mixture of sodium and magnesium. It was found that this reaction could be successfully carried out by two methods: (1) addition of sodium and magnesium before the initial reaction and (2) periodic injection of sodium during reaction of zirconium tetrachloride with magnesium. The largest quantity of metal was found to be recovered from experiments in which a mixture of sodium and magnesium was used. Magnesium appeared to be a better reductant than sodium because magnesium-reduced zirconium contained less oxygen and exhibited lower hardness numbers than sodium-reduced metal.

Jan 1, 1962

By William J. Campbell

Evaluation by the Bureau of Mines of published expansion values for magnesium oxide shows significant variation in values, which may be attributed to sample variables, experimental errors, or systematic differences between measuring techniques. To eliminate the sample variable in measuring expansion, thermal expansion characteristics of a high-purity polycrystalline magnesium oxide were determined by 21 cooperating laboratories using one or more of the following techniques; X-ray camera, X-ray diffractometer, dilatometer, interferometer, and telemicroscope. All expansion values were corrected by the author to a single reference temperature of 25° C. Linear expansion was expressed as a power series in the form of the following equation. Expansion (percent) = [[ A + B (?t) + C (?t)2] ?t 104] The constants, A, B, and C, were determined by least square techniques for X-ray camera, X-ray diffractometer, and dilatometer data separately, and for combined data of all five techniques. Expansion values are tabulated from 26° C. to 1,400° C. in 2° C. intervals using constants derived from X-ray camera data. Below approximately 500° C., expansion values obtained by dilatometric and interferometric methods are significantly lower than those by X-ray methods; above 500° C., this bias decreases rapidly. Comparison of results within methods showed the least variance for X-ray camera results; dilatometer and X-ray diffractometer results have about the same variance. The average deviations, in percent, between observed and calculated expansion values among methods were approximately 10 percent from 100°C. to 300°C., 5 percent from 300°C. to 500°C., and 2 percent from 500°C. to 1,400°C. Maximum deviations were approximately twice as large in most instances.

Jan 1, 1962

By Oliver C. Fursman

These investigations were conducted to determine conditions for recovery of nickel and copper from Funter Bay, Alaska, sulfide ore and recovery of nickel from nickel-silicate ore, Nickel Mountain, Riddle, Oreg. Samples of Funter Bay cupriferous and nickeliferous pyrrhotite ore, were treated by beneficiation, roasting, electric smelting of roasted are for matte production, chlorination, leaching, and sulfatizing roasting with subsequent leaching. Funter Bay and Nickel Mountain ores were smelted together to produce matte. Total sulfide flotation, followed by magnetic separation of the tailings to recover entrained nickel-bearing pyrrhotite, resulted in the highest nickel recovery in beneficiation tests on Funter Bay are. Overall beneficiation resulted in recovery of 98.5 percent of the copper and 95.4 percent of the nickel in the concentrate that contained 3.5 percent copper and 1.7 percent nickel.

Jan 1, 1962

By E. C. Perkins

As part of a program for developing methods of using domestic titanium deposits, the Bureau of Mines investigated methods for chlorinating titanium slags prepared from titaniferous minerals by electrosmelting. Titaniferous slags were made from ilmenites in the following deposits: Valley County, Idaho; Trail Ridge, Fla.; Aiken, S. C.; and Maclntyre, N. Y.; titaniferous magnetite from Iron Mountain, Wyo., were also evaluated. The tests were made in two chlorinators, a 4-inch and a 36-inch unit. Preliminary testing was done in a 40-millimeter bench-type unit. Chlorine gas was contacted with a loose mixture of titaniferous slag and carbon at a high temperature to form titanium tetrachloride. The moving-bed system used in this work involved a downward movement of feed countercurrent to the chlorine flow, and residues continuously removed from the bottom of the reactor. The performance characteristics of these slags depended on their composition, which varied widely according to the geographic source of the ore. The results showed that all but two of the slags could be chlorinated as effectively as rutile, converting 70 to 80 percent of the titanium to the tetra-, chloride. The two slags that proved difficult were made from New York ilmenite and Wyoming titaniferous magnetite. These slags contained enough magnesium to cause clinkering, which necessitated that the bed be prematurely withdrawn before more than 70 percent of it could react. The iron content of the slags did not interfere with operating the chlorinators. The data from the 4-inch and the 36-inch units were in agreement on the relative amenability of the slags to chlorination.

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 H. L. Burmeister

This is one of a series of publications by the Bureau of Mines dealing with mining methods and costs at representative operations in the United States. The report describes all phases of the mining methods for the open-pit operation and milling practices employed at the Vermont Asbestos Mines in Lamoille and Orleans counties, Vermont. A brief history of discovery and development of these asbestos deposits is given, and the ore deposits are described. Methods employed in exploration, sampling, and estimation of tonnage and grade are outlined. A breakdown of available cost figures is summarized in the last section. All asbestos ore produced in this area has been won by the use of surface-mining methods. Two quarries, the Lowell and the "C" Area, are in operation. The quarries combined are producing and the mill is processing approximately 3,500 tons of ore per 3-shift day The average 40,000 tons of crysotile asbestos fiber produced at this plant annually accounted for 96 to 98 percent of the total fiber produced in the United States in 1958. The mine is located (fig. 1) approximately 4 miles north of Eden Mills village on the southeastern flank of Belvidere Mountain (fig. 2).

Jan 1, 1962

By J. G. Donaldson

Nickel containing less than 0.01 percent of total metallic impurities was produced at the Rolla Metallurgy Research Center of the Bureau of Mines by electrodeposition from purified electrolytes. The first report on this research4 described purification of electrolytes by selective precipitation and by liquid-liquid extraction. This second report describes a procedure: or electrodepositing high-purity nickel from electrolytes purified by passing a nickel ammine solution through a column of an ion exchange resin. The nickel electroplated directly from the ammine solution without further treatment; a titanium cathode and two platinum anodes were used. The nickel deposit was dense, smooth, and adherent, and contained less than 0.001 percent each of cobalt, copper, and iron, and spectrographically detectable traces of aluminum, magnesium, and silicon. Nonmetallic impurities in the nickel metal were carbon and sulfur, each present in concentrations of less than 0.01 percent. The results of several experiments planned to purify solid nickel salts by zone refining are also reported. These salts, after purification, were intended for use in preparing electrolytes for deposition of high-purity nickel. Results were not encouraging so that the more promising ion exchange procedure was emphasized chiefly.

Jan 1, 1962

By R. P. Maloney

Since mining operations began in 1900, Government geologists and mining men have periodically recorded the presence of the minerals of mercury and antimony in the extensive gold placer deposits near Flat in the Iditarod district of the Yukon River region, Alaska. No serious effort was made to recover the cinnabar contained in the gold placer gravels, and there is no evidence that veins of cinnabar and stibnite exposed in the placer operations (as reported by the Geological Survey) were ever explored or developed. A large monzonitic intrusive, which is the dominant geologic feature of the immediate area, is believed to be the lode source of the valuable minerals in the placer deposits. In contact with the monzonite are argillite and quartzite, metamorphic products from the Cretaceous shales and sandstones.

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 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 W. W. Agey

The Bureau of Mines examined and tested the rhodonite deposits of the Silverton lead-zinc district, San Juan County, Colo., as a possible source of domestic manganese. Exploration and development work by several mining companies and preliminary reconnaissance of the area by Bureau of Mines engineers indicated the presence of extensive manganese resources in the form of rhodonite. This report summarizes the results of laboratory beneficiation tests made on samples of different type and grade material obtained from surface and underground exposures of seven veins in the district. Surface and underground examinations revealed the presence of several prominent veins that could be traced up to 2 miles for a single vein along the surface. The principal veins average about 50 feet in width and apparently carry rhodonite to considerable depth. Underground samples were taken from the Sunnyside, Silver Queen, Washington, Independence, and Scotia veins. Samples also were taken from surface exposures of the Sunnyside Extension and Hidden Treasure veins.

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 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 Murray Jacobson

Facts obtained by the Bureau of Mines on the dust-explosion hazard in air of materials used in the plastics industry are presented for 313 samples studied in the laboratory. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum energy required for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent ignition and flame propagation, and, in some instances, on the limiting oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle shape, additives, and resin structure on explosibility are discussed. Relative explosibility of the materials is related to the ignition sensitivity and explosion severity and is denoted by an empirical index. Recognition of the degree of hazard will facilitate adoption of adequate measures for preventing ignition and explosion during manufacturing or processing.

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 Harold W. Lipper

Helium production and shipment reached new peaks in 1.361. The Bureau of Mines produced 727 million cubic feet, 13 percent more than the 1960 record, and shipped 552 million cubic feet, 16 percent more than the 1960 record. Production exceeded demand for the third successive year, enabling the Bureau of Mines to add 174 million cubic feet to the volume stored underground for future use. At the end of 1961, the total volume of helium in underground storage in the Clifside gasfield was 44-7 million cubic feet. Contracts to implement a long-range helium conservation program were completed with four companies, obligating all the contracting authority of $47.5 million a year made available by the Congress. The four companies will finance, build, and operate helium extraction plants to recover from natural gas an annual average of 3.1 billion cubic feet of helium that would ordinarily be wasted when the helium-bearing natural gas is used for fuel.

Jan 1, 1962

By J. P. Capp

The Bureau of Mines conducted field-scale experiments in underground gasification of coal with oxygen-enriched air. A path about 140 feet long was linked at the rate of LO feet per day through a coalbed hydraulically fractured with a mixture of starch gel and sand. During the best gasification period, which extended for 2-1/2 days, 785,000 std. c.f. per day of 124-B.t.u. gas was produced. In other periods the heating value at times was almost 300 B.t.u. per std, c.f,, but sustained production of such gas was not achieved. During gasification, a total of 50 tons of coal was gasified and 114 tons of coal was carbonized. Approximately 12 million B, t .u. per foot of nominal path was recovered at the surface.

Jan 1, 1962

By Robert Hall

The Lynch Creek beryllium-tungsten prospect was investigated as part of the domestic beryllium resource studies by the Bureau of Mines. This prospect is in the Birch Creek mining district, Lander County, Nev., 9 airline miles south of Austin. A tungsten mine was operated intermittently from 1952 to 1957. Beryl was identified in the pegmatite dikes in 1960, and the lode claims were relocated. No beryl has been produced. Rocks in the area are Paleozoic sediments2 cut by pegmatite and aplite dikes and quartz stringers. Beryl occurs in random pockets, as disseminations throughout the dikes, and in occasional pockets in the quartz stringers.

Jan 1, 1962