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By R. Barany

The heats of the glass-crystal transformation of nepheline (Na0.7794K0.2206AlSiO4) and wollastonite (CaSiO3) and the heat of formation of nepheline at 298.15° K were determined by solution calorimetry. For the glass-crystal transformations, the heat values were -9.0 ± 0.3 kcal/mole for nepheline and -8.1 ± 0.2 kcal/mole for wollastonite. The heat of formation of nepheline was -34.8 ± 0.6 kcal/mole from the oxides and -501.0 ± 0.5 kcal/mole from the elements.

Jan 1, 1966

By P. C. Good

Work was done to determine conditions necessary for efficient electrodeposition of aluminum from fused chloride electrolytes. Aluminum was deposited from a molten chloride salt electrolyte over a temperature range of 150° to 750° C. At lower temperatures in a heat-resistant glass cell, aluminum was deposited on stainless steel and on aluminum cathodes. The deposit was recovered in the form of light, feathery dendrites that could not be consolidated. At 750° C, molten aluminum was deposited at cathode current efficiencies as high as 90 to 100 percent on titanium diboride cathodes and in molten aluminum cathodes. Nitride-bonded silicon carbide was the best cell material, although porcelain was also used. The electrolyte consisted of a mixture of sodium and potassium chlorides in 1 to 1 mole ratio, containing aluminum chloride in concentrations ranging from 2 to 30 weight-percent in cells holding up to 1,000 grams of electrolyte. Generally favorable results were attained in studies made at temperatures greater than the melting point of aluminum.

Jan 1, 1966

By J. W. Stevenson

The Bureau of Mines investigated the influence that atmospheric pressure changes exert in a gassy coal mil on a ventilating air current with a system of bleeder entries. During the season when abnormal barometric fluctuations usually occur, recording instruments monitored the air current ventilating an active coal-producing area. It HL he rate of coal production caused a more significant change in methane concentration than did barometric change. The hazard that accompanies methane release due to expansion of the gob gases during atmospheric lows was minimized by the effective bleeder system.

Jan 1, 1966

By Willis Beckering

The Bureau of Mines designed a cell having four variable compartments in series to facilitate analysis of multicomponent mixtures. Use of the cell considerably decreases the time required for differential absorption analyses. A solution of a major component is placed in each compartment, and the light absorbed by each of these components is varied by increasing or decreasing the path length of the appropriate cell. Simple calculations then establish the amount of the component present. In analyzing unknown mixtures, compensation is made for compounds known to be present, and the differential spectrum representing components not accounted for is recorded and analyzed.

Jan 1, 1966

By Albert F. Baker

Techniques were developed and circuitry was assembled for measuring the total and volume resistances to the flow of electric current through solid specimens of anthracite. The two-, three-, and four-terminal test methods demonstrated the extreme sensitivity of resistivity to differences in anthracite characteristics and showed response to changes resulting from variations in structure, temperature, and moisture content.

Jan 1, 1966

By D. G. Kesterkel

Low-melting thoriurnrbase binary alloys or metal solutions were prepared by two different techniques involving the electrolysis of ThO2 dissolved in fluoride melts. Experiments were performed at 950° to 1,250° C using electrolytes containing ThF4 and various alkali and alkaline earth fluorides. In the first method, electroreduction of ThO2 and deposition of thorium on a nickel or iron cathode formed a molten alloy that dripped off and collected on the bottom of the cell, or in a tungsten cup. An electrocodeposition technique was used to prepare thorium-base alloys or solutions containing nickel, iron, chromium, or manganese. Electrolytic reduction of the component metal oxides and simultaneous deposition of the two metals on a tungsten cathode yielded a liquid alloy product. Complementary experiments were performed on the fused fluoride electrowinning of dendritic thorium from Th02 at 1,075° to 1,200° C in which thorium crystals were recovered and arc-melted into buttons. Major contaminants were aluminum, carbon, copper, iron, oxygen, and silicon, totaling 0.2 percent.

Jan 1, 1966

By Rogers F. Davis

The Bureau of Mines developed a new method for the determination of oxides of nitrogen in diesel exhaust gas. The procedure, a modification of the Saltzman method, uses a NO2 absorbent for the diesel exhaust gas; the colorless absorbent becomes purple on contact with N~. When used properly this procedure gives satisfactory results in 2 hours, whereas the standard phenoldisulfonic acid method required approximately 8 hours. The new method is not satisfactory for determination of oxides of nitrogen in the overrich fuel to air ratio range.

Jan 1, 1966

By Paul V. Mullins

Review and evaluation of all available data on the vapor pressure of car-bon dioxide at the ice point, including previously unpublished results obtained by the Bureau of Mines, are presented. Suggested corrections and adjustments to all the data yield an average value of 26,136.4 mm mercury. Indicated agreement is within plus 1 part in 8,000 to minus 1 part in 11,000. A novel pressure bomb in which a sample of pure carbon dioxide is placed and sealed by a diaphragm fluid separator and its use as a reference pressure standard for extended and repeated use in the calibration of deadweight gages is described.

Jan 1, 1966

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions4 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1966

By C. J. Walker

The Bureau of Mines undertook a theoretical and laboratory study to determine the feasibility of using ethylene as a tracer for natural gas in underground gas-storage reservoirs. The study indicated that ethylene was a useful gas tracer in underground gas storages. Tracer losses were not excessive. Laboratory tests were conducted at pressures as high as 500 psia in both wet and dry consolidated-sandstone cores, evaluating tracer loss with gas blends containing natural gas with different concentrations of ethylene tracer. Under certain conditions losses were less than 17 percent.

Jan 1, 1966

By H. C. Fuller

A method was devised and developed by the Bureau of Mines for decomposing manganese sulfate at significantly lower temperature than that required by the conventional procedure of using heat alone. This technique, called the partial reduction method, effected decomposition at 700° to 800° C, as compared to 900° 1,000° C normally required. The process consisted of heating, in the absence of oxygen, a mixture of manganese sulfate and a controlled quantity of a reducing agent. The suitability of commercial-type equipment was tested in laboratory-size models of an externally heated rotary kiln, a r bbled muffle-hearth furnace, and a fluidized-bed reactor. The rabbled-hearth furnace gave the best results with the least operating difficulty produced a gas containing more than 80 percent SC and eliminated 96 percent of the sulfur when coal was used as the reductant. Sintering of the powdery decomposition product produced an agglomerate containing, in percent, 63.6 Mn and 0.4 S.

Jan 1, 1966

By R. L. Hopkins

The work described was performed to determine whether sulfur compounds of the thienothiophene class occur in crude oil. The presence or absence of various classes of sulfur compounds in crude oils is of interest and value to petroleum science. The Bureau of Mines, for the first time, identified hydro-carbon products of desulfurization that point directly to the identity of two individual thienothiophenes, namely 3-methylthieno[2,3-b]thiophene and 2-meth-ylthieno[3,2-b]thiophene, in Wasson, Texas, crude oil. These identifications, described in detail, were accomplished using microdesulfurization, mass spectrometry, and gas-liquid chromatography.

Jan 1, 1966

By R. L. Hopkins

Fifteen alkyl cycloalkyl sulfides and three dicycloalkyl sulfides were synthesized to provide reference compounds in the search for these classes of sulfur compounds in crude oils. In synthesizing sulfides by alkaline alkylation the order in which the reactants were added was shown to determine the yield and purity of the product.

Jan 1, 1966

By A. J. Forney

This report summarizes the findings of methods of treating caking coals in a fluid bed to destroy their caking properties. In batch tests it was found that several coals, including those with a free-swelling index greater than 8, could be decaed at temperatures from 400° to 425° C with a fluidizing gas composed of inert gas or steam containing 0.2 percent oxygen and a minimum residence LS,-;,' of 5 minutes. When treatment decreased the free-swelling index from about 8 to 1-1/2 or lower, the resulting treated coal was noncaking. In a continuous unit with continuous feed and discharge of coal, slightly more severe conditions were required to decake the coal. For 18- to 100-mesh coal a temperature of 430° to 440° C and an oxygen-to coal ratio of 0.4 cubic foot of oxygen per pound of coal feed was necessary. Finer mesh sizes required lower oxygen-to-coal ratios. In tests using air only as the fluidizing medium and treatment temperatures well below the softening range, the caking properties of 150- to 200-mesh coal were destroyed in 30 to 40 minutes of residence time at 200° C. Coarser sizes of 18 to 48, 48 to 100, and 100 to 150 mesh required longer residence time.

Jan 1, 1966

By Leo A. Schrider

This report analyzes the successful low-pressure gas drive in the Keener sand of the Bonds Creek oilfield, Pleasants and Ritchie Counties, W. Va.) and predicts its future performance. Core analysis from two wells and electrical and radioactivity logs were used to evaluate the reservoir characteristics. Production records over a 37-year period indicate that over 240,000 barrels of oil have been produced from the Keener sand by low-pressure gas injection. Decline-curve analysis shows that 165,000 additional barrels should be recovered from 108 acres of productive sand by continuing this secondary-recovery method.

Jan 1, 1966

By Charles M. Mason

The Bureau of Mines evaluated equipment and procedures for drop-weight testing of explosive liquids as prescribed by Test 4) a widely used method. It was demonstrated that partial ignitions, originally designated as negative results, should be designated positives; it was also shown that wear or erosion of the sample cups and the type of mount used for the apparatus had important effects on the results. Relative sensitivity as measured by Test 4 was found to vary slightly with temperature. The Bureau also designed a fixed 2-kg weight and associated electromagnetic release, which subsequently were incorporated as standard in a revision of Test 4. The original concept that the test involves only adiabatic compression was found to be an oversimplification; an alternate mechanism for the initiation process is proposed in which due consideration is given to the effects of cavitation and microjets.

Jan 1, 1966

By Robert M. Doerr

The oxidation kinetics of Ni-Y alloys in the range 0.04 to 8 weight-percent Y, and of high-purity Ni, were compared by the use of a sensitive volumetric apparatus. The reactions followed approximately the parabolic rate law; for oxidations in 02 at 0.5 atm and 1,200° C, the parabolic rate constant was about 0.37 + (0.064) (Y-2.11) mg cm-2 min-1/2, where Y represents the weight-percent Y in the alloy. Internal oxidation of Y occurred in the alloy specimens and the resultant Y203 particles, which were in patterns related to the eutectic structure of the alloys, served as markers showing that the subsequent oxidation of the surrounding Ni was by inward diffusion of O. The scale consisted in each case of NiO, but the inner parts of the scale on the alloy specimens included the patterned Y203 particles. The thicknesses of the inner parts of the scale depended directly on the Y concentration, and the thicknesses of the Y2O3-free outer parts of the scale were inversely related to the Y content of the alloys. There is thus a relationship between the thickness of the outer part of the scale and the protectivity of the scale. Outward diffusion of Ni and inward movement of 0, from the inner boundary of the Y2O3-free part of the scale, is proposed as a mechanism for these results.

Jan 1, 1966

By A. L. Service

Idaho has nearly 6 billion tons of potential sources of phosphorite, 10 to 31 percent P2O5' above and within 100 feet below entry level, the largest potential of any State in the United States. In 1963 Idaho ranked third after Florida and Tennessee in total mine and marketable production of phosphate rock; Montana ranked fourth. This report describes phosphate deposits, mines, and prospects in 10 districts covering most of the Idaho phosphate field. All mine production of phosphate rock in Idaho comes from surface mines and is processed to phosphate fertilizers, phosphoric acid, and elemental phosphorus. Producing districts are Fort Hall (Gay mine), Trail Creek (Conda and Ballard mines), and Crow Creek (Georgetown Canyon mine). FMC Corp. and J. R. Simplot Co. at Pocatello have the largest elemental phosphorus and fertilizer production facilities, respectively, in the State, followed by Monsanto Co. and El Paso Natural Gas Products Co. (formerly Central Farmers Fertilizer Co.). The only other major phosphate processing plant in the State is the phosphoric acid and phosphate fertilizer complex at Kellogg operated by the Bunker Hill Co. In 1963 a plant was constructed and put on line at Monsanto, Idaho, to recover vanadium from ferrophosphorus produced by electric furnace operations in the area. El Paso Natural Gas Products Co. completed construction of a fertilizer and phosphoric acid plant near Conda in 1965. There is a small fertilizer plant producing phosphate fertilizers for local consumption in Soda Springs.

Jan 1, 1966

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By H. J. Coleman

Knowledge of the types of naturally occurring sulfur compounds in petroleum is of both theoretical and practical interest to petroleum chemists and geologists. This knowledge has been extended by the identification of 77 sulfur compounds, including 36 thiols, 23 chain sulfides, and 18 cyclic sulfides in a 111° to 150° C boiling range distillate of Wasson, Texas, crude oil. The characterization procedure used in separating and identifying these compounds included isothermal distillation, vacuum fractionation, liquid-solid chromatography (alumina adsorption), chemical treatment, gas-liquid chromatography, microdesulfurization, and infrared analysis. The procedural steps described represent a systematic method of sulfur compound analysis considered applicable for determining the nature and concentration of the sulfur constituents present in any straight-run petroleum distillate of the above-boiling range.

Jan 1, 1966