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By William E. Young

There are many large rhodonite-bearing veins containing manganese in the Eureka-Animas Forks area of the San Juan Mountains in Colorado. The Sunnyside vein is the largest known vein in the area. As observed on the surface, the vein is mineralized over 8,000 feet and attains a maximum width of 200 feet. The average width of the vein and its branches and ramifications is 58 feet in the area that was mapped in detail. The weighted-average analysis of surface and underground samples from the northeastern extension of the Sunnyside vein is 8 percent manganese. Most other known veins in the area have a similar manganese content. The Hidden Treasure vein lies southeast of the Sunnyside-No Name-Mastadon vein. The weighted average of the analyses of surface and underground samples from this vein is 13 percent manganese. Exposures of the Scotia-Silver Chord vein are visible over a strike length of 4,000 feet on Treasure Mountain. Diamond-drill holes show that the vein contains 10 percent or more manganese to a depth of 400 feet. The vein has an average width of 28 feet. The Independence vein is exposed on the surface for a distance of 600 feet and has an average width of 6 feet. Three cut samples taken across the vein had an average content of 20.7 percent manganese. Sampling of the outcrops of eight veins in the Placer Gulch area also indicates manganese. Numerous other veins cropping out in the surrounding area are similar to the outcrop of the Sunnyside vein system mineralogically and are worth investigating.

Jan 1, 1966

By W. H. Oppelt

Two exploratory gasification tests of limited duration were made at Dorsten, Germany, with strongly coking Pittsburgh-bed coal in a fixed-bed pressure gasifier. To reduce the coking potential of the Arkwright coal, ash refuse from the gasification of Dorsten (Leopold) coal was added to pre-pare coal-ash mixtures which contained nominal 20 and 30 percent ash. Major adjustments in principal process variables at the beginning of the tests resulted in wide fluctuations in the rate of gas production, gas offtake temperature, and carbon dioxide concentration in the gas. Because a higher steam-to-oxygen ratio was used in the tests than was customarily employed for routine operation, gas production was lower, and steam and oxygen consumption was higher. After operating conditions had been improved, the results of a 12~-hour-long test with addition of sufficient ash refuse to obtain a nominal 30 percent ash concentration indicated that operation is feasible with this coal mixture using a fixed-bed pressure gasifier equipped with a rotating coal distributor and stirrer.

Jan 1, 1966

By E. P. Ferrero

Analyses of 38 crude oil samples from 25 fields in Algeria, Libya, and Nigeria are presented in this report. The 38 crude oils are listed alphabetically by country and field. Also shown are the geographic and geologic sources of the samples analyzed, the companies that supplied the samples, the general characteristics and analytical and computed data, and the production for the fields from which the samples were obtained.

Jan 1, 1966

By James A. West

COUNTRIES of the Near East, with the world's largest and insist prolific petroleum resources, produced nearly 277 percent of the world's estimated total output of crude& oil in 1964 and accounted for about 60 percent of world exports of this commodity. Although petroleum largely dominated the mineral industry of tine area, production of antimony, chromium, copper, mercury, boron, potash, and phosphate rock was of world significance. Production of crude oil in Near East countries reached a record high of 7,520,000 barrels per day in 1964, an increase of nearly 11 percent over that of 1963. Kuwait maintained its position as the leading producer, accounting for almost 28 percent of the area's output. Saudi Arabia, Iran, and Iraq followed with 22.5, 22.2, and 16.5 percent of total area output, respectively. Despite record production, the Near East, proved crude oil reserve remained in excess of 211 billion barrels, or more than two-thirds of the estimated world proved crude oil reserve.

Jan 1, 1966

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966

By Harry R. Johnson

Laboratory experiments were conducted to study the carbon deposition characteristics of a high-gravity, paraffin-base crude oil. The results of these experiments indicate that a fuel supply adequate to initiate a combustion wave can be deposited in high-gravity-oil reservoirs. These results are significant because there has been considerable doubt whether oils over 35° API gravity are able to deposit sufficient fuel. Considered in these studies were the effects of air flux, temperature, initial oil saturation, and time on carbon deposition. Conditions that maximized carbon deposition in the laboratory and an understanding of the nature of carbon formation are shown by graphical interpretation of the data. Statistical techniques were used to design and analyze the results of the retort tests. For the same amount of laboratory work, this approach yields more information about the systems that were studied than the classical method of research presently used in many laboratories. In addition, the accuracy of calculating the effect of each variable on carbon deposition is twice that of the classical approach. This paper develops the statistical approach to research without complex mathematics, thus enabling the reader to grasp the concept of how statistics can be applied to study many complicated problems.

Jan 1, 1966

By J. P. Morris

A diphenyl ether calorimeter for measuring high-temperature heat contents of ferrous alloys and iron-and steelmaking slags was constructed and calibrated with specimens of molybdenum, alumina, and platinum that were heated to temperatures ranging from 1,720° to 1,875° K. The standard deviation of the calibration measurements was 0.37 percent. By measurements of the enthalpy of delta and liquid iron, the heat of fusion of iron was found to be 3,298 ±100 cal per mole.

Jan 1, 1966

By R. L. Benner

The Bureau of Mines investigated the ZnO-Fe2O3-Fe3O4 system at 1,000°, 1,300°, and 1,400° C, with oxygen pressures between 1.0 and lx10-4 atmospheres. The results, divided into the thermodynamic properties as related to the spinel structure, and the thermodynamic properties as related to zinc concentrate roasting, were used to calculate the activities of ZnO, Fe2O4, and Fe3O4 within the spinel solid solution region of the ternary system, and the pseudo-binary activities of ZnFe2O4 and Fe304. The activities of both systems show large positive deviations from Raoult's Law, especially at high Fe3O4 concentrations. The free energies, the enthalpies, and the entropies of mixing for the binary system were calculated from the binary activities, and the entropies of mixing were compared with two statistical models, one representing an ideal solution, and one representing the mixing of a normal with an inverse spinel. The binary entropy of mixing seemed to be better represented by the latter statistical model, indicating that the tetrahedral and octahedral cations of the reactants tend to remain in the product, even at the high temperatures of the study. This comparison also indicated that the cations of the components are the major contributing factors to the thermodynamic properties.

Jan 1, 1966

By Jr. Taylor

The following heats of solution have been measured in 1.160 molal H2SO4 at 25° C: AH298, kcal./mole Be(c) + 77.44(H2SO4?47.849 H2O) H2(g) + BeSO4 (soln) -92.83 ± 0.11 BeSO4 ?(c) + 77.44 (H2SO4?47.849 H2O) BeSO4(soln) -16.45 ± 0.02 BeSO4?2H2O(c) + 77.44(H2SO4?47.849 H2O) BeSO4?2H2O(soln) -5.395 ± 0.019 BeSO4?4H2O(c) + 77.44 (H2SO4?47.849 H2O) BeSO4?4H2O(soln) 1.513 ± 0.010 Combining these data with other experimental results and data taken from National Bureau of Standards information yielded the following heats of formation at 298° K:

Jan 1, 1966

By W. L. Falke

Procedures in which manganese compounds are reduced and the metal is volatilized and selectively condensed, a hitherto neglected area, were investigated. More than 95 percent of the manganese was recovered from high-melting-point ores whether vacuum volatilization or atmospheric pressure volatilization was used, but neither process is economically attractive under present price-cost conditions.

Jan 1, 1966

By R. E. Cumings

The Bureau of Mines made electrorefining tests in inert-atmosphere, molten salt cells to develop methods for the preparation of high-purity molybdenum. Seven of the electrolytes investigated were suitable for the preparation of refined metal. The electrolytes were composed of molybdenum chloride in alkali chlorides or mixtures of alkali and alkaline-earth chlorides. An electrolyte composed of potassium chloride and potassium hexachloro-molybdate was selected for a larger scale, more detailed study on the basis of its ease of preparation, its ability to retain the molybdenum salt, and the type of deposits obtained. High-purity molybdenum in the 99.99-percent-purity range was successfully prepared as dense plate up to 80 mils thick and as dendritic crystals. The temperature of electrolysis and the current density were major factors in determining whether plate or dendritic crystals of molybdenum were obtained.

Jan 1, 1966

By L. J. E. Hofer

THIS BULLETIN analyzes and summarizes research at the Bureau of Mines dealing with the preparation, properties, and reactions of iron carbides in the period 1948-60, part of which was sponsored by Wright Air Development Laboratories. The objective was to develop better catalysts for the synthesis of methane and higher hydrocarbons from hydrogen and carbon monoxide. The investigations resulted in the first adequate characterization of epsilon iron carbide, which later proved to be an important intermediate in the tempering of martensite in steel. At temperatures near 170° C, the carbon in carbon monoxide reacts nearly quantitatively with finely divided alpha iron to form an iron carbide in which the metal atoms occupy the positions of the close packed hexagonal arrangement with lattice parameters of ao=2.754 A and co=4.349 A. The carbide has a composition within 2 atomic percent of that required for the formula Fe2C, a Curie point of about 370° C, a specific magnetization of 160.4 ergs per gauss-gram Fe at 50° C, and a ferromagnetic moment of 1.70 Bohr magnetons. Epsilon iron carbide can be converted to chi iron carbide by thermal treatment at 343° C for about 70 hours. The chi iron carbide so formed has a Curie point of 247° C, a specific magnetization of 142.5 ergs per gauss-gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 5.5 Bohr rnagnetons per iron atom. Direct synthesis of this carbide from carbon monoxide at 240° C indicates a composition within 7 atomic percent of that required for Fe2C. Chi iron carbide can be converted to cementite at 550° C in about 315 minutes. The theta iron carbide so prepared has a Curie point of 210° C, a specific magnetization of 147.3 ergs per gauss gram Fe at 50° C, a ferromagnetic moment of 1.72 Bohr magnetons per iron atom, and a paramagnetic moment of 3.9 Bohr magnetons per iron atom. Pure chi iron carbide reacts to form theta iron carbide by the elimination of free carbon. In the presence of an excess of free iron in intimate contact with the carbide, chi iron carbide reacts with the free iron to form theta iron carbide. The second reaction proceeds at an appreciable rate at 320° C and can be used to snythesize finely divided theta iron carbide with no free-carbon impurity at low temperatures. The ease of the reaction in the presence of free iron suggests that chi iron carbide is an intermediate in the tempering of epsilon iron carbide to theta iron carbide as it proceeds in steels. Experiments on carbon steel show that the magnetic moment of the iron atoms in martensite is about 2.2 Bohr magnetons per atom, a value approximately the same as that of the iron atoms in alpha iron. The Curie points of epsilon iron carbide, chi iron carbide, and theta iron carbide were found -in various specimens of tempered steel to be 10° to 20° C lower than normal values. This shift is probably the result of manganese in solid solution. Preparations of various compositions of epsilon iron carbonitrides show many effects of extensive isomorphism between epsilon iron carbide and epsilon iron nitride. The action of carbon monoxide on finely divided alpha iron at 400° C results in free carbon deposits containing filaments about 0.1 micron in diameter and several times as long. The filaments are characterized by nuclei of dense material located midway from each end of the filament. Although carbiding to near completion at 240° C over periods of about 300 hours produces a preparation containing no appreciable percentage of epsilon iron carbide, very brief periods of carbiding of the order of a minute result in the formation of detectable epsilon iron carbide even at temperatures as high as 325° C. The data indicate that epsilon iron carbide is an intermediate in the formation of chi iron carbide during its formation from carbon monoxide in the gas phase. Attempts to convert cementite to chi iron carbide by cold work increased the Curie point but did not change the X-ray powder diffraction pattern.

Jan 1, 1966

By L. J. E. Hofer

The Bureau of Mines determined rates of adsorption and desorption of methane as a function of particle size and temperature, using coals from the Pocahontas No.3 seam (lvb) from the Bishop mine of western Virginia, and the Pittsburgh seam (hvab) from the Pursglove No. 15 mine of northern West Virginia. For a given coal sample and temperature, the rate curves for adsorption and desorption are essentially the same when expressed on a fractional approach to equilibrium basis. The rates of adsorption and desorption increased eightfold as the particle size was decreased from 6-8 to 270-325 mesh per inch. The adsorption process appears to be diffusion controlled. Rate of sorption processes increased with increasing temperature; however, the amount adsorbed at equilibrium decreased.

Jan 1, 1966

By Henry C. Meeves

The Bureau of Mines, between 1956 and 1963, examined 18 major pegmatite districts in Arizona, Colorado, New Mexico, South Dakota, Utah, and Wyoming to evaluate their content of beryllium, a material in short domestic supply that has become increasingly important to modern industry. This examination report includes the salient statistics on the production of pegmatite minerals other than quartz and feldspar; and brief descriptions of 170 specific pegmatite deposits.

Jan 1, 1966

By George H. Holmes

The water situation in Nevada mineral and related industries is described in this report. It contains information on the sources and adequacy of supply to current operators, requirements and uses, quality and costs, geography, hydrography, precipitation and evaporation characteristics, and Nevada water laws. Also, information is given on the water requirements of one public utility powerplant, and the source and consumption of water in four major cities. Water distribution at 24 operations is shown on schematic waterflow diagrams. The mineral industries of Nevada in 1962 used 8.6 billion gallons of nee' water and reused 3.8 billion gallons for a total usage of 12.4 billion gal¬lons. The copper industry was the major water user. The 1962 value of all mineral production in Nevada was $85.5 million. The large amount of water required to maintain this high production is obtained principally from ground-water sources in alluvial valleys and the permeable rock formations of some mountain ranges. Some water is also obtained from perennial streams and springs. Sources of water utilized by existing industry ore near most mineral industry operations; however, seven companies are forced to pipe water distances ranging from 2 to 8 miles. Although water supplies of presently operating companies are adequate at most operations, several companies resort to large-scale reuse of water as a matter of conservation and economics. Acquisition of water by new operators is possible but takes considerable negotiation. Water rights, surface and underground, are controlled by the State. The quality of the water is satisfactory for most purposes. Analyses of 19 samples, listed in the appendix, show the range in water quality at various plants throughout the State. Costs of delivering new water to current operations range from 2 to 26 cents per 1,000 gallons with an average of 10 cents per 1,000 gallons for power and maintenance. No firm costs for recirculating water were available; estimated costs range from 1.5 to 2.5 cents per 1,000 gallons. The mineral-product value of the entire Nevada mineral industry in 1962 was equivalent to $10 per 1,000 gallons of new water and $26 per 1,000 gallons consumed. Projection of the 1962 water requirements of the Nevada mineral industry indicates that the demand for new water will increase from 8.6 billion gallons in 1962 to 11.9 billion gallons in 1980, a 43-percent increase. Water requirements ill the year 2000 are estimated as 14.8 billion gallons, an increase over 1962 water demand of 78-percent.

Jan 1, 1966

By E. J. Kloos

The Bureau of Mines evaluated all previously approved gas masks to determine their ability to provide respiratory protection against each of the following six selected amines: ethylenediamine, diethylamine, n-butylamine, ethylamine, methylamine, and hydrazine. Minimum requirements were a 24-minute service life at a flow rate of 64 liters per minute (32 liters per minute for hydrazine) and an amine concentration of 1.0 volume-percent (0.5 volume-percent for hydrazine). The three masks meeting these requirements were the LG4, Willson Products Division, The Electric Storage Battery Co.; the GMD-SS, Mine Safety Appliances Co.; and the 084-PHOV-R, Acme Protection Equipment Co.

Jan 1, 1966

By Robert S. Warfield

Eight samples of high-volatile bituminous coal, each large enough for a study of its coking properties by the Bureau of Mines, were obtained from a location along the Kukpowruk River, Arctic Northwestern Alaska. Bench scale and pilot plant carbonization studies with several patterns of coal blending were conducted. The data from these tests were compared to data from similar tests on a coking blend used by the Kaiser Steel Corporation at Fontana, Calif. The majority of the samples representing the 20-foot seam was found to have significant coking properties, and produced coke approaching metallurgical quality when blended with selected coking coals. Although oxidation effects were evident in the samples representing upper portions of the seam, it appears that the whole seam could be used.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted petrographic classification and flotation studies to determine if acid-grade concentrates could be obtained from individual and composite samples from the Meade Peak member of the Phosphoria Formation, Idaho. The petrographic studies were made to determine the effect of compositional features on concentration of phosphates. The ore grade, ovule size, and clay content were the main features affecting grade and recovery of phosphate. Flotation results on roasted ore with a tall oil emulsion scheme showed that beds containing over 10 percent P2O5 could be beneficiated and composited with the two high-grade beds to produce a composite concentrate containing 31.9 percent 05 at 84.3 percent recovery. Treatment of these intermediate-grade phosphate beds by flotation increased ore reserves over 200 percent and increased the ore-to-waste ratio in the ore zone from 1:5.7 to 1:0.27.

Jan 1, 1966

By Paul M. Buttermore

As part of a national canvass of water use the Bureau of Mines compiled data on water requirements in the petroleum and natural gas industries for the calendar year 1962, specifically in well drilling, secondary-recovery operations, and natural gas processing plants. Total new water use in the petroleum industry of the United States, excluding refining, was 5.3 billion barrels. Secondary-recovery operations and natural gas processing plants required about 2.5 billion barrels of new water input; each of these requirements was about eight times greater than that for well drilling. Total use, including recirculated water, was 45.3 billion barrels of which 3.4 billion barrels was consumed. The greatest use of recirculated water was for natural gas processing, amounting to 38.2 billion barrels. Projections of total water use show that by 1975, 75.4 billion barrels will be used by the petroleum industry, of which 10.2 billion barrels will be new water. By 1985, the total use requirement will be 92.8 billion barrels, of which 13.1 billion barrels will be new water.

Jan 1, 1966

By Erie C. Donaldson

Gas-displacement tests were made in Berea Sandstone and Arbuckle Lime-stone cores to determine the relative permeabilities to gas, oil, and water for two-and three-phase dynamic systems. Three-phase relative permeabilities were obtained by displacing oil and water from the core with gas and measuring the flow rates of the three fluids simultaneously. It was found that relative permeabilities to fluids in a porous medium are affected by the saturation distributions of other fluids in the medium as well as by their own saturation distributions.

Jan 1, 1966