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By R. T. Johansen

The wettability of petroleum reservoir materials by water and crude oil has been recognized as an important factor in determining waterflood behavior. The problem of simulating and studying reservoir conditions and characteristics, to produce laboratory results congruous with field experience, has been examined by many methods. (1, 2, 3, 4).4/ The most generally accepted approach to this problem is determining wettability of the porous medium by imbibition methods; or, after solvent extraction, predetermining the wettability of the samples by coating the surface of the medium to render it preferentially oil-or water-wet (3, 5). The emphasis of wettability studies has been placed on the characteristics of the reservoir materials with little consideration being given to the fluids themselves. Therefore, the wetting tendencies of crude oils have been investigated by a recently developed method (6). Imbibition and the more general phenomena of capillary pressure are the most direct ways to measure wettability. The simplest type of capillary pressure observations involves the use of an interfacial-tension capillarimeter, which does not produce as separate values either interfacial tension or contact angle. Actually, these quantities do not have independent significance in reservoir engineering, and the property of wettability they are intended to evaluate is given, immediately by capillarimetric measurements.

Jan 1, 1961

By Alla D. Mah

Relatively pure aluminum nitride (AIN) recently has been prepared in sufficiently large amounts to permit a variety of experimental studies.4/ Several mechanical and chemical properties have been investigated, which show that this substance has good potentialities as a container for liquid aluminum, gallium, and boric oxide. The present work by the Bureau of Mines was undertaken to obtain thermo-dynamic data pertinent to the calculations regarding thermal stability and reactivity of aluminum nitride. The following measurements were made: (1) determination of the heat of formation from the elements at 298.15° K.; (2) determinations of the heat capacity over the temperature range 51° to 298.15° K. and the evaluation of the entropy at 298.15° K. therefrom; and (3) determinations of the heat content over the temperature range 298.15° to 1,800° K. These data are combined to obtain free energies of formation from the elements between 298.15° and 2,000° K.

Jan 1, 1961

By Lowell Stroud

Since 1929, the Helium Activity of the Bureau of Mines has operated a helium-extraction plant at Amarillo, Tex. The natural gas that supplies this plant is obtained from the Cliffside geologic structure 12 miles to the northwest and over the years, has become known simply as "Cliffside gas," There is need for published data on the low-temperature phase equilibria of helium-bearing natural gases. To date, little information has been published on the equilibrium phase compositions, solution of helium in condensed natural gas, condensation characteristics, or equilibrium vaporization coefficients for methane, nitrogen, and helium in helium-containing systems. A windowed phase equilibrium apparatus (8)6 was used to obtain 105 equilibrium samples, representing 35 experimental conditions of condensed Cliffside gas at pressures of 100, 200, 300, 400, and 500 p.s.i.a. and temperatures from 0° to -270° F. Data on equilibrium vapor-liquid composition for Cliffside gas are presented in both tabular and graphic form and are discussed in detail to show their relationship to certain criteria that must be met to effect an efficient separation of helium from natural gas by means of low-temperature processes. Facts about condensation characteristics and solution of helium in the liquid phases are included, The important relationship of these two factors in decreasing the percentage of total helium lost by solution in the liquid phase is discussed.

Jan 1, 1961

By John Ward Smith

This paper describes and evaluates a method that the Federal Bureau of Mines used to determine the ultimate composition of the organic material in 10 samples of oil shale from the Mahogany zone of the Green River formation in Colorado and Utah. Since interest has centered on the Mahogany zone, the richest section of the deposit, these 10 samples were chosen to provide a broad representation of this zone with the objective of obtaining generally valid ultimate composition values. The most probable organic composition for the Mahogany zone and the 95-percent confidence limits for each component average (in weight-percent of organic material) are: Carbon 80.5 ± .4 Hydrogen 10.3 ± .1 Nitrogen 2.4 ± .1 Sulfur 1.0 ± .1 Oxygen 5.8 ± .5 As only minor variations in composition were observed, the organic material of this particular bed is quite similar over a wide geographic area.

Jan 1, 1961

By D. P. R. Smyth

The limestone reef reservoir at Swan Hills consists essentially of a "buildup" of successively smaller atoll-like layers. Precipitation of calcium carbonate within the lagoonal area of each layer essentially kept pace with growth of the outer organic lattice. Within the reef mass, six de-positional environments characterized by specific suites of fossils (or fossil fragments) and associated limestone textures are recognized as follows: ( 1) Aerated moderately agitated water of normal marine salinity (widespread shelf or submerged reef-built platform). Thamnopora-type corals, Amphipora, "pancake" stroma-toporoids, crinoids, articulate bra-chiopods, rare rugose cup corals, and ostracods occurs in light gray-buff skeletal microgranular limestone of low permeability. (2) Semi-stagnant quiet water of normal marine salinity (leeward side of reef). Crinoids, articulate brachio-pods, rare thamnopora-type corals, Amphipora, pancake and bulbous stromatoporoids, rugose cup corals, ostracods and gastropods occur in impermeable dark brown argillaceous skeletal calcilutite with thin black bituminous shale beds and rare dark chert nodules.

Jan 1, 1961

By Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961

By D. A. Wilson

Several promising systems for selectively oxidizing the iron in an iron-tin alloy commonly called "hardhead" were investigated in a research project conducted to devise a method for recovering tin from this troublesome alloy. A satisfactory oxidation method was developed and tested successfully on melts of 2,000 grams. Molten hardhead (near 1,080° C.) was blown with air to oxidize iron and leave tin in the reduced state. Recovery of available tin was 96 to 98 percent. Tin products contained 2 to 0.1 percent iron which was reduced to 0.06 percent by filtration at 250° C. Iron oxide formed during oxidation was absorbed by a fluid flux cover composed of 43 percent silica, 17 percent burned limestone, and 40 percent fused borax. Less successful but nevertheless promising results were obtained with mixtures of steam and hydrogen which were sufficiently selective at temperatures between 600° and 950° C. but did not result in complete oxidation of iron. Carbon dioxide-carbon monoxide mixtures also oxidized iron selectively but incompletely. Both stern and carbon dioxide systems produced sufficiently encouraging results to additional research on these systems.

Jan 1, 1961

By Donald J. Frendzel

The post-World War II expansion of the Soviet petroleum industry has established the U.S.S.R. as a major oil-producing nation and has led to Russian reentry into the international petroleum trade. The rapid growth of Soviet petroleum production will allow the U.S.S.R. to displace Venezuela as the world's second largest oil-producer in 1960 and to narrow further the gap between Soviet and U.S. crude-oil production. U.S.S.R. crude oil output was only a tenth of U.S. production in 1946, but it will be more than a third at the end of 1960 and more than half in 1965. The Soviet Seven-Year Plan (1959-65) for oil provides for substantial increases in petroleum production, refining, storage, and distribution facilities. Crude oil production and primary distillation capacity are to double, considerable storage capacity is planned, and pipelines for crude oil and petroleum products are to increase threefold. According to the Soviets, the initial phases of this plan (1959 and 1960) have been completed successfully. However, this progress has been achieved with difficulty.

Jan 1, 1961

By N. Gritzuk

The area of Canada with which we are here concerned consists of Yukon Territory and Northern British Columbia. Generally it lies west of the coastal mountain range and access to the sea can be gained at only selected points which are relatively few. It is served by the Alaska Highway as well as a provincial and territorial system of roads permitting transport of mining products to Whitehorse in Yukon Territory. This town it the northern terminus of the White Pass and Yukon Route, which system provides a rail service between Whitehorse and Skagway, Alaska a distance of 110 miles, and thence to Vancouver, British Columbia, by the coastal Motor Vessel C. J. Rogers, a distance of an additional 890 miles. At present the service between Vancouver, B.C. and Whitehorse, Y. T. is on a fourteen day basis. The coastal vessel, capable of carrying 3,200 tons of cargo, was specially designed and built in 1955 for handling containerized cargo and general cargo northbound, and containerized and palletized asbestos fibre, and palletized lead and zinc concentrates southbound.

Jan 1, 1961

By John D. Corrick

Three species of chemosynthetic iron- and sulfur-oxidizing autotrophic bacteria have been isolated from the leaching waters of copper mining areas. These species are: The sulfur-oxidizing Thiobacillus concretivorus, the iron-oxidizing Ferrobacillus ferrooxidans, and a sulfur- and iron-oxidizing bacterium closely resembling Thiobacillus ferrooxidans, INTRODUCTION Among several suggested new processes for treating marginal ores in the United States, none is more intriguing than the possibility of extracting metals from low-grade materials by the action of microorganisms One phase of a Federal Bureau of Mines investigation toward developing such a procedure was to isolate and identify specific chemosynthetic iron and sulfur. oxidizing autotrophic bacteria native to certain domestic copper deposits where leaching is practiced. The bacteria or microorganisms considered important to this investigation are those capable of producing solutions of ferric sulfate and sulfuric acid. Solutions of this type are excellent solvents for some copper minerals By establishing the presence of these bacteria at certain copper-leaching areas, strength would be given to a theory that microbial activity is partly responsible for the oxidation that takes place at these areas. Their presence also advances possibilities for controlled use of microbial action in metal extraction processes. Leathen4/ has demonstrated that one of the chemosynthetic iron-oxidizing bacteria, Ferrobacillus ferrooxidans, can oxidize 200 parts per million of ferrous iron to the ferric state in 3 days,

Jan 1, 1961

By P. G. Clites

A laboratory furnace was developed by the Federal Bureau of Mines for use in studying the interrelationships among variables associated with skull melting and casting high-temperature metals. Although additional work is necessary to determine the extent to which the information obtained by using this furnace can be extrapolated to larger furnaces of the same type, many casting characteristics of metals and alloys can be determined on equipment of this size. This furnace is a laboratory-size, consumable-electrode, skull-casting furnace equipped with a water-cooled copper ladle. The ladle, which is a tilt-pour or over-the-lip type, has a volume of approximately 30 cubic inches and provides up to 20 cubic inches of molten metal for castings. Castings of various reactive and refractory metals, including zirconium, titanium, hafnium, columbium, molybdenum, tantalum, and tungsten, have been produced. In addition, castings of iron, chromium, and copper have been made. The simplicity and versatility of the apparatus would make it useful to metallurgical laboratories preparing cast specimens.

Jan 1, 1961

By R. C. Tait

The gold at Giant Yellowknife is intimately associated with a complex mixture of sulphides, including pyrite, arsenopyrite, stibnite, and a wide variety of antimony sulpho-salts. Direct cyanidation has never been feasible. Recovery is almost entirely dependent upon flotation, roasting of flotation concentrate, and cyanidation of calcine. In November 1958, an Edwards-type roaster and an early prototype, two stage Fluosolids roaster, were replaced by a large two-stage Fluosolids roaster of improved design. The new roaster was started at "safe" medium temperatures, but early in 1959, temperatures in both stages were gradually and deliberately lowered to determine whether continuous autogenous roasting could be maintained under exacting low temperature conditions necessary for good extraction. Operation is smooth and continuous with first and second stage temperatures controlled at 925° and 875°F respectively. Plant cyanide ex-traction compares very favourably with extraction from low

Jan 1, 1961

By Edwin B. Cook

Studies of flame and combustion phenomena at the Bureau of Mines have been facilitated by computer evaluation of the thermodynamic properties of gases formed by constant-pressure burning.4 5 This report is the sixth of a series6-10 presenting results of such calculations; it deals also with constant-volume deuterium-air flames.

Jan 1, 1961

By E. G. King

Thermodynamic data for the hydrated varieties of alumina are sparse, and those for the common clay minerals are virtually nil. This paper partly fills the vacuum by reporting low-temperature heat-capacity measurements and entropy evaluations of diaspore (A10(OH)) and three clay minerals of the composition A12Si207?2H20 - kaolinite, dickite, and halloysite. The heat-capacity measurements were made in the temperature range 510 to 298.15° K., and the entropies were evaluated at 298.15° K. Diaspore has an unusually low heat capacity and entropy compared with boehmite (another mineral of the same chemical composition). The entropies of the three clay minerals differ too little for entropy to be the important factor relating to differences in the thermal stability of these substances.

Jan 1, 1961

By H. U. Ross

ROASTING is usually thought of as a process in which finely crushed or ground ore is heated with air in a suitable furnace in which the ore is rabbled or agitated in such a way as to insure complete reaction between the oxygen of the air and the oxidisable constituents of the ore. Roasting in this sense is used only to a very limited extent in the iron and steel industry. This is because, in most iron ore deposits mined today, the ore is of a type that does not require roasting. Where this process is used, it is usually because of some special circumstance, such as a peculiar economic condition, that warrants it. If roasting is looked upon in the broader sense as a gas-solid chemical reaction carried out at an elevated temperature in which both gaseous and solid products are formed, then the process is used in the iron and steel industry to a greater extent

Jan 1, 1961

By A. L. Engel

This report describes results of laboratory-scale experimental treatment of nine ores containing gold and silver, including samples of products of previous plant treatment, from ore deposits in California and Nevada. The samples treated were taken by engineers of the Bureau of Mines during investigations of these ore deposits. The information reported is of interest for development of the mining districts represented or in future Investigations of similar ores from other sources. The treatment methods were as simple as possible. More complicated treatments were tried when required, The applicability of the methods and their limitations in treating the ores are shown by the data in this report. The following treatment methods were employed in the experiments described: Screen analyses were made to determine distribution of values in various screened-sized portions of crushed ore, or to determine optimum size to which a particular ore should be crushed or ground to liberate values, and some-times to determine residual values in various-sized portions of treated material.

Jan 1, 1961

By E. R. Palowitch

A centrifugal float-and-sink test procedure has been developed by the Bureau of Mines to reduce the time for the gravimetric separation of coals finer than l4-mesh from as long as 24 hours to less than 1 hour. Comparative tests indicated that centrifuging a minus 14-mesh Pittsburgh-bed coal for 20 minutes at 1,500 revolutions per minute produced results that compared favorably with static float-and-sink test results. Standard deviations of the mean recovery and ash content of the float obtained centrifugally ranged from 1.31 and 0.04 percent, respectively, at 1.30 specific gravity to 0.21 and 0.05 percent, respectively, at 1.60 specific gravity. As in static separations, retreatment of the products separated at low specific gravities was required.

Jan 1, 1961

By Gerald V. Gibbs

Quadratic functions, Q(hkl), are given to six places in increments of 0.01° for 2? from 0° to 90° for CuKa and from 25° to 180° for CuKa1. The wavelengths used for Cu in the computation are those agreed upon by the Editorial Commission of the International Tables for X-ray Crystallography (1950): CuKal 1.54051 A.; CuKa2 1.54433 A. INTRODUCTION At the Federal Bureau of Mines laboratory, Norris, Tenn., X-ray diffraction crystallography using tubes with copper targets revealed a need for a handy reference for the quadratic functions of copper radiation. The tables presented here were prepared to satisfy that need. The quadratic form Q(hkl) may be expressed in terms of the Bragg diffraction angle 2? and of the wavelength ? as

Jan 1, 1961

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Harrison County, W. Va. It is one in a series of Federal Bureau of Mines reports planned to determine coals suitable for the production of metallurgical coke, either as mined or after beneficiation. Over 6.5 million tons of coal was produced in Harrison County, W. Va., in 1958, of which over 3.7 million tons was cleaned mechanically in seven preparation plants. All of the coal cleaned was from the Pittsburgh bed. It has been estimated that more than 1,816 million tons of coal remains in the county in beds 12 inches or more thick. The Pittsburgh and Redstone beds were selected by the Bureau for a study based on current production rates and estimated minable reserves. Sample locations were selected following a study of the literature, conferences with mining engineers and mining company officials in the field, and examination of the available sites. Six samples were collected from the Pittsburgh bed, and three samples came from the Redstone bed, Float-and-sink tests of the samples collected from the Pittsburgh and Redstone beds showed that neither coal could be upgraded to a metallurgical fuel under the standards set up for this study, even after intensive preparation. Finer crushing of the samples moderately increased the yields and slightly reduced both the ash and the sulfur contents in the 1.30-specific-gravity float fractions. Finer crushing slightly decreased the yields in the 1.58-specific-gravity float fractions, whereas it reduced the sulfur content 0.11 percent for the Redstone sample and 0.46 for the Pittsburgh sample.

Jan 1, 1961

By Martin H. Stanczyk

The direct dissolution of a typical zinc sulfide flotation concentrate by elevated temperature and pressure leaching was investigated. The concentrate assayed about 55 percent Zn, 32 percent S, 6 percent Fe, and 1 percent Pb and contained minor quantities of copper and precious metals. The influence of various factors on the dissolution of the zinc in acidic and ammoniacal pulps when using oxygen as the oxidant was determined. The tests revealed that the sphalerite was difficult to oxidize. Complete dissolution of the mineral required vigorous and intimate nixing of the gaseous, liquid, and sold phases. The addition of pyrite or sulfuric acid to water slurries of the concentrate was required to obtain a high zinc extraction when leaching under acidic conditions. The quantity of pyrite and acid used was about 0.125 and 0.25 pound, respectively, per pound of zinc sulfide contained in the leach charge. In tests with acid, about 96 percent of the zinc was extracted from the concentrate in 1 hour at 200° C. when the oxygen partial pressure was 75 pounds per square inch gage or higher. Leaching with a continuous flow of air as the oxidant gave results that were almost as good as those obtained when oxygen was used, In tests with air fed through the autoclave at 320 liters per hour, 95 percent of the zinc was dissolved in 1 hour, Acid leach solutions assaying approximately 58 grams Zn per liter and containing Fe, Ni, Cr, and Cu impurities were produced in the better tests. The leached residue consisted essentially of red iron oxide together with substantially all of the lead and precious metals.

Jan 1, 1961