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By John P. Powell

A comprehensive study of the effects of hydraulically fracturing water-flood wells in Oklahoma has been made by the Federal Bureau of Mines. This report presents results of that study and an analysis of some of the factors governing the results of fracture treatment on waterflood properties. Originally, hydraulic fracturing was used to stimulate oil production from old wells producing by primary methods, and its application to water-flooding was regarded with skepticism by most producers. However, since 1953 the number of fracture treatments of both oil and input wells in waterfloods has increased steadily. Hydraulic-fracture treatments in waterfloods have generally been successful in stimulating production from oil wells and increasing the rate of injection into input wells. Hydraulic fracturing has enabled several producers to turn probable failures into economically successful projects.

Jan 1, 1961

By T. E. Gray

This report describes the preparation characteristics of the signifi¬cant coalbeds in Preston County, W. Va. It is one in a series of reports planned to determine coals suitable for the production of metallurgical coke, either as mined or after beneficiation. Over 2 million tons of coal was produced in Preston County, W. Va. in 190, none of which was cleaned mechanically. Estimates as of January 1, 1959, indicate that more than 3 billion tons of coal remained in the county in beds 12 inches or more thick. The Bakerstown, Mahoning, Upper Freeport, and Upper Kittanning beds were selected by the Bureau of Mines for study based on current production and estimated minable reserves. Sample locations were selected after study of the literature, conferences with mining engineers and mining company offi¬cials in the field, and examination of available sites. Four samples were collected from the Bakerstown and Upper Freeport beds and one each from the Mahoning and Upper Kittanning beds.

Jan 1, 1961

By M. R. Geer

The use of the cyclone as a dense-medium cleaning device was first described by Driessen6/ in 1945, after development of the process in the Netherlands during the German occupation of World War II. A pilot plant was built in the Netherlands soon thereafter, and the first commercial plant was built in 1948. By 1958, 18 plants were operating or under construction.7/ Thus, economic factors in Europe, where the high cost of coal places a premium on efficient cleaning, dictated rapid adoption of the cyclone. American reception of the process differed. The Bureau of Mines presented the results of its own small-scale cyclone experiments in 1946;8/ showing a sharp separation between coal and impurity; adoption by industry now is taking place. There is now much greater emphasis on the efficient cleaning of fine coal, and the first American cyclone plant has begun operating; others are planned or under construction. With the present interest in improved treatment of fine coal, the Bureau of Mines felt that additional performance data on the cyclone would be helpful to industry. Therefore, a complete, open-circuit pilot plant was built to make cleaning trials on American coals covering a wide range of washability characteristics. Five raw coals and one middling product were included in the investigation, and each was cleaned at several densities; 17 cleaning trials are reported.

Jan 1, 1961

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 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 W. Beckering

In characterizing tars obtained by the low-temperature carbonization of North Dakota lignite, infrared spectra have been an invaluable aid in both qualitative and quantitative examination. Quite, early in the tar-research program of the Federal Bureau of Mines it became evident that the small number of published spectra available for hydroxy-aromatics would be inadequate for comparative purposes when dealing with the wide range of compounds present in coal tar; therefore, compiling a catalog of spectra was begun as a continuing part of the tar program. Because these spectra should be valuable to other investigators in this and related fields, they are being presented in these reports. This supplement to the original publications presents the spectra (figs, I to 32), representing 32 compounds, largely phenolic materials. The major problem of this project has been the availability of materials for examination. Most of the compounds included in this supplement were synthesized at the Bureau of Mines Lignite Research Laboratory. Some were obtained from commercial sources, whereas the compound 2'-hydroxy-l-phenylnaphthalene was synthesized at the Bureau of Mines laboratory in Bruceton, Pa. The spectrum of 2-ethyl-4-methylphenol, figure 32, is a correction of the spectrum presented as figure 26 in the original reports

Jan 1, 1961

By J. B. Gayle

Coke-pushing difficulties have been the subject of much controversy but relatively little scientific investigation. Nevertheless, continuing pushing difficulties can greatly decrease the life of a coke oven and should therefore be considered in the selection of the blend and operating conditions used for coke production. The present Federal Bureau of Mines investigation was undertaken to correlate results of previous investigators and to supplement these results to the limited extent practical by us of an experimental slot-type oven. To this end, pushing pressures have been determined routinely for Tuscaloosa oven tests conducted during the past 10 years. Nevertheless, the accumulated information remains incomplete in many respects, and in view of the recognized inadequacies of the data, publication is now undertaken only because of the scarcity of published information on this important problem and the discontinuation of carbonization studies with this oven.

Jan 1, 1961

By R. W. Lewis

The Federal Bureau of Mines Boulder City Metallurgy Research Laboratory conducted experiments in order to develop a spectrochemical method for determining the concentrations of impurities In high-purity tungsten. This report presents a procedure, developed by these experiments, for determining 19 impurities in high-purity tungsten. Metal samples were thermally converted to the oxide, mixed with graphite, which was prepared and mixed with an internal-standard element, and excited in a d.c. arc. Sixteen of the impurity elements were determined with one set of conditions, using germanium as an internal standard. Lanthanum was used as an internal standard in the tests for boron and chromium. Molybdenum required the substitution of sodium chloride for the graphite and the use of copper electrodes. Data on the precision of the method are included in this report. The coefficients of variation vary considerably but average about 15 percent. Higher concentrations of impurities than those investigated may be determined with some modifications of the testing procedure, provided attention is given to the possibility of interelement interferences.

Jan 1, 1961

By E. R. Palowitch

This report stems from a study by the Bureau of Mines of the possibility of reducing coal filter-cake moisture by applying radiant heat directly to the filter cake while under vacuum during the drying phase of the filter cycle. One disk of a 4-foot-diameter vacuum filter was equipped with gas-fired radiant-heat generators and the effect of radiant heating on the moisture content of a variety of filter cakes was studied. The results of this investigation show that this process can best be described as a filter aid capable of increasing the effectiveness of conventional filtration approximately 6 percentage points of moisture. The operating cost of removing water by this method is somewhat lower than the average operating cost of thermal drying and is considerably cheaper when the total cost is considered. Removal of water from coal that has been wet-cleaned is an important part of the overall coal preparation process. Water is a contaminant, and it is foolish to wash coal to reduce its ash content and add inert water in the process. In some instances the removal of water is actually more important than the removal of ash-forming minerals; its weight adds to the cost of transportation, and its evaporation during burning or carbonizing absorbs useful heat. Fine coal that contains more than about 10 percent moisture is notoriously difficult to handle. A problem thus exists for which there are sound practical and economic reasons to seek a solution.

Jan 1, 1961

By Scott W. Hazen

In recent years many mining companies have recognized that their chance for continued economic survival depends on the adaptation of technological advances in their operations. Increased productivity through new developments in mining methods and improvements in equipment has made mining and processing of lower grade ores possible. Cost analysis has produced accurate data on the costs for development, production, and processing of ore. All of these changes and cost studies have shown the necessity for increased accuracy in determining the grade of ore. Methods of estimating grade in a mineral deposit have not kept pace with the technological advances in the other areas. The same methods are in use today as in the past. Experience and judgment are major criteria of accuracy and the results are highly subjective. In 1953, as part of its research program to develop a better understanding of fundamentals of mining technology, the Federal Bureau of Mines began a sampling method research project at its Denver Mining Research Center. The basic objective of the project is to investigate sampling methods and to study the adaptation of the techniques of statistical analysis to mine sampling.

Jan 1, 1961

By R. J. Leary

Iron and steel scrap has accounted for 45 to 50 percent of the metallics used by the steel industry. In an electric furnace which utilizes a 100-percent cold charge consisting of about 99 percent scrap and 1 percent pig iron, sensible heat from molten pig iron is not present as it is when hot metal is charged to open hearths and converters. A study of means for more efficient utilization of iron and steel scrap in steelmaking indicated that the time and fuel requirements to melt scrap were important cost factors, particularly in arc-furnace steelmaking. A process to preheat scrap economically prior to charging into the arc furnace has been developed, utilizing efficiently the heat from combustion of fossil fuels as a substitute for electric-arc heating in the initial stage of arc-furnace steelmaking. Scrap is loaded into a portable vertical cylindrical furnace body that is open at the top and has a perforated dropout door at the bottom. In the heating operation, the furnace body containing scrap is placed upon a hollow base connected to a flue, and then the burner and combustion-chamber unit is lowered on top of the furnace body. The stream of hot-combustion products flows down through the bed of scrap imparting heat to it, and the cooled gases exhaust through the flue. After the heating operation the furnace body containing hot scrap is transported to the arc furnace for charging. Thus, the furnace body serves as a charging bucket for top-charged arc furnaces, enabling this preheating process to be integrated into existing material-handling patterns in many arc-furnace plants.

Jan 1, 1961

By Bernard Porter

The solubility of UO2 was determined at 1,250° C. in ternary melts of UF4 and BaF2 with CaF2, LiF, and SrF2. The solubility of Ce02 was measured at 800° and 850° C. in a solution of CeF3, BaF2, and LiF. The amount of La203 which dissolves at 950° C. in a binary mixture of LiF and LaF3 and a ternary of LiF, LaF3, and BaF2 was also measured. In each case, the amount of soluble oxide was mound to be less than 5 weight-percent. A procedure was developed for filtering fused, oxide-saturated fluoride melts in order to obtain a representative sample for chemical analysis. The oxide content of the samples was determined by an inert-gas fusion procedure.

Jan 1, 1961

By N. H. Coates

As part of a joint program of the U.S. Atomic Energy Commission and the Federal Bureau of Mines for using nuclear energy to supply process heat, the Bureau designed and constructed a pilot-scale simulated nuclear reactor system. Although workable components were developed,5 the simulated nuclear reactor could not be operated continuously at its design conditions of 2,500°F. and 250 p.s.i.g. because the refractory materials used for insulation deteriorated. Replacement of these materials with porous carbon permitted sustained operation at design conditions, and a 1,000-hour demonstration run was completed successfully. No serious operating difficulties developed during the test. Leakage of helium after 1,000 hours was only 3 to 4 std. c.f.h. Inspection after the run revealed no damage to any of the components. Including earlier runs during previous research5 the system has been operated about 4,000 hours, of which 1,120 hours have been at 2,500° F. or higher. The helium-recycle compressor performed satisfactorily with no main¬tenance whatever for 2,445 hours, with about 2,000 hours at 900° to 1,000° F.

Jan 1, 1961

By Joseph Grumer

An instrumented spherical vessel has been used for many years to study laminar combustion waves. Concurrent measurements of flame speed and pressure-rise rates have led to evaluations of burning velocities, the pressure dependence of the burning velocity, and the expansion ratios of the gases passing through the combustion wave. For the most part, these studies have involved flames initially at atmospheric or subatmospheric pressure. The old spherical vessel used by the Bureau of Mines was not designed for use at elevated pressures. Moreover, being made of wrought iron, it was susceptible enough to corrosion to prohibit its use with many combustible mixtures that figure in industrial research. In mid-1956, under sponsorship of the Office of Naval Research, the Bureau undertook the development of a stainless steel spherical vessel capable of withstanding explosions of gaseous mixtures at initial pressures as high as 20 atm. and initial temperatures as high as 250° C. The design called for a double array (cross) of closely spaced small windows for observation of the flame as it traversed the vessel and a piezoelectric transducer to measure concurrently pressure-rise rates. Because no commercial contractor was willing to bid on the construction of such a vessel, it was built at the Bureau's Bruceton machine shop.7

Jan 1, 1961

By K. K. Kelley

Thermodynamics data for silicates have applications in the fields of extractive metallurgy, ceramics, and geochemistry. To facilitate these applications, up-to-date tables of heats and free energies of formation are needed. It is the purpose of this report to supply such tables for anhydrous silicates. During the last 15 years the heats of formation of a substantial number of anhydrous silicates have been reliably determined at or near room temperature. This resulted from the development (first by the Bureau of Mines and later by the Geophysical Laboratory of the Carnegie Institution of Washington, by the Institute of Geology of the University of Helsinki, Finland, and by the Department of Geology of the University of Chicago) of accurate solution calorimeters, employing hydrofluoric acid as the reaction medium. Specific references to work of these laboratories will be made in the next section of this report. Also, entropy data at 298.150 K. and high-temperature heat-content values are available for many of these silicates, mainly owing to work of the Bureau of Mines. Most of these entropy and heat-content data have been compiled in Bureau of Mines Bulletins (13, 15).3

Jan 1, 1962

By Paul Meadows

This Bureau of Mines report presents operating practices and results of pressure maintenance and secondary recovery by water injection or by water injection supplemented by gas injection. Particular emphasis is placed on the results of water injection, which is the principal oil-recovery method employed in projects covered by this report. No attempt is made to study gas-injection projects or operations that are considered water-disposal projects. Also, this report does not include water-injection projects that have not been in operation long enough to evaluate results. Figure 1 is a map of north Louisiana showing the geographical locations of the projects included in this report. Most of the data used in this study were supplied by unit operators, operating companies, and the Louisiana Department of Conservation. Reservoir information and recovery data are generally those supplied by the operators, but include revisions where deemed necessary.

Jan 1, 1962

By S. R. Borrowman

This investigation by the Bureau of Mines was undertaken to develop information on the extractive metallurgy of thorite ores because potential ore bodies of this mineral have been found recently in Colorado, Idaho, and Montana. Basic information on thorite ore treatment that would be useful in appraising the potential of these and other domestic thorium resources was developed. The work was done mainly on thorite ore containing 3.87 percent ThO2 from the Powderhorn district, Colo., and on a composite sample containing 0.52 percent ThO2 from the Wet Mountains district, Colo. Limited tests of d corroborative nature subsequently were made on a sample containing 2.30 percent ThO2 from the Lemhi Pass area on the Idaho-Montana border.

Jan 1, 1962

By Gerald V. Gibbs

As a part of the Bureau of Mines long-range program in asbestos, synthetic asbestiform compounds and minerals were prepared and described. Fundamental structural data on two such compounds are given in this report. Crystallographic data are provided for the synthetic isotypic compounds potassium-lead silicate, K2.Pb4 -Si8021 (I), and lead-aluminum silicate, Pb2. Pb4 .Al2Si6O21 (II). The space group symmetry 14/mmm was assigned provisionally to I and II on evidence of single crystal and piezoelectric measurements. A statistical evalua¬tion of indexed powder diffraction data revealed the cell edtes of I to be a 11.816 and c 7.932A and those of II to be a 11.723 and c 8.044A. The phases are uniaxial with observed refractive indices eD 1.790, an ?D,699 and eD 1.884, cusp 1,807, respectively. The atomic structure of I and II may be based on a complex of chains of silicon-oxygen tetrahedra lying along the c cell edge similar to the type of chain structure postulated by Pauling for scapolite. K2.Pb4.Si8021 and Pb2.Pb4 Al2Si6021 were first described by Geller and Bunting (5, 6)4 as fibrous compounds similar in crystal habit to asbestos. These authors gave powder diffraction data, although no attempt was made to find the cell edges or to index the powder diffraction patterns. Later, Shell and others (9) conducted a crystallochemical study of these fibrous silicates in search of a substitute for strategic asbestos. Their single crystal data revealed K2.Pb4 -Si8021 to be tetragonal body-centered with cell edges a 11.66, c 7.95 A. Pb2.Pb4 Al2Si6021 was concluded to be isotypic with K2.Pb4 -Si8021 on the basis of similar powder diffraction patterns, chemistry, and physical properties. No attempt was made, however, to index the powder diffraction record nor to determine the appropriate space group of either compound.

Jan 1, 1962

By K. C. Dean

A flotation method was developed by the Bureau of Mines for concentrating pollucite, a cesium-aluminum-silicate mineral that may contain from 20 to 40 percent cesium oxide. Separation of the pollucite from three typical ores was achieved by froth flotation of the associated micas, feldspars, and other gangue minerals, using sulfuric and hydrofluoric acids and a cationic-type collector. A low-tenor, 8 percent cesium ore from Maine was upgraded to 20 percent cesium with recovery of 87 percent of the cesium. Relatively high- grade ores from Canada and Southern Rhodesia were beneficiated at lower ratios of concentration to 28 and 29 percent cesium content respectively with recovery of over 92 percent of the cesium. In addition to concentrating the cesium content of ores, the method also effectively separates cesium from sodium, potassium, and lithium, and in certain ores from rubidium. This is accomplished by selective froth flotation of the alkali metal-bearing gangue minerals such as lepidolite, other micas, and feldspars. Since the alkali metals, especially potassium and rubidium, are difficult to separate chemically or thermally from cesium to prepare high- purity cesium products, separation by physical mans is important.

Jan 1, 1962

By J. H. Holden

Operations involving the processing of coal, oxygen, and steam into synthesis gas by means of two pressure-type gasifiers have demonstrated the effect of heat loss and operating variables on carbon gasified and oxygen and coal requirements. Carbon gasified is the fraction of carbon in the coal that is converted to gas. Oxygen and coal requirement is the quantity of each that is needed to produce a unit volume (M std. c.f.) of carbon monoxide and hydrogen. Operating pressure of the gasifiers ranged from 150 to 300 p.s.i.g. and coal was fed at 200 to 500 lb./hr./cu.ft. of reaction-zone space. Oxygen-to-coal ratios were 8.5 to 10.5 std. c.f./lb. Heat loss and residence time have opposite effects on carbon gasified; increasing the heat loss decreases the carbon gasified, but increasing the residence time (by raising the operating pressure or reducing the coal-feed rate) increases the carbon gasified. The effects of these two factors are difficult to separate because they usually change simultaneously. A comparison of the results obtained from the operation of two gasifiers with different levels of heat loss, however, permitted the effect of heat loss to be separated from that of pressure and coal-feed rate. When the results were deter- mined on the basis of constant heat loss, increase of the residence time increased the carbon gasified until the reaction virtually had come to completion. For example, at 150 p.s.i.g., decreasing the coal-feed ratio from 500 lb./hr./cu.ft. to 200 lb./hr./cu.ft. substantially increased the carbon gasified. At 300 p.s.i.g., however, changing the coal-feed rate had little effect on the carbon gasified because the reaction had almost reached completion and further increase in residence time resulted only in a negligible change.

Jan 1, 1962