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Established as a Society February 26, 1957 OFFICERS AND COMMITTEES Wayne E Glenn, President Earl M Kipp, President-elect John S Bell, Past President R A Morse, Vice-President W D Owsley, Vice-President Everett G Trostel, Treasurer Joe B Alford, Executive Secretary 6300 North Central Expressway Dallas 6, Texas

Jan 1, 1960

By Marvin W. Wilson

The Federal Bureau of Mines has conducted laboratory experiments simulating underground gasification of coal to study the feasibility and mechanism of the process and determine the chemical and physical characteristics of a coal-bed during gasification. Laboratory and small-scale field experiments also were made to investigate the properties of coal and other factors affecting the electrolinking-carbonization method of preparing a path through a coalbed before gasification. Laboratory experiments simulating underground gasification of coal: Experiments with a laboratory retort indicated that bituminous-coal deposits could be gasified in place to produce a combustible gas.

Jan 1, 1960

By Kenneth H. Johnston

For the past several years, Bureau of Mines petroleum engineers have arranged tours of selected waterflooding projects for the spring meetings of the Kansas-Oklahoma Waterflood Association. These tours are conducted to demonstrate unique operating methods and new field equipment and to provide additional opportunities for exchanging information. Each of these tours has been supplemented by a published report describing in detail the projects visited. This report has been prepared for distribution during the 1960 spring tour of four waterflooding projects in Greenwood County, Kans. (fig. 1). Three of the projects produce oil from the Bartlesville sand, and one produces from the Cattleman sand. The Bartlesville-sand floods have been in operation from 4 to 12 years and have produced about 3,910,000 barrels of waterflood oil from the injection of approximately 64,715,000 barrels of water, a cumulative water-injected to oil-produced ratio of 17 to 1. The Cattleman- sand flood, which has been operating for 3-1/2 years, has produced about 842,000 barrels of waterflood oil from the injection of approximately 9,305,000 barrels of water, a cumulative water-injected to oil-produced ratio of 11 to 1.

Jan 1, 1960

By J. L. Konchesky

The technical feasibility of gasifying powdered, noncoking, low-rank coal with steam in an externally heated tube has been demonstrated. The tube, 112 ft. of alloy-steel tubing shaped into a helix, served as an electrical conductor of electricity used for heating. The effects of the following variables were studied: Residence time of coal in reactor, average reaction temperature, steam concentration, and rank or geologic age of coal. Reaction pressure was maintained in the range 19-26 p.s.i.a. High carbon conversions and large yields of synthesis gas were obtained with low-rank coal. In one test, for example, about 88 pct. of the carbon in a subbituminous C coal was gasified at 1,910* F. with a residence time of 1 sec. The gas contained 58 pct. H2, 19 COD 15 CO, and 3 CH4; the yield was 30 cu. ft. (at 32' F. and 14.7 p.s.i.) of synthesis gas (CO + H2) per pound of dry coal.

Jan 1, 1960

By R. H. Hiltz, R. W. Douglass

Large-grain specimens of iodide titanium prepared metal-lographically were stain etched using the technique of New York University as modified by Watertown Arsenal Laboratories. Orientations of grains showing an abnormal response to stain etching were determined by back-reflection X-ray techniques. X-ray results showed that a-titanium grains, oriented such that their basal planes were parallel to the polished surface, have a slower reactivity to stain etching than any other orientation. Grains oriented such that their basal planes made small angles with the polished surface exhibited reaction rates between that of the true basal orientation and the normal rate. As the angle with the surface increases the reactivity increases up to a maximum angle of 14 deg. Basal planes making an angle with the surface of greater than 14 deg show normal reactivity to stain etching. These data, plus work on polycrystalline specimens, indicate that the oxidation rate of titanium might be reduced by correct alignment of crystal planes. ThE earliest observed phenomenon in the micrography of titanium was the occurrence of a grains which exhibited no birefringency. Even though a titanium possesses a hexagonal-close-packed structure and should be optically anisotropic, it can appear optically isotropic, when the crystal is so oriented that its intersection with the polished surface is perpendicular to the axis of symmetry. During the develoment of color staining techniques for titanium: it was noted that the a phase did not stain uniformly. Staining of specimens of commercially pure titanium resulted in a micro-structure of blue-colored grains, among which were randomly oriented a few grains exhibiting colors between the initial yellow and the final blue color. Under polarized light, these off-colored grains appeared to be optically isotropic. More intense study with polarized light, however, showed only the yellow grains to be isotropic. The intermediate colored grains exhibited weak birefringency, which at first glance is not detectable due to the strong birefringency of the surrounding structure. Aminoff2 and Straumanis3 have previously shown that in zinc the basal orientation is less reactive than other orientations. Leidheiser4 showed the same thing to be true for the hexagonal-close -packed configuration of cobalt. Thus, it would appear that the basal-plane orientation is responsible for the abnormality in stained titanium. Later work by Leidheiser5 on cobalt has shown that other planes besides the basal plane exhibited reaction rates slower than the normal rate. Reported planes were the (100), the (1011) and several planes making small angles with the basal plane. The last observance appears not to be due to the reactivity of the reported plane but due to the reactivity of the basal plane which is very close to being parallel to the surface. There are, then, two possible explanations for the range of colors observed in stain-etched a titanium. Since extensive research on the effect of orientation on surface reaction has failed to provide any definite trend, these two explanations are not adequate in themselves. Planes showing the retarded reactivity differ not only for different crystal structures but for metals of the same crystal structure and even for different reactions of the same metal. Tragert,6 Leidheiser,7 Tammann,6 and wagner9 have shown copper to exhibit retarded reactivity on the (111) plane. However, Leidheiser10 has shown that under other conditions the retarded reactivity of copper is associated with the (100)

Jan 1, 1960

By Robert M. Grogan

Fluorspar is the commercial name for fluorite, which is the mineral having the composition CaF2, calcium fluoride. Its valuable properties are due to its content of fluorine, and it is the only important commercial source of that element. The name is derived from the Latin fluere, to flow, because the mineral melts easily and is a good flux. History The mineral has been known since Greek and Roman times, when it was used for drinking cups and ornamental slabs. Various peoples including the Chinese and the American Indians have carved ornaments from large crystals. Its usefulness as a flux was known to Agricola, who wrote about it in 1546.1 Mining began in England about 1775 15 and at various places in the United States during the period 1820 to 1840.28 Substantial production was achieved first in the period 1888 to 1900 in consequence of the development and widespread adoption of the basic open hearth method of making steel, in which fluorspar is used as a flux. After that, production and usage was stimulated by growth in the steel, aluminum, chemical, and ceramic industries and accelerated by World Wars I and II. The organic fluorides called "Freons" entered the picture in 1931, and the use of anhydrous HF as a catalyst in the manufacture of alkylate for high octane fuel blends began in 1942. The development of the froth flotation process in the late 1920's, a differential flotation scheme for separating fluorspar from galena, sphalerite, and other minerals in the 1930's, and the application of heavy-media concentrating methods to the treatment of low-grade ores in the 1940's were outstanding technological contributions that enabled increased production of fluorspar concentrates. Composition and Properties Fluorite in its purest form contains 51.1 pct calcium and 48.9 pct fluorine. Substitution of small percentages of cerium and yttrium for calcium have been noted.4 Mechanical inclusions of gases and fluids such as petroleum and water, and of other solid minerals such as pyrite, marcasite, and chalcopyrite are common. The fluorspar of commerce contains attached and admixed mineral impurities, chiefly calcite, quartz, barite, celestite, and various sulfides. It is interesting that the purest commercial form in which the mineral is sold, acid grade concentrate, contains a minimum of 97 pct CaF2, and as such is of comparable purity to many reagents used in chemical laboratories. Fluorite has a marked tendency to occur in large, well-formed crystals sometimes six to ten inches on a side. It crystallizes in the isometric system, frequently forming cubic and octahedral crystals or combinations thereof. The mineral also occurs in massive and in earthy forms, and in crusts or globular aggregates with radial fibrous texture. Crystalline fluorspar exhibits a great array of colors, from colorless and water clear to yellow, blue, purple, green, rose, red, bluish and purplish black, and brown. The colors are often arranged in alternating bands parallel to cube faces. They may be altered by exposure to X-rays, heat, ultraviolet light, and pressure, and are caused by a variety of factors including the presence of trace impurities and displaced ions in the lattice. Sometimes the changes induced by X-rays can be reversed by ultraviolet radiation. The mineral has a hardness of 4, and is the model of that hardness on the Mobs scale.

Jan 1, 1960

By C. Stamberg, W. McGuire, R. C. Carlson, L. W. Vollmer

"The selection of materials and pre-cautionary measures for handling natural gas and condensate containing aqueous hydrogen sulphide are presented. Based on the results of a pilot production test and laboratory studies, together with several years . of operating experience, it was found that the behaviour of materials in sour gas environments can be predicted sufficiently accurately for engineering purposes.The selection of proper materials is essential for preventing sulphide-stress cracking. Where high strength materials are not required, low car-bon steel is used. Components requiring high tensile strength and hardness characteristics should be made from K-monel or properly heat-treated carbon-manganese-molybden-um and AISI 4140 steels. Welded connections are a potential source of sulphide-stress cracking. Consequently high quality welding and strict inspection are suggested as the most economical precautionary measures available.A maintenance program based,. where possible, on visual inspection of equipment and/or test spools located at strategic points should be used to follow weight loss and putting corrosion in sour gas environments. If severe weight loss or pitting corrosion is encountered, inhibitors have been found to be an effective deter-rent."

Jan 1, 1960

By Eugene T. Sheridan

This circular presents data on individual plants of the fuel-briquet and packaged-fuel industries that responded to the Bureau of Mines annual economic survey and reported production for 1959. The companies named herein represent virtually all producers of processed fuels of mineral origin. A few small companies may not have been canvassed or failed to respond, however, as some plants operate intermittently, and the survey is voluntary. No consideration was given to size of the plant and all plants that reported commercial production were included. Specifically excluded were plants that manufactured briquets from wood charcoal. Fuel briquets and packaged fuel are manufactured solid fuels, fabricated from fine-sized mineral fuels by mixing with binders and compressing into small individual shapes. Briquets usually are produced as small, pillow-shaped pieces, 2 to 4 inches long, weighing 2 to 4 ounces. Packaged fuel consists of 3- to 4-inch cubes, 6 or 8 of which are wrapped in heavy kraft paper to form a package weighing 10 to 15 pounds. The overall size of a popular package is 10-112 x 7 x 3-1/2 inches. Briquets are durable, may be stored outdoors, and shipped and used as bulk fuel. Packaged fuel is fragile, and must be stored indoors to keep it from deteriorating. Whereas briquets are consumed in many areas as a general residential fuel, packaged fuel is more of a specialty item, used at times as a supplement to other fuels. Package fuel is burned without removing the paper and referred to as the "white-glove" fuel.

Jan 1, 1960

By J. P. Capp

This experiment, one of a series on underground gasification of coal, was an investigation by the Federal Bureau of Mines of hydraulic fracturing as a means of increasing the air acceptance of a coalbed to permit introducing combustion air and removing product gases. Specific objectives of the investigation included: (1) Fracturing a coalbed; (2) determining the distance the coal was physically affected; (3) ascertaining the effect of the fracture on air acceptance of the coalbed; and (4) gasifying the coal. The coal was fractured with a fluid consisting of 15,000 lb. of sand mixed with 10,000 gal. of fuel oil and 5,000 gal. of kerosine, injected at pressures up to 900 p.s.i.g. and rates up to 425 g.p.m. The oil served as the fracturing medium, and the sand as a propping agent to hold the fracture open. From the fracture point, (the place in the bed where the fluid was injected), the fracture extended 200 ft. or more along the face cleats, somewhat less along the butt. cleats, and was confined to the coalbed. At the fracture point, the bed accepted about 500 std. c.f.m. of air, which was an etghtyfold increase. Fracture effects were extensive, as airflow was noted from old mine workings and outcrops 600 to 800 ft. from the fracture point. It is probable the actual fracture was much less than 600 ft. and that normal coalbed permeability beyond the fracture limits was responsible for this flow. This indicated that effects of the fracture extended beyond the area of coal physically affected. Although no attempt was made to gasify coal more than 200 ft. away, these effects plus the natural permeability of the bed likely would permit combustion beyond the outer limit of the fracture. As these experiments continued for more than 2 years, and greater air acceptance due to the fracture was observed at the beginning of each test, it is apparent that the effects of the fracturing persist for a considerable time.

Jan 1, 1960

By Henry H. Ginsberg

The effectiveness of 0.01 pct. molybdenum, as ammonium molybdate impregnated on coal, on the hydrogenation of a high-volatile bituminous C coal at 8,000 p.s.i.g. and 460° to 480° C. has been studied in a pilot plant by the Federal Bureau of Mines. Under these conditions, the Bureau obtained 98 to 99 pct. conversion5/ of coal to liquids and gases at throughputs of 29 to 101 lb. of m.a.f. coal per cubic foot of reaction space per hour. At 460° C. the indicated yield of oil ranged from 63 pct. (based on m.a.f. coal) at a throughput of 35 lb./c.f.h. (pounds per cubic foot per hour) to 68.5 pct. at a throughput of 58 lb./c.f.h., and the yield of gaseous hydro-carbons ranged from 25.5 to 19 pct. at the same throughputs. The maximum measured yield of oil boiling under 325° C. was 47 pct.

Jan 1, 1960

By J. Nutting, J. W. Cahn

WITH the development of thin film techniques for the direct examination of metals in the electron microscope some new problems in quantitative metallography have become apparent. In order to obtain certain contrast effects in the electron optical image when examining thin films from alloys containing dispersed phases, it is essential to use films of a thickness at least two or three times greater than that of the mean particle diameter of the dispersed phase. From micrographs of such specimens it may be desired to obtain the volume fraction of the dispersed phase and the number of particles of the phase in a unit volume of the matrix. Under these conditions the particles sectioned by

Jan 1, 1960

By A. C. Johnson

This report is one of a series being prepared by the Bureau of Mines on exploration, development, mining methods, and costs at various mines in the United States. It describes operations at the Black Rock mine, Wah Chang Mining Corp., Mono County, Calif. The purpose of these reports is to promote development and conservation of our mineral resources by disseminating technologic information on mining methods, practices, and costs. The Black Rock tungsten mine of the Wah Chang Mining Corp. is 33 miles north of Bishop, Calif., in the Benton Range, Mono County, Calif. The property was acquired in August 1950 and a well-planned program of exploration, development, and exploitation resulted in a good production record with low costs. Operations were halted in July 1957, about 6 months after suspension of the tungsten purchase program by the Federal Government.

Jan 1, 1960

By H. E. Powell

A laboratory mineral-dressing investigation was conducted by the Federal Bureau of Mines on four limonitic and four sideritic iron ores from the North Basin of the east Texas iron-ore district. The samples, composited from drill cores, were considered representative of the iron-ore reserves of the area. The objectives of this research were twofold: (1) To devise a mineral-dressing method whereby the yield from currently mined east Texas iron ores might be increased and the grade improved, and (2) to extend such treatment to include the lower grade ferruginous materials that are not amenable to beneficiation by simple washing and, therefore, are not being exploited. Of the mineral-dressing methods used in this investigation, magnetic separation of roasted are was shown to be the most effective. Results show that, by this method, a laboratory recovery of 82 percent of the iron is attainable at a grade surpassing that obtained by current plant practice and that both limonite and siderite are amenable to concentration by the process. The existence of large deposits of iron are in eastern Texas has been recognized for over 100 years. These ores were first exploited during the Civil War and were mined intermittently until about 1911. From that time until 1944 when the Defense Plant Corporation financed the erection of three blast furnaces to use these east Texas ores, production was almost at a standstill.4/

Jan 1, 1960

By Thomas J. Blalock

The volumetric determination of uranium according to the method of Sill and Peterson (6),3/ which uses cerate oxidimetry after the separation of interferences such as sulfides and cupferrates, has been used for some time by the Bureau of Mines and gives satisfactory results for many of the samples tested. However, in those instances where the uranium content did not exceed a few tenths of 1 percent and iron was present in the range of 10 to 40 percent (as Fe203),4/ the method was cumbersome and unreliable. The need for a more accurate procedure for the determination of small amounts of uranium in the presence of large amounts of iron, such as in shale or black sands, prompted this investigation. The Bureau desired that materials containing as little as 60 p.p.m. of uranium be assayed within reasonable limits of accuracy. One of the primary aims of this work has been to eliminate, as far as possible, the necessity for repeated cup ferron extractions.

Jan 1, 1960

By A. J. Miller

Estimates of interstitial water saturation derived from capillary pres-sure data are compared with residual water saturations found by the analysis of cores out in oil-base drilling fluid. A theoretical explanation for the high-rate of water production from the Bellshill Lake Field is proposed, based on the interpretation of the capillary pressure data.

Jan 1, 1960

By J. Duby

"A description is given of a series of tests performed to determine the comparative effects which dynamic and static straining, in compression, have on the physical strength properties of mild steel and an aluminum alloy. The dynamic deformation was imposed during the passage of single stress pulses of about 100 micro-second duration. These pulses were recorded with strain gauges mounted near both ends of the specimen. The resulting records were analysed using a simple wave theory; there from the dynamic stress-strain curves for the respective metals were deter-mined and were then compared with the static stress-strain relation. The respective hardnesses of the metals after deformation are evaluates by means of static stress-strain curves in compression. The micro-structures of the metals before and after deformation are also shown. It is observed that dynamic de-formation considerably modifies the rate of strain hardening. This modified hardening appears to be persistent. The observed differences in physical strength properties and micro-structures are discussed in the light of the accepted dislocation theory for metals."

Jan 1, 1960

By J. W. Eckerd

This report describes an investigation of the technical feasibility of using a conventional commercial-size (10-ft. i.d.), rotating grate, dry-ash-removal type gas producer to make producer gas from chestnut-size bone anthracite. Test instruments were installed, and some minor changes were made in the equipment to handle the large quantities of materials expected. Extensive tests, lasting about 4 weeks, were planned, using 35 to 50 percent ash chestnut anthracite bone. However, operations were suspended after 8 days when it became apparent that to use this type of fuel satisfactorily substantial changes in equipment and operating procedures would be required. Nevertheless, enough data were obtained to indicate that gas could be produced continuously and routinely from bone coal in this type of producer whenever conditions justified the necessary development work.

Jan 1, 1960

By C. W. Taylor, F. L. Martin

"THE DICTIONARY defines Metallurgy as the ""science or art of separating metals from their ores and refining them for use"". In these days, however, such a definition is not detailed enough.The modern science of metallurgy is based on two fundamental sciences, physics .and chemistry, and is sub-divided into two major fields: Process Metallurgy and Physical Metallurgy. These fields of metallurgy are now so comprehensive and involved that even the graduate metallurgist has to specialize in one or the other.In recent years, the relatively new science or technology of non• destructive testing has also entered the industrial scene, with tremendous impact and ramifications. So much so that, certainly, no .discussion on metallurgy can be complete without including some reference to it.Obviously, one paper cannot hope to cover in detail the relationship of the whole science of metallurgy to the mining industry. Consequently, only a very brief reference will be made to the field of Process Metallurgy, our major concern being with Physical Metallurgy and Non-Destructive Testing."

Jan 1, 1960

By Louis C. Brichta

This report summarizes the progress made by the Federal Bureau of Mines in assembling and compiling a catalog of available logs of drill holes and maps of mine developments in the Tri-State Zinc-Lead District in northeastern Oklahoma, southeastern Kansas, and southwestern Missouri. It supplements an interim report (11)3/ published in 1955, and for convenience of the reader repeats much of the general descriptive matter pertinent to the district contained in that report. The work of procuring and recording the data was begun in August 1949 and was recessed in May 1959. The catalog preserves the records of accomplished explorations and mine developments in the district and provides a readily available source of information for individuals and firms interested in planning mineral explorations, Government agencies estimating of reserves of mineral resources, and the mining industry for general use.

Jan 1, 1960

By E. G. King

THIRD-LAW entropy data for zirconium-containing compounds are sparse. Kelley a lists entropies at 298° K. for the oxide, tetrachloride, nitride, and silicate, as well as for the metal. The present paper presents heat capacities between 51° and 298° K. and entropies at 298.15° K. for the zirconates of the alkaline-earth metals-calcium, strontium, and barium. The authors believe magnesium zirconate does not exist as a stable compound at room temperature. Entropies of formation from the constituent oxides also are given. MATERIALS The materials used in this investigation were synthesized and analyzed in the Berkeley Laboratory of the Bureau of Mines. Calcium zirconate was prepared by heating an intimate mixture of reagent-grade calcium carbonate and pure zirconia for 30 hours between 1,200° and 1,300° C. and for 32 hours between 1,400° and 1,500° C. As part of the heating schedule, the sample was ground and mixed seven times. Periodic analyses and minor adjustments of composition were made. Analysis of the final product gave 31.19 percent calcium oxide (theoretically 31.28 percent) and 68.67 percent zirconia (theoretically 68.72 percent). The X-ray diffraction pattern agreed with that in the ASTM catalog.

Jan 1, 1960