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By Bernard Lewis

This report summarizes the fundamental research and technical studies conducted by the Explosives Branch of the Bureau of Mines from July 1, 1943, to June 30, 1949. It is the thirteenth of a series of annual reports, which have aimed to bring to the reader a resume of the research results that have appeared in published form during each fiscal year. The work of the Explosives Branch covers a number of activities - explosives research, explosives testing, flame and combustion research, flammability of gases and vapors, dust-explosions research, and technical studies in the experimental mine. An important part of the work of the branch is fundamental research to advance our knowledge and understanding of explosion processes. Considerable emphasis has been placed on studies of ignition and flame stabilization, as it is felt that an understanding of these processes should assist materially in alleviating explosion hazards in coal mines. The results are also finding important application in the development of jet propulsion. Studies of the explosibility of gases, vapors, and dusts saving thousands of lives and are preventing the destruction of much property. In innumerable instances in which potential explosion hazards exist, safe operating procedures have been recommended from data taken in the Laboratory. Aware of the value to national security of research results of combustion, flame, and explosion, the Army, Navy, and Air Forces are actively supporting important phases of this fundamental research.

Jan 1, 1950

By W. J. Kroll

This investigation was undertaken with the idea of studying a number of unconventional methods for making chromium to determine whether production cost could be lowered and to discuss some of the more recently described processes. These comprise carbon reduction of the oxide in vacuum, nitride dissociation, fusion electrolysis of the chloride, amalgam method, iodide dissociation, calcium reduction of the oxide, hydrogen reduction of the chloride, and reduction of this compound with zinc and with magnesium. Preference is given this latter method, which is shown in a flow sheet. Special attention is given purification of the chloride and separation of the vacuum at about 900° C. A reduction method for the elimination of traces of oxide contained in pure chromium by pure hydrogen obtained from the dissociation of zirconium hydride is described. The various methods are compared in a table in the appendix. Aluminothermic and silicothermic methods for the reduction of chromium oxide and the aqueous electrolysis have been disregarded in this investigation.

Jan 1, 1950

By L. H. Harrison

In coal mines equipped with electrically driven mechanical mining equipment, the problem of protection for electrical circuits and machinery important, because the hazards of fires and explosions resulting from electrical failures is greater than in most other industries. There is need for better methods and improved protective devices for this service. Studies and tests designed to determine possible value of the short-circuiting contactor as an electrical device for coal mine service were investigated. Preliminary made to determine the operating characteristics of the device, after which tests were made under actual service in three coal mines. Ordinarily, electrical protection in coal mines is divided into three classes, as follows: 1. Overload protection that is intended to protect against damage from overheating and excessive mechanical strain due to overloading. 2. Short-circuit protection that provides a means of de-energizing the equipment instantly when an accidental short circuit occurs in the equipment or on the power system. Short cm protection tends to damage from fires and, explosions resulting in the dissipation of large amounts of electrical energy in a short circuit. 3. Ground fault protection that, in its various forms, is intended, to maintain the frames of electrical equipment at or near the same potential surfaces in contact with the earth for the purpose of safe-guarding human life.

Jan 1, 1951

By A. J. Kraemer, H. M. Thorne

The following account of oil-shale operations in Australia is based upon infor- mation obtained by the authors while visiting Australia from September 15 to October 7, 1947, supplemented by published data, and augmented by analyses of samples of oil shale and its products at the Oil-shale Research and Development Laboratories of the Bureau of Mines at Laramie, Wyo. The primary objective of the authors' trip to Australia was to obtain, first hand, information regarding the equipment and methods used by National Oil Proprie- tary, Ltd., at Glen Davis, New South Wales, in mining oil shale, extracting oil from it, and refining the shale oil. This company was operating the only oil-shale plant that had been active in Australia since 1945. The plant comprised an oil-shale mine, 104 modified Pumpherston (Fell) retorts in 2 batteries, a hele refinery, and a 3-inch gusoline pipeline to the railroad loniing terminal t Sun Junction, 30 miles away. There were, also, the usual and necessary any uralities, such as a power house, mechanical shops, offices, and laboratories One Information regarding the company's operations was wance because of its bear- Ing upon the synthetic liquid fuels program of the Bureau of Mines, pursuant to the Synthetic Liquid Fuels Act of April 5, 1944 (30 U.S.C., 321-325, as amended). objective of the Bureau's program. In accordance with the maniate of the Act, is to furnish American industry cost and engineering data necessary for the development of synthetic-liquid fuel industry, and an obvious means of obtaining some of these data is to learn how oil shale is being mined and retorted and how shale oil is re- rined in countries where these operations have been conducted on a plant scale for many years. The authors spent 2 weeks at the plant of National Oil Proprietary, Lt., at Glen Davis, and were afforded every opportunity to obtain letailed and specific information regarding all aspects of the company'a operations.

Jul 1, 1951

By K. E. Stanfield

This report presents the results of analytical studies made on two series of oil-shale samples from the Mahogany ledge of the Green River mine the character of the various grades of oil shale that are being mined and processed into shale oil and refined products at the Bureau of Mines Oil-Shale Demonstration Plant at Rifle, Colo. The analytical work was part of a synthetic liquid fuels program being conducted at the Petroleum and Oil-Shale Experiment Station, Laramie, Wyo. The 16 oil shales ranG6d in color from a gray brown ( or a sample that assayed 10.5 gallons of oil per ton to a very dark brown for a sample that assayed 75.0 gallons of oil per ton. In general, the samples were similar as to the types of organic and inorganic matter that they contained but varied widely in the amounts or these constituents. The principal constituents were calcite, dolomite, illite, and yellow organic material, while the minor constituents were quartz, feldspar and plagioclase feldspar, pyrite, marcasite, analcite, opal, black organic material, and small woody fragments. Some micro-fossils, spores and pollen grains were found also.

Jan 1, 1951

By G. S. Scott

Safety problems in the mining and allied industries have led the Bureau of Mines to investigate over a period of years; the flammability (explosibility) of many types of combustible atmospheres principally at ordinary pressure; the results of these investigations have been made available as a bulletin. However, more recently, the demand for information on the flammability of gaseous mixtures at high and low pressures has increased greatly. In particular, the rapid development of high-altitude aviation has brought demands for information on the flammable (or explosive) characteristics of certain gases and liquids at low pressures. The present report gives the results of about 900 tests made to determine the flammability of the lighter paraffin hydrocarbons mixed with air and nitrogen at pressures of 400 200, 100 and 70 ram. Hg. The gases tested include natural gas, methane, ethane, propane normal butane and isobutane. The minimum pressures at which these gases are capable of propagating flame whorl individually mixed with air also were investigated.

Jan 1, 1952

By W. W. Agey

As a part of the program of investigation of domestic sources of manganese in the western United States, engineers of the Bureau of Mines examined. and obtained samples of ore from two properties in the vicinity of Barstow, San Bernardino County, Calif. In addition to these, samples from two other properties in the same vicinity were submitted by the owners. As the ores were too low-grade to be acceptable for the direct production of ferromanganese, beneficiation studies were made to determine the amenability of the ores to concentration by ore dressing. The Big Reef manganese claims axe about 140 miles east of Barstow, Calif. The claims were leased by W., E. Thurber of San Gabriel, Calif., from the owner, C. S. VanDoren of Daggett., Calif. Manganese oxides occur as a replacement deposit in heavily brecciated andesite along a fault plane. Four samples were taken by an examining engineer of the Bureau of Mines from the ore zone, which, when composited, were representative of all the exposed ore. Preliminary tests were made on lot B, and final tests wore made on the composite sample. The Trans-Oceanic property is about 20 miles southeast of Barstow, near Newberry, in the. Pisgah mining district, Calif. The sample, submitted by the owners, was taken from a 1,000-ton reject clump from a hand-sorting operation. The ore occurs as a replacement of rhyolite.

Jan 1, 1952

By K. C. Dean

During the course of the investigation of manganese mineral occurrences in the western United States, the Bureau of Mines collected several lots of ore' from properties in the vicinity of Winkelman, Ariz. As none of the ores would be marketable directly, an investigation was made to determine their amenability to concentration by ore dressing. The Geronimo group of claims is in Pinal County, 8 miles west of Winkelman, Ariz. The manganese oxides occur as cementing material in ore zones of conglomerate. Representative samples of a 2-ton lot of ore cut from outcrops of two lenticular deposits were laboratory-tested. Two 1-ton samples from the Benningfield property were similar in physical characteristics but differed in grade. This claim is 11-1/2 miles south of Winkelman and about 1 mile west of the San Pedro River on the south side of Putman, Wash. The manganese minerals occurred as nodules and lenses, replacing limestone, in a capping over a dark, igneous dike. The North Star group consists of five claims on the west side of the San Pedro River 14 miles south of Winkelman. The ore consists of a low-grade, manganese oxide-calcite occurrence interspersed with stringers of higher-grade material and is present as filling in a fissure zone in porphyry. Two samples were obtained by the examining engineer; one sample represented run-of-mine material, the other represented ore from the vein that could be hand-sorted or selectively mined.

Jan 1, 1952

By Jr. Sillers

To prove to .the satisfaction of all concerned that electrolytic manganese from our low-grade domestic ores could be substituted satisfactorily for ferro-manganese made from high-grade foreign fires, an extensive series of tests was conducted in cooperation with industry, in which electrolytic manganese pro-duced by, the Bureau of Mines at its Boulder City, Nev., Station was substituted for the ordinary ferro grades in the production of ferrous and nonferrous metals and alloys and welding-rod coatings. Over 1,200,000 pounds of manganese was given out for this purpose. The objectives of the tests were accomplished, and for some purposes electrolytic manganese was shown to be superior to other grades because of its high purity. The only serious objection that can be raised against electrolytic manganese is its price, which puts it out of reach for most purposes. Even if the price were to be lowered to a point where it would be in line with ferro grades, it is questionable whether electrolytic manganese from domestic ores could supply more than a small part of the needs of American industry because of the large volume of domestic ore that would have to be processed to supply a satisfactory feed for the electrolytic process. Thus, although electrolytic manganese is highly desirable from a metallurgical standpoint, it could not be expected to substitute for more than a fraction of our domestic manganese requirements.

Jan 1, 1952

By Heber E. Peterson, Sill. Claude W.

"INTRODUCTION In the usual volumetric determination of uranium, the solution containing uranium is reduced in a Jones reductor, yielding a mixture of trivalent and tetravalent uranium; the trivalent uranium is oxidized to the tetravalent state by bubbling a stream of air through the solution. The resulting solution of tetravalent uranium is titrated with a standard oxidant, generally sulfatoceric acid, dichromate, or permanganate. It seemed likely that the same general procedure could be used in determining semimicro quantities pf uranium if the conditions affecting the variables involved were understood more clearly than at present. In the method described below, the use of ferric sulfate to oxidize tetravalent uranium allows the titration to be made at room temperature in an essentially colorless solution with sulfatoceric acid. The latter oxidant in turn permits the use of the very stable indicator, ferroin; with its sharp color change and exactly reproducible blanks.Solutions of uranyl sulfate were prepared by diluting a stock solution that had been standardized gravimetrically according to the method of Lundell and Knowles (8).3/ Solutions of sulfatoceric acid were prepared according to the directions of G. F. Smith (12) and were standardized against arsenic trioxide in the presence of osmic acid according to the directions of Glen (5). The cerium solutions were stored in 18-liter carboys fitted with siphon arrangements so that the bottles did not need to be opened and protected from light in a dark cupboard. Under these conditions, even the 0.01 N solution changed by less than 1 part per thousand over a period of about 6 months."

Jun 1, 1952

By Rollie P. Dobyns

The K.M.A. reservoir was discovered to be oil bearing at a depth of 3,719 feet on March 11, 1931. Extensive development, however, was not begun immediately, because the discovery well had a low initial daily oil production, and market conditions for oil were unfavorable. Development of the field progressed slowly for the next 6.5 years. In the latter part of 1937, a wildcat well approximately 2 miles southwest of the discovery well was drilled on a magnetometer high and completed with an initial flowing production of 2,018 barrels of 430 A.P.I.-gravity oil in 12 hours. Rapid development of the southwestern part of the K.M.A. field was begun immediately and continued until over 700 wells were drilled and approximately 12,500 acres proved oil productive. Because of the large size of the entire K.M.A. field, this report is limited in scope to the southwestern part only, and the discussion that follows pertains to this area only. The closing date for production statistics is August 1, 1949. The K.M.A.? structure is a complex anticline having a maximum closure of 250 feet, and the K.M.A. formation is composed of sediments that grade from limestone through sandy lime and limy sand to sandstone with thin streaks of shale. Two "distinct members of the K.M.A. formation, zone I and zone II, are oil productive. Core analyses indicate the average porosity to be 16.5 percent for zone I and 16.1 percent for zone II. A relationship was established from core data, which showed the correlative permeabilities to be 42.1 millidarcys for zone I and 39.5 millidarcys for zone II, whereas the arithmetical averages of the permeabilities were 84 millidarcys for zone I and 216 millidarcys for zone II. Connate-water saturations were 17.5 percent for zone I and 20.0 percent for zone II. The porosity-saturation method, using a thickness-correction factor, was employed to calculate the volume of 168.1 million barrels of stock-tank oil initially in place in the reservoir. Analyses of the reservoir oil indicate that, although the initial reservoir pressure was 1,750 p.s.i., the original reservoir oil was saturated to only 1,300 p.s.i., at which pressure 1 barrel of stock-tank oil contained 525 cubic feet of ea~ in solution.

Jan 1, 1952

By H. Kenworthy

Sulfide-ore concentrates containing cobalt, nickel, copper, lead, and iron from the operations of the National Lead Co. at. Fredericktown, Mo., were treated successfully on a laboratory scale to recover more than 90 percent of the cobalt, nickel, and copper. A cobalt -nickel-bearing, lead-copper matte., produced by the St. Joseph Lead Co. at Herculaneum, Mo., was treated to produce a lead-zinc fume, a copper sulfide concentrate, and a cobalt nickel-iron product, netting a recovery of over 75 percent of the cobalt and about 90 percent of the nickel and copper. National Lead Co. bulk concentrates were chlorinated with gaseous chlorine to form anhydrous metal chlorides and sulfur chlorides, sulfur chlorides were recovered by distillation, a high percentage of the ferric chloride was converted to ferric oxide, and the chlorinated residual metals were extracted with water. Metal ions were removed from leach liquors by pH-controlled fractional precipitation as hydroxides. Cobalt solutions "were prepared from cobaltic hydroxide, and procedures were developed to remove contaminating metal ions. Purified cobalt solutions were employed as electrolytes for deposition of high-purity cobalt.

Jan 1, 1953

By Bernard Lewis

This report summarizes fundamental research end technical studies conducted in the Explosives and Physical Sciences Division, Region VIII, of the Bureau of Mines in the 2 years July l, 1950, to June 30, 1952. It is the fifteenth of a series of, ordinarily, annual reports whose aim has been to provide the reader with a resume of the research results that have appeared in published form during each fiscal year under the authorship of members of the staff. These are referred to throughout the report. ACKNOWLEDGMENTS Acknowledgments art, made to the following members of the Division wider whose mediate supervision the described studies were carried out. Stuart R. Brinkley, Jr., chief, Mathematical and Theoretical Physics Section, and special assistant to the chief of the division.

Jan 1, 1953

By J. B. Gayle

In a modern blast furnace, production depends, to a large extent, on the rate at which the furnace gases can be forced through the charge. Since these gases must make their way through the voids between particles of coke, ore, and limestone, the size and size distribution of the stock-column materials are of considerable importance. Also, because the coke pieces support the weight of the overburden and provide the majority of the voids through which the gases pass, their ability to withstand the shattering and abrading forces to which they are subjected should be related to the maximum obtainable production for any particular furnace. Although the wide acceptance of this point of view is indicated by the ever-increasing demand for stronger and more uniform blast-furnace cokes, economic considerations demand that a quantitative evaluation of the relation between coke quality and blast-furnace performance be made available to the industry at the earliest possible date. The following studies of size-distribution patterns and breakage processes were, therefore, conducted as a part of a preliminary investigation intended as a basis for future studies of the relation between coke quality and blast-furnace performance. The major findings may be summarized as follows: 1. New evidence for the presence of two independent distributions of sizes in run-of-oven cokes has been obtained, and a method for characterizing and estimating the relative importance of the individual distributions has been demonstrated. This method has also been used to study the different types of degradation taking place during the tumbler test.

Jan 1, 1954

By Alfred Traverse

The Brandon lignite is a small deposit of very low rank coal near the village of Forestdale in the town of Brandon, Vt. It occurs in association with other sediments, principally sands and silts. This lignitic coal has attracted considerable scientific interest since the middle of the 19th century because of the abundance of fossils in the sediment and the rarity of lignite in New England. A cooperative investigation has been developed by E. S. Barghoorn, W. Spackman, and the author in which different phases of the problem have been worked on in a coordinated research program. This paper presents results of an investigation of the very abundant fossil pollen and spores and some other microfossils of the deposit. The studies on which this manuscript is based were made in large part at Harvard University in partial fulfillment of the requirements for a Ph. D. degree.

Jan 1, 1955

The complex organic chemicals in coal differ from those in petroleum mainly by the ratio of carbon atoms to hydrogen atoms; this ratio is about 2 for coal and 1 for petroleum. By changing the ratio, coal can be converted into compounds similar to those found in petroleum. In. very simplified form, omitting here the special conditions required, the paths by which this can be done are: [ ] Part or all of the coal is first gasified by reaction with steam and oxygen, either in a gasifier or while the coal is still in place underground. The resulting gas is mainly hydrogen and carbon monoxide, with impurities that .must be removed before further processing by one of the following routes.

Jan 1, 1959

By J. B. Zadra

Tungsten metal, chemically equivalent to commercial grade, is produced by electrolysis of impure tungsten compounds or scheelite in an alkali, phosphate or borate electrolyte. A preliminary investigation of fused-bath electrolysis shows the effect of electrolyte composition, temperature, and current density on current efficiency, yield, crystal structure, and purity of product. Experiments show that tungsten can be electrowon from scheelite in a fused alkali, phosphate, or borate bath with similar results. Studies on electrolyte composition show that the addition of sodium chloride is essential to both electrolytes in treating scheelite. Although its main function is to react with or flux the CaO, it also increases the bath fluidity. Temperature studies revealed optimum ranges between 900° and 1,100° C.; 900° C. proved satisfactory for tungsten trioxide, and 950° to 1,050° C. for scheelite. Current efficiencies were satisfactory for all current densities ranging from 10 to 57 a./dm.2. Yields were 400 to 650 g./kw.-hr. over the same current-density range. Crystal size and purity of the product are functions of temperature, current density, and amount of impurities in the electrolyte. Deposited crystals vary in shape from spherical grains to clusters of dendritic hexagonal needles, and in size from smaller than 35 to 570 microns. The purity of the tungsten metal produced ranges from 99.7 to 99.94 percent.

Jan 1, 1959

By J. D. Ramsdell

To obtain information on the effects of cobalt on microstructure and tensile properties of titanium-vanadium-cobalt alloys, the composition ranges of 4 to 16 percent vanadium with 1 to 4 percent cobalt have been studied. The beta phase was not completely retained with vanadium additions up to 16 weight-percent or in the same alloys containing up to 4 percent cobalt.

Jan 1, 1960

By John D. Bardill

A cooperative project between the Bureau of Mines, Department of the Interior, and the Montana School of Mines, investigating results of hydraulic systems for transporting sand slurries for emplacement, was begun in August 1955. In such circumstances, the Bureau provides funds for a fellowship leading to a Master of Science degree as well as available instruments, tools, supplies and equipment. The School provides the ore-beneficiating laboratory with its equipment for use as a pilot plant. The success of a hydraulic backfilling method employing mill tailings depends largely upon the physical characteristics of the tailings. One of these characteristics is size distribution, especially in the finer size ranges. When being emplaced underground, almost impervious layers of slimes separate from some types of mill tailings containing a high percentage of slimes and settle on the top of the sand fill. These coatings may be so dense that the water in the slurry cannot percolate through them for proper drainage. Successive layers of fill in a stope, each with an impervious coating on top, sometimes build up a hydrostatic head, creating pressure on the bulkheads. This may cause breaks in the lining material, inducing sand runs and flooding the level and sumps below. Deleterious slimes flocculated and disseminated throughout the sands should help prevent the formation of impervious slime layers, increasing percolation and settling rates.

Jan 1, 1960

By M. Vanpée, H. G. Wolfhard

Jets of hot gases issuing into explosive gaseous mixtures are efficient agents of ignition . The ignition temperature is defined as the temperature of the jet as it enters the cold explosive mixture which is just high enough to produce ignition . Such data have been published recently.5/ The investigators note especially that no correlation seems to exist between hot - gas ignition temperatures and spontaneous ignition temperatures , although there is a rather loose relation with limit flame temperatures . Before a more quantitative theory of the hot - gas ignition process can be attempted effectively , several questions must be answered : ( 1 ) Can the reactions leading to ignition be described by an Arrhenius type activation energy? ( 2 ) Is ignition preceded by an induction period ? ( 3 ) What is the rate - determining process of the ignition ? (4) And how does turbulence affect this type of ignition ?

Jul 1, 1960