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By Raymond L. Carpenter

In connection with its continuing studies of the characteristics of alloys and alloying elements, the Bureau of Mines investigated the crystal structure of fused boron. This report describes how the structure of fused boron was found to be rhombohedral by the powder method for crystal-structure determinations by X-ray diffraction. The determinations of the crystal structure of boron reported in the literature were made on crystals prepared by various methods such as electrolysis, thermal decomposition of a boride, or by hydrogen reduction of boron tribromide. Table 1 summarizes the data found in the literature on the crystal structure of boron. The information shows the following: (1) Three structures have been reported for boron, (2) boron prepared by different processes--or even by varied conditions of a process--produces crystals of different structure, and (3) no information is given on the crystal structure of fused boron.

Jan 1, 1960

By L. J. Kane

Conventional methods for determining the size of dust suspended in a gas require that agglomerates (clusters of particles) first be broken into particles, but in evaluating industrial dust-removing equipment the size of the agglomerates as they actually exist in the gas stream is far more important. This paper presents results of an investigation by the Federal Bureau of Mines to develop methods for determining the size of dust agglomerates suspended in a gas stream. The studies are part of the Bureau's continuing research on synthetic liquid fuels. The size and size-distribution of agglomerates as they exist when the gas reaches the filter was determined by using a membrane filter in conjunction with a dust count under a microscope. A membrane filter is a cellulosic sheet about 150 microns thick containing millions of holes per square centimeter--holes of uniform diameter that run directly through the sheet without interconnection.

Jan 1, 1960

By Warren M. Mahan

A rotary kiln process was developed by the Federal Bureau of Mines to produce consistently an iron product containing 3 to 7 percent nickel. Cuban laterite and serpentine ores were smelted in a gas-fired batch-rotary kiln) 5 feet in diameter and 9 feet long. The metal contained 2 to 4 percent carbon, with little or no silicon, and could be produced on a large scale with modest capital investment. A total of 121 tests was run using this procedure. The tests were conducted with a maximum temperature of 2,625° F., using linings of firebrick containing 40 to 70 percent alumina. Slags in the kiln were acid to neutral. The material in each batch passed through three stages: (1) Sponge metal, (2) carburization, and (3) balling and meltdown. Half the tests were made while firing the kiln with atmospheric-temperature air; the remainder were fired with preheated air. Tests showed that preheated air decreased fuel requirements, dust losses, and reducing agent, and increased the capacity of the kiln.

Jan 1, 1960

By T. A. Sullivan

Research undertaken by the Bureau of Mines in 1938 has resulted in the development of titanium from a laboratory curiosity to a commercial metal. Along with processes for producing the metal, it was necessary for the Bureau to develop methods for analyzing the metal, raw materials, and intermediate products. Some of the methods developed have been published.3 4 5/ General Services Administration (GSA) was responsible for purchasing titanium metal under Defense Production Act contracts with commercial producers. GSA designated the Federal Bureau of Mines to analyze this metal and establish its compliance with Government specifications. A substantial quantity of tin was found in some of the samples analyzed, and in July 1957 tin was added to the list of impurity elements to be determined. The specifications limited the amount of tin in titanium sponge to a maximum of 0.10 percent. A program was immediately initiated to investigate methods and techniques for determining tin in the range of 0 to 1.0 percent. A method accurate at the 0.10 percent level was necessary, as this level was the critical range for acceptance or rejection of the metal.

Jan 1, 1960

By Norwood B. Melcher

This report describes preliminary experiments by the Federal Bureau of Mines on the practicability of adding raw pellets of taconite concentrate to blast furnace feeds. The usual industrial practice is to harden the pellets by heating before they are charged to the furnace. The Bureau research demonstrated that raw pellets could be successfully smelted in an experimental furnace with no significant change in coke consumption and only a moderate increase in dust losses. The dust loss was 43 pounds per ton of metal for an all-pellet charge, compared with 7 pounds per ton for an all-sinter charge. Raw taconite pellets undergo only slight degradation during charging to the furnace if 1 percent bentonite is used as a binder. INTRODUCTION Fines and concentrates must be consolidated or agglomerated into larger masses before they can be smelted in a commercial blast furnace. Such agglomeration is usually done by sintering, pelletizing, nodulizing, or briquetting. Sintering has been the more common practice, but with the advent of taconite concentrates pelletizing is increasing in importance.

Jan 1, 1960

By A. L. Engel

This publication describes further research by the Federal Bureau of Mines in beneficiating domestic manganese ores. The ores selected for treatment were typical of many manganese deposits in California and Nevada in that they have not been economical to mine because they are low grade or contaminated with siliceous minerals and are not amenable to physical concentration.3 4/ It would be desirable to develop a simple treatment method resulting in nearly complete extraction of manganese from these ores and applicable to small-scale operations. Sulfation reduction appeared to be such a method. The studies reported in this publication were directed toward sawdust or lignin-sulfonates as reducing agents. Sawdust, as waste from lumbering, and lignin-sulfonates, byproducts of woodpulp papermaking, are comparatively cheap and may be available in areas where manganese ores are found. Sugar, oils, and coal were also tried as reducing agents.

Jan 1, 1960

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960

By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By C. G. Kirkland

An apparatus for determining trace impurities in Grade-A helium by mass spectrometer methods was designed and built by the Federal Bureau of Mines. Grade-A is the designation for helium commercially produced by the Bureau. Its nominal purity is 99.995 percent. The device, following a suggestion by Deaton, concentrates the impurities in the helium by freezing them out in a coil-and-trap assembly cooled by liquid helium. A known volume of helium is passed through the trap, the concentration ratio determined, and samples of the concentrated impurities are analyzed by mass spectrometer methods. The apparatus has been in service for approximately 20 months and has satisfactorily met all requirements. Over 200 analyses were made of helium contained in conventional cylinders, obtained from the Amarillo, Exell, Otis, and Navajo Helium Plants, during the 6-month period ending March I, 1959. Total impurity concentrations, in parts per million, were as follows: Amarillo, 19.1; Exell, 17.1; Otis, 11.3; and Navajo, 6.6. Neon and nitrogen were the major impurities. Complete data are shown in table 4 in the body of this report.

Jan 1, 1960

By M. G. Zabetakis

This publication describes an investigation conducted by the Federal Bureau of Mines regarding the cause of an explosion of a dephlegmator or fractionating column at the Cities Service Oil Company Refinery, Ponca City, Okla., January 22, 1959. The column was that used with the refinery's No.1 Dubbs Coker. The explosion caused the death of an employee of the refinery and resulted in extensive damage to the refinery and to nearby property. The Bureau's study of the explosion began January 26.

Jan 1, 1960

By G. V. Sullivan

This report describes an investigation by the Bureau of Mines of flotation techniques for the recovery of chromite from fine-grained disseminated ores. Reported work on the concentration of chromiferous materials shows that flotation has been applied almost exclusively to slime-free pulps. Therefore, chromium recoveries that could be obtained by flotation were related to the amount of slime rejected. However, results of recent studies by the Bureau of Mines showed that des liming is not a requisite to selective concentration of chromite. Laboratory-scale tests on seven ore types from the more important chromium-bearing areas of the Pacific Northwest showed flotation to be technically feasible for treatment of all but one of the samples. Concentrate grades were affected more by the composition of the chromite mineral than by the grade or character of the ore. Test results from three of the samples showed that, without prior desliming of the pulp, 78 to 91 percent of the chromium could be recovered in concentrates of 90 percent or more chromite; two samples responded to similar treatment, resulting in concentrates of more than 80 percent chromite with recoveries of 85 and 89 percent chromium. One sample of mill products, subjected to severe weathering, required removal of the primary slime to obtain a concentrate of 65 percent chromite with only 75 percent chromium recovery.

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 E. J. Ostrowski

The Bureau of Mines experimental blast furnace, Bruceton, Pa., was operated to determine the feasibility of replacing part of the burden coke requirements with solid fuels injected directly into the smelting zone. This report describes preliminary experiments and information resulting from such an interchange. These experiments were made on an all-sinter burden, using two parts sinter to one part fuel. Anthracite fines were injected intermittently into the smelting zone of the furnace by compressed air through auxiliary tuyeres. The interval between injection periods ranged from 5 to 15 minutes. A maximum of 28 percent of the stock column coke bur-den was replaced. This percentage replacement caused furnace malfunction, but the overall percentage of these experiments indicated that 20 to 24 percent of the coke requirements could be replaced in this way. The metallurgical coke consumption was decreased by as much as 377 pounds (25.3 percent) per ton of pig metal produced. Buckwheat anthracite No.4 was used in this experiment; however, such solids as bituminous coal or coke fines also could be used. The frequency as well as the quantity of solid fuel injected has a direct bearing on furnace performance.

Jan 1, 1960

By A. J. Barry

Two methods of testing anchorages of headed expansion-type mine roof bolts were investigated by the Federal Bureau of Mines to determine whether they are acceptable for general use. In both methods a load was applied to a tightened bolt with a hydraulic jack. A total of 80 tests, 40 using each method, was conducted in 4 test areas in 3 commercial coal mines. Electric resistance strain gages were used in all tests to indicate true bolt load as the bolt was tightened and when an additional load was applied with the hydraulic jack. The results indicate that: 1. The relationship between the true bolt load and the jack load will vary according to the test method until the two loads become equal. The bolt load-jack load relationship below this point can be determined only with strain gages. 2. The point at which the two loads become equal can be estimated by noting the load when the hardened washer becomes loose in one method, and when the bearing plate becomes loose from the roof in the other. It also can be approximated for either method of testing by noting the load when the first abrupt change in the slope of the jack load-bolt displacement curve occurs. 3. The anchorage characteristics of the test bolt can be determined from the data obtained from either method by examining the slope of the jack load-bolt displacement curve above the point at which the true bolt load is equal to the jack load.

Jan 1, 1960

By V. B. Dale

This paper is one of a Federal Bureau of Mines series covering the mineral resources of the Nation. It briefly describes most of the tungsten deposits in Cochise, Pima, and Santa Cruz Counties, Ariz. Most of the descriptions are from field examinations by the two senior writers, prior to July 1957. Wolframite first was identified in Arizona in 1896 by W. P. Blake, Territorial Geologist. Tungsten mining began about 1900 in the Little Dragoon deposits of Cochise County, and about 1901 in Las Guijas district of Pima County. The price history of tungsten is an erratic one; consequently, production has been erratic. Prices rise during wars and periods of national preparedness. Production of tungsten ore was stimulated greatly by a Government purchasing program, announced on May 10, 1951, wherein the Government agreed to purchase standard-grade tungsten concentrates at $63 per short ton unit5/ for 5 years or until 1,468,750 units were purchased. This was later increased to 3,000,000 units, and after this amount had been purchased in June 1956, the purchase of an additional 1,500,000 units was authorized. Government purchase, however, was suspended in December 1956 before completion of this latter program, and the price of tungsten concentrates declined sharply. The price had dropped to $15 per short ton unit, duty extra,6/ by the last part of July 1957.

Jan 1, 1960

By Joel N. Van Sant

The rapidly expanding economy of the West, with its growth of heavy industry, and increased steel production, is primarily responsible for the refractory clay industry's concern over the adequacy of the clay supply in States of the Great Plains and Rocky Mountains. Hence, the investigation by the Federal Bureau of Mines of the occurrence and use of refractory clays in North Dakota, South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona has been encouraged by the major consumers and producers of this commodity. The Wyoming investigation is a part of the national program devised to close gaps in the domestic supply of specific types of clays to determine their characteristics and properties and to provide information that will assist the refractory-clay industry. Forty-two locations of clay-bearing rock in 17 areas in Wyoming were examined (fig. 1). Location 3 was not examined during this survey. Its description was taken from an earlier report. Locations 20, 21, and 22 were previously reported but were, also, examined by the Bureau. No samples were collected from these locations because field examination indicated that the shales were not refractory grade. The Hulett, Aladdin, and Newcastle areas are discussed in the section on the Black Hills district; the other 14 areas are described separately.

Jan 1, 1961

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By J. B. Gayle

The rate of oxidation of coals with nitric acid has been used by earlier investigators4 5 6/ for determining fusain and for studying petrographic composition. These workers accumulated considerable evidence indicating that, for coals ranging from lignite to low-volatile in rank, the method gives values for fusain that agree satisfactorily with those obtained by optical methods. One group5/even concluded that, when discrepancies are noted between results obtained by chemical and microscopic methods, the results based on the oxidation reaction are probably the more reliable. Unfortunately, after concluding that the method was valid, most of these workers apparently lost interest. As a result, no attempt to exploit or apply the method to problems of utilization has been reported. Recent studies of the influence of inert petrographic constituents on the properties of cokes made from various coals7/ have indicated a need for additional means of characterizing coals and blends used for carbonization.

Jan 1, 1960

By D. Bienstock

The Fischer-Tropsch synthesis is practicable in a reactor where the exothermic heat of reaction is removed by circulating large quantities of recycle gas through a catalyst bed of high-voids content. At an hourly space velocity of 1100, the feed gas, a mixture of 1.5 parts hydrogen to 1 of carbon monoxide, was converted 90 percent, producing hydrocarbons predominantly in the gasoline range. At these conditions a recycle-to-fresh gas ratio of 40:1 was enough to give excellent temperature control with a pressure drop of 1.5 p.s.i. per foot of bed using a steel catalyst in the form of lathe turnings. Steel parallel plates, although offering lower resistance to gasflow, were less reactive and less durable. INTRODUCTION The Federal Bureau of Mines has been engaged in a research and development program since 1944 on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a synthesis gas--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va.; and the synthesis of gasoline by catalytically reacting the carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By Jack D. Ramsdell

Electrorefined, magnesium-reduced, and sodium-reduced titanium samples were evaluated for recrystallization behavior, effect of cold rolling on tensile properties, and bend ductility. Curves were determined for the softening of 2.5 to 80 percent reduced cold-rolled metal that was annealed over a temperature range of 300° to 800° C. Upon annealing, coarsening of the grains was found to occur for reductions in thickness of less than 20 percent in titanium made by all three processes. The presence of metallic impurities greatly inhibits coarsening for reductions in thickness below 20 percent, but for reductions in excess of 20 percent grain size is essentially constant at each annealing temperature. The three grades of titanium did not harden excessively from cold rolling; both tensile and bend ductility were good for reduction in thickness up to 80 percent. Upon annealing, softening occurs between 400° and 600° C., and, based on microstructure and property studies, full annealing is accomplished after 30 minutes at 700° C. for the magnesium-reduced and electrorefined titanium and at 800° C. for the sodium-reduced titanium.

Jan 1, 1960