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By A. D. Hahn

This report describes and gives the results of an examination by the Federal Bureau of Mines of ilmenite-bearing placer sand deposits in the 24-mile long valley of Otter Creek, Kiowa and Tillman Counties, Okla. Drilling and sampling was completed in three periods between October 1956 and September 1957. Mineralogic studies and mineral-dressing tests on recovery of ilmenite and other heavy minerals from composited samples of the sands were made in Bureau of Mines laboratories at Rolla, Mo., in 1957 and early 1958. Otter Creek rises in and drains the southwestern extremity of the Wichita Mountains, which are represented locally by knolls and ridges of gabbro and granite surrounded by plains floored with flat-lying Permian red beds. The valley fill consists of a basal sand-clay component, derived from weathering of the igneous rocks, and an overlying silt-clay alluvium. Ilmenite is present in significant quantity and recoverable grain size only in the basal sand-clay.

Jan 1, 1960

By W. J. Wenger

THIRTY-FOUR analyses of crude oils from the fields of the Four Corners Area of Arizona, Colorado, New Mexico, and Utah are presented and compared. The samples, taken from formations in four geological time periods, have high gravity and low-sulfur, -nitrogen, and -asphalt content. Generally, the oils are paraffinic in the low-boiling fractions, with increasing naphthenicity in the higher-boiling fractions. Oils from Cretaceous formations resemble other Cretaceous oils in the Rocky Mountains, but oils from Permian and Pennsylvania formations are unlike other oils of these ages in the Rooky Mountains. The differences in the oils are minor and cannot be used to distinguish between fields or between producing formations. With minimum special processing, the oils should yield large amounts of good-quality motor fuels. INTRODUCTION The only place in the United States where four States have a common junction is known as the Four Corners Area. This area (fig. 1) includes the northeast corner of Arizona, the southwest corner of Colorado, the northwest corner of New Mexico, and the southeast corner of Utah. It includes three major geological basins: The Black Mesa, the San Juan, and the Paradox. Major oil developments have occurred in both the San Juan and Paradox basins, but no discovery of commercial importance has been made in the Black Mesa basin.

Jan 1, 1960

By F. E. Block

This investigation was made as part of a larger program to develop basically new methods for preparing yttrium metal in high-purity form. It was performed under a cooperative agreement between the U.S. Atomic Energy Commission (AEC) and the Federal Bureau of Mines. Laboratory-scale tests were made to devise methods for preparing high-purity, anhydrous yttrium trichloride, for reducing the yttrium trichloride with sodium or lithium, and for consolidating the resulting yttrium sponge into ingots.

Jan 1, 1960

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 J. S. Berber

Bastnasite is a natural fluocarbonate of the cerium group and affords an abundant and high-grade source of the lighter rare-earth elements. As part of a broad research program in rare-earth element technology, the Federal Bureau of Mines directed extensive experimental work to separating and purifying the rare-earth elements in bastnasite. By the use of a combination of techniques--classical chemical, ion exchange, and solvent extraction--the processing of a bastnasite concentrate to obtain the individual rare-earth elements, or groups of elements, was accomplished. A bastnasite concentrate, containing about 60 percent rare-earth oxides, was sulfated with concentrated sulfuric acid to eliminate the carbon dioxide, fluorine, and silica. Calcination at 1,200° F. made the gangue matter insoluble, thus permitting the separation of the soluble rare-earth sulfates. Essentially 100 percent of the rare-earth elements were recovered by this procedure. Since the rare-earth sulfate solution contained only trace amounts of nonrare-earth elements, subsequent separation procedures were simplified.

Jan 1, 1960

By D. D. Walker

Scheelite, the most abundant tungsten mineral in the Philipsburg region of Montana, is found in replacement deposits and along fissures and cracks in limestone at various distances from contacts with acidic igneous rocks. It also occurs at the limestone-igneous contacts, but typical garnet tactites are developed in only a few places in the region. The most favorable host rocks for scheelite mineralization are the Jefferson, Hasmark, and Madison limestones. Scheelite is exposed in float, outcrops, and surface and mine workings along a 2-mile-wide belt extending southwest from Lost Creek beyond Silver Lake, a distance of 15 miles or more. (See fig. 1.) Some scheelite is found in veins formerly mined for silver. Powellite and molybdenite occasionally are present with the scheelite. Hubnerite occurs in quartz veins in the Black Pine area 10 miles northwest of Philipsburg. These quartz veins occur in the quartzites of the Precambrian Spokane formation. Tungsten production in the region has come almost exclusively from scheelite deposits, both lode and placer. During a 6-year period beginning in 1943 a total of 142.0 tons of 63-percent W03 concentrate was produced by H & H Mines Co. In the early 1950's, the Trigger mine produced 4,000 tons of 1-percent W03 ore and the Tip Top 650 tons of 2.0-percent W03 ore and 2,906 tons of 2.2-percent ore. There has been sporadic production from some of the smaller properties in the area.

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 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 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 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 H. H. Heady

A naphtha obtained by destructive, recycle hydrogenation of crude shale oil, produced by gas-combustion retorting of Colorado oil shale, was found by the Bureau of Mines to contain 49.1 percent paraffins, 20.3 percent cycloparaffins, 7.8 percent olefins, and 22.8 percent aromatics. The naphtha contained only minor amounts of sulfur, nitrogen, and oxygen compounds. Compounds containing less than 5 carbon-atoms per molecule were removed by distillation before analysis. The paraffins where predominantly straight-chain compounds; n-Hexane was present in the largest quantity, and the other straight-chain paraffins decreased in amount as the molecular weight increased. The cycloparaffins, which contained both cyclopentanes and cyclohexanes, were evenly distributed throughout the boiling range. Although the naphtha had been produced by hydrogenation, it contained a small quantity of olefins. Straight-chain olefins with a terminal double bond comprised about two-thirds of these compounds. Among olefins with an internal double bond, those having trans configuration were present in three times the quantity of those in the cis form. In the aromatics all but one of the alkylbenzenes having nine or less carbon-atoms per molecule were identified; toluene was present in the greatest quantity. Only a few of the higher molecular-weight homologs were identified. The composition of the naphtha was computed from analyses of 105 narrow¬boiling distillation fractions. Volume, density, refractive indices, bromine number, and an ultraviolet spectrum were determined on each fraction. From these data the hydrocarbon-group composition of each fraction was estimated. A silica gel adsorption analysis was used to check the values of nearly one-third of the fraction calculated from physical-property data. Mass and infrared spectra were obtained on some fractions for identifying individual compounds or types of compounds, such as terminal olefins.

Jan 1, 1960

By R. M. Becker

THIS IS a progress report on a study of the application of statistical practice to mine and mineral sampling undertaken by the Federal Bureau of Mines to provide sound theoretical and practical data for use of the mineral engineering professions. One of the problems in mine sampling is determining the reliability of the results. For certain types of sampling data (random data) the reliability of the results can be stated mathematically. For other types of data there is no known means of quantitatively expressing reliability. In applying measures of reliability to a set of random data, some knowledge or assumption of the characteristics of the particular data is necessary. In many fields these characteristics are well known. However, in mining, where the data are in assays, these characteristics are not well known.

Jan 1, 1961

By W. H. Ode

Because trade increased among various nations after World War II, the Coal Committee of the Economic Commission for Europe established a Classification Working Party in 1949 to develop an International system for classifying coal. Although national classification systems existed, they had been developed in accordance with characteristics of domestic coals without reference to coals of other countries. Terms for describing similar or identical coals differed in each nation. This caused confusion in evaluating coals shipped in international trade and also hampered exchange of technical information on problems of coal utilization. Experts4/ participating in the classification project early in their work agreed that two systems should be formulated, one for the higher rank coals or so-called "hard" coals in European terminology and the other one for the lower rank coals, the latter designated mainly as brown coals and lignites in the various countries. Rank refers to the degree of metamorphism (progressive alteration) in the natural coalification series from lignite and brown coal to anthracite. The system for classification of hard coals was published late in 1956 as a document of the United Nations.5/ Results of a study for applying this system to American coals were published in 1958.6/

Jan 1, 1960

By M. F. Koehler

[THE LITERATURE contains relatively few thermodynamic values for interoxidic compounds, and these often are unreliable. This is especially true of data for ferrites and aluminates for which heat of formation determinations may involve extreme experimental difficulties. This report contains the results of new experimental work for obtaining the heats of formation of five ferrites (Ca2Fe2O5, CaFe2O4, MgFe2O4,, NaFeO2, and LiFeO2) and one aluminate (CaAl4O7), and a review and revision of previous similar work of this laboratory on five aluminates (Ca3A12O6,, 12/7 CaO-Al2O3, CaAl2O4, NaA1O2, and LiAlO2), The results for the 11 compounds are combined with entropy and high-temperature heat content data to derive tables of heats and free energies of formation (both from the oxides and from the elements) for the temperature range 298° 1,800° K, The relative stabilities of the compounds are discussed. The presented data all have application to ceramic reactions, and those for the calcium and sodium aluminates are applicable in considering soda-lime sintering processes for extracting alumina from silicate minerals such as day and labradorite.]

Jan 1, 1961

By W. J. Wenger

Oil fields in the Powder River Basin of Wyoming have produced 731 million barrels of petroleum through 1959. Production in 1959 was 32 million barrels, the highest production since 1924. The record production was in 1923, when the Basin produced 38 million barrels of oil and the Salt Creek field, then at its peak, produced 35 million barrels. In this report, the characteristics of crude oils found in the Basin are used as a basis for determining the best re-fining uses for the oils and for predicting the characteristics of oils that may be discovered in the Basin in the future. Analyses of 108 oils sampled over a period of 30 years are presented Crude oils of two major types are produced from the Powder River Basin. One has a low sulfur content and occurs in younger formations, and the other has a high sulfur content and occurs in older formations. The oils with low sulfur contents are generally light colored and waxy, and may be either paraffinic or naphthenic. The oils with high sulfur contents are usually dark colored and asphaltic; only their low boiling fractions are paraffinic. Alteration appears to account for the anomalous properties of some oils found at shallow depths. Shapes and slopes of correlation index curves classify the oils into the same two groups as their sulfur contents, with gently sloping curves representing the low-sulfur oils and steep curves representing high-sulfur, asphaltic oils,

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

By Paul L. Campbell

Investigations by the Federal Bureau of Mines of methods of upgrading tar obtained by low-temperature carbonization of lignite showed that ß,ß?-oxydipropionitrile, ß,ß?-iminodipropionitrile, and ß,ß'-thiodipropionitrile were effective solvents for extracting aromatics (aromatic hydrocarbons plus polar compounds) from coal-tar neutral distillate fractions. Batch extraction showed that these solvents extracted approximately the same percentage of aromatics from various neutral oil fractions boiling between approximately 170° and 350° C. In continuous countercurrent extractions using oxydipropionitrile and iminodipropionitrile, approximately 30 to 35 vol.-pct, and 65 to 70 vol.-pct, of the aromatics in 170° to 350° C. neutral distillate oil were extracted at room temperature when solvent-to-oil ratios were 2:1 and 12:1, respectively. As the concentration of aromatics in the neutral distillate oil fraction decreased, the capacities and, to some extent, the selectivities of these solvents for the remaining aromatics decreased. Aromatics were isolated from the extracts and the solvents recovered by washing the extract fractions with a low-boiling paraffinic hydrocarbon such as heptane, using hydrocarbon-to-extract ratios of at least 2:1. The heptane wash removed most of the aromatics but only part of the polar compounds (compounds containing oxygen, sulfur, and nitrogen) from the extracts. The recovered oxydipropionitrile and iminodipropionitrile, containing polar compounds, were effective in extracting aromatics from neutral distillate oils. The contaminated solvents showed essentially the same capacities and selectivities as the pure solvents.

Jan 1, 1961

By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

By W. A. Calhoun

The purpose of this investigation was to develop economical mineral dressing processes for removing objectionable quantities of impurities, such as quartz and pyrite, from refractory clay deposits in east central Missouri. The presence of excessive quartz in these clays causes crazing. Pyrite causes bloating and unsightly dark blobs on the surface of fired refractory brick. The iron concentration in the proper state of oxidation may also act as nucleation centers for carbon crystal growth which can result in bursting of the refractory. Numerous deposits, representing a very large tonnage, have been examined and prospected by various refractories companies and found to contain impurities in objectionable quantities. Upgrading these clays would greatly extend our reserves of high-quality refractory clays. Wet-tabling and wet-cyclone concentration were found to be effective for removal of impurities from clays. Of the two methods, wet-cyclone concentra¬tion would be cheaper and more effective. Although wet-tabling improved the refractory properties of each clay, beneficiation by wet-cyclone produced clays of superior quality. Clay recoveries by wet-cycloning ranged from 56.1 to 81.8 percent of the weight of the crude samples, and the beneficiated clays contained from 71.9 to 94.4 percent of the total alumina. The pyrometric cone equivalent (PCE) was increased from 1 to 3 cones by wet-cycloning. The beneficiated clays also met the reheat shrinkage requirements on refiring to 1,400° C. Missouri is one of the major domestic sources of fare clay. In addition to deposits of high-grade refractory clays, there arc many deposits that contain small percentages of impurities, which render the clays unfit for the production of high-heat-duty firebrick. Development of methods to beneficiate these submarginal clays to usable materials would greatly increase commercial fire clay resources.

Jan 1, 1961