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By Eliot J. White

The physical properties and clay mineral content of the major oil-producing formations in the Powder River Basin of Wyoming were determined by analyses of cores from 100 wells. Interrelationships were established among permeability, restored water saturation, clay content, and bulk swelling capacity of the crushed sample and used to estimate the susceptibility of the formations to water damage. The ratio of water permeability to gas permeability (kw/ki) offers a convenient scale for semiquantitatively estimating the water sensitivity of sands. The irreducible water saturation was also found to have a similar relationship to the clay mineral content and the water sensitivity of the sands. The average relation of water permeability to gas permeability is different for each sand, as shown by the curves, and the relative positions of the curves indicate the degree of water sensitivity of each sand from which the susceptibility to water damage may be estimated. How accurately these estimates show formation behavior under field operations will not be known until studies of field performance can be made. The water permeabilities of the Muddy, Minnelusa, and Tensleep sands average about the same as the gas permeabilities, and these sands are classified as insensitive. The water permeabilities of the Sussex and Shannon sands, at the other extreme, are much less than the gas permabilities [when average ki is 30 millidarcys (md), kw is 6.1 md], and these sands are classified as highly water sensitive. The sensitivities of the five other sands are between these extremes.

Jan 1, 1962

By George E. Fish

This report describes investigations conducted by the Bureau of Mines from 1957 through 1959 in the Roseland anorthosite-titanium belt of Nelson and Amherst Counties, Va., for the purpose of studying the titanium resources of the area. Three titanium deposits containing much saprolite ore derived from the decomposition of anorthosite and diorite were selected for detailed study Following a reconnaissance of the reported titanium occurrences in the belt. These three deposits occur in or are associated with anorthosite. Most of the occurrences are situated on or near the contact between the anorthosite and the gneissic country rock. The saprolite deposits are as much as 1.5 miles long, 1,000 feet wide, and 100 teat deep and contain significant reserves of titanium-bearing material estimated in excess of 20 million tons. Where it was penetrated by drilling, the unweathered rock beneath the saprolite contains nearly the same titanium values as the saprolite.

Jan 1, 1962

By M. E. Tyrrell

The purpose of the work leading to this report was two-fold: (1) To determine the properties of cemented tungsten carbide modified by the addition of one, two, and five percent of titanium diboride, and (2) to compare the properties of these mixtures when sintered, hot-pressed, and flash-welded (resistance-sintered). Minor additions of titanium diboride to mixtures of 94 percent WC and 6 percent Co decrease mechanical strength but increase oxidation resistance in proportion to the amount of the addition. One percent of titanium diboride increased the hardness by 2 Rockwell A units. Hot-pressing produced compacts with the highest density and the best mechanical strength, but losses of cobalt were high and grain growth was pronounced.

Jan 1, 1962

By C. J. Thompson

In the course of the work currently conducted by the Bureau of Mines in cooperation with the American Petroleum Institute Research Project 48 on identifying sulfur compounds in petroleum, a micromethod was developed (12)5 for catalytically removing the sulfur atom from sulfur compounds. The product is the residual portion of the molecule; the structure otherwise was unaltered except for hydrogenation of any unsaturated bonds that were present in the original compound. Positive identification of sulfur compounds isolated from crude oils is a difficult problem. Direct comparison of properties of the unknown with those of reference compounds is often impossible because of the limited number of reference sulfur compounds available. However, a relatively large number of pure hydrocarbons is available, and the conversion of the sulfur compound to a hydrocarbon enhances the possibility of identification. The technique also can be used to prepare microquantities of scarce hydrocarbons by hydrogenating compounds that are readily available.

Jan 1, 1962

By H. J. Seim

An ion-exchange-instrumental analysis technique is described for analyzing impurities at 1 to 1,000 parts per million level in rare-earth metals. A cation-exchange flame photometric method is used for the alkali and alkaline earth groups of metals, and an anion-exchange procedure is used in conjunction with polarographic and X-ray fluorescence techniques for selected transition elements. The standard deviation is about 6 percent, and the average error, about 5 percent.

Jan 1, 1962

By Jerry B. F. Champlin

The successful injection of liquids into subsurface permeable formations for production stimulation, storage, or waste disposal requires a rapid, precise, and accurate method of determining the permeability of porous solids. This report describes a method and apparatus, developed by the Bureau of Mines, that use the principle of specific-volume permeametry. Calibration of the apparatus over a wide range of permeabilities and standardization of several apparatus constants have eliminated many of the tedious calculations and problems of manipulation common to some other methods. Improvements in reproducibility and accuracy have resulted from reducing experimental measurements to one parameter--time. Specific permeabilities of reservoir rock samples are determined directly from a chart that relates elapsed time to a permeability equivalent to that determined by bubble-tube measurements.

Jan 1, 1962

By David Burgess

Natural gas is a general term applied to the gas obtained from oil or gas wells. It is the most widely used of all gaseous fuels. The principal disadvantage in the use of this and other gaseous fuels is the difficulty encountered in the storage and transportation of large quantities in the gas state. Handling in the liquid state is possible, but reduced temperatures are required since methane (table 1) is the principal component of most natural gases that are used as fuels. Actually, liquid storage has been utilized both here and abroad;3 however, the Cleveland disaster4 has pointed out the need for a critical evaluation of the hazards involved in the storage of this cryogenic fuel. Accordingly, a program was undertaken to obtain basic data that could be used to assess these hazards. In this report, the factors to be considered in an evaluation of the fire and explosion hazards associated with any fuel are each discussed briefly. These factors are then used to assist in the design of experiments for the evaluation of the hazards associated with liquefied natural gas (LNG) relative to those associated with other common fuels. Experiments have been conducted on the vaporization of LNG, the mixing of LNG vapors with air, the effect of temperature and nitrogen dilution on the limits of flammability of methane in air, the burning rates of LNG and other fuels, flame radiation, and extinguishment of fires above liquid pools. Based on the results of these experiments, LNG can be stored safely in suitably designed above-ground tanks surrounded by earthen dikes in much the same manner as gasoline.

Jan 1, 1962

By R. V. Lundquist

This report describes results of tests on the desilication of solutions resulting from the leaching of lime-soda sinters. Desilication was accomplished by heating the solutions in an autoclave. A liquor relatively free of silica was obtained after 30 minutes of heating at 200 p.s.i.g. in the presence of lime. The addition of lime improved desilication, but the rate and efficiency of desilication was effected by the quality of lime used. The optimum quantity of lime for effective desilication was about 6 grams per liter. A lesser quantity gave poorer desilication, and a greater quantity increased the alumina loss without improving desilication. The alumina loss was approximately proportional to the lime added. A complex structure, called artificial noselite in this report, was the only silica bearing compound detected in the desilication precipitate. Other compounds present were Ca(OH)2 (calcium hydroxide), CaCO3 (calcium carbonate), and Ca [A1(OH)6]2 (hydrated tricalcium aluminate). Sodium carbonate in the leach liquor retarded the formation of the calcium aluminate; hence it decreased the alumina lost to the precipitate. The extraction of alumina from aluminum silicate materials by the limestone soda-sinter process has been investigated by the Bureau of Mines for many years. The process consists of the following major operations: Blending the aluminum silicate with limestone and soda ash in such proportions that dicalcium silicate and sodium aluminate are formed on sintering; leaching the sinter in a carbonated caustic solution to extract the soluble alumina; purifying the leach liquor by the precipitation of soluble silica (this precipitate is designated desilication precipitate in this paper); precipitating alumina trihydrate from the purified liquors by carbonating with carbon dioxide gas; and calcining the trihydrate to alumina. Commercial grades of

Jan 1, 1962

By H. R. Babitzke

The purpose of this investigation was to evaluate the potential of columbium-hafnium alloys as structural materials for use at elevated temperatures. The work described in this report was conducted to determine the properties of columbium-hafnium alloys and to select the more promising ones for further improvement. Properties determined in this report were machinability, hardness, workability, tensile strength, and oxidation resistance. Ten ingots, ranging from 100 percent columbium to 70 atomic-percent hafnium, were prepared and subjected to tests. The test results showed that the alloys with 33 and 50 atomic-percent hafnium were superior in workability, strength, and oxidation resistance. For the alloy series tested, the strength and hardness values increased with the increasing hafnium content. Maximum values were reached with 50 atomic-percent hafnium. The oxidation resistance was poorest at the 1 atomic-percent hafnium level but improved with increasing hafnium content through 70 atomic-percent. Eight of the ten ingots were fabricable at room temperature. The two remaining ingots, those with 5 and 10 atomic-percent hafnium, required hot-working.

Jan 1, 1962

By E. C. Perkins

Preliminary experiments are reported utilizing bacteria to leach manganese from a variety of domestic low grade manganiferous materials. In two large leaches manganese extraction ranged from 71.7 to 92.5 percent, and the products analyzed over 48 percent manganese. Nutrient requirements and leaching time experiments were made. The mechanism of leaching is not understood, but is different than the mechanism encountered in the microorganism accelerated leaching of copper in the presence of sulfide minerals.

Jan 1, 1962

By W. W. Agey

This report summarizes results of bench-scale metallurgical studies by the Federal Bureau of Mines on three composite samples representative of the low-grade manganese ores purchased by the General Services Administration (GSA) and stockpiled at Deming, N. Mex., and Wenden, Ariz. Bench-scale flotation tests at the Salt Lake City Metallurgy Research Center showed that all three composites could be beneficiated by flotation to recover 88 to 90 percent of the manganese in concentrates that assayed from 38.5 to 39.0 percent Mn, 10 to 12 percent insoluble, 5 percent CaO, 3 to 5 percent Fe, and 1.3 to 1.7 percent combined Pb plus Zn plus Cu, Sintering studies indicated that specification-grade material could be made from these concentrates by sintering above 1,000° C, and adding either sodium or calcium chloride to the charge to insure removal of enough lead and zinc to meet the specifications.

Jan 1, 1962

By D. W. Frommer

Composite samples of nonmagnetic taconite from the western Mesabi range were evaluated by reductive roasting, fine grinding, and magnetic separation to determine potential sources of concentratable material. Although large tonnages of nonmagnetic taconite are known to occur in the western Mesabi district, these materials are not as yet a commercial source of iron ore. The technique employed permits the evaluation of individual composites and blocks of composites in terms of responsiveness to a process of potential commercial significance. The 159 composites, from open-pit mines located between Grand Rapids and Chisholm, Minn., were evaluated in the following sequence: 1. Minus 8-mesh material was roasted at 500° C. in hydrogen. 2. The roasted are was ground to one or more sizes in the minus 100-to minus 400-mesh range. 3. The roasted ground ore was magnetically separated in a Davis tube. 4. Composites were classified according to degree of grinding required to produce minimal concentrates. (Minimal concentrates are herein defined as those containing less than 10 percent silica, and responsive composites as those yielding minimal concentrates.)

Jan 1, 1962

By J. Robert Wells

The Bureau of Mines has developed a spectrochemical procedure for determining 19 impurity elements in high-purity titanium metal, titanium oxides, and titanium halides in which all samples are converted to titanium dioxide. Determination of these impurities was studied in the general concentration range of 0 to 1,000 p.p.m., but different determination limits were found for the various elements. The procedure is quantitative for 18 elements but semi-quantitative3 for beryllium and has an overall relative standard deviation of 15.8 percent. Two mixtures were used, one composed of graphite and lithium carbonate plus gallium oxide and the other of graphite and lithium carbonate plus germanium dioxide. Each mixture was blended mechanically with an equal weight of titanium dioxide. Lithium carbonate served as buffer-diluent. Gallium was the internal standard for 1 impurity element, germanium for 7, and titanium for the remaining 11.

Jan 1, 1962

By R. C. Bates

Uranium mine workers? daily exposure to radon daughters was estimated by two methods of sampling, detailed and spot-check. Both methods involve time- weighting measured exposure levels to arrive at an average exposure figure. Random sampling, or sampling without regard for the duration of exposure, has proved inadequate for estimating average exposure levels. During the first phase of the study, the breathing zones of eight workmen in three underground uranium mines were sampled for an entire shift; 20 to 36 radon-daughter samples were collected per man-shift, Analysis of these data indicated that a suitably accurate estimate of the full-shift exposure could be made by time weighting a considerable lesser number of representative radon-daughter samples. This analysis led to the spot-check method of estimating full-shift exposures to radon daughters. Additional detailed studies were made in seven mines to Learn more about the full-shift radon-daughter exposures and to test the spot-check method, In all, 617 radon-daughter samples were taken in 10 underground uranium mines during 26 man-shifts, and the spot-check method was tested 35 times.

Jan 1, 1962

By A. G. Starliper

The report covers studies by the Bureau of Mines on the removal of metallic values in two waste products from the Longhorn tin smelter at Texas City, Tex. One product was a slag that contained tin, tungsten, iron, tantalum, and columbium. The other product was a spent acid solution that contained tin, tungsten, iron, lead, copper, zinc, and silver and that came from presmelting treatment of impure tin concentrates. Molten slag was treated with sulfur or sulfur compounds and with coke, calcium carbide, or gaseous reductants to form tin sulfide that volatilized from the charge and to reduce tungsten along with iron and silicon to form a carbon-bearing metallic layer. The metallic layer was treated by an oxidizing alkali roast and then was water-leached to extract the tungsten. The waste acid was used in other experiments to dissolve an iron-tin- tungsten alloy (hardhead) obtained by direct reduction of the slag. An insoluble fraction containing tungsten, silver, silicon, columbium, and tantalum was removed, and copper was cemented on metallic iron, Tin was recovered by cementation on zinc plates, and lead was precipitated by adding sulfate ion. Iron was precipitated by increasing the pH which left a solution containing principally zinc. Slabs of hardhead were electrolyzed in an electrolyte consisting of waste acid to plate out groups of metals at different pH?s. The time did not permit thorough exploration of this method of treatment.

Jan 1, 1962

By R. W. Lewis

Spectrochemical procedures were developed using dc arc excitation for the determination, in parts per million, of 18 impurity elements in electrorefined beryllium and high-purity beryllium oxide. The metal samples were dissolved in dilute hydrochloric acid, evaporated to dryness, and converted to the oxide in a muffle furnace at 900° C. Germanium oxide was added as an internal standard for the determination of 15 of the elements, copper oxide for boron and molybdenum, and neodymium oxide for calcium. The average coefficient of variation was 11 percent with the exception of copper, which averaged about 43 percent.

Jan 1, 1962

By P. S. Jacobsen

In 1960 over 93 percent of the coal cleaned mechanically in the United States was cleaned in processes that utilized water or dense-medium suspensions of fine solids in water. Thus, in the process of removing deleterious ash-forming and sulfur-bearing minerals, another deleterious substance--water-- is added to the coal. The subsequent removal of the water from the coal, and the concomitant recovery of the coal from the water, is not troublesome in the sizes coarser than 1/4-inch. In the finer sizes, however, it is a difficult procedure that often costs more than the original washing operation. Because of the importance of liquid-solids separation in coal preparation, the Bureau of Mines has a continuing program of research in this field. The objective is to make available information on the performance characteristics of various types of equipment available for liquid-solids separations, thus promoting the wise selection of equipment for specific applications, and, thereby, more effective processing of coal. Results of work on flocculation as an aid to filtration5 and the sieve bend screen6 have been published. The present investigation of the screw-type classifier operating in combination with the cyclone was undertaken primarily because such classifiers are comparatively new to coal preparation and information on their performance is not available. The cyclone has become well-known since its introduction in this country by the Bureau of Mines in 1948.7 Use of the cyclone in conjunction with the screw-type classifier represents an attempt to provide the maximum recovery of solids at minimum moisture content.

Jan 1, 1962

By Leonard Obert

Between 1927 and 1957, sodium borate minerals were mined by underground methods in the Kramer District, Kern County, Calif. In 1957, surface mining methods were initiated, and during the next two or more decades it is probable that most of the production from the district will be obtained from open pits. However, part of this borate deposit is sufficiently deep that surface mining may not be economical and, hence, at some future date underground methods may again be employed. This report was prepared to document the underground mining methods employed in the district before 1957. The general geology of the district and the detailed geology of each of four mine sites are presented, together with a mineral and mechanical description of the ore and enveloping rock. The report also describes the stoping, extraction, pillar support, methods of artificial support, and other factors that affect the structural characteristics of these mines.

Jan 1, 1962

By J. D. Brown

The electron optics, vacuum system, and sample stage assembly for the Bureau of Mines? electron probe X-ray spectrograph were purchased. Four scanning curved-crystal spectrometers, two reflection- and two transmission-type, were designed and constructed by the authors. The reflection spectrometers are placed in a vacuum chamber for measurement of long-wave-length X-radiation. Detection, pulse-amplitude discrimination, and recording circuits are provided for the simultaneous measurement of four X-ray spectral lines. Minimum spot size is approximately 2 microns in diameter at 30 kilovolts and a sample-to-ground current of 5 x 10-8 ampere. At this voltage and current the limit of detection with reflection spectrometers is less than 0.05 weight-percent for most elements. The limit of detection for elements determined by transmission-type spectrometers, evaluated at 35 kilovolts and 5 x 10-8 ampere, is approximately 0.1 weight--percent for all elements having excitation voltages below 20 kilovolts. In general, reflection spectrometers exhibited satisfactory but poorer resolution than the transmission type, resolution of the spectrometers being limited primarily by crystal imperfections, with greater mosaic structure being introduced by the grinding process for the reflection crystals. Several applications of the electron probe X-ray spectrograph are described. Analysis of a uranium-steel is discussed in detail to illustrate calculation of composition from measured X-ray intensities.

Jan 1, 1962

By Michael G. Zabetakis

The autoignition temperatures (A.I.T.'s) of natural and synthetic lubricants in air were generally found to decrease with increasing pressure. Of the two types of fluids, synthetic and natural, studied in some detail, the phosphate esters had higher A.I.T.'s at any pressure between 1 and 200 atmospheres than the mineral oils. Most of the A.I.T. data obtained in this study obeyed the relationship predicted by Semenov's theory of ignition.

Jan 1, 1962