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By E. E. Creitz

Application of the usual chemical methods to the determination of beryllium in the mineral-dressing products of a spodumene pegmatite was found to be unsatisfactory as to speed, accuracy, sensitivity, and range of analysis. A spectrographic method is described for the determination of beryllium. Samples are ground, mixed with borax, high-purity, flake graphite, and an internal standard; then they are fused, reground, pelletized, and excited with a high-voltage-spark discharge. Investigation of several spectrographic techniques to overcome matrix effects are described. The method developed gives results for beryllium in the concentration range from 0.002 to 5.0 percent; the average probable error of duplicate determinations was below 3.0 percent of the quantity present. INTRODUCTION The main source of beryllium in pegmatite is the mineral, beryl. Many of the conventional methods for the determination of beryllium in beryl are not suitable for control purposes because of lack of speed and accuracy, especially in the range below a few tenths percent. Beryl resists the usual chemical attack and can be lost in a hurried chemical analysis.

Jan 1, 1958

By Frank L. Gaddy

In this report, a description of mine practices, the preparation of roof bolts for laboratory experiments, the results of tensile-strength determinations, and a discussion of results of these tests are presented. Certain restrictions are recommended for roof bolts subjected to repeated bending, and two methods of complying with these limitations imposed by the restrictions are presented. The practice of bending steel roof bolts for installation in areas where the height of the opening was less than the length of the bolts required to support the immediate roof adequately has been adopted recently in several coal mines in lieu of sectional rods designed for that purpose. In addition, a few of these same mines have been reclaiming the bent rods and reusing them numerous times. The purpose of this study was to determine if these practices decreased the strength of such bolts and thus jeopardized the safety of the men working in these mines.

Jan 1, 1958

By A. L. Engel

High extractions of lead, gold, and silver resulted from treatment of an oxidized, arsenical refractory ore by chloride volatilization. The ore was roasted in an oxidizing atmosphere at 1,000° C. for 1 hour. The chloridizing reagent was 300 pounds of CaC12?2H20 per ton of ore. Ninety-nine percent of the lead, 98 percent of the gold, and 96 percent of the silver, and only 6 percent of the arsenic, were volatilized. These results indicated that a satisfactory method could be developed for treating this type of ore. Recovery and separation of the volatilized values and developing metallurgical and operating data for this process require further investigation on a more extensive scale. Tests by gravity concentration, flotation, and cyanide leaching did not give satisfactory results.

Jan 1, 1958

By J. R. Nettle

The electrodeposition characteristics of seven binary alloys of titanium have been investigated. The object of the electrorefining experiments with an alloy was to determine the efficiency of titanium separation from individual alloying elements under established conditions. Reported results are only indicative. It is conceivable that numerous duplications of tests might give average maximums that would vary from those noted in this report; however, in the few tests that were repeated, the magnitude of transfer of the alloying elements was of the same order. The results detailed herein are for a given set of conditions. Many combinations of operating variables are possible, and the results achieved under different conditions probably would differ from those reported.

Jan 1, 1958

By M. R. Geer

American and European practices in cleaning fine coal are strikingly different. The tables, launders, classifiers, and pneumatic devices used in America are seldom employed in Continental Europe, where much of the fine coal is cleaned in feldspar jigs, often supplemented by froth flotation of the extreme fines. This difference in choice of cleaning equipment may be fortuitous, but in large measure can be attributed to a difference in economic factors. Coal being more costly in Europe, there is greater emphasis on efficient cleaning of all sizes, including the extreme fines, and it is common to produce a high-ash middling for "on-site" consumption to avoid any waste of fuel value. The feldspar jig has been found advantageous under these conditions. In the United States fuel coal must be prepared as cheaply as possible, and metallurgical coal must be prepared as efficiently as possible; thus in both branches of preparation practice, any cleaning device that promises greater economy or higher efficiency warrants consideration. The feldspar jig, as employed in Europe, has a much higher unit capacity than the wet table used so extensively here and therefore offers economy in the capital costs of a washery through saving in space. As pointed out by Vissac,4/ the jig operates under automatic control, and therefore can cope with fluctuations in quality of feed. Maintenance costs for a single, large-capacity unit, such as the feldspar jig, would be expected to be lower than those for a battery of low-capacity cleaners. These considerations led the Bureau of Mines to undertake an investigation of the feldspar jig to determine its possible usefulness in this country.

Jan 1, 1958

By R. V. Higgins

This report presents the results of a study of water injection in the HX sub-pool fault block V-B, in the Upper Terminal zone, Wilmington field, California, and is based on data obtained to May 1957. An earlier report3/ describes the results of gas injection in part of the field. The principal purpose of the pilot flood was to determine whether a sand having a permeability of 1,200 millidarcys and containing oil having a viscosity of 17 centipoises could be waterflooded effectively. The results of a preliminary study by engineers of the Long Beach Harbor Department of oil recoveries from areas where encroaching edgewater was active and the results of an independent study by a consultant retained by the Long Beach Harbor Department were favorable to a trial waterflood. After these preliminary studies, a detailed petroleum-engineering exam-ination was made of the technical details. As a result, a peripheral flood was started in June 1953. The peripheral flood was deemed desirable because the producing wells are bottomed a short distance from the edgewater. The HX subpool was selected for the pilot test because it is an isolated section of the Upper Terminal zone and is separated from the adjoining pools by faults on the east and west and by edgewater on the north, south, and west. Several petroleum-engineering methods were applied to evaluate the performance of the waterflood, and all showed that injecting water stimulated oil production.

Jan 1, 1958

By R. W. Stahl

Coal mining has been revolutionized by the continuous miner. This machine has replaced, or has combined into 1, 3 former operations: Cutting, blasting, and loading. During the 25-year period before this machine was introduced, advances had been made in transportation, but the actual "coal getting" remained virtually the same. As frequently occurs, the multiple-purpose continuous miner introduced a new hazard--more rapid liberation of methane. The coal output formerly obtained from 10 to 20 working places might now be obtained from 1. It is true that circulation of air was generally increased; but the bulk of this machine virtually precludes continuous flow of air across the face, where gas may accumulate. Apprehension about this possible hazard led the Bureau of Mines to test face atmospheres during operation; and Report of Investigations 5288, Methane Buildup During Cutting and Continuous Mining Operations (published in 1956), presents proof that real danger may be present in many otherwise well ventilated mines.

Jan 1, 1958

By C. H. Riggs

THIS REPORT give's the results of a study of the central and south parts of the Cushing oilfield, including a description of the geology, a review of the production history, and estimates of oil reserves available by secondary-recovery methods. Each of the major producing zones of the field is treated separately. The report, which is one of a long series of field studies the Bureau of Mines has conducted over the past 40 years, was prepared to aid operators to increase oil recovery and to help prevent underground waste in the Cushing field, in the State of Oklahoma, and in the United States. The geology and production history are presented not as a review of past behavior of the Cushing field but rather to interpret the possibilities for increased oil recovery by future development of this and similar areas. The field, which is in the northwest corner of Creek County, Okla., was discovered in 1912 and developed during 1913 and 1914. For several years it, was one of the most important areas producing high-grade crude oil in Oklahoma. Although some oil has been recovered from each of 10 separate reservoirs, nearly 98 percent of the total recovery of oil in the area studied was from 4 major producing formations (table 1). Of these, only the Bartlesville [ ]

Jan 1, 1958

By William J. Campbell

The purpose of this investigation was to develop a rapid, accurate method of analysis for small amounts of calcium in wolframite concentrates. This analysis is necessary to determine if the wolframite concentrates meet United States National Stockpile Specification P-57R2, which limits the calcium content to 0.2 percent. Because of the small depth of the sample analyzed in fluorescent X-ray spectrography, the calcium Kaline intensity was a function of the chemical composition of the calcium-bearing particle as well as the total matrix composition. This particle-composition effect was particularly important in this analysis, as the calcium may be present as a carbonate, tungstate, phosphate, etc. Three methods of preparing the sample eliminated the variation of calcium Ka intensity with mineralogical occurrence: (1) Reduction in particle size by extensive grinding, (2) chemical fusion with sodium carbonate, and (3) solution of the calcium by an acid attack.

Jan 1, 1958

By H. R. Shell

To obtain a better understanding of the crystallization of fluoride containing amphiboles from melts, an investigation of the range of stability between fluoramphi-boles and other minerals was conducted by the Bureau of Mines. This study has shown that the stability of fluoramphiboles is strongly influenced by both fluoride concentration and isomorphic replacement. Over 150 reactions were made with different compositions and reaction conditions. substitutions attempted and the phases that formed when the composition was crystallized by cooling from the melt are discussed. The attainment of equilibrium in these multicomponent systems is not claimed. Many ions that would be expected to enter the amphibole structure instead resulted in crystallization of phases other than amphibole. Those compositions that resulted in a high yield of acicular fluoramphibole by crystallization from the melts are shown in table 2. The fluoramphiboles obtained from melts typically had an acicular crystal habit and a hardness of 6 to 7 on the Mohs' scale. Although many had relatively high length to cross section ratios, none were fibrous; it was concluded that the possibility of synthesizing a fibrous fluoramphibole from a melt was low. However, many compositions can be crystallized into a tough, hard, impact-resistant mass of interlocking acicular crystals.

Jan 1, 1958

By F. W. Smith

To determine whether preheating coals before carbonization would improve the coking properties of the coals, particularly the weaker coking coals, 3 coals, 1 each from Illinois, Kentucky, and Pennsylvania, and a blend of the Illinois with a Pocahontas coal were preheated before testing for coking properties in the Bureau's BM-AGA pilot oven. The effects of preheating on the chemical and physical proper-ties of the coals and on the yields of carbonization products and strength of the coke produced from the preheated coals were determined, as were also the effects of bulk density, gaseous atmosphere, and residence time during preheating. Most benefit from preheating was found with weaker or oxidized coking coals, whereas the more strongly coking coals and blends showed little effect. Direct charging of preheated coal to the coke oven without cooling gave better coke, increased yield of tar, and decreased yield of gas. INTRODUCTION Although 94 percent of today's coal production comes from fields east of the Mississippi, the Eastern States have only about one-third of the Nation's recoverable reserves. West Virginia, which now produces more than any other State, has much smaller reserves than Utah, Colorado, and Wyoming.5/ However, the manufacture of iron and steel in Western States, which has increased greatly since World War I, is handicapped by the scarcity of high-grade coking coals, such as are plentiful in the Appalachian region. Unless a practical method of improving the cokemaking property of local coals is developed, ferrous metallurgical industries in the West must continue to use inferior coking coals and to pay high shipping charges for better coals.

Jan 1, 1958

By Irving Hartmann

At the 9th International Conference of Directors of Safety in Mines Research a paper6/ was presented describing the initial phases of research by the Safety in Mines Research Establishment at Buxton, England, on the remote control of timber fires with high-expansion foam plugs in a rock tunnel. The work received extensive publicity, and great interest was aroused by the implied possibility that the method might be used successfully to control coal-mine fires, which for various reasons cannot be approached and attacked by standard fire fighting measures and frequently require sealing extensive, valuable coal properties and lead to loss of production and coal reserves and occasionally loss of lives. To investigate the practicability of the foam-plug technique under American min¬ing conditions, with room-and-pillar-type extraction and multiple entries, the Bureau of Mines in 1957 began an investigation at its Experimental Coal Mine, Bruceton, Pa, In preparation for this work it was necessary to rehabilitate and reinforce an elliptical tunnel in the mine where studies had been made, many years ago, leading to development of a ventilation system used in the Holland Tunnels between New York and New Jersey, and in many other vehicular tunnels.

Jan 1, 1958

By R. E. Morgan

Two sizes of Pennsylvania anthracite were gasified in the new-type Lurgi pressure generator at the Dorsten, Germany, works of the Steinkohlengas, A. G. These tests demonstrated that Chestnut-size anthracite and a Rice-Buckwheat mixture containing 27 and 19 percent ash, respectively, could be gasified satisfactorily at an elevated pressure in a fixed bed with oxygen and steam. These coals were especially prepared to approximate a rough-cleaned coal and a washed and screened product. The operating data obtained from the two tests and materials requirements are summarized. A wide range of reactant ratios could not be tested, nor could optimum operating conditions be determined, as the generator was being used throughout the testing program, employing normal operating practices, to produce gas for the gas grid; and the most economical coal, steam, and oxygen ratios may not have been used. Comparative costs are presented of the raw materials required for producing a high-B.t.u. gas, based on the operational data obtained from these tests and, to some extent, on data extrapolated from laboratory experimentation. A flowsheet of a proposed process for producing a high-B.t.u. gas by Lurgi gasification, followed by methanation, is also included.

Jan 1, 1958

By P. M. Sullivan

Galvanizers' sal skimmings have been treated by two methods of leaching in attempts to produce preflux solutions suitable for use in galvanizing operations. Both water-leaching and acid-leaching procedures are effective, except in severely exhausted skimmings when water-leaching becomes impractical. A preliminary analysis of the skimmings is not required. Solutions in the recommended concentration range can be produced conveniently by control of pH, specific gravity, and chlorine content. A technician would require only a short period of training to be able to perform the operations described.

Jan 1, 1958

By R. T. Johansen

The adverse effects on waterflooding and well-completion methods of clay minerals indigenous to petroleum-production formations recently have received considerable attention. Knowledge of the types and amounts of clay minerals present would allow estimates of the response of such formations to injected or infiltrated water; however, the random distribution of clays in sedimentary formations makes direct evaluation of ?water sensitivity? desirable. A method for the direct evaluation of water sensitivity has been developed, based on measurement of water-vapor adsorption. Correlation of such data with the results of nitrogen-adsorption measurements provides valuable information on the content and properties of clay minerals in sedimentary rocks. The method is relatively simple and has the advantage that it may be used with small, irregularly shaped chips or shale-streaked samples, as well as with typical core samples. Methods previously employed required separating the clay from the rest of the reservoir-sample material and then performing a clay analysis either by X-ray diffraction, differential thermal analysis, liquid permeability, or a combination of these methods (2,3) .3/ This water-vapor-adsorption method requires measuring only a few points on the isotherm to tell whether or not the sample is water sensitive. The goal of these measurements is not to determine the type or amount of clay present, but what will be its sensitivity to flood water. This method gives a direct means of solving this problem.

Jan 1, 1958

By Charles B. Kenahan

The chemical and galvanic corrosion properties of commercially pure titanium, a titanium-manganese alloy, a titanium-aluminum-tin alloy, 2 titanium-copper alloys, and 2 titanium-aluminum alloys were studied. Tests were conducted in synthetic ocean water, tapwater, 1-percent sodium hydroxide, 5-percent ferric chloride, and 5-percent ammonium sulfate solutions, various concentrations of sulfuric and hydro-chloric acids, and 1-percent oxalic acid. All tests were carried out at 35° or 60° C., with a flow of air or helium. Dissimilar metals involved in galvanic-couples experiments were aluminum, magnesium, and stainless steel. Electrode-potential measurements on single (uncoupled) specimens were also measured. Commercially pure titanium and the titanium-base alloys were generally quite similar in their resistance to corrosion, whether alone or in. contact with a dissimilar metal. Contact with the titanium metals caused aluminum and magnesium to corrode by galvanic action. Coupling with stainless steel in sulfuric acid solutions decreased the normal corrosion rate of the titanium metals. Contact with aluminum in air-aerated oxalic acid and 0.1N sulfuric acid solutions resulted in cathodic corrosion of titanium and the titanium-base alloys; however, there were a few exceptions. The copper alloys showed better corrosion characteristics than titanium in certain sulfuric acid solutions but were more susceptible to chemical attack in some hydrochloric acid solutions.

Jan 1, 1958

By W. T. Wertman

A research program to aid development of better and more efficient methods for producing petroleum and increasing its ultimate recovery from underground formations is an integral part of the work of the Bureau of Mines on conservation of the Nation's natural resources. Economic, efficient production of recoverable oil and gas from a reservoir depends to a great extent upon the best and most accurate information that can be obtained from a study of the reservoir rock and its fluid contents. Information on oil and water saturation is pertinent and essential in wildcat, extension, and pool wells for good reservoir operations and prediction of performance. This report presents results of an investigation by the Bureau of Mines of core recovery and degree of drilling-fluid contamination occurring during cable-tool coring operations using oil-base mud. Representative core samples were obtained from 6 major oil-producing sands in 8 fields of West Virginia, Pennsylvania, and New York. Field-mixed, oil-base drilling mud was used for the first coring test, and lightweight, premixed oil-base mud, with an organic chloride tracer added, was used in coring eight other wells. Tracer analyses were made to determine contamination of core by drilling-fluid filtrate. Core analyses, including oil and water content and minimum interstitial water-saturation tests, were made on selected core samples to compare and evaluate water saturations determined by the two methods.

Jan 1, 1958

By Frank C. Morris

This report presents the results of a Bureau of Mines study to identify clays found in several petroleum-reservoir rocks in the Tejon-Grapevine area, Kern County, Calif., and to determine the effect of water sensitivity of the clays on the permeability of the reservoir rocks. The clays in the porous rocks were examined in detail, and the clay-mineral types were identified by differential thermal analysis, X-ray diffraction, and optical and dye-staining methods. Fresh-water damage to the permeability of the oil-reservoir rocks was indicated by a study of 125 core samples from productive formations. The study indicated that, although clays were generally less than 5 percent of the reservoir rocks, they swelled in water, particularly fresh water, and nearly blocked the flow channels through which oil flows to the well, effectively reducing the permeability of the formations. The average permeability of rock decreased from 1,600 millidarcys in air to 620 millidarcys in salt water and 120 millidarcys in fresh water. The dominant clays in the oil-bearing sandstones were members of the montmorillonite group. They were associated with smaller quantities of clays found to be in the mica or illite group. None of the cores appeared to contain clays of the kaolinite group. In the lower section of the J.V. sandstone indications of what appeared to be the mineral sepiolite were noted.

Jan 1, 1959

By L. C. Brichta

During a study of the Badger-Peacock area from October 1950 to June 1953, the Federal Geological Survey and the Federal Bureau of Mines completed nearly 98 miles of resistivity profiling and drilled 96 test holes aggregating 17,628 feet of bore, In addition, seismic profile measurements were made along 8 traverse lines for an aggregate length of about 16,600 feet. The geophysical surveys were conducted by the Geophysics Branch of the Geological Survey; the drilling was done by the Bureau of Mines. Electrical-resistivity measurements disclosed 21 low-resistivity anomalies and 1 high-resistivity anomaly. Correlation of the resistivity data with the geological information revealed by the drilling disclosed that the low-resistivity anomalies indicated either slumped shale deposits in limestone sinks or undisturbed deposits of shale lying in erosional depressions in the limestone. The high-resistivity anomaly indicated hard, undisturbed limestone at or near the surface.

Jan 1, 1958

By H. Kenworthy

The objective of this investigation was to evaluate the technical feasibility of smelting certain low-grade domestic iron ores in an electric furnace. Laboratory-scale experiments showed that a high recovery of iron in the form of pig iron can be obtained from east Texas ores containing less than 25 percent iron. The pig iron was amenable to standard-or electric-furnace-refining methods for producing steel. Car-bon, silicon, and phosphorus were the primary impurities removed in refining. Overall recoveries of iron as pig iron exceeded 95 percent, in contrast with commercial mineral-dressing recoveries on these particular ores of 50 percent of the iron as a 45-to 50-percent iron concentrate.

Jan 1, 1958