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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 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 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 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 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 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 Leonard Obert

The various underground rooms in the Bureau of Mines Oil-Shale mine, Rifle, Colo., have been open for periods ranging from 3 to 5 years. During this time 3 roof falls have occurred; 1 was induced, and the other 2 were unintentional. The three roof falls are described in this report. Two causative factors are discussed -a time-dependent deterioration of the roof rock and an unfavorable system of jointing that occurred in the strata overlying the present roof horizon. Irrespective of cause, the operating life of any stoping area would have been short com-pared with the life of the roof (1 to 4 in the most unfavorable instance), if a high-production system of mining had been employed. The report is concluded with several recommendations that should be considered in planning future mining operations.

Jan 1, 1958

By R. P. Maloney

The Bureau of Mines conducted a reconnaissance of the less accessible parts of the Beluga River coalfield in August 1957 to determine, if possible, which areas were most favorable for developing large reserves of coal suitable for open-pit mining. Several outcrops of subbituminous coal were observed within an area about 30 miles long and 3 miles wide; neither the length nor the width of the coal-bearing area was delineated by the examination. Coal beds 30 feet thick or more outcrop at two places, and beds 5 to 20 feet thick or more outcrop fairly abundantly along the Beluga River and its tributaries The coal measures appear to occur in a series of folds. The overburden comprises glacial gravels and poorly cemented sandstones and ranges from 20 to 400 feet in depth. Few partings were seen in any of the coal beds. Samples ranged in calorific value from 6,240 to 8,246 B. t. u. on an as-received basis. Adequate water is available for stripping by hydraulic methods.

Jan 1, 1958

By M. M. Barr

Rapid expansion of the titanium-metal industry focused attention upon ilmenite as a possible substitute for the more expensive and less abundant rutile in producing titanium tetrachloride. Most of the rutile available for this use is imported. Preliminary studies were undertaken to determine the chlorination characteristics of high-titanium slags produced by electric-arc furnace smelting of alluvial Idaho ilmenite at the Federal Bureau of Mines Northwest Electrodevelopment Experiment Station, Albany, Oreg. Low silicon, calcium, and aluminum contents of the slags enhanced their potential value for chlorination.

Jan 1, 1958

By G. W. Birge

This report describes the carbonizing properties of the principal coal beds of McDowell County, W. Va. Coals from 14 coal beds were selected for study: Upper Cedar Grove, Middle Cedar Grove, Lower Cedar Grove, Eagle, Douglas, Iaeger, Sewell, Welch, Beckley, Fire Creek and Pocahontas Nos. 3, 4, 5, and 9. Selection was based upon estimated minable reserves. McDowell County coals rank either as high-volatile A, medium-volatile, or low-volatile bituminous coal, and this variation in rank is reflected in the wide diversity of the carbonization properties of the coals. All coals tested were either satisfactory as mined or could be upgraded to meet present chemical standards for metallurgical coke; the coals produced strong coke, as determined by ASTM shatter and tumbler tests.

Jan 1, 1958

By R. R. Wells

This report summarizes the results of laboratory investigations by the Alaska Mining Experiment Station, Juneau, to determine the practicability of treating cinnabar-stibnite ore by bulk flotation and controlled-atmosphere roasting of the concentrate. Ore from the Red Devil mine near Sleetmute, Alaska, was selected for testing; it is typical of ores widely distributed throughout the Kuskokwim River Basin. The material, consisting of stibnite and cinnabar in ankerite, dolomite, and quartz, assayed 1.55 percent Hg and 2.87 percent Sb. Continuous treatment of the ore in a laboratory flotation circuit recovered 95.7 percent of the mercury and 82.6 percent of the antimony in a concentrate that assayed 20.4 percent Hg and 34.6 percent Sb.

Jan 1, 1958

By W. H. Ode

In 1949 the Coal Committee of the Economic Commission for Europe, Geneva, Switzerland, established a Classification Working Party, to develop an international system for classifying coal. This project was necessitated by the increased trade in coal among various nations following World War II. Although national classification systems existed, they had been developed to cover the characteristics of domestic coals without reference to coals of other countries. Different terms for describing similar or identical coals in each nation caused confusion in evaluating coals shipped in international trade. Experts from Austria, Belgium, Bulgaria, Czechoslovakia, Denmark, the Federal Republic of Germany, France, Greece, Hungary, Italy, the Netherlands, Poland, Sweden, the Union of Soviet Socialist Republics, East Germany, the United Kingdom, the United States of America, and Yugoslavia participated in various stages of the classification work. Walter A. Selvig was appointed by the Bureau of Mines as the technical expert to represent the United States because of his experience in developing and standardizing methods of analyzing and classifying American coals. He served on the Classification Working Party until his retirement from the Bureau of Mines early in 1956. Extensive laboratory work was done in connection with the classification studies at the Pittsburgh Experiment Station of the Bureau of Mines.

Jan 1, 1958

By K. K. Kelley

Synthetic fluorphlogopite mica (KMg3AlSi3010F2) is a relatively new product developed at the Norris (Tenn.) Station of the Bureau of Mines, Thermodynamic data have applications both in the production and use of this product, and the work described in this paper was undertaken to fill the need for such data. Measurements were made of the heat of formation at 298° K., the heat capacity between 50° and 298° K., the entropy at 298° K., and the heat-content and entropy increments between 298° K. and a maximum of 1,804° K. These basic data are combined to obtain heats and free energies of formation of the mica from the elements and from molecular constituents at temperatures ranging from 298° to 1,800° K. Minimum heat requirements to form melted mica from commonly used ingredients were calculated.

Jan 1, 1959

By W. T. Wertman

A research program to aid development of better petroleum-recovery technology is in progress at the Appalachian Experiment Station, Bureau of Mines, Morgantown, W. Va. The work is part of the overall effort of the Federal Bureau of Mines to effect true conservation of the Nation's natural resources. Knowledge of the magnitude of the interstitial water content of oil-bearing formations is important to petroleum-reservoir engineers because of the influence of water on fluid flow during oil production and because of the significance of water volume in oil-reserve evaluation. Such information on Appalachian oil-bearing formations is needed to aid in planning secondary oil-recovery projects. Generally, the interstitial water content of oil sands can be estimated by one or more of the following methods: Analysis of cores obtained with oil-base drilling fluid, electric logging, restored-state or capillary-pressure tests, centrifuge tests, evaporation tests, or mercury-injection tests.

Jan 1, 1959

By D. H. Baker

THIS REPORT presents the technique and equipment used in determining the hardness of titanium sponge. Detailed descriptions are given of the methods used in preparing test samples for chemical analysis and hardness testing, the method of melting and surfacing test ingots, and the technique of reading Brinell-hardness impressions. The arc-melting furnace described, for which engineering drawings are included, will produce from 70 to 90 double-melted buttons each 8 hours of operation. Experimental data are also presented depicting the effect on hardness of the methods of surfacing specimens, temperature of test specimens, and the effect of time at test load. These data show that surfacing of the specimen involves no critical machining operations but that the test surface must be paralleled by a relatively flat surface for contact with the anvil of the Brinell tester. The heating of a specimen to 150° C. during surfacing does not materially affect the results if the ingot is cooled to room temperature before the hardness impressions are made. The optimum time at load appears to be approximately 30 seconds, but load times of as much as 1/ ½ minutes will not cause major errors.

Jan 1, 1959

By J. W. Jensen

This report was prepared as a background reference for future publica¬tions concerning the damping capacity of metals and alloys. It contains a broad description of the theory and methods of measuring damping capacity and correlates the developments of the past decade in terminology, units, and techniques. Damping-capacity instrumentation at the Mississippi Valley Experiment Station, Rolla, Mo., is described. The bibliography contains over 150 references to recent articles, each tabulated as to material investigated and test variables, such as frequency, stress, mode of vibration, and temperature. INTRODUCTION After it discovered high-damping manganese-copper alloys before World War II, the Bureau of Mines began research on the damping capacity of alloys and has continued to expand this activity to the present time. In physical metallurgy, damping capacity has become an important research tool in the Bureau. The physical measurement of the damping properties of alloys was begun at the College Park laboratories, and later conducted at Salt Lake City under the direction of Dr. E. V. Potter. Among the many articles resulting from this work, Damping Capacity of Metals (108)3/ has received frequent men¬tion in more recent literature and describes briefly the methods of measurement employed at that time.

Jan 1, 1959

By H. Dolezal

A laboratory study of acid-ferrous sulfate treatment of low-grade manganese ores from the Cuyuna range, Minnesota resulted in 93-percent extraction of manganese as manganese sulfate with consumption of 3.8 pounds of H2S04 per pound of extracted manganese. Two types of ore were treated in consecutive stages. The first are contained carbonate minerals of manganese and iron, both soluble in H2S04 solution. The second ore contained manganese oxide minerals, insoluble in straight acid solution but soluble in the ferrous sulfate solution obtained from treating the first ore. Leaching data were obtained by countercurrent percolation of coarse (minus-1/2-inch) ore particles at room temperature and by agitating minus-65-mesh ore particles in heated solution. Extraction of manganese and acid consumption were the same, but the percolation leach required 6 days compared with 1 hour for hot agitation. Variations in the size of ore particles treated, leaching time, acid concentration, solution temperatures, and method of applying ferrous sulfate solution to the oxide ore were studied. The effects of several reagents for removing iron from solution and improving filtration were also studied.

Jan 1, 1959