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By A. L. Service

The four periods of test operation described in Report of Investigations 5219 indicated that planer mining of phosphate rock was feasible. Corrective measures proposed for design deficiencies indicated in test 4 had to be evaluated, however; and, before the attempt to design a prototype production model, it was considered advisable to test the original machine under more severe operating conditions. Planer A was modified, therefore, during the latter half of 1955, and one additional period of experimental operation was conducted in the Anderson mine of the Montana Phosphate Products Company near Garrison, Mont., during the first 4 months of 1956. Test 5 was made in a stope, where the phosphate bed had been offset in a number of places by minor faults. Considerable difficulty was found in negotiating the irregularities caused by these faults, and productionwise the test was not as successful as some of the previous ones. Information obtained, however, was valuable in designing model B.

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 Earl R. Maize

Epoxy and polyester-type resins were injected into coal-mine roof strata of the thick Freeport coal seam in Allegheny County, Pa., at test sites in roof that had been exposed several weeks, in newly exposed roof, and in strata over solid coal. Test results indicate that the method of strengthening bituminous-coal-mine roof by injecting a bonding material into the roof strata can be developed into a safe, efficient support system. If roof bonding will become a standardized method of roof support and reinforcement or if it can be effective when used with other types of roof support can be determined only by extensive experimentation in various coal beds. Observations and conclusions are shown at the end of this report.

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

By M. M. Kirk

Forced-air cooling of cold-mold arc furnaces for melting zirconium and similar metals has been investigated and found to be practical from the stand-point of heat transfer. It is believed that this technique offers a significant reduction in explosion hazard from that inherent in water cooling, the current industrial practice. A copper crucible, with longitudinal, integral-type fins and with an outer jacket to confine the airstream, appears to be the best general design for air-cooled operation. Cutting the fins into short segments and bending the segments to produce a herringbone effect increased the airstream's turbulence and was found, on test, to increase the heat transfer up to 35 percent.

Jan 1, 1959

By D. W. Frommer

As one phase of a general problem of recovering sulfide slimes, mineral-dressing research was conducted on flotation tailing from the St. Joseph Lead Co., Bonne Terre, Mo., mill to recover a significant portion of the residual, finely divided galena. Production of a high-grade concentrate was not part of the immediate objective. Only a reasonable ratio of concentration of lead sulfide slime was sought, since the problem of upgrading by mechanical or extractive processes would be considered in the later stages of this study. The results show that, from a feed material averaging 0.20 percent lead (about 70 percent finer than 400-mesh), a recovery of up to 45 percent could be effected by flotation in rougher concentrate analyzing up to 6.5 percent Pb. These results were obtained by using larger quantities of various xanthates and sodium sulfide than used customarily in mills. Sodium sulfide, which is ordinarily detrimental to flotation of galena, was beneficial in this case.

Jan 1, 1959

By R. L. Montgomery

The heats of formation of lanthanum sulfate and the enneahydrate are -939.8 ± 3.1 and -1,587.1 ± 3.2 kcal. per mole, respectively. The heat of hydration is -32.5 ± 3.5 kca1. per mole. These values were obtained from heat-of-solution measurements of lanthanum oxide and salts. Low rates of solution precluded more accurate determinations of the thermal data. The heat of formation of the chloride was similarly observed to be -256.18 ± 0.28 kcal per mole. Heats of solution and combustion of lanthanum metal yield mutually concordant results, and earlier discrepancies reported in the literature may be ascribed to impurities.

Jan 1, 1959

By Russell R. Trengove

The largest potential reserves of manganese in Nevada are in the Pioche district. To date, these large reserves of 10-to l2-percent manganese cannot be upgraded economically. Other large, low-grade deposits, such as the Virgin River and Boulder City deposits in Clark County, cannot be considered immediate sources of manganese. Reserves of the principal manganese deposits in Nevada, based on the most reliable estimates, total about 17 million tons analyzing 7.6 to 13.6 percent manganese. Most of the deposits are of a type that cannot be prospected systematically but have been prospected and developed in the course of productive mining operations. To realize production from low-grade deposits that are amenable to concentration, a ready market must be provided. Thus far, Government stockpiles have been the major outlet for these low-grade ores. Research and experimentation over a period of years have led to development of several processes technologically applicable to these low-grade ore bodies, but their economics is not sufficient to allow competition with imported ores on the open market.

Jan 1, 1959

By C. M. McKinney

This report contains Bureau of Mines routine crude-oil analyses of 20 samples from5 areas on the arctic slope of Alaska. Two samples were condensates from the South Barrow gasfield, Barrow Lakes area. The remaining 18 samples were crude oils from the following areas: Barrow Lakes, 1 seepage sample; Umiat, 10 well samples; Cape Simpson, 1 seepage sample and 3 well samples; Fish Creek, 2 well samples; and Wolf Creek, I well sample. Table 1 summarizes information on the origin of the crude-oil samples, and table 2 summarizes characteristics of the samples. Item numbers in both tables correspond to item numbers of the analyses at the end of this report, and the samples are referred to by these numbers throughout the text.

Jan 1, 1959

By C. H. Riggs

This report describes the geology and reviews the oil-production history of the Dutcher sands of Pennsylvania age in the Muskogee oilfield. The geology and production history are presented not alone as a review of the past behavior of the field but also to interpret the possibilities for future production of oil from semidepleted sands in this and similar areas. The Muskogee field, one of the oldest oil-producing areas in Oklahoma, yields paraffin-base oil of 40° API gravity -a gravity higher than that of most Oklahoma oils. Oil was discovered in the townsite of Muskogee in 1894 but was not produced in commercial quantities until 1904. A peak yearly rate of 1,340,000 barrels of oil was attained in 1910 (see table 1).

Jan 1, 1959

By A. L. Engel

This investigation was undertaken to assess the feasibility of processing an extensive deposit of iron ore near Palisades, Eureka County, Nev., previously penalized for high phosphorus content. The experiments described indicate a satisfactory accomplishment of objective. Chemical treatment will permit a high-phosphorus iron ore to be used. Leaching with acid solution effectively lowers the phosphorus content with a [gligible] loss of iron. The use of hydrochloric acid is preferred because [ ] does not contaminate the ore and the cost is lower. Minus-1/2-inch ore was satisfactorily leached in 24 hours, minus-1/4-inch ore, in 8 hours, and minus-10-mesh ore, in 3 hours. About 40 pounds of acid per ton of ore was consumed in each instance.

Jan 1, 1959

By Leonard F. Heising

Domestic production of Metallurgical-grade manganese has contributed such a small percentage of the United States industrial demands that areas known to contain large tonnages of low-grade manganese ore have been investigated by the Bureau of Mines to reduce this country's dependence on foreign ores. A major source of low-grade manganese is the Cuyuna iron range in Minnesota. The entire Cuyuna iron range is covered by an overburden of glacial drift that, in some places, reaches depths of 200 feet or more. Prospecting and exploration must be guided by geophysical methods, drilling results, or projections of exposures found in operating mines because there are no outcrops near the productive parts of the range. Past drilling for the purpose of outlining iron ore generally was confined to the highly oxidized zones. Much of the manganese with which the Bureau of Mines is concerned occurs in thin-bedded unoxidized iron formations, too low in iron content to have been of interest to those seeking commercial iron ore. The primary objective of the core-drilling reported here was to obtain cores of different classes of manganiferous rocks and to determine whether or not the samples were amenable to beneficiation.

Jan 1, 1959

By W. Hodge Caraway

This report presents the results of an evaluation of several indirect methods of measuring the water content of oil-reservoir rocks. The water content of oil-base cores is considered to be most nearly representative of the water content of the undisturbed petroleum reservoir and therefore, the direct method of measuring the volumes of water in cores cut in oil-base drilling fluid was adopted as a standard for comparison. The indirect methods evaluated included (1) displacement through a semipermeable membrane by air, (2) centrifuge, (3) evaporation, (4) mercury injection, (5) chloride dilution and (6) electric logs. Approximately 270 samples of cores from petroleum-reservoir rocks were used in the study. The cores, most of which were cut with oil-base mud in the hole, were taken from oilfields in California, Texas Gulf coast, Colorado, Oklahoma, and Alaska.

Jan 1, 1959

By David J. Kusler

This report describes a primary or direct, continuously sampling, and automatically averaging gravimetric method for analyzing gaseous mixtures of carbon dioxide, carbon monoxide) hydrogen, and (by volume measurement) nitrogen. The gaseous mixture is analyzed by passing it at a controlled and definite rate through a system that permits carbon dioxide and water retained by appropriate absorbents to be determined and the residual-gas volume (essentially nitrogen) to be measured. The accuracy and dependability have been established by comparison with very carefully conducted Orsat analyses. The method was developed for, and has been satisfactorily applied to, the analysis of blast-furnace top gas. It permits relatively attention free operation, using simple and low-cost materials usually found as basic equipment in the analytical laboratory. It provides, over a wide range of time or sampling intervals (from less than 1 to over 24 hours), the average composition, in terms of volume-percent, for those components usually determined in blast-furnace gas, if (as is usual) the flow rate of gas from the blast furnace is essentially constant over a selected analysis interval. Oxygen and methane are not determined; but, since these gases are normally absent or present only in traces, their analysis is seldom required.

Jan 1, 1959

By B. C. Parks

This paper is a report on the relationships between petrographic composition, chemical composition, physical properties, and thermal behavior of banded bituminous coal. It describes the relationships between petrographic composition, behavior in various laboratory tests, and carbonizing properties of different petrographic types of coal that occur in relatively thick benches in a single bed of high-volatile A bituminous coal - the Hernshaw bed of Boone County, W. Va. Thin-section microscopic analysis and free-swelling index determinations of the thin-section samples were made of a standard column sample. A standard face sample, a representative channel sample, and representative samples of two prominent petrographic benches of bright and dull coal were subjected to chemical analyses and free-swelling-index, plasticity, dilation, agglutinating, low-temperature carbonization, and BM-AGA retort tests. A float-and-sink separation was also made of part of the standard face sample. The fractions from this gravity separation were subjected to petrographic and chemical analysis and free-swelling-index, plasticity, and dilatation tests.

Jan 1, 1959

By L. Allan White

Instrumental analysis is an indispensable tool to many phases of research on rare-earth metals and their compounds; therefore, the development of new and improved instrumental techniques is essential. This report describes an emission spectrometric analytical method using direct-current carbon-arc excitation of various rare-earth-oxide mixtures. Lanthanum oxide serves the dual purpose of an internal standard and a constant major constituent. The versatility of the method was demonstrated by three different applications: (a) Analysis of complex rare-earth concentrates; (b) determination of impurities in high-purity rare-earth oxides; and (c) detection of rare-earth elements in other types of matrices, such as those resulting from beneficiation of rare-earth ores. The average error of analysis in the concentration range of 0.2 to 10.0 percent was 14.6 percent for a group of complex synthetic mixtures of rare-earth oxides. An average error of analysis in the concentration range of 0.05 to 0.50 percent was 21 percent for a group of high-purity rare-earth oxides.

Jan 1, 1959

By D. E. Wolfson

This report describes the carbonizing properties of the principal coal beds of Allegheny County, Pa., which rank low in the high-volatile A bituminous classification. Seven coal samples from 3 coal beds were selected for study, as follows: 2 each from the Redstone and Pittsburgh beds and 3 from the Upper Freeport bed. Selection was based on estimated reserves. The samples of Upper Freeport and Pittsburgh coals were satisfactory chemically for producing metallurgical coke. The ash contents of the samples of Redstone coal were moderately high. One of the samples of Redstone coal was high in sulfur content, and it would be difficult to upgrade to meet present metallurgical standards.

Jan 1, 1959

By J. J. Demeter

As part of its work on converting coal to fluid fuels, the Federal Bureau of Mines has been studying the synthesis of liquid fuels from carbon monoxide and hydrogen by Fischer-Tropsch synthesis. A fluidized bed of nitrided, fused-iron catalyst has been operated successfully to produce high yields of oxygenated compounds. Trouble-free operation continued for over 800 hours, and the test was terminated voluntarily. About 85 percent of the fresh feed was converted when the unit was operated at a space velocity of 500 hr.-1, a 12:1 recycle-to-fresh-feed-gas ratio, a 300-p. s. i. g. pressure, and a temperature of 252° C. When operating at a fresh-feed-gas space velocity of 1,000 hr.-l and a 9:1 ratio of recycle to fresh gas, conversion of fresh feed was 68 percent, and the product yield was 235.9 grams per cubic meter of synthesis gas converted. The oxygenate and C5 and heavier hydrocarbon yield was 110.6 grams per cubic meter of gas converted, 83 percent of this was oxygenates. The atom ratio of N:Fe of the catalyst, initially 0.455, decreased to 0.288 by the end of the 800-hour experiment. Nevertheless, the yield of oxygenated compounds per cubic meter of H2 + CO converted at the end of the run was approximately the same as that obtained 500 hours earlier with identical operating conditions. X-ray analysis of the discharged catalyst indicated that only ?-iron carbonitride was present. Sieve analysis of the discharged catalyst indicated that only 2 percent of fines was produced during the reduction, nitriding, and synthesis.

Jan 1, 1959