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By J. E. Wilson

The Pittsburgh carbonization laboratory of the Bureau of Mines has determined the expansion or contraction of more than 300 coking coals in a modified Bethlehem-type sole-heated expansion tester. Information on the actions of coals or blends of coals when coked is extremely valuable to operators of commercial-scale coke ovens. Coals that expand abnormally or beyond expectations can cause extensive damage to coke ovens and result in costly shutdowns and repairs. Although test results for many of the coals have been given in various Bureau of Mines publications, considerable information was not published. Thus, it is the purpose of this report to furnish coal operators and the coking industry with a current appraisal of the expanding properties of all coals tested by the Bureau before September 1, 1958. These data should be useful in the normal long range planning of coal and coke production and will be essential if the demand for coking coals increases abnormally or when reserves of higher grade coals are depleted.

Jan 1, 1959

By William J. Campbell

These investigations were undertaken as part of a program to determine the optimum X-ray spectral lines to use for analyzing the wide variety of samples received by the X-ray Laboratory. Theoretical calculations and experimental data derived from these investigations show that longer wavelength spectral lines, > 2A, are very useful for many analytical problems. Because of the low fluorescence yield of the elements of atomic numbers 13-22 and the small depth of penetration of their X-ray spectral lines, these elements were originally considered to be insensitive; however, these studies show that the wide dispersion of their spectral lines, coupled with their weak beta lines, permits the use of wide collimation, thus increasing the line intensity. More importantly, the background due to scattered primary radiation is very low in the long-wavelength region.

Jan 1, 1959

By A. C. Rice

This report describes a chemical process for preparing solutions of trivalent rare-earth chlorides from sulfate solutions obtained by treating bastnasite concentrate. The chief impurity in the final solution is cerium, and this element is less than 1 percent of the rare-earth oxides. The solution is used directly in the separation of rare-earth elements by ion-exchange methods. The attractive features of the process are that the chemicals are inexpensive and the steps few. The process starts with precipitating the rare-earth hydroxides from sulfate solutions with caustic soda. After the hydroxides are dried to oxidize the cerium, they are treated with dilute hydrochloric acid to dissolve away the trivalent rare-earth elements, leaving the tetravalent cerium. Details for controlling the leaching step are described. The process shortens older procedures by omitting the usual oxalate or double-sulfate-precipitation step.

Jan 1, 1959

By R. M. Jimeson

Pressure-drop measurements through beds of granular iron, lathe turnings, steel wool, and parallel-plate assemblies were made at linear velocity and gas-density ranges expected in the Fischer-Tropsch hot gas recycle process.4/ Equations relating pressure drop, linear velocity, gas density, and bed porosity were derived. The results indicate that the exothermic heat of reaction can be removed at a lower cost by using catalyst beds with high porosity. INTRODUCTION The Fischer-Tropsch hot-gas-recycle process requires a catalyst offering low resistance to gas flow as one condition to economic feasibility. Conventional granular or spherical catalysts used during early development of the process in Germany did not meet this requirement. Large pressure drops across these beds made the cost of recirculating the gas excessive. The Federal Bureau of Mines is investigating the process by using novel and unusual catalysts that offer little resistance to gas flow. Pressure-drop measurements across these types of catalyst beds are discussed in this report.

Jan 1, 1959

By M. J. Ferrante

A process was investigated for preparing Specification-grade nickel (containing less than 1 percent cobalt) by stripping it electrolytically from a nickel sulfate-boric acid solution and using the stripped electrolyte for the preferential dissolution of nickel from basic carbonates of nickel and cobalt. The basic carbonates were produced at the plant at Nicaro, Cuba, owned by the U.S. Government. Determination of the optimum conditions for deposition of Specification-grade nickel indicated that the upper limit of cobalt concentration was 0.1 gram per liter. The pH, temperature, and concentrations of nickel and boric acid in the electrolyte were not critical. An aluminum cathode and two lead anodes were used at a cathode current density of 1.2 amperes per square decimeter.

Jan 1, 1959

By Raymond O. Dannenberg

The gas-combustion retort developed by the Federal Bureau of Mines at the Rifle Oil Shale Project near Rifle, Colo., is a continuous, gravity-feed retort. The heat required to convert the kerogen in the oil shale to liquid oil is generated by the combustion of product gas and carbonaceous residue remaining on the retorted shale after the kerogen has been converted to oil, gas, and residue. A study of the effects of the process variables on retort operation, product yields, and product properties is important to the successful solution of the problems encountered in the development of a satisfactory process. Statistical methods were used to design the experiments and analyze the effects of the rate of shale throughput, the composition of dilution gas, the height of the shale bed above the air entry, air-gas distributor design, shale size range, and the ratios of the flow rates of the various gas streams entering the retort to the rate of shale throughput.

Jan 1, 1960

By F. P. Haver

The purpose of this investigation was to determine the effect of common impurities, that is, oxygen, nitrogen, carbon, and iron, on the Brinell hardness of electrolytic titanium. On a weight basis, nitrogen had the greatest hardening effect, followed by oxygen, carbon, and iron in order. The hardening effects of oxygen and carbon were almost identical up to a concentration of approximately 0.1 percent by weight. Above this concentration, the relative hardening effect of carbon decreased rapidly, possibly because of its limited solid solubility in a-titanium. Hardness vs. composition curves for both oxygen and nitrogen were essentially straight lines over the range of Brinell hardness numbers (B.h.n.) covered in the investigation. The hardness of titanium was also determined as a function of the percentage of impurity atoms. On this basis, iron in concentrations up to 0.17 atomic percent had a greater hardening effect than either oxygen or carbon. INTRODUCTION Determination of the as-cast hardness of arc-melted titanium is a method of quality control widely used in industry. Numerous studies4/ have been made of the effect of impurities on the hardness obtained by this method. However, most of them have been based on the use of either iodide titanium or commercially pure Kroll sponge (B.h.n. >90), as a starting material.

Jan 1, 1959

By Sidney Katell

An estimated capital investment of $76,499,800 will be required for a plant designed and built to produce 90 million standard cubic feet per day (std.c.f.d.) of synthetic pipeline gas through Lurgi gasification of bituminous char. This investment figure does not include the pretreatment plant, the cost of which is assumed to be reflected in the cost of the char fed to the gasification system. Shift conversion, C02 removal, and methanation are required after gasification in the Lurgi unit to make a gas suitable for pipeline transmission. Capital investment data are based upon equipment costs, January 1959. Based on a 90-percent or 330-day operating year, the operating cost before profit and Federal taxes with the char price as a variable will amount to the following: [ ]

Jan 1, 1959

By John Nagy

Limited experiments in the laboratory with specimens of mine rock from a Virginia bituminous coal mine indicate that natural gas-air mixtures can be ignited by sparks generated by rubbing friction of sandstone against sand-stone, shale against sandstone, sandstone against (roof-bolt) steel, and shale against steel. Such sparks, generated during a roof fall, may have initiated a recent gas explosion in this Virginia mine, although this cannot be stated with certainty. No ignitions of gas were produced by sparks or heat generated by impact friction between mine rocks or steel, during tension breaks of roof bolts, or by pull tests of roof bolts through their washers and roof plate. However, this negative result of limited experiments does not preclude the possibility of gas being ignited by these conditions.

Jan 1, 1960

By E. Morrice

The metallurgical laboratory data developed in this study indicate an improved electrowinning process for producing higher purity cerium ingot. A typical sample of the Reno electrocerium contains 99.9 weight-percent cerium and the following impurities: Total other rare-earth elements, less than 0.04 percent; iron not detected; silicon and aluminum, less than 0.02 percent each; calcium plus magnesium, less than 0.01 percent; carbon, 0.01 percent; oxygen, 0.002 percent; hydrogen, 0.0003 percent; and nitrogen, 0.0015 percent.

Jan 1, 1960

By D. W. Frommer

Mineral dressing research was conducted by the Federal Bureau of Mines under a cooperative agreement with the St. Joseph Lead Co., on three samples of iron ore from the Pea Ridge deposit in central Missouri. The objective was to provide information on how to upgrade these submarginal ores and produce marketable concentrates. Samples were prepared from drill-hole cores of similar composition and character to produce (1) a medium-grade mixed hematite and magnetite, (2) a high-grade mixed hematite and magnetite, and (3) a high-grade magnetite. In all three ores phosphorus and sulfur constituted objectionable impurities; excessive amounts of silica were also present in the medium-grade ore.

Jan 1, 1960

By Joel N. Van Sant

THIS REPORT describes the occurrence, mining, and use of refractory clay in Colorado within Region III of the Federal Bureau of Mines, which includes the States of North arid South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona. Field work by the Bureau of Mines, United States Department of the Interior, included examination of active and abandoned refractory-clay mines as well as a reconnaissance survey and sampling of numerous clay-bearing formations exposed in Colorado. Information from the survey and the sampling will help guide private industry in its search for virgin sources of refractory clay. Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation. Most of the refractory clay mined in the Denver-Golden district of Colorado is not used for refractory purposes but is blended with other clays in the manufacture of structural clay products. The predominantly flint-clay de-posits in the Pueblo and Fremont County districts are mined and utilized chiefly in fabricating refractory products.

Jan 1, 1959

By R. V. Higgins

As part of a study of application of the Buckley-Leverett method to an analysis of oil-reservoir performance covering a wide range of relative permeabilities and oil saturations, a method has been devised for quickly deter-mining average water saturation at breakthrough from relative permeability data. The base for the relative permeability used in the report is either the permeability to air or the effective permeability to oil at the irreducible water saturation. The permeability to air also was used because of the large backlog of air permeabilities available to reservoir engineers. The basic data were calculated by an electronic computer and are presented in a single graph from which the point of breakthrough may be obtained. In this study the water saturation at the beginning of the depletion is the connate or interstitial or irreducible water saturation. These water saturations are considered to be synonymous and to have a practical value.

Jan 1, 1960

By T. E. Gray

This report describes the preparation characteristics of the more significant coalbeds in Monongalia County, W. Va. It is one of a Bureau of Mines series planned to determine coals suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.5 million tons of coal was produced in Monongalia County in 1957, of which more than 7 million tons was cleaned mechanically in 8 cleaning plants. On January I, 1954 the Bureau of Mines estimated that 1,576 million tons of recoverable coal remained in the county in beds 28 inches or more thick.

Jan 1, 1960

By C. M. Frost

Two Federal Bureau of Mines recycle hydrogenation experiments to prepare catalytic cracking feed stock were made at 3,000 pounds pressure with crude shale oil retorted from Green River (Colo.) shale in the gas-combustion retort. The hydrogenated product from the first experiment, made at 784° F., was used for investigating the effects of nitrogen content on catalytic cracking yields and for determining the quality of the catalytically cracked gasoline. Hydrogenated product containing 0.14 percent or more of nitrogen produced less gasoline when cracked in a CAT "A" unit than was obtained from East Texas light gas oil cracked at the same conditions; product containing 0.10 percent or less nitrogen produced a quantity of cracked gasoline equal to that obtained from the East Texas light gas oil. The catalytically cracked gasoline had research octane numbers calculated to be approximately 95 clear and 103 with 3 ml. of tetraethyl lead. The principal product from the second experiment, made at 828° F., was a low nitrogen content gas oil which was used for investigating the yields of cracked products obtained when it was catalytically cracked to different degrees of conversion. Yields of cracked products, when plotted as functions of conversion, were essentially the same, within the experimental range of the data, as published yields from catalytic cracking of East Texas heavy gas oil; however, yields from cracking the shale-oil product did not display the sensitivity to change of cracking temperature that has been found for East Texas gas oil.

Jan 1, 1960

By Oliver C. Fursman

This work was conducted to determine the feasibility of producing aluminum-silicon alloys in a pit-type, three-phase electric-arc furnace. Two carbon-lined furnaces were used in the tests. The power input ranged from 120 to 240 kw. in the small furnace and from 420 to 460 kw. in the large furnace. Energy consumption ranged from 5.3 to 11.5 kw.-hr. per pound of alloy produced and electrode consumption, from 240 to 510 pounds per ton of alloy produced. A wide range of crude aluminum-silicon alloys was produced by direct smelting of clays or similar aluminum silicate raw materials, using hogged fuel or wood chips as the major source of carbon in the furnace charge, and silicon of high grade was produced by smelting quartz. The aluminum content of the aluminum-silicon alloys ranged from 15 to 55 percent. Alloys produced from a white opaline-silicate clay were relatively free of iron, titanium, and other impurities. Those produced from western fire clays and kyanite, although richer in aluminum, contained considerable amounts of impurities. The purity of the alloys depended largely on the composition of the raw materials.

Jan 1, 1960

By W. L. Hunter

This report describes results of beneficiation and smelting studies conducted by the Federal Bureau of Mines on chromite samples from the Emma Belle and Seiad Creek prospects in the Seiad Creek area, northern California. Samples were chosen from this area because the ore is typical of disseminated types that represent a sizable domestic reserve. The two samples were similar in composition, and both responded in like manner to gravity beneficiation. As the ore was banded, considerable coarse gangue was rejected in laboratory sink-float from a minus-3/4-inch, plus-6-mesh fraction without excessive chromium loss at a medium density of 3.32. An average of 85.6 percent of the chromium was recovered in the sink product, which analyzed 35 percent chromic oxide (Cr203). Tabling yielded concentrates containing 49 percent or more Cr203; however, recoveries, ranged from only 33 to 45 percent. A combination of tabling and electrostatic separation of the table middlings showed that the chromium recovery could be increased to about 73 percent; the composite concentrate averaged 53 percent Cr203.

Jan 1, 1960

By J. W. Eckerd

The crushing of chestnut-size (1-5/8 by 13/16 inch) Pennsylvania anthracite in four commercial crushers (impact) jaw) hammer-mill) and gyratory types) was studied by the Bureau of Mines to determine which could produce the largest proportions of buckwheat Nos. 1 and 2 sizes (9/16 by 3/16 inch). Single pass dry and wet crushing techniques and the effect of stage crushing were evaluated. Calculations were made to show the effect of closed-circuit reduction on production rates and yield of the various sizes. The data show that the gyratory crushers produced the greatest percentage of the desired sizes. A ring-type hammer mill produced the greatest tonnage of buckwheat No.1 and rice (14.9 tons per hr.) during dry grinding tests) but the yield of these sizes was only about 55 percent) as compared with 62 to 70 percent for the gyratory crushers. The impact and jaw crushers produced the smallest amount of buckwheat and rice and the largest quantity of oversize material.

Jan 1, 1960

By M. M. Wong

A brief investigation was made to determine the feasibility of electro-refining beryllium in a KCI-LiCI-BeC12 bath. Thin, platelike crystals of beryllium metal were produced by electrolyzing technical-grade beryllium metal beads (about 94-percent purity) as the soluble anode. Operating cell conditions were: Temperatures of 450° to 600° C.; an inert atmosphere; bath compositions of (1) 38.1 mol. percent KC1, 54.8 mol. percent LiCl, and 7.1 mol. percent BeC12 and (2) 36.7 mol. percent KC1, 52.7 mol. percent LiCl, and 10.6 mol. percent BeC12; cell voltages of 0.30 to 0.80; and initial cathode current densities of 50 to 435 a./sq, ft. Current efficiencies ranging from 87 to 96 percent were obtained. Qualitative spectrographic analyses of the metal products indicated that impurities were reduced. This technique offers the possibility of producing a grade of beryllium purer than that now generally available, which may have better mechanical properties.

Jan 1, 1960

By J. E. Wilson

A bench-scale expansion tester using 71 grams of coal was developed to determine the practicability of an apparatus of this size to investigate the effect of variables such as oxidation, blending, bulk density, inerts, size consist, petrographic differences, and rate of heating on the expanding properties of coal. The value of this tester is shown by the correlation that exists between its results and those of the larger scale sole-heated oven expansion apparatus used in commercial plants. From tests on 32 coals the standard error of estimate for predicting sole-oven results from bench-scale results is ± 5.3 percentage points. A standard deviation of the difference between pairs of tests in the latter apparatus of ± 2.1 percentage points was determined for 31 samples. In the sole-heated oven test the expansion of a coal at constant pressure is directly proportional to the dry coal bulk density. Tests in the bench-scale tester show a similar relationship between expansion and bulk density. When the blending ratios of high-and low-volatile coals are varied, similar changes in expansion are observed in both the sole-heated oven and the bench-scale tester. Therefore, the effect of other variables on expansion should be similar in the latter apparatus.

Jan 1, 1960