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By Mary F. Koehler

Interoxidic compounds, such as vanadates, have not been studied extensively in the field of thermodynamics. This is a report of three vanadates of sodium--metavanadate, pyrovanadate, and orthovanadate. Vanadates of other metals will be considered in future reports. The heats of formation at 298.15° K. of the three sodium vanadates (both from the oxides and from the elements) were derived from the results of sodium hydroxide solution calorimetry. Free energies of formation were obtained by combining heat and entropy values. The results support the conclusion that the three sodium vanadates were stable with respect to all possible decompositions in which vanadium retains its pentavalency.

Jan 1, 1960

By James P. McGee

Preliminary calculations show an economic advantage in using nuclear energy to supply the endothermic heat required for gasifying coal. It should be noted that the various assumptions used in preparing these calculations must undergo further evaluation through additional engineering design and research. The proposed system for gasification is the indirect process cycle with helium heated in a nuclear reactor and passed through an exchanger-type gasifier for the reaction of coal and steam to form CO (carbon monoxide) and H2 (hydrogen gas).

Jan 1, 1960

By W. M. Dressel

A simple, reliable field test for beryllium in rocks has been developed by the Rolla Metallurgy Research Center of the Federal Bureau of Minas. A small portion of the pulverized rock is fused with a sodium carbonate-sodium hydroxide flux in a wire loop. The fused mass is dissolved in water, a few drops of quinizarin solution are added, and the solution is viewed under ultraviolet light. A pink-to-orange fluorescence reveals the presence of beryllium in a sample containing as little as 0.013 percent beryllium (0.26 percent beryl). INTRODUCTION New and potential uses for beryllium make necessary a more intensive search for this metal, which is so similar to aluminum in its chemical reactions that it is not separated from aluminum in ordinary chemical analyses. The principal ore mineral of beryllium is beryl, a beryllium-aluminum silicate, which contains only 5 percent beryllium. This mineral is so similar to quartz in appearance that it is not always possible to distinguish one from the other in the field. While the distinction may be made easily with a petrographic microscope, few prospectors have access to such an instrument, and fewer still know how to use it.

Jan 1, 1960

By W. A. McKinney

A sample of oxidized copper ore from a large deposit located in Pinal County, Ariz., about 50 miles northeast of Tucson, was treated by the Federal Bureau of Mines in a small-scale continuous pilot plant by a procedure which comprised acid curing complemented by water leaching and countercurrent decantation washing in a series of drag classifiers. A feed was prepared by pugging minus 1/4-in, ore with concentrated sulfuric acid and about 10 pct, of eater, followed by curing in batches for about 24 hr. The cured ore was fed continuously to a leach drum, where it was mixed with advance solution from the countercurrent washing system to dissolve the sulfated copper. The pulp was thickened and washed in four Esperanza-type classifiers, using a flocculating agent to obtain rapid settling and thickening. The leached ore pulps thickened satisfactorily in the drag classifiers when about 0.8 lb. of a polyacrylamide flocculant per ton of dry feed was used. Clear overflow liquors were obtained, and classifier rake products containing about 60 pct. solids were produced, As much as 90 lb./hr. of ore was treated in the plant, with a recovery of 60 pct. of the total copper or 80 pct, of the acid-soluble copper when 2 tons of water per ton of feed was used in washing. The acid consumption was 4.3 lb./lb. of copper recovered. On the basis of the maximum feed rate employed and the effective pulp-settling area of the classifiers, a total of 1 sq. ft. of pool area was required per ton of dry feed per day for the thickening and washing operations. The washing efficiency in the test was 95 pct.

Jan 1, 1960

By Raymond L. Carpenter

In connection with its continuing studies of the characteristics of alloys and alloying elements, the Bureau of Mines investigated the crystal structure of fused boron. This report describes how the structure of fused boron was found to be rhombohedral by the powder method for crystal-structure determinations by X-ray diffraction. The determinations of the crystal structure of boron reported in the literature were made on crystals prepared by various methods such as electrolysis, thermal decomposition of a boride, or by hydrogen reduction of boron tribromide. Table 1 summarizes the data found in the literature on the crystal structure of boron. The information shows the following: (1) Three structures have been reported for boron, (2) boron prepared by different processes--or even by varied conditions of a process--produces crystals of different structure, and (3) no information is given on the crystal structure of fused boron.

Jan 1, 1960

By I. L. Feld

This Bureau of Mines report describes the development of a simple method of producing low-phosphorus hematite concentrates from certain submarginal southeastern iron ores. The investigation was undertaken to obtain additional information on the Clinton iron ore outcrops at the southwestern extremity of the Birmingham district of Alabama and to assist in the development of operating techniques that would make it profitable to use the marginal ores of this area for blast-furnace feed. Batch and continuous pilot-plant tests demonstrated that a relatively simple wet scrubbing treatment) followed by a desliming operation to reject argillaceous (clayey) gangue, consistently yielded a marketable granular hematite product. Iron losses were relatively high but could be tolerated in view of the low treatment cost.

Jan 1, 1960

By Jack D. Ramsdell

Electrorefined, magnesium-reduced, and sodium-reduced titanium samples were evaluated for recrystallization behavior, effect of cold rolling on tensile properties, and bend ductility. Curves were determined for the softening of 2.5 to 80 percent reduced cold-rolled metal that was annealed over a temperature range of 300° to 800° C. Upon annealing, coarsening of the grains was found to occur for reductions in thickness of less than 20 percent in titanium made by all three processes. The presence of metallic impurities greatly inhibits coarsening for reductions in thickness below 20 percent, but for reductions in excess of 20 percent grain size is essentially constant at each annealing temperature. The three grades of titanium did not harden excessively from cold rolling; both tensile and bend ductility were good for reduction in thickness up to 80 percent. Upon annealing, softening occurs between 400° and 600° C., and, based on microstructure and property studies, full annealing is accomplished after 30 minutes at 700° C. for the magnesium-reduced and electrorefined titanium and at 800° C. for the sodium-reduced titanium.

Jan 1, 1960

By Earl T. Hayes

THIS BIBLIOGRAPHY has been assembled to aid research by the Bureau of Mines, and others on high-purity tungsten. It appears approximately 50 years after the development of ductile tungsten-one of the first metals to be produced in a high-purity form. Requirements of the missile age are ever more demanding that engines rout hotter and space vehicles fly higher and faster. Thus, it has become necessary to reexamine all conventional materials of construction as well as to investigate new combinations. At this stage of our technology we have alloys capable of operation at 1,800° F. and several possibilities of developing some. that will be satisfactory up to 2,500° F. Strength-weight comparisons, detrimental to tungsten at, lower temperatures, disappear at this point, mid tungsten or its alloys appear to be the only metal capable of operation at truly high temperatures. The aim of this bibliography has been to include only references that concern improving the purity of tungsten-from processing the ore to treating the finished metal. In this sense it is a selected and not a critical bibliography. The period front January 1911 through February 1959 has been covered. Because repent literature has the greatest, value, most of the selected items refer to publications issued within the pest 5 years.

Jan 1, 1960

By D. J. Bauer

Liquid-liquid extraction techniques were investigated by the Federal Bureau of Mines for the fractionation of rare-earth solutions. Separatory funnel work using tri-n-butyl phosphate (TBP) for extracting ceric nitrate from solutions containing sulfate ion resulted in almost complete extraction. Similar tests using primary amines for splitting trivalent rare-earth pairs and fractions gave promising results. The ceric nitrate extraction procedure was scaled-up by use of pressure-bubbler equipment, a series of spray towers for extraction, washing, and stripping. In this case only 84 percent ceric nitrate extraction efficiency was achieved. This work was done using dilute sulfuric acid for stripping.

Jan 1, 1960

By L. J. Kane

Conventional methods for determining the size of dust suspended in a gas require that agglomerates (clusters of particles) first be broken into particles, but in evaluating industrial dust-removing equipment the size of the agglomerates as they actually exist in the gas stream is far more important. This paper presents results of an investigation by the Federal Bureau of Mines to develop methods for determining the size of dust agglomerates suspended in a gas stream. The studies are part of the Bureau's continuing research on synthetic liquid fuels. The size and size-distribution of agglomerates as they exist when the gas reaches the filter was determined by using a membrane filter in conjunction with a dust count under a microscope. A membrane filter is a cellulosic sheet about 150 microns thick containing millions of holes per square centimeter--holes of uniform diameter that run directly through the sheet without interconnection.

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

"A bed, British Columbia, Canada, coal, carbonizingproperties B 510Pa., coal, washing characteristics RI 4941A' bed, Pa., coal, washing characteristics RI 4834"

Jan 1, 1960

By V. B. Dale

This paper is one of a Federal Bureau of Mines series covering the mineral resources of the Nation. It briefly describes most of the tungsten deposits in Cochise, Pima, and Santa Cruz Counties, Ariz. Most of the descriptions are from field examinations by the two senior writers, prior to July 1957. Wolframite first was identified in Arizona in 1896 by W. P. Blake, Territorial Geologist. Tungsten mining began about 1900 in the Little Dragoon deposits of Cochise County, and about 1901 in Las Guijas district of Pima County. The price history of tungsten is an erratic one; consequently, production has been erratic. Prices rise during wars and periods of national preparedness. Production of tungsten ore was stimulated greatly by a Government purchasing program, announced on May 10, 1951, wherein the Government agreed to purchase standard-grade tungsten concentrates at $63 per short ton unit5/ for 5 years or until 1,468,750 units were purchased. This was later increased to 3,000,000 units, and after this amount had been purchased in June 1956, the purchase of an additional 1,500,000 units was authorized. Government purchase, however, was suspended in December 1956 before completion of this latter program, and the price of tungsten concentrates declined sharply. The price had dropped to $15 per short ton unit, duty extra,6/ by the last part of July 1957.

Jan 1, 1960

By Sidney Katell

This study presents the economics of the hot-carbonate purification process for removing C02. It considers three variations of the process in order to meet the design specifications, which call for a feed-gas flow of 10 million standard cubic feet per hour (std.c.f.h.) with C02 inlet concentrations of 10, 20, and 30 percent and exit C02 values of 5, 2, 1, 0.5, and 0.1 percent. Inlet pressure and temperature are 350 pounds per square inch [e] (p.s.i.g.) and 300° F., respectively. Estimated capital and operating costs are shown in the following to tabulations: [ ]

Jan 1, 1960

By J. B. Gayle

This investigation was conducted by the Federal Bureau of Mines to compare the selectivities of diverse flotation reagents and also of flotation and float-sink methods of separation. Flotation tests, using sodium chloride, an alcohol-type frothing agent, and a kerosine-pine oil mixture as reagents, were made on seven coking-coal samples representing four different beds. The results indicated equivalent selectivities relative to sulfur rejection when entrapment effects were minimized by recleaning the various products. Selectivities relative to ash rejection were also equivalent for some coals; for others, the selectivities of the reagents tended to increase in the order sodium chloride, alcohol-type frother, and kerosine-pine oil. Float-sink tests on these same coals generally gave results indicating better selectivities than those obtained in flotation tests at comparable levels of recovery.

Jan 1, 1960

By W. M. Mark

This investigation was undertaken to develop methods to improve the quality of titanium sponge produced by the Bureau of Mines modification of the Kroll magnesium reduction process. Research revealed that by systematic elimination of detrimental impurities introduced with the raw materials and by improved handling and processing techniques, high-quality ductile titanium with a hardness of less than 110 B.h.n. (Brinell hardness number) can be produced consistently. This improvement was accomplished by helium (or argon) stripping of residual atmospheric and other dissolved gases from the titanic chloride, preliminary dehydration of crude titanium sponge, and careful regulation of the titanium tetrachloride (TiC14) feed rate to the reactors.

Jan 1, 1960

By Arthur Matzick

The oil shale from the Mahogany zone of the Green River formation in northwestern Colorado has the greatest potential in the United States for early utilization. A large reserve of adequately rich shale is available to support a sizable industry, and crushing of tremendous tonnages will be required if conventional processing methods are used. This report presents Bureau of Mines data on crushing experiments, physical properties, and related information for Colorado oil shale. Among the properties important to crushing are slab-forming tendency, resilience, slippery character of the richer grades, and heterogeneous nature of an average charge of Colorado oil shale.

Jan 1, 1960

By J. B. Gayle

Oven widths for experimental and commercial slot-type ovens differ appreably in most instances; the experimental ovens usually ranging from 10 to 14 inches and the commercial units from 14 to 21 inches. Application of results obtained with experimental ovens to commercial practice thus requires major extrapolations. A critical survey of the literature indicated that sufficient information about the effects of variations in oven width on the carbonizing process is not available to permit such extrapolations to be made with any considerable degree of confidence.

Jan 1, 1960

By R. L. Montgomery

Electronegativities of the rare-earth elements were calculated from heats of formation. The values obtained from different compounds varied widely. The postulates of Pauling's electronegativity theory were interpreted for bonds that are primarily ionic; the study showed that many compounds obey rules of the form expected. Revised electronegativity values are given for the more electropositive elements, including the rare-earth metals (which are near magnesium in electronegativity). Estimates of un-known heats of formation are made from electronegativities and are compared with other estimates. INTRODUCTION Calculation of the electronegativities of the rare-earth elements is interesting to show how these metals stand relative to the other metals and to each other, and also possibly to systematize the thermochemical data on them.

Jan 1, 1960

By James P. McGee

Use of nuclear reactors to furnish high-temperature heat is a field that has not received as much attention as propulsion and electric power production. Investigations are being conducted under a joint Atomic Energy Commission (AEC)--Bureau of Mines research program to determine the feasibility of using nuclear heat for chemical processing. A part of this process-heat-reactor program is the study of a system in [hich] helium transfers heat from 8 nuclear reactor to a chemical processing [essel]. This requires construction of (1) a nuclear reactor to operate with helium exit temperature of 2,500° F. and with pressures in the range of 250 to 500 p.s.i.g. and (2) a processing vessel (heat exchanger) to convert the enthalpy of the helium into chemical process reaction heat. Neither component exists at present, and development of each promises to be a formidable task. To aid in the study of such a system, the Bureau of Mines has designed and constructed a vessel heated by electrical induction to simulate a source of nuclear fission heat. This vessel is undergoing preliminary testing. Gasification of coal and reforming of hydrocarbons are promising uses for nuclear heat. It appears that a higher price per unit of nuclear heat can be tolerated for chemical processing than that allowable for power generation.

Jan 1, 1960