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By Thomas L. McVay

The Bureau of Mines made laboratory batch and small-scale continuous flotation tests of a sample of pegmatite rock from a deposit of the Lithium Corporation of America, Inc., near Kings Mountain, N.C., to determine the feasibility of producing commercial-grade spodumene concentrates. Various reagents and flotation procedures were tested to determine the optimum conditions for floating the spodumene and retarding the gangue minerals. The best results were obtained when sodium fluoride and lignin sulfonate were used as the pulp conditioner and oleic acid was used as the spodumene collector. The continuous flotation tests indicated that commercial-grade. spodumene concentrates analyzing 6.4 pct. Li2O could be produced with recovery of 77 pct. of the lithia in the ore.

Jan 1, 1962

By W. M. Merritts

A joint investigation by the Bureau of Mines and the Christopher Coal Co. at the Humphrey No. 7 mine, operating in the Pittsburgh coalbed in northern West Virginia, was undertaken to gain more insight concerning the hazardous emission of methane gas in mining, This report describes the equipment, procedure, and results. Horizontal bleeder holes drilled in the faces drained large quantities of methane, eliminating downtime of mining equipment. Also, larger quantities of methane were removed by forcing 14 to 25 g.p.m. water at 25 to 200 p.s.i. 5 pressure into the bleeder holes, In one infusion test a fluorescein dye was added to the infusion water; in later mining operations, the infusion water was traced for a distance of 1,500 feet. With vacuum pump applied to the horizontal hole the gas-flow rate increased, and the methane content decreased.

Jan 1, 1962

By Lindsay D. Norman

Eleven major pyrometallurgical processes and operations suggested for recovering manganese from domestic resources are described. These include seven pyrometallurgical processes that usually yield a ferroalloy or a product from which ferromanganese can be produced in one operation. The remaining four involve pyrometallurgical operations whose products require either an additional two-stage process to produce ferromanganese or chemical processing to recover a high-quality manganese oxide product.

Jan 1, 1962

By Michael G. Zabetakis

Vaporization of a solvent into an airstream at temperatures above the flash point of the solvent is hazardous if vapor is liberated at a rate that is sufficient to produce a flammable mixture. In may operations, the formation of such a mixture is prevented by rapid diluton of the vapors with air. The minimum air requirements for the dilution process are determined by the composition of the lower limit mixture at the temperature and pressure of interest. Because limits of flammability cannot always be calculated with sufficient accuracy for a proposed operation, they .rust often be determined experimentally. The present Bureau of Mines investigation was prompted by an application in which the lower limits of flammability of a number of solvent mixtures were required over a range of temperatures at atmospheric pressure. These limits were to be used along with available solvent-vaporization-rate data to establish minimum airflow rates needed to prevent the formation of flammable mixtures in an industrial process. Lower limits of flammability were determined for a number of mixtures containing methyl ethyl ketone, tetrahydrofuran, toluene, ethyl alcohol, and ethyl acetate in dry air-at atmospheric pressure and temperatures between 16° and 200° C. The experimental values were found to be in good agreement at with those predicted by Le Chatelier's law; variations with temperature were in fair agreement with those predicted by a modified Burgess-Wheeler law.

Jan 1, 1962

By James R. Kerr

Although metallurgical benefits of processing metals in a vacuum or reduced atmosphere have been realized for a hundred years, the problem of creating a vacuum in the range from 10-0 to 10-4 mm. of mercury in a moderately sized furnace chamber has been difficult to solve. The demand for these and lower pressures, with the advent of World War II, for separating the fission-able uranium isotope from its stable twin by the electromagnetic process, gave impetus to developing pumps capable of delivering extremely low pressures. With the release of data by the Atomic Energy Commission on methods of securing high vacuum in large equipment, steel companies took the initiative, and the growth of the vacuum-melting industry was assured. Vacuum-induction melting of steel in the United States began on a small scale in early 1945 and in 10 years grew to 60,000 pounds per month or 720,000 pounds per year. The years following 1954 showed tremendous expansion, culminating in 1958 in a capacity of more than 36 million pounds.

Jan 1, 1962

By Sidney Katell

This report is an economic evaluation of the production of hydrogen in a continuous system by the steam oxidation of partially reduced iron oxide in a fluidized bed at 7 atmospheres using producer gas to reduce the iron oxide. The oxidation-reduction step is based on experimental data obtained by the Bureau of Mines at the Pittsburgh Coal Research Center. The estimated capital requirement for a plant producing 30 million std. c.f.d.3 of 99.8 percent purity hydrogen at a discharge pressure of 450 p.s.i.g. is $13,100,000, using January 1961 equipment cost data. Based on a 330-day operating year, the operating cost before profit and taxes with coal price as a variable is estimated to be:

Jan 1, 1962

By William J. Campbell

Expansion measurements of platinum, added as an internal standard, are used for thermal calibration of X-ray cameras and diffractometers. Accuracy of the temperatures derived by this technique depends on the precision of expansion measurements and the reliability of reference expansion data. Temperature measurements to ± 1° C. require ?d or ?a to be determined within ± 0.001 percent. Selected expansion data are concluded to be reliable to 2° C., 5° C., and 25° C., over the temperature ranges 0° C. to 700° C., 700° C. to 1,000° C., and 1,000° C. to 1,700° C., respectively. Tabular expansion values from 25° C. to 1,700° C. in 2° C. intervals were calculated from the following equation; Expansion, percent = [8.91 + 1.28 x 10-3(t-25) + 0.04 x 10-6(t-25) ] [t-25.104 ] These tabular values facilitate future corrections of published temperatures as more reliable expansion-temperature data become available.

Jan 1, 1962

By Michael G. Zabetakis

The spillage of liquid diethyl ether in rooms at floor level and 3 feet above the floor resulted in flammable vapor-air mixtures in the immediate vicinity of the exposed liquido The liquid temperature was found to decrease by as much as 35° C., with a resultant decrease in vaporization rate. A search of the literature yielded numerous references to unstable peroxide (residue) formed by the autoxidation of ether. Such residues appear to constitute an explosion hazard in the condensed state.

Jan 1, 1962

By Walter C. Lorenz

In connection with its renewed study seeking solutions to problems created by release of acid water from bituminous coal mines, the Bureau of Mines recently surveyed reports already written on the subject. This publication is based on that search. The Problem Poor distribution of water is evident on an ordinary geographic map of the United States. The more abundant supplies of surface water appear to be centered in the northeast, the southeast, and the central humid areas of the country. It is in the midst of this abundant surface water, in the Ohio River Valley, that most of the bituminous coal is mined. Varied industry has located in the valley to use the coal and the river. The coal is a source of power and o raw material. The river provides transportation for raw and finished materials; equally important, it provides the water that is used for cooling and processing in manufacturing. It also serves as a vehicle for the disposal of waste.

Jan 1, 1962

By R. Barany

In this paper, closed expressions have been obtained for the frequency spectrum of a Born-Karman square lattice in terms of elliptic and hyperelliptic integrals. This work is part of continuing research by the Bureau of Mines with the thermodynamic properties of metals and minerals. Although other workers have obtained various types of approximations for the general case of the frequency spectrum of a square lattice, no one previously has obtained closed analytic expressions for this spectrum. To understand the optical and thermodynamic properties of crystals, several investigators have studied the distribution of frequencies of normal modes of vibration of the crystal lattice. Born and Karman3 laid the foundation for the theory of lattice dynamics and obtained detailed results for the case of a one-dimensional lattice. Blackman4 used numerical techniques to estimate the frequency distribution of a two-dimensional square lattice. Mbntroll5 analytically determined the frequency distribution of a square lattice for a particular value of the force constants. He also studied the more general problem and obtained some analytic approximations, using the method of moments. However, the calculations by this method were so difficult that it was not always practicable to carry them out. Van Hove6 and Montroll7 studied the nature of the singularities in the frequency spectrum of both a two and

Jan 1, 1962

By R. L. Lincoln

The effects of adding from 1 to 50 atomic percent (a/o) to vanadium were investigated by the Bureau of Mines. Properties studied included as-cast and annealed hardness, microstructure, fabricability at room temperature and elevated temperature, tensile strength, electrical resistivity, and oxidation resistance at 625° and 800° 2. Additions of small amounts of hafnium resulted in lessened as-cast hardness, decreased electrical resistivity, impaired roll- ability, increased oxidation resistance, and greater tensile strength. Larger amount of hafnium caused greater as-cast hardness, increased electrical resistivity, further impaired rollability, continued increase in oxidation resistance, and lessened tensile strength. INTRODUCTION The purpose of this study was to determine the effect of hafnium additions on the properties of vanadium and to learn if this binary alloy had any special or unusual properties. This investigation is a part of a larger research project in which new and expanded uses of vanadium are being sought. Domes tic vanadium is found frequently in combination with uranium, and because of the demand for uranium as a nuclear fuel, there now exists a surplus of vanadium-bearing minerals and vanadium pentoxide as a byproduct of uranium production. Primary principles of conservation demand that greater use be made of this readily available surplus; finding suitable metals to alloy with vanadium to enhance its properties is one way to increase its utilization. This report is the result of an investigation of the effects on the properties of vanadium when hafnium is added in amounts from 1 to 50 a/o.

Jan 1, 1962

By Alla D. Mah

The need for more and better basic thermodynamic data for the oxides of many of the rare metals is evident to anyone who attempts thermodynamic calculations involving these substances. In continuation of a Bureau of Mines program to meet this need, this paper reports new experimental values of the heats of formation at 298.15° K. of the hexagonal crystalline variety of germanium dioxide and germanium dioxide glass. The values were obtained by means of combustion calorimetry and sodium hydroxide-solution calorimetry. The calorimetric results also made possible the derivation of values for the heat and entropy of fusion of hexagonal germanium dioxide at its melting point. The newly measured data were combined with previously known entropy and high-temperature heat content values to obtain heats and free energies of formation of germanium dioxide (in the hexagonal crystalline, glassy, and liquid states) over the temperature range from 298.15° to 2,000° K.

Jan 1, 1962

By R. C. Bates

Uranium mine workers? daily exposure to radon daughters was estimated by two methods of sampling, detailed and spot-check. Both methods involve time- weighting measured exposure levels to arrive at an average exposure figure. Random sampling, or sampling without regard for the duration of exposure, has proved inadequate for estimating average exposure levels. During the first phase of the study, the breathing zones of eight workmen in three underground uranium mines were sampled for an entire shift; 20 to 36 radon-daughter samples were collected per man-shift, Analysis of these data indicated that a suitably accurate estimate of the full-shift exposure could be made by time weighting a considerable lesser number of representative radon-daughter samples. This analysis led to the spot-check method of estimating full-shift exposures to radon daughters. Additional detailed studies were made in seven mines to Learn more about the full-shift radon-daughter exposures and to test the spot-check method, In all, 617 radon-daughter samples were taken in 10 underground uranium mines during 26 man-shifts, and the spot-check method was tested 35 times.

Jan 1, 1962

By C. J. Chindgren

Upgrading of commercial red cake and recovery of vanadium oxide from uranium-vanadium mill solutions were investigated by the Bureau of Mines. Alternative procedures potentially useful for manufacture of high-quality vanadium oxide at the mill site were explored and developed. The simplest and best procedure for converting commercial red cake containing about 10 percent combined sodium and potassium oxides (Na20) (K20) into a 98- to 99-percent vanadium pentoxide (V205 product appeared to be a metathesis in an ammoniacal solution of ammonium sulfate. Molybdenum, as well as the alkali metal oxides, was removed from the red cake by this procedure at a modest expenditure of labor and reagents. When preparing vanadium oxide of higher grade, it was necessary to dissolve the red cake and reprecipitate the vanadium as ammonium metavanadate. Calcination at 450° C, decomposed the metavanadate and yielded oxide of about 99.5 percent V205. By recyrstallizing the metavanadate before decomposition, an oxide product approaching 99.9-percent purity was obtained.

Jan 1, 1962

By Robert K. Koch

Laboratory-scale studies on defluorination of natural and synthetic fluorspars by pyrohydrolysis at 1,500° C. were made to determine the feasibility of developing a process for producing hydrogen fluoride from siliceous fluorspars. It was found that the reaction (at 1,500° C.) is not promising for process development, even though a silica-free offgas can be generated. The primary difficulty is the low hydrogen fluoride content of the offgases; an HF content of 6 percent was the best achieved. Previous research by the Bureau of Mines has demonstrated that offgases averaging 27 percent hydrogen fluoride can be produced under carefully controlled conditions at 1,280° C. The lower temperature process is a better method for production of HF. However, charges in which the CaF to Si02 mole ratio varied from 0.4 to 2 could be processed with similar results. Also, combined alumina and ferric oxide contents up to 25 mole-percent did not noticeably alter the rate of defluorination. Therefore, virtually any natural siliceous fluorspar would respond in essentially the same manner when exposed to water vapor at 1,500° C.

Jan 1, 1962

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1962

By Clark F. Grain

These investigations were undertaken as part of the Bureau of Mines program for the development and evaluation of high temperature nonmetallic materials. This report consists of thermal expansion and phase inversion measurements by high-temperature X-ray diffractometry on the principal oxides of beryllium (BeO), calcium (CaO), titanium (TiO2 ), zirconium (ZrO2 ), hafnium (HfO2), and thorium (ThO2); all were high-purity commercially available oxides. Thermal expansion values were calculated from unit cell dimensions measured at selected temperatures. Expansion was determined parallel to each major crystallographic axis for the anisotropic oxides: BeO, TOi2, ZrC2, and HfO2. Combined random and systematic errors in the thermal expansion values are considered to be less than 3 percent of the total expansion at 500° C. and approximately 2 percent at 1,000° C. No hysteresis in the expansion curves was noted between heating and cooling cycles. The Bureau's values were compared with published expansion measurements obtained by X-ray diffraction, dilatometric, interferometric, and telemicroscopic techniques. For anisotropic oxides, average linear expansion values were calculated from the volume expansion.

Jan 1, 1962

By F. H. Gibson

In recent years physico-chemical techniques have been applied for rapid analysis of coal and coke ash as replacements for classical wet-chemical methods. Although the classical methods are accurate, they are time consuming because many chemical separations are necessary to complete an analysis, and they require skilled analysts for accurate work (12).4 For the past several years the Bureau of Mines has applied some of the newer physico-chemical techniques in its continued search for new and improved methods at analysis. The methods of analyzing coal and coke ash evolved from this work include spectrophotometric methods far SiO2, A120, , Fe203 , TiO2, and P2O5; chelatometric titration for CaO and MgO; and flame photometry for Na20 and K2O. The methods are rapid and direct, are suitable for analyzing a group of samples at the same time in production work, and dire results with almost the same accuracy as classical procedures. With the new methods, complete analyses in duplicate can be obtained at a rate of 2 to 3 times that of conventional methods.

Jan 1, 1962

By J. Burlin Johnson

In small-scale blasting experiments conducted in the Bureau of Mines laboratory, small charges were used to produce craters in blocks of concrete mortar. The results are compared with larger scale experiments of other research workers, and the comparison demonstrates the similarity of the results obtained and indicates that small-scale blasting should be a useful tool for predicting large-scale blasting effects. INTRODUCTION The purpose at this investigation was to conduct blasting experiments in mortar in the laboratory and then, by comparing the results with those from larger scale field blasts in rock to determine to what extent, if any, the laboratory results resemble those in the field. The work described herein was the initial phase of a project aimed at evaluating small-scale blasting as a tool for use in improving blasting techniques. It is evident from the stand-point of control and cost that small-scale blasting would be valuable in the study of rock fragmentation by blasting in mines and quarries, if the extrapolation is valid.

Jan 1, 1962

By K. E. Tame

Pollution from radioactive nuclides, principally Ra226, in liquid waste from uranium mills can be minimized by reusing the waste solution within the mill. Such reuse of waste solution in the Vitro Chemical Co.-type process was investigated in the laboratory. Vitro employs an acid leaching process for dissolution of the uranium, countercurrent decantation for liquid-solid separation and washing, and amine solvent extraction for recovery of the uranium from solution. The simulated reuse of barren raffinate in the mill circuit was carried through two separate laboratory campaigns of 29 and 31 cycles. Conventional chloride stripping of the amine was employed in the first campaign, whereas nitrate stripping was used in the second campaign. Dissolution of uranium from the are in the acid leaching circuit averaged 96 percent. Washing efficiencies of 98 to 99 percent were attained by using 4 volume tons of combined raffinate and makeup water per ton of ore. Uranium recovery from the pregnant solution using a 5-percent solution of amine LA-1 in kerosine ranged from 99.3 to 99.9 percent.

Jan 1, 1962