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By J. G. Donaldson

Nickel containing less than 0.01 percent of total metallic impurities was produced at the Rolla Metallurgy Research Center of the Bureau of Mines by electrodeposition from purified electrolytes. The first report on this research4 described purification of electrolytes by selective precipitation and by liquid-liquid extraction. This second report describes a procedure: or electrodepositing high-purity nickel from electrolytes purified by passing a nickel ammine solution through a column of an ion exchange resin. The nickel electroplated directly from the ammine solution without further treatment; a titanium cathode and two platinum anodes were used. The nickel deposit was dense, smooth, and adherent, and contained less than 0.001 percent each of cobalt, copper, and iron, and spectrographically detectable traces of aluminum, magnesium, and silicon. Nonmetallic impurities in the nickel metal were carbon and sulfur, each present in concentrations of less than 0.01 percent. The results of several experiments planned to purify solid nickel salts by zone refining are also reported. These salts, after purification, were intended for use in preparing electrolytes for deposition of high-purity nickel. Results were not encouraging so that the more promising ion exchange procedure was emphasized chiefly.

Jan 1, 1962

By A. A. Cochran

The purpose of this Bureau of Mines research was to investigate the theoretical and practical aspects of using ionizing radiation to promote chemical reactions that are of interest to metallurgists, and to carry out a radiation study of a suitable reaction. The effect of 44,000 roentgens per hour of 120,000-volt X-rays on the chlorination of highly pure mixtures of rutile, carbon, and various catalysts at temperatures up to 540° C. is described. At these low temperatures, recoveries were very low; however, in the eight different systems studied, an increase in yield due to X-rays was statistically significant in two instances and was of borderline significance in a third instance. In the other five systems, the differences in yield were not significant. Impurities and added catalysts caused relatively large variations in the yield of TiC14 from the reaction. Although the catalysts employed were reported in the literature as positive catalysts for the reaction, most of them were negative catalysts for the highly pure system studied. With only one exception, each increase in the purity of the charge resulted in a decreased yield of TiCl4. The experimental results indicate that many substances catalyze the reaction studied and suggest that the differences in reactivity of the charge stocks may be due to their various contents of positive and negative catalysts.

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. Gall

This report describes Bureau of Mines experiments in gasifying coal in a helium-heated tube-coil reactor. The purpose of this work was to investigate helium as a medium for transferring heat from a nuclear reactor to gasify coal or for use as high-temperature process heat. A laboratory-scale system was designed and constructed to demonstrate feasibility. In preliminary tests with this system, in which the coal was fed as a water slurry, the helium-heating and recycling equipment operated well. Considerable difficulty was experienced, however, in preheating coal slurry to the desired range of 400° - 1,000° F. without plugging the preheaters. Five different preheaters plugged with coke or with salts leached from the coal. The longest operating period wan 12 hours. These difficulties were partly due to the relatively small equipment and flow rates. The gasifier processed l pound per hour of low-rank coal at 300 p.s.i.g. and 1,800° F., with the carbon conversion limited to 20 to 30 percent by the short residence time and slow heat-transfer rate.

Jan 1, 1962

By Frank A. Peters

This evaluation of the sulfurous acid process for the production of metallurgical-grade alumina is the first of a series concerning various known methods of extracting alumina from low-grade aluminous materials and was undertaken to permit comparison with other processes. In the process with which this Bureau of Mines report is concerned, calcined clay is leached under pressure with 20 percent sulfurous acid and then filtered to remove a siliceous residue. The aluminum sulfite remaining in the filtrate is precipitated as a monobasic sulfite which, together with iron sulfite, is then decomposed under pressure to form a crude alumina hydrate and iron oxide. This intermediate product is purified in a modified Bayer process to yield alumina suitable for electrolytic reduction to aluminum. A study estimate (16)3 is used for these evaluations. The capital cost, not including land, is estimated at $95,701,600 on a Marshall and Stevens index basis of 240.0 for a plant producing 1,000 tons a day of alumina or 350,000 tons a year. The annual operating cost for this size plant is estimated at $22,831,100 or $65.23 per ton of alumina using clay at $1 per ton. Depreciation and local taxes are included in the estimate, but profit and Federal taxes are not considered.

Jan 1, 1962

By J. R. Nettle

The development of a process for upgrading offgrade titanium metal by electrorefining in molten salt led to an investigation of the electrotransfer characteristics of selected metals when alloyed with the titanium to be refined. Previous tests on seven binary titanium alloys showed that the degree of transfer of the alloying constituent depends on the constituent and on the operating procedurese.5 This report describes tests on electrorefining ternary mixtures of titanium with selected metallic elements. Ten alloys were prepared from high purity titanium and 2-1/2 percent of each of the metal pairs selected from the same elements used in the binary study; manganese, vanadium, chromium, zirconium, tin, molybdenum, aluminum. Operating variables were similar to those investigated in the binary alloy study that gave minimum alloy metal transfer. The data presented indicate the transfer characteristics of the various metals and combinations tested relative to each other.

Jan 1, 1962

By Robert H. Merrill

Several investigators have obtained solutions for the concentration of stress around circular, ovaloidal, elliptical, and rectangular holes in an elastic, isotropic, semiinfinite plate subjected to uniaxial and biaxial stress. These solutions are used to evaluate the changes in stress around openings immediately under the undercut normally used in conventional block caving operations. The evaluations are based on the assumption that a horizontal undercut removes most of the vertical component of a biaxial stress field. The location and magnitude of the significant changes in stress concentration around the opening are computed. Conditions under which the assumptions used in the evaluations may or may not be consistent with conditions around block caving mines are discussed, and examples of preferred opening shapes for a biaxial (hydrostatic) stress field are shown. This report is a summary of one phase of an investigation to establish design methods for the size and shape of mine openings used in block caving mining methods .

Jan 1, 1962

By W. T. Abel

The rate of the steam-carbon reaction, which is of fundamental importance to coal gasification, was determined by passing steam over graphite specimens suspended in an electrically heated tube. The measurements were made at 1,900° to 2,400° F. and at steam-feed rates of 0.1 to 2.0 moles of steam per mole of carbon per minute. At the maximum steam-feed rate, the reaction rate of carbon ranged from 0.4 percent per minute at 1,900° F. to 7 percent per minute at 2,400° F. Up to about 2,200° F., the steam-feed rate had only a slight effect; above this temperature, it limited the reaction velocity when the final mole fraction of steam in the reaction products was much less than 1.

Jan 1, 1962

By E. G. King

Heat of formation values for mercuric sulfide appear in all the comprehensive listings of thermodynamic data, but experimentally determined entropy values have been lacking. Consequently, all free energy calculations involving mercuric sulfide have been based upon estimated entropy values. This paper reports Bureau of Mines measurements of the low-temperature heat capacity of red mercuric sulfide (cinnabar) and the entropy value at 298.15° K. derived therefrom. The entropy value was combined with heat data to obtain free energy values for the formation of red mercuric sulfide from liquid or gaseous mercury and from rhombic or gaseous diatomic sulfur.

Jan 1, 1962

By R. S. Warfield

Following World War II, the rapid increase in both military and civilian activity in the area served by the Alaska Railroad stimulated interest in the availability of local sources of nonmetallic minerals that might be used for building materials. Except for abundant sand and gravel and some pumice, the construction industry of the area depended entirely on high-cost imports for building materials of mineral origin. Because continued rapid growth was anticipated, development and use of local sources of such materials was advocated by both military and civil authorities to reduce the high costs of con¬struction and bolster the unstable economy of the area. The U.S. Department of the Interior began a program On included examining the numerous deposits of nonmetallic minerals accessible to the Alaska Railroad to determine their possible use as raw materials for the construction industry. Preliminary field investigations were made by the Geological Survey. The more promising deposits were subsequently examined and sampled by Bureau of Mines engineers, and the samples were subjected to the laboratory tests necessary to indicate the chemical and physical characteristics of the raw materials or their products. Such field and laboratory investigations were conducted on clay, shale, argillite, limestone, gypsum, and pumice taken from various parts of the area. In initial phasees of the work, done irate 1948 through 1952, many of the deposits examined were suitable for proctoring building materials. Results of the work completed during that period have been published in a Bureau of Mines report3 giving general information and detailed data on more than 35 deposits that were investigated.

Jan 1, 1962

By W. A. Calhoun

This report gives results of metallurgical investigations performed by the Bureau of Mines on mineral samples taken during April 1959, from Hawaiian bauxite deposits on the islands of Kauai, Maui, and Hawaii. The bauxite samples were tested at the Bureau's Rolla Metallurgy Research Center, Rolla, Mo., to determine if alumina could be extracted. The results were encouraging. Extraction of the alumina by the American Bayer type digest of crude ore samples from Kauai, Maui, and Hawaii recovered 78.8, 73.1, and 70.0 percent, of the total alumina, respectively. These recoveries were increased to 82.8, 85.5, and 79.5 percent by modifying the treatment, which consisted essentially of calcination and weak caustic desilication to provide a residue. The residue was then treated with calcium oxide and digested in a strong caustic solution to extract the alumina.

Jan 1, 1962

By J. V. Batty

Radioisotopes of selenium (se78) and tellurium (Te123) were successfully employed by the Bureau of Mines as tracers in metallurgical research directed to developing improved methods for volatilizing these elements from low-tenor raw materials. Prior research, guided and controlled by conventional analytical methods, was seriously hampered by inconsistent selenium and tellurium analyses, by the slowness of the conventional chemical methods, and by the poor accountability of these volatile elements in test products. Methods were devised and evaluated for admixing the radioactive tracer with typical raw materials and then following the deportment of the selenium and tellurium by radiometric methods with occasional chemical analysis checks. These techniques were found unusually effective in (1) quantifying the completeness and the rate of volatilization of selenium and tellurium while heating the raw materials at different rates to different temperatures and (2) accurately tracing and quantifying the distribution of minute amounts of these volatile elements in the several products made by high-temperature treatment and in the several units comprising the experimental equipment.

Jan 1, 1962

By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

By Philip E. Niebuhr

A procedure, which can be performed in the field by nonanalytical personnel, is given for sensitive spot tests for detecting tellurium or selenium. The expressed need of a field test for detecting small amounts of tellurium, which may be accompanied by relatively large amounts of selenium, has led to the development of this method. Tellurium search has been impeded by the lack of a satisfactory test from the standpoint of sensitivity and specificity. A quantitative laboratory method exists, but it is expensive and relatively laborious. Several other qualitative tests are known, but they require unstable solutions, which must be freshly prepared for use, and a greater variety of laboratory equipment. The particular advantages of the test described are its simplicity and the stability of the reagents required, there-fore is is well adapted for field use. Also, this test was found to be of practical use in the analytical laboratory when screening samples, thereby reducing analytical costs. The roughly quantitative interpretation of the results can save time by indicating the approximate size of the sample taken for a quantitative determination.

Jan 1, 1962

By Joseph M. Singer

This research project had two main objectives: (1) To identify the smoke limits of gaseous fuel-air mixtures and (2) to obtain and evaluate basic chemical information on the formation of smoke in very rich flames near the smoke limit. Such information would do much to establish the circumstances for car-bon deposition in gas appliances and in other types of combustors. Based on tests with ethylene and propane, these studies showed the following: 1. Smoke limits are related to the yellow-tip limits of the fuel. Previous research established sufficient data to permit prediction of yellow-tip limits on gas burners using a wide variety of fuels. The present study of smoke limits deals only with ethylene-air flames, but the concept that was developed is probably applicable to other fuels.

Jan 1, 1962

By W. J. Boone

The Bureau of Mines has programmed for publication a series of Reports of Investigations of studies it has undertaken on low-temperature phase equilibria of several helium-bearing natural gases. This report is the second of a series of papers of the same general title; it is anticipated that additional reports of this series will be published. The advent of a helium conservation program and the prospect of production of helium by private industry, make it especially desirable to publish these data. This report describes phase equilibria related to a natural gas that is processed for helium at the Bureau's Exell Helium Plant (located about 35 miles north of Amarillo, Tex.). Carbon dioxide and water in the gas were removed before making the study; hence the data obtained are representative of the gas stream immediately after similar preliminary treatment in the plant process. Phase equilibrium data were obtained for conditions from -50° to -275° F. and from 100 to 500 p.s.i.a. Analyses of samples were made as follows: For a given run at a selected temperature and pressure, samples of the vapor and liquid phases were analyzed by mass spectrometer, and an additional sample of the liquid phase was analyzed for helium by means of special apparatus (7). 4

Jan 1, 1962

By David E. Fogelson

One model each of three different makes of portable displacement seismographs was calibrated on a shaking table capable of 5,000 pounds of force, Calibration tests were conducted in the frequency range of 5 to 200 c.p,s, and in the amplitude range of 0,002 to 0.05 inch peak-to-peak, The seismographs were tested under two mounting conditions: (1) The feet of the instrument were bolted to the shaking table, and (2) the feet were resting on emery cloth affixed to the table, The results of these tests show that, in the frequency range of 5 to 40 c.p,s, and for vibration levels less than 0.2 g, the magnification for all three instruments is constant with input level but varies slightly with frequency. For vibration levels greater than 0.4 g. and for frequencies greater than 40 c.p.s., the magnification of all three instruments shows large variations with frequency and amplitude of table motion.

Jan 1, 1962

By Willard L. Hunter

The research described in this Bureau of Minus report was conducted to improve the chromium-iron ratio of offgrade chromite. Two methods were used: (1) Iron was selectively reduced from chromite by carbothermic reduction in an electric-arc furnace, and (2) a mixture of carbon, chromite, and sometimes fluorspar was chlorinated to remove a substantial part of the iron. Chromite concentrate from the Mouat deposit in Montana and from northern California was used in the test work. Chromium-bearing slag and chromite that had been beneficiated by a roast-leach process were each smelted to produce high-carbon ferrochromium. Iron was selectively reduced in a laboratory-scale., electric-arc furnace. Carbon additions to the smelting charges varied from 40 to 100 percent of the stoichiometric requirement, and slag basicities were varied from 0.4 to 1.0 chromium-iron ratios of more than 4:1 were obtained with 89 percent recovery of chromium in a chromium-bearing slag.

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

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