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By S. L. May

Investigations by the Federal Bureau of Mines indicate that hafnium and zirconium compounds of acceptable purity can be extracted from Nigerian zircon concentrates. Chlorination and caustic soda fusion techniques were used to extract 85 to 95 percent of the valuable metals from the concentrate. The extracted hafnium and zirconium compounds were purified by recrystallization of the oxychlorides or by formation of complex salts during chlorination. The zirconium-hafnium product of the recrystallization method contained 15 parts per million of uranium, and the product of the salt-complex method contained less than 10 parts per million of uranium. The hafnium was separated from zirconium by solvent extraction methods. A zirconium product containing 0.3 percent hafnium and a hafnium product containing 4 percent zirconium were obtained. At the request of the Atomic Energy Commission (AEC), work was started to develop techniques for processing Nigerian zircon concentrates in commercial installations presently engaged in producing zirconium and hafnium metals from ores. The Nigerian zircon has a high hafnium content, but the presence of uranium and thorium is a problem not normally encountered in processing zircon concentrates.

Jan 1, 1961

By J. W. Town

This report summarizes the results of laboratory investigations conducted by the Federal Bureau of Mines to obtain hydrometallurgical information on the dissolution of mercury sulfides from ores, flotation concentrates, and pure mercuric sulfides. Statistical methods were used to design the experiments and evaluate the resulting data. Studies demonstrated that cinnabar is readily soluble in sodium sulfide, partly soluble in potassium sulfide, and essentially insoluble in ammonium sulfide. Additions of sodium hydroxide or potassium hydroxide to sodium sulfide solutions increased mercury extraction slightly; when either was added to potassium sulfide or ammonium sulfide solutions, mercury extraction was equal to that of sodium sulfide. Tests at the Albany Metallurgy Research Center showed that sodium sulfide would completely dissolve chemically pure mercuric sulfide, more than 95 percent of the cinnabar in 5-percent mercury flotation concentrates, and 60 to 90 percent of the cinnabar in low-grade ores. The double-leach tests showed that potassium sulfide would dissolve over 90 percent of the arsenic in mercury-arsenic products and 1 to 10 percent of the mercury; then sodium sulfide-hydroxide solutions would dissolve 80 to 90 percent of the remaining mercury and 5 to 10 percent of the arsenic.

Jan 1, 1961

By F. W. Wood

A program of research was conducted by the Bureau of Mines to investigate anomalies in electrical-discharge behavior during consumable-electrode arc melting of titanium and to study the effects of these irregularities on arc-furnace explosions. A major effort was devoted to an experimental survey of arc behavior and a qualitative definition of discharge phenomena.3/ An important conclusion was that the "glow" of industrial arc-melting terminology is not a glow discharge but a skittering arc in a displaced position. The conditions that permit displaced skittering were tentatively defined. The displaced skittering arcs tended to damage melting crucibles in two ways, and details of possible mechanisms leading to crucible rupture and explosive reactions have been proposed accordingly. However, no acceptable means of preventing crucible damage was discovered.

Jan 1, 1961

By J. S. Browning

Laboratory and pilot-plant tests of spodumene-beryl pegmatites of the Kings Mountain, N. C., area resulted in development of a new and improved method by the Bureau of Mines for separating and recovering spodumene, mica, and beryl. The process was successfully applied to other domestic pegmatites and a spodumene flotation-plant tailing containing about 0.5 percent beryl. The method comprised soap flotation of the spodumene, using combinations of sodium fluoride and lignin sulfonate as conditioning agents to recover 80 to 85 percent of the contained lithia in concentrates assaying over 6 percent Li20. About 80 percent or more of the beryl was retarded in the spodumene tailing. The beryl subsequently was activated, floated, and cleaned in a secondary circuit to yield beryl concentrates containing 6 to 7 percent BeO. The tests also demonstrated that a good recovery of high-grade mica could be produced.

Jan 1, 1961

By A. L. Engel

This report is a compilation of preliminary and, in some cases, more extensive concentration experiments by the Federal Bureau of Mines on low-and medium-grade fluorspar ores from three localities in Nevada and one in California. The work was done on samples obtained from Shoshone mine, Nye County, Valery mine, Pershing County, and the Broken Hills mine, Mineral County, all in Nevada, and Dirty Weather mine, Inyo County, Calif. These investigations were made to aid in the development of domestic fluorspar resources, in line with the Bureau's long-established program of conservation of mineral resources. The treatment methods employed in the experimental work described included simulated or "heavy-liquid" gravity concentration of coarse minerals and comparatively fine-grained minerals, and flotation concentration of finely-ground minerals. These methods were attempted in order to beneficiate the ores and produce concentrates which could be marketed readily, with as high a recovery rate as possible, while using simple treatment methods suitable for small-scale operation.

Jan 1, 1961

By R. T. Johansen

The wettability of petroleum reservoir materials by water and crude oil has been recognized as an important factor in determining waterflood behavior. The problem of simulating and studying reservoir conditions and characteristics, to produce laboratory results congruous with field experience, has been examined by many methods. (1, 2, 3, 4).4/ The most generally accepted approach to this problem is determining wettability of the porous medium by imbibition methods; or, after solvent extraction, predetermining the wettability of the samples by coating the surface of the medium to render it preferentially oil-or water-wet (3, 5). The emphasis of wettability studies has been placed on the characteristics of the reservoir materials with little consideration being given to the fluids themselves. Therefore, the wetting tendencies of crude oils have been investigated by a recently developed method (6). Imbibition and the more general phenomena of capillary pressure are the most direct ways to measure wettability. The simplest type of capillary pressure observations involves the use of an interfacial-tension capillarimeter, which does not produce as separate values either interfacial tension or contact angle. Actually, these quantities do not have independent significance in reservoir engineering, and the property of wettability they are intended to evaluate is given, immediately by capillarimetric measurements.

Jan 1, 1961

By Murray Jacobson

Data obtained by the Federal Bureau of Mines on the dust explosion hazard in air are presented for 220 samples of agricultural products. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum electrical energy for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent flame propagation, and, in a few instances, the permissible oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle size and source of sample on explosibility are shown. The relative ignition sensitivity, severity of explosion, and overall explosibility of the materials are characterized by empirical indexes. This report contains Ma obtained by the Bureau in laboratory studies on the explosion hazards of agricultural dusts. Recognition of the dangers will encourage adoption of adequate measures to prevent ignition and explosion during preparation, processing, and utilization of the materials. Agricultural products constitute one of the largest groups of materials used in America. More than 260 million tons of various grains, much of which now exists in dust form, was grown in 1958.6/ Over 600,000 tons of the annual production of 200

Jan 1, 1961

By W. A. Calhoun

The purpose of this investigation was to develop economical mineral dressing processes for removing objectionable quantities of impurities, such as quartz and pyrite, from refractory clay deposits in east central Missouri. The presence of excessive quartz in these clays causes crazing. Pyrite causes bloating and unsightly dark blobs on the surface of fired refractory brick. The iron concentration in the proper state of oxidation may also act as nucleation centers for carbon crystal growth which can result in bursting of the refractory. Numerous deposits, representing a very large tonnage, have been examined and prospected by various refractories companies and found to contain impurities in objectionable quantities. Upgrading these clays would greatly extend our reserves of high-quality refractory clays. Wet-tabling and wet-cyclone concentration were found to be effective for removal of impurities from clays. Of the two methods, wet-cyclone concentra¬tion would be cheaper and more effective. Although wet-tabling improved the refractory properties of each clay, beneficiation by wet-cyclone produced clays of superior quality. Clay recoveries by wet-cycloning ranged from 56.1 to 81.8 percent of the weight of the crude samples, and the beneficiated clays contained from 71.9 to 94.4 percent of the total alumina. The pyrometric cone equivalent (PCE) was increased from 1 to 3 cones by wet-cycloning. The beneficiated clays also met the reheat shrinkage requirements on refiring to 1,400° C. Missouri is one of the major domestic sources of fare clay. In addition to deposits of high-grade refractory clays, there arc many deposits that contain small percentages of impurities, which render the clays unfit for the production of high-heat-duty firebrick. Development of methods to beneficiate these submarginal clays to usable materials would greatly increase commercial fire clay resources.

Jan 1, 1961

By V. M. Benson

A simplified, routine method for determining lithium in lithium-bearing rock is presented. The sample is decomposed by repeated treatments with nitric, hydrofluoric, and perchloric acids. Since this procedure does not appreciably dissolve beryl, interference by beryllium (the principal interfering cation) is minimized for most samples. The salts are brought into solution with water and enough citric acid-ammonium citrate buffer is added to make the final volumetric dilution 0.20 M with respect to citrate. The addition of citrate greatly reduces anion interference in the hydrogen-oxygen flame, slightly increases the intensity of the lithium 671 millimicron emission line, and reduces the effect of most of the interfering cations to the extent that analytical separations are not necessary. The accuracy of results of single determinations of lithium in a pegmatite containing spodumene, lithium-bearing mica, and beryl are approximately equal to that obtained by other flame methods, INTRODUCTION This investigation was undertaken in Bureau of Mines laboratories to develop a reliable, rapid, routine analytical method for determining lithium in lithium-bearing minerals. The requirements of the procedure were that the method should be applicable to the analysis of a variety of lithium-bearing ores and test products, and the results would be reasonably accurate for materials containing 0.05 to 8 percent Li20.

Jan 1, 1961

By D. A. Wilson

Several promising systems for selectively oxidizing the iron in an iron-tin alloy commonly called "hardhead" were investigated in a research project conducted to devise a method for recovering tin from this troublesome alloy. A satisfactory oxidation method was developed and tested successfully on melts of 2,000 grams. Molten hardhead (near 1,080° C.) was blown with air to oxidize iron and leave tin in the reduced state. Recovery of available tin was 96 to 98 percent. Tin products contained 2 to 0.1 percent iron which was reduced to 0.06 percent by filtration at 250° C. Iron oxide formed during oxidation was absorbed by a fluid flux cover composed of 43 percent silica, 17 percent burned limestone, and 40 percent fused borax. Less successful but nevertheless promising results were obtained with mixtures of steam and hydrogen which were sufficiently selective at temperatures between 600° and 950° C. but did not result in complete oxidation of iron. Carbon dioxide-carbon monoxide mixtures also oxidized iron selectively but incompletely. Both stern and carbon dioxide systems produced sufficiently encouraging results to additional research on these systems.

Jan 1, 1961

By William J. Campbell

One of the principal objectives of the Bureau of Mines program for developing super refractory materials is to obtain fundamental data on the physical properties of refractory oxides. This particular investigation obtained accurate thermal expansion coefficients for alpha alumina and evaluated, critically, those coefficients with other published values. High-temperature X-ray diffractometer measurements, by the Bureau, showed that alpha alumina expands anisotropically with expansion parallel to the c axis approximately 10 percent greater than parallel to the a axis. Thermal expansion characteristics of four different alumina samples were determined up to 1,200° C.; the results are presented in both tabular and graphical form. The combined random and systematic errors in the measurements are considered less than 3 percent above 500° C, and approximately 2 percent at 1,000° C. No differences in expansion were observed between the samples or between the heating or cooling cycles.

Jan 1, 1961

By D. H. Baker

These investigations were conducted to determine the feasibility of molten salt electrorefining of zirconium scrap, offgrade sponge, and alloys under contract number AT(11-1)-475 between the Atomic Energy Commission and the Federal Bureau of Mines. Offgrade zirconium sponge having a Brinell hardness of 169 can be refined by this technique to produce metal having, consistently, a Brinell hardness of less than 90. Also, zirconium alloy scrap, approximating zircaloy-2 in composition, can be refined to recover zirconium metal with a Brinell hardness of less than 100 that is essentially free of the major alloying elements. Analysis showed that the quantities of these elements were decreased as follows: iron from 0.27 to 0.002, tin from 1.36 to 0.001, nickel from 0.02 to 0.001, and chromium from 0.12 to 0.002 percent.

Jan 1, 1961

By James E. Mauser

This report deals with the investigation of a continuous process for producing pure zirconium. It covers the construction, operation, and maintenance of the semicontinuous reactor. The report covers a study of test variables, such as reactor temperature and reluctant charge weights, and evaluates the results, such as billet metal hardness, residual billet salt content, and suitability of a purified billet as a consumable electrode for arc melting. The purpose of this project was to develop an inexpensive and continuous process for producing pure zirconium. The process developed, termed the semicontinuous reactor process, produced billets of compacted zirconium sponge. The metal was produced by reducing zirconium tetrachloride with sodium and magnesium beneath molten byproduct salt. Hydraulic rams at each end of a vertical reaction tube compacted the sponge and ejected it as a billet. These billets were purified by heat under vacuum to remove entrapped salt. The goal was to utilize the purified billet directly as a consumable electrode for arc melting.

Jan 1, 1961

By R. L. Grant

The principal official test performed by the Bureau of Mines to determine the permissibility of coal-mine explosives, commonly referred to as the gallery test, has been in use at the Bruceton station for many years (2, 16).4/ In this test the explosive under study is loaded into the borehole of a steel cannon and fired into a flammable mixture of natural gas and air or natural gas, air, and coal dust. To meet the requirements for permissibility, the explosive must not ignite the gas mixture under the conditions of the test. There is little doubt that these tests have succeeded in the main objective, namely, to screen the relatively safe from the relatively hazardous explosives. It has been generally conceded that adoption of permissible explosives by the coal-mining industry in the United States has substantially reduced the frequency of disastrous underground explosions caused by blasting. In recent years, however, research workers planning programs for improving the safety of coal-mine explosives have felt the growing need of a more quantitative method for measuring the incendivity of explosives based on a better understanding of the role of the important variables in the gallery tests, Accordingly, it was decided to apply certain statistical methods and techniques to the gallery test to develop it into a more precise tool for evaluating permissible explosives. One of the first and more important methods applied for this purpose was the up-and-down technique (6,7,17), It was demonstrated (14,15) that the weight of the explosive charge directly affects the ignition probability of the natural gas-air atmosphere and that the curve of ignition probability versus charge weight is a cumulative normal curve. Following these experiments, a program, still in progress, was set up to study how the addition of sodium chloride to various permissible-type ex-plosives affects their incendivity. This program resulted in 3,294 shots,

Jan 1, 1961

By W. M. Dressel

The Federal Bureau of Mines has obtained data by differential thermal analysis of the various minerals that represent the nation's resources in manganese. These data are supported by X-ray diffraction analysis, chemical analysis, mineralography, and optical mineralogy, and provide fundamental information on the response of each mineral to thermal treatment in oxidizing, reducing, and neutral atmospheres. The information can be applied advantage¬ously in the identification of manganese minerals. Its greatest potential value, however, lies in the application of the quantitative data on the reaction temperatures, rates, and products to the more efficient extraction of manganese from U.S. ores. Thermal analysis curves are presented for certain manganese minerals, namely hausmannite, bixbyite, braunite, pyrolusite, lithiophorite, cryptomelane, hollandite, manganite, rhodochrosite, and rhodonite. The original minerals and the products of their thermal decomposition were identified by X-ray diffraction analysis, supplemented by chemical analysis and mineralogical identification.

Jan 1, 1961

By R. P. Jewett

The object of this investigation was to correlate the crushing strength of green pellets prepared from magnetite, specular and earthy hematite with the particle size of these respective raw materials. In this study no attempt was made to correlate the strength of fired pellets and particle size. The effect of particle size upon a number of fine ores and concentrates was studied. Much of the low-grade ore reserves in the Lake Superior Region must be finely ground before concentration and then agglomerated for iron and steelmaking processes. Fine natural ores also must be agglomerated. Pellets constitute an important type of agglomerate. Considerable handling occurs during screening to remove undersize and oversize pellets, and in transfering green unfired pellets from the balling machines to the heat-hardening equipment. As a result the strength of the green pellets is a factor of great importance.

Jan 1, 1961

By E. C. Perkins

The purpose of the research described in this report was to develop techniques for using ilmenite from domestic deposits for the production of titanium tetrachloride. The research was done by the Federal Bureau of Mines in cooperation with the General Services Administration under contract DMP-116, Utilization of Domestic Ilmenite. Bench-scale continuous chlorination of an Idaho ilmenite containing 27.9 percent titanium and 35.6 percent iron yielded a crude titanium tetrachloride suitable for purification and for the production of titanium metal and pigment. A summary of the results of 380 hours of operation showed that 82.4 percent of the titanium was chlorinated, with 92.5 percent utilization of chlorine. The construction- of a. quartz tube chlorinator 4-inches in diameter and 24 inches long is described with the necessary details of operation.

Jan 1, 1961

By H. S. Caldwell

The objective of this investigation by the Bureau of Mines was to develop and test for laboratory use a retort embodying many features required for practical commercial-scale applications of vacuum distillation of metals. A gas-fired vacuum retort was developed comprising a hollow, cylindrical graphite liner encased in a thin shell of stainless steel. The liner prevents the shell from collapsing under vacuum and protects it from corrosion by metal vapors and the molten metal charge. The vacuum-tight shell protects the liner from oxidation and flame erosion. The retort was used to distill zinc from dross and die-casting scrap. More than 99 percent of the zinc was recovered as a condensate containing 99.8 to 99.9 percent zinc. (Atmospheric distillation recovers 95 to 98 percent at a purity of 99.5 percent zinc.) Distillation rates of 50 pounds of zinc per hour were attained at a temperature of 65° C. with pressures ranging between 50 and 100 microns. Distillation at this low temperature is not practicable at atmospheric pressure. Also, the retort is suitable for distilling other volatile metals such as cadmium and magnesium.

Jan 1, 1961

By A. E. J. Gallagher

This report summarizes the results of flotation studies conducted by the Federal Bureau of Mines on samples of extremely fine-grained lead-zinc sulfide ores. Samples from five ore deposits in the Pine Creek area, Coeur d'Alene district, Idaho, and one deposit in the Metaline district, Washington, were studied at the Albany Metallurgy Research Center to determine the recovery of sulfide lead and zinc by flotation. During the investigation it was found that flotation could be effectively applied to the selective recovery of exceedingly fine-grained lead and zinc sulfide minerals. Separation of galena and sphalerite was obtained on pulps ground through 1,600-mesh, in which most of the particles were smaller than 5 microns. Selectivity and recovery of minerals in this fine size range were enhanced by use of a chemical dye, diphenylthiocarbazone, as a galena promoter. Although unsuccessful on one ore, application of the dye in treatment of two other very fine-grained ores yielded lead concentrates containing over 62 percent Pb at recoveries in excess of 85 percent. More than 55 percent of the lead in these concentrates occurred as particles smaller than 2 microns.

Jan 1, 1961

By Miles B. Royer

The experimental blast furnace has attracted increasing interest during the past decade as a practical means for investigating a broad range of blast-furnace smelting problems. Under experimental-furnace conditions, information can be obtained with less expenditure of time and raw materials and, therefore, at lower cost than comparable information could be obtained under industrial operating conditions. Furthermore, the experimental furnace may be operated beyond the range of smooth operation, even to failure, to delineate the limits of operability. Such deviation from normal operating practice would be economically intolerable in industrial operations where production and operating stability might be disrupted. The Federal Bureau of Mines experimental blast furnace at Bruceton, Pa., near Pittsburgh, has been operated and under development since 1951. However, the usefulness of this experimental data to industrial practice was somewhat nebulous in early experiments, and the correlation of the experimental blast furnace with the industrial blast furnace was not known.

Jan 1, 1961