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By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By K. K. Kershner

Sulfide ore concentrates containing cobalt, nickel, copper, lead, and iron were salt roasted and leached on a laboratory scale. More than 95 percent of the cobalt, nickel, and copper was recovered. Heating patterns for salt roasting different concentrates were established. More cobalt, nickel, and copper were recovered from a bulk concentrate composed of a mixture of copper concentrate and iron concentrate. This mixture corresponded roughly with the mixture of these materials in stockpiles in southeastern Missouri. A temperature range of 375° to 400° C. was best for salt roasting. Metal chlorides were leached at a pH of 1 from chloridized charges of concentrates, Although the amounts of cobalt, nickel, and copper extracted were high, the amount of iron dissolved simultaneously interfered with subsequent separation and recovery of these metals. The amount of dissolved iron was reduced substantially by steam treating chloridized charges of bulk concentrate at 300° C. In this way, the ratios of cobalt, nickel, and copper to iron in leach liquors permitted satisfactory separation and recovery of these metals. INTRODUCTION The Federal Bureau of Mines is experimenting with chloridizing reactions.4 5 6 7/ Salt roasting of sulfide ores and concentrates, or their calcines, to form metal chlorides has certain advantages. Chlorides of

Jan 1, 1961

By E. R. Palowitch

A centrifugal float-and-sink test procedure has been developed by the Bureau of Mines to reduce the time for the gravimetric separation of coals finer than l4-mesh from as long as 24 hours to less than 1 hour. Comparative tests indicated that centrifuging a minus 14-mesh Pittsburgh-bed coal for 20 minutes at 1,500 revolutions per minute produced results that compared favorably with static float-and-sink test results. Standard deviations of the mean recovery and ash content of the float obtained centrifugally ranged from 1.31 and 0.04 percent, respectively, at 1.30 specific gravity to 0.21 and 0.05 percent, respectively, at 1.60 specific gravity. As in static separations, retreatment of the products separated at low specific gravities was required.

Jan 1, 1961

By Paul L. Campbell

Investigations by the Federal Bureau of Mines of methods of upgrading tar obtained by low-temperature carbonization of lignite showed that ß,ß?-oxydipropionitrile, ß,ß?-iminodipropionitrile, and ß,ß'-thiodipropionitrile were effective solvents for extracting aromatics (aromatic hydrocarbons plus polar compounds) from coal-tar neutral distillate fractions. Batch extraction showed that these solvents extracted approximately the same percentage of aromatics from various neutral oil fractions boiling between approximately 170° and 350° C. In continuous countercurrent extractions using oxydipropionitrile and iminodipropionitrile, approximately 30 to 35 vol.-pct, and 65 to 70 vol.-pct, of the aromatics in 170° to 350° C. neutral distillate oil were extracted at room temperature when solvent-to-oil ratios were 2:1 and 12:1, respectively. As the concentration of aromatics in the neutral distillate oil fraction decreased, the capacities and, to some extent, the selectivities of these solvents for the remaining aromatics decreased. Aromatics were isolated from the extracts and the solvents recovered by washing the extract fractions with a low-boiling paraffinic hydrocarbon such as heptane, using hydrocarbon-to-extract ratios of at least 2:1. The heptane wash removed most of the aromatics but only part of the polar compounds (compounds containing oxygen, sulfur, and nitrogen) from the extracts. The recovered oxydipropionitrile and iminodipropionitrile, containing polar compounds, were effective in extracting aromatics from neutral distillate oils. The contaminated solvents showed essentially the same capacities and selectivities as the pure solvents.

Jan 1, 1961

By J. B. Gayle

During the past several decades, there has been a steady increase in the number and size of experimental ovens used for carbonization research. Although many were originally intended principally for studies of coal expansion, current practice usually includes determinations of the properties of the experimental cokes. With respect to size and shatter characteristics, the cokes from the larger experimental ovens closely approximate those from duplicate charges carbonized in commercial ovens; however, they are consistently lighter and frequently less resistant to degradation by abrasive forces. To minimize these differences, some operators dry the experimental charges before carbonization. The resulting higher dry coal charge densities do, in fact, yield cokes with gravities closely approximating those produced commercially from the same coal or blend but without drying. The drying of the experimental charges may be criticized on the grounds that it represents a departure from commercial practice and may result in oxidation of the samples; for these reasons, the practice has not been universally adopted.

Jan 1, 1961

By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

By Robert H. Merrill

This report summerizes the various studies made to determine the size and support of roofs in the upper shale formation, White Pine Copper Mine, Michigan. These studies were a cooperative effort of the White Pine Copper Company and the Federal Bureau of Mines. Before this investigation, the upper shale formation had been found to contain about 30 to 40 percent of the total mineralization in the ore zones. Investigators estimated that this shale could be economically mined by room-and-pillar methods, provided that the roof would stand over spans of 25 to 32 feet. The problem remained to determine the number of bolts required to safely support these spans. Unbonded fractures in the roof structure of the deposit complicated the use of laboratory methods for determining bolted roof support. Therefore, a method was devised to determine the in-place support which would consider the unbonded fractures. In this method the roofs of 3 rooms with spans of 20, 28, and 36 feet were intentionally overbolted as the rooms were mined. Following stability tests that sometimes exceeded 6 months, the bolts were selectively removed and roof sag, roof strain, and changes in bolt loads were measured concurrently. The number of bolts required for support of these spans was computed from these data.

Jan 1, 1961

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 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 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 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