Search Documents

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 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 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 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 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 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 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 John E. Shelton

The growing interest in beryllium as a structural material, and its in-creased use in recent years for atomic energy application, have led both government and industry to express concern over the inadequacy of the beryllium resources in the United States and the free world. Contemplated and proposed uses for this unique material will surpass the capacity of the domestic beryllium mining industry to supply raw material, which is presently extracted from relatively small deposits by hand sorting. The need for a simple beneficiation process for beryl ores has long been recognized by the Bureau of Mines, but to date no single process has proved satisfactory for treating deposits containing a sufficient tonnage of beryl ore to warrant commercial exploitation. As a part of the Bureau's continuing effort to develop an economical recovery process, this report describes flotation research on samples of beryl-bearing pegmatites from the George Roebling mine in Connecticut, and the Colony mine in New Hampshire. The study resulted in two methods of treatment to which the ores responded reasonably well.

Jan 1, 1961

By J. W. Town

As part of the Federal Bureau of Mines titanium resources examination program, samples from seven deposits in the Pacific Northwest were tested for amenability to various beneficiation techniques. The samples obtained by the Bureau's Office of Mineral Resources at Spokane, Washington represent a large potential source of titanium. This report summarizes the results of tests at the Bureau's Metallurgy Research Center, Albany, Oregon. Recoveries from tabling placer samples were about 50 percent at grades of 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50

Jan 1, 1961

By Leland A. Yerkes

Refining aluminum from crude aluminum alloys by the subhalide reaction was investigated to develop a method of producing aluminum by means other than electrolysis of its oxide. The best materials and design for the apparatus and also optimum operating conditions, including temperature, pressure, vapor flow rate, and composition of alloy charge were studied. In the subhalide process, aluminum-trihalide vapor reacts with aluminum in the alloy under high temperature and low pressure, forming volatile aluminum monohalide which reverts to aluminum metal and aluminum trihalide on cooling. The only halide used in this investigation was aluminum trichloride. The crude aluminum-silicon alloys used as the principal raw material contained from 21.9 to 36 percent aluminum, and significant quantities of iron and titanium. These alloys were produced by direct electric smelting of clays. Graphite tubing that was heated by an induction coil proved to be satisfactory material for the laboratory reactor chamber, Enclosed in an insulated glass or quartz pipe, the reactor was used in both vertical and horizontal positions with various baffle and tray arrangements for directing the trihalide vapor both over and through the alloy. Aluminum trichloride vapor was generated in the sublimer at one end of the glass pipe, passed into the reactor where contact was made with the crude alloy, and aluminum monochloride gas was formed. When the gaseous mixture of aluminum monochloride and unreacted tri-chloride passed out of the reactor and entered the condenser, the gases were cooled to 900° C. or less, causing the monochloride to disproportionate into aluminum and aluminum trichloride vapor. The aluminum was deposited on the condenser walls while the aluminum trichloride vapor was carried out of the condenser and into the opposite end of the glass pipe where it solidified on the cooled copper coils.

Jan 1, 1961

By W. L. Hunter

The research on this report was conducted to obtain information on the feasibility of producing ferro chromium of varying silicon and carbon contents from domestic chromite. Concentrates from the Mouat deposit were chosen because they typify the chromite found in the Stillwater complex, the largest domestic reserve, and are similar in composition to other extensive North American and foreign deposits. Batch-smelting tests designed to produce high-, medium-, and low-carbon ferrochromium were made in single phase and three-phase, electric-arc, steelmaking furnaces. Agglomeration studies were made in a rotary kiln. Continuous smelting tests were made to yield data on the production of high-carbon ferro chromium and low-carbon ferrochromium-silicon. The carbon content of high-carbon ferrochromium was lowered to the medium-carbon range by oxygen injection. Mouat stockpile concentrates were nodulized in a gas-fired rotary kiln using quartz, limestone, and fluorspar additions in the proportion necessary to flux the slag. The nodules were smelted in a continuous test using coal, coal char, and mixtures of the two consecutively as reductants.

Jan 1, 1961

By J. G. Walters

In 1928, the Coal Carbonization Section of the Federal Bureau of Mines, in cooperation with the American Gas Association, began a survey of the carbonizing properties of American coals. A standard test method for evaluating the carbonizing properties of coals that met the following conditions was developed: To yield products similar to those obtained in commercial operations. To produce yields sufficient to permit analyses and tests of quality. To be laboratory size. To be convenient to operate. To permit reproducible control of test conditions and results. This test method has become known as the Bureau of Mines-American Gas Association (BM-AGA) test (53),3/ and more coals of greater variety have been tested in this apparatus than in any other of similar scale.

Jan 1, 1961

By Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961

By J. T. Dunham

Zirconium has possible use in industry where severe corrosion conditions are encountered because it resists attack from a variety of corrosive environments. However, very little experimental testing has been done to evaluate the corrosion behavior of zirconium when simultaneously subjected to high tensile stresses and exposed to corrosive environments. This investigation was initiated for an evaluation test, but was limited to environments consisting of ferric chloride solutions which were known to attack zirconium and were shown to promote stress-corrosion cracking in preliminary tests. Tests for cracking susceptibility were conducted by the Bureau of Mines to show the effect of stress, solution concentration, air aeration of solution, and the method of mechanical processing. Tensile stress was applied to the specimens by a constant-load method which proved more reliable than a constant-strain method.

Jan 1, 1961