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By R. E. Lindstrom

A study of ion-exchange resin crosslinkage and eluant flow rate, resin-bed shape, and addition of separating ions to feed stock was undertaken to determine their effect on the separation efficiency of ion-exchange on bastna-site-rare-earth elements. Results show that 12-percent divinylbenzene (DVB) crosslinkage resin is detrimental to separation efficiency at flow rates over 2 to 5 ml./min./sq. cm.; whereas, separation with 4-percent DVB crosslinkage resin is relatively unaffected by flow rates between 2 and 10 m1./min./sq.cm.

Jan 1, 1959

By Farrel W. Lytle

Instrumental analysis has become an indispensable tool in research and production of the rare-earth elements. This development can be attributed mainly to a combination of two factors--the marked chemical similarity of the rare-earth elements, which excludes classical methods of analysis, and the speed and accuracy of instrumental-analysis techniques. With continued improvements in methods of producing high-purity rare-earth elements, keeping pace instrumentally is becoming much more difficult. Accordingly, greater emphasis is being placed on improving instrumental limits of detection and accuracy. The methods employed most frequently for determining impurities in rare-earth elements involve use of the optical-emission spectrograph (3, 4)4/ and the spectrophotometer (9). Although numerous X-ray-emission spectrographic methods (6-8) have been developed for analyzing rare earths, these techniques have not included detection of low-level impurities. This investigation was conducted to find the precision and accuracy of X-ray fluorescence in deter-mining impurities in rare-earth oxides in the 0.01-to 1.0-percent-concentration range.

Jan 1, 1959

By E. A. Magill

This report is one of a series prepared by the Bureau of Mines on manganese deposits of the Northwestern States. It describes properties on the Olympic Peninsula, Wash. Exploration by the Federal Bureau of Mines in 1939-40 and 1954-55 on several typical deposits is summarized, and examination data are presented for other manganese deposits on the peninsula. An attempt was made to list all known occurrences; however, some properties are abandoned, and their exact location is unknown.

Jan 1, 1960

By H. C. Carpenter

Data are presented comparing results obtained with 17 different catalysts in hydrogenating crude shale oil to gasoline in single-pass operation. A method is described for predicting the maximum yield of gasoline obtainable at constant pressure for each catalyst from results of a limited number of experiments at different temperatures. Operating variables have considerable influence on yields and properties of products. With most of the catalysts, at operating temperatures below 890° F. liquid yield exceeded 100 volume-percent. Above this temperature the volume of liquid product decreased rapidly. Maximum gasoline production in most instances was achieved at a temperature higher than that at which the maximum volume of liquid product was produced.

Jan 1, 1959

By M. R. Geer

Traditionally, fine coal is more troublesome than the coarser sizes at every step of the coal-preparation process--screening, cleaning, dewatering, and drying. Therefore the present trend toward a higher proportion of fines in the run-of-mine product, brought about by changes in mining practice necessitated to increase productivity, has added greatly to the task of preparing coal for the market. One of the more difficult and costly problems involved is that of recovering fine solids from the washery water. These fine solids should be recovered in the interest of conservation, and they must be removed to provide recirculating water of proper quality. If there is a plant effluent, it must meet increasingly stringent requirements against stream pollution. Vacuum filtration has been used for years at a few plants to recover the extreme fines, but its additional cost discouraged general adoption until recently. Now, with growing emphasis on better solids recovery, filtration is becoming more widespread. Many coal slurries filter readily, giving high cake rates and clean filtrates. Others, however, particularly those containing either a high proportion of material finer than 200-mesh or an appreciable amount of clay, are much more difficult to filter. Many of these refractory slurries can be rendered more filterable by flocculation. A previous report of Bureau of Mines research dealing with flocculation alone was published in 1940.5/

Jan 1, 1959

By D. J. Bauer

This report covers a phase of an extraction project carried out as part of a research program on rare-earth technology. The current project--the production of pure cerium compounds--is an intermediate step between ore processing and metal reduction. In this connection, a study on a separatory-funne1 scale was made on nonreducing extractants for recovering cerium (IV) from tri-n-butyl phosphate (TBP) and of methods for recovering the cerium nitrate from the strip solution. Dilute sulfuric acid was found to be 100 percent effective in stripping cerium (IV). Several precipitants were effective in recovering the cerium from the strip solution, and ethanol was especially promising. A scaled-up investigation was made into the use of spray-tower type equipment to perform the function of extracting, washing, and stripping. This equipment, referred to as the pressure-bubbler, utilized the system developed on the separatory-funnel scale. Feed solutions were prepared from a bastnasite concentrate by two techniques. Of these, the sulfated bastnasite solution was most successful, resulting in 86-percent recovery of the cerium at 99.7+-percent purity.

Jan 1, 1959

By William J. Campbell

These investigations were undertaken as part of a program to determine the optimum X-ray spectral lines to use for analyzing the wide variety of samples received by the X-ray Laboratory. Theoretical calculations and experimental data derived from these investigations show that longer wavelength spectral lines, > 2A, are very useful for many analytical problems. Because of the low fluorescence yield of the elements of atomic numbers 13-22 and the small depth of penetration of their X-ray spectral lines, these elements were originally considered to be insensitive; however, these studies show that the wide dispersion of their spectral lines, coupled with their weak beta lines, permits the use of wide collimation, thus increasing the line intensity. More importantly, the background due to scattered primary radiation is very low in the long-wavelength region.

Jan 1, 1959

By V. A. Nieberlein

Problems of design involving the high-temperature characteristics of materials of construction have focused attention on tungsten, the metal with the highest melting point. To study the properties of this metal a method was needed to produce tungsten of high purity easily and consistently. The Bureau of Mines has made tungsten metal in massive form on a laboratory scale by hydrogen reduction of tungsten hexafluoride (WF6). Metal made in this manner had a purity of 99.99 percent or better, with reference to all detectable impurities, including gases. The process tolerated a wide variation in operating conditions, and the results with respect to total impurities as low as 0.01 percent were reproducible.

Jan 1, 1959

By A. C. Rice

This report describes a chemical process for preparing solutions of trivalent rare-earth chlorides from sulfate solutions obtained by treating bastnasite concentrate. The chief impurity in the final solution is cerium, and this element is less than 1 percent of the rare-earth oxides. The solution is used directly in the separation of rare-earth elements by ion-exchange methods. The attractive features of the process are that the chemicals are inexpensive and the steps few. The process starts with precipitating the rare-earth hydroxides from sulfate solutions with caustic soda. After the hydroxides are dried to oxidize the cerium, they are treated with dilute hydrochloric acid to dissolve away the trivalent rare-earth elements, leaving the tetravalent cerium. Details for controlling the leaching step are described. The process shortens older procedures by omitting the usual oxalate or double-sulfate-precipitation step.

Jan 1, 1959

By Foster Fraas

Almost all minerals show irreversible changes in electrical conductivity after heating in the temperature range 100° to 800° C. This effect can be detected with only a limited number of minerals with the standard ionizing-electrode-type separator, which differentiates between nonconductors and conductors in the single-particle resistivity range of 1011 to 1013 ohms. Tests outside this range with other type separators, such as the static field type, increase the number of minerals with which the effect can be detected to almost all that were tested. Irreversibility may be the result of an alteration of adsorption layers, volatilization of surface cations or anions, or an oxidation or reduction. One example is limonite, which decomposes to hematite and passes through two minima and two maxima in conductivity in the temperature range 100° to 900° C.

Jan 1, 1959

By F. P. Haver

The purpose of this investigation was to determine the effect of common impurities, that is, oxygen, nitrogen, carbon, and iron, on the Brinell hardness of electrolytic titanium. On a weight basis, nitrogen had the greatest hardening effect, followed by oxygen, carbon, and iron in order. The hardening effects of oxygen and carbon were almost identical up to a concentration of approximately 0.1 percent by weight. Above this concentration, the relative hardening effect of carbon decreased rapidly, possibly because of its limited solid solubility in a-titanium. Hardness vs. composition curves for both oxygen and nitrogen were essentially straight lines over the range of Brinell hardness numbers (B.h.n.) covered in the investigation. The hardness of titanium was also determined as a function of the percentage of impurity atoms. On this basis, iron in concentrations up to 0.17 atomic percent had a greater hardening effect than either oxygen or carbon. INTRODUCTION Determination of the as-cast hardness of arc-melted titanium is a method of quality control widely used in industry. Numerous studies4/ have been made of the effect of impurities on the hardness obtained by this method. However, most of them have been based on the use of either iodide titanium or commercially pure Kroll sponge (B.h.n. >90), as a starting material.

Jan 1, 1959

By Eldon C. Pattee

THE BUREAU OF MINES began an investigation of tungsten resources of Montana in September 1953. This report presents information obtained from July 1955 to September 1957 on tungsten deposits in and near the Mount Torrey batholith. The batholith comprises part of the Pioneer Mountains of Beaverhead County in the southwest corner of Montana. Included in the report are assays and preliminary-examination data on 22 properties. Tungsten minerals are known to occur in 19 of the properties. The major producer is the Brown's Lake mine which has produced more than 625,000 tons of ore. Nearly all of the deposits are in the Lost Creek, Utopia, and Bald Mountain mining districts along the east and south margins of the Pioneer Mountains. The districts are less than 27 miles from Dillon, Mont.

Jan 1, 1960

By Joel N. Van Sant

THIS REPORT describes the occurrence, mining, and use of refractory clay in Colorado within Region III of the Federal Bureau of Mines, which includes the States of North arid South Dakota, Nebraska, Wyoming, Colorado, Utah, New Mexico, and Arizona. Field work by the Bureau of Mines, United States Department of the Interior, included examination of active and abandoned refractory-clay mines as well as a reconnaissance survey and sampling of numerous clay-bearing formations exposed in Colorado. Information from the survey and the sampling will help guide private industry in its search for virgin sources of refractory clay. Library research of published and unpublished reports from various Federal, State, and private sources was conducted during the early phase of the investigation. Most of the refractory clay mined in the Denver-Golden district of Colorado is not used for refractory purposes but is blended with other clays in the manufacture of structural clay products. The predominantly flint-clay de-posits in the Pueblo and Fremont County districts are mined and utilized chiefly in fabricating refractory products.

Jan 1, 1959

By E. D. Calvert

Molybdenum has been successfully cast into static and rotating molds in conventional equipment used for casting titanium and zirconium. Melting was accomplished by using an arc potential of 36 to 40 volts with a current of 10,000 amperes. Pouring efficiency, after a skull had been formed in the crucible, averaged 70 percent. Techniques are described by which four successful castings were made. Tensile properties on specimens cut from one centrifugally cast tube averaged: Tensile strength, 39,800 p.s.i.; yield strength (0.1 pct. offset), 35,300 p.s.i.; elongation, nil; reduction in area, nil; impact strength, 2 ft.-lb.; hardness DPH (diamond pyramid hardness) 180. Mold reaction was not evident in shapes cast in machined graphite. This was not true, however, for rammed graphitic-base molds.

Jan 1, 1960

By Sabri Ergun

The method of constant compositions involves the determination of the time required for the attainment of a given conversion at various temperatures. Heretofore, it has been used in evaluating the energy of activation only. A development of the method, made in the present study, makes possible the evaluation of the functional dependence upon composition and the frequency factor in addition to the energy of activation. INTRODUCTION Kinetics of reactions are best analyzed in the light of the mechanism, energy requirements, and forces involved in the reaction. Such physico-chemical information is not often available in solid state phase transformations. The reaction rates are followed by changes in a physical property during the course of the reaction, and repeating the experiment at different temperatures permits the determination of activation energy only. The possibility of a complete kinetic analysis by such a purely "phenomenological" approach has been questioned.4/ In this report a method is developed making possible the evaluation of the functional dependence upon composition and frequency factor in addition to the energy of activation. The application of the method to a study of solid state order-disorder changes is demonstrated.

Jan 1, 1960

By R. V. Higgins

As part of a study of application of the Buckley-Leverett method to an analysis of oil-reservoir performance covering a wide range of relative permeabilities and oil saturations, a method has been devised for quickly deter-mining average water saturation at breakthrough from relative permeability data. The base for the relative permeability used in the report is either the permeability to air or the effective permeability to oil at the irreducible water saturation. The permeability to air also was used because of the large backlog of air permeabilities available to reservoir engineers. The basic data were calculated by an electronic computer and are presented in a single graph from which the point of breakthrough may be obtained. In this study the water saturation at the beginning of the depletion is the connate or interstitial or irreducible water saturation. These water saturations are considered to be synonymous and to have a practical value.

Jan 1, 1960

By J. H. Holden

The Federal Bureau of Mines is doing research and development work on a pressure-gasification pilot plant for producing synthesis gas directly from pulverized coal, oxygen, and steam. A pressure-gasification pilot plant has been constructed, and an investigation was made with the following basic objectives: 1. Determining the effect of varying pressure (75, 100, 150, and 300 p.s.i.g.), coal rate (400, 700, and 1,000 pounds per hour), and oxygen-to-coal ratio (8 to 11 std, c,f. per pound), on percentage of carbon gasified, oxygen and coal requirements per unit of CO + H2 produced, exit-gas temperature, and heat loss. The steam-to-coal ratio was maintained at approximately 0.3 pound per pound. 2. Development of a stabilized gasification zone or reaction space. 3. Improvement in operability of the pilot plant.

Jan 1, 1960

By C. M. Frost

Two Federal Bureau of Mines recycle hydrogenation experiments to prepare catalytic cracking feed stock were made at 3,000 pounds pressure with crude shale oil retorted from Green River (Colo.) shale in the gas-combustion retort. The hydrogenated product from the first experiment, made at 784° F., was used for investigating the effects of nitrogen content on catalytic cracking yields and for determining the quality of the catalytically cracked gasoline. Hydrogenated product containing 0.14 percent or more of nitrogen produced less gasoline when cracked in a CAT "A" unit than was obtained from East Texas light gas oil cracked at the same conditions; product containing 0.10 percent or less nitrogen produced a quantity of cracked gasoline equal to that obtained from the East Texas light gas oil. The catalytically cracked gasoline had research octane numbers calculated to be approximately 95 clear and 103 with 3 ml. of tetraethyl lead. The principal product from the second experiment, made at 828° F., was a low nitrogen content gas oil which was used for investigating the yields of cracked products obtained when it was catalytically cracked to different degrees of conversion. Yields of cracked products, when plotted as functions of conversion, were essentially the same, within the experimental range of the data, as published yields from catalytic cracking of East Texas heavy gas oil; however, yields from cracking the shale-oil product did not display the sensitivity to change of cracking temperature that has been found for East Texas gas oil.

Jan 1, 1960

By W. L. Hunter

This report describes results of beneficiation and smelting studies conducted by the Federal Bureau of Mines on chromite samples from the Emma Belle and Seiad Creek prospects in the Seiad Creek area, northern California. Samples were chosen from this area because the ore is typical of disseminated types that represent a sizable domestic reserve. The two samples were similar in composition, and both responded in like manner to gravity beneficiation. As the ore was banded, considerable coarse gangue was rejected in laboratory sink-float from a minus-3/4-inch, plus-6-mesh fraction without excessive chromium loss at a medium density of 3.32. An average of 85.6 percent of the chromium was recovered in the sink product, which analyzed 35 percent chromic oxide (Cr203). Tabling yielded concentrates containing 49 percent or more Cr203; however, recoveries, ranged from only 33 to 45 percent. A combination of tabling and electrostatic separation of the table middlings showed that the chromium recovery could be increased to about 73 percent; the composite concentrate averaged 53 percent Cr203.

Jan 1, 1960

By J. W. Eckerd

The crushing of chestnut-size (1-5/8 by 13/16 inch) Pennsylvania anthracite in four commercial crushers (impact) jaw) hammer-mill) and gyratory types) was studied by the Bureau of Mines to determine which could produce the largest proportions of buckwheat Nos. 1 and 2 sizes (9/16 by 3/16 inch). Single pass dry and wet crushing techniques and the effect of stage crushing were evaluated. Calculations were made to show the effect of closed-circuit reduction on production rates and yield of the various sizes. The data show that the gyratory crushers produced the greatest percentage of the desired sizes. A ring-type hammer mill produced the greatest tonnage of buckwheat No.1 and rice (14.9 tons per hr.) during dry grinding tests) but the yield of these sizes was only about 55 percent) as compared with 62 to 70 percent for the gyratory crushers. The impact and jaw crushers produced the smallest amount of buckwheat and rice and the largest quantity of oversize material.

Jan 1, 1960