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By J. V. Batty

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

Jan 1, 1962

Jan 1, 1962

By W. W. Agey

The Bureau of Mines examined and tested the rhodonite deposits of the Silverton lead-zinc district, San Juan County, Colo., as a possible source of domestic manganese. Exploration and development work by several mining companies and preliminary reconnaissance of the area by Bureau of Mines engineers indicated the presence of extensive manganese resources in the form of rhodonite. This report summarizes the results of laboratory beneficiation tests made on samples of different type and grade material obtained from surface and underground exposures of seven veins in the district. Surface and underground examinations revealed the presence of several prominent veins that could be traced up to 2 miles for a single vein along the surface. The principal veins average about 50 feet in width and apparently carry rhodonite to considerable depth. Underground samples were taken from the Sunnyside, Silver Queen, Washington, Independence, and Scotia veins. Samples also were taken from surface exposures of the Sunnyside Extension and Hidden Treasure veins.

Jan 1, 1962

By G. E. Johnson

A bench-scale study was made of removing hydrogen sulfide from synthesis gas at elevated pressure by iron oxide impregnated on wood chips. The gas contained 0.02 to 0.06 percent oxygen. The removal of hydrogen sulfide by iron oxide impregnated on wood chips is more efficient at elevated pressure. At constant space velocity, longer periods of operation at 400 p.s.i.g. are possible before the exit gas reaches a given maximum concentration of hydrogen sulfide, compared with 200 p.s.i.g. or atmospheric pressure. In tests at room temperature, 60° C., and 100° C., the most effective removal of hydrogen sulfide was obtained at room temperature and the least effective at 100° C. Dry impregnated wood chips removed only about half as much hydrogen sulfide as chips wetted to a water content of 50 percent.

Jan 1, 1962

By Murray Jacobson

Facts obtained by the Bureau of Mines on the dust-explosion hazard in air of materials used in the plastics industry are presented for 313 samples studied in the laboratory. Information is given on ignition temperature of dust clouds and layers, minimum explosive concentration, minimum energy required for ignition, explosion pressure and rates of pressure rise, amount of inert dust required to prevent ignition and flame propagation, and, in some instances, on the limiting oxygen concentration in an atmosphere to prevent ignition by spark and by heated surface. The effects of particle shape, additives, and resin structure on explosibility are discussed. Relative explosibility of the materials is related to the ignition sensitivity and explosion severity and is denoted by an empirical index. Recognition of the degree of hazard will facilitate adoption of adequate measures for preventing ignition and explosion during manufacturing or processing.

Jan 1, 1962

By W. J. Boone

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

Jan 1, 1962

By J. P. Capp

The Bureau of Mines conducted field-scale experiments in underground gasification of coal with oxygen-enriched air. A path about 140 feet long was linked at the rate of LO feet per day through a coalbed hydraulically fractured with a mixture of starch gel and sand. During the best gasification period, which extended for 2-1/2 days, 785,000 std. c.f. per day of 124-B.t.u. gas was produced. In other periods the heating value at times was almost 300 B.t.u. per std, c.f,, but sustained production of such gas was not achieved. During gasification, a total of 50 tons of coal was gasified and 114 tons of coal was carbonized. Approximately 12 million B, t .u. per foot of nominal path was recovered at the surface.

Jan 1, 1962

By Frank B. Fulkerson

Of the about 60 million pounds of aluminum used in the Pacific Northwest in 1960, 40 million pounds or two-thirds was used by 10 companies. One of these companies made airplanes and missiles; one manufactured roofing, siding, and tubing; three produced truck tractors, truck bodies, or truck trailers; two made architectural metal products; one made irrigation and industrial products; one was a general foundry; and one was a shipyard. These companies contributed to regional growth by developing markets outside the area; some have worldwide sales. Aluminum consumption increased at an average rate of 7 percent annually from 1954 to 1960. Airplane manufacture, formerly preeminent in aluminum use, no longer was in first place in 1960. By industrial group, the leading users were manufacturers of building products, 30 percent; airplanes and missiles, 22 percent; truck tractors, truck bodies, and truck trailers; 17 percent; general foundries, 5 percent; ships and boats, 4 percent; mobile homes, 4 percent; other transportation equipment, 3 percent; and irrigation equipment and all other products, 15 percent.

Jan 1, 1962

By Edwin E. Maust

In response to the ever- increasing demand for high temperature materials, the Bureau of Mines instituted a program for the study and development of superrefractories, One of the major tools obtained for use in this research was an image furnace of the double-paraboloidal mirror type. Although extensive theoretical analyses of solar furnace performance may be found in the literature, comparable detailed information on the double-paraboloidal-mirror image furnace has been nonexistent. This report presents an analysis based on an investigation undertaken to ascertain the limitations and characteristics of the furnace so that it can be used most effectively. The quantitative determination of the energy available at the image, the control of this energy by mans of a 60-inch iris diaphragm, and its variation with position and time relative to the heat source used have all been dealt with in detail. The quantitative results were obtained using a specially designed waterflow calorimeter and these measurements, in conjunction with the theoretical analysis, are used to present a fairly complete description of the furnace and its capabilities.

Jan 1, 1962

By G. W. Brock

Experiments in the form of aging of overstrained tension specimens and elevated temperature tension testing, have been carried out on recrystallized arc-cast molybdenum. The aging behavior of molybdenum was found to be strongly dependent on the degree of plastic strain present in the lattice: the reason for this being the low solid solubility for the common interstitial elements in molybdenum. GEORGE W. BROCK, formerly Research Associate, Department of Theoretical and Applied Mechanics, University of Illinois, Urbana, III., is Research Associate, Department of Engineering Sciences, IBM Research Center, Yorktown Heights, N. Y. Manuscript submitted January 19, 1961. IMD THE term strain aging is familiar in connection with the recovery of the yield point in mild steel after tensile overstraining, and there are other instances where it is known to exert an appreciable effect on mechanical properties. For example, steel exhibits a greater tensile strength at mildly elevated temperatures than at room temperature and serrated stress-strain flow curves occur under certain conditions. It has been known for a number of years that the phenomenon of strain aging is directly connected with the presence of carbon and nitrogen in the lattice; and extremely small amounts of either element are sufficient to produce the effect. In this study, the aging behavior of overstrained tensile specimens of recrystallized molybdenum has

Jan 1, 1962

By Richard F. Hewlett

Engineers at the Bureau of Mines Denver Mining Research Center have been a research program investigating the theory and application of mine sampling. Part of this program is an investigation of the efficiency of sampling methods that involves development of sampling-method theory through simulating ore-deposit samples and assays, using - electronic digital computer. Theoretical developments are checked against actual ore-deposit sampling, assay, and production data by the commonly used polygonal and triangular methods of computing grade and tonnage of ore reserves. To speed the computing procedures, a program has been developed utilizing a medium-size digital computer for computing ore reserves by the polygonal method. This program calculates nine prismoids per minute at a total cost of $0.21 per prismoid. The complete program, written for an augmented IBM 650 computer, is described in detail; it can be used without change for computing ore reserves for a low-grade deposit. Modifications necessary to convert the program to compute ore reserves for virtually any other type of deposit or grouping of ore horizons also are given; however, the program is limited to using only vertical drill-hole data.

Jan 1, 1962

By R. Ward Stahl

Fire is still a scourge of the mining industry, although many precautionary measures have been and are being taken to reduce the incidence of fires and to combat them. Generally, the success of fire extinguishment is directly proportional to the speed of attack, and the speed of attack in turn is dependent upon the availability of materials and trained personnel. Preparations for firefighting are frequently neglected because they are considered emergency needs and do not contribute directly to coal production. Fire incites panic--a fact often overlooked--but such chaos can be minimized by training people in the use of equipment and procedures. Heat, smoke, and fumes hamper the approach to a fire; however, a relatively new technique of attacking fires with high-expansion foam may well contribute greatly to firefighting. The foam is transported to a fire and used at a considerable distance, thus permitting the firefighters to work more safely.

Jan 1, 1962

By K. E. Tame

The Bureau of Mines is studying possible modifications in conventional uranium ore-processing steps to confine and permit controlled disposal of radioactive wastes. A potential method of minimizing pollution from radio-active nuclides, principally radium 226, in uranium mill waste streams is to reuse the waste solutions within the mill. Such reuse of waste solution in the Kerr-McGee Shiprock-type process was investigated in the laboratory. The Shiprock mill employs a two-stage acid-leaching process for dissolution of the uranium, countercurrent decantation for liquid-solid separation and washing, and organophosphorus solvent extraction for recovery of the uranium and vanadium from solution. The simulated use of barren raffinate instead of fresh water in the mill circuit was carried through a laboratory campaign of 28 interlocked leaching, washing, and solvent extraction cycles. About 99 percent of the uranium and 91 percent of the vanadium were dissolved from the are, Washing efficiency in the thickener circuit averaged about 99.5 percent when the pulp was washed with enough barren raffinate and makeup water to recover 2.5 tons of pregnant solution per ton of ore. The only solution discarded was that contained in the washed and thickened leach residue. A buildup of salts due to recycling of solutions did not adversely affect operation of the washing circuit.

Jan 1, 1962

By H. P. LeVan

The aced for reliable reserves of the essential element, manganese, has been a continuing concern of the Federal Government for more than three decades. Because of the increasing vulnerability of outside sources of supply efforts have been intensified to find a means for beneficiating United States domestic deposits. The deposits of most interest would of necessity be near, or have access to, suitable transportation to processing plants. The Georgia manganiferous iron deposits represent some 10 million tons4 of ore readily available to southern iron and steel industries, if a manganese recovery process capable of functioning in the presence of large quantities of iron can be developed. In addition, a successful method for beneficiating the Georgia ore could produce a significant quantity of high-grade iron concentrate. The Differential sulfatization process developed 47 the Bureau of Mines5 seemed to be well suited for this application, particularly because it results in low concentrations of iron in the leach liquors with relatively complete extractions of manganese. In this process, manganese in the presence of iron is preferentially reacted with sulfur dioxide at elevated temperatures and subsequently extracted with water.

Jan 1, 1962

By Fred A. Williams

The cause of many deaths and extensive property damage in coal mines resulting from explosions and mine fires has been directly attributable to electric cable failures (including splice failures). The Federal Bureau of Mines data show that out of 355 underground coal mine fires investigated from July 1952 to January 1960, 103 (29 percent) were directly related to trailing cables. These cable failures resulted in the death of 7 men and injuries to 37 others. These potential hazards have become greater, obviously, through the widespread adoption of mechanized mining methods with electric-driven machinery powered through trailing cables according to Young,4 68.1 percent of the total bituminous and lignite production of the United States was mined underground in 1959. About 85 percent of this production was attained by mechanized loading methods. A large majority of the mines using the hand- loading methods also used equipment with trailing cables such as cutting machines, drills, and gathering locomotives. The problem of minimizing the loss of life, resources, and equipment from cable failures should be of concern to the management of all coal mines. It would be misleading to imply that no consideration has been given to the problem and its associated hazards. Through research cable manufacturers have endeavored to develop trailing cables that will withstand the severe service imposed by underground mining conditions. Technical research groups have undertaken studies for determining improved procedure and materials for field splices. Coal companies have instituted cable maintenance programs with a view toward the reduction of cable failures and consequent improvement in safety and efficiency of operations. Safety agencies are alert to unsatisfactory cable handling practices, poor workmanship in field splicing, mechanical

Jan 1, 1962

By R. J. Stokes

S. Floreen (international Nickel Co.)— One fairly simple way to differentiate between em brittle me nt due to surface microcracks or due to a dislocation barrier effect might be to load a brittle rock salt crystal in tension to some stress just below the fracture stress and then immerse the loaded crystal in water. If a surface film is retarding plastic flow then one should observe some plastic deformation of the rock salt as

Jan 1, 1962

By L. B. Pankratz

Present-day interest in the rare-earth elements and their compounds, for both metallurgical and ceramic uses, makes it highly desirable to accumulate basic thermodynamic data that can be applied to theoretical considerations of the processing of these substances. Such data still are seriously lacking. This Bureau of Mines paper reports the results of high-temperature heat content measurements of the sesquioxides of four rare-earth elements--europium, gadolinium, neodymium, and samarium--and of the closely related element, yttrium. The temperature ranges covered by the measurements are as follows: Monoclinic Eu2O3, 298°-1,802° K. Cubic Eu203, 298°-1,350° K. Monoclinic Gd203, 298-1,802° K. Cubic Gd203, 298°-1,550° K. Hexagonal Nd203, 298°-1,795° K. Monoclinic Sm203 298°-1,798° K. Cubic Sm203, 298°-1,149° K. Cubic Y203, 298°-1,799° K.

Jan 1, 1962

By Philip E. Niebuhr

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

Jan 1, 1962

By A. H. Daane, R. L. Myklebust

The yttrium-manganese system has been investigated by thermal, metallographic, and X-ray diffraction methods. There are three intermetallic compounds present: YMn2 which melts congruently, YMn4, which undergoes syntectic decomposition, and YMn,, which undergoes peritectic decomposition. The compound YMn4 is ferromagnetic at room temperature with a Curie temperature of 214°C. There are eutectics at 25.2, 60.9, and 82.0 wt pct Mn which melt at 878°, 1100°, and 1075°C, respectively. Crys-tallographic data are given for YMn4, and YMn12 . The terminal solid solubilities are low. In a general program of study of yttrium metal in this laboratory some alloy systems of this metal with elements of the first transition period have been examined. This work was originally instigated by experiences in cladding yttrium with jackets of some protective metals such as Inconel for high-temperature service in air.' In some cases a low-melting phase was observed to form between the Inconel and the yttrium resulting in failure of the samples. In characterizing this reaction, a survey was made of the systems of yttrium with chromium, manganese, iron and nickel,, and it was found that a eutectic was formed between these metals and yttrium on the yttrium-rich side of the system. This present study of the Y-Mn system was carried out to examine in more detail the alloying nature of yttrium, and to correlate trends that have been observed in previous related studies. It was observed by Voge13 that in the systems of lanthanum, cerium, and praseodymium with each of the metals in the first transition series, the tendency to form compounds diminished in the order nickel, cobalt, and iron while no compounds were formed with manganese, chromium, or titanium. Beaudry and Daane4 observed a similar behavior in the systems of yttrium with some members of the first transition series except that the tendency for compound formation was greater. Both the Y-Ti5 and Y-Cra systems consist of simple eutectics, while in the Y-Fe,7 Y-CO, and Y-Ni4 systems, there are four, eight, and nine compounds, respectively. In addition to the above trends, the similar atomic radii and electronegativities of yttrium and thorium invite a comparison between their alloying behaviors with a common element such as manganese. In crys- tallographic studies, Florio et al.' have identified three intermediate phases in this system which are ThMn2, Th6Mn23, and ThMn,,. Gschneidner and Waber10 have examined published information on alloy systems of the rare-earth metals and have correlated this information with current alloying theory. From their study, they predicted that the Y-Mn system would contain one intermetallic compound. On the basis of this prediction, the trend in the alloying behavior of yttrium with the elements of the first transition series and the alloying behavior of thorium with manganese, one might expect from one to three intermetallic compounds to form in the Y-Mn system. A consideration of Hume-Rothery's rules of alloying based on size-factor, electronegativity, and valency suggested a small terminal solubility and possible compound formation. The present study was undertaken to confirm these predictions of low terminal solid solubility and compound formation and to establish the general alloying behavior of yttrium with manganese. EXPERIMENTAL Materials. The manganese used in this investigation was obtained from the Foote Mineral Co. as electrolytic plates of 99.9 pct stated purity; the yttrium metal was prepared in this laboratory. Table I gives the analyses of these materials. For the solubility studies at the yttrium-rich end of the alloy system, distilled yttrium, whose major impurity was 200 ppm Ti, was used. Preparation of Alloys. The alloys were formed by comelting the two metals in an are-melting furnace under an atmosphere of argon. The buttons thus formed were inverted and remelted three to five times to promote homogeneity. Due to the high vapor pressure of manganese, it was assumed that the weight lost during are-melting was all manganese. This assumption was based on the very good agreement observed between calculated compositions and chemical analyses of several alloys. The compositions of the dilute alloys used for solid solu-

Jan 1, 1962

By A. R. Taylor

In recent years, thermodynamic data have been used to a greater degree than ever by the chemical and metallurgical engineer as a means of predicting and controlling chemical reactions. To satisfy the spiraling demand for basic physical data needed for the calculations, the Bureau of Mines is studying the heat capacities of a variety of chemical compounds at high and low temperatures. This paper is one of a series presenting such data. The heat capacities of two alkaline earth compounds, strontium bromide and strontium nitrate, were measured in a temperature range of 60° to 300° K. in an adiabatic calorimeter and at temperatures of 300° to about 1,200° K. in a Bunsen ice calorimeter. The construction and operation of the calorimeters are discussed in other reports.3 4 The heat-capacity data presented in this report were extrapolated to 0° K., and smooth values of heat capacity, entropy, enthalpy function, and free-energy function were calculated and tabulated at even 10-degree intervals. The enthalpy data were fitted with algebraic equations by applying the method of least squares; calculations a£ heat-capacity values, entropy, enthalpy function, and free-energy function were made at even 50-degree intervals. The heat and entropy of fusion of strontium bromide were calculated from the enthalpy measurements.

Jan 1, 1962