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By E. G. King

Many of the rare-earth oxides are now commercially available in pure form and they have a variety of potential technical uses. Thermodynamic data for these oxides, however, are rather sparse. It is one of the functions of the Bureau of Mines to fill the need for this type of information. This report gives the results of low-temperature heat-capacity and high-temperature heat-content measurements by the Bureau of Mines of lanthanum sesquioxide. The entropy at 298.15° K. was evaluated and heat-content and entropy increments above 298.15° K. were obtained to 1,800° K. The results were combined with the known heat of formation at 298.15° K. to derive heats and free energies of formation at higher temperatures. Sufficient information is now available to permit reliable thermodynamic calculations involving lanthanum sesquioxide within the temperature range 298° to 2,000° K.

Jan 1, 1961

By J. G. Croeni

The high thermal-neutron cross section of gadolinium and the good mechanical and corrosion properties of titanium suggest that alloys of these two metals might be useful as control rod material. To aid in establishing the feasibility of this combination, the Federal Bureau of Mines investigated the titanium-gadolinium system. The results indicate that the system is composed of a single eutectic reaction and a peritectoid reaction involving the alpha-beta transformation of titanium. The eutectic isotherm extends from 1 to 99 pct, gadolinium at 1,240° C. The established eutectic composition is about 95 pct, gadolinium. The peritectoid reaction occurs at 885° C. and extends almost over the entire composition range. Hardness increases slightly with additions of gadolinium, and little change is obtained by heat treatment. Alloys containing less than 10 pct. gadolinium are amenable to extensive cold-working, but alloys having higher percentage of gadolinium content are only moderately cold-workable. All alloys can be hot-worked in iron sheathing at 750° C. Observation indicates that all compositions possess good machinability. Corrosion resistance to water at room temperature is apparently poor, especially in the gadolinium-rich alloys. INTRODUCTION A combination of the good mechanical and corrosion properties of titanium and the variety of thermal-neutron cross sections characteristic of the rare-earth metals suggests that alloys of these metals may be used for control rod materials. For this reason the Bureau of Mines proposed a study of the titanium-gadolinium alloy system, and the Atomic Energy Commission sponsored the investigation.

Jan 1, 1961

By R. D. Pehke, J. F. Elliott

The solubility of nitrogen in liquid pure iron has been measured as a function of pressure and temperature. Sieverts' Law is obeyed at all pressures up to 1 atm and the temperature coefficient of solubility is 8 x 106 %/°C. The solubility of nitrogen in liquid iron alloys has been studied by the Sieverts' method and by the sampling method. The solubility is decreased by Al, C, Co Cu, Ni, 0. Si atzd Sn, and it is increased by Cr, Cb, Mn, Mo, Ta, W, and V. Interaction coefficients eN, for the effect of these elements on nitrogen dissolved in liquid iron, are reported. 1 HE effect of nitrogen upon the properties of steel may be desirable or not, depending upon the composition, processing treatment, and the use of the product. To understand the behavior of nitrogen in the various steelmaking processes, it is necessary to have reliable fundamental data pertaining to the solubilities, rates of solution, and chemical reactions of nitrogen in steel, particularly in the liquid state. In an effort to extend our knowledge in these areas, an investigation of the thermodynamics and kinetics of the solubility of nitrogen in liquid iron alloys was undertaken. The thermodynamic aspects of the study are presented in this paper. The solubility of nitrogen in liquid pure iron has received the attention of several investigators whose results are summarized in Table I. Reasonable agreement among the more recent researches1-l8 is found for the solubility of approximately 0.044 wt pct at 1600°C and 1-atm pressure of N,, for the temperature coefficient of solubility being small but positive, and for adherence to Sieverts' law for pressures up to 1 atm. The solubility of nitrogen in a number of binary liquid iron alloys has been studied: Fe-A1,3 Fe-As,16 Fe-C,3, 71 18, 19, 20 Fe-Cr ,5,7, 10, 11, 15 21 Fe-Co,'4, '6 Fe-Cu,'6 Fe-Mn,10, 11, 18 Fe-Mo,13, 16 Fe-Ni,10, 11, 13, 15, 16 Fe-O,16, 17, l9 Fe-p,7 Fe-S,l6 Fe-Sb,16 Fe-Se,lg Fe-Si,4) 97 '77 187 19>2° Fe-Sn,16 and Fe-v.51 '3 A few ternary systems have been studied, most of which were reviewed by ~angenberg" who applied the methods suggested by WagnerPz3 Chipman,24 Darken and G~rry, and Morris and Buehl26 for predicting solubilities in multicomponent alloys. Langenberg22 and Humbert and Elliott15 compared the solubilities computed from simple binary alloy systems with experimental measurements of nitrogen solubilities in liquid iron containing two or more alloying elements. The interaction coefficients for nitrogen in

Jan 1, 1961

By E. J. Pasierb, H. W. Paxton

Mavkers ill a diffusion couple in the iron-chromium system move towards the high chromium side indicating Dcr > DFe at the marker composition. By a combituztion of measurements of D& and D a: a function of composition, this is also shown independently. DFe is calculated as a function of composition. and shown to be in reasonable agreement with measured values by other workers. MEASUREMENTS of marker movements in diffusion couples have been used from time to time to demonstrate that a vacancy or interstitial mechanism may be operative. Since there is a possibility that ring diffusion1 may be operative in chromium, the present experiments are of interest in showing some non-ring mechanism in iron-chromium alloys around the equiatomic composition. EXPERIMENTAL PROCEDURE The movement of markers originally at the interface between 1-in. sq sections of pure Cr (6 mm thick) and outer slabs of 30 Cr-70 Fe alloy was followed as a function of time at temperatures from 1150" to 1425"C, in a Kanthal-wound furnace. Temperature control was +5°C over extended periods. The analyses of these alloys are given in Table I. Selection of suitable markers presented a considerable experimental problem; the eventual solution was to draw quartz rod down to 0.01 cm and seat this in V-grooves 0.01 cm deep on each side of the chromium prior to welding. A preliminary experiment in which the groove was machined in the alloy gave identical results. Welding was accomplished by passing a heavy current through specimens under moderate pressure in a helium atmosphere. This method produced good welds with a planar interface as shown by subsequent metallo-graphic investigation. Any markers which did not adequately fill their groove and showed subsequent contamination from the atmosphere during heat treatment were not considered reliable. The composite sample was ground and metal-lographically polished on the four sides perpendicular to the interface. Fiducial marks (deep milled slots) were made outside the diffusion zone to check on total volume change. All necessary measurements were made on a metallograph reading to +0.0005 cm. The samples were wrapped in tantalum foil and given diffusion anneals for times to 200 hr in carefully purified dry hydrogen in a sealed McDanel porcelain tube. Chromium-zirconium chips were introduced near the specimen as an additional getter. The specimens were cooled relatively slowly after the diffusion anneal to preserve the McDanel tube but no significant error in effective time at temperature was thereby introduced. At least 1 mm was ground off the surface before measurements were taken. It was observed that the grain size following short diffusion anneals was several mm and was appreciably larger in the 30 Cr alloy than in the pure Cr. No significant grain boundary penetration was present as indicated by the etch limit. The results are presented in the next section. Measurements of D were made by standard sectioning techniques with chemical analysis. Machining difficulties limited the

Jan 1, 1961

By R. L. Bailey

"The Acheson D-3 Pool was discovered in August 1950, and contains 88 producing oil wells on 40 acre spacing. Initial oil-in-place was 118 million stock tank barrels and initial well potentials averaged 2,000 barrels per day.In early 1956 studies of hydraulic interference between the Acheson and Leduc D-3 Pools were conducted on the Carter Petroleum Reservoir Analyzer. These studies indicated that the natural water drive to Acheson would be incapable of replacing reasonable withdrawal rates over the life of the pool. To avoid shrinkage losses a scheme of pressure maintenance by water• injection was therefore instituted in March 1957.This pressure maintenance scheme is notable because pressure is being effectively maintained by high volume injection through one well located on the flank of the pool. Close control on reservoir behaviour is maintained by regular bottom-hole pres-sure surveys and observation of water cuts on producing wells. No evidence of pressure gradients or channelling of the injected water has been observed to date, and the water-oil contact has remained level over the whole field. It is possible to control the average reservoir pressure within very close limits by varying the rate of fresh water injection.Ultimate recovery estimated from the rise of the oil-water contact and calculated water influx to December 31, 1958, is 335 barrels per acre foot, or a total of 91.4 million barrels from the pool. This compares to 217 barrels Per acre foot or a total of 59.4 million barrels indicated from laboratory test data."

Jan 1, 1961

By W. J. Verner, J. R. Lucas

Billions of tons of bulk solid materials are processed through our industrial plants each year, and the tonnage is steadily rising. It has been estimated that for every dollar spent in industry as a whole, approxinlately 30 cents is consumed in the handling of bulk solid materials. It is in this category that tremendous savings are possible through the use of improved techniques. Since World War 11, the mining, steel, chemical, and grain industries, among others have made use of increased materials-handling automation in order to gain some of these savings. However, in a chain of automatic operations, every link must be completely reliable, for if there is a single failure, the whole system immediately becomes ineffective. Only too often the weak link in the chain proves to be the flow of bulk solids from bins. To contribute to the fundamental knowledge in this area, a research study has been continuing at The Ohio State University. The principal objective of the investigation has been to study the internal stresses existing in confined bulk solids. LITERATURE SURVEY Literature studies have revealed that many outstanding people have made contributions to the field of bulk solids. For instance, C. F. Jenkin,1 suggested: a. The pressure on a bin wall is not directly proportional to the depth beneath the surface of material in the bin. b. The vertical pressure distribution on the base of a bin is not actually uniform but is a variable. c. Arches form in bins as a result of very small deformations of the material in the bin. This deformation causes a series of gaps to appear, and consequently causes the disappearance of diagonal forces that cannot act across these gaps. The removal of the diagonal forces causes horizontal forces to be introduced which seem to be the chief cause of arching. 11. A. Janssen,4 in 1895 in connection with his experiments on bins, derived a differential equation to describe both the lateral and vertical pressure in bins with vertical sides. This represents a significant contribution to bulk solid theory, and thus its solution is reproduced as follows: L = KV = RW/U' [l-e -U'KY/R] I where L is the lateral pressure of the bulk solid in psf., V is the vertical pressure of the bulk solid in psf., K is the ratio of the lateral pressure to the vertical pressure at any point, R is the hydraulic radius of the bin in feet, W is the density of the bulk solid in lbs. per cubic feet, U' is the coefficient of friction between the stored material and the bin wall, and Y is the head of material above the point in question in feet. In 1903, Jamieson,6 in an elaborate series of experiments on full sized bins measured vertical and lateral pressures by hydraulic diaphragms. He determined many values for mediums of corn, wheat, peas, and flaxseed. In 1951, Caughey, Tooles, and scheer3 measured both lateral and vertical pressure in deep bins by using strain guages on steel bands. Values were calculated for cement, gravel, sand, soy beans, shelled corn

Jan 1, 1961

By L. S. Darken, H. A. Wriedt

THE constitution diagram of the iron-copper system derived by Daniloff' exhibits, at the iron-rich end, phase fields similar to those of the iron-carbon diagram. At 1484° 1094°, and 850°C there are, respectively, a 6-y-L peritectic, a y-E-Lperitectic, and a a-y-E eutectoid. The phase designated E is copper-rich, containing 4 pct Fe or less according to the temperature. The composition of copper-saturated ferrite (a-solid solution) has been determined previously only twice as a function of temperature. By electrical conductivity measurements, Buchholtz and Köster2 found 3.4 pct Cu in ferrite at a eutectoid temperature of 810°C. They represented the composition of saturated ferrite by the equation, log (%Cu) = 4.32-4125 (1/T) Gregg and Daniloff3 reported that Köster later modified his opinion, raising the indicated eutectoid temperature to 833 °C and the copper content of eutectoid ferrite to 3.7 pct. The literature contains several indications4-7 that the work of Köster and his co-workers is not reliable. Norton,8 using an X-ray method, found that 1.4 pct Cu dissolved in ferrite at the approximate eutectoid temperature of 850°C and that the solubility decreased to about 0.3 pct at 700°C. Below 700°C his experimental data show almost no change in solubility. These findings, although inconsistent with the work of Ruer and Goerens4 and of Smith and Palmer,7 have been used generally since their publication. In investigations involving the observation of arrests in temperature during continuous heating or cooling the precise location of the eutectoid temperature has been obscured by a large hysteresis. The more reliable work 579 where the results are not effected by this hysteresis indicates a eutectoid temperature between 840° and 850°C. The foregoing discrepancies, along with a few observations in this Laboratory relating to the precipitation of copper from ferrite, prompted us to rein-vestigate the lower temperature portion of the Fe-Cu system. In this investigation the solubility of copper in ferrite was obtained by the chemical analysis of high-purity iron equilibrated with copper-silver alloys. This method eliminated the necessity for retaining by a quench the physical state of the specimen existing at the equilibration temperature. EXPERIMENTAL The reaction of the iron with the copper alloy was

Jan 1, 1961

By Evan Just

?We are certain there is need for research in every phase of mining." This statement by R. M. Crump of the Jones and Laughlin Steel Company (047) paraphrases opinion widespread among mining people. It is undoubtedly true. In preparation for this presentation, 193 organizations were asked to describe their mining research efforts. 60% responded, The meaning of "research" was taken in several different ways. The continual efforts of progressive companies to improve themselves were reported as research. We will call this and any effort to solve specific and immediate problems "practical research". The continuing investigation of subjects of long range interest will be called "basic research".

Jan 1, 1961

By Marvin L. Whisman

Several parameters controlling the reproducibility of tritium determina¬tion in organic compounds by liquid scintillation counting were evaluated by the Federal Bureau of Mines. These included optimum volume of scintillator solution for maximum counting efficiency, reproducibility of counting a sealed commercial standard and comparison with duplicate counts on laboratory-prepared samples. The error introduced by using microliter pipets, optical differences in counting vials, reproducibility of counting organic samples where quenching is a factor, reproducibility of counting laboratory-prepared samples with an added internal standard, optimum ratio of internal standard activity to sample activity, effect of sample volume upon counting efficiency, count rate at which coincidence losses become apparent, and reproducibility of organic compound radioassay by the standard addition technique are outlined. From the evaluation of these parameters, a technique that can be applied routinely to organic compounds containing tritium has been established, and details are included in this report.

Jan 1, 1961

By J. S. Kirkaldy, W. J. Slater, G. R. Mason

Activation analysis for copper and manganese in 10 mg samples machined from aluminum-base diffusion couples has been used in the study of ternary diffusion in the Al-Cu-Mn system. The accuracy, economy and convenience of the method are considered to be very competitive with other methods for analysis of such small samples. Neutron-activated aluminum-zinc alloys in the range from 10 per cent to 100 per cent zinc have been equilibrated with a known volume and the vapors subsequently condensed and collected. The vapor pressures relative to pure zinc (the thermodynamic activities) have been determined at 550°C' by recording the relative count of /'-rays from zn65 in the collected samples. The method is a sensitive one, although subject to serious obstacles to experimental accuracy.

Jan 1, 1961

By R. M. Becker

THIS IS a progress report on a study of the application of statistical practice to mine and mineral sampling undertaken by the Federal Bureau of Mines to provide sound theoretical and practical data for use of the mineral engineering professions. One of the problems in mine sampling is determining the reliability of the results. For certain types of sampling data (random data) the reliability of the results can be stated mathematically. For other types of data there is no known means of quantitatively expressing reliability. In applying measures of reliability to a set of random data, some knowledge or assumption of the characteristics of the particular data is necessary. In many fields these characteristics are well known. However, in mining, where the data are in assays, these characteristics are not well known.

Jan 1, 1961

By D. E. Redmon

The Federal Bureau of Mines has studied the locations and general features of 90 pegmatites found in north-central New Mexico. The dominant valuable product of the pegmatites is muscovite, both sheet and scrap. However, the Harding pegmatite in Taos County is mined only for beryl. Many attempts have been made to recover scrap mica on a large scale by mechanical beneficiation of pegmatite, but the operations heretofore have been short-lived. The Globe mine and the Apache mine, both near Petaca in Rio Arriba County, have been the most important sources of sheet mica in New Mexico. Recognition of the growing need for some of the minerals derived from pegmatites led the Bureau of Mines to investigate the occurrences of pegmatite.

Jan 1, 1961

By C. W. DeLong, L. L. Farnham, L. A. Stewart

This paper is one of a series covering mineral resources of the Nation . It describes briefly most of the known manganese deposits of eastern Arizona , which for the purpose of this report includes the counties of Navajo , Apache , Gila, Graham, Greenlee , Pinal , Pima , Santa Cruz , and Cochise . With few exceptions , these descriptions are the result of field examinations by the writers . Work on this paper was begun in May 1956 , and in the following 18 months 151 deposits were examined . The distribution of the deposits by counties is as follows : 1 in Navajo , and 1 in Apache , 37 in Gila , 4 in Graham, 13 in Greenlee , 25 in Pinal , 13 in Pima , 12 in Santa Cruz , and 45 in Cochise . In surveyed areas the locations of the deposits are described by section , township , and range and in unsurveyed areas , by approximate projections of these subdivisions . The township and range numbers refer to the Gila and Salt River base and meridian . The history, production, ownership , geologic setting , and mining methods used are discussed for most of the deposits that were visited . Probably , some occurrences have been overlooked , but all of the principal ones have been examined . Ore dressing studies were made of typical ores from several of the larger districts . The work was performed in the laboratory of the Bureau of Mines Tucson Metallurgy Research Laboratory . The results of these studies are given with the descriptions of the deposits from which the samples were taken .

Jan 1, 1961

By T. N. McVay

The various applications of beryllium and its compounds in atomic - energy technology and a growing recognition of possible increased utilization of the metal in the aircraft and space - missile fields have resulted in increased interest in domestic and world reserves of beryllium . Unfortunately, little dependable data on beryllium resources and reserves are available , as past consumption of the element has been small and only limited prospecting and exploration work has been done . The scarcity of resource information is attributed partly to the difficulty of recognizing beryllium minerals in the field . These minerals frequently do not have distinctive characteristics of specific gravity, color , or other physical properties , that enable ready identification by the average prospector . This is particularly true of fine - grained minerals . As a result , a simple field test for identifying beryllium- bearing rock is needed . Recognizing this , technologists of the Federal Bureau of Mines investigated several of the proposed qualitative chemical tests for beryllium . This report describes various modifications of one of these methods to make it more suitable for use in the field . In the modified method , duplicate samples are fluxed -- one with potassium bifluoride and one with potassium bisulfate -- followed by dissolution of salts in water , conversion of the solution to an alkaline condition, addition of morin , and examination of the solution for fluorescence under short -wave ultraviolet light . This method provides a fast , dependable field test for beryllium minerals containing as little as 0.2 percent beryl or its equivalent . The test involves no radiation hazards , and it can be performed by persons having no technical training ; therefore , it should be useful to prospectors in discovering beryllium mineralization .

Jul 1, 1960

By J. M. Seward, W. D. Dietzman, M. E. Hawkins

Analytical studies of formation waters are widely used by the petroleum industry as an aid in solving problems such as identifying intrusive waters , corrosion studies , treating injection water , and choosing open or closed water- injection systems . The solution of a problem is often simplified when reliable analyses of the waters under consideration have been made previously . Chemical analyses and electrical resistivity measurements are presented on 267 samples from 74 fields in south Arkansas , and 199 samples from 80 fields in north Louisiana .

Jul 1, 1960

By H. L. Gibbs

Many factors contributed to the decision to build a radiochemical laboratory at the Salt Lake City Metallurgy Research Center to investigate the application of radioactive isotopes and chemical compounds in extractive metallurgy. These reasons included the notable success achieved in biological sciences with radioisotopes, the development of reliable instruments and methods for identifying the isotopes and measuring their activities, and the commercial availability of radioisotopes in a variety of forms and known activities. The paramount reason, however, was the realization that better methods were needed for guiding and quantifying research to resolve the complex extractive metallurgy problems under study at the Research Center. This is the first of a series of reports describing the application of radioisotopes and radioactivity techniques in extractive metallurgy. The report includes a discussion of licensing and safety requirements, a general description of the laboratory and the methods used, a definition of the nature and scope of the research program, and a synopsis of the more important problems studied. Subsequent reports will concern radioactive techniques for solving specific problems in mineral dressing, hydrometallurgy, and pyrometallurgy.

Jan 1, 1960

By J. B. Gayle

The rate of oxidation of coals with nitric acid has been used by earlier investigators4 5 6/ for determining fusain and for studying petrographic composition. These workers accumulated considerable evidence indicating that, for coals ranging from lignite to low-volatile in rank, the method gives values for fusain that agree satisfactorily with those obtained by optical methods. One group5/even concluded that, when discrepancies are noted between results obtained by chemical and microscopic methods, the results based on the oxidation reaction are probably the more reliable. Unfortunately, after concluding that the method was valid, most of these workers apparently lost interest. As a result, no attempt to exploit or apply the method to problems of utilization has been reported. Recent studies of the influence of inert petrographic constituents on the properties of cokes made from various coals7/ have indicated a need for additional means of characterizing coals and blends used for carbonization.

Jan 1, 1960

By R. F. Tenney

This report has been prepared because little detailed information has been published on the production and use of anthracite producer gas for industrial-process and brick-kiln heating. To obtain this information, an investigation was conducted by the Federal Bureau of Mines in cooperation with a building-brick manufacturer (firing both periodic and tunnel kilns with anthracite producer gas) and with a manufacturer of anthracite-gas producers. In addition to a study of available plant records, 2 weeks was spent in systematic observation and measurement during regular operation of the Hazleton Brick Co. plant, Hazleton, Pa., in July 1953. This report presents the results of this investigation and a description of producer and periodic-kiln equipment, operating procedures, and labor requirements. A summary of the conditions of producer and kiln operation is given for the 2-week observation and for the 11 preceding months. The two 10-foot standard anthracite-gas producers consumed 301 tons of Rice and Buckwheat No. 1 anthracite, as delivered, averaging over 13,000 B.t.u. per dry pound during the 2-week period, with a producer hot-gas efficiency of 95 percent, at an average gas offtake temperature of 5400 F. The yield of gas5/ of 153 gross B.t.u. per cubic foot amounted to 140,000 cubic feet per ton of fuel as fired, or 73,500 cubic feet per kiln heating hour, which was sufficient for kiln requirements.

Jan 1, 1960

By Gill Montgomery

This report covers operations at the Crystal-Victory and Minerva No. 1 mines in Hardin County, Ill., which are operated by the Minerva Oil Co., Fluorspar Division, with offices in Eldorado. It describes the exploration, development, and mining practices, giving costs of each. Transportation, equipment, power, labor, and other influencing factors also are discussed. The mining methods employed are those most applicable to the flat-bedded replacement deposits common to the Cave-in-Rock section of the Southern Illinois fluorspar district. The fluorspar beds occur from surface exposures to 1,000 feet deep. In this district churn drilling is the method practiced for exploring flat-bedded deposits from the surface. Aerial photography and geochemical methods for indicating mineralization have been helpful in planning a drilling program. A program usually includes enough drilling to obtain only sufficient data on the value of the ore body and its structure to justify initial development and purchase of the mineral rights under option.

Jan 1, 1960

By W. A. Grosh

Records show that much of the lead produced in the Upper Mississippi Valley lead-zinc field was taken from natural openings along crevice systems at shallow horizons or at the surface. During the early history of the district, the shallow deposits were worked intensively; but in recent years the production of lead, except as a byproduct of deeper mining for zinc ores, has not been significant. Considering the methods of early mining, the character of mineralization, and the fact that galena can still be found on the surface of the old digging areas, it was reasoned that enough mineralization might remain on and above bedrock to permit, through the use of modern equipment and methods, economical re-treatment of surface material in the digging areas.

Jan 1, 1960