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By N. Parlee, V. C. Kashyap

The solubilities of nitrogen in liquid iron and liquid Fe-Ni, Fe-Mo, Fe-V, and Fe-Mo-V alloys were measured by the Sieverts method. Measurements were made at 1600° to 1800°C on binary alloys up to 20 pet Ni, 10 pet V, 10 pet Mo; and on ternary alloys containing 0 to 3 pet V with 0 to 5 pet Mo. The results on liquid iron confirm that Sieverts' law is obeyed in the range 50 to 750 mm pressure. The measured solubilities and their temperature coefficients are in general agreement with other modern authors. The logarithms of the activity coefficients of nitrogen in the binaries are approximately linear functions of the pet of alloying element. A method suggested by Wagner, Chipman, and others for predicting gas solubilities in complex alloys from solubility data on binaries was applied to the Fe-Mo-V alloys. Reasonably good agreement was obtained between calculated and experimental solubilities. NITROGEN'S solubility in liquid iron has been studied by a number of investigators. It is reasonably well established that the solubility of nitrogen follows Sieverts' law at least up to 1 atm partial pressure and that the solubility increases gradually with temperature. The solubility of nitrogen in Fe-X binary liquid systems has been investigated in only a few cases. Only the systems Fe-Cr,3-5, 7 Fe-V,3 Fe-Mn,3, 5 Fe-Ni,3, 5 Fe-Si,B, H Fe-C, L, H and Fe-P4 appear to have received any study. The only work on liquid Fe-V was done by Brick and Creevy.3 This was limited to 13.5 pet and 26.5 pet V, but no exact temperatures were recorded. No work whatsoever appears to have been done on liquid Fe-Mo alloys and even work on Fe-Ni alloys is rather scant. The work on liquid ternary systems is still more limited, and the only publication available appears to be that of Wentrup and Reif,7 who studied the Fe-Cr-Mn and Fe-Cr-Ni alloys. Rassbach, Saunders, and Harbrecht17 have reported work on the solubility of nitrogen in stainless steel but this was not a systematic study of any particular system. Commercial alloys usually contain several alloying elements. Thus, it often becomes important to be able to predict the nitrogen solubility in systems containing two or more added elements without the necessity of making measurements. Wagner,14 Chipman," Darken and Gurry," and Morris and Buehl 14 have suggested means by which this may be accomplished, and Langenberg14 has recently applied one of these methods to nitrogen solubility in complex liquid alloys. This paper reports the results of nitrogen solubility determinations on Fe-Ni, Fe-Mo, Fe-V, and Fe-Mo-V alloys and compares calculated and experimental solubilities in the ternary alloy. Attempted measurements on Fe-Cr alloys were not successful by the experimental method employed. Experimental Method The general method of solubility measurement was that of Sieverts.' The apparatus and procedure were essentially the same as used by Liang, Bever, and Floe."' The equipment consisted of a small vacuum furnace heated by a 6 kw induction unit, gas measuring apparatus, and a gas purification train. The crucibles used were Norton Alundum with alumina sand around them for insulation. The crucibles were charged with 100 to 200 g of material, about 180 g or nearly filling the crucible being found most satisfactory. Hot volumes were determined with argon and ranged from 95 to 130 cu cm (stp). Temperature measurements were made with a Leeds and Northrup optical pyrometer which was calibrated periodically against the melting point of iron in the same apparatus."-'* Good quality nitrogen, hydrogen, and argon gases were further purified and dried in standard purification trains. The sources of the high purity iron and other alloying elements used were as follows:

Jan 1, 1959

By W. L. Heidenreich

This report describes the methods and results of field investigations conducted by the Bureau of Mines between December 1956 and December 1957 on seven deposits of nickel-cobalt-iron-bearing laterite and weathered serpentine near the west coast of Puerto Rico east and south of Mayaguez. These deposits were named, for purposes of identification, Guanajibo, Punta Guanajibo, Las Mesas, north and south deposits of the Rosario Southeast group, and the west and east deposits of the Maricao Southwest group. In addition, the lower 17 miles of the Guanajibo River Valley was tested at widely spaced intervals for possible concentrations of magnetite and chromite in the alluvial sands. The objective of the investigations was to appraise, by drilling and sampling, the two largest deposits--the Guanajibo and Las Mesas. Testing of the smaller deposits was much more restricted. Field investigations consisted of mapping, drilling with power auger, sampling drill-hole sections, and pre-paring samples for chemical analyses, mineralogical studies, and metallurgical tests. The work was financed jointly under a cooperative agreement by the Bureau of Mines and the Economic Development Administration, an agency of the Puerto Rican Commonwealth.

Jan 1, 1959

By Eugene T. Sheridan

The 25th annual survey of the peat industry by the Bureau of Mines, United States Department of the Interior, disclosed that 79 companies produced and sold peat from 81 operations in 21 States in 1958. Peat is a carbonaceous deposit, formed under water or in a water-saturated environment from plant material. It is the first stage in the development of coal and, when properly dried, can be used as fuel. Although 98 percent (estimated) of the total world production is used for energy purposes, the status of peat in the United States is somewhat unique in that none is used for fuel, and practically all is consumed as an agricultural product, chiefly for soil improvement purposes. The domestic peat industry has expanded rapidly since World War II, and production in 1958 was 327,813 net tons valued at $3,445,767. More than one-half million ton of peat was consumed in the United State in 1958, however, as 269,096 tons was imported.

Jan 1, 1959

By Alexander E. Morrow

Oxygen breathing apparatus for use in mines was introduced to the United States in 1907. Despite their intended purpose of safeguarding lives, the apparatus led to the deaths of many men because of inherent or developed defects in the equipment, lack of training,, physical shortcomings of wearers, and improper procedures. The Bureau of Mines pioneered in research and training to curb logs of life among users of such apparatus and promoted development of safer equipment and procedures. As a consequence, deaths have been far less frequent. In 1944 the Bureau issued Information Circular 7279, Loss of Life Among Wearers of Oxygen Breathing Apparatus. That publication listed the case histories of 26 deaths that had occurred since the introduction of such equipment to American mining. The author, the late G. W. Grove,3/ asserted that further loss of life could be avoided if good equipment were used, teams were properly trained, and the basic principles of safe procedure were followed. This publication is a sequel to I.C. 7279 and contains information on eight deaths among wearers of oxygen breathing apparatus that were overlooked in the original compilation. It also describes the single death that occurred since I.C. 7279 was published.

Jan 1, 1959

By W. T. Wertman

A research program to aid development of better petroleum-recovery technology is in progress at the Appalachian Experiment Station, Bureau of Mines, Morgantown, W. Va. The work is part of the overall effort of the Federal Bureau of Mines to effect true conservation of the Nation's natural resources. Knowledge of the magnitude of the interstitial water content of oil-bearing formations is important to petroleum-reservoir engineers because of the influence of water on fluid flow during oil production and because of the significance of water volume in oil-reserve evaluation. Such information on Appalachian oil-bearing formations is needed to aid in planning secondary oil-recovery projects. Generally, the interstitial water content of oil sands can be estimated by one or more of the following methods: Analysis of cores obtained with oil-base drilling fluid, electric logging, restored-state or capillary-pressure tests, centrifuge tests, evaporation tests, or mercury-injection tests.

Jan 1, 1959

By Carl Rampacek

Recent research by the Bureau of Mines has demonstrated that the segregation process has merit for treating oxidized and mixed oxide-sulfide copper ores. The process comprises heating the crushed ore with salt and coke or other carbonaceous materials at about 700° C. to produce fine flake copper, which then is recovered by conventional copper-flotation methods. Bench-scale laboratory tests of a number of oxidized and mixed copper ores assaying 0.78 to 5 percent Cu gave copper recoveries of 73 to 96 percent. The flotation concentrates assayed 21 to 76 percent Cu, depending on the ore being treated.

Jan 1, 1959

By J. J. Becker

Changes in magnetic properties with particle size are used to study the precipitation process in a Cu-Co alloy. In particular, the effect of a field during aging in producing anisotropy is shown to occur entirely during the growth of the particles, after precipitation is complete. HEAT-treatment in a magnetic field is done commercially to improve the magnetic properties of a number of materials. These can be divided into solid-solution alloys and precipitation alloys. The Permalloys are representative of the first type, and magnetic annealing greatly increases their maximum permeability. On the other hand, in precipitation alloys such Alnico 5 the important result is an increase in maximum energy product. The effect of the field in all cases is to bring about an additional magnetic anisotropy, uniaxial in nature, which makes the hysteresis loop more upright when measured in the direction in which the field was applied. The structural origin of the anisotropy brought about by magnetic annealing is not well understood. In the solid solution alloys, one possible explanation is based on ordering.' Another possibility is the orientation of like-atom pairs.' The precipitation systems known to respond to magnetic heat treatment are Alnico 2, in which the effect was first discovered," Alnico 5, cobalt ferrite (oxide),' and Cu-Co alloys.3 n these materials, the field affects the precipitation process itself in some way. Although there has been much work on Alnico 5. its nature is still incompletely understood. According to Geisler,' the precipitation reaction is of the

Jan 1, 1959

By F. D. Everett

The Burgin shaft of Bear Creek Mining Co. near Eureka, Utah, was sunk during 1956 and 1957 as part of an exploratory program, searching for lead, zinc, copper, silver, and gold ore bodies hidden from the surface by several hundred feet of volcanic rocks. This paper describes the sinking methods and operating practices of Centennial Development Co., contracting firm for Bear Creek Mining Co., in sinking a 3-compartment vertical shaft 1,100 feet. The operation featured the Cryderman positive-action, clam-type shaft mucker. The shaft was completed in 142 days by a shaft crew of 10 men and a top force of 10 men, including supervision.

Jan 1, 1959

The final session of the meeting was preceded by a movie, "Contact That Kills," which was a color film clearly pointing out various causes of electrical accidents in mines and how such accidents could he prevented. This film was made underground and produced by the U. S. Bureau of Mines for use in teaching accident classes. President R. R. Williams, Jr., called the meeting to order and introduced Mr. Leif Arentzen of the Lee-Norse Company, Charleroi, Pennsylvania, who spoke on "Coal Mining in Australia." The text of his address is as follows: "I arrived in Australia in February of this year-my father sent me over there for an installation. He preceded me as he does in most things, and set up a showing of our machine in Australia. We had 200 of the top level coal mining men visit this showing. They were interested in what the Americans are doing and what the American manufacturer had to offer them. Conditions in Australia are very similar to our mining conditions in the United States and they have looked to us, the coal industry in general, because we have the know-how in answering some of their problems. They feel that European methods and their type of machines are too inadequate to cope with their conditions. My visit was to South Wales, 60 miles south of Sidney. Their mining operation resembled mining coal in Florida. The work is on about a 500-ft. elevation about three miles from the ocean and when you turn around and see about 30 miles of beach, it is quite a picture - the Pacific Ocean is so blue. The coal seam is about ten feet of relatively clean coal. Labor relations are very, very taught right now. They are agitated by a strong Communistic influence and their weekly publication is known as the ?Common Cause,? which is against mechanization of coal mines." Mr. Arentzen enlarged on the fact that America was the example they held before them and described the Australian coal men and their character.

Jan 1, 1959

By Van E. Shaw

Three comparatively simple, efficient, and rapid extraction methods for the dissolution of yttrium and rare-earth elements from a euxenite carbonate residue have been developed, using dilute sulfuric acid as the solvent. Extraction processes have resulted in yields of 98+ percent of the total rare-earth elements and yttrium contained in the residue and have given preliminary separation between the cerium-group and the yttrium-group rare-earth elements. Extraction procedures presented are: Procedure 1. -The recovery of total rare-earth elements and yttrium by a cold dilute sulfuric acid leach at a pH of 2.5. Procedure 2. -The recovery of yttrium and yttrium-group rare-earth elements by leaching with dilute sulfuric acid at 125° F. and a pH of 3.0, with subsequent recovery of the cerium-group rare-earth elements by a cold dilute sulfuric acid leach of the residue at a pH of 2.5. Procedure 3. -The recovery of the total rare-earth elements and yttrium by fractional leaching as in procedure 1, followed by boiling the sulfate solution, which precipitates the cerium-group rare-earth elements and leaves the yttrium-group rare-earth elements in solution.

Jan 1, 1959

By J. P. Powell

The application of secondary producing methods for recovering additional oil from known fields has been recognized for many years as important to the economy of the nation. One of the most successful secondary methods is waterflooding, which conserves our natural resources by preventing premature abandoment of stripper leases and revitalizing previously abandoned areas. Waterflooding as a secondary-recovery method was introduced into the Midcontinent region in 1931, and its use as such has become widespread. As with most new methods, the most favorable fields and leases received primary attention, whereas those with viscous oil or less favorable sand characteristics were bypassed. Numerous reports3 4 5 6/ have been published giving the results of individual waterflooding projects, In this report, attention is directed to the effect of a single factor, the viscosity of the oil produced,

Jan 1, 1959

By C. Feng, C. Elbaum

Knoop hardness measurements were carried out on large grains of iodide titanium containing different amounts of oxygen. For each oxygen content the hardness is recorded ainingas a function of the crystal orientation and of the angle 4 between the indenter diagonal and the projection of the C (hexad) axis in the surface. The results can be expressed by the following relation; hardness = n-k cos 2ø, where n and k are constants for a given oxygen content and crystal surface orientation. A NISOTROPY of hardness is a well-known phe-nomenon and has been reported for many metals.1-3 At the present time, however, such information is not available in the literature for titanium. Consequently, a systematic study of the simultaneous effects of oxygen content and crystallographic orientation on the hardness of titanium was undertaken in this laboratory. Evaluations of oxygen content in titanium are frequently carried out through hardness tests. Although such procedures may be justified in small grain specimens, the results of the present investigation indicate that the anisotropy of hardness should be taken into account in the case of coarsegrained specimens as well as in the case of pronounced preferred orientation. Materials and Experimental Procedures Iodide titanium, 99.99 pet pure and containing of the order of 0.002 wt pet O, was used throughout this investigation. The metal was arc melted in an argon atmosphere and cold rolled into strips 1/16 in. thick. These strips were subsequently recrystal-lized and strain annealed in vacuum (10" mm Hg or better) at 850°C in order to produce crystals varying in diameter from 10 to 25 mm. Oxygen was introduced into selected large crystals by heating at 700°C in an atmosphere of pure oxygen under an observed pressure of approximately 50 mm Hg. Each sample was subsequently annealed in vacuum at 850°C for 100 hr, in order to homogenize the oxygen content throughout the specimen. It was found that longer annealing was not necessary, for no change of surface hardness in a given direction was detected after prolonged annealing. The oxygen content was determined by the difference in weight of the specimens before and after the oxidation-annealing cycle. The accuracy of oxygen determination is within ±0.1 mg in samples weighing 0.5 to 1 g. A vacuum fusion analysis of oxygen was performed on several samples and gave results in good agreement with the ones obtained by the weight change. It should be emphasized that expected weight losses through evaporation of the metal in vacuum at 850°C' are many orders of magnitude lower than the precision of these measurements. Following the annealing treatment, both oxidized and unoxidized crystals were carefully polished. All detectable traces of surface cold working were removed by repeated polishing and etching. Laue back reflection X-ray patterns were taken for each crystal for the purpose of determining the orientation and ascertaining the absence of substructures detectable by this method. Hardness measurements, using a 1 kg load, were subsequently carried out on a Tukon hardness tester equipped with a Knoop indenter. The Knoop indenter was used throughout this work because indentations obtained by means of a Vickers indenter are considerably distorted due to the anisotropy of the elastic constants in titanium. Such distortions are much less pronounced in the case of Knoop indentations, although for some orientations a cer-

Jan 1, 1959

By L. W. Berger, and R. I. Jaffee, D. N. Williams

The effects of hydrogen on the properties of binary Ti-A1 alloys containing 2.5, 5, and 7 pct aluminum and ternary alloys of the same compositions with added interstitial elements oxygen, nihrogen, and carbon were stzdied. Aluminum increases the apparent hydrogen solubility of the a-phase, resulting in a marked increase in resistance to impact embrittlement. In the Ti-5Al and Ti-7Al alloys, for example, the addition of 180 and 305 ppm hydrogen, respectively, did not cause embrittlement, while unalloyed titanium was embrittled by as little as 75 ppm. The role of aluminum in increasing hydrogen solubility of the a-phase probably accounts for the excellent hydrogen tolerance of a-ß alloys containing considerable amounts of aluminum. There is some evidence that aluminum retards the rate of hydride precipitation. If so, these alloys may be susceptible to slow-strain embrittlement. UNALLOYED a-titanium is extremely sensitive to small amounts of added hydrogen in that there is a marked decrease in notch properties. For example, as little as 100 ppm hydrogen is sufficient to lower the room-temperature notch-impact strength from over 100 to less than 20 in.-lb.' This loss of impact Strength has been associated with the Presence of hydride phase in the microstructure. Hydrogen in the amounts encountered in commercial practice

Jan 1, 1959

By J. B. Elizondo

This paper, which describes mining methods and practices at the Piokee mining unit and the Piokee expertmental mining project of The Eagle-Picher Co. in northeast Oklahoma, is one of a series being prepared by the Federal Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The Piokee unit, comprising the Piokee, Rowe, Lucky Syndicate, and parts of the Netta White and Otis White leases, is in the SW1/4, W1/2NW1/4SE1/4, and W1/2SW1/4SE1/4 sec. 17, T. 29 N., R. 23 E., Ottawa County, Okla. (figs. 1 and 2), The 200-acre tract is adjacent to the town of Picher and near the heart of the Picher field of the Tri-State zinc-lead mining district.

Jan 1, 1959

By Douglas D. Donald

The New Jersey Zinc Co. successfully holed through a 2 1/2-mile haulage tunnel connecting its new Ivanhoe shaft with the Van Mater Shaft at Austinville, Va. This 8x 10-ft cross-section tunnel was driven from both ends and met at a point approximately a mile from one shaft and a mile and a half from the other. In order to make certain that the faces met accurately on line and grade it was necessary to refine conventional mine surveying practices. The mines that are serviced by these shafts are located in the southwestern part of Virginia approximately midway between Roanoke and Bristol at the west foot of the Blue Ridge. While the presence of lead-zinc sulfide ores has been known in this area for more than 200 years, it was in 1902 that New Jersey Zinc Co. acquired the Austinville property, which has been in constant operation since that time. About ten years ago the company undertook an extensive diamond drilling program at Ivanhoe several miles to the southwest. This program was successful in locating sufficient ore to justify the purchase of a number of the properties in this area and plans were made to develop the new orebodies. The discovery of this ore as well as substantial addi- tional reserves at Austinville resulted in a decision by the company to increase its daily milling capacity to 3000 tons, of which about 1000 tons would be supplied from the Ivanhoe mine. After careful consideration of all possible methods of transporting this volume of ore from Ivanhoe to the mill, it became evident that diesel locomotive haulage through a 2½-mile tunnel between the two mines would best suit prevailing conditions. Since the lowest operating level, known as the 1100 level, of each mine would be at approximately the same elevation, it was obvious that such a tunnel should be driven on this level. Not only would this tunnel facilitate feeding Ivanhoe ore into the underground crusher and skip loading installation at Austinville, but it would also open up a known orebody 5000 ft southwest of the Van Mater shaft. In addition it would provide a valuable diamond drilling base from which a large and a potentially favorable but untested block of ground might be explored. In order to hasten the completion of the tunnel, it was felt that it should be driven from both ends. ENGINEERING CONTROL PROCEDURES It was vital that the tunnel junction be made accurately on line and grade; thus it was felt that engineering control of an unusually high degree of reliability was required to prevent an accumulation

Jan 1, 1959

By J. D. Lubahn

Prior tests by Dorn, where the strain rate in a tensile test was suddenly changed, have shown a small, but definite rate-history effect to exist. If this effect is neglected in the calculation of creep behavior from tensile results, an error should occur. This paper shows that this error is smaller than experimental scattering, and may be neglected. DORN1 has found a small but definite rate-history effect in the aluminum alloy 250 at liquid-nitrogen temperature using tensile tests with an abrupt rate change. Such an effect is to be expected from pre-viously known2-6 temperature-history effects, together with general experience that effects produced by changing the strain rate a large amount are simi-

Jan 1, 1959

This report is the 21st in a series summarizing research and technologic work on coal and related investigations by the Federal Bureau of Mines - the Chard of the series published on a calendar-year basis 2/ Subject publica¬tions of the Bureau during 1956 are cited, and pertinent Bureau work is described briefly. The most effective method of conserving our important coal reserves is through improved technology of production and utilization. Associated problems form the program of the Bureau.3 4 5 6/ Potential production is depend¬ent on a knowledge of the quantity and quality of the reserves, and the Bureau continues to contribute information on this subject. Many problems are being studied that relate to improvements in current production, including mining methods and health and safety measures. Preparation of mined coal is necessary for its most efficient utilization. Preparation by conventional methods is being studied, as well as the development or new methods. Fundamental studies on the structure and properties of coal are necessary to insure full advantage of the special qualities of different coals. Controlling factors in the efficient use of coal in combustion, carbonization, gasification, and direct and indirect hydrogenation of coal are being studied continuously, and new processes are being investigated. The many advances in all these fields are discussed.

Jan 1, 1959

By R. F. Zaffarano

Data presented on the physical characteristics of the reservoir oil, Aneth field, represent the initial phase of a study of Paradox basin reservoir oils being made by petroleum engineers of the Federal Bureau of Mines, Petroleum Research Center, Laramie, Wyo. The purpose of the study is to determine the original reservoir-oil characteristics in several important new discoveries in the Paradox Basin and to investigate correlations between the properties of these reservoir oils and structural or areal position within the basin, If migration is limited and oil accumulates near its source, then it seems probable that few differences should be found in the composition and characteristics of reservoir oils occurring in given age rocks and within the confines of a geological basin. Within these limits, conditions that effected the formation of oil and its transfer from parent to storage rocks probably were rather uniform in an area the size of most of our geological basins. However, if oils should migrate considerable distances, it seems logical to expect that the relative quantities of gas and liquid components may differ in traps occurring along the direction of migration, corresponding with the theory of differential entrapment (5).4/

Jan 1, 1959

By W. H. Zieman

"THIS IS THE THIRD of the consecutive Annual Forums on Grinding that were instituted by Mr. L. E. Djingheuzian in 1957. The first was on the subject of Ball Milling (Transactions, Volume LX, 1957) and the second on The N on-Cataracting Ball Mill (Trans-actions, Volume LXI, 1958). From the discussions at these forums it was evident that one of the most important factors affecting the efficiency of grinding is the shape of the liners. In order to make a study of liners in use, it was •decided to seek the co-operation of operators across the country by sending out questionnaires requesting basic information. Additionally, these operators were urged to set down briefly any pertinent information on the subject acquired through experience and experiments at their own particular plants. A compilation and analysis of these data were to form a basis for discussion at the Forum on Liners at the Annual Meeting in Montreal, April, 1959. The response of the milling fraternity to this solicitation was most gratifying, and clearly indicated the importance attached by the operators to the effect of liner design upon overall grinding performance."

Jan 1, 1959

By R. L. Montgomery

The heats of formation of lanthanum sulfate and the enneahydrate are -939.8 ± 3.1 and -1,587.1 ± 3.2 kcal. per mole, respectively. The heat of hydration is -32.5 ± 3.5 kca1. per mole. These values were obtained from heat-of-solution measurements of lanthanum oxide and salts. Low rates of solution precluded more accurate determinations of the thermal data. The heat of formation of the chloride was similarly observed to be -256.18 ± 0.28 kcal per mole. Heats of solution and combustion of lanthanum metal yield mutually concordant results, and earlier discrepancies reported in the literature may be ascribed to impurities.

Jan 1, 1959