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By M. M. Fine

This report presents the results of laboratory mineral-dressing investigations by the Bureau of Mines of 14 individual or composite character samples from deposits in the Batesville manganese district. It will be noted that some concentrates have met or approached analytical specifications for metallurgical manganese ore although great variations in both physical and chemical composition from once deposit to another make each a new problem. In most cases it is evident that a substantial loss of manganese has occurred in the various slime and tailing products. An important aspect of this work is the research being conducted on manganese-bearing limestones. Recent reconnaissance indicates that this resource constitutes one of the major domestic reserves of manganese. Laboratory study has shown that ferrograde concentrates can be recovered from samples of manganese-bearing limestones from two properties. Research on samples from other areas is still underway.

Jan 1, 1957

By K. K. Kershner

The purpose of this investigation was to develop methods on a laboratory scale for recovering tin from metallurgical slime, Tin chlorides were volatilized using mixtures of hydrogen chloride and reducing gases, such as hydrogen, carbon monoxide, hydrogen sulfide, ethane, propane, and butane. Optimum conditions were found to be n mixture of 3:1 of hydrogen and hydrogen chloride at 475° C. Over 95 percent of the tin was volatilized as chlorides. Low temperatures and relatively rapid rates of reaction are distinct advantages of the chloride volatilization process. Research is being continued with various slimes and will be extended to tin ores, where the method offers interesting economic possibilities in comparison with current tin-smelting practice.

Jan 1, 1957

By C. A. Kumke

The Korean crisis and the cessation of Russian manganese-ore shipments to the United States in 1950 reemphasized the almost total dependence of the domestic steel industry on foreign supplies for metallurgical-grade manganese ore. In this emergency, Congress authorized the Bureau of Mines to undertake experimental mine and process development work on the known large reserves of low-grade manganese ore in the Artillery Mountains region in Mohave County, Ariz. The objective of the work was to obtain the basic mining and metallurgical data needed to make specific plans for initiating exploitation of the deposits within 3 years if high-grade foreign ore could not be obtained during the emergency. The manganese deposits of the Artillery Mountains region are in an area of about 25 square miles on the north side of the Bill Williams River in southern Mohave County. Lasky, of the Federal Geological Survey, has estimated reserves at 175 million tons of manganiferous material assaying 3.5 to 4 percent Mn. Although the man¬ganese occurs in various Tertiary and Quaternary formations as both bedded and fissure vein deposits, the more important syngenetic deposits are found in upper and lower manganiferous zones in the sedimentary beds of playa and alluvial fan origin that constitute the Chapin Wash formation.

Jan 1, 1957

By R. W. Huber

A consumable-electrode arc-melting furnace was constructed at the Bureau of Mines Physical Metallurgy Laboratory, College Park, Md., for the production of uncontaminated titanium and titanium-alloy ingots. The furnace was designed to allow for evacuating to very low pressures and back filling with helium and argon mixtures for melting at or near atmospheric pressure. Vacuum melting at a few millimeters pressure was also used with a mixture of helium and argon gas sweeping the crucible. For research purposes a 25- to 30-pound ingot, 4 inches in diameter by 15 inches in length, was selected to provide, enough 1/2-inch plate for extensive tensile and impact testing of standard size specimens. Enough plate was also provided for testing by other Government laboratories. The homogeneity of several alloy ingots was determined, and excellent results were obtained. By using a large electrode-to-ingot-area ratio and high currents or power inputs to the arc furnace rather uniform ingots were routinely prepared.

Jan 1, 1957

By Parkhurst D. H

It is shown that a differential colorimetric technique can be used as a routine method for the estimation of titanium in beach sands, and their ore dressing products. The method will tolerate the presence of most of the other elements usually found in beach sands. The accuracy is shown to be within the limits of ±0ò31 per cent for concentrates containing more than 95 per cent titanium dioxide and ±1 per cent for tailings containing 0ò2 per cent titanium dioxide. The method is described for use with a Hilger "Spekker" absorptiometer.

Jan 1, 1957

By G. E. McElroy

Ventilation-pressure surveys are required to determine the rates of pressure losses in various parts of mine-airway systems. These may be determined directly by differential pressure measurements or deduced from absolute pressure measurements, Despite the confusion caused by its inverted nonlinear scale, the altimeter has special application to pressure surveys in mines in which only small differences in elevation are involved, as is true for most of our large bituminous-coal mines in these, the judicious use of information obtained by pressure surveying can result in greatly improved working conditions as regards health and safety and, in many instances, can yield large financial returns. The main purposes of this report are to discuss methods of using altimeters for pressure surveys and to present the particular methods of making surveys and calculating the results of surveys used by the Mine Ventilation Section of the Bureau of Mines.

Jan 1, 1957

By Robert F. Pettit

This paper on methods and costs of mining and milling iron ore at the Iron Mountain mine of Ozark Ore Co., St, Francois County, Mo., is one of a series of Bureau of Mines reports on methods, practices, and costs of mining and milling throughout the United States. The Iron Mountain operation is notable for its successful transition from open-pit to underground mining, for use underground of large earth-moving equipment, and for development of a multilevel room-and-pillar mining method. Milling methods also have undergone transitions - from hand sorting and log washing in the early days to gravity concentration. Milling ultimately may include flotation to recover additional iron from products now discarded as tailing,

Jan 1, 1957

By Elmars Ence, Harold Margolin

The Ti-Fe and Ti-Fe-0 systems were re-examined because of the controversy regarding the existence of Ti2Fe, and to consider all available data points to the existence of Ti,Fe. The Ti-Fe-0 system contains two ternary compounds: E, corresponding to Ti2Fe; and y. SEVERAL authors have investigated the constitution of titanium-rich alloys of the Ti-Fe system. The most extensive study of titanium-rich portions of the Ti-Fe system was by Van Thyne, Kessler, and Hansen,' who investigated this system up to 50 pet Fe and used the highest purity materials available for their alloy preparation (iodide titanium was used for alloys up to 20 pet Fe). According to Van Thyne et al., phase relationships in the region of investigation are governed by phases a,ß, and TiFe. No evidence of an intermetallic compound Ti,Fe was found. although earlier. works by Laves and Wallbaum,' and Duwez and Taylor' reported its existence. Rostoker's study on the occurrence of TilX phases" confirmed the findings of Van Thyne et al. Rostoker proposed that the compound Ti Fe found by Duwez does not exist but is actually a ternary compound, Ti1Fe3O, originated by inadvertent oxygen contamination. The partial isothermal section of the ternary Ti-Fe-0 system as reported by Rostoker' seems to confirm this explanation. In the course of phase diagram work conducted at New York University, however, certain irregularities were observed to be associated with ternary systems of the type Ti-Fe-X. The ternary phase 6, observed in the systems Ti-Fe-Mo' and Ti-Fe-V." was found to be structurally identical to the com-pound Ti2Fe as reported by Duwez and Taylor, and to Rostoker's compound Ti1,Fe2O. Since the amount of oxygen possibly present in the Ti-Fe-Mo and Ti-Fe-V systems could not account for the observed amounts of the compound, it appears that the d phase in these systems is not Ti,Fe,O. On the other hand, considering the amounts of the 6 phase, particularly in the Ti-Fe-Mo system, the location of the phase was uncertain. It was felt that the introduction of the Ti2Fe phase would alleviate some of the inconsistencies of the two systems. Because of the uncertainties relating to the phase Ti2Fe, or Ti1Fe2O, it appeared worthwhile to re-examine the Ti-Fe and Ti-Fe-O systems in the vicinity of these compounds with highly sensitive metallographic techniques and with X-ray methods. Experimental Procedure Alloy Preparation—For the study of the binary system four alloys were prepared, containing 26.9 (30 wt pct), 34.0 (37.5 wt pet), 41.2 (45 wt pet), and 56.3 (60 wt pet) atomic pet Fe, and for the ternary Ti-Fe-O system 18 alloys were prepared in the composition range of 1.6 to 16.9 atomic pet 0 and 24.3 to 55.7 atomic pet Fe. The materials used for the Ti-Fe alloys were iodide titanium (99.98 pet Ti, 0.002 pet 0) and Ferro-vac-E iron (99.95 pet Fe, 0.0052 to 0.0072 pet 0). For the Ti-Fe-O study the materials used were sponge titanium containing less than 0.06 pet 0, Ferrovnc-E iron, and Baker's analyzed TiO2. The nominal weight and atomic percentages of the ternary alloys prepared are shown in Table I. Melting—Charges of 10 to 15 g were melted in a nonconsumable arc furnace in argon atmosphere according to the technique described elsewhere.'" Since there was practically no weight loss through the various stages of melting and oxygen losses have not been observed previously, it appeared justifiable to use nominal composition for interpretation of data. Iodide titanium control buttons, of the same mass as the Ti-Fe charges, and melted under the same conditions, were used to check hardness pickup during melting. A hardness increase of 2 to 3 Vhn was found. Heat Treatment—The specimens were annealed in quartz capsules under argon. To avoid contact between the specimen and capsule material all specimens were wrapped in titanium sheet. The annealing times are given in Table 11. The attain-

Jan 1, 1957

By W. H. Oppelt

A small, annular-retort gasifier having a nominal capacity of 40 pounds of lignite per hour was designed and constructed at the Lignite Experiment Station, Grand Forks, N. Dak. The purpose of the investigation was to increase the capacity of an annular-retort gasifier by better temperature distribution in the heating chamber (adjacent to the annulus) and by supplemental internal heating with controlled amounts of air. Correct control of air admission should yield crude ammonia-synthesis gas having a (H2+CO)-N2 ratio of 3. Dakota Star stoker-size lignite was used during the exploratory experimental program. The effects of temperature level and distribution in the heating chamber and of addition of air to the reactor were investigated. Hydrogen - carbon monoxide ratios ranged from 1.9 to 2.5, and (H2+C0)-N2 ratios were as low as 2.9. Hourly gas production ranged from 970 to 2,580 cu. ft., or 62.0 to 164 cu. ft. per sq. ft. of heated surface, or 350 to 940 cu. ft. per cu. ft. of reactor volume. Data from the small gasifier could be readily correlated with those previously obtained in the commercial-scale unit under comparable experimental conditions.

Jan 1, 1957

By Wilbur I. Duvall

This report presents experimental data on crater formation in four rock types. From an analysis of these data a general theory of rock breakage by explosives is deduced. This theory accounts for most of the rock breakage and other phenomena that occur when a concentrated charge is detonated in a drill hole near a free surface. From instrumented crater tests and high-speed motion pictures of the explosions, various experimental checks on the deduced theory of rock breakage are made. The general mechanism of rock breakage by explosives as described in this report is outlined briefly below. The detonation of the explosive charge creates a high gas pressure in the charge hole, which in turn generates a compressive strain pulse in the surrounding rock. This compressive strain pulse travels outward in all directions from the charge hole. Near the charge hole the amplitude of this strain pulse is sufficient to cause crushing of the rock. However, as the strain pulse travels outward its amplitude decays rapidly until no further crushing of the rock is possible. The compressive strain pulse continues to travel outward until it is reflected by a free surface. Upon reflection the compressive strain pulse becomes a tensile strain pulse. As the strength of rock in tension is much less than in compression, the reflected tensile strain pulse is able to break the rock in tension, progressing from the free surface back toward the shot point. In other words, the rock is pulled apart, not pushed apart.

Jan 1, 1957

By E. D. Wilson

A study of factors related to subsidence was specified in a project proposal entitled "Structural Analysis of Block-Caving Operation, San Manuel Copper Mine, Pinal County, Ariz.," approved by the Bureau of Mines early in 1953. This proposal was designed by Charles H. Johnson, then chief of the Base Metals Branch of the Minerals Division, Washington, D. C., assisted by Dr. Leonard Obert, chief of the Applied Physics Branch, Region VIII (now Region V), College Park, Md., and E. D. Gardner, chief mining engineer, Bureau of Mines, Washington, D. C. It read as follows: This project is a study of the mechanics of undercut block caving in a deep ore deposit. The San Manuel is a low-grade disseminated copper deposit containing nearly a half billion tons of ore lying at depths of 500 to 2,000 feet. Development is just starting. Production is to begin in 3 to 4 years (in 1956) at a rate of 30,000 tons of ore a day, or 60,000 tons of copper a year. A Government loan of $90,000,000 /subsequently increased to $94,000,000/ and a long-term Government purchase contract support the capital investment, which will total about $110,000,000.

Jan 1, 1957

By E. C. W. Perryman

BEFORE describing the methods used for fabricating uranium into various shapes and sizes it is necessary to illustrate briefly the unusual conditions under which uranium has to operate when used as a fuel element in a reactor. During reactor operation, for every fission that occurs two atoms of intensely radioactive fission products are produced together with two or three neutrons. The neutrons that are ejected possess several m.e.v. of energy and when one of them strikes an atomic nucleus, that atom acquires up to 105 e.v. of kinetic energy. This is large enough to displace the atom from its lattice position and send it shooting through the crystal, displacing other atoms out of their lattice positions. The net result is that a large number of vacancies and interstitial atoms are formed within the crystal lattice which sometimes have profound effects on the physical and mechanical properties of the material in question.

Jan 1, 1957

By E. S. Machlin

The possibility that formation of voids under creep-rupture conditions may take place by the condensation of vacancies has been investigated theoretically. It has been concluded that nucleation of voids under creep-rupture conditions by vacancy condensation is highly improbable. However, growth of pre-existant voids by vacancy condensation is probable. A number of predictions made in this theory have been verified by the data. It has been predicted and checked that the product of rupture life and steady-state creep rate for preannealed metals and single phase alloys is an approximately invariant quantity, independent of stress, temperature, and atomic number for a given type structure. The direction of the effect of cold work on this product has been predicted and found in agreement with experiment. A number of experiments to evaluate the vacancy condensation mechanism further are described. SEVERAL papers have appeared recently which speculate on the origin of voids formed at grain boundaries under stress.' ' The object of this paper is to examine quantitatively the proposition that the voids produced in a creep test are a result of vacancy condensation. A result of this paper is a theory of creep-rupture. Void Nucleation Application of standard nucleation theory" to the problem of void nucleation leads to the following conclusions: 1—Homogeneous nucleation of voids requires a supersaturation ratio (concentration of vacancies in supersaturated to that in saturated solution) of 400 for a reasonable surface energy of 1000 erg per cm-and 1.4 for the improbably low surface energy of 10 erg per cm. 2—Heterogeneous nucleation of voids at plane interfaces between two phases requires a supersaturation ratio of 2.5 for a typical contact angle of 145 3-—Void nucleation about a solid particle may be accomplished at a supersaturation ratio of 1.17 for a typical value of work of adhesion? of 60 erg per The work of adhesion is the surface work 10 replace two solid-vauor surfaces by a solid-solid interface. enr ' between an oxide and a metal in the presence of a surface active element such as sulphur. Estimates of the supersaturation ratio at which voids are produced in diffusion experiments yield a maximum of 1.01. Inasmuch as the foregoing mechanisms of void nucleation probably will not operate at this level—too low a surface energy is required—the investigatol. is led to the conclusion that voids must already exist. That is, nucleation of voids probably does not occur. Rather, existing submicroscopic voids grow out to visible size. Already existing voids might be produced during solidification or working. Supercritical sized parlicles which contain cracks may act as heterogeneous void nuclei. Gas pockets may act as void nuclei. Experiments are desired to determine the nature of the heterogeneous void nuclei which grow out to voids in both diffusion and creep experiments. Void Growth Void growth might occur in at least two possible ways, depending upon whether the already existing void nuclei are at grain boundaries or within the grains. In the case of a spherical void far from a crystal boundary, vacancies are generated during creep as a consequence of the migration of suitable dislocation jogs' and are also annihilated at sinks. Under these conditions, a steady-state concentration of vacancies is built up in the crystal, defined by the condition that for any differential volume the rate of generation of vacancies in that volume equals the rate of annihilation of those vacancies." This equality would lead to the development of a gradient of vacancy concentration radially outward from the void surface up to a radius where the vacancy lifetime becomes equal for all directions of vacancy migration. The distance over which this vacancy concentration gradient extends equals about 2vD,T* where D, is the vacancy diffusivity and T:' the vacancy lifetime in a crystal outside the gradient in a zone of constant vacancy concentration. The vacancies generated in the region over which the gradient exists will annihilate more often at the void than elsewhere. Approximately a little over one-half the vacancies generated in the gradient zone will annihilate at the void. Hence, the growth rate of the void is given by on where R is the radius of void in centimeters, is the atomic volume, and R is the rate of generation of vacancies, number per centimeter" per second. R D and T* may be estimated in terms of other physical parameters." In particular, R = n.j e/b [3] where n is the average number of vacancy produc-

Jan 1, 1957

By Robert H. Merrill

This report summarizes the first phase of studies to determine the design and behavior of an unsupported roof in an experimental room in limestone. The selection of a roof horizon and the design of the room were results of an investigation of the geology of the formation, the physical properties of samples from the proposed roof, and calculations from the theory of gravity-loaded beams. The design of the opening, some physical properties of the roof in place, and the behavior of the roof were checked by tests in a full-scale experimental room. The room was instrumented to measure roof deflection, separations in the roof strata, and incipient failure. The dimensions of the room before instrumentation was installed were 10 by 100 feet; the room was widened in successive increments to 40 by 100 feet. Between widening operations periods up to 6 months were allowed to provide a time test of the roof spans. The results of the measurements of deflection and separations showed that the lowest 6-inch layer in the roof became detached as the room was widened. This layer was eventually removed after standing without failure for about 4 months at room dimensions of 40 by 100 feet.

Jan 1, 1957

Unfortunate occurrences resulting in injuries, loss of life, and destruction of property by explosion, fire, and other mishaps during shaft sinking in the past few years have focused the attention of the Bureau of Mines on the need for safety standards for such operations. Several States have some rules and regulations applicable to local conditions, and several Bureau publications (including some now out of print) cover the hazards that may be encountered in shaft sinking. Certain requirements of the Federal Mine Safety Code and Federal Coal Mine Safety Act may be applied, but there are no definite, uniform standards that will guide those desiring to sink a shaft safely and bring about uniform safety inspections.

Jan 1, 1957

By J. R. Nettle

A method has been developed in the laboratory for successfully electro-refining titanium metal. Refining is accomplished in e fused-salt electrolyte using offgrade metal as the anode and collecting the purified metal at the cathode. The characteristics and requirements of the various alkali chlorides tested as electrolytes are discussed in relation to relative ease of purification and serviceability. The various types of cells designed and tested for electrorefining are illustrated and their method of operation discussed. The individual advantage of each cell and the purpose for which it was designed are reviewed. The magnitude of the cathode current density was found to depend largely upon the quantity of soluble titanium chloride in the electrolyte. The physical condition of the anode also greatly affected the cathode current density.

Jan 1, 1957

By R. L. Fullman, J. W. Cahn

A method is derived for obtaining the distribution of sphere diameters and plate thicknesses (or pearlite spacings) from size distribution functions obtained along randomly oriented lines. The method described offers several advantages over existing methods. IT is often of interest to measure not only the average particle size but also the distribution in sizes of particles dispersed in an opaque material, such as an alloy. Particles of a single size will exhibit a range of apparent sizes on the plane of polish. If the sample contains a distribution of particle sizes, the distribution of observed sizes on the plane of polish is related to the distribution of actual particle sizes by an integral equation, For example, a distribution of sphere sizes, N(r),

Jan 1, 1957

By Jesse A. Miller

ALTHOUGH the element titanium was discovered by William Gregor in 1790, over a hundred years passed before it was put to commercial use. The first commercial application of titanium was as an alloy additive to iron and steel, and the first ferroalloys were produced domestically in 1906. Titanium pigments were developed somewhat later and have been produced in the United States since 1918. The use of titaniferous material in welding-rod coatings first gained acceptance ill the mid-30's. The metal titanium has only had commercial importance since 1948; domestic production for that year was 10 tons. The relative importance of these major uses of titanium in various forms may he gaged by the consumption of titanium dioxide (Ti02) for these purposes in 1954. Of a total of 440,000 short tons of Ti02 consumed in 1954, 95 percent of the total was consumed for pigments; 2 percent for welding-rod coatings; 1 percent for non-titanium-base alloys and carbide; and 2 percent for miscellaneous uses. The titanium-metal industry is in its infancy, but it has more than doubled its output every year from 1948 to 1954, reaching 5,370 short tons in 1954.

Jan 1, 1957

With the sinking of the No. 3 Shaft at North Broken Hill Limited, it was necessary to construct adjacent to the shaft a new changehouse for mining and surface personnel.It was also probable that as the older sections of the North and British leases were worked out, all employees at present working in these sections would be transferred to the No. 3 Shaft area. This could ultimately result in all personnel employed by North Broken Hill Limited being concentrated in this area, requiring the construction of new administration offices, workshops, mine store, etc., also in this area.

Jan 1, 1957

Six years ago it was my responsibility to give the presidential address, and now that privilege has come my way again. On that occasion we were gathered atWhyalla and I took the opportunity of putting before members some observations on the problems we then faced in Australia, and some gains we had been able to chalk up during those early postwar years. You may recall that we were then just beginning to emerge from the difficulties of postwar reconstructions - of fuel and power shortages, and a grossly inadequate manpower for the tasks facing us. The expansion of manufacturing industry in Australia greatly stimulated by wartime activities, and by the postwar developments of many institutions - ran ahead of the supporting services and of the supply of labour to do thejobs. For many industries this unfortunate state of affairs had meant operating at rates well below their installed capacities and therefore levels of output insufficient for Australia's rapidly growing needs. When I last spoke to you these problems were still with us, though their intensity was beginning to lessen as a result of vigorous efforts by industry and governments to reduce them. But I must confess that my thoughts on that occasion were full of those problems and of the effect they were having on the iron and steel industry of this country-of the coal shortage, the labour shortage, and the many other difficulties we were then faced with - and all at a time when the stepping up of our postwar expansion programme was of vital concern to all of us.What a different picture it is six years later! How greatly has the scene changed for the better. In 1951 Australia's postwar immigration programme was only in...

Jan 1, 1957