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By V. F. Parry

The object of this report is to present certain pertinent data on the physical and chemical properties of South Arcot lignite and to present the results of several special tests to show how the raw lignite can be upgraded to superior fuels for certain special uses. The Bureau of Mines Branch of Coal Technology laboratories at Denver have advocated the drying and carbonization of all low-rank fuels for special uses and have introduced and developed new techniques for upgrading and refining noncoking coals. Application of these techniques to the South Arcot lignites was the object of the investigation, and this report presents significant data necessary for planning a fuel program based on utilization of dried and carbonized dusts. In general, the South Arcot lignite is similar in chemical properties to the high-moisture lignites found in the United States and has some physical properties similar to Australian brown coals. The samples submitted for test had lost moisture before delivery to the laboratory, and it has been necessary to estimate the analysis of the lignite in place in the mine. Various observations made in India by qualified technicians indicate that the bed moisture content of the entire seam is in the range of 54 to 56 percent. For estimating purposes in this report, the bed moisture content has been taken as 56 percent and the ash content of the fresh coal as 2.5 percent. The average analysis estimated for the as-mined lignite is: [Moisture percent 56.0 Volatile matter do.22.0 Fixed carbon do.19.5 Ash do.2.5 Heating value B.t.u. per lb. 4,890]

Jan 1, 1957

By O. C. Blade

This report on the properties of aviation gasolines and aviation jet fuels produced in the United States during 1956 was made under a cooperative agreement between the American Petroleum Institute and the Bureau of Mines of the United States Department of the Interior. Analytical data are presented for 120 samples of aviation gasoline and for 38 samples of aviation jet fuel. The analyses were made on samples typical of the manufacturers' 1956 production in their laboratories and the results submitted to the Bureau of Mines for compilation. The products of 20 manufacturers of aviation gasolines and of 17 producers of aviation jet fuels are represented.

Jan 1, 1957

By L. E. Djingheuzian

IN 1953, Lewis (1) published an article which brought forth a great amount of discussion by grinding engineers. In his contribution to discussion the present writer (2) suggested that, for the most efficient performance of a ball mill, there must be a .definite relationship between Cn, per cent critical speed, and V p, per cent mill volume occupied by the ball charge. Later, he ( 3) was able to publish some grinding data from Wright-Hargreaves milly which appeared to bear out this contention. It is with this view to establishing a fundamental relationship between Cn and Vp that the idea of this Forum was conceived. Accordingly, a questionnaire was prepared and copies of it were mailed to over eighty Canadian mill operators. This questionnaire did not include a question on dilution on the assumption that each mill operator was using the most efficient dilution for his operation, nor was a question on efficiency of classification included since it was thought that the inclusion of efficiency of dassification in the questionnaire at this preliminary stage might render the forum discussion,. while everybody was trying to find his bearings, too unwieldy. However, it is evident that, as discussions develop, this forum will have to define a uniform method for establishing most efficient classification in grinding circuits

Jan 1, 1957

By Cyril Wells, Paul E. Busby, Donald P. Hart

EARLY workers in the field have established that the diffusion of nitrogen follows normal diffusion laws. Concentration-penetration data from layer analyses of reasonably pure iron specimens nitrided in an atmosphere of CO-NH, are given in the literature,' and were utilized to calculate diffusion constants for nitrogen. The diffusion of nitrogen in y-iron may be represented approximately by the equation D - 1.07x10-' e-:".'m'"'r The diflusion coefficients, D, given by this relation represent mean values, since carburization occurred simultaneously with nitriding. The rate of diffusion in a-iron has been determined from calculations based on data obtained by measuring the internal friction of samples at each of several frequencies and temperatures.' The expression for the diffusion of nitrogen in a-iron derived from these experiments is D= 1.4x10-1 e-it tudent Increasing carbon content decreases the diffusion of nitrogen in a-iron.3 Oxygen, either dissolved or combined, has been shown' to exert a marked influence on the diffusion of nitrogen from a nitriding atmosphere. D values increase rapidly with increasing amount of dissolved oxide in the metal, but diffusion is completely inhibited if preliminary oxidation has produced the slightest trace of iron oxide on the surface. Diffusion coefficients have also been calculated from permeability and solubility data,' but these values are of questionable accuracy since the boundary conditions assumed may not actually exist. Experimental Method The method selected for determining the diffusion coefficient of nitrogen in a-iron in the present investigation was the so-called fractional saturation method. This method consists of heating the specimen in an atmosphere of H2-NH8 mixtures of known composition for a predetermined time. Following this treatment, the specimen is analyzed for nitrogen; and the diffusion coefficient is calculated from a known relationship of the fractional saturation, time of diffusion, and dimensions of the specimen. This relation is based on a solution of Fick's second law and assumes that the surface of the specimen immediately reaches a given concentration which remains constant during the diffusion anneal. Tabular solutions are available4-5 and provide the relationship between fractional saturation and the quantity \/Dt /a, where D is the diffusion coefficient in cm2 per sec, t is the time of the diffusion anneal in seconds, and a, in the present experiments, is the half-thickness of the slab specimen in cm. The method is adequately discussed elsewhere.9-10 Material The material for this study consisted of 3/32 in. thick (0.24 cm) carbonyl iron plate. The major impurities in this iron are oxygen and carbon, which are readily removed by long time high temperature treatment in an atmosphere of purified hydrogen. In order to reduce the diffusion anneal time for saturation runs, some of this material was rolled to a thickness of 0.015 in. (0.038 cm) prior to the hydrogen treatment. Hydrogen treatments were carried out in a hydrogen-purified Armco iron tube heated in a global

Jan 1, 1957

By H. F. Yancey

The Baum-type jig used so widely to clean bituminous coals has not been adopted for anthracite. If proved suitable for anthracite, its use might lower preparation costs in some plants. Cleaning trials on a Pennsylvania anthracite in a laboratory-size Baum-type jig were undertaken by the Bureau of Mines to provide indicative information that would be helpful in determining whether the cost of a full-scale installation would be justified. Clean coal surpassing standard anthracite specifications was obtained in all sizes from Stove through No. 5 Buckwheat. Recovery effi¬ciencies were acceptable down to 3/16-inch size, but there was excessive loss of coal in the finer sizes. Thus the fine refuse produced in a commercial plant might re¬quire retreatment. A comparative cleaning trial in a dense-medium pilot plant provided a recovery efficiency only l percent higher than obtained in jigging.

Jan 1, 1957

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