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By M. G. Zabetakis

This publication describes an investigation conducted by the Federal Bureau of Mines regarding the cause of an explosion of a dephlegmator or fractionating column at the Cities Service Oil Company Refinery, Ponca City, Okla., January 22, 1959. The column was that used with the refinery's No.1 Dubbs Coker. The explosion caused the death of an employee of the refinery and resulted in extensive damage to the refinery and to nearby property. The Bureau's study of the explosion began January 26.

Jan 1, 1960

Although alternating-current (a.-c.) power systems and equipment have been used in coal mining for many years, most mines in the United States are powered mainly by direct current (d.-c.). There are several logical reasons for this, but the use of d.-c, equipment is, in most instances, a direct outgrowth of the original practice of using such power for haulage systems. For traction equipment such as the electric trolley locomotive the d.-c. motor has ideal operating characteristics, and thus it has been widely used for haulage locomotive service. The first efforts at electrification of coal mines started with the haulage system and from there branched out to include the many types of electrically powered mining machinery used in the industry today.

Jan 1, 1960

By Carl Rampacek

Laboratory and small-scale continuous pilot-plant investigations made at the Tucson Metallurgy Research Laboratory of the Bureau of Mines have demonstrated that the copper segregation process is applicable to the treatment of oxidized and mixed oxide-sulfide copper ores regardless of the gangue constituents. The process comprises heating the ore to a temperature of 750° C. with small quantities- of sodim chloride and coke to produce metallic copper, which then is recovered by flotation. Tests were made on' 23 copper ores of different types containing 0.8 to 5 percent Cu, .The copper recoveries ranged from 73 to 96 percent in concentrates assaying 10 to 62 percent Cu, depending on the grade and type of ore, The direct operating cost for a 1,000-ton-per-day furnace and flotation plant is estimated at about- $3 per ton of ore.

Jan 1, 1960

By W. Gibson Jaworek

It has become apparent in recent years to everyone intimately concerned with the future of the American fuels industries that the growth in demand for energy has become a topic receiving considerable attention, and that investigators are leaning more and more toward a mathematical approach to deduce what pattern that growth will follow. Though coal has been included by necessity In all-studies of future energy markets, it has not been the subject of mathematical analysis or description as frequently as has been total energy or some of the other fuels, particularly petroleum, It is the intent in this particular paper, to subject bituminous coal consumption to a preliminary mathematical scrutiny which can lead to a more logical estimation of the general level of bituminous coal consumption for the next decade, as well as formulating an approach toward describing how coal consumption may vary as the result of the annual variations in activity in the United States, economy, The approach utilized is more sophisticated than the mere projection of the historical trend of bituminous coal consumption. Such a projection would lead to a continuation of the recent decline, indicating that coal consumption would reach zero some thirty years from now. On the other hand, the mathematical analysis described here is a relatively simple, straightforward approach and- is not intended to represent the-ultimate in mathematical economic analysis as now practiced, It is hoped that this will contribute to our knowledge of bituminous coal markets. Even more, it is hoped that it will help arouse a greater interestin utilizing mathematical and statistical analysis when studying the bituminous coal industry. - Since this is a preliminary study, comments and criticisms are anticipated.

Jan 1, 1960

By F. R. Cattoir

The Federal Bureau of Mines refined chromium from an aqueous electrolytic process in molten sodium chloride-chromium chloride electrolytes. Oxygen and nitrogen contents were reduced by a factor of 10 to 40, but most other impurities were little changed. The product usually contained a little more iron than the feed. Since iron was entering the bath from the iron pot and the graphite liner at a nearly constant rate, contamination of the chromium deposits by it was more serious at low currents and deposition rates. A few runs in an iron cell with a nickel liner yielded chromium containing one half as much iron as the feed, but up to 1.5 pct. nickel. In all cases the anode feed lay in the bottom of the container, which itself was used as the anode connection. With a 12-in. cell, variations in applied voltage from 0.05 to 1.5, in current from less than 10 to over 100 a., and in initial cathode current densities from less than 100 to over 2,000 a./sq.ft. had little or no effect upon the analysis of the metal produced) except for iron content. Changes in bath analysis from 3 to 11 pct. chromium were also without effect. These changes did bring about large differences in the physical forms of the crystals obtained. The thick heavy crystals produced at low voltage and current contained voids which made them difficult to leach free of chlorides. Easiest to leach were the thin leaf-like crystals obtained at around 1 v.

Jan 1, 1960

By Victor Erickson

ECONOMIC recovery, which began in 1958, carried through into 1959 but was somewhat retarded by the 116-day steel strike beginning in July 1959. Recovery and economic growth increased production and consumption of mineral fuels 3 percent above 1958. The increase was accomplished despite a drop of 26 percent in coal exports. Prices remained constant during the year so that the value of production and consumption also increased 3 percent over 1958. Stocks in the hands of producers at yearend were little changed from the supply at the beginning of the year. Employment in the field of mineral fuels decreased 6.4 percent from 1958. Average hourly earnings were up 7 percent, and average hours worked were up 5 percent, with the result that weekly earnings gained 11.8 percent. Internal freight rates were relatively constant, but ocean tanker rates declined both in 1958 and 1959 from the high rates charged during the Suez crisis. The index of major input expenses decreased for anthracite, held constant for bituminous coal, and increased for petroleum. The index of labor cost per dollar of product and per ton of product declined again in 1959 to a new low in anthracite and bituminous-coal mining industries.

Jan 1, 1960

By R. F. Rolsten

VAN Arkel 1 prepared ductile tantalum by the thermal decompoiition of tantalum pentachloride on a resistively heated wire (2000° C) in an evacuated bulb maintained at 100°C. Burgers and Basart2'3 observed the formation of a mixture of tantalum carbide and free metal when a carbon deposition base was used. campbel14 suggested the thermal decomposition of the iodide if a lower decomposition tem- perature was desired. To date, the details for preparing high-purity iodide tantalum have not been disclosed. EXPERIMENTAL The tantalum to be purified was symmetrically placed around the clear quartz deposition surface centrally located within a 64 mm cylindrical Vycor bulb. The deposition vessel usually employed5 was modified6 by incorporating a reentrant fin,mer in place of the customary metal filament in the head

Jan 1, 1960

By R. J. Leary

A small electronic digital computer employing punched cards has been used to facilitate the solution of a variety of problems in Bureau of Mines pyrometallurgical research. In this work the computer has been found to be economical for solving both simple problems that occur repeatedly and those involving complex or iterative calculations. Each of these classes of problems and their respective solutions are described. These small computers can be used effectively by researchers when they work in consultation with a computer specialist. Close team work produces the required solutions in less time, and, oftentimes, in a more useful form. Participation in programming by researchers develops in them a skill for evaluating the suitability of problems for electronic computing.

Jan 1, 1960

Yallourn brown coal and its characteristics have been the subject of innumerable papers and discussions. The Lurgi process adopted for the production of Towns gas by the gasification of brown coal has been described frequently in literature.The application of the Lurgi process for the gasification of Yallourn briquettes has naturally lead to some unexpected problems. Rather than attempt to review the whole field of experience gained in the first two years of operation of the gasification plant at Morwell, this paper attempts to describe two problems encountered, peculiar to the fuel used, and the steps taken in overcoming them.THE PROCESS AND PLANTTo clarify the conditions surrounding the problems, it is necessary to briefly describe the gasification and cooling processes and plant.Brown coal briquettes are gasified in a pressure generator, using a mixture of steam and oxygen as a gasifying medium. Crude gas produced in the generator is washed and cooled in the waste heat boiler and coolers. Figure 1 shows an arrangement of the generator and coolers. The gasifying medium enters the generator through a hollow shaft in the base. This shaft drives the grate, which has three purposes: (a) to distribute the gasifying medium into the fuel bed; (b) to extract the ash from the fuel bed; (c) to support the fuel bed.Briquettes enter the top of the generator through the coal lock chamber and the fuel bed is maintained at a reasonably...

Jan 1, 1960

By J. W. Eckerd

The crushing of chestnut-size (1-5/8 by 13/16 inch) Pennsylvania anthracite in four commercial crushers (impact) jaw) hammer-mill) and gyratory types) was studied by the Bureau of Mines to determine which could produce the largest proportions of buckwheat Nos. 1 and 2 sizes (9/16 by 3/16 inch). Single pass dry and wet crushing techniques and the effect of stage crushing were evaluated. Calculations were made to show the effect of closed-circuit reduction on production rates and yield of the various sizes. The data show that the gyratory crushers produced the greatest percentage of the desired sizes. A ring-type hammer mill produced the greatest tonnage of buckwheat No.1 and rice (14.9 tons per hr.) during dry grinding tests) but the yield of these sizes was only about 55 percent) as compared with 62 to 70 percent for the gyratory crushers. The impact and jaw crushers produced the smallest amount of buckwheat and rice and the largest quantity of oversize material.

Jan 1, 1960

By J. W. H. Clare

An equilibrium isotherm at 550°C is given for ternary alloys rich in aluminum containing 0 to 15 wt pct Cr and 0 to 20 wt pct Mn. Phases encountered are: aluminum solid solution; stable temary compound G; and MnAl8,. In addition, a limited number of alloys were annealed at 450°C to check for differences from the 550°C isotherm. These experiments limited the composition of the G phase at 550°C and further experiments established that the G Dhase is not stable above 590 ± 1 °C. RAYNOR and Little1 established several equilibrium isotherms using aluminum-rich alloys containing up to 5 pct of the elements chromium and manganese. These isotherms showed that, in addition to an a solid solution and the two binary intermediate compounds 8 and MnAl6, a stable ternary compound ex-isted in the system. This phase was called the G phase because of its ghostly appearance in micro-sections. Little, Raynor, and Hume-Rothery2 found a similar phase in binary aluminum-manganese alloys and, as a result of their experiments, concluded that the G phase was a metastable phase existing in the aluminum-manganese system. This phase was stabilized by the addition of chromium. The constitutional work of Raynor and Little,' although showing the existence of the G phase in the aluminum-chromium-manganese system, did not establish precisely the composition limits of the phase or the temperature above which the phase became unstable and disappeared from the system. The work described in this paper was undertaken to provide this information. An examination of the previous work' showed that an isotherm at 550°C would provide the required data regarding composition in the shortest possible time, as the (a + G) phase field narrows considerably at higher temperatures. The same work showed that the G phase ceased to exist between 580° and 595°C. A more precise estimate of the transformation temperature would therefore be obtained by annealing selected alloys at successively higher temperatures beginning at 580°C. EXPERIMENTAL PROCEDURE 1) Materials Used—The experimental alloys were prepared from four master alloys containing 15.00 w pct Cr, 15.28 wt pct Cr, 19.80 wt pct Mn, and 19.38 wt pct Mn which were made from super-purity aluminum, electrolytic chromium, and electrolytic manganese. The aluminum was of 99.996 pct purity, the principal impurities being copper, iron, and silicon. The chromium and manganese were 99.9 pct pure, the principal impurities being antimony, calcium, and magnesium. 2) Preparation of the Experimental Alloys—The alloys were prepared in 20-g quantities by melting together the requisite amounts of master alloy and aluminum in an alumina-lined crucible and, after thorough stirring with an alumina rod, cast into a cold copper mold to give ingots 1/4 in. in diam and 3 in. in length.

Jan 1, 1960

By J. W. MacDonald

Two coal mine shafts recently completed in Franklin County, Ill., afford experience and accomplishment to warrant review, These shafts provide access to a tract with a potential recovery of one hundred million tons. This work provided the initial sinking by other than a contractor's organization since 1918. Four additional shafts required during the interim were sunk under contract arrangement with others. Supervisory contact and inspection afforded experience to govern planning and conduct of the recent work.

Jan 1, 1960

By E. Morrice

The metallurgical laboratory data developed in this study indicate an improved electrowinning process for producing higher purity cerium ingot. A typical sample of the Reno electrocerium contains 99.9 weight-percent cerium and the following impurities: Total other rare-earth elements, less than 0.04 percent; iron not detected; silicon and aluminum, less than 0.02 percent each; calcium plus magnesium, less than 0.01 percent; carbon, 0.01 percent; oxygen, 0.002 percent; hydrogen, 0.0003 percent; and nitrogen, 0.0015 percent.

Jan 1, 1960

By Paul W. McGann

This paper presents a methodology for long-range studies of petroleum supply, to meet projected demands, that involves modifications of procedures used previously. This paper continues a series of papers on this general topic in the AIME, the most elaborate recent one being that by Warren Davis given in February 1958. The procedures considered here begin with the assumption that the governmental framework of regulations and taxes remains fixed- but that price changes. After .these procedures have been reviewed, the effects of changing certain governmental controls, will be considered in order to judge their potential effects on future supply. This is an essential step because controls cannot be expected to' remain static in a situation changing as much as the petroleum. industry and because such changes are within-the scope of alternative ways of adjusting to impending problems. The first procedure begins with: a) trends in drilling success, b) relation between field income from oil and gas and footage drilled, c) declines in capacity from production, d) trends in capacity of new and producing wells, e) all monetary values are in constant 1958 dollars, and f) target amounts of domestic crude petroleum production. 'From these components projections are obtained of: 1) numbers of future producing wells required, 2) footage drilled, 3) new wells drilled, 4) crude oil found, 5) capacity of producing wells, 6) completion costs, 7) finding costs, 8) production costs, and 9) average wellhead crude oil price consistent with the footage-field income relationship.

Jan 1, 1960

By Walter Kawa

In connection with its research in producing synthetic liquid fuels from coal, the Federal Bureau of Mines studied reactions of iron and iron compounds with hydrogen and hydrogen sulfide in batch autoclaves. The Bureau hoped to gain indirect evidence regarding the chemical changes that iron catalysts undergo when they are used in the hydrogenation of coal. The information obtained may be helpful in identifying the active form or forms of iron catalysts. At 450° C., with hydrogen at hundreds of atmospheres and hydrogen sulfide at 1 or 2 atmospheres, the thermodynamically stable form of iron is ferrous sulfide in the case of the metal, magnetite, ferric oxide, ferrous sulfate, ferrous oxalate, or the chlorides of iron. However, complete conversion to ferrous sulfide was not achieved at temperatures of 400° to 500° C. for kinetic reasons. Extensive sulfiding of iron, magnetite, ferric oxide, and ferrous oxalate occurred below 400° C., and some conversion of ferrous sulfate to ferrous sulfide occurred at 400° C. In the hydrogenation of coal, ferrous sulfide is the form of iron likely to be available for heterogeneous catalysis when starting with the metal, oxide, sulfate, or oxalate.

Jan 1, 1960

By Ben Habermann

"The object of the work described in this paper was to increase the understanding of the relation that capillary pressure of a rock, hydro-dynamics, and accumulation of oil in stratigraphie traps have to one an-other. The hydrodynamic oil-water tilt equation is derived by considering the two vector gradients involved: (1) buoyancy of oil in water and (2) hydraulic gradient.Recent theories show the necessity for oil to have a continuons phase in the reservoir rock in order to mi-grate; this fact applies to hydro-static as well as to hydrodynamic conditions. Hydrostatically, the displacement pressure of the rock deter-mines the amount of oil that can be trapped behind a permeability barrier. If the buoyancy of oil in water exceeds the displacement pressure, oil will migrate up-dip; an oil trap will be formed where displacement pressure is greater.In stratigraphie traps the pressure drop caused by moving water is positive when its direction is down-dip, helping accumulation; and it is negative when its direction is up-dip, forcing the oil into the tighter section of the reservoir. Theoretically, pro-vided we have data such as: (1) the displacement pressure of an up-dip permeability pinchout, (2) density difference between the oil and water in place, and (3) the direction and magnitude of the hydrodynamic gradient (if any), the possible extent of a stratigraphie oil accumulation down-dip can be predicted.To test the above theory sample cores from three wells in the Denver Basin were analyzed and the oil column that could be held under hydro-static conditions was calculated. After the hydrodynamic influence was considered, the results were compared with actual field data.The significant fact shown by this investigation is that the calculated oil column in one reservoir very closely approximates the actual extent of the oil column in a well. Also in accordance with the theory, the capillary pressure caused by the buoyancy of the oil column exceeded the measured displacement pressure on core samples from another productive field. For very tight shaly sand and questionable oil shows, the interpretation of data is very critical, as shown by experiments on core samples from a third field."

Jan 1, 1960

By R. V. Higgins

As part of a study of application of the Buckley-Leverett method to an analysis of oil-reservoir performance covering a wide range of relative permeabilities and oil saturations, a method has been devised for quickly deter-mining average water saturation at breakthrough from relative permeability data. The base for the relative permeability used in the report is either the permeability to air or the effective permeability to oil at the irreducible water saturation. The permeability to air also was used because of the large backlog of air permeabilities available to reservoir engineers. The basic data were calculated by an electronic computer and are presented in a single graph from which the point of breakthrough may be obtained. In this study the water saturation at the beginning of the depletion is the connate or interstitial or irreducible water saturation. These water saturations are considered to be synonymous and to have a practical value.

Jan 1, 1960

By J. T. McGrath, G. B. Craig

Tensile tests on aluminum single crystals, grown from the melt, revealed that the yield stress of these crystals was raised as the amount of striation substructure was increased. The number of striation-type boundaries was varied by changing the rate of growth of the crystals. The results are interpreted in terns of a blockage of dislocation movement by striation boundaries. IMPERFECTIONS are known to have a large effect on the mechanical properties of metals. Teghtsoonian and Chalmers 1 studied a block or striation-type substructure in tin and found that the formation of the striations depended upon rate of crystal growth and orientation. They found that the angular misorienta-tion between neighboring striations varied between 15 min and 5 deg. Atwater and chalmers2 investigated striations in tin and lead, and found that purity was another factor which influenced their formation. There was a limiting purity above which the striations were straight and regular. There is little information in the literature concerning how substructures in melt-grown crystals affect strength. washburn3 introduced small-angle boundaries into zinc by a shear process and found a subsequent increase in yield stress which he attributed to the presence of these boundaries. Lauriente and pond4 found the critical resolved shear stress in aluminium crystals grown from the melt, to increase with etch pit density. The etch pits were used as an indication of growth imperfections. In Hibbard's5 work on lineage structure in copper crystals grown from the melt, he tested one crystal containing interlineage boundaries, and found a 50 pct increase in the critical resolved shear stress. Fleischer and Chalmers6, in a recent paper, mention briefly that, in the production of aluminium crystals from the melt when the growth rate was raised from 1.2 to 18 cm per hr, the yield stress increased 50 pct. They felt that the increase in yield stress with rate of growth might be attributed to a higher concentration of impurities in the gage length and also might be affected by the increased number of small-angle boundaries (striations). The present investigation was undertaken to determine the effect of the striation substructure on the strength of aluminum single crystals. EXPERIMENTAL PROCEDURE Aluminum single crystals of 99.9992 purity were grown from the melt using a technique described by Chalmers.7 The growth rate was varied from 0.6 to 20 mm per min, thus producing crystals with varying numbers of striation boundaries. To avoid prior deformation, the crystals were chemically cut to the desired length with a saturated solution of cupric chloride. They were then annealed at 580°C for 24 hr and allowed to cool slowly in the furnace. Finally, the specimens were electropolished using an electrolyte of 5 parts ethyl alcohol and 1 part perchloric acid. Each specimen was approximately 5 in. in length and 0.125 sq in. in cross section. The average orientations of the 5 series of crystals studied are shown on the stereographic projection of Fig. 1. The crystals were strained approximately 2 pct in a soft tensile machine. The strain sensitivity was 3.6 x 10-4 cm over a 5-cm gage length.

Jan 1, 1960

By Henry H. Ginsberg

The Federal Bureau of Mines made pilot plant investigations of the process requirements necessary to produce heavy fuel oil by the liquid-phase hydrogenation of bituminous coal. The investigation was carried out in three separate series of experiments. The first series studied the effect of temperature and contact time on product distribution at 3,500 p.s.i.g. and 420° to 480° C. in the presence of 0.1 wt.-pct../ stannous sulfide plus 0.05 wt.-pct. iodoform based on gross coal. As a result of increased contact times and temperatures, the conversion-6/ and yield of hydrocarbon gas increased, the viscosity of product oil decreased, and elimination of oxygen, nitrogen, and sulfur from coal increased. The yield of oil did not indicate any definite trend with changes in temperature and contact time. The yield of oil ranged from 76 to 85 pct. for Pittsburgh coal and from 60 to 85 pct. for Rock Springs coal. Asphaltenes in the product oil ranged from 17 to 38 pct. of the total oil for Pittsburgh coal and from 12 to 22 pct. for Rock Springs coal. Fuel oils meeting Bunker C or American Society for Testing Materials (ASTM) Grade 6 specifications were produced with Rock Springs coal at 0.2- to 1.0-hr. contact time and 440° to 480° C. and with Pittsburgh coal at 0.3- to 1.0-hr. contact time and 420° to 460° C. In the second series of experiments tin, nickel, iron, and zinc were evaluated as catalysts for the hydrogenation of Rock Springs coal to heavy fuel oil at 3,500 p.s.i.g. and 460° C. Using the apparent conversion of coal as criterion of catalyst activity, at a contact time of 0.45 hr. tin was the most effective catalyst; nickel and iron were nearly as effective, but the use of zinc resulted in much lower conversion. When the contact time was increased to 0.80 hr., the apparent conversion of coal was essentially the same for each of the catalysts. When the yield of oil boiling below 3550 C. was used as criterion of catalyst activity, at 0.45 hr. the order of activity was tin, iron, nickel, and zinc; at 0.80 hr. tin was far superior and the others were essentially equal. The product oils contained from 8 to 20 pct. asphaltenes.

Jan 1, 1960

By A. H. Willis

In this paper the results of an exploratory study conducted by personnel of the Knolls Atomic Power Laboratory on 18.6, 22, and 40 wt pct uranium-zirconium alloy will be presented. LARGE power output and long life or endurance from small, compact nuclear reactors require the use of enriched uranium for a fuel material. However, the ability to remove heat from the element, the tolerable fission product concentration, or some physical limitation of the system can limit the allowable fuel enrichment, or the volume of the fuel. In such an event, the fuel-element designer must find a suitable diluent for the uranium. Zirconium is an attractive material for such a purpose as it has good nuclear properties and a low absorption cross section. Because it has a good corrosion resistance in water, zirconium is a suitable cladding and the uranium-zirconium alloy makes a good core material. The alloy has a high thermal conductivity, a low elastic modulus, and a low thermal-expansion coefficient, all of which tend to minimize the thermal stresses in the core. Furthermore, the unirradiated material is reasonably ductile and has adequate strength. DESCRIPTION OF SAMPLES Two types of cylindrical samples were used in this study 1) short, 1/2-to 1-in.-long samples to test the irradiation stability of the alloy and 2) 2-ft-long samples to investigate the resistance of an element to longitudinal deformation. Composite samples having 0.060-to 0.140-in. core diameters and clad with a 0.010-in. thick zirconium jacket were fabricated by coextrusion and by hydrostatic pressure bonding of the cladding to the preformed core material. Both fabrication processes produced the uniform metallurgical core-to-cladding bond which was felt necessary to minimize the uncertainty of the central core temperature. Both consumable-arc and induction-melting techniques were used to melt the uranium-sponge zirconium core alloy. Since a graphite crucible was used in induction-melting this alloy contained more carbon impurity, which resulted in a finer grain size than the arc-melted alloy. The core to cladding interface was uniform in elements coextruded from the fine-grain, induction-melted core material, while those elements fabricated using arc-melted core material had very irregular interfaces because of the coarser grain size. Both cold-worked and heat-treated fuel materials were irradiation tested. Cold-worked alloys were swaged to about a 5 pct final reduction in area without subsequent annealing. The heat-treated alloys were heated to 800°C, held at temperature for 15 min and furnace-cooled to about room temperature. This

Jan 1, 1960