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By P. T. Gallagher, W. A. Oates

THE partial excess entropy of interstitial solutes in metals, SXS , has usually been interpreted as being principally vibrational ever since the initial statistical treatment of hydrogen in metals by Fowler and Smith-ells. The vibrational entropy is considered being due to the optical modes of the light interstitial atom. Little attention has been given to the magnitudes of the values of SXS'. Leiser and Witte2 and Ebisuzaki and O'Keeffe3 have noted that for hydrogen in metals Si is approximately constant for different metals. On the other hand if it is assumed that the interstitial solute is an isotopic defect then, as shown by McLellan, SXS should vary from metal to metal as follows: where S is the standard entropy of the solvent and Mi, M, are the masses of the interstitial and solvent atoms. respectively. Fair agreement with this equation was found for oxygen in silver and nitrogen in iron4 and for carbon in iron.= Ln a subsequent analysis of metal- hdrogen systems McLellan' found a variation of $' from metal to metal but not in a manner expected from the isotopic impurity equation. However, a possible correlation between the energy of solution, Ei, and sf was noted. Similar correlations have been noted for certain dilute substitutional solid Solutions 7, 8 and recently Kubaschewski 9 has demonstrated a correlation between integral heats and ex-

Jan 1, 1970

Jan 1, 1962

By J. J. Calaman, D. H. Fleming

DURING 1950 the jet-piercing process was used commercially in the piercing of primary blast-holes in magnetic taconite at the preliminary taconite plant of .the Erie Mining Co., Aurora, Minn. The Erie Mining Co. purchased a jet-piercing machine and associated equipment in 1949, and the machine has been in operation since its installation in the summer of that year. An overall view of the pit with the JPM-1 jet-piercing machine in operation is shown in Fig. 1. During three months of 1949 and continuously since February 1950, production piercing took place under all pit conditions. By the end of October 1950, a total of 15,000 linear ft of hole had been pierced in an open pit handling an average of 1200 to 1800 tons of crude a day in one 8-hr shift. While it is recognized that this output does not approach the millions of tons a year planned for the developing Minnesota taconite projects, the machine as a unit has been operating under conditions probably more adverse than those that eventually will be encountered in the large operations. This pilot operation has permitted evaluation of the piercing problem in the full-scale taconite plant. This paper describes jet-piercing process funda- mentals, important features of the latest jet-piercing burners and machine, actual piercing results obtained, and new developments that give promise of materially increasing overall process efficiency. To produce the blasthole, jet-piercing utilizes thermal energy, as contrasted with the application of mechanical energy in churn drills and jackham-mers. The heart of the process may be termed a tailored flame produced by a rocket-type burner, thermodynamically similar in every respect to that of the giant rockets being developed for military purposes. The heat release in the combustion chamber of the burner is about 50x10' Btu per cu ft per hr as compared with 5x10' for most modern steam generators.* Combustion of liquid petroleum fuels (kerosine, diesel oil, or No. 2 fuel oil) with gaseous oxygen in the burner chamber at pressures of 100 to 200 psi results in temperatures of about 4300°F. Expansion of the hot combustion gases through divergent nozzles produces high-temperature supersonic jets having measured velocities of about 6000 fps. Impinging the flame jets on rock causes a thin surface layer to expand and break away from the base as a result of the thermally induced stresses. This spalling action is aided further in chert and quartzite by the 0.82 pct volume change resulting from the 6 to p quartz inversion at 1066"F.t The dynamic action of the jets whisks the spalled rock

Jan 1, 1952

By C. H. Mathewson, Kent R. Van Horn

Copper and the copper-base solid solutions readily form twin crystals when plastically deformed at a suitably elevated temperature or annealed after cold deformation. In fact, no feature of the microstructure of these materials is more prominent or characteristic than these straight-sided bands or simple lines of division which sometimes come from groups of thin polysynthetic lamellae, penetrating part way or wholly through the parent grain substance, but often divide the grain into a few or perhaps only two crystallographically related parts. Nearly always the bands as seen in the usual microscopic examination of a specimen come into vivid contrast with the adjacent crystalline material owing to the inherent difference in orientation. Bands which under special conditions of orientation cannot be seen with vertically incident light are often visible under oblique illumination and, when this fails, contrasting effects usually may be obtained by using polarized light. There is no longer any doubt that these synthetic banded structures obtained in the ordinary course of working and annealing are due to twinning of the spinel type which was observed long ago in a number of metals crystallizing in the isometric system.' It has been customary in metallurgical literature to designate these synthetic twins, which grow into prominence during an annealing process, as "annealing twins" without regard to the actual mode of their formation, which is, indeed, obscure and with scant recognition of the fact that prior deformation is essential, no twins having been observed in metal of known unstrained history. This is questionable; especially in view of the fact that in a number of metals and minerals, reorientation into the twin configuration is known to occur as a result of a simple shearing mechanism along the recognized twinning planes and the

Jan 1, 1930

By H. M. St. John

THE melting department is the heart of the foundry. From it clean metal flows to the molding floor, in the right quantity, at the right time and at a sufficiently low cost-or, if not, the foundry fails to thrive. Since it is our purpose here to discuss present-day melting practice in the foundry, it may be well at the start to emphasize the wide differences in foundries and the conditions under which they must operate in order to reach the goal stated in the first paragraph. In every foundry, large or small, jobbing or captive, the same factors must be dealt with but they are of varying consequence and must be dealt with in varying ways in different foundries. Particularly in the nonferrous industry, there is so wide a variation in the composition of alloys used and in the character of castings made that no one type of furnace, nor any one method of operation, can be expected to produce the best results at all times. The present discussion will not attempt to include all nonferrous metals. It is intended to cover only the copper-base alloys in which copper is the dominant element, most of which are commonly known as brass or bronze. The discussion is further limited to the melting of these copper-base alloys for use in sand-casting foundries. Die-casting plants, the brass-rolling mills and certain other metal industries have melting problems peculiar to those industries, which will not be considered here. The following considerations are elemental in all foundries and are listed in what is believed to be the relative order of their present-day importance: I. The melting department must meet the foundry's requirement for dean, fluid metal, of specified composition and purity, at a temperature suitable for the work the foundry has in hand. This is the prime consideration in any foundry, at any time, anywhere. 2. Working conditions surrounding the melting furnaces and attending their use must be good. 3. The cost of molten metal at the mold must be as low as possible. 4. The operating characteristics of the furnaces must be sufficiently flexible, to meet normal variations in foundry requirements. 5. The operation and maintenance of the melting equipment must not require more skill and experience than is available in the particular foundry in question. METAL QUALITY It is not a function of the melting furnace to refine or improve the quality of the metal but simply to melt it without impairing its quality. Good practice requires, therefore, that care must be taken to supply the melting department with metal of inherently good quality, assured by specification or otherwise, having all the properties necessary to produce the castings desired. An alloy contains a number of primary elements, which must be present in definite proportions if the castings made from it are to have the desired properties. If the castings are made to a customer's specification, this will state the range within which these principal elements (for example, copper, tin, lead and zinc) are permitted to vary.

Jan 1, 1946

By W. S. McCain, B. A. Wilcox, A. H. Clauer

The creep and creep-fracture behavior of a Ni-200-2Th0, alloy has been studied over the temperature range 816° to 1038°C and stress range 4000 to 19,000 psi Specimens having their axes either parallel or transverse to the final sheet-rolling direction were tested in air, and the apparent activation energy for creep was found to be 92 kcal per mole, regardless of specinien orientation. The stress dependence 01- the steady-state creep rate, was satisfied by where n depended on orientation; n = 9.7 for rrzaterial transverse to the rolling direction and n = 24.3 for material parallel to the rolling direction. In the latter case, the relation was also valid. The rupture strength of material parallel to the rolling direction was -1.5 times gveater than the transverse rupture strength. Several tests in vacuum revealed that here the creep rate was higher and rupture life lower than for comparable tests in air. THERE is an increased interest today in producing improved dispersion-hardened alloys for high-temperature structural applications. This had led various materials designers to modify existing alloys, such as thoriated nickel. One system that has received considerable attention is based on chromium additions to Ni-ThO2, with the obvious motive of improving the oxidation resistance. Another effect of chromium is that of lowering the stacking-fault energy, y, of nickel. For example, the addition of 30 wt pct Cr decreases y from -225 erg per sq cm for pure nickel1 to -70 erg per sq cm.' This decrease in y could have several effects on the deformation behavior. There is some evidence that cross slip of dislocations around Tho2 particles is a mechanism of tensile3 and creep4 deformation in TD Nickel (Ni + 2 vol pct ThO2) at temperatures below 0.5 the absolute melting point of nickel, T,. A decrease in ? by chromium additions should increase the difficulty of cross slip. Also it has been suggested that the high-temperature (T > 0.5Tm) rate-controlling creep process in "recrystallized" Ni-Tho2 alloys is the climb of edge dislocations over Tho2 particles.5 According to weertman6 a decrease in the stacking-fault energy should decrease the dislocation climb velocity resulting in a decreased steady-state creep rate. Thus, chromium additions to recrystallized Ni-Tho2 alloys would be expected to decrease the creep rate, all other conditions being constant. However, a difficulty arises when the stacking-fault concept is applied to high-temperature creep of dispersion-strengthened metals which are produced on a commercial or semicommercial scale. This occurs because the materials are processed so that they have a high-stored energy of cold work, and the other substructural effects could obscure any influence of stacking-fault energy per se. An example of an alloy with a high stored energy of cold work is TD Nickel bar. This material has a fibrous grain structure (1 I diam by 10 to 15 p long), and the structure is stabilized by the ThO2 particles. Annealing at high temperatures, e.g., 3 hr at 1300°C, causes no recrystallization or grain growth.4 Previous work by the authors4 showed that the high -temperature creep behavior of TD Nickel could not be related to any simple dislocation theory of creep, and this probably was associated with the complex initial structure of the material.

Jan 1, 1968

By R. E. Cech

Metallographic observations on hydrogen-reduced nickel oxide crystals suggest that nucleation of nickel occurs at structural singularities in the oxide. The fully reduced structure contains micron-diameter, worm-like voids occupying 40 to 50 pct of the volume. The crystallographic orientation relationships between nickel oxide and nickel resulting from oxide reduction are recorded and discussed. THE process of reduction of oxide to metal is one of considerable complexity involving a chemical reduction reaction, mass transport of reducing agent to the point of reaction and of reaction product away from it, and finally a transformation whereby metal atoms released from the oxide rearrange to form a stable reduced phase. In addition, nucleation of the reduced phase affects the overall reaction kinetics. Thus far only the thermodynamic aspect of reduction has received the attention warranted by the importance of

Jan 1, 1960

[America,-Dear, G. C. Anniston.-Klugh, B. G. Auburn. *Poor, R. S. Bankhead.-Armstrong, W. D. Bessemer.-Creveling, J. G. Lindstrom, W. A. McKenzie, W. C. Mitchell, F. R. Birmingham.-Abbott, C. E. Armstrong, G. R. Austin, W. W., Jr. Ball, T. L. Beard, A. H. Benjamin, F. S. Blackburn, E. C. Blair, A. J. Blair, C. S. Blair. H. W.]

Jan 1, 1946

By B. Egeberg

IN A previous paper1 the authors dealt with the physical properties of cold-rolled and heat-treated Britannia metal of the approximate composition Sn, 91 per cent., Sb, 7 per cent. and Cu, 2 per cent. It was found that cold rolling to more than 50 per cent. reduction produced a continuous softening of the metal when measured by the Brinell machine, whereas the Shore instrument indicated increased hardness; that the strength of the material followed the Brinell hardness and that the metal therefore became weaker the more it was cold-rolled; and further, it was found that hardness and strength could be largely restored to the cold-rolled metal by "baking" for about one hour at any temperature, between 200° and 450° F., the melting point. The higher the baking temperature, the more effective was the heat treatment as far as increased hardness was concerned. It seemed to be of little importance whether the metal was soaked or not at the baking temperature for a great length of time and the rate of cooling seemed to be immaterial. The present paper deals with the same alloy and more particularly with the resistance towards various forms of stress - tensile, bend and deep drawing. The metallography of Britannia metal has in part also been covered and an explanation attempted for the abnormal behavior of this alloy.

Jan 1, 1929

By J. F. Nester, J. B. Schroeder

COMPOUNDS of rare-earth and iron-group elements are of technical interest because of their unusual magnetic properties. To date, however, all magnetic measurements1-4 have been made with polycrystalline, often polyphase, samples. For the measurement of anisotropic properties, single-crystal samples are necessary to avoid the averaging effect of randomly oriented grains. The purpose of this note is to describe a technique with which we have grown relatively large single crystals of YCo5, NdCo5, DyCo5, and "YFe9". Crystal growth of these materials is complicated because: 1) the binary equilibrium diagrams are, in general, not well-established; 2) in those cases where phase-equilibrium data are available, the compounds of interest are generally formed by peritectic reaction; 3) the molten component metals are chemically very reactive, making contaminaticn of the melts by the crucible material a serious problem. Techniques such as arc or levitation melting followed by strain annealing have been tried5)' in the past with these materials, but with little success because of the peritectic reactions and the inherently poor process control. For this reason we chose to use the zone-melting technique of Mason and cook7 for our work, since past workers8 have had some success in preparing single crystals of peritectic compounds by this method.

Jan 1, 1965

By R. W. Raymond

The important question of the metallurgical value of the coals of the Rocky Mountains and the Pacific Coast is to be settled, of course, by practical experiment. Meanwhile, as I have had occasion to point out, the proximate analyses of these coals throws little light upon it, and is, indeed, likely to mislead the metallurgist, if he compares it with the results of similar analyses upon bituminous and semi-bituminous coals. With the view of showing how large a proportion of the material usually classed as(" volatile matters " consists of combined water, or oxygen and hydrogen presumably in chemical combination, I have collected a number of ultimate analyses from various sources, in the following tables. The numbered analyses in the first table are as follows: No. 1. Monte Diabolo coal—Analyst, H. S. Munroe, Col. School of Mines. 2. Weber Canon, Utah, " " " 3. Echo Canon, " " " " 4. Carbon Stat'n, Wyoming, " " " 5. " " " " " 6. Coos Bay, Oregon, " " " 7. Alaska, " " " 8. " " " " 9. Canon City, Colorado, " Dr. T. M. Drown, Philadelphia. 10. Baker Co., Oregon, " " " 11. Blockcoal,SandCr'k,Ind., " Prof. E. T. Cox. This table affords some suggestive comparisons, to facilitate which a remark or two, explanatory of its construction, will be useful. In the ultimate analysis of coals, the proportions are frequently calculated (as, for instance, in the report for 1872 of Prof. Cox, State

Uranium, discovered in 1949 at Rum Jungle, 40 miles south of Darwin, N. T., was mined and processed to U3O8 from 1954 to 1963 by the Territory Enterprises Pty. Ltd. TEP is a Government company managed by Conzinc RioTinto of Australia Ltd. During this period, the uranium oxide was sold under contract to the Combined Development Agency, a joint Anglo-American uranium procurement agency. When the contract terminated in 1963, more than 31/4 million pounds of uranium oxide had been delivered which had been mined from three open pits. Copper ores, found with the uranium, necessitated the addition of a copper circuit to the concentrator. Copper concentrates containing 12,981 pounds of copper were also produced. Rum Jungle was the largest single industrial enterprise in the Northern Territories and, as such, was an important economic and social factor in this sparsely settled tropical region. To stretch out the life of this enterprise for the above reasons, and with the added possibility that the uranium market might improve, the Commonwealth mined out and stockpiled 650,000 tons of ore containing 9.6 lb of U,O, per ton, which is sufficient to sustain the treatment plant at 200 tpd until about 1971. In the plant, uranium is recovered from solution by solvent ex- traction. Current output is being stockpiled pending suitable market conditions.

Jan 10, 1964

By Peter N. Calder, G. H. Blackwell

The development of an open pit slope monitoring system, from equipment selection and justification to complete computer data storage and analysts, Is described. Methods of overcoming the Limitations of the electronic transit/distance measuring device and survey system selected are discussed. Results of the monitoring program showed that blasting was a major cause of Instability, and, after much experimentation, suitable blast patterns for mine production and pit wall integrity were designed. The experiences gained with double benching 'and wall cleanup procedures are discussed . The monitoring program also indicated that water was a contributor to instability, and methods of dealing with water In a rock with a low storage coefficient and transmissibility are described. Because of the danger of falling rock, photogrammetric methods are used for joint mapping and analysis, this work being contracted out. Joint strengths are measured on-site using a portable shear tester. Finally, a discussion of a complex failure is given.

Jan 1, 1983

By W. K. Godfrey

The highest compressive strength cement has the highest bond strength in tests in which the cement is subjected to a confining pressure. After perforating, the bond strength is reduced to nearly zero when the pipe is supported by weak cement. Perforating does not affect the bond strength, however, when the pipe is supported by strong cement. Pipe supported by weak cement is damaged by perforating with expendable capsule jets, but is not damaged by perforating with the hollow carrier gun. High strength cements are recommended for oil wells that are to be perforated. Introduction The purpose of this work is to determine the effect of jet perforating on the bonding strength of oilwell cement at simulated down-hole conditions. Bond strength is a good criterion for determining the effectiveness of cement in performing its main function, i.e., that of isolating zones. According to the literature on the subject, the optimum cement strength for perforating is low and should not exceed 2,000 psi compressive strength. This conclusion was based on the appearance of bullet and jet perforations in neat and gel cements largely done in the absence of a confining pressure more than 15 years ago. Discussion Literature A relatively weak cement has been recommended in the literature as having optimum properties for perforating. In 1947, Oliphant and Farris tested bullet perforating of neat cements at various curing times.' Some of the tests were made at down-hole conditions. They reported that the optimum cement strength for perforating was about 2,000 psi compressive strength. Enlarged holes occurred when strength was too low, and the cement shattered and cracked when the strength was too high. In 1951, Morgan and Dumbauld tested bullet and jet perforating of neat and gel cements at surface conditions.' They reported that optimum cement has a compressive strength less than 2,000 psi. In their tests at atmospheric pressure, high strength cement shattered and cracked when perforated. Thus, the optimum cement strength was based on the appearance of neat and gel cement after perforating. In 1953, Clark showed a relation between cement strength and fluid shutoff.' He concluded that a 500 psi compressive strength is required for good fluid shutoff and that maximum bonding ability is developed at approximately 1,000 psi compressive strength. In 1964, Bell and Shore invalidated most of the conclu sions by the previous authors when they demonstrated that atmospheric pressure tests cannot be used to determine casing deformation and damage that will result from perforating under down-hole conditions.' They showed that the higher the hydrostatic pressure, the more restricted will be the expansion of gases generated by the charge. Less casing deformation and damage occurs under down-hole conditions than at atmospheric pressure. In recent work, Bearden et al. reported that jet perforating at surface pressure with the hollow carrier gun caused the cement sheath to shatter and crack.' The perforating, however, did not seriously affect the pressure required to leak past the casing cement bond. Only three cementing mixtures were tested, and presumably they had strengths in excess of 2.000 psi. Bearden et al. also reported that the hydraulic bonding strength increased as the compressive strength increased. Their hydraulic test showed that approximately 1,000 psi pressure is sufficient to break the casing cement bond for a well aged neat Portland cement sheath. Unfortunately, the tests were not run with a confining pressure, so Bearden et al. were merely measuring the strength of their outer 8%-in. casing. In our investigation, we measured the hydraulic bond strength of cement to pipe under a confining pressure and found that the bond strength was not limited to 1,000 psi. Cement Bond The bond strength is a good criterion for measuring the effectiveness of cement in performing its main function, that of preventing interzonal communication of fluids behind the casing. Measuring bond strength after perforating should be a good quantitative method of determining optimum cement properties, and should be a better method than that used by previous investigators,11 ' who simply observed the appearance of the cement after perforating.

Jan 1, 1969

By John V. Beall

Hard as the Revett quartzite are conditions governing the deep mines of the Coeur d'Al6ne. In fourscore years of mining, heat and pressure have been the rewards of preseverance. Such obstacles are the natural concommitant to search for ore at depth. But high cost and shortage of miners is a creeping frustration of the decade. These grim observations were made on a trip to the mines of the Coeur d'Al6ne in the first week of May. But the bouncy optimism of competent mining engineers and geologists overrides by far the tough conditions. This is the story of what they are doing. I think they are setting the stage for the wonder mines of tomorrow. I didn't meet all the people or see all the mines, so there are unfortunate gaps in the story. Then too, sometimes the muck and water blotched my notes, or I couldn't write fast enough or I was too tired. No matter. There is much to tell and, because it is basically a human story, I am flouting the rules of technical journalism and couching it in the neglected "I" person. First then, a little history . . . .

Jan 7, 1966

By George W. Hezzelwood

THE Balatoc mine, one of the Haussermann group,† is on the Island of Luzon, the largest of the Philippine group, about 260 km north of Manila, and 12 km from the city of Baguio The Baguio district is the most important gold-mining area of the Philippines, with 14 producing mines in 1939, milling 2,358,804 tons of ore, yielding [P]40,881,048, approximately 55 per cent of the total Philippine production of [P]74,131,216 PRODUCTION HISTORY The Balatoc mine began production In January 1929 with a 150-ton cyanide mill Increases in mill capacity have taken place as follows March, 1932, to 330 tons June, 1933, to 470 tons December, 1933, to ;15 tons July, 1934, to 700 tons December, 1934, to loon tons May, 193, to 1200 tons October, 1938, to 1300 tolls April, 1939, to 2000 tons January, 1941, to 2T50 tons Production during the period of expansion has steadily increased in total value in spite of the fact that grade of ore milled has dropped-from $31 06 in 1929 to $5 78 in1940 Annual reports give production as shown in Table I, the average value, being based on gold at the old price of $20 67 per ounce [ ] GEOLOGY The ore occurs in quartz-calcite veins that vary in width from narrow stringers to mineralized zones 40 to 30 ft wide Wall rocks consist largely of diorites, with some andesite, and a fragmental breccia called locally the "Balatoc plug " Texture of the ore varies widely in the different vents-from a soft, highly altered, gouge material filled with quartz fragments through a soft, unaltered quartz-calcite to a hard, massive quartz ore Three major vein systems have been extensively developed, and smaller amounts of work have been done on several others These veins strike east-west to N 60°, clipping south from 50° to 90°, and are essentially tension breaks between a series of faults or shears striking N 30°E to N 30°E and clipping southeast from 50° to 90° The shear veins and tension veins probably formed more or less simultaneously,

Jan 1, 1942

By Edmund Davenport

Tier; production of thorium of high purity by the Ca-CaCl2 reduction has been described by Marden and Rentschler,1 who also reported some of the properties of the coherent, ductile metal obtained from this pure thorium powder. The present paper describes the properties of thorium produced by the Ca-CaCl2 process modified in some details to meet commercial conditions. The principal effect of these changes in process has been an unavoidable increase in the oxide content of the thorium.

Jan 1, 1929

By I. Cornet

With the greatly expanding use of magnesium during the war, it appeared necessary to the War Metallurgy Committee that the notch sensitivity of magnesium alloy extrusions be further investigated and the influence of various factors upon notch sensitivity be noted. Accordingly, the National Defense Research Committee of the Office of Scientific Research and Development placed a research contract with the University of California, supervised by the War Metallurgy Committee. The work discussed herein was done under "Restricted" Project NRC-21, reported in Dec. 1943~; it has been released for publica-tion by the O.S.R.D. Scope of the Investigation The notch sensitivity of various magnesium alloy extrusions was determined under axial tension, and also under several conditions of nonaxial tension. Hardness, grain size and other metallographic features were observed; stress-strain data were obtained, and the chemical compositions of the alloys were determined, in order to correlate these quantities with thc notch sensitivity. Notch sensitivity under axial tensile load was determined for a few specimens which had been cold worked to various degrees by tensile prestraining. Magnesium alloy extrusions studied included Dowmetal 0, X, J, and A(. For comparison, extrusions of aluminum alloy 24s-T, cast bars of aluminum alloy 122-T2, and cast bars of magnesium alloy C were also tested. The specified chemical composition of these alloys is given in Table I. All bars tested were within specification limits of composition. Investigation of thc tensile notch sensitivity of various magnesium alloy extrusions, under conditions of axial and eccentric load, showed little or no correlation with stress-strain or other conventional data. Since the many uncontrolled variables present might mask significant relationships, one alloy was selected for intensive study. Magnesium 0 alloy extrusions were subjected to experimental heat treatments, and the ,Changing hardness, tensile strength, microstructure, and notch sensitivity observed. Experimental Techniques and Procedures Tensile Testing Bars used for axial loading were machined with % in.- and with 34-in. minimum diam1 and included specimens with 60" V notches (Fig I and 2). Each V-notched specimen was roughed out carefully and then finished with a honed tool. These Y-notched bars were sampled frequently, sectioned, polished, and examined at 500 X magnification to control

Jan 1, 1949

By S. C. Schaeker, A. W. Schlechten, A. H. Larson

PARRAVANO and Malquori' studied the equilibrium of H2S-Hz with molybdenum and its lowest sulfide which they believed to be MoS2. Mc Cabe' has shown that its composition is actually Mo2S3 and determined its dissociation pressure by means of Knud-sen effusion measurements. Stubbles and Richard- son3 have recently studied the equilibrium of gas mixtures of H2S-HZ with the two-phase solid mixtures of Mo-MozS3 and Mo2S3-MoS2. The latter investigators found that M02s3 deviated slightly from the stoichiometric composition, but they did not determine the homogeneous region of the disulfide phase. Morimoto and Kullerud, studied the Mo-S system by quenching, microscope, and X-ray methods and concluded that the disulfide is stoichiometric. The present investigation was concerned with the measurement of the sulfur vapor pressure variation with composition at 1100°C in the homogeneous region of "MoS2". These measurements were made by reacting: 1) molybdenum powder (99.97 pct Moj with sulfur vapor, and 2) MoS1.g9 (formed by reaction of Mo + H2S) with sulfur vapor in a quartz capsule. Conditions were controlled to form an equilibrated phase within the homogeneous region of the disulfide. The quartz capsule was sealed off initially under a vacuum and the residual gases were gettered by titanium powder contained in one end of the capsule. A mixture of Mo + S or MOS,., + S was in the other end. The section containing the titanium powder was heated for 24 hr at 700°C and then removed by flame sealing. The end of the capsule containing the charge was then heated to 1100°C. The other end of the capsule was maintained at a temperature which would produce the desired sulfur pressure in the capsule (liquid sulfur distilled from the charge mixture was retained in this end). After equilibration, the capsule was removed from the heating assembly and rapidly air-cooled. It is assumed that equality existed between the total sulfur pressures (PT) in the two ends of the capsule and not between the partial pressures of the different molecular species (S, SZ, Three separately controlled heating elements were used to maintain the proper temperature gradient over the length (approximately 12 in.) of the capsule. A thermocouple-Wheelco "Capacitrol" system was used for temperature control of the two end heating elements within 2"C. The center heating element was controlled directly by a " Power -stat". Separate controlling and measuring thermocouples were used for both end heating elements. Pt-Pt(l0 pct Rh) thermocouples were used for 1100°C and Chromel-Alumel thermocouples were used for lower-temperature control and measurement of the assembly. Silver foil was wrapped around the end of the capsule containing the liquid sulfur to insure a constant temperature zone. The thermal gradient over the entire length of the capsule was measured to: 1) ascertain that the length of the constant temperature zone of the liquid-sulfur end and the sulfide end was sufficient, and 2) ascertain that the liquid-sulfur zone was the zone of lowest temperature. The data obtained in this investigation are shown in Fig. 1 and Table I. The total sulfur pressure (PT) and p(S2) were calculated from the data of Braune et UZ.~ The compositions of the equilibrated disul-

Jan 1, 1964

By H. A. Baumann, A. J. Rostosky

EVER since the first installation of wet-washing methods of coal preparation, the removal of the water added by the washing process has created serious technical and operating problems. The rapid development and widespread adoption of wet washing has necessitated a corresponding development of dewatering methods and equipment. The amount of water retained by coal varies with the size of the coal. The moisture that is largely on the surface of the particles is easily shaken off coarse coal; thus coarse coal can be dried comparatively easily and quickly. Fine coal presents a larger surface area than does coarse coal, so its capacity for retaining moisture is greater. In fine coal, moisture below about 5 per cent is held between the coal particles and its removal is difficult. Draining and drying of the finer sizes is a major problem at many washeries. Two common problems of coal-washing practice that are intimately connected with dewatering and drying are the clarification of washery water and the prevention of stream pollution. The first field has been studied from many angles, including the use of coagulating and settling agents followed by vacuum filters to remove the solids, and the use of sludge tanks with dewatering screens incorporated therein. In many districts, the disposal of sludges into streams has been stopped by law. The lack of space for impounding sludges has created problems of disposal in other districts. Reduction in moisture means a saving in freight costs as well as the elimination of difficulties in unloading and storing. Excess moisture in coal causes it to freeze in localities where severe climatic conditions pre¬vail. Excess water in coals to be used in the production of coke and manufactured gas has a chilling effect on the walls of the oven or retort. Dryness of coal is important in producing good briquettes.

Jan 1, 1943