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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 Nicholas T. Camicia

Coal is one of our oldest known commodities. Historic evidence indicates that this fossil-formed fuel was used in China and in Wales some 3000 to 4000 pears ago. Coal was discovered in North America in 1679 by French explorers in northern Illinois, and in 1700 a colony of Huguenots came across bituminous coal in Virginia. One might think by this long history of a single commodity that the string was about played out. Quite the contrary, coal is in greater demand than ever before and coal mining today is a modern industry. It is in an unprecedented growth period as the nation-and the world-demands more and more energy coincident with dwindling reserves of other fossil fuels. By the year 2000 the demand for coal is expected to at least double the current level of some 600 million tons annually despite the advent of nuclear power. To meet this challenge, the coal industry is vitally in need of an increasing supply of technically trained and progressive manpower. And, coupled with a serious shortage of engineers and technicians, it represents a rich vein of occupation opportunities-all the way up to top career levels. Today, coal mining is a complex, highly specialized industry concerned with more than just getting coal from the earth and putting it into the furnaces of the consumer. The industry is concerned with the environment, with maintaining a viable ecology. Recognizing the ramifications of global economics, the industry is very much aware of its important position in contributing to a constantly rising standard of living throughout the world. The key to rewarding employment in the coal industry is skill-skill that has been developed by education, training, and experience. None of these alone is enough; all three are necessary today to produce the skill needed to meet the employment requirements of the coal industry. Routine manual labor will no longer do the job in coal mining. In the United States coal mining has been mechanized to a degree unsurpassed anywhere else in the world, and the coal worker must be thoroughly

Jan 1, 1973

By Henry G. Granger

DURING upwards of three thonsand miles of canoc-travel in South America, including several mishaps, the writer has unfortunately lost his book of notes taken during the year 1894 in Dutch Guyana, or Surinam. But a year spent in a foreign country, visiting its principal mining properties, is necessarily productive of indelible memories and impressions, and some of these may be of interest to the Institute. The Guyanas include British, or Demerara, Dutch, or Surinam, French, or Cayenne, and the Disputed Territory, or that portion of Brazil on the northeast coast of South America. After passing the picturesque mountainous coasts of Colombia and Venezuela, one reaches a low, flat mud-bank which extends far out into the sea, so that from the steamer, over a couple of leagues of turbid, shallow water, one call just see the dismal outline of the pestilential "bush" that fronts the Caribbean sea, clear around to the mouth of the Amazon. Here, iii the order mentioned above, are the Guyanas. So much has been said about this out-of-the-way section during the late excitement over the Venezuela boundary question, that the historical part of the subject may be advantageously condensed. Gold-mining in the Guyanas is altogether placer-mining, and is of the same general nature throughout; hence by describing the methods in use in Surinam and the results there achieved, ail idea will be given of the work throughout the field. The product of this section is about three to four millions of dollars annually, mostly from Demerara, not because of superior richness of its placers, but as a result of its very much larger population, which exceeds twice the aggregate census returns of both Surinam and Cayenne. Mining ill all this section is of comparatively recent date, and is indirectly due to the decline of the sugar-industry. After the introduction of beet-sugar scores

Jan 1, 1897

By William P. Blake

In the recent litigation for the possession of franklinite by one party and of zinc-ore by the other party, it was shown by the evidence of experts familiar with the original condition of the outcrops that at Mine Hill a more or less disticctly defined layer of red zincore underlay the heavier and larger body of the franklinite, so-called ; this layer or bed of zinc-ore dipping under the franklinite upon the western cropping, while at Stirling Hill, two miles south, the conditions were apparently reversed, the zinc-ore overlying the franklinite. An explanation being required, it was shown, first, that at both places, at Mine Hill on the north and at Stirling Hill on the south, the ore-bed lies in a synclinal or trough-like fold with the red zincore under the franklinite; and secondly, that at Mine Hill, we see chiefly the outcrop of the western part of the folded bed and at Stirling Hill the eastern part; the Mine Hill cropping being on the western slope, and the Stirling Hill cropping on the eastern slope of the hill. Thus the ''back vein" at Stirling (the western outcrop) corresponds with the front-vein at Mine Hill, and, like it, has the red zinc-ore on the foot-wall, while the front-vein or eastern cropping at Stirling corresponds to the back-vein or eastern cropping at Mine Hill in the part of the bed generally known as the " buckwheat-field vein." If the ore-bed were continuous in one synclinal trough between the two localities, no further explanation would be required. But it is not so ; and the synclinal folds at both places pitch steeply to the north, bringing the beds to the surface in horseshoe-like curves at their southern ends or croppings, and carrying the beds far below the surface northwards. This justifies a doubt

Jan 1, 1895

By Che-Yu Li, J. L. Gregg, W. F. Brehm

Oriented, oxygen-doped niobium bicrystals were tested in liquid lithium. The grain boundaries were attacked preferentially. The depth of the penetrated zone varies as (time)2. The penetration was aniso-tropic, had a high activation energy, and increased with the increased oxygen doping level. A possible model was proposed to account for the experimental observations. 1 HE grain boundary penetration of a metallic system by liquid metal has been studied by several investigators. Their results are summarized by Bishop.' Most of these works show that the penetration by liquid metal corresponds to the phenomenon of liquid metal wetting. In the case of a grain boundary, wetting will occur when twice the solid-liquid interfacial tension is smaller than the grain boundary tension resulting in the replacement of the grain boundary by two new solid-liquid interfaces. Other possibilities exist; for example, the atoms of the liquid metal may diffuse into the grain boundary region due to chemical potential gradient. The gradient can be produced by impurity segregation or simply be due to the increase in solubility in the grain boundary region. The penetrated grain boundary in these cases may remain solid at the test temperature. The Nb-Li system has been of considerable interest because of its possible technological applications. For fundamental interest it provides a possibility of studying the grain boundary penetration process which is not controlled by the wetting mechanism. The pure niobium is not attacked by the liquid lithium, but if niobium containing more than 300 to 500 ppm oxygen by weight is exposed to liquid lithium, corrosion occurs at the solid-liquid interface and preferentially at grain boundaries. Previous investigators2-' have proposed that this preferential corrosion at grain boundaries is caused by oxygen segregation there, with subsequent inward diffusion of lithium to form a Li-Nb-0 compound. These investigators also found that the corrosion could be retarded by adding 1 pct Zr to the niobium to precipitate the oxygen as ZrO2 upon proper heat treatment. However, there are no quantitative data on the kinetics of the grain boundary penetration process to test the validity of the proposed corrosion mechanism. In this work an investigation of this penetration process in oriented bicrystals was made as a function of the oxygen doping level in the bulk niobium and the grain boundary orientation. A possible model for the penetration process based on the experimental results was proposed. EXPERIMENTS Oriented niobium bicrystals were grown by arc-zone melting oriented single-crystal seeds.7 These bicrystals contained simple tilt boundary. The [001] directions in the two grains were tilted about a common [110]. The bicrystals were 31/2 in. long and 5 by 4 in. in cross section with the straight, symmetric, planar grain boundary longitudinally bisecting the crystal rod. The bicrystals were doped with oxygen by anodically depositing a layer of Nb2O on the surface in a 70 pct HNO solution at 100 v, using a stainless-steel cathode. The specimens were homogenized by annealing in evacuated quartz tubes at 127 5°C. Oxygen content of the niobium was measured from microhardness values, after DiStefano and Litmman.' Supplementary checks were made with vacuum-fusion analysis.7 Individual test specimens cut from the doped bi-crystal rods, about by by % in. in size, were tested inside double jacket sealed capsules. The inner jacket was niobium, the outer was stainless steel. The niobium inner jacket eliminated the problem of dissimilar-metal mass transfer.' The lithium (99.8 pct pure, obtained from Lithium Corp. of America) was handled only in a purified argon atmosphere in a Blickman stainless-steel glove box. After introduction of lithium, the capsules were sealed by welding. Further detailed experimental procedures are given in Ref. 7. The capsules were heat-treated in vertical Marshall resistance furnaces. Temperatures were controlled to When heating above 1100°C, it was necessary to seal the furnace work tube and flow argon through to prevent failure of the stainless-steel outer jacket of the capsule. Tests were made on 6" 2", 16" 2, and 33" i2" bicrystals at oxygen levels up to 2600 ppm by weight in the 6' and 16" crystals and with 1300 ppm oxygen in the 33' crystals. The oxygen levels were controlled to 100 ppm. Most of the quantitative data were obtained from 16" bicrystals between 800" and 1050°C. The capsules were quenched into water after the test and cut open with a water-cooled abrasive wheel. The capsules were then submerged in water, which dissolved the lithium and freed the specimen. Measurement of the depth of the penetrated zone in the grain boundary was done either on metallographically prepared surfaces or directly on the grain boundary plane after the specimen was fractured in tension in the grain boundary plane. The depth of penetration measured by both methods agreed well. Further details describing these techniques have been reported elsewhere.'p7

Jan 1, 1969

By L. A. Weakly

The Viburnum ore trend is the largest, single known ore body of lead in the world. Four well-known mining companies operate in the trend, which is approximately 64 km (40 miles) long and up to 610 m (2,000 ft) wide, located some 121 km (75 miles) southwest of St. Louis, MO. Total production from the mines for 1979 was 33 kt/d (36,000 tons) of ore or 472 kt/a (520,350 tons) of lead and coproduct metal. The district is the number one producer of lead, providing 90% of the United States' output with its coproducts, zinc ranking second, and copper and silver both ranking sixth in total US output. Mining is done in a stratiform deposit approximately 305 m (1,000 ft) in depth with the host rock principally dolomite. Ore is mined in large open stopes by the method commonly referred to as room-and-pillar mining. Mining methods and equipment are fairly similar, with the mines classified as trackless, all mining equipment operates on rubber tires. This paper will present a description of the different methods and equipment used to move ore from the active heading underground to the ore shaft for hoisting to the surface. Basically, three methods are incorporated: front-end loader and truck haulage combination; front-end loader and truck, with main line track haulage combination; and front-end loader and truck, with conveyor haulage combination. The logistics of each system, such as method of use, equipment specifications, ore handling rate, and those cost figures that could be made public, will be included.

Jan 1, 1983

By L. C. Morganroth

CARBONIFEROUS CLAYS FROM a geological standpoint, but scant attention has been paid to fire-clay beds. Only within the last few years have they been the subject of individual investigation, prior to this time having been considered only in their relation to coal seams. While the relative importance of coal and fire clay is still immeasurably in favor of coal, yet an industry as large as that of fire clay is entitled to a measure of attention. A discussion of the Carboniferous clays is practically a discussion of the clay beds in the Appalachian basin, since more than 90 per cent. of these clays mined are from this region. The clays are confined to the northern end of the basin, or the States of Pennsylvania, Ohio, Kentucky, Maryland and West Virginia, ranking in importance about in the order named. The clay deposits of the Carboniferous period have been divided into two classes; those found in the Pottsville conglomerate series of rocks, and all those that are found in the formations above, for the reason that the clay beds above the Pottsville series all resemble each other in properties, composition and appearance, and all are distinctly different from the bed found in the Pottsville formation. The bed of clay found in the latter formation is unique in that flint clay is practically restricted to it. (A variety of flint clay is occasionally found in these upper deposits but this is in such small amounts as to be negligible.) Carboniferous clays occur between stratified rocks; sandstones, limestones, etc., in the same manner as coal veins. They are often accompanied by a coal vein although where the clay is of a workable thickness the coal is generally too thin to work. The clay beds are sometimes known by the name of the coal seam at which horizon they occur. Clay beds may be from a few inches up to 20 ft. in thickness. They may consist of all soft clay all flint or both soft and flint.

Jan 2, 1916

By John M. Hartman

An examination as to irregularity of wear around the nose of the Witherbee tuyeres showed a section through the nose near the top as per Fig. 1, and a section only a half-inch beyond as per Fig. 2. The molten iron flowing over the nose of the tuyere had melted off the metal until the water in the tuyere prevented further melting. These tuyeres have a division in the annular water-space (see Fig. 2) to turn the current of water at the top, and the watersupply pipe is carried to within 1 inch of the nose. The constant supply of cold water in the nose of the tuyere kept it well cooled and preserved. But half an inch on the other side of the division the metal had melted off, as is shown by Fig. 1. There was no means of effecting a circulation at this point so long as the water was discharged from the butt of the tuyere. A pipe having been placed on the discharge-side of the division, the same as on the supply-side, in order to secure a circulation of the water at the nose on the discharge-side, it was found that the metal did not burn off. The nose being found to give out at the bottom, a division was placed in the annular water-space at the bottom, terminating 1 inch from the nose. This made a sharp current of circulation in the nose at the bottom, and prevented the burning of the metal there. A positive circulation at the nose, top and bottom, is a necessity with the present fast driving of furnaces, and prolongs the life of the tuyeres. The proper metallic composition of tuyeres is a question constantly agitated. A trial of ordinary yellow-metal* tuyeres was made 12 years ago. They did their work just as well

Jan 1, 1899

By Alan M., Bateman

MR. JORALEMON'S dispassionate discussion of this subject in TECHNICAL PUBLICATION 340 of the Institute shows clearly some of the failures and successes of geology in the discovery of ore deposits. He forces us to recognize, with humility, that chance has played a greater part than geology in the recent discovery of several great copper deposits. I think, however, he wrongly ascribes to unexpected or chance discovery some deposits that were found as a direct result of geological investigation. I refer to the Rhodesian copper deposits,, particularly Roan Antelope and Mufulira, both mentioned by him as having been found by chance. Also,. I think Mr. Joralemon's paper, inadvertently, does not- give the proper credit for the early recognition of the possibilities of these deposits. I feel sure that Mr. Joralemon and the gentlemen given credit by him will welcome any further information on this subject that will throw light on what will some day- be of. historical interest and importance. Consequently, I should like to set forth some additional data that throw light on who should receive the most credit, and' to indicate that, in my opinion, sound. geological reasoning and not chance is to be, credited for the development of the. Roan Antelope and Muf ulira mines.

Jan 1, 1931

By B. Ancker, E. R. Parker

The small-angle dislocation-boundary density of nickel and some of its alloys was investigated as a function of strength. It was found that the strength is a linear function of the density for pure nickel and for Ni-Ti alloys, but not for Ni-Co alloys. The results are interpreted in terms of dislocation theory. THE processes by which metals deform are still poorly understood, even though there has been a concentrated research effort in this field during the past fifteen years. Single crystals and individual grains in polycrystalline aggregates often develop a subgrain structure when deformed. Substructure formation occurs as a result of local plastic bending and its development is augmented by annealing at moderate temperatures.' Investigations made to date, largely qualitative in nature, have shown that the substructure is composed of a network of small-angle boundaries. The purpose of the present paper is to present some quantitative data on substructure (obtained by X-ray techniques) and to correlate the results with the strength of the metal in which the substructure existed. Nickel and some of its alloys were used for the experiments. The presence of certain kinds of foreign atoms greatly alters the formation and effect of the substructure. Polycrystalline tensile specimens were prepared from high purity nickel, two Ni-Ti alloys, and two Ni-Co alloys; the composition of these materials is given in Table I. Tensile specimens having a reduced section 1/4 in. diam by 3 in. long were machined from materials which were refined, cast, forged, and swaged in the authors' laboratories. The specimens were annealed for 1/2 hr at 1150°C, a treatment which produced grains having a diameter of approximately 0.5 mm. This rather large grain size was used to facilitate later examination of the substructure. Duplicate specimens of pure nickel and of each alloy were strained various controlled amounts in tension at room temperature and recovered for 1 hr at 800°C. (This strain induced prior to recovery will be referred to hereafter as the "prestrain.") One of each of the recovered specimens was pulled in tension at room temperature to obtain the stress-strain curves. The other bar was cross-sectioned in the gage length, carefully polished, and deeply etched to remove all cold-worked material. This specimen was then examined by the X-ray microscopic technique2 to determine the nature and magnitude of the substructure. The use of duplicate specimens permitted a direct correlation between tensile properties and substructure characteristics. X-ray microscopic studies were made with an apparatus constructed to have an average resolving power of about 4 microns. The monochromatic radiation reflected from grains which were oriented favorably was recorded on fine-grain photographic plates. These were examined at Xl00 which represents the true magnification, since there was essentially none in the X-ray system. This permitted detection of angular differences between subgrains of as little as 10 min. A very large number (over 100) of grains for each specimen was examined at this magnification and the number of substructure boundaries per grain was tabulated. An accurate relative measure was obtained under fixed experimental conditions, e.g., same grain size, resolving power, magnification, etc. The greatest source of error lay in counting the subboundaries, but this proved to be surprisingly small when repeated counts were made by different investigators. Furthermore, as the subsequent analysis indicates, whatever human error was introduced was not significant. Analysis of the Substructure Data When the number of substructure boundaries per grain was plotted against the frequency, skew (asymmetrical) distribution curves of the type shown in Fig. 1 were obtained. These are smoothed curves for the 1 atomic pct Ti in nickel alloy subjected to various prestrains and are representative of the curves obtained with all the metals. Since skew-distribution curves cannot be analyzed by elementary statistical methods, detailed investigations were undertaken in order to 1—test the consistency

Jan 1, 1955

By J. G. Faller, L. P. Skolnick

The distribution of cobalt and vanadium over non-equivalent crystallographic sites in C14-type Zr(VCo), alloys has been investigated. An anomalous X-ray scattering technique developed by Skolnick, Kondo. and lavine7 by which the separation in the scattering factors of two similar atoms can be enhanced was employed. Six alloys spanning the pseudobinary section ZrV1.6Co0.4-ZrVO.6CO1.4 at 10pct steps showed a nonrandom compositionally dependent distribution. Specifically, at high vanadium content cobalt preferentially occupied sites of type (6h) and vanadium, sites of type (2a; at low vanadium content the reverse was observed. In addition to the distribution fraction the structural parameters x and z were obtained. There was no significant deviation of these parameters from those obtained in the ideal C14 structure. Certain suggestions are made to account for the observed nonrandomness in the distribution of atoms on the two types of sites. INTERMETALLIC compounds of formula AB2 iso-morphous with MgCu2, MgZn2, and MgNi2 are known as Laves phases. Because Laves phases exhibit high symmetry and coordination numbers, the highest possible for an AB2-type compound,1 they are among the most frequently observed compounds in nature. In recent years interest has centered about the purely transition metal Laves phases2-' in efforts to understand the function of atomic size and electronic structure in the formation of these compounds. It has been observed that pseudobinary Laves phase systems often show a variation of structure across the phase diagram. Such a system is the ZrV2-ZrCo2 in which the structure varies from cubic MgCu2 to hexagonal MgZn2 to cubic MgCu2.4 Some understanding about the conditions under which the second modification is stable can perhaps be gained by studying the distribution of cobalt and vanadium atoms on lattice sites in the MgZn2 modification of the system ZrV2-ZrCo2. In both the MgZn2 and MgNi2-types there exist nonequivalent positions open to occupancy by the B element, whereas in the MgCu2 prototype all sites are equivalent. Skolnick, Kondo, and La-vine7 have developed an anomalous scattering technique suitable for this type of investigation. Whereas the influence of size on the formation of a Laves phase is well recognized, no substantial evidence has been put forth in support of the size ratio dependence of a particular prototype. Berry and Raynor8 suggested that RA /RB ratio does indeed affect the type of structure that is chosen, MgZn2 compounds tending to cluster about 1.225 while MgCu2 compounds were found at larger deviations from this ratio. Dwight,3 however, from a study of 164 Laves phases does not believe this generalization to be justified. Electronic effects are certain to play a part in the stability of Laves phases in general and in the choice of a structure type in particular. For example, size along would favor the formation of Laves compounds of Ti, Zr, Hf, Ta, or Nb as the A element with nickel or copper as the B element. The absence of such is attributed to an unfavorable electron : atom ratio by Elliott and rostoker.4 Early experiments of Laves and witte9 with pseudobinary and pseudoternary systems of the three prototypes established the dependence of crystal structure upon electron: atom ratios. They observed that the MgCu2 structure dissolved elements of higher valency until the electron: atom ratio of =1.8 was reached; the MgZn2 likewise dissolved elements of lower valency replacing zinc. witte,6 from calculations of the electron : atom volumes of Brillouin Zones, obtained limits of stability for the prototypes MgCu2 and MgZn2. Elliott and Rostoker4 used these limits with considerable success in the all-transition element Laves phases they investigated. According to witte,6 compounds between the electron :atom ratios of 1.80 and 2.32 were of the MgZn2 type; those above and below exhibited the MgCu2-type structure. On the basis of these limits and an assumed valency of zirconium based upon the near tetra-valence of titanium, Elliott and Rostoker obtained valencies for the first transition series elements. For the Laves phases with which this investigation is concerned, ZrV2 and ZrCo2, the authors calculated electron :atom ratios of 2.54 and 1.56, respectively. These ratios are for the MgCu2-type structure and straddle the stability band of the MgZn2 modification. One could, therefore, predict that a pseudobinary system ZrV2-ZrCo2 should pass through the MgZn2 modification in traversing the composition diagram from one end to the other. Implicit in this assumption is a smooth change of the electron: atom ratio from 2'54 to 1.56. MOSS10 states that his finding the low temperature structure of ZrCr2 to be C15 instead of C14 alters greatly Elliott's valency of zirconium and hence the assumed valencies of the other metals. Such a quantitative correlation of structure with electron : atom

Jan 1, 1963

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By Neil O. Johnson

In the cyanidation of gold, silver and mixed ores, the solids, suspended in the pulp after fine grinding, primary settling and scries agitation arc subjected to a washing step known, generally, as countercurrent decanta-tion, abbreviated C.C.D The conventional C.C.D. plant consists of a series of separate thickeners—three to five in number—arranged in series on slightly different elevations. Solids settled in the first thickener are pumped at maximum density into the second thickener, where they arc diluted with weak solution overflowing the third. After settling in the second thickener they are pumped to the third, where the process of repulping with still weaker solution is repeated, and so on throughout the system, until they reach the last thickener and are repulped with barren solution or water. Recently there has been developed a new type of thickener, known as the Dorr Washing Tray Thickener, consisting of up to five individual thickeners, which performs in a single unit all the functions of a conven-tional C.C.D plant. Fig. 1 illustrates the essential features. It is a multicompartment tray thickener, in which the trays operate in scries instead of in parallel for countercurrent washing. Feed enters the top compartment via a central, semisubmerged feed well. Strong solution overflows into a peripheral launder. Solids settle to the bottom, are raked to the center and flow into the top of the second compartment, directly below, via an inverted cup and scal. Solids pass downward, compartment by compartment, against a counter flow of wash solution and finally of fresh water. Thus, in accord-:trice with the basic C.C.D. principle, the solids transfer the dissolved metal content to the wash solution and finally are removed by a diaphragm pump from the bottom compartment virtually free of valuable material. Similarly, the wash water, as it flows through the system, becomes increasingly enriched in dissolved metal until it overflows from compartment two and returns to the process.

Jan 1, 1939

By William P. Mason

FoR reasons unnecessary to enter into here, I was called upon to contradict the statement that " closed metallic vessels, partly filled with water and heated, do not become shattered by violent explosion, but simply rupture by over-pressure;" and the following experimental results were obtained in support of my position : A piece of drawn brass tubing (telescope-tubing) 1 1/2 inches in diameter and 15 inches long was closed at both ends by screwing on heavy caps of bronze. Before closing the second end the vessel was half filled with river water, the cap was then screwed on, and the closed vessel was supported upon two iron anvils, and heated in the interval between the supports by a large Bunsen lamp. The resulting explosion (which was doe to over-pressure only and not to any more occult cause) was exceedingly violent. No small damage was done to the room in which the experiment was undertaken; and the noise was like that of a cannon. Those of the pieces which could be recovered are shown in Fig. 1. Upon examining the wreck, it was noticed that one of the heavy bronze end-caps had preserved its circular section and still contained that portion of the barrel of the tube which had been screwed into it, while the other end-cap contained no portion of the tube, and was moreover sprung into a shape more or less elliptical, as if from excessive lateral strain. It was also observed that the large pieces of the shattered boiler predominated towards the end which had been closed by the un-sprung end-cap. The reasonable explanation, in view of the facts, was, that over-pressure had caused the boiler to yield through the screw-threads at A B, Fig. 2, and the righthand end-cap had blown off, thus leaving the boiler half filled with water, greatly super-heated for the new (atmospheric) pressure to which it was suddenly reduced; that this water had consequently sprung instantly into steam with dynamite effect, shattering the tube and springing the remaining end-cap. The large pieces would be expected at the open end of the boiler, as at that point the "tamping "would have been that of the atmosphere only. This explanation assumes a rupture to have been caused by gradually increased pres-

Jan 1, 1893

By Oliver C. Ralston, Foster Fraas

VIRTUALLY all commercial use of electrostatic separation has employed separators depending on differences of conductance of the broken, solid mixtures treated by them. The two main types of conductance separators have been: (1) Those in which the separating field is as near a static field between two charged electrodes as it is possible to maintain in the face of the usual leakage that takes place between electrodes with some 5 to 50 kv tension between them and spacing of l/z to 3 in.; (2) those in which a convective discharge of corona or spray type, but not a spark discharge, takes place between the carrier electrode and a charged electrode facing it, which is of very restricted area, such as a row of needle points or a small diameter wire parallel to the face of the carrier electrode. The present paper deals with this latter type. The principle is usable in separators where the carrier electrode, usually grounded, has the shape of a roller, a conveyor belt, a vibrating table, a sloping chute, or a nearly vertical plate. The innovation studied by us has been the use of the convective field for charging material on the carrier electrode and succeeded by a field between the carrier electrode and an electrode made of a true dielectric which cannot take on a charge by conduction but is charged by being in the radius of the corona discharge. The acquired charge is of the same sign as that of the corona but is not dischargable by contact with a good conductor. However, high-tension charge tends to leak off because of the ionization of the ambient air. The field between this electrode and the carrier electrode is as near static as it is possible to obtain. There are some differences in behavior of this electrode and that of the gas tube electrode used by Sutton, as will be discussed below. Both electrodes cause increased adhesion of nonconductive particles to the carrier roll. The particles are pinned there because they are convectively charged on their outer surfaces facing the corona electrode. The electrodes also cause increased rate of release of conductive particles tending to be pinned by corona charging but conveying the charge to the grounded carrier roll almost as rapidly as it is received by the particles.

Jan 10, 1950

By Frank Doxey

AT Dominion Steel & Coal Corp. it has long been recognized that continued mechanization of mine operations is necessary in the Pictou, Cumberland, and Sidney coal fields of Nova Scotia. The varied physical conditions in these fields call for special consideration of individual cases before planning is finalized. Because standard equipment cannot be procured which would operate successfully, many experiments have been necessary over the years to keep pace with the progress made in other countries. There are two mines, producing 2000 tpd, located in the Pictou coal field. The field is badly distorted and crossed by many faults. Seams are highly inclined and irregular and vary in thickness from 5 to 40 ft. Entries are difficult to maintain because of squeezing of the coal. ribs and movement of the roof and pavement. Output from the three operating mines in the Cumberland field is 3000 tpd. The field is highly inclined, inclination varying from 12° to 32°. Overlying beds consist of shales and massive sandstone lenses of extreme toughness and are responsible for bumps when the stresses are relieved by extraction. At greatest depth these are among the deepest coal workings in the world. Depth of cover ranges from 2300 to 4000 ft. This prohibits room-and-pillar working and necessitates longwall operation. Working of contiguous seams concurrently to maintain output increases the already difficult conditions. The Sydney field, with a frontage of about 30 miles, is the most important of the Nova Scotia coal fields. With the exception of one small area it is now wholly submarine. Output is approximately 21,000 tpd. Seams are 21/2 to 8 ft thick, and cover in the areas varies from 600 to 2300 ft, with an average of 1500 ft from sea bottom to the top of the seam. The seams dip in a seaward direction, pitches ranging from 6" to 4.0". The shoreline is the last place of entry to the seams and distance from the bank to the working faces is generally over 3½ miles, in some cases as much as 6½ miles. Ventilation is a problem and requires the construction of large permanent airways. Getting and Loading Coal: In 1925, in view of heavy pressures exerted by thickness of cover overlying the seams, roadways and pillars of the room-and-pillar system being worked began to break up and coal was lost. It was decided that a change in the method of extraction in areas with heavy cover was necessary, and experiments were made with many short walls and longwalls varying between 90 and 250 ft. Trial and error proved that the best operating length was between 400 and 500 ft, delivering all coal to the dip, with roadways to the face following a level course. The change-over was gradual, and the technique of roof control developed with the system, so that falls to the face are now very infrequent. An advantage of longwall mining is that it yields 95 pct extraction, especially important in coal seams of high quality or in seams where faults or disturbances restrict the workable areas. This percentage of extraction is based on the fact that the longwall advancing system takes development faces where pitch permits instead of driving headings and leaving roadway pillars. This system yields high tonnage during development and limits loss in extraction to duff left during operations. Accompanying disadvantages, on the other hand, are the heavy construction cost of main roadways and the necessity of driving all new flank face roadways through the gob. If the main roadways are driven through the solid, and large enough pillars are left on each side for protection against flank face weights, then the width of solid coal is approximately 1700 ft. This represents 10.6 pct of the coal available, or 89.4 pct extraction of the whole. These pillars, however, are of such size that they provide a useful pillar drawing area as a final operation of the mine. It may be that although the seam cannot be generally mined by the room-and-pillar method, it can be adapted to

Jan 1, 1955

By Robert U. King

The Climax Molybdenum Company's mine is situated on the Continental Divide at Fremont Pass in Lake County, Colorado. Elevations at the mine range from 11,000 it. to over 12,000 ft. The ore body is on the south flank of Bartlett Mountain, a prominent peak in the Ten Mile Range. A horizontal section of the mine, such as the Phillipson level (Fig. I), shows the outer ore zone as an annular ring varying in width from 300 to 800 ft., surrounding barren silicified rock. In vertical section the outer ore zone is dome shaped (Figs. 2 and 3), the apex of which is truncated at the surface by glaciation, exposing part of the ore body. The outer ore zone overlies the barren core and is itself overlain on the flanks of the dome with unmineralized rock. An ore zone of similar shape underlies the barren core of silicified rock, known as the Central Ore Zone (Figs. 2 and 3). Molybdenite is distributed uniformly through a zone of moderately silicified granite, schist and quartz monzonite (early) porphyry, around a highly silicified core. The molybdenite occurs in veinlets associated with fine granular quartz and pyrite, replacing altered and fractured granite, schist, and porphyry, and as coatings on numerous fractures cutting these rocks. Intense fracturing of all rocks is a characteristic feature of the Climax ore body. Most fractures are mineralized and no longer represent planes of weakness. Much fracturing is postmineral, however, and these fractures are generally filled with sericite or gouge, or remain as unmineralized joints separating otherwise massive rock into blocks of various size. Study and Mapping of Caving Characteristics Important differences in the behavior of caving of various blocks of ore at Climax have been recognized, involving arching of the rock over caved stopes, tendency of caved rocks to funnel, and size of caved rocks. Also, new problems have arisen associated with future mining on the Phillipson level, and may occur with proposed development of lower levels, such as excessive stress on mine pillars caused by large masses of overlying stable rock, and higher costs in maintenance of mine workings in soft, weak rock. To explain the differences and to provide solution for these problems, a study of geologic structure was undertaken early in 1944, to determine whether it would be possible to map cavability of rock from physical features exposed in mine workings and in diamond-drill cores. A comparison of known caved areas was made and rocks were classified structurally according to strength or degree of cavabil-ity. As nothing of this nature had been done before at Climax, the approach to the problem was rather indefinite. Several trials were made with negative results, but collectively indicated a suitable method. This was to examine all mine workings and diamond-drill cores, record-

Jan 1, 1946

By R. V. Mrazek, F. E. Block, S. B. Knapp

The mixed homogeneous and heterogeneous kinetics of the thermal decomposition of tungsten hexacarbonyl were studied by employing a batch reactor. The system was such that a sample of tungsten hexacarbonyl could be injected into the preheated reactor, and the progress of the reaction followed by a simple pressure measurement. Both the homogeneous and heterogeneous reactions were found to be first order, and approximate activation energies were determined for each reaction. It is shown that the dis-proportionation of carbon monoxide to give carbon and carbon dioxide cannot be the source of carbon in tungsten deposits prepared by this reaction. The kinetics of the thermal decomposition of tungsten hexacarbonyl have been investigated as part of a continuing study by the U.S. Bureau of Mines on the decomposition of organometallic compounds. Reactions involving the thermal decomposition of metal carbonyls have a potential application in the preparation of pure metals and fine metal powders. Indeed, it was these applications which provided the impetus for much of the early work involving the carbonyls of nickel1 and iron.' The relative lack of study of other metal carbonyls can be traced to the comparative difficulty in synthesizing these compounds. The most common use for tungsten hexacarbonyl has been as an intermediate in vapor-phase plating.7'8 However, attempts to obtain a carbon-free deposit of tungsten by this method have not been successful, and some investigators have taken advantage of the carbon contamination and used this process to form tungsten carbide deposits.lo Other investigators have studied the thermodynamic properties11"14 and molecular structure of tungsten hexacarbonyl. However, very little is known about the kinetics of this thermal decomposition, the mechanisms involved," or the source of carbon in the resulting plate. In contrast, studies have been made of the kinetics of the thermal decomposition of nickel tetracarbonyl, iron pentacarbonyl, and molybdenum hexacarbonyl.'l It has been found that these thermal decompositions occur by a mechanism which is partially heterogeneous in nature. Information available on the equilibrium constants for the decomposition of tungsten hexacarbonyl was used to determine a temperature range, 500" to 560°K, in which the reaction could be expected to be essentially complete. APPARATUS The apparatus used allowed the injection of a sample of tungsten hexacarbonyl into a preheated batch reactor and the use of a simple pressure measurement to follow the progress of the reaction in the sealed reactor. The pressure was sensed by means of a pressure transducer (Consolidated Electrodynamics Corp., 0.3 pct)* capable of operating at the *Reference to specific products is made to facilitate understanding and does not imply endorsement of such brands by the Bureau of Mines._______ reaction temperature. This type of sensing element was chosen to avoid the problem of condensation of the sublimed carbonyl in the capillary tubing leading to any type of remote pressure-sensing device. stirring was provided by rotating the entire apparatus. Glass beads placed in the reactor provided a pulsating agitation. To minimize thermal gradients in the reactor walls, the reactor was constructed of aluminum. The support tube which held the reactor in the furnace was thin-walled stainless steel to minimize heat conduction out of the reactor. As a result of these measures, a nearly uniform temperature (°C) was maintained throughout the reactor. Fig. 1 is a schematic diagram of the apparatus. The small gear motor rotated the entire apparatus at about 200 rpm. The bearings shown at the ends of the air cylinder were perforated to allow air to be fed to the charging piston and to allow inert gas to be fed to the reactor during the preheating period. The sample was simultaneously injected and sealed inside the reactor by operation of the air piston. Fig. 2 shows a cross section of the air cylinder and the adjoining portion of the support tube leading to the reactor. The sample carrier is shown in place at the right-hand end of the injection rod extending from the air piston. The piston is shown in the retracted position, as it would be prior to the start of an experiment. The small Teflon gasket which encircled the sample carrier at the end of the injection rod sealed the reactor when the sample was injected. This seal was maintained throughout the test by maintaining air pressure on the piston. The sample carrier was a 2-in. section of thin-walled, -in.-diam nickel tubing with an internal blank about 1 in. from the base and with the base end sealed.

Jan 1, 1969

By J. F. Martin, L. M. Melnick, R. Rapp, R. C. Takacs

Recent studies on the determination of hydrogen in steel have shown that the hot-extraction method for removing hydrogen from a solid sample is preferable to its removal from a molten sample by vacuum fusion or by fusion in vacuum with tin. A number of techniques are available, however, for determining the hydrogen so extracted. They include: thermal conductivity, gas chromatography, pressure measurement before and after catalytic oxidation of the hydrogen to water and removal of the water, and pressure measurement before and after diffusion of the hydrogen through a palladium membrane. These techniques have been evaluated on the basis of initial cost, maintenance, speed and accuracy of analysis, and applicable concentration range. The results of this study showed that the palladium-membrane technique is best suited for routine use. FOR some time investigators have been concerned with the origin, form, and effect of hydrogen in steel. In such stdies', the analysis for hydrogen constitutes one of the most important phases. It is quite apparent that the results for hydrogen concentrations in a given steel are dependent on the method of obtaining the sample, storage of the sample until analysis, preparation of the sample, and analysis of the sample, including all the facets inherent in the calibration and operation of an apparatus for gas analysis. There are a number of means available for determining hydrogen. This is a critical study of some of the more common techniques in use today. In most conventional melting and casting methods, hydrogen concentrations of 4 to 6 parts per million (ppm) in steel are quite common. Because of the undesirable effects of hydrogen on steel there has been increased use of techniques such as vacuum melting,' vacuum casting, and ladle-to-ladle stream degassing, which lower the hydrogen content to levels on the order of 1 to 2 ppm. Therefore, the method used for determining hydrogen in steel must be sensitive and precise. In any analytical procedure for gases in metals there are two distinct operations—the extraction of the gas from the metal and the analysis of the extracted gas. To extract the gas from the steel, three methods have been employed: 1) fusion of the sample with graphite at high temperature; 2) fusion with a flux, such as tin, at a lower temperature; and 3) extraction of the hydrogen from the solid sample at a temperature below the melting point of the steel. Fusion with graphite is the least-acceptable method. The blank in this method is higher and more variable than in either of the other two methods. The hydrogen fraction of the total gas composition usually is between 10 and 50 pct; thus, a larger analytical error is possible. The vacuum-tin fusion4 extraction of hydrogen is probably the most rapid method in use today; the extraction time is usually about 10 min. However, with this system a bake-out of the freshly charged tin for 2 hr is necessary and a change of crucible and a charge of fresh tin are required after each day of operation whether one or thirty samples have been analyzed. In addition, frequent checks of blank rates are required since CO and Na are continually being given up by the steel samples dissolved in the tin bath. The composition of the gas in this method lends itself readily to analysis; although the hydroge concentration may fall to as low as 50 pct, more often it is above 90 pct, thus allowing a more precise analysis (because of less interference from other gases). In 1940 ewell' published the hot-extraction method for extracting hydrogen from the solid sample, comparing analysis for hydrogen extracted at 600°C with similar analysis for the gas extracted at 1700°C by fusion with graphite. Good agreement for hydrogen was obtained between these two methods, provided sufficient time was allowed for extraction at the lower temperature. carsone obtained good results in his comparison of this hot-extraction method with vacuum-tin fusion. Subsequent work by Geller and sun7 and Hill and ohnson' has shown that steel samples should be heated to at least 800°C to effect the release not only of the diffusible hydrogen but also of the "residual" hydrogen that may be present as methane. Since the rate of evolution of hydrogene9l0 depends on such factors as sample size and composition, thermal history, and extent of cold work, a fixed extraction time is not possible. Extraction times of 30 min are normal, but 2 hr are not unusual. Induction or resistance heating may be used in the hot-extraction method. With resistance heating the

Jan 1, 1964

By Ralph Hultgren, Prodyot Roy

Manganese vapor pressures from 1250° to 1500°K were measured by conventional Knudsen and torsion-effusion methods in twelve Fe-Mn alloys with compositions from 9 to 80 at. pct Mn. The Knudsen re-sults agveed approximately with previous measurements found in the literature which indicated the solutions were nearly ideal. However, except for the higher manganese compositions, the initial torsion readings indicated much (up to 50 pct) higher vapor presszcres than the Knudsen method. These high readings decreased steadily with time. The results are interpreted as due to depletion of surface concentration of manganese during evaporation. Thus the initial torsion readings are the most nearly correct and Knudsen methods on alloys are to be regarded with suspicion unless it can be demonstrated that diffusion rates are rapid enough to replenish surface concentrations depleted by evaporation. For the lowest manganese contents and highest temperatures, depletion causes initial torsion readings to be too low. FEW thermodynamic data are available for alloys of the high-melting transition metals due primarily to experimental difficulties at the high temperatures involved. Measurement of vapor pressure is one of the most promising techniques to be applied to this problem. From the vapor pressure of a component of an alloy phase, its activity or its partial molar Gibbs energy can be directly calculated. From measurements over a sufficient range of temperatures and compositions the partial and integral Gibbs energies, enthalpies, and entropies may be determined through Gibbs-Duhem integration. For solid phases of variable composition, which commonly are found in alloys, measured vapor pressures are low because of depletion of the surface concentration of the more volatile component as it is selectively vaporized. Diffusion from the interior tends to restore the depleted concentration. The seriousness of the effect depends on the relative rates of diffusion and vaporization. Although depletion has been recognized as a factor,' direct measurements of its rate are lacking and quantitative estimates of its effect on measurements are uncertain. In the present work the vapor pressures above a series of Fe-Mn alloys have been measured by the torsion-effusion method. This method permits a measurement of the vapor pressure of manganese as soon as the sample comes to temperature and continuously throughout the run. The rate of decline of the apparent vapor pressure measures the rate of depletion and the torsion reading at zero time should be correct. At high manganese concentrations (70 and 80 at. pct Mn), the torsion reading remained nearly constant; surface depletion was negligible. There was a slow drop in measured pressure due to bulk loss of manganese from the sample. However, for lower manganese contents, especially at high temperatures, the depletion effect was considerable and the apparent vapor pressure decreased steadily with time. For these alloys the Knudsen method should give pressures which are too low. The measurement of pressure in the Knudsen method cannot be made until enough manganese has been vaporized to be weighable. The Knudsen result is therefore an integrated average between the initial and final vapor pressures. To verify this, conventional Knudsen measurements were also made with results in approximate agreement with previously published Knudsen measurements for these alloys. As expected, for the lower manganese contents the initial torsion readings of pressure were as much as 50 pct higher than the Knudsen. THE APPARATUS The apparatus, shown in Fig. 1, is capable of operating to temperatures up to 2000°K. A vacuum of 5 x 10"6 mm Hg can be maintained. Temperatures were measured to +3° by a W-Re thermocouple placed in the dummy cell, N. The torsion cell consisted of two alumina crucibles with holes in their covers. They were placed in the molybdenum holder shown suspended from the torsion wire. Rectangular torsion wires (1 by 4 mm) were found to have superior sensitivity and less residual distortion than circular (2-mm-diameter) wires. The precision of angular measurement was found to be *0.025 deg; the variation is no doubt due to temperature fluctuation and vibration. For the Knudsen experiments the alumina cell was set on the support, N. SAMPLE PREPARATION 800-g samples were prepared by melting together electrolytic iron and electrolytic manganese and pouring the melt into a water-cooled copper mold. Melting and pouring were done under a helium at-

Jan 1, 1965