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By Henry Lloyd Smyth

In 1891-92 1 was entrusted with the geological survey of part of the large area lying between the Marquette and Menominee iron-ranges in the Upper Peninsula of Michigan, and extending from the Republic trough on the north, through portions of the valleys of the Michigamme and Fence rivers, to and including the intermediate Felch mountain range on the south. Until a few years back the larger part of this area has been very difficult of access, and much of it is difficult still. The rock-surface is for the most part covered with swamp, forest and glacial deposits of various kinds, and therefore has not invited geological study. For these reasons the district, as a whole, with the exception of the Felch mountain range, remained almost unknown from a geological standpoint until our work in 1892. Our main object was to map the pre-Cambrian rocks, particularly the iron-bearing formations of Algonkian or Huronian age, and to obtain as much information as possible with reference to their sequence and structure, In carrying out this purpose, the use of simple magnetic instruments was found to be of the greatest assistance, and indeed indispensable. In this paper the results of our experience in tracing magnetic rocks by means of the disturbances produced in these instruments, have been brought together in systematic form, with such references to the particular area as are necessary in order to illustrate general principles, with the hope that they will prove useful to other workers in the same region, or in other regions where similar conditions may be encountered. The writer was efficiently aided in the field-work by Messrs. Samuel Sanford and Charlea N. Fairchild for nearly the whole period, and E. B. Mathews and H. F. Phillips for part of it,

Jan 1, 1897

By M. E. Wadsworth, G. W. Warren

INTRODUCTION Hydrometallurgical processes for the extraction of metal values can be divided into two broad categories: (a) Processes involving the treatment of high grade material (e.g. finely divided mineral concentrates); and (b) processes which treat lower grade material (ores, waste dumps, etc.). This discussion will be directed primarily toward the first category, but in either case a fundamental knowledge of the intrinsic kinetics and thermodynamics is necessary to understand the behavior of the system. The bulk of research efforts in the last decade along these lines has been aimed at the recovery of copper (1-8). However much information has also been reported on uranium (9, 10) , zinc (11) , cobalt and nickel (12, 13). More comprehensive reviews on these areas are also available (14). As discussed by Sepulveda and Herbst (15, 16) one of the most difficult problems facing process designers is the acquisition and scale-up of reliable information concerning the intrinsic kinetics of leaching systems. The scale-up or modeling of these multiparticle systems is far more complex than that of homogeneous ones. This is due to the numerous rate determining steps which are possible with heterogeneous reactions and the broad distribution of properties of a multiparticle feed such as particle size and mineralogical composition (16). In addition, other factors must also be considered such as interactions between particles, the anisotropic nature of individual particles, the effect of solution chemistry, and electrochemical phenomena. All of these factors must be taken into account, often simultaneously. The thrust of this paper will be to more closely examine how the factors mentioned above can be treated. Some elementary examples of

Jan 1, 1980

By Earl S. Bardwell

The determination of suitable and safe annealing temperatures is one of the most important problems arising in the operation of a copper rolling mill. Certain of the larger mills have worked this problem out for themselves and in these mills the operation has become more or less standardized. In some of the mills pyrometers are used to measure the temperature of the annealing furnaces and careful watch is kept to see that overheating does not take place. In a considerable number of the mills, however, dependence is placed entirely on the judgment of the operator. The almost total lack of literature bearing on this subject seems sufficient warrant for the publication of this paper. ' The discussion of this subject naturally divides itself into two parts: (1) The effect of annealing temperature on physical properties; and (2) changes in the microstructure of refined copper due to cold rolling and annealing. I. The Effect of Annealing Temperature on Physical Properties For the purpose of investigating this phase of the subject six test bars were selected, varying in oxygen content between the limits of 0.036 and 0.070 per cent. The chemical composition of each of these test bars was as follows: Bar Number 1 2 3 4 5 6 Copper + silver...... 99.95 99.92 99.945 99.94 99.95 99.93 Oxygen.............. 0.041 0.070 0.046 0.050 0.036 0.058 As + Sb............. 0.0038 0.0038 0.0038 0.0038 0.0031 0.0031 The bars were heated in an electric muffle to about 1,650" F. and rolled into rods. The rods were annealed, pickled, and drawn to No. 12 B. & S. gauge wire. The wire which was to be used for the annealing test was cut into 38-in. lengths and each length made into a coil 6 in. in diameter. The separate coils were marked so that they might readily be identified

Jan 1, 1915

By H. C. Schultz, F. K. Middleton Hunter

Certain local conditions were known to govern in large measure the successful adaptation of liquid-oxygen explosives to the large-scale blasting at Chuquicamata. The wide variation in hardness of the rock at this mine makes necessary the use of several types of explosives. A locally manufactured, relatively cheap black powder is used in blasting the softer waste and capping material, where a thorough displacement breaks the ground sufficiently. Before the introduction of L. 0. X., an ammonia dynamite of about 65 per cent. strength was being used exclusively in the harder underlying orebody, where a strong disruptive as well as a displacement effect is required for breaking the ore. The L. 0. X., as developed for quarry work in the United States, has a practically pure carbon cartridge material, and the explosive has an extremely high rate of detonation, which should therefore cause it to develop usefully its full disruptive effect in hard ground. The individual blasts at Chuquicamata arc large, black-powder shots which dislodge masses of rock averaging 250,000 tons each, and dynamite shots which dislodge masses averaging 80,000 tons each. It was desirable, therefore, to attempt to displace with L. 0. X. the faster, higher-cost ammonia dynamite used in the smaller blasts. It was not considered practical to attempt to displace the low-cost black powder with 1,. 0. X., as estimated costs showed no probable saving if this were accomplished. Since it was desirable to continue shooting relatively large blasts for effective operation, it was recognized that larger storage facilities than had been in use would be needed for the liquid oxygen. Because of the difficulty of transporting and discharging large storage containers of efficient design, the better plan appeared to be storage and discharge of the liquid at the place of manufacture, and transportation of the filled soaking boxes to the blast. Present Liquid-oxygen Plant An experimental unit with a rated capacity of 75 liters per hour was erected during the latter part of the year 1926 to prove the effectiveness of L. 0. X. at this mine, its cost, and possible efficiency of large-scale storage of the liquid. With this experimental unit 200,000 tons of ore

Jan 1, 1928

By J. L. Tokich, A. R. Troiano

INTRODUCTION SINCE 1921, when Hull' discovered that cobalt can exist in the face-centered cubic and hexagonal close-packed modifications, the transitions that occur in cobalt have been extensively studied. It is generally agreed that on heating the hexagonal lattice changes to the cubic structure at temperatures ranging from 400 to 500°C although considerable doubt exists as to the exact temperature. Data concerning the temperature of the transformation on cooling are much less concordant and their interpretation has not been satisfactory. The study is further complicated by the fact that many investigators have reported the existence of a high temperature allotropic change in the range 850 to 1020°C, at which the cubic lattice reverts to the hexagonal modification. The transition on cooling, which has been reported as occurring at various temperatures from approximately 400 to 100°C, is of particular interest. Troiano and Greninger2 have recently suggested and considered the possibility of allotropic transformations occurring in pure metals by a shear-type, diffusionless (martensite) transformation. The case of cobalt was specifically discussed and certain observations of previous investigators evaluated in terms of this type of transformation. Table 1 briefly outlines the methods and results of previous investigators of the transformation temperatures of cobalt. MATERIALS AND METHODS The major portion of this investigation was performed with cobalt sheet containing a total of 0.2 pct impurities with carbon present to the extent of 0.1 pct. After melting in an induction furnace under an atmosphere of hydrogen, the carbon content analyzed 0.03 pct. Some observations were repeated with hydrogen reduced cobalt compresses analyzing 99.9 pct pure. No significant variations in results were observed employing the as-received sheet, the remelted stock, or the cobalt compresses. Filings for X ray diffraction analysis were sealed in evacuated glass ampoules. Pyrex glass tubing was used for temperatures below 600°C and for higher temperatures clear fused quartz was satisfactory. After appropriate heat treatment at various temperatures, the specimen ampoules were furnace cooled, air cooled or quenched by crushing under distilled water. This allowed a range of cooling velocities from less than one degree C per sec to greater than 1,000°C per sec. X ray diffraction patterns were taken with a Debye camera and filtered characteristic cobalt K-alpha radiation. The proportion of the existing phases was roughly approximated by visual examina-

Jan 1, 1948

By R. Ebeling, M. F. Ashby

The paper is in two parts. The first develops the formulae and method needed to calculate the size, nu)nber, spacing, and volume fraction of hard or inert particles in the interior of a specimen from measurernents made on an extraction replica; throughout, the spread of- particle sizes in a single specimen is taken into account, and the extraction efficiency of the replica is considered. A method for testing whether the particles are randotnly distributed in space is described, and the spacing of randomly distributed particles is discussed. The second Part describes the application of the method to copper containing spherical particles of silica; the description includes an estimate of the errors involved, and a comparison of this with alternative methods. All parameters except uolume fraction can be determined satisfactorily, and the method offers advantages over other electron-,rzicroscopic techniques when dealing with hard particles in a softer matrix, or inert particles in a chem-ically less inert matrix. 1 HE experimental measurement of sizes and numbers of discrete particles of a second phase embedded in a matrix material from opaque, plane sections has been considered by many authors, notably by Fullman.' It is assumed that, when the specimen is sectioned, the particles are also sectioned, so that the diameters of the circles of intersection of particles with the plane of the cross section ("surface diameters") are measured. It is difficult to derive the distribution of true particle diameters ("volume diameters") from measurements of the distribution of "surface diameters" on a plane section. The measurement of size and numbers of small second-phase particles by transmission electron microscopy through thin foils of matrix containing the particles has been described by Cahn and ~uttin~' and by ~illiard.~ Because of overlap and the fact that particles which intersect the foil surface may be sectioned whereas those in the bulk of the foil are not, it is again difficult to measure the true distribution of particle sizes. The use of replicas for this sort of measurement has not been analyzed in detail. A replica made from an opaque cross section, thus replicating the circles of intersection of particles with the plane of section, is analyzed by Fullman's method and suffers from the same difficulties. Under certain circumstances, however, extraction replicas can be used, and offer a special advantage in that they make the determination of the true distribution of particle diameters particularly simple. It is the purpose of this paper to describe this extraction replica method. Consider the example of an alloy consisting of SiOz particles, whose mean diameter is about 1000A, dispersed in a copper matrix. When the alloy is sectioned and mechanically polished, the particles are not sectioned, because they are much harder than the matrix, and so will be either left in the surface or pulled out whole, and because the particle size is smaller than the abrasive size of even the finest abrasive. The particles are chemically inert in solutions which chemically etch or electropolish the matrix, so that chemical treatments do not section the particles either. (Experimental measurements of particle shape in this alloy confirm this—truncated particles are never seen.) Small, hard or inert, particles are therefore not sectioned when the specimen is sectioned and polished. An extraction replica taken from this polished surface shows the true "volume" diameter of each extracted particle; the distribution of diameters seen on the replica is the surface distribution of true "volume" diameters, and the volume distribution of true "volume" diameters is easily derived from it. The extraction replica method is not subject to the difficulties associated with sectioning of particles, and avoids the problem of overlap from which the transmission method suffers. The method is well-suited for studying hard particles in a soft matrix. Examples are provided by internally oxidized alloys, oxide-dispersion strengthened metals like T.D. Nickel, and carbides, nitrides, and strong intermetallic compounds in metals. It should be possible to adapt polishing techniques in alloys containing softer but inert particles to avoid sectioning the particles (say by electropolishing or etching). The method is tested and illustrated in Sections 8 and 9 by applying it to a dispersion of spherical SiO2 particles in a copper matrix. I) SYMBOLS Symbols are defined where they first appear in the text. Volume fractions of particles are denoted by the symbol f, particle diameters by x, center-to-center particle spacings by D, and numbers of particles by N. Mean particle diameters and standard deviations about these means are denoted by x and a. Both arithmetic (subscript A) and geometric (subscript G) means are employed. In this paper we measure the distribution of true diameters of particles which touch or pass through a random-plane section of the specimen. We may want to know the distribution of particle diameters in the

Jan 1, 1967

By R. D. Reiswig, J. M. Dickinson

The 0s-Ir equilibrium diagram was determined. The diagram is of the simple peritectic type, with a peritectic temperature of about 2660°C. The solid miscibility gap is narrower than previously reported, the nearly vertical solvus lines occurring at about 42 and 63 wt pct 0s. Widmanstaetten figures resembling martensite in some of the two-phase alloys account for a previously suspected transformation. In view of the long history of use of such alloys, it is surprising that the 0s-Ir equilibrium diagram has not yet been completely determined. The boundaries of the miscibility gap in this system have been estimated to be between 24 and 39 wt pct 0s and 79 and 100 wt pct OS. It has been predicted3 that alloys of ruthenium, osmium, and rhenium with the fcc platinum metals should solidify peritectically in their two-phase regions. The metallographic examination of natural osmiridium alloys has been said4 to indicate, by the presence of a martensitic structure, the existence of a transformation or a phase separation. On the basis of superconducting transition temperature measurements, a 70 at. pct 0s alloy was found5 to be two-phase prior to annealing. EXPERIMENTAL The elemental components used in this work were obtained from several suppliers as sponge. The purities, stated by each supplier to be in excess of 99.8 pct, were confirmed in each case by a semiquantitative spectrographic analysis. The pure components were premelted in an inert-gas tungsten arc furnace with the evolution of some fume, crushed, and pickled for use as alloy melting stock. Upon arc melting to the final compositions, no fume evolution was observed. Because weight losses of the order of 15 mg or less were observed in preparing alloy buttons weighing 15 g, "synthetic analyses" were used in determining the compositions of the alloys. Alloys used in this investigation contained 15, 20, 33, 40, 42, 43, 45, 50, 55, 60, 63, 64, 66, 70, 79, and 80 wt pct 0s. Heat treatments of the alloy buttons and pieces thereof were performed in a previously described6 tungsten tube furnace under pressures of 105 torr or less. It was found that homogenization treatments on the specimens were essential to remove the severe coring which was present, a 3-hr treatment above 2300°C removing all the metallographi-cally visible evidence of coring. Following the various heat treatments, the specimens were "vacuum-quenched" by melting a tungsten fuse wire and allowing them to drop onto a water-cooled copper plate. In a few instances, specimens were quenched into molten tin for comparison, but no difference was apparent. Vacuum-quenched specimens cooled from 2400°C to below a red heat in less than 60 sec. Typical equilibration times varied from 3 hr above 2300°C to 88 hr near 1100°C. The utilization of successively longer equilibration times and the approach to equilibrium from both directions indicated that the times used were sufficient to give a close approach to true equilibrium. Heat-treatment temperatures were measured with a calibrated Leeds and Northrup optical pyrometer through a 0.120-in. lateral sight hole in the tungsten heater tube. It was known that the assumption of black-body conditions inside the 1-in.-diam by 10-in.-long tube was unwarranted. The empirical results of work with thermocouples and melting

Jan 1, 1964

By Arthur Taggart

A GENERAL awakening of interest among mill men concerning the mechanical efficiencies of their crushing machines is evident from a perusal of the recent files of mining publications. Considering the large part of the power bill which must be debited to the crushing department, such. interest is natural. When, however, the articles on the subject are read, the only statement upon which the writers agree is that fine grinding consumes a large amount of power, and that the machine which, from a concentration standpoint, offends as a slime producer is, for that reason, a serious offender in wasting power. When the mill man attempts to find a method for measuring the power wasted, or to compare the efficiency of one machine with that of another for the same work, he is confronted with a choice of methods which lead to conflicting results. There are two reasons why the work of crushing is not more generally understood. In the first place, experimental data are difficult to obtain; and in the second place, before these data can be put in general form certain assumptions must be made. A difference in these assumptions by different investigators has led to conflicting conclusions. This conflict has resulted in the proposal of two laws. The first of these is the so-called Rittinger's law, which is variously stated as follows: . "The work of crushing is proportional to the reduction in diameter."-R. H. Richards: Ore Dressing, p. 304 (1903). "The Work required to crush rock is very nearly proportional to the reciprocals of .the diameters crushed to."-A. Del Mar: Engineering and Mining Journal, vol. xciv, No. 24, p. 1129 (Dec. 14, 1912). "The Work done in crushing is proportional to the surface exposed by the operation, or better expressed for this purpose, the Work done on a given mass of rock is proportional to the reciprocal of the diameter of the final product, assuming that all the mass has been reduced to one exact size, which is only theoretically possible."- A. 0. Gates: Engineering and Mining Journal, vol. xcv, No. 21, p. 1039 (May 24, 1913).

Jan 1, 1914

By Ian Wark

IT has been shown1 that in the absence of heavy metal salts, the nature of the alkali used to promote differential flotation-whether caustic soda, lime or sodium carbonate-is unimportant. The hydroxyl ion is the active depressant upon which differentiation depends, and the pH value determines whether a film of collector forms on any given mineral surface. Even when sodium cyanide is used in conjunction with alkalies, it is the pH value and not the nature of the alkali or its concentration that is important, for upon the pH value alone depends the fraction of the added sodium cyanide that is present as cyanide ion, which is the true depressant. When heavy metal salts become dissolved from partly oxidized ores, or are added intentionally as activators, conditions are different, and metallurgists have found that lime and sodium carbonate do not give identical results, even when added in amounts sufficient to produce the same pH value. In the few instances in which we had attempted to confirm this view, we had failed to do so, for, with nothing to guide us, we had inadvertently chosen solutions that gave contact curves of a "stand-ard type," which correspond to conditions of ready floatability. Now, however, we find that, in the presence of copper salts, and within a restricted range of reagent concentrations, the nature of the anions present is important, and that sodium carbonate does influence the results, apart from the usual effect due to its influence on pH value. With the recognition of this anion effect, and with the control of temperature already introduced,' it appears that the factors of major importance in connection with this set of reagents have been taken into consideration, and that the results obtained and the conclusions drawn from contact tests will be of more immediate value to the operator.

Jan 1, 1939

By C. A. Czako

INTRODUCTION In recent decades sintering and pelletizing of finely divided materials have become the primary tonnage producing modes of agglomeration. This statement is especially true in the iron and steel industry and, to a lesser degree, in the nonferrous, chemical and non-metallic minerals processing industries. In every industry the main objectives in agglomerating fines are essentially the same, namely to convert ores, minerals and chemicals of undesirable fineness into agglomerates characterized by a size consistency desirable for subsequent use or processing. Depending on the type of agglomeration process selected and the conditions maintained during agglomeration, the physical process of increasing size is complemented by a number of other unit processes. These processes can occur simultaneously, consecutively or in an overlapping manner. Some of these additional unit processes are incidental to the agglomeration operation, but at the same time can be critical, depending upon the subsequent use of the product. Accordingly, during processing, conditions have to be controlled to either suppress or enhance the extent of completion of these unit processes. The purpose of this report is to review laboratory testing as the basis for engineering modern sintering and pelletizing plants. Considering that most typical applications are for the iron and steel industry, agglomeration of ferrous materials is reviewed and discussed. When these total processes are adapted to suit non- ferrous materials, chemicals, or non-metallic substances, the over- all approach remains the same; only the processing parameters are affected as necessitated by the different nature of the materials.

Jan 1, 1977

By R. J. Piros, Brusenback, D. A. Dahlstrom

DEWATERING fine coal has been a serious problem to many operators who desired to wet-wash finer sizes and maintain high recovery. Centrifugal driers have become popular for this purpose for sizes between 3/8 in. and 14 mesh. Below 14 mesh the perforated screen centrifuges lose a large per- cent in the effluent solid bowl types that do retain -14 mesh coal, produce excessive degradation, tend to retain the highest ash fraction in any size fraction, and are subject to abrasion, which results in higher maintenance. In 1949 Truax-Traer Coal Co. planned a cyclone installation at their Ceredo preparation plant to recover coal down to 150 mesh with approximately a 14-mesh top size. Since available centrifugal equipment was not considered satisfactory, an investigation of rotary vacuum filters was begun in cooperation with the Peterson Filters and Engineering Co. to determine the suitability of the Peterson Top Feed Reservoir (TFR) filter. This investigation, which is described below, has resulted in a highly satisfactory installation of two 6x10-in. Peterson TFR filters that have been in operation over a year. After some preliminary laboratory batch vacuum filter tests, a pilot plant double-drum Peterson TFR filter was installed at Ceredo to prove the feasibility of vacuum filtration and determine optimum conditions. The full scale units were then installed on the basis of the pilot plant results. This was followed by an extensive research program on vacuum filtration in the laboratory at Northwestern University to investigate basic design and operating variables and their influence on final moisture con- tent of the filter cake. A method of scale-up from laboratory batch tests to the full-size unit was also proposed and proved. Because of the importance of dewatering fine coal today, it was felt that the results of the three steps should be made available for the use of others facing this problem. The work at Northwestern is given in a theoretical section following the discussion of the pilot plant and full- scale operation. Fig. 1 is a flow diagram of the cyclone and filter installation. The feed is drawn from below the

Jan 1, 1952

By Lawrence Adler

In-situ rock has well-recognized rupture and yielding responses. Attention is called to an intermediate response, granulation, which consists of an evenly distributed, small-scale crumbling accompanied by swelling. Granulation results in a negative slope for the inelastic portion of the stress-strain curve as successive interlocks are destroyed, and the load-carrying capacity of the material is reduced. Volumetric swelling with softening also takes place. The prerequisites for such a response are moderate confinement and a uniformly distributed defect pattern. Since rock masses, as well as rock as an intact material, have such patterns in their jointing and texture, respectively, granulation is characteristic of them. The presence of granulation can be demonstrated for a very wide scale, ranging from laboratory testing to regional geologic phenomena. The response of an engineered structure is considered in detail. Granulation appears to be dependent upon internal moments, the formation of which can be controlled by engineering design. The practical implications of such control can be significant in optimizing underground instability and in improving excavation techniques. Rock is usually considered to behave inelastically under high load, by fracturing as a brittle material, or by yielding as a ductile material, ignoring time dependency. These responses, which are characteristic of metallic behavior, appear idealized in Fig. 1, where linear-elasticity approximates the initial behavior. However, another major deformation mechanism peculiar to rock has long been recognized in geology, the granulation of an interlocked material. Granulation consists of a uniformly distributed fracturing and crumbling of the material, accompanied by swelling and softening. Predictably, the associated inelastic portion of the load-deformation curve has a negative slope,

Jan 1, 1971

By Howard Eavenson

SOME time ago, in a conference considering the mechanizing of a group of mines, I was asked if I knew of any data showing the relative frequency of accidents due to the use of 275 or 550-volt current inside mines and having a recollection of seeing some in print, the answer was made that I would find what was available. Subsequent search failed to find any pub-lished records of any kind giving such figures and none of the compensation agencies of whom inquiry was made were able to supply any, excepting the Pennsyl-vania Compensation Rating and Inspection Bureau, which had some data covering a few months for some companies in that State. The inquiry was confined to the three largest producing States, Pennsylvania, West Virginia, and Illinois. The inspection departments of neither of the first two had any such records, and in Illinois, only 275 volts has been allowed inside the mines for many years. A laborious inquiry has resulted in the data, shown in Table 1, which on this account was confined to the years 1921 and 1925, the latter being the latest figures available. In each State, to find the mines using 275 and 550-volt current respectively, it was necessary to list the mines from the Coal Catalog, and then to complete the list by inquiries from the companies directly, from Operators' Associations and from Inspection Depart-ments. As the mines not electrified, and those using

Jan 5, 1928

By Gilbert Santoro

In this study tantalum carbide filaments of various compositions in the fcc region were prepared by heating a tantalum wire in a measured amount of hydrocarbon vapor. Such properties as tensile strength, transverse-rupture strength, microhard-ness, lattice parameter, electrical resistivity, and magnetic susceptibility were measured as a function of carbon content. Some of these properties showed a maximum or a minimum between a carbon-to-tantalum molar ratio of 0.80 and 0.85, the composition range at which the color changes from metallic gray to gold. The recent literature has shown that in the large homogeneity range for the fcc phase of the Ta-C system there is a marked variation for such properties as microhardness,' electrical resistivity, ' thermodynamic properties,z'3 lattice parameter and superconductivity. In addition to the technological interest of these variations within a single phase, important theoretical benefits may ensue from a continuous investigation of properties vs stoichiometry in tantalum carbide and other refractory defect compounds, for example the effect of the metal-metal distance and crystal structure upon bond formation and electronic structure. Whether there is a similar variation of the tensile strength is of practical importance. Of theoretical interest would be the knowledge of how the magnetic susceptibility varies with carbon composition. Both of these properties, as well as the transverse-rupture strength, were determined for tantalum carbide filaments in the fcc phase region. The lattice parameter, the electrical resistivity, and the microhardness were also investigated and compared with values appearing in the literature. EXPERIMENTAL PROCEDURE Material Preparation. Tantalum carbide specimens of various carbon content were prepared by statically carburizing high-purity tantalum filaments in measured quantities of pure hydrocarbon gas. The filaments, which were 10 mil in diameter and 20 or 40 cm long, were heated by their own resistance at temperatures from 1800" to 2200°C using alternating current in some cases and direct current in others. Tantalum wire from two sources was used. One had a reported purity of 99.96 wt pct Ta. The ingot from which this wire was drawn had been electron beam-melted as the final step in its purification. The reported purity of the other wire, which was prepared by a powder metallurgical process, was 99.88 wt pct Ta. The impurities of both tantalum sources are listed in Table I. Spec-trographic-grade toluene or research-grade propane was used as the source of carbon. The apparatus for the carburization of the filaments is shown schematically in Fig. 1. The system was evacuated to 1 x l0-' mm of Hg when using the electron beam-melted tantalum and to less than 1 p when using the less-pure tantalum. Neither the difference in the base vacuum, nor in the hydrocarbon gas, nor in the tantalum filaments resulted in any detectable difference in the properties studied in this work. However, only the carbides prepared from the higher-purity tantalum were used in the magnetic-susceptibility determinations. Once the base vacuum had been reached, the system was flushed with the hydrocarbon and re-evacuated. For any desired composition of the carbide, hydrocarbon gas was allowed to leak into a constant-volume flask to a predetermined pressure. These pressures were measured by a Cartesian diver-type mercury gage with a range from 0 to 20 mm and with a scale expanded to nine times. The hydrocarbon gas was allowed into the reaction tube and the filament was quickly raised to the reaction temperature. The slack in the filament due to thermal expansion was taken up by drawing out the movable electrode with a screw mechanism. The filaments were kept at temperature from a few minutes to 200 hr. In the majority of cases the heating time was 6 hr. The reaction tube was cooled by cascading water on its outer surface. By means of an ammeter and a voltmeter the electrical resistance at the reaction

Jan 1, 1963

By William B. Phillips

The concentration of natural magnetites has been carried on in this country for several years, and more or less information has been collected on the subject. Various inventors, availing themselves of the magnetism which is inherent in such ores, have devised machines for separating the impurities from the ore by means of the electric current; and a greater or less degree of success has rewarded their painstaking and persevering efforts. We are now fairly in position to judge of the value of the process as applied to such material. It is not my purpose to speak of this matter further than may be required by the emergencies of the case. I shall assume that most engineers and metallurgical chemists are already acquainted with what has been done at the Chateaugay mines, at Mineville, at the Benson mines, at the Weldon and Ogdensburgh mines, and at Cranberry; although, at this latter place, there has not been so much done as we could wish. I shall not now speak of the various types of separators. From the time of William Fullarton, to whom was granted an English patent, in 1792, for separating iron-ore by the application of magnetic attraction, down to the present time, a great. many devices have been suggested, and a great many patents taken out for this purpose; but it is not necessary now to enter upon a discussion of their merits. Perhaps, at some future meeting of the Institute, after we shall have experimented further with some of the machines on the market, there may be an opportunity to contribute something to the current knowledge of the efficiency and economy of separating-machines. In this paper I propose to give, as briefly as possible, the results already reached in converting a non-magnetic ore into magnetic ore, and then concentrating it over a magnetic separator of the alternate-polarity type. I am aware of the work

Jan 1, 1896

By Charles L. Mantell, Kurt Straler

The hydrogen reduction of Cr2O3 to chromium metal was found to be feasible at very low water-vapor concentrations, corresponding to dew points of -38° to -24°C, over a temperature range of 1130" to 1490°C. Hydrogen reduction under these conditions was predicted by the calculated equilibrium curves which also indicated that CrzOs is reduced directly to chromium without forming the intermediate oxide, CrO. This reduction path was confirmed by X-ray diffraction analysis. The percent reduction of Cr2O3 at each reaction temperature was constant with time, suggesting an inhibiting effect of water vapor. A small increase in the residual water-vapor concentration of a single temperature, 1490°C, strongly retarded the rate of reduction This effect was expressed by an empim'cal equation which indicated a direct relationship between "distance from equilibrium" and the rate of reduction. me effect of temperature over the range of 1130" to 1490°C was expressed in an Arvhenius plot of log rate vs reciprocal absolute temperature. From this curve the apparent enthalpy of activation was found to be 29,600 cal. Based on the hypothesis that the rate of reductiun is contvolled at the oxide-metal interface, an over-all rate equation consistent with the experimental data and the thery of absolute reaction rates was formulated. A simplification of this expression to an Arrhenius equation was justified by the overriding effect of temperature on the rate of reaction for the minimum water-vapor concentration range. MOST of the metals in Subgroup V1 of the periodic table can be prepared commercially by direct reduction of their oxides by hydrogen or carbon monoxide, at temperatures considerably below the melting points of both the metals and their oxides. Chromium is an exception, being generally reduced from its ore, Cr2O3 . FeO, by silicon in an electric arc furnace which operates above the melting point of the Fe-Cr alloy or above the melting point of chro- mium if a chromium oxide be the starting material. In reduction of chromium oxide by hydrogen, either reduction does not occur at all or the rate of reduction is extremely slow. Theoretical considerations based on the high, exothermic, free energy of formation of Cr2O3 compared to the oxides of the other Subgroup VI metals, molybdenum, tungsten, and uranium, would also suggest a slow rate of reaction and a high activation energy. Interest in the direct gaseous reduction of fine-powdered ores in fluidized beds was considered justification for examination of this reaction. In order to develop a basis for a continuing study of the commercial feasibility of the direct gaseous reduction of chromite, a study of the kinetics of the reduction of Cr2O3 with hydrogen was undertaken. To the authors' knowledge no accurate kinetic data for this reaction have been obtained. Neither has an activation energy been determined nor has an attempt been made to establish a mechanism of reaction. LITERATURE Maier10 compared the data of I. Y. Granaat,6 H. von Wartenburg and S. Aoyama, and G. Grube and M. Flad7 with that derived from calorimetric and ther-modynamic properties for the equilibria for the reduction of Cr2O3 with hydrogen. These results, plotted as the log of the equilibrium constant vs absolute temperature for the reduction of Cr2O3 and the intermediate oxide, CrO, to chromium, show agreement between the differently derived data. In both cases the equilibrium constants were extremely low. Maier showed that, over a temperature range of 1000° to 2000°K, Cr2O3 is more readily reducible than CrO. Granat assumed that CrO was preferentially formed from Cr2o3 above 1100°C. Grube and Flad's analysis of their reaction products in the 895" to 1000°C range indicated the coexistence of only Cr2O3 and chromium. The hydrogen reduction of the other Subgroup VI metals, molybdenum, tungsten, and uranium, shows that reduction of the higher oxide proceeds through all of the intermediate oxides before being reduced to the metal. Since evidence pointed to an anomaly in the reduction behavior of Cr2O3, the authors investigated the reduction path of Cr2Os.to chromium. This was done theoretically with more recently available free-energy data and experimentally by X-ray diffraction analysis. This work reinforces Maier's conclusion.

Jan 1, 1964

By H. F. Korman, M. C. C. Mow, P. K. Dai

INTRODUCTION Detonations of high explosives in soil and rock have been used frequently in civil engineering applications. Of particular interest in recent years has been the development of test methods to simulate the desired blast and shock environments for the testing of protective structures. The United States Air Force, in particular, the Air Force Weapons Laboratory, in conjunction with the Defense Atomic Support Agency, has in recent years, developed special technology for simulation testing of protective structures in soil and rock media. Such a technology, although initially developed for military applications, is rapidly finding its way into civil applications. One of the major problems in the design of the simulation test is the correct prediction of ground motion induced by the detonation of high explosives. This paper presents a useful prediction method which is developed specifically for ground motion in rock that is induced by the detonation of a buried planar array of explosive columns (See Figure 1). The technique of simulating shock environment using such an array is called the Direct Induced High Explosive Simulation Tech- nique (DIHEST). Normally, each shot hole may contain canisters of ammonium nitrate positioned at various depths, or a slurry explosive with detonators positioned along its length (See Figure 1). The depth and width of the array, the spacing of shot holes, the spacing of detonators, the degree of containment, and the charge weight are the variables which govern the induced ground motion

Jan 1, 1971

By F. A. Schaufelberger

Early work on chemical precipitation of metals from metal salt solutions is reviewed. The chemistry and thermodynamics of precipitating copper, nickel, cobalt, and cadmium metals by reaction with hydrogen are discussed. Mechanisms of metal precipitation, nu-cleation, growth, and agglomeration are reviewed, as well as some solubility phenomena of cleation,gases and solids at elevated temperatures. Experimental data presented deal mainly with the reaction of copper sulfate solution with Hz. METAL can be recovered from a leach solution either indirectly by precipitation as a compound that is later reduced or directly by electrolysis, cementation, or chemical reduction, for example, with hydrogen. The widely used electrowinning processes suffer from the inefficiency of converting fuel to low voltage dc and from low current efficiency when complete recovery is attempted. With the batch hydrogen reduction methods outlined here, a unit of fuel converted to hydrogen in modern gas reform plants will make two to three times as much metal as can be obtained with electrolysis. With continuous hydrogen reduction, four to six times as much metal is obtained. Precipitation by reducing a metal salt solution with H, has been known for almost 100 years.' Commercial use of the process, however, awaited the research and development program initiated by Chemical Construction Corp. Within the last few years this program has brought about construction of commercial plants, listed on p. 701. Ideal hydrogen reduction will precipitate a pure metal from a solution obtained by commercial leaching methods at a rapid rate without excessive temperatures and pressures. The metal precipitate will be of desired size and density, less than a percent left in the vessel being deposited on the wetted parts. The present discussion will outline Chemical Construction Corp.'s early development program and will discuss the chemistry and mechanics of reducing copper, nickel, cobalt, and cadmium from solution by H2. Work on selective reduction of nickel from cobalt has been described earlier.2 The article is not concerned with precipitation of copper by disproportionation of cuprous solutions where yield is limited" to 50 pet.* It does not discuss use of gaseous reducing agents other than hydrogen, such as SCV which may lead to contamination with sulfur, or CO," which is considerably more expensive than hydrogen and produces a gaseous reaction product, CO2.† The article does not include use of other nongaseous reducing agents: which are far more expensive than CO. Also, notes on the history, engineering design, and performance of commercial plants have been given elsewhere." It will be shown that a pure metal can be precipitated by reduction with hydrogen from solutions obtained by commercial leaching methods when the solution cohposition is controlled and proper acidity, proper metal ion concentration through controlled complex formation and hydrolysis, and adequate agitation for suspension of metal and for transfer of reducing gas are maintained. Reasonable temperatures and pressures are used which are less excessive than those used by previous workers, although they are maintained at above equilibrium values because of process kinetics.' It has also been found necessary to induce nuclea-tion and to control growth and agglomeration in order to get a powder product of suitable physical properties. Review of the Literature Muller, Schlecht, and Schubardt of I. G. Farbenm claimed a successive reduction of silver, copper, nickel, cobalt, and zinc from ammoniacal solution by applying progressively higher temperatures and hydrogen pressures. Metals produced by this technique were not pure, since no attempt was made to adjust the solution composition between the different reductions. It is doubtful that the zinc product contained any metallic zinc. The major contribution to the literature" was made by the Ipatiews,12 who prepared platinum, iridium, copper, nickel, cobalt, lead, tin, arsenic. antimony, and bismuth at often extreme conditions, up to the critical temperature of water (373"C), at 1500 to 7500 psi, for as long as several days. Even cadmium and zinc were claimed to have been observed in trace quantities precipitated together with basic salts. In the early experiments solutions were not stirred. Extensive formation of oxides and basic salts occurred. probably long before sufficient hydrogen could be supplied in the unstirred liquid to decrease the metal concentration in solution by reduction. The importance of hydrogen pressure was

Jan 1, 1957

By R. F. Hollis, C. K. McArthur

PRIOR to the application of anion exchange, all recovery of uranium from acid leach liquors precipitated an impure product requiring further upgrading before it could be refined. The ion exchange process, on the other hand, provides excellent selectivity for extracting soluble uranium from leach liquors, so that high grade concentrates can be produced directly. The discovery that uranium is readily adsorbed by anion exchange resins, together with the experience of resin and equipment manufacturers in water treatment, led to rapid development of ion exchange in a multiple column operation. Many processing plants using fixed bed ion exchange are in operation or under construction in Africa, Australia, and Canada. There are a limited number in the U. S. Although the fixed bed process has been highly successful, the feed to the ion exchange columns must be a clear solution, which is obtained by filtration or by countercurrent decantation of leached pulps. With some ores, poor filtration or settling characteristics make production of a clear solution difficult. Most processing plants in the U. S. receive their ores from a number of small mines, and there is considerable variation in the settling and filtering behavior of the ores. An ion exchange process was therefore desirable in which the uranium could be recovered directly for the leached pulp by adding ion exchange resin, which could be then separated from the pulp by a screening operation. The process would thus resemble the cyanide-charcoal process in which gold is adsorbed from cyanide pulp by means of activated charcoal. Preliminary tests in which leached pulps were directly contacted with resin beads led to the development of the RIP process.

Jan 4, 1957

By R. W. Smith, K. H. Lee

Bond type simulated closed-circuit grindability tests and batch grindability tests were run on six pure minerals plus a limestone and a taconite ore. The simulated closed-circuit tests were made at five different meshes of grind. The minerals tested varied widely in hardness and breakage pattern. For all simulated closed-circuit tests both Bond and Holmes work indices were calculated and compared. The Bond grindability testlm6 has been widely and quite successfully used for predictions of such items as ball mill power requirements and as an aid in plant comminution equipment selection. The test is interesting in that although run as a series of batch tests it is over-all a simulated closed-circuit test with a circulating load of 250%. The simulated closed-circuit feature is probably the primary reason for the notable success of the test. Perhaps the major criticism that can be brought against the test is that it is time consuming, since it normally takes a trained technician about an eight-hour shift to perform it.4 For many purposes this is an acceptable time requirement. However, if a grindability test is to be used for mill control purposes it should be performed in as short a time interval as possible, preferably under an hour. Sometimes in industry strictly batch tumbling mill tests are run and an attempt is made to correlate such batch tests with plant mill operation. Then an attempt is made to adjust operating tumbling mills based on data from the tests. The tests, however, frequently do not correlate well with operating data. The purpose of the present work was to explore some of the similarities and differences between a simulated closed-circui.t grindability test and a batch type test. Six different minerals plus a limestone and a taconite ore were tested in the experimentation. These materials varied widely in hardness, breakage characteristics, etc. Standard dry Bond grindability tests were mn on all materials at 48, 65, 100, 150 and 200 meshes of grind. Feed material was prepared by stage cmshing to -6 mesh. Initial feed volume was 700 cc. Care was taken to maintain the standard constant weight (about 20125 gm) and number of balls (283) during all the tests. Rotational speed was 70 rpm. Table I lists the materials studied along with pertinent data regarding the materials and Bond grindabilities obtained. In addition, dry batch tests were performed on all materials. These tests were made in the same mill as was used for the Bond tests. An identical ball charge and an identical feed volume were used. After rotating the mill for a predetermined number of revolutions at the same rotational speed as for the Bond test, the material was removed and separated from the ball charge. A screen analysis was performed on this product. Knowing the original size distribution of the feed and the size distribution of the product, it was possible to calculate the grindability or grams of a particular mesh produced per revolution of the mill. After the screen analysis of the product, the various fractions were recombined and placed back in the mill for further grinding. After grinding for additional revolutions of the mill the procedure was repeated. Thus, it was possible to obtain grindabilities for each material at a number of meshes of grind and for various revolutions of the mill. Grind-abilities obtained from batch tests are shown in Table 11. COMPARISON OF BOND AND BATCH GRINDABILITIES Figs. 1A through 1D show relationships between batch and Bond grindabilities. Figs. lA, lB, 1C and 1D show respectively graphs indicating the relationships for batch tests run for 100, 300, 500 and 700 revolutions of the mill. For a particular material on each graph, points are shown for 200, 150, 100, 65, and 48 meshes of grind except for several missing coarse meshes of grind for galena which did not fall conveniently on the figures. For each material and graph the point nearest the origin is for 200 mesh, the next for 150 mesh, the next for 100 mesh, etc. Considering Fig. lA, it is interesting to note that all relationships shown are essentially straight lines. There are, however, considerable differences

Jan 1, 1969