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By A. A. Smith, J. S. Smart, A. J. Phillips

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By A. J. Phillips, A. A. Smith, J. S. Smart

The preparation of a sufficient quantity of high-purity copper for extensive laboratory use in the study of impurity effects has been an integral part of a research program in progress at the Central Research Laboratory of the American Smelting and Refining Co. for the past several years. Initially the degree of purity desired was that necessary to meet two essential requirements for experimental accuracy: (I) no impurity was to be present in the copper in an amount capable of producing a detectable effect on the properties to be studied, (2) even the minor changes in propertties caused by the addition of extremely small amounts of individual elements were to be measured without significant interference from contaminants. In the course of the investigation, evidence has accumulated to justify the conclusion that this copper is of exceptional purity; in fact, no impurity can be detected by any chemical method or spectrographic technique known to the authors. The present paper describes the method of production of the copper and presents some of its properties. Preparation oF High-purity Copper The elimination of impurities from commercial electrolytic copper is accomplished by a three-step purification process. The first operation consists of an electrolysis through a purified CuSO4-H2SO4 electrolyte using bagged anodes, low current density (5 amp. per sq. ft.) and low tem- perature (25°C max.). The electrolyte is prepared from commercial Cu2SO4 and is purified by heating the solution and adding I gram Fe as Fe2(SO4)3 to each 100 grams dissolved copper; sufficient hydrated oxide of copper, prepared from Cu2SO4 and NaOH, is supplied to precipitate Fe(OH)3, which carries down arsenic, antimony, tin, selenium, tellurium and other minor constituents. Silver and remaining traces of lead are removed by addition of Na2S to the acidified filtrate, which is then reatered after standing hot overnight. The cold solution is made up to 30 grams per liter Cu and 150 grams per liter H2SO4 and introduced without addition agents into the electrolytic system, which consists of a double row of hard-rubber battery boxes with the inside webbing and partitions removed, arranged in seven steps of ascending height. Electrolyte is uniformly supplied to the two highest cells by glass siphons operating from a constant-level reservoir, and flows by gravity through the bank of seven cells, entering each at the bottom and leaving at the top. Glass air lifts continuously supply the returning liquid to the constant-level reservoir for recirculation. Each cell contains three 4 3/4 by 4 3/8 by 1-in anodes cast from high-quality electrolytic wirebar copper, various lots of which have been used with equal success. The anodes are pinned to sheet copper hangars shaped to prevent crawl of the electrolyte to the multiple-wired bus bars—which would result in fouling of the contacts—-and hang inside wool flannel bags stretched over open wood frames. The deposit

Jan 1, 1941

By A. A. Watts, R. I. Jaffee, F. C. Holden, H. R. Ogden

Hypoeutectoid Ti-Cu alloys are responsive to heat treatment, and considerable variation of mechanical properties may be produced by transformation of the ß phase. Control of cooling rate, isothermal transformation, or quench tempering determine the transformation structure and properties. The transformation products are similar to those of carbon steel. THE equilibrium diagram for the Ti-Cu system has been studied by various investigators, and the most recent diagram is that determined by Jou-kainen, Grant, and Floe.' The titanium-rich portion of this diagram is reproduced in Fig. 1. The alloy compositions and annealing temperatures used in this work are shown. The Ti-Cu alloys containing up to 17 wt pct Cu are representative of an active eutectoid alloy system. Joukainen et a1.l have stated that ß phase cannot be retained on quenching and this has been confirmed in the present work. The similarity between the Ti-Cu system and the Fe-C system is evident and, as will be shown later, many of the transformation products appear to have similar microstructures. Heat treatments in this program were designed to produce the structures of primary interest for study and determination of mechanical properties. Experimental Procedures Preparation of Alloys: Five ½ lb ingots, ranging in composition from 0.8 to 6.83 pct Cu, were prepared by double arc melting in an atmosphere of high purity argon. Titanium melting stock was obtained from high purity iodide titanium, and copper additions were made from copper wire clippings. Segregation was reduced by inversion melting, in which the once-melted ingots were inverted in the crucible and remelted. The double-melted ingots were forged at 1600°F to ¾ in. diam rods, with both heating and forging operations being carried out in air. Surface scale was removed by grit blasting and grinding, after which the forgings were vacuum annealed at 900°C. The alloys then were swaged to ¾ in. diam rod at 750°C and test specimens were cut from this material. The vacuum annealing operation was to remove dissolved hydrogen, which is commonly present in the iodide titanium as-received. Although vacuum fusion analyses were not obtained for all these alloys, past experience indicates that the 6 hr treatment with a limiting pressure of 10- to 10-5 mm of Hg is sufficient to reduce the hydrogen level to 10 to 30 ppm. Vacuum fusion analysis of the 0.8 pct Cu alloy showed 19 ppm of hydrogen. In addition to the five hypoeutectoid alloys, three 15 g ingots were prepared with nominal copper additions of 9, 10, and 11 pct. Fabrication procedures were similar, except that these alloys were rolled to 0.040 in. sheet. Microstructure specimens only were obtained. Table I shows analyzed compositions and fabrication temperatures for these alloys. Heat Treatments: All heat treatments were made in potentiometer-controlled, resistance-wound tube

Jan 1, 1956

By Quentin D. Singewald, B. S. Butler

Some of the broader relations between structure and ore deposition along the London fault, deduced from a thorough study of the geology of the eastern part of the Mosquito Range, should be of general interest to economic geologists. The first part of this paper is a generalized statement of the geology of the region in which the London fault is located; it may be supplemented by reference to several earlier publications by the writers and to the U. S. Geological Survey's Professional Paper 148, on the Leadville district. The second part deals with the structure of both the fault and the disturbed zone adjoining the fault. The third part discusses the salient features of the ore deposits, particularly emphasizing structural control. The two generalized maps are complementary to one another but contain too many data to show on a single small map. The London fault is between Leadville and Alma, and the ore deposits along it are said to lie in the Alma district. Field work in this district, during six summers since 1927, has been a part of the cooperative work of the U. S. Geological Survey, the State of Colorado, and the Colorado Metal Mining Board. The writers have made use of work by R. D. Butler, J. W. Vanderwilt and R. E. Landon. G. F. Loughlin and C. H. Behre, Jr., who have worked on the west side of the range, have contributed valuable suggestions. Mining men of the district have aided in many ways. General Geology Pre-Cambrian Rocks.—The oldest rocks in the district are schists, correlated with the Idaho Springs formation of the Front Range. Quartz-mica schist predominates, but other types occur locally; almost everywhere the rocks show considerable lit-par-lit injection. Intrusive into the schists are two varieties of granite, only one of which is widespread. It is a fine-grained, porphyritie, gray granite correlated with the Silver Plume granite of the Front Range. Near the head of Buckskin Gulch a

Jan 1, 1937

In recent years, with the advent of new steelmaking procedures, the emphasis has turned away from conventional teeming and has been directed toward continuous casting. This paper points out the fact that there are still new methods being considered to decrease the problems and costs associated with conventional teeming. Although Inland has had no experience with the repair of mold lugs, we do find some problem with damaged ears associated with mechanically capped steel. When pouring bottle tops, any crane movement or leak from the pouring nozzle may result in steel over the top of the mold which, in turn, may result in the shearing of the mold lugs during stripping. Recent back pouring practices increase the chances of this occurring. At Inland's steelmaking shops, we have tried to combat this problem by various methods such as burning the steel from around the top of the mold at the pouring stand with oxy-gas torches. Last year, No. 4 BOF began a conversion from round to elliptically shaped bottle top caps. This change has greatly reduced the chance of splashing due to crane swing by increasing the dimension in the direction on normal swing. The answer to this particular problem is, however, tighter control of pouring performance. We are presently engaged in a process of re-education of personnel and experimentation with different materials and designs of nozzles, heads, and sleeves to help us achieve our goal.

Jan 1, 1972

By Malcolm F. Hawkes

AUSTENITE grain size has long been recognized by metallurgists as an important property of steels because of its influence on toughness, hardenability, machinability and creep strength. Much research has been carried out on wrought steels to develop methods for disclosing austenite grain size, and to provide knowledge of the grain-size -characteristics of steels produced and heat-treated in various ways. Much less work in these fields has been done on steel castings; partly because, owing to the variable and complex microstructures of cast steels, it is frequently very difficult to obtain results that are not questionable. The object of this investigation, therefore, was to establish, for a wide variety of carbon and alloy cast steels, suitable methods for disclosing austenite grain size and some knowledge of the grain-size variations to be expected. The steel foundryman is interested in austenite grain size at two different stages in the manufacture of his products; one is just after the steel is cast, and the other is after any reheating operation carried out above the critical temperature range. In both, it must always be kept in mind that the grain size being sought is actually a previous austenite grain size, and that the austenite no longer exists once the steel has cooled to room temperature. The problem of the investigator is always to use evidence obtained from the structure at room temperature to deduce this previous austenite grain size, which was established the last time the steel existed at a temperature above the critical range. Since most steel castings today are at least annealed or normalized, the measurement of austenite grain size established by heat-treatment will be considered first. More than So commercially produced cast steels representing a wide variety of compositions and melting practices were used in the study. For each steel, grain-size determinations were made after each of three widely varying heat-treating schedules; namely, one hour at 1550°F, one hour at 1700°F, and six hours at 1700°F. The list of steels and results obtained on them will be found in the appendix. (See page 21.) A discussion of the knowledge gained on the applicability of various test methods and on grain-size characteristics of cast steels in general follows. MEASUREMENT OF AUSTENITE GRAIN SIZE ESTABLISHED BY HEAT TREATMENT METHODS SUITABLE FOR DETERMINING AUSTENITE GRAIN SIZE AFTER HEAT- TREATMENT AT ORDINARY TEMPERATURES AND TIMES It was desired, as one of the results of this investigation, to be able to recommend to steel foundries a method, or methods, of disclosing grain size best suited to accurate

Jan 1, 1947

By R. Silverman, H. Blumenthal

It was found that despite the similarity of chemical analyses of different titanium carbides used as base materials for cermets, the physical properties, especially transverse-rupture strengths, of test bars were different. Hence this metallographic study attempts to link physical properties to micro-structures. It is shown that microstructure, grain shape, and grain growth are functions of three interrelated factors: 1—powder production procedure, 2—surface conditioning of the particles, and 3—impurities either contained in the original powder or acquired during ball milling. An explanation is offered for the "coring effect," long observed, but heretofore of unknown origin. The explanation is based on assumption of an oxide film and on chemical analyses which substantiate these findings. TITANIUM carbide has become in recent years a material of great interest in the high temperature field. Consequently, many manufacturers in the United States and Europe are producing titanium carbide for cermet applications as well as for additions to the well known tungsten carbide tools. All present commercial processes of titanium carbide production utilize the chemical reaction of titanium dioxide and carbon to form as nearly as possible stoichiometric Tic. This reaction is carried out in three ways: 1—in a menstruum of molten metal,' 2—in the solid state, either in a protective atmosphere2 or in vacuum;" or 3—in an are-melting operation. In spite of the fact that the pure carbides obtained in these operations are almost identical chemically, the physical properties vary considerably when they are combined with a binder (Ni, Co) to form cermets. This fact led the authors to examine metal-lographically nickel-bonded titanium carbide in order to find the possible reasons for this behavior. Materials and Methods Five different titanium carbides were used in this investigation. They are identified in Table I. The first four materials were used in the as-received condition. Material E, received in lumps, was crushed to —100 mesh and carried through a flotation process in order to bring its graphite content in line with the other products. A Galagher flotation cell was used with pine oil as frothing agent. The chemical analyses of the investigated materials are given in Table 11. The binder used was carbonyl nickel of 9 to 14 microns particle size, supplied by A. D. Mackay. The materials were ball milled at a ball to charge ratio of 6:1 using procedures described under "Experiments and Results." All particle sizes mentioned are averages determined with a Fisher Sub-sieve Sizer. Test bars (lx0.40x0.16 in.) were prepared by 1—hot pressing to 85 to 95 pct of theoretical density at pressures between 1 and 1½ tsi and temperatures from 1600" to 1800°C, 2-—-cold presssing after 3 pct camphor had been added, or 3—wet pressing, both 2 and 3 at pressures between 5 and 10 tsi. All pressed bars were sintered in a vacuum of 105 to 10-6 mm Hg for 2 hr at 1350 °C. Transverse-rupture strengths were determined by breaking on a Baldwin Universal Testing Machine over a 9/16 in. span. Densities were measured by water displacement. The preparation of the specimens for micrographs was done according to Silverman and Doshna Luscz." All magnifications are at X1000. A sodium picrate electrolytic etch was used. Experiments and Results The influence of ball-milling procedure, ball-milling medium, pressing procedure, and sintering procedure on the microstructure of 80/20 — TiC/Ni were investigated. Ball Milling of Materials A, B, and C in a Steel Mill: Figs. 1 and 2 show microstructures of hot-pressed and vacuum-sintered test bars of materials A and B after the respective materials had been ball milled to 2.1 microns particle size in a steel mill and mixed with 20 pct Ni binder. Material A (Fig. 1) shows considerable grain growth. Also evident is a tendency of the carbide grains to coalesce. The density is 98 pct and the low transverse-rupture strength of 111,000 psi is probably caused by many large grains and an unfavorable packing factor. Almost all grains show a slight indication of "coring." Material B (Fig. 2), although showing grain growth, still has many small particles and a better distribution of binder and carbide due to the relative absence of the coalescing tendency. "Coring" can be observed in almost all grains. The high transverse-rupture strength of 179,000 psi and the density of 100 pct are believed to be due to the many small grains completely surrounded by the binder phase. There is also a preference to form spherical grains with material A, while most grains of material B preserve their angular shapes. Material C, of which no picture is given, stays between A and B in every respect. Rounding of some grains can be observed as well as coring, but the latter to a lesser degree than with material B. Its densification is good and the transverse-rupture strength obtained is 142,000 psi. Ball Milling of Materials A, B, C, and E in a WC Mill: When the Tic powders were ball milled to 2 microns particle size in a we mill, then ball-mill mixed with 20 pct Ni binder, hot pressed, and vacuum

Jan 1, 1956

By R. E. Mussler, F. E. Block, T. T. Campbell

An exploratovy study was made to deternzine the feasibility of preparing beryllium by the metallother-. mic reduction of beryllium oxide. The procedure involved heating a relatively nonvolatile metal reductant in contact with beryllium oxide in a vacuum. Beryllium vapors formed in the reaction were condensed as a coherent deposit on a heated surface. Reductants tested included tanthanun, yttrium, thorium, Th-Mg, and Zr- Ti alloys, and the hydrides of lanthaniir~z, yttriunz, and zirconiur?7,. Test ten7pevatures ranged from 1350'to 175O' C, and reaction times ranged frot 30 to 100 lzr. In most cases metal recoveries were lola, although yields close to 90 pct of theoretical were obtained with latzthanum, yttrium, and zirconium reductants. In most cases metal deposits were contanzinated by beryllides, /ls/cally of the Beln M or Bel3 M type. BERYLLIUM has a variety of unique properties including light weight (sp gr 1.85), low thermal neutron absorption cross section, high scattering cross section, excellent dimensional stability, high strength to weight ratio, high melting point (1285"C), high specific heat, and high thermal conductivity. Interest in beryllium as a structural material in aerospace and nuclear-reactor applications is based on these properties. In general, the potential of beryllium has been only partially realized, largely because of the brittleness of poly crystalline forms of beryllium, difficulties associated in its fabrication, and joining problems encountered in its use in structural applications. Several excellent books and monographs are available to those interested in the occurrence, extractive metallurgy, and utilization of beryllium.1"* Although an extensive amount of research on beryllium has been in progress during the past 10 years, much of the work has been concerned either with the so-called "ductility problem" or with the development of methods of fabrication and evaluation of properties of various commercial or purified grades of metal. A recent survey of the literature indicates that only limited efforts are presently being directed toward developing new methods for reducing beryllium compounds to metal. Two major commercial methods now used to produce beryllium are the magnesium reduction of beryllium fluoride and e lec trow inn ing of beryllium from fused sodium chloride-beryllium chloride salt baths. Only a limited amount of work has been done on the direct reduction of beryllium oxide. Major factors which complicate this method are the great stability of beryllium oxide and the reactive nature of beryllium metal. The stability of the oxide necessitates extremely high reduction temperatures and vacuum operation to liberate beryllium metal vapor and cause reactions of the following type to proceed: XBeO(s) +YM(s)-MYOX(s) + XBe(& As early as 1939, roll' used this reaction for the direct reduction of beryllia by zirconium and titanium, and later in 1952 ~a~el~ studied the reduction of beryl-

Jan 1, 1967

C. A. ROSE, New York, N. Y. (written discussion *).-Without doubt the excellent results obtained at Ajo will cause surprise among metallurgists; 75 per cent. average capacity and 80 per cent. extraction during the first year of operation of a plant using a new metallurgical process are figures that speak for themselves. It is obvious that the most troublesome feature of the process is the fouling of solutions. The effects of this are most evident in the electrolytic tank house; but apparently the solutions are so heavily loaded with salts that their dissolving power is also impaired. This is indicated by the fact that copper comes into solution during washing after the leaching of the ore is completed, as shown by the decreasing ratio of acid to copper in the various washes tabulated in Table 4, and also by the fact that 4.9 per cent. of the total copper in the ore remains in the tailings in a soluble form. Even though the extraction in leaching and the ampere efficiency in electrolysis would be benefited by keeping the salts in solution at a lower concentration, it is doubtful whether it would pay to decrease these salts by discarding more electrolyte without other changes in the, process, since this would increase the amount of cement copper produced, which is already very large. If, however, it would not disturb the process otherwise, this object could be accomplished by increasing the range of electrolysis, so that solution going to the tank house would contain, say, 4 per cent. copper and 1 per cent. acid, and the solution returned to the leaching plant 1 1/2 per cent. copper and 4.8 per cent. acid, and by increasing the volume of solution to be discarded, this to be taken from the electrolyzed solution returned to the leaching plant. By this arrangement, more salts will be removed from the system per ton of cement copper produced; and if sufficient solution is discarded to keep the iron content down to 1 1/2 per cent. it would he feasible to recover the copper from

Jan 4, 1919

By John A. Church

In May, 1878, I had the honor of presenting to the Institute, at the Chattanooga meeting, some observations upon the heat of the Comstock Lode, and since then the subject has attracted some attention and criticism, in the course of which, L have observed errors of apprehension which I beg leave to correct now. Mr. John Arthur Phillips discussed it before the Geological Society, his paper being printed in the Quarterly Journal for August, 1879." His criticism is based upon that part of my paper in which I quote a number of analyses of the mine waters, to illustrate the fact that the heat does not come from the oxidation of pyrite. I pointed out that these waters contain only an insignificant proportion of sulphuric acid, and not enough to account for even one per cent. Of

Jan 1, 1880

By J. S. Aronofsky

The first step in a quantitative analysis ot the mechanism of oil displacement by water in a fractured reservoir is usually conceded to be the solution of the differential equation describing the saturation distribution of two immiscible fluids flowing in a porous medium, where the capillary pressure is taken into account. In such a system the production mechanism may consist of displacement of oil both by the flow of water due to natural or artificially imposed pressure gradients and by imbibition, which implies a flow of water not due to external pressure gradients. Owing to the presence of the two oil displacement mechanisms, the mathematical model given by the differential equation intended to describe the system may not properly represent the behavior of the physical system. In fact, in the reservoir the rate of water advance may be very slow, and in the case of a fractured reservoir with a great number of large fractures, the pressure difference determining the flow of water through the matrix may be much less than 1 lb/'psi over lengths of a few feet. In such a case, imbi-bition (the exchange between oil in the matrix and water in the fractures resulting from capillary forces) may become, with time. a significant element of the production mechanism. It occurred Lo the authors, however, that without going into a physical analysis of the process of production, it might be possible by means of simple abstract reasoning to throw some light on the variation of recovery with time under conditions occurring in a highly fractured oil reservoir with rising water table. The object of this paper is to present both the reasoning and its application to a reservoir of the highly fractured type. Specifically, the analysis given here was undertaken to try to explain the increase of recovery (as defined later) with time as observed in this reservoir, without having to assume unlikely variations in the reservoir parameters with depth. This attempt has been successful as will become clear upon comparison of the computed recoveries with the actual field data. ABSTRACT MODEL Let us consider a small volume. of porous matrix saturated with oil at time, t = 0. Let the process of oil displacement by water start at time, t = t,,. At some time, t, the process will have terminated. Then a volume of oil equal to or smaller than the original oil contained in the matrix will have been produced. The first basic assumption that describes the model and guides the forthcoming reasoning is that the oil production from the small volume. dv, is a continuous monotonic function of time and that it converges to a finite limit. Such an assumption is not inconsistent with the results of laboratory waterflood tests as well as with results of imbibition tests where this is, in fact, observed. The second basic assumption is that none of the properties which determine the rate of convergence change sufficiently during the process to affect this rate or the limit. Let it be assumed that the form of the function of time relative to production from the matrix volume. dv, is given by where V,(t) is the volume of oil produced up to that time t. R is the limit toward which the recovery converges, A is a constant giving the rate of convergence, and V,(t) is the volume of oil originally in place in the volume, dv. It should be noted that recovery at time I will be understood here to he It follows that r. tends to R as t tends to infinity. CONSTRUCTION OF RESERVOIR FROM ABSTRACT MODEL Let the reservoir consist of a series of identical blocks of porous matrix stacked vertically and separated by fractures. Let each of these blocks satisfy the conditions of our abstract model. These conditions are: (1) that recovery is a continuous mono-tonic function of time converging to finite limit, and (2) none of the properties that determine the rate of convergence change sufficiently to affect the rate or the limit. Let water be rising in fractures so that oil production from any part of the block starts when the water comes in conLact with it. TOTAL RECOVERY FROM THE RESERVOIR COMPARED TO RECOVERY FROM A SINGLE MODEL ELEMENT As stipulated in Eq. 1, in the case of the abstract model,

Jan 1, 1947

By C. W. Parmalee

The ideal fuel for burning ceramic wares is the one that, among other characteristics, has little or no sulfur. For that reason wood was long considered the most desirable fuel but its high cost has practically eliminated its use except in regions where it is very abundant or other circumstances warrant its choice. The fuels commonly employed are natural and producer gas, oil, and coal. The last named is undoubtedly the most important, not only in this country but abroad. Occasionally anthracite is used but the larger part is bituminous. The quality of the coal used depends on the kind and the value of the products being manufactured. For some materials, such as common brick, hollow block, etc., the quality of the coal is of less importance than in the manufacture of polychrome terra cotta, pottery, porcelain, etc. It is obvious that in burning clays that contain notable amounts of pyrite, marcasite or gypsum, as is the case with many common clays, the sulfur content of the fuel is of much less importance. The permissible amount of sulfur in the coal used will depend on the kind of product being manufactured. "A good sample1 of coal commonly used in pottery ovens has something like this quantity of sulfur: total sulfur, 1.20 per cent.; sulfur in ash, 0.11 per cent.; volatile sulfur, 1.09 per cent." This is based on English pottery practice. Correspondence with a. number of leading manufacturers in this country has produced the following figures: Sanitary Ware.—(a) 1.0 per cent, maximum, (b) 0.5 per cent. Sewer Pipe.—(a) 1.2 per cent., (b) 1.1 per cent, present run, 3.0 per cent, has been used. Terra Cotta.—(a) 0.5 per cent, basis of contract, 1.0 per cent, approximate. Pottery.—1.0 per cent, contract, 1.5 per cent, probable content. Enameled Brick.—1.3 per cent, maximum, (a) and (6) designate different firms giving figures. Since a pottery kiln for sanitary ware will require about 14 tons of coal for a bum, the quantity of SO2 that will be generated from a 1-per

Jan 1, 1920

By F. D. Mahone

Much crude oil, as produced from the well, carries varying amounts of water, which may be present as free water in globules sufficiently large to settle out, in time, if the fluid is allowed to stand, or as an emulsion formed by myriads of minute water particles, each surrounded and entrapped by a film of oil through which it cannot break under the action of gravity alone. Such an emulsified mixture of oil and water is commonly termed "cut oil." When such an emulsion is subjected, under proper conditions, to the influence of a high-potential alternating-current field, the minute water particles rupture the enveloping oil films and coalesce into larger water droplets this procedure continuing until all the water is freed into drops of such size that they readily settle out. This action has been photographed by the micro-moving-picture camera; under the microscope, the breaking-up of the emulsion, as described, is seen to be accomplished in a few seconds. The low power requirements of the process, from records of commercial plants, substantiate the theory that the action is that of a multitude of electrical condensers in series, rather than that of a number of conducting paths. The minute water particles serve as the metallic elements, or plates, of the condensers and the separating oil acts as the dielectric. Such surface charges as the particles may have are removed, and the intervening oil is broken, probably electrically by the voltage and mechanically by the attractive force between adjacent oppositely electrified particles. The principle of breaking up an emulsion under the influence of an alternating electric field was discovered by F. G. Cottrell and Buckner Speed, through experiments conducted, at the University of California, which resulted in a plant being installed on the property of the Lucile Oil Co. in the Coalinga field, California, early in 1909. This plant was able to reduce 14-per cent. emulsion to less than Pper cent. with commercial success. Standard Cottrell Apparatus The present standard Cottrell apparatus consists essentially of the electric treater and a settling or trap tank. The treater is a galvanized-iron tank approximately 3 ft. in diameter and 10 ft. high, which con-

Jan 1, 1924

By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By Strathmore R. B. Cooke, Thomas E. Bam

The paper discusses the mineralogy, structure, and strength of magnetite pellets fired in air and in a neutral atmosphere at various temperatures. The information obtained from this investigation is used to explain the origin of the structures occurring in pellets produced by pilot-plant operation. MUCH experimental work has been performed on i-VL the mechanism of agglomeration and pelletiz-ing of moist ore and concentrates and on the process of firing agglomerates, but except for the work of Tigerschiold and Ilmonil much of the published information is empirical, and the literature contains no information concerning the structure of fired pellets. Results of a preliminary study of the micro-structures occurring in pellets produced both in the laboratory and on a pilot-plant scale are presented in this paper. Most of the results were obtained from pellets prepared from Mesabi magnetic taconite, but through the courtesy of the staffs of the Minnesota Mines Experiment Station and the Bethlehem Steel Co., fired pellets produced from limonite and hematite ores and from Lebanon magnetite have also been examined. The work has been restricted almost entirely to pellets produced without additives, the exceptions being those in which coal was added to the filter cake before rolling. Schwartz has described the microstructures occurring in ore sinters produced under reducing conditions.' Many of the structures and constituents he describes are common to fired pellets, but the constituents normally occur in markedly different proportions. His statement that "in all satisfactory sinter the amount of hematite is small, perhaps not over 2 or 3 per cent" is inapplicable to pellets produced by pilot plant operation or by any process in which air is not deliberately excluded. Pilot plant pellets contain over 90 pct by weight of hematite, and those produced in the smaller furnaces of the Minnesota Mines Experiment Station contain more than 80 pct of that constituent. Preparation of Specimens It is difficult to examine unfired pellets microscopically because of their insufficient coherency to withstand sectioning and polishing. Fired pellets sometimes lack coherency and frequently contain holes which are troublesome during polishing. Impregnation of both air-dried and fired pellets is readily accomplished by the use of methyl metha-crylate monomer." The dry pellets are covered in a test tube with excess monomer, to which a small amount of accelerator has been added. When the test tube is placed in a cooling bath and evacuated with an aspirator, most of the entrapped air is removed, and disruption of weak pellets by boiling of the monomer is reduced to a minimum. Polymerization is then effected by immersion of the test tube in a water-bath at about 45"C, this temperature being held for 4 or 5 days. The test tube may then be broken away from the solidified mass and the pellets sectioned by a carborundum wheel or a diamond saw. Where time is important, impregnation is carried out at a higher temperature by Meyer's method.' Air-dried pellets must be impregnated with especial care; otherwise swelling occurs and the solids are displaced. It is more important to be certain that the monomer forms a reasonably complete network throughout the specimen than that all entrained air is removed, and for this reason the vacuum technique may be omitted. Impregnated agglomerated products and pellets are extremely coherent, section well, and may be polished either by hand or by machine. Hand polishing is not satisfactory for the examination of conditions existing at the boundaries of grains, and for this machine polishing must be used. The Graton-Vanderwilt machine gives excellent results, provided that pressure on the specimen is considerably in excess of that recommended by the manufacturer. Mineralogy of Fired Pellets Only two opaque iron minerals, magnetite and hematite, have been recognized in pellets. The complete identity of, these artificial minerals with their corresponding natural counterparts is shown by their mineralographic characteristics and their X-ray structures. Wiistite has not been found. Slag is the most common transparent constituent of fired pellets. Occasionally conditions have been appropriate for the crystallization of fayalite from the slag, and at other times another crystalline sil-

Jan 1, 1953

By L. A. Dale, D. A. Dahlstrom

Closed-water circuits are justified today from two standpoints: economical operation and prevention of stream pollution. In today's modern preparation plant, it has been found very desirable to have the plant circulating water maintained at a relatively low solids concentration of around 3%. In so doing, bene-ficiation equipment can operate at a much higher efficiency. However, makeup water requirements would become excessive if the fines were to be removed from the preparation plant by bleeding a 3% solids concentration to a tailings pond. With the ever increasing percentage of —200 mesh coal, clay and slimes in the raw coal, coupled with the creation of these fines within the preparation plant, the need for water conservation for economy reasons becomes even more important. Because of stream pollution laws, tailings ponds have become very costly to operate and maintain, resulting in the necessity of employing an in-plant method of water recovery. Accordingly, the primary system employed in water recovery in the coal preparation plant today consists of a solids concentration device to thicken refuse solids while at the same time producing a sufficiently clarified effluent that can go back to the preparation plant for water reuse. The thickened product is then normally passed to a dewatering device that will produce a handleable solid that can be disposed of

Jan 1, 1965

By J. S. Billheimer, B. H. Sage, W. N. Lacey, C. G. Yundt

As a part of a general investigation of the separation of bitumen from hydrocarbon mixtures a study was made of a restricted quaternary system composed of methane, decane, tetralin, and bitumen. The work was limited to a pressure of 8000 psi, a temperature of 220 °F, and to a fixed relative proportion of decane, tetralin, and bitumen. The measurements permitted the determination of the distribution of these components in each of the fluid phases. It was not possible to distinguish a second liquid phase in the course of these measurements. Gas-liquid equilibrium "constants" of each of the components were found to vary markedly with the composition of the system while temperature and pressure remained fixed. INTRODUCTION The separation of bitumen frorn naturally occurring hydrocarbon mixtures has been of importance for a number of years in the production of petroleum, especially in the California area. The deposition of this material from crude oils was noted in earlier studies of the solubility of natural gas in crude oil.¹,²,3 Studies of the separation of bitumen from crude oils from the Greeley and Santa Fe Springs fields were carried out."." The behavior of these systems appeared complex and studies of two restricted ternary systems involving mixtures of n-pentane, tetralin, and bitumen,' and of decane, tetralin; and hitumen, confirmed this belief. Reviews of the literature pertaining to the separation of bitumen from naturally occuring and refined hydrocarbons are available." The important effect of methane in the separation of bitu- men from naturally occurring hydrocarbon mixtures was apparent from the earlier studies and for that reason it appeared desirable to investigate a restricted quarternary system involving mixtures of methane. decane, tetralin, and bitumen; data concerning the behavior of mixtures of decane. tetralin. and bitumen having already been obtained.V his study was restricted to a pressure of 8000 psi," a temperatue of 220° F, and fixed relative proportions of bitumen, decane. and tetralin. This composite constituent, hereinafter designated as the less volatile constituent, was made up of 0.0455 weight fraction bitumen. 0.0909 weight fraction decane, and 0.8636 weight fraction tetralin. The experimental method involved bringing together mixtures of methane and the less volatile constituent in varying proportions in a constant volume container at the pressure and temperature indicated above. The composition of each of the phases was determined and from this the extent of the separation of bitumen was established. MATERIALS The bitumen used in this investigation was obtained from the same stocks employed in earlier studies. The crude material from the North Coles Levee field was stored in the laboratory] in a closed drum for a period of five years. Several samples from this stock were subjected to refining operations which were described earlier,' and every effort was made to follow the same procedure in all cases. It was necessary to prepare supplies of bitumen for this investigation at two rather widely different times. These materials have been identified as samples 1 and 2. The composition of the crude bitumen after it was washed with n-pentane at room temperature

Jan 1, 1949

By W. N. Lacey, C. G. Yundt, B. H. Sage, J. S. Billheimer

As a part of a general investigation of the separation of bitumen from hydrocarbon mixtures a study was made of a restricted quaternary system composed of methane, decane, tetralin, and bitumen. The work was limited to a pressure of 8000 psi, a temperature of 220 °F, and to a fixed relative proportion of decane, tetralin, and bitumen. The measurements permitted the determination of the distribution of these components in each of the fluid phases. It was not possible to distinguish a second liquid phase in the course of these measurements. Gas-liquid equilibrium "constants" of each of the components were found to vary markedly with the composition of the system while temperature and pressure remained fixed. INTRODUCTION The separation of bitumen frorn naturally occurring hydrocarbon mixtures has been of importance for a number of years in the production of petroleum, especially in the California area. The deposition of this material from crude oils was noted in earlier studies of the solubility of natural gas in crude oil.¹,²,3 Studies of the separation of bitumen from crude oils from the Greeley and Santa Fe Springs fields were carried out."." The behavior of these systems appeared complex and studies of two restricted ternary systems involving mixtures of n-pentane, tetralin, and bitumen,' and of decane, tetralin; and hitumen, confirmed this belief. Reviews of the literature pertaining to the separation of bitumen from naturally occuring and refined hydrocarbons are available." The important effect of methane in the separation of bitu- men from naturally occurring hydrocarbon mixtures was apparent from the earlier studies and for that reason it appeared desirable to investigate a restricted quarternary system involving mixtures of methane. decane, tetralin, and bitumen; data concerning the behavior of mixtures of decane. tetralin. and bitumen having already been obtained.V his study was restricted to a pressure of 8000 psi," a temperatue of 220° F, and fixed relative proportions of bitumen, decane. and tetralin. This composite constituent, hereinafter designated as the less volatile constituent, was made up of 0.0455 weight fraction bitumen. 0.0909 weight fraction decane, and 0.8636 weight fraction tetralin. The experimental method involved bringing together mixtures of methane and the less volatile constituent in varying proportions in a constant volume container at the pressure and temperature indicated above. The composition of each of the phases was determined and from this the extent of the separation of bitumen was established. MATERIALS The bitumen used in this investigation was obtained from the same stocks employed in earlier studies. The crude material from the North Coles Levee field was stored in the laboratory] in a closed drum for a period of five years. Several samples from this stock were subjected to refining operations which were described earlier,' and every effort was made to follow the same procedure in all cases. It was necessary to prepare supplies of bitumen for this investigation at two rather widely different times. These materials have been identified as samples 1 and 2. The composition of the crude bitumen after it was washed with n-pentane at room temperature

Jan 1, 1949

Discussion of the paper of FRANCIS S. PEABODY, presented at the St. Louis meeting, October, 1917, and printed in Bulletin No. 125, May, 1917, pp. 775 to 781. THE CHAIRMAN (CARL SCHOLZ, Chicago, I11.).-Coal wastage is undoubtedly one of the most prominent topics before the coal operators of the United States today. Even those who have been in the business only 25 years, like myself, know that the exhaustion of coal is something that should and must, be curbed. If it is not, before long we shall discover that the great coal resources of the country are not what we-thought they were; we have been so accustomed to work at the best and thickest coal alone, that it will be difficult for us to realize one of these clays-and that (lay is not far distant-that we are no longer the rich nation in coal that we thought we. were. In this connection I feel obliged to attach a little blame to the Geological Survey for misleading the people. There are several members ,here who assisted in that work, and I am going to ask them to defend themselves. The Geological Survey deals with coal seams of much less thickness than we could now expect to, mine, particularly with the present high wages, excepting at a prohibitive cost. The Geological Survey, in its estimates, does not discriminate between thick and thin seams, but simply estimates our resources at so many hundred thousand billion tons of coal. I believe they include seams from 15 to 18 in thick, but you all know that a vein below 3.5 or 4 ft. is not considered economical to mine at this time. R. V. NORRIS, Wilkes-Barre, Pa.-Mr. Peabody has evidently been thinking almost entirely of Illinois conditions, with which I regret to say I am absolutely unfamiliar. In some West Virginia mines the total recovery at present is considerably over 90 per cent. and extraction-, as high as 97 or 98 per cent. are claimed.

Jan 1, 1918