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By E. F. Loiseau

In a paper on the manufacture of artificial fuel, read at the Philadelphia meeting of February, 1878, I enumerated the difficulties which I had to overcome before succeeding in the mixing of coal-dust and clay, the compressing of the same mixture, and the water-proofing of the lumps. The drying of the lumps, after leaving the press, was the remaining difficulty, and it mas expected that a plan devised by Dr. Charles N. Cresson, of Philadelphia, would enable us to dry the fuel as rapidly as it was moulded, and that a continuous production could in that way be obtained. The company was reorganized. The works were purchased by the new company at an assignee's sale, and the oven was modified, according to Dr. Cresson's plan. Anticipating a possible failure, I had prepared a plan by which I expected to be able to demonstrate that anthracite coal dust nixed with pitch, could be manufactured with our present machinery slightly modified ; so that after all, if we were compelled to give up the attempt to make fuel for domestic use, there was a possibility of succeeding in the manufacture of a good steam-fuel. The plan suggested by Dr. Cresson for drying the pressed lumps of coal-dust cemented with clay, did not work as well as we expected. It enabled us to dry more fuel than we did before, but it could not be made to dry more than one half of the lumps produced by the press. The plan mas abandoned, and I was authorized to experiment with coal-dust and coal-tar pitch. The cement which is used in Europe to conglomerate coal-dust is usually dry pitch, which is prepared by separating from the tar, at a temperature of 572' Fahrenheit, the volatile matters which it contains. Some manufacturers, however, employ crude tar, others, a rich tar, which has been cleared of 25 per cent. of its volatile substances, by heating it to 392' Fahrenheit. But with common tar very weak fuels are obtained, which do riot burn well, and give out a strong smell and a great deal of smoke ; it is also necessary to subject them to a baking process, in order to solidify them, and to eliminate the more volatile of the materials contained. This operation of course requires a special plant, the cost of which increases sensibly the price of manufacture, without counting the products

Jan 1, 1880

By E. F. Loiseau

IN a paper on the manufacture of artificial fuel, read at the Philadelphia meeting of February, 1878, I enumerated the difficulties which I had to overcome before succeeding in the mixing of coal-dust and clay, the compressing of the same mixture, and the water-proofing of the lumps. The drying of the lumps, after leaving the press, was the remaining difficulty, and it was expected that a plan devised by Dr. Charles M. Cresson, of Philadelphia, would enable us to dry the fuel as rapidly as it was moulded, and that a continuous production could in that way be obtained. The company was reorganized. The works were purchased by the new company at an assignee's sale, and the oven was modified, according to Dr. Cresson's plan. Anticipating a possible failure, I had prepared a plan by which I expected to be able to demonstrate that anthracite coal dust mixed with pitch, could be manufactured with our present machinery slightly modified ; so that after all, if we were compelled to give up the attempt to make fuel for domestic use, there was a possibility of succeeding in the manufacture of a good steam-fuel. The plan suggested by Dr. Cresson for drying the pressed lumps of coal-dust cemented with clay, did not work as well as we expected. It enabled us to dry more fuel than we did before, but it could not be made to dry more than one-half of the lumps produced by the press. The plan was abandoned, and I was authorized to experiment with coal-dust and coal-tar pitch. The cement which is used in Europe to conglomerate coal-dust is ,usually dry pitch, which is prepared by separating from the tar, at a temperature of 572° Fahrenheit, the volatile matters which it contains. Some manufacturers, however, employ crude tar, others, a rich tar, which has been cleared of 25 per cent. of its volatile substances, by heating it to 392° Fahrenheit. But with common tar very weak fuels are obtained, which do not burn well, and give out a strong smell and a great deal of smoke ; it is also necessary to subject them to a baking process, in order to solidify them, and to eliminate the more volatile of the materials contained. This operation of course requires a special plant, the cost of which increases sensibly the price of manufacture, without counting the products

Jan 1, 1880

By P. G. Shewmon, H. E. Collins

We have studied the effect of adsorbed sulfur on the surface self-diffusion of copper using eight diflerent surface orientations and the grain boundary grooving method. The eight orientations studied were the four lying near the low-index surfaces—(loo), (Ill), and two directions in the (110)-plus four higher-index surfaces. Surface-diffusion measurements were made over a range of HZS concentrations (in Hz) from 3 to 1500 ppm between 830°and 1050°C. The results can be divided into two groups—Group 1 contains the two (110) surfaces while Group 2 contains the remaining six surfaces. In Group 1, increasing the temperature increases the effect of Hz S on DS for the Hz S range 5700 ppvn. Qs and Do increase with increasing H2S concentration in this Hz S range. Beyond this range, increasing the temperature decreases this effect on D,; also Q, and Do decrease. In Group 2, increasing the telnperature decreases the effect of H2 S on D, for the H2S range studied, and Qs and Do decrease with increasing Hz S concentration. In any study of surface phenomena, there invariably arises the question of the possible presence of and effect of adsorbed impurities. Such questions are well-founded since the presence of adsorbed atoms can sometimes produce marked changes in the kinetics of surface-energy-driven processes. In the last few years, values of the surface self-diffusion coefficient, D,, have been determined on a variety of metals by studying the decay of scratches or the growth of grain boundary grooves.L~3-L0~L3 Yet there has been relatively little work done in which the concentration of an adsorbed impurity was systematically varied and the effects observed. Work of this sort would provide some basis in fact for the assertions often made about the ro1.e of adsorbed impurities in the differences between the results of different workers in different atmospheres and on different metals. It also is relevant to those cases in which surface monolayers produce profound effects in commercially important processes. The most marked example of such effects is the ability of nickel or palladium to increase the sintering rate of tungsten by many orders of magnitude.' The aim of this work was to study the effect of sulfur partial pressures on the surface self-diffusion of copper. It was felt that this in conjunction with a study of the degree of adsorption and type of active sites involvedL8 would provide a wide range of data for one system and hopefully lead to some insight into the mechanism by which sulfur adsorption influences copper diffusion. The main reasons for choosing the Cu-S system were, first, faceting was reported not to accompany the adsorption of sulfur. This is required if our experimental technique is to work. Second, Oudar has determined a high temperature adsorption isotherm for this system, an event which puts the Cu-S system almost in a class by itself.I4 EXPERIMENTAL PROCEDURE Initially, we considered studying the effect of an adsorbed impurity on surface self-diffusion of copper using isolated (or single) scratch smoothing as the technique and oxygen as the impurity. Copper was chosen as the material because the effects of orientation and anisotropy of the surface self-diffusion coefficient, D,, of copper in a dry hydrogen atmosphere had been studied extensively by Gjostein' and by Shewmon and ~hoi.~,~ The isolated scratch technique was chosen because both the effects of surface orientation and anisotropy of D, in a given surface could be easily studied with this method.~ Oxygen was tried as the impurity because Robertson and Shewmon""~ had studied its adsorption on copper at 1000°C over the range of oxygen partial pressures of 10"22 to 10-l3 atm. After several preliminary runs, it became evident that neither the scratch technique nor the impurity oxygen would be satisfactory for this work. Scratching deforms an annealed surface so that the region near the scratches recrystallizes, thereby disrupting the scratch profiles. One can avoid this by deforming the specimen sufficiently before scratching to give complete recrystallization on subsequent heating.4 However, as a result of Gjostein's success in scratching and annealing undeformed gold single crystals without local recrystallization,13 we attempted something similar with copper single crystals using a 0.7-mil diamond phonograph needle mounted in a Tukon hardness tester. All specimens recrystallized upon being annealed. Also, some copper specimens were sent to Gjostein to be scratched using his technique. The results were the same. As a result, the scratch technique was dropped in favor of the grooving of symmetric grain boundaries. Preliminary work using oxygen showed that faceting began to occur before oxygen adsorption had any measurable effect on D, at 938°C (at Pbo/P, = 0.12). Since heavy faceting would interfere with the measurement, we decided to use a sulfur-containing atmosphere (H2S/H2). Work by Oudar and Benard' and Robertson" showed that sulfur absorbed on copper and that faceting was not observed.

Jan 1, 1967

Executive ARTHUR S DWIGHT, Chairman B THAYER CHARLES F RAND P MATHEWSON J V W REYNDERS Membership WILLIAM H BASSETT, Chairman W Y WESTERVELT Vice-chairman P MATHEWSON H G MOULTON F T RUBIDGE Finance WALTER H ALDRIDGE, Chairman GEORGE D BARRON GALEN H CLEVENGER

Jan 1, 1923

By Earl 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:

Jan 8, 1914

By Richard E. Goodman

Rock slope stability assumes different roles in decision making as a mining venture develops and, accordingly, geological investigations vary in thought and in deed according to the project stage. During exploration, stability questions bear on the decision whether or not to mine, because their resolution affects the cost of mining. During the mine lay-out stage, stability is a key factor in deciding how to mine. Finally, during mine operation, stability affects safety and operating costs, and therefore, pit productivity. Among the many considerations influencing stability, rock mass classification and geological environmental factors count heavily. The rock mass behavioral class depends upon the rock character and its degree of fracturation. The loads on the rock are derived from the environmental factors of initial state of stress and the water regime. Of course, stability is also tied to a host of non-geological factors such as the pit geometry, mining style, relative wealth, philosophy of mine operation, and accident history. METHODS OF STABILITY EVALUATION AND CORRESPONDING INVESTIGATORY TOOLS The purposes of the geological investigation are to identify and evaluate the geological factors influencing stability so that the vital questions can be analyzed. The tools selected for stability analysis reflect the stage of development of the mining scheme and therefore the geological investigations, which must furnish data for the analyses and must vary with the project stage. For exploration and mine planning, the methods of resolving stability questions must meet the need to evaluate numerous parameters in limited time; examples of such methods are stereographic projections (1, 2, 3) charted solutions(4) and simple physical models (5, 6). An investigation program that employs geological mapping tools and aids to mapping, such as geophysics, with relatively few rock tests, is in balance with these analytical methods. First data about the water regime are obtained from observed piezometric levels, and the initial state of stress is queried simply through geological inference and experience. In the layout stage more elaborate physical scale models (7) and perhaps finite element models (8, 9, 10, 11, 12), will be relevant to the design process and therefore much more detailed geological investigation is required. The scale of observation of both rock material and joints will be significantly enlarged and mechanical tests of rock and joint strength

Jan 1, 1972

By William Crane

OPERATORS of diamond drills have long been familiar with thread-like markings or riflings on cores but apparently have given but little serious thought to the conditions that are responsible for their production. The opinion generally held by those who have observed the phenomena is that the riflings are produced directly or indirectly by vibration, but so far as the writer is aware no systematic attempt has been made to demonstrate the fact. A careful search through the literature on diamond-drilling practice has been rewarded by only one reference to such markings of cores. J. N. Justice1 writes, "Of the peculiarities met with in the core, I will mention only one. The core from the "H" drill, at about 360 ft. came out rifled and pentagonal. The change from the circular to the pentagonal was sudden, and for 9 ft. this structure was maintained, when suddenly it returned to the circular. I have not been able to find any one who can explain the cause of this change of form. The drill men marveled at it and suggested vibration, six-stone bits, and several other hypotheses Which need not be mentioned." The writer became interested in the matter of core riflings some 10 years ago while in the Flat River lead region of Missouri, where many remarkable examples of "rifled" cores were observed and collected. Since that time similar phenomena have been observed in various localities throughout the United States and Canada, and samples have been gotten together illustrating a large number of variations in form. After a careful study had been made of the material at hand it seemed desirable that certain data should be obtained from the experience of others regarding the normal action of diamond drills in forming cores, portions of which are occasionally rifled, before an attempt was made to draw any conclusions as to their cause.

Jan 5, 1916

By Augustus J. Bowie

THE discovery of the auriferous cement gravel deposits in and near Deadwood Gulch, Lawrence County, Dakota Territory, in 1876, created a mining excitement, and rush to the Black Hills. Numerous ten and twenty-stamp mills were built on Deadwood Gulch ; Central City and the town of Deadwood sprang into existence, and became the centres of the mining industry of the Hills. Gold quartz deposits were subsequently discovered and located on a so-called mineral belt, extending from Whitewood Creek on the south, to Deadwood Gulch on the north. A northerly group of these quartz locations was purchased in December, 1877, by parties in San Francisco,, who formed a company, incorporated under the name of the Father de Smet Consolidated Gold Mining Company. This company immediately commenced the work of exploration. The deposits were proved to be extensive, and easily mined, but it was found that the ore, on an average, would not. yield more than $10.00 per ton* of 2000 pounds. At this time the cost of supplies and materials in the Hills was high. Miners' wages were $3.50 per diem, and custom mills charged $6:00. per ton. The successful working of mines on "the belt" necessitated cheap milling. The ores being of so low grade,† this could be accomplished only with large and economically running mills. To insure the greatest possible economy, the Father,& Smet mill * Up to December 31st, 1879; the de Smet mine had produced bullion of the value of $718,211.68 from 76,155 tons of ore, being an average value of $9.41 per ton. During the year ending December 31st, 1879, the mine produced 46,344 tons, which yielded $425,360.42, or $9.18 per ton. The total gross cost of working for the corresponding period, including deadwork, exchange, legal expenses, fete., wits $219,914.82. The yield of the mine for the year 1880 (Engineering and Mining Journal, February 5th, 1881), was $600,011, with total expenses of mining and milling, of $313,108. † The first 4083 tons extracted from the de Smet mine, were selected, yielding $62,783.97. The next 25,728 tons produced $230,067.24. The total 29,811 tons were weighed, and worked at custom mills. The yield of the first 409 tons from tine Golden Terra Mine was $11.44 per-ton.

Jan 1, 1882

ON FEBRUARY 13, 1953 the Miami Copper Company signed a contract with the United States Government, through the Defense Materials Procurement Agency, whereby it under- took, with a base price of 27.359 per lb (subject to escalation based on wage scales and wholesale-price indices), to exploit a new ore body in its mine in Gila County, Arizona. Recoverable ore was estimated at 23,000,000 tons, averaging about 0.677 per cent copper. Moreover, the proportion of oxidized copper, difficult to recover by flotation concentrating, was so high that an average net recovery of only ten pounds per ton (0.5 per cent) was expected. The company proposed to mine the ore by the underground method known as undercut block-caving. Unfortunately the ore body, as has been true of all Miami's ore bodies, lay so deeply buried that no possibility existed of adopting opencut mining as has been done in recent years at Miami's neighbors, Ray and Inspiration. Probably the most distinctive characteristic of Miami's operations has been the extent to which it has developed and improved methods and equipment for underground mining. True, necessity was a potent stimulant, because its available ores since 1926 have been exceptionally low-grade; so, if the enterprise were to survive, it was necessary to keep costs at the minimum. This fact does not detract, however, in any way from the remarkable achievements of Miami engineers in conducting efficient and low-cost underground mining.

Jan 1, 1957

By Fred C. Bond

Many grindability tests have been made in the Allis-Chalmers laboratory since the tabulated results were last published.' The lists of standard ball-mill and standard rod-mill grindability tests are brought up to date in this paper, and considerable new material is added. This includes a tabulation of open-circuit grinding tests, with impact and compression-crushing tests. The standard ball-mill grindability tests (Table I) were made in a standard laboratory ball mill, 12 by 12 in. inside, running at 70 rpm, with a charge of 285 iron balls ranging from 1½ to 3/4 in. in diameter and weighing 20,125 grams. Seven hundred cubic centimeters of minus 6-mesh stage-crushed dry feed was used, and the circulating load was maintained constant at 250 pct by adjusting the number of mill revolutions for each grinding period. Tests were made at all mesh sizes from 28 to 200, and the grindability is the number of net grams of screen undersize produced per revolution. The table includes 479 tests. It has been calculated that the ball mill does 52.3 joules of useful work on the ore per revolution2 with 93 joules input to the mill. The standard rod-mill grindability tests (Table 2) were made in a laboratory tilting rod mill, 12 in. in diameter by 24 in. long inside, with a wave-type lining, running at 46 rpm. The grinding charge consisted of six I1/4-in. diameter and two 13/4-in. diameter steel rods, all 21 in. long and weighing 33,380 grams. The mill was rotated level for eight revolutions, then tilted up 5' for one revolution, down 5° for one revolution, and returned to level for eight revolutions. It was discharged by tilting downward at 45° for 30 revolutions. Feed consisted of 1250 cc of minus in. stone and the circulating load was maintained constant at 100 pct by adjusting the number of mill revolutions for each grinding period. Tests were made at all mesh sizes from 3 to 65, and the rod-mill grindability is the number of net grams of screen undersize produced per revolution. The table includes 105 tests. The impact and compression-crushing tests (Table 3) are given in a table that is an extension of a previous publication8 in which the method of testing was described in detail. Two equal hammers weighing about 30 lb each were arranged to strike simultaneous blows on opposite sides of the test specimen. Broken pieces of rock passing a 3-in. square and retained on a 2-in. square were set up with the smallest dimension between the hammers, and this distance was measured. The height of the hammers was increased slightly before each blow until the specimen broke, and the foot-pounds per inch of thickness was calculated. Ten pieces

Jan 1, 1949

By C. D. Hall, F. E. Dollarhide

Fluid Ioss agent.s for crude oil and for water have been studied in dynamic tests. A treatment using a spearhead with a fluid loss agent followed by plain fluid appears feas ible in crude oil, but not in water. An equation for spearhead depletion shows that spurt loss relative to fracture width must be low, if the portion of spearhead fluid in the treatment is to be small. The presence of colloidal matter in crude oils aids the fluid Ioss agent. Unlike in kerosene, where flow limited the agent deposition, in crude oils the filter cake continually formed and leak-off declined. The volume-time relation varied somewhat for different crudes, but was best described by a square root of time function. Spurt loss was inversely proportional to agent concentration. After the fluid loss agent initiated the filter cake, the crude oil colloids built on it effectively. A 2-minute or a 5-minute spearhead with double the normal agent concentration gave the same fluid Ioss curve as the same concentration did for a 30-minute test. The agents tested in water gave fluid Ioss plots on which, for the first few minutes, volume was proportional to the square root of time, but later became proportional to time. For fracture area calculation the customary square root of time function is a satisfactory approximation. Leak-off rates and spurt losses were higher in water systems than in oils. The spurt Ioss tended to be inversely proportional to concentration. In spearhead tests, the filter cakes were not eroded by water flow. However, the rather high spurt loss values make spearhead treatments impractical for water-based fluids. Introduction The effects of dynamic testing conditions on the performance of fluid loss agents in kerosene have been studied previously.' We have extended the work to include crude-oil- and water-based fracturing fluids. An understanding has been gained of the mechanisms of formation and functioning of the filter cakes of fluid loss agents. The practical aspects of evaluating performance of agents in relation to fracture area calculations also are considered. The feasibility of using the fluid loss agent in a spearhead stage of the treatment is examined further for both types of fluids. Experimental Procedure The dynamic fluid loss tests were performed in an apparatus similar to the high-pressure apparatus described in a previous publication.' A fracturing fluid was circulated over a rock surface located in a closed pressurized loop. The fluid flowed axially over the cylindrical surface of a core 2 in. in diameter X 3.5 in. long, mounted (with the flat ends sealed off) in a pipe, with 0.117 in. annular clearance. The filtrate was collected in a central hole in the core and led through valves to graduated cylinders. Provision was made for changing quickly the circulating fluid during the test (spearhead runs) without interrupting the filtration pressure. The only modifications were to add heating tapes and water jackets for the tests with crude oils, all conducted at ISOF, and to change all parts exposed to the test fluid to stainless steel for the tests with water-based fluids. The latter tests were made at room temperature, 80F. Three crude oils were tested. A mixed crude, obtained from a local refinery, contained a considerable amount of light ends. For safety reasons, it was stripped to 250F vapor temperature before use in the fluid loss tests. The other two oils were used as obtained from lease tanks. One was a greenish-brown, 37" API paraffinic crude, and the other was a black, 32" API asphaltic crude. The fluid loss agent for oil, here designated for brevity as Agent A, was Adomite@ Mark II*, a granular solid commercial agent, the same as previously tested in kerosene.' Three different compositions of fluid loss agents were tested in Tulsa tap water. Agent B was adomit& Aqua*, a solid commercial fluid loss agent, comprising clays and hydrophilic gums principally derived from starch. Agent C was a mixture of three parts of Agent B with two parts of silica flour. Agent D was Dowel1 J137, a mixture of guar gum and silica flour. The test cores were cut from contiguous blocks of Berea or Bandera sandstones. For the oil tests, the cores were oven dried, evacuated, saturated with kerosene, and the kerosene permeability was measured. The cores used with the water-based fluids were pretreated by saturating with 3 percent calcium &loride solution to minimize pemeability damage by the fresh water due to clay migration. The

Jan 1, 1969

By C. F. Gates, H. J. Ramey

Recent literature shows that pronounced increases in oil recovery can result from the use of miscible systems in recovery operations. This literature also points out certain problems associated with maintaining miscibility, e.g., compositional changes resulting from alterations in pressure and temperature or from zone dilution. The purpose of the work described in this paper was to study miscible zones for possible use in waterflooding operations and examine the manner in which these zones break down. The fluid system selected for study was oil—terNary-butyl alcohol—water, which, because of its narrow range of miscibility, is ideally suited for investigation in short, linear systems. The laboratory-observed effects on oil recovery and zone stability of a number of variables are reported. Among the variables investigated were miscible zone size, viscosity ratio, length of travel, and interstitial water saturation. Results obtained with this system show that interstitial water adversely affects recoveries because of premature phase break. Salinity of the water further aggravates Ais situation. This effect, although pronounced for this system, would probably occur in any fluid system containing an alcohol. As expected, viscosity ratio has a decided influence on recovery efficiency and zone stability. The results also show that use of a suficieno zone size, even though the system has poor phase characteristics, yields higher oil recoveries than are obtained from straight water floods. Length-of-travel studies showed a square root relationship between zone growth and path length for favorable viscosity ratios. No such clear-cut dependence was observed under unfavorable viscosity conditions. INTRODUCTION As new oil reserves have become increasingly more difficult and expensive to find and develop, the oil industry has devoted more and more time and money to finding more efficient methods for exploiting known reserves. The increasing number of water floods is one manifestation of this attempt to improve oil recoveries from existing fields. Since considerable quantities of oil are by-passed by the waterflood process, it is only a partial answer to the problem. The search continues. Of late, several proposed processes have received the critical attention of investigators. Among them are gas drives, in situ thermal reactions and miscible displacements. The present paper is concerned with miscible displacements in conjunction with water floods. Recent literature1- reports that, under proper conditions, oil recoveries from LPG floods, propane sweeps, condensing gas drives, etc., approach 100 per cent of the oil in place in the region contacted by the flood. This literature also points out some of the problems associated with these processes, one of the main ones being the maintaining of miscibility. Compositional changes resulting from pressure and temperature variations or from zone dilution give rise to phase breaks and loss of miscibility, the conclusion being that, after loss of miscibility, much of the beneficial influence of the zone is lost.' The results of the subject work show that, if sufficient zone material exists ahead of a phase interface, considerable improvement in oil recovery can be obtained. In order to increase our understanding of the behavior of miscible systems as they degenerate into immiscible processes, a laboratory system having rapid deterioration characteristics was needed. The fluid system oil—ter tiary-butyl alcohol (TBA)—water possesses these properties and was the system investigated. Although these fluids are different from those generally employed in miscible studies, an understanding of their behavior can be applied to other miscible slug processes. However, under conditions where mass transfer maintains a miscible system through multiple contacts, e.g., enriched gas drive or high pressure gas drive, the observed behavior of alcohol zones would not be applicable. The variables of interest were zone size, viscosity ratio, length of travel, initial water saturation, rate and core characteristics. Of these, only the effects of the following on zone breakdown and oil recovery are reported in detail: (1) zone size, (2) path length, and (3) initial water saturation. The effects of viscosity ratio and core characteristics are discussed in conjunction with other variables. Although initial water saturation is not envisioned as important to the phase behavior of hydrocarbon systems, e.g., LPG, it is important in alcohol systems. The properties of the fluids and cores used are given in Table 1. As previously stated, this fluid system was selected because of the limited range of miscibility

By Craig R. Barrett, Jack L. Lytton, Oleg D. Sherby

The types of substructures developed during high-temperature creep of (110)[001]-oriented polycrys-talline Fe-3.1 pct Si were examined by electroetching of dislocation sites. Edge dislocations were observed to accumulate adjacent to grain boundaries and poly-gonize perpendicular to their glide planes to form a "Pile-up" of nearly parallel tilt boundaries. The dislocation density developed within the grains during steady-state creep was found to increase with increasing stress. The formation of periodically spaced groups of edge dislocations along grain boundaries was observed, and it was proposed that these formed to relive bending stresses at grain boundary shear .faults. Grain boundary serrations developed at these faults, and it was suggested that this was a result of localized grain boundary migration at the polygonized groups. THE authors have conducted a series of high-temperature creep tests on (110)[001]-oriented poly-crystalline Fe-3.1 pct Si sheet. The creep specimens were examined at various stages of creep by means of electrolytic etching of dislocation sites using the chrome-acetic acid solution developed by Morris.' Hibbard and Dunn2 have demonstrated that the etch pits produced with this technique correspond to single dislocations. It is the purpose of this paper to present and discuss the dislocation substructures which were formed during high-temperature creep at constant stress. EXPERIMENTAL PROCEDURES The polycrystalline Fe-3.1 pct Si sheet employed in this study contained a (110)[001] texture. This texture was quite strong, and the elastic properties of the sheet closely approached those of a single crystal of iron.3,4 A typical analysis in weight percent for this material is 3.1 Si, 0.1 Mn, 0.003 C,

Jan 1, 1965

Jan 1, 1967

By J. H. Swisher

The solubility of sulfur and rate of solution of sulfur in pure Lron were measured in H2S + H2 and H2S + H2 H2O gas mixtures. The solubility and diffusivity of sulfur at 1410°Care 0.13 pet S and 1.0 x 10-5 sq cm per sec, respectively. The solubility iS the same, but the rate of sulfurization is slower in the presence of H2O in the reacting gas. Under these conditions, the over-all rate is controlled jointly by a slow surface reaction and by solid-state diffusion; the mechanism for the surface reaction has not been identified. KNOWLEDGE of the behavior of sulfur in solid iron is desirable for the metallurgy of such products as free machining steel, where a high sulfur level is required, and inclusion-free high-strength steels, where the sulfur specifications are very low. The present investigation was undertaken to check previously reported values for sulfur solubility and diffusivity in 6 iron, and to study the poisoning effect of chemisorbed oxygen on sulfurization kinetics in H2-H2S-H2O gas mixtures. All of the experiments were performed at 1410°C. The thermodynamic behavior of sulfur in 6 iron was the subject of a paper by Rosenqvist and Dunicz.' The sulfur solubility at 1400" and 1500°C was determined by equilibrating pure iron specimens with H2-H2S gas mixtures. The maximum solubility of sulfur in 6 iron was alsc determined by Barloga, Bock, and parlee2 by reacting iron wires with sulfur in sealed capsules. In another investigation, the diffusion coefficient of sulfur in 6 iron at temperatures up to 1450°C was measured by Seibel.3 The method used was to measure sulfur concentration profiles in diffusion couples containing radioactive sulfur EXPERIMENTAL Apparatus. A vertical resistance furnace wound with molybdenum wire and containing a recrystallized alumina reaction rube was used for the experiments. The hot zone in the furnace was approximately 2 in. long with a temperature variation of ±3oC. The hot zone temperature was automatically controlled to within ±2°C, and the test temperature was measured with a pt/Pt-10 pet Rh thermocouple before and after each experiment. Flow rates of the reacting gases were obtained using capillary flow meters. Materials. The source of H2S in the gas train was a premixed cylinder containing 5 pet H2S in H2. This mixture then was diluted with additional hydrogen and argon. In some experiments, water vapor was introduced by passing hydrogen and argon through a column containing 10 pet anhydrous oxalic acid and 90 pet oxalic acid dihydrate. The vapor pressure of water above this mixture is well-known.4 Argon was used as a diluent to minimize thermal segregation of H2S in the furnace5 and to reach higher H2O:H2 ratios than could be obtained in mixtures of H2 and H2S alone. Argon was purified by passage over copper chips at 350°C and subsequently over anhydrone. Hydrogen was purified by passage over platinized asbestos at 450°C and then over anhydrone. The H2-H2S mixture was purified by passage over platinized asbestos and then over P2O5. The specimen stock was made by melting and vacuum-carbon deoxidizing electrolytic "Plastiron" in a zirconia crucible. The principal impurities are listed in Table I. In some of the equilibrium experiments, six-pass zone-refined iron was used to minimize impurity side effects. This zone-refined iron had a total impurity level of about 25 ppm. Procedure. Specimens were annealed in hydrogen for a period of at least 2 hr at the beginning of each experiment. The specimens were held in the reacting gas for times varying between 10 min and 17 hr, and cooled to room temperature in a water-cooled stainless-steel block at the bottom of the furnace. The pH2S/pH2 ratios reported are those for gas equilibrium at 1410°C. Calculations based on available thermodynamic data8 showed that the only other gaseous8 species that formed in significant amounts in the furnace were S2 and S. Even when water vapor was introduced into the gas mixture, the concentrations of SO2, SO, and so forth, were negligible. The initial partial pressure of H2S was therefore corrected for its partial dissociation to S2 and S in determining the equi-

Jan 1, 1968

By R. E. Zimmerman, T. W. Guy

IN approaching the problems of sampling coal, a brief statement of certain facts that are more or less taken for granted may be helpful: 1. The coal-mine operator needs reliable data as to the physical and chemical characteristics of his coal in order to plan and control intelligently its mining, preparation, and marketing. The consumer needs such data in order to select the equipment and the coal best suited to meet his requirements, to check the quality of fuel delivered, and the efficiency of its use. Various government control agencies require such data as a basis for classifications and establishment of limits, for use in carrying out the requirements of federal, state or municipal laws. 2. All such data must be obtained by analyses, measurements, or tests made on samples, which are taken to represent the coal tested. It is now becoming generally recognized that, in accordance with statistical laws, test results from samples are not expected to represent the exact qualities of the lot or lots from which they are taken, except within statistical, or "expected" limits. Such limits are definitely specified by some present standards of the American Society for Testing Materials and the British Standards Institution. 3. Samples that give ash within satisfactory limits are usually assumed to be sufficiently accurate for other analyses, except under special conditions such as meeting close specifications for coals showing wide variability in sulphur, fusibility of ash, or other quality. 4. In modern coal sampling the increment is recognized as the basis for taking samples. For a given accuracy the number and weight of increments specified are increased with: (a) the expected ash, and (b) the top size designation of the lot to be sampled. 5. It is extremely important that every sampler recognize that: the specified number and weight of increments are minimums, and that the precautions to be used in order to take them properly are also minimums; that in the reduction of the gross sample the sizes specified for the coal after each stage of the crushing are maximum; that the quantities specified to be taken after each crushing stage are minimum; that any short cuts or failures to meet the requirements specified will reduce the statistical accuracy of the results, although it is possible that one or two checks on a few results may seem to show otherwise.

Jan 1, 1950

By H. W. Graham

THE young metallurgist of today who thinks casually of the technical literature of the steel industry might conclude that little has been published concerning the Bessemer process. This conclusion is true as relating to the last decade or two, but there is a fairly voluminous Bessemer literature in the period of 1860 to 1910, Since that time, however, an entirely new level of metal-lurgical knowledge of steelmaking has been reached; and the present paper is simply an effort to look broadly from this new level and to bring the recorded history of the process up to date, It is an effort to appraise the acid Bessemer method of steelmaking in the light of today's technical knowledge thereof. In this paper matters of history will be dealt with only insofar as they contribute to an understanding of today's situation. Attention will be directed to the apparent causes of past developments in seeking to perceive the true direction of trends now in existence and effective as bearing upon future developments. The paper will discuss the economics of the Bessemer process, but only to the extent that will bear upon the metallurgist's understanding of his respon-sibility. The problem of the quality of Bes-semer steel will be reviewed and examples will be given of the technical data upon which the reasoning of the paper is based, Matters of engineering design, mechanical maintenance, operation and metallurgical investigation will be surveyed. Compari-sons will be made between the Bessemer and open-hearth processes for the sake of clear and ready understanding,

Jan 1, 1940

By HENRY JULLUM

THE ARGONAUT' mill stands at the crest and spreads down the western slope' of a hill, which incidentally covers the' outcrop of the Argonaut vein' at this point. The collar of the main shaft of the mine is situated on the eastern slope of the same hill 120 ft. below the highest ?point. The present mill, built in 1916, was designed to treat 250 tons per 24-hr. day. This capacity has not been attained recently owing to the inability of the mine to produce enough ore while extensive development and underground construction were under way. At present, however, the mine is more than able to take care of the mill requirements.

Jan 1, 1932

By D. L. Luffel

This paper presents two main developments: (1) a short, constantly accelerated centrifuge method of measuring drainage capillary pressure properties of cores, and (2) a new analytic method of treatment of centrifuge measurements to obtain saturation-capillary pressure relations. Toward the first objective, a clever experimental method is presented which is certainly more rapid than previous centrifuge methods. Toward the second objective, a new analytic method is derived to eliminate the approximate method of Hassler and runner. The derivation of this new analytic method, however, appears to be in error. The new analytic solution is developed as Eq. 5 in Appendix A. At the beginning of this derivation, the average wetting phase saturation of a core is expressed as, where is the centrifuge angular velocity. Eq. D1.2 makes explicit the dependence of S and S upon The second equation shown in Appendix A expresses the relation between the three variables Since for a given porous medium the saturation is uniquely related to capillary pressure, the functional dependence of S upon P is trivial, i.e., Pc.ri does not actually appear. Thus, the function 5 (r, ) may be expressed as a new function, S*, of PC, , alone The author transforms the variable of integration in Eq. Dl through use of Eq. D2 and writes

Jan 1, 1965

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