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Clarence M. Haight, Franklin Furnace, N. J. (communication to the Secretary*).—In that part of Mr. Wilson's paper describing the Gilman cut-and-fill system, a few features do not appear to be fully explained. In what way is the waste used for filling obtained? The text mentions that if waste is encountered when driving the filling raises, these raises are stopped until the fill is needed; that seems to suggest mining the capping for fill, which might make the backs of the stopes bad as the stopes approach the top of the ore. If, on the other hand, the fill is brought to the raises in cars, are the crosscuts that are necessary in ore or waste? Is the cost of this fill included in the stoping costs given? The second, or lower, series of stopes will present a different problem to that which the first series (under the capping) gave. Although no mention is made in the text, it would seem that the second series of stopes will have to be worked on center lines which are offset half the stope width, 20 ft., from the centers of the stopes above, in order to take advantage of the "rafter" effect of the stringers so named. How is the fill to be introduced into the lower stopes? There are no crosscuts mentioned to provide for this; or is it intended to tap the filled stopes above for the fill? In the latter case the method of control of this fill will be of interest. Ore that will admit of a stoping width of 40 ft. with the lengths mentioned in the description is stronger than any with which many mining men are familiar. Has the practice of starting to mine a second stope before the preceding one is filly completed been tried to any extent? If

Jan 1, 1917

By J. L. O’Brien, M. Suenaga, K. M. Ralls, V. F. Zackay

The effecls of aging a1 400°C on tile resistive transition at 4.2°K of a superconducling 70Zr-30Nb alloy are reporled. Microstrclural changes were studied by critical temperature, resistiue critical field, residual resistiuily, and microhardness measurements and by X-ray diffraction, optical microscoby, ad replication electron microscopy. The result of the aging treat- A defect-free Type 11 superconductor in a magnetic field above Hc1 cannot sustain a transport current runt is a fine array of w-phase pavticles with a mean center to center interparticle spacing of about 800A. At an aging time of 300 hr the maximum onset critical current density is rcached. The particle size at the maximum current density if about 4202. At times longer than 300 hr effective particle impingement leads to lower onset critical current densities. perpendicular to the applied field without power loss in the sample.'-3 This power loss is due to flux line motion caused by the Lorentz force and is manifested by a longitudinal voltage.4-6 When defects are present in the material, flux lines are pinned until the Lorentz force exceeds the "pinning force". That is, it is thought that flux lines reside in free-energy wells existing at the defects, and the critical Lorentz force is that which when integrated over distance will supply the free-energy difference necessary to move the flux

Jan 1, 1968

By M. Van Siclen

THE outstanding fact in connection with dust disease in the United States at present is the growing recognition of its seriousness by state officials and by the more progressive operators of mining, metallurgical and allied industrial plants. The same may perhaps be said of labor in some of its better organized centers, but the average independent non-union workman continues, .as of yore, to suffer the toll of disability and even of death from dust inhalation without realization of the source of his ill-being. Progress in the betterment of the handling of sufferers from dust disease and of the conditions creating dust hazards in mining and allied industries is pursuing a course similar to that of the now widespread campaign against accidents, in which the risk is more obvious, more severe, and was naturally recognized sooner. The coming on of dust disease is generally relatively slow and its immediate effects not infre-quently masked by or attributed to other diseases. Marked exceptions to this general rule have occurred in districts where the dust is particularly pernicious, such as the Rand and Joplin; yet such exceptions, unhappy in themselves, opened the eyes of medical men, and of those in other localities charged with the responsibility for the welfare of industry, to the much more widespread if less spectacular hazard existing from the inhalation of dust in all rock-excavating operations and all industrial operations creating inorganic dust, whether it be crushing and grinding, sand-blast-ing, granite-cutting, or what not. Advancement to date in the United States in prevention and treat-ment has been slow, yet the record shows that quantitative methods for determining the degree of hazard and means for decreasing it were being developed as far back as 25 years ago; and that more rapid progress may be looked for from now on. In 1908, in this country; F. L Hoffman?(1) discussed the mortality from consumption in dusty trades, especially brass foundries; and in 1913 E. R. Hayhurst(2) described the effects of inhalation

Jan 1, 1933

By Albert J. McIntosh

With petroleum consumption declining temporarily after V-J day, the oil industry is urged to use this period as a kind of stopgap to rebuild its war-depleted inventories and help cushion the effect of this decline on producers and refiners. Higher inventories should be reestablished, since recent experiences have indicated that, by and large, the present inventories of crude oil are too low even with the tremendous current production available. The following analysis indicates that inventory levels could be built up to about 490,000,000 bbl. by the end of 1947, an increase of about 40,000,000 bbl. over the reported stock estimated for the war's end. If at the end of the war the military have some 20,000,000 bbl. on hand, this inventory will either be resold to the industry or certain demands that have been assumed to be met by industry will be supplied out of these military stocks, which would leave about 20,000,000 bbl. (net) to be built up from current production. For stock rebuilding the industry could use 10,000,000 bbl. of crude plus 10,00,000 bbl. of products, totaling 20,000,000 bbl. If this were spread over a year, this would mean 55,000 bbl. a day. By analyzing the average inventories held in a year with the total quantity of goods handled during the year, the following study and tables indicate how far the inventories should increase in the immediate postwar period. Introduction For the period immediately following V-J day, most of the petroleum economists have forecast a considerable decline in the total consumption of petroleum and its products in the United States. This will be caused by the elimination of most of the military demands and the inability of civilians to immediately replace automobiles, burners, etc., and thus increase their requirements to make up for the military decline. When the automobile industry has been back on full production for two or three years, civilians will be able to consume much larger quantities of gasoline. Delay in the manufacture of new oil burners and the time it takes to construct new homes, adds up to the same story for distillate fuels. In reviewing this outlook, the question has arisen whether the petroleum industry should not use this period of lower consumption as a kind of stopgap to rebuild its war-depleted inveritories and help cushion the effect on producers and refiners of this sudden drop in requirements. Some persons have indicated that hundreds of thousands of barrels a day could be used for this purpose extending over a year or more. Refineries will be in existence, which could run over 5,000,000 bbl. of crude oil a day and crude-oil production might be running 600,000 to 700,000 bbl. a day above the demands now forecast for the period after V-J day. Reasons for. Making Inventories In order to plan intelligently for this period, the petroleum industry should determine the needs for the establishment of higher inventories for crude and petroleum products than have been carried during the war. The reasons for trying to make such a determination are as follows:

Jan 1, 1945

By E. T. Turkdogan, P. Grieveson

Experimental results are given for the rate 0.f solution of nitrogen in y iron in the temperature range 1000° to 1200°C. It is shown that, when purified reacting gas is used, the rate-controlling process is the diffusion of nitrogen into the iron. The difhsiuity of nitrogen in y iron is calculated from the results and the equation logD = —(8800/T) — 0.04 is recommended to represent the temperature dependence of the diffusivity. In some experiments using unpurified nitrogen, solution rates are found to be slower than those attributable to a solely solid-state diffusion process. Indications are that in the presence of impurities in the gas, e.g., H,O, chemisorption of nitrogen at the surface is hindered and becomes a rate-controlling process for the transfer of nitrogen across the gas -metal interface. ALTHOUGH the solubility of nitrogen in y iron at known nitrogen activities has been well-established,'-a the kinetics of the solution of nitrogen in iron are not known. The work of Darken, Smith, and Filer' indicates that at temperatures below about 1300°C the rate of solution of nitrogen in y iron is controlled by a chemical reaction at the metal surface, while at temperatures above about 1300°C the rate-controlling process is the diffusion of nitrogen in the metal. Fast and verrijps studied the denitro-genization of y iron using wet hydrogen at 950°C and their results clearly indicate that the rate of nitrogen removal is controlled by diffusion of nitrogen in the metal. In Part I of this series of papers, the kinetics of the solution of nitrogen in y iron are discussed in the light of the present experimental work. EXPERIMENTAL Apparatus. The reaction chamber consisted of a platinum wire-wound resistance furnace with a re-crystallized alumina reaction tube. The temoerature of the furnace, which was automatically controlled to approximately 1°C, was measured with a Pt/Pt-13 pct Rh thermocouple and a potentiometer. The temperature distribution in the working zone of the furnace was determined using a calibrated Pt/Pt-13 pct Rh thermocouple and the hot zone was found to be approximately 3 in. long with a temperature variation of * 3°C. A series of experiments was also carried out at 1000°C and pressures above atmospheric using a pressure vessel which was similar in construction to that described elsewhere.1° Materials. Ferrovac E grade iron used in all ex-

Jan 1, 1964

By T. H. Alden

A correlation has been found in rock-salt structure single crystals between the latent hardening, measured by the direct stress activation of oblique slip systems, and the stress-strain behavior in simple compression. Materials with high latent hardening, like LiF, strain-harden at a low rate (Stage I) even when severely constrained. KCl, in contrast, shows low latent hardening and a tendency to strain-harden at a high rate (Stage 11). This correlation suggests that oblique slip is essential for Stage II hardening of these materials. THE role of secondary slip in the strain hardening of metal single crystals is a topic of lively controversy. On the one hand are theories in which secondary dislocations participate directly in Stage II hardening in the fcc metals, for example through the production of sessile dislocations,1 forest intersections, or jog formation. Much of the experimental evidence on which these theories are based has been reviewed by Clarebrough and Hargreaves.~ On the other hand, a recent theory5 denies that secondary slip has an essential role in Stage II hardening or in the transition from Stage I to Stage 11. In the latter view, Stage I is not terminated by an increase in the activity of secondary systems but by the exhaustion of undeformed material.6 The experiments reported in this paper will not resolve this controversy since the materials being studied are cubic ionic crystals rather than metals. However, the results do show in an unusual way a direct connection between "secondary" (nonortho-gonal or oblique) slip and strain hardening in these materials. Specifically, a correlation has been found between two independently measured properties, first the latent hardening of oblique (110)(1i0) slip systems as measured by direct stress activation of these systems, and second the stress-strain behavior at small strains. From prior work, it was known that in most cubi-cally oriented rock-salt structure crystals, two orthogonal slip systems operate and exclude the other equally stressed pair, oblique to the first pair.7'8 This observation apparently indicates that a significant interference exists between slip on oblique (110) planes and a relatively small interference between orthogonal (110) planes. The present experiments were begun with the intent of obtaining a quantitative measure of this difference by means of a study of latent hardening in these crystals. I) EXPERIMENTAL METHODS The experiments were basically of two types, first the determination of stress-strain curves by compression along a single (100) axis, and second the measurement of latent hardening by compressive prestrain along one cube axis followed by the determination of the yield stress in a second (latent) cube direction. All tests were done at room temperature in an Instron machine by compression between lapped, parallel steel faces. Three specimen shapes were used. For long crystals (nominal dimensions, 1/8 in. square by 1/2 in. long) the ends were lubricated with an oil-graphite mixture. Superior results with short crystals (about 1/8 in. cube) were obtained using 0.003-in. teflon film.' Thin crystals (1/4 in. square by 3/32 in.) were used for latent-hardening measurements and similar results were obtained with either lubricant. Test specimens were cleaved from Harshaw single crystals which had been irradiated to a dose of lo8 roentgen using a cobalt-60 source. The irradiation raises the yield stress and tends to prevent plastic deformation during sample preparation.10 Prior to testing, the irradiation hardening was removed by an anneal at 400°C. Ideal compression specimens have flat, parallel faces. In short specimens particularly, satisfactory results demand a close approximation to this ideal. In the present work, cleaved surfaces were often used directly as compression faces. The degree of success using this method depends on two factors: 1) the smoothness of cleavage faces, and 2) the extent to which the crystal is deformed or crushed by the chisel during the cutting of a long crystal into short pieces. Unfortunately, only one material of those studied, LiF, was completely satisfactory. NaF, NaC1, KC1, and KBr behaved less well so that

Jan 1, 1964

By Jack A. Crichton, Henry J. Gruy

This paper discusses methods used in the estimation of natural gas reserves and the general conditions under which the various methods are applicable. The factors used in estimating natural gas reserves are reviewed. Errors which have been found to occur frequently are listed. Introduction The estimation of natural gas reserves has become of paramount interest because of the increasing importance of gas in the nation's economy. Gas is a most desirable fuel, a fact substantiated by the continued rise in the market demand. In addition, new uses for gas are being developed by the chemical, plastic, and associated industries, and plants are being built to make gasoline from natural gas. These are a few of the factors contributing to the importance of the nation's natural gas reserves. With the increased importance of gas there is an increase in the need for reliable estimates of the magnitude and availability of natural gas reserves. These estimates are being used currently: (I) to determine which fields contain sufficient available reserves to justify the construction of pipe-line outlets to serve particular markets; (2) to design pipe lines necessary to serve those fields adequately;] (3) to determine the location of industrial and chemical plants; (4) to finance the development of gas properties, and the construction of gas pipe lines; (5) to determine fair and adequate depletion allowances and depreciation rates; (6) to justify applications for gas pipe lines before various regulatory bodies; (7) to determine the number of wells required to exploit the reserves most economically; (8) to aid in establishing values for the purchase or sale of gas properties, and for purposes of inheritance taxes; (9) to determine equities under unitized operations; (10) to provide a basis for calculating the economics of gas-cycling operations. History or Estimation of Natural Gas Reserves The natural gas industry in the United States had its beginning during 1826 when natural gas was used for lighting the city of Fredonia, N. Y. The first natural gas pipe line was a 25-mi]le wooden line constructed from hollowed logs, connecting West Bloomfield and Rochester, N. Y. There is no record of an attempt to estimate the gas reserve at West Bloomfield but an attempt was made to determine the capacity of the well by measuring the time required to 611 a large balloon. One of the earlier publications concerning estimation of natural gas reserves is the "Manual for the Oil and Gas Industry," published by the Treasury Department, United States Internal Revenue, in i9i9. The following methods of computing "gas depletion" are listed: (I) production decline of the gas well or property; (2) decline in open-flow capacity; (3) comparison with the life history of similar wells or properties, particularly those exhausted Art

Jan 1, 1949

By C. S. Brooks

Several of the commonly used methods for deter-mination of effective grain densities of minerals have been evaluated for accuracy and precision, and their applicability to various types of petroleum reservoir minerals tested. Consideration was given to the effect of consolidation, swelling clay, and wettability on these grain-density determinations. Procedures with helium displacement, a modified low-pressure Boyle's law porosimeter, and liquid displacement (water, n-decane, and n-octanol) were tested. The helium-displacement procedure was used primarily as an independent reference for which the effects of fluid-solid interaction, e.g., adsorption and wettability, were negligible. The procedures with the Boyle's law porosimeter and with liquid displacement are the methods in common use. Minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The number of samples tested, while not large, was adequate to permit application of statistical methods. Grain-density measurements on calcite (Iceland spar) provided a basis of comparison for the accuracy and precision of the procedures under investigation for a material with a high degree of chemical and physical homogeneity and for which fluid-solid interactions were at a minimum. Liquid-displacement procedures (water or n-decane) provided the greatest reliability and precision for measurement of the grain densities of the limestone tested. Gas-displacement procedures (helium or Boyle's law porosimeter) provided the greatest reliability and experimental convenience, if not the greatest precision, for the measurement of the grain densities of the swell- ing clay, Wyoming bentonite, and the shah sandstones which -contained appreciable amounts of swelling, in-terstitial clays. These experiments were designed to evaluate the applicability of the grain-density procedures in common we to some of the less tractable minerals—tight limestones, shaly sandstones, and swelling clays. The results should provide a useful basis for a selection of the method most suitable for application to the various petroleum reservoir minerals encountered and especially for use in the estimation of formation porosity. INTRODUCTION These experiments were undertaken to evaluate the accuracy and precision of several commonly used methods for determination of effective grain densities of minerals, and to test their applicability to various types of petroleum reservoir minerals. Consideration was also given to the effect of consolidation, clay, and wettability on these grain-density determinations. Procedures used included measurements with helium displacement, with a modified low-pressure Boyle's law porosimeter, and with liquid displacement (water, n-decane, and n-octanol). The minerals investigated included calcite, West Texas limestone core samples, California sandstone core samples, and Wyoming bentonite. The accurate determination of the porosity of petroleum reservoir formations, in particular those of low porosity, has received much attention. Both bulk-volume and grain-volume measurements necessary in the evaluation of porosity have been examined by many investigators with the objectives of improving both the accuracy and the precision of these determinations. In this investigation statistical criteria for selection of the most reliable and suitable procedure for use with a given type of mineral are demonstrated. The grain-volume measurement procedures appear to be the most susceptible to improvement.

Jan 1, 1958

By J. W. Rutter, K. T. Aust

The migration of individual, large-angle grain boundaries has been studied as a function of tempereature and solute concentration in specimens of zone i.e filled lead containig very small additions of silver and of gold. Tile results are compared with various the-ories of grain boundary migration and with observations made prev.iorlsly of grain boundary migration in similar specimens of zone-refined lead containing tin additions. A previous investigation by the authors dealt with [he temperature dependence of grain boundary migration in bicrystals of zone-refined lead containing small additions of tin.' It was shown that tin additions as low as a few parts per million cause a large decrease in the grain boundary migration rate at any given temperature, as well as a marked increase in the temperature dependence of the migration rate. It was found that existing theories of grain boundary migration. based on the motion of dislocations. or upon the concept of atom transfer in groups across the boundary (group process theory). or upon the control of grain boundary motion by volume diffusion of impurity atonls along with the boundary. are incapable of accounting for the observations. The single process theory of grain boundary migration. which is an absolute reaction rate calculation based on the transfer ui atoms singly across the moving boundary, was found to predict the migration rate reasonably well for a number of boundaries whose motion was shown to be very little influenced by impurities, but not for boundaries whose illation was influenced markedly by impurities. It was concluded that the elementary process of grain boundary migration involves the activation of single atoms during transfer across the boundary. and that inadequate knowledge is available to permit the influence of impurities to be properly taken into account. The present study was initiated to check the validity of the above conclusions with other alloy systems, namely high-purity lead with small additions of silver and of gold. Both silver and gold diffuse faster. and with a lower activation energy of volume diffusion. than does tin in lead;' consequently, a study of the effects of silver and gold on grain boundary migration in high-purity lead offered a means of testing theories of boundary migration based on bulk diffusion of the solute (eg. ref. 3). In addition. it was hoped that the present work, in comparison with the results for tin in lead, would provide information concerning which factors are important in determin- ing the interaction between solute atoms and a grain boundary. EXPERIMENTAL PROCEDURE The preparation of bicrystals of zone-refined lead, with various silver or gold additions, was identical to that previously described for the lead-tin alloys.''4 Each bicrystal consisted of a striated crystal which was grown from the melt. and an adjacent striation-free crystal which was introduced by artificial nucleation and growth.''4 The striation or lineage substructure in the melt-grown crystal provided the driving force for grain boundary migration. During the preparation of striated single crystals by growth from the melt, it was found that silver or gold concentrations as low as 2 or 3 ppm by atoms were sufficient to cause formation of the hexagonal cell structure. which is due to the presence of impurity, during freezing. This structure is revealed on the solid-liquid interface by decanting the liquid during freezing. The hexagonal cell structure was observed previously4 in zone-refined lead crystals with tin contents above approximately 200 ppm by atoms. These concentrations of silver, gold, or tin are in agreement with the predicted amounts required for cell formation in lead,5'6 under the present conditions of freezing.4 The absence of cell structure at decanted interfaces, therefore, served as a useful indication that the silver or gold contents were less than 2 or 3 ppm by atoms in the specimens as grown. It was found that grain boundary migration occurred only very slowly when the solute content approached that necessary for cell formation. As a result, the present experiments were conducted with silver or gold additions less than 1 ppm by atoms. This impurity level is well within the solid solubility limits for silver and gold in lead.7 The annealing treatments, measurements of grain boundary velocities, and orientation determinations were carried out as described previously.' However. each bicrystal was also chemically polished in a solution consisting of 8 parts glacial acetic acid and 2

Jan 1, 1961

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By B. M. Larsen, T. E. Brower

Introduction and Summary By "thermochemical factors" we refer to those variables which affect the net heat which must be put into the bath in order to make a heat of steel from any given set of charge materials. This is admittedly only one phase of the production rate problem. The whole problem includes also consideration of rate of charging, flame radiation intensity, rate of optimum fuel input obtainable without undue damage to the furnace structure and any variations in conditions such as stirring, slag volume or viscosity which affect the rate at which heat can flow down and away from those exposed surfaces where the heat is first received from the flame. Because a given type of charge in a shop is often considered as being nearly constant in both physical and chemical characteristics from one heat to another, and because such a state of affairs may be thought of as resulting in a reasonably constant net heat requirement, this requirement is usually neglected as an invariable, inevitable matter, about which nothing can be done. With normally variable charge, and variable percentages of limestone and cold pig, however, the net heat requirement can be subject to very appreciable change; it may also be affected by such things as the currently popular procedure of blowing oxygen into the bath. To bring the general problem of production rate into better perspective, therefore, it seems worthwhile to try to evaluate the net bath heat requirement and the amount by which it may change through variation in different factors. Because our calculated values of net heat are admittedly uncertain, we have tried to check them in part by statistical data on actual production rates over rather large groups of commercial heats. The results of calculation of net heat requirements in a wide range of actual commercial practices may first be summarized briefly. We find a wide range between the extremes of different practices, as would be expected, with duplex practice (essentially blown metal plus hot metal) having essentially a zero net heat requirement, an all-cold charge practice somewhat over I million Btu per ton of steel and a high hot metal practice about 0.75 million Btu per ton. Over the commercial range of scrap plus hot metal practice, increasing the percentage of hot metal from 40 to 78 pct, with other factors nearly constant, decreased the net heat by only some 5-10 pct. The net heat is increased by about 1.2 pct for each I pct of the metallic charge present as cold pig. Calculated values of oxygen supplied by air varied from about 25 up to 60 lb per ton of steel, and in a 60 pct hot metal practice, an increase from 32 to 52 Ib oxygen from air decreased the calculated net heat from 0.88 to 0.74 million Btu per ton. Use of pure cold oxygen to substitute for about one half of the total charge ore (about 28 Ib oxygen replacing 145 Ib ore per ton of steel) decreased the

Jan 1, 1949

By Robert H. Dickson

Limestone replacement and contact metamorphic orebodies are 80 irregular that sampling and estimating are far less. exact than in more regular types of deposits; both the mineralized masses and the lenses of ore within them are extremely irregular. So much development work is required to find the ore that the expense of blocking out great tonnages is prohibitive; furthermore, the rock near these orebodies is so heavy that drifts or raises cannot be kept open for many years without excessive repairs. As a result, few mines in limestone have more than three years supply of ore in sight. As most of the ore, is developed by stoping— not by drifting, raising, or drilling—estimates of ore developed do not indicate the total amount of ore that may be expected; they simply indicate the relative condition of the mines. But even if they are to do this, they must be made according to a fixed plan, intelligently carried out. The estimates of ore in the Calumet & Arizona Copper mines, Warren District, Ariz., have been of much value to those who plan the mining and development work. This paper describes the methods of sampling and estimating used in these mines. Sampling Samples are taken in various ways and depend on the condition of the working and the purpose for which the sample is to be used. Drifts, crosscuts, and raises are sampled by channels or by taking a grab off each mine car as it is filled. Stopes are usually sampled by drill holes or by taking a representative sample off each mine car; the latter, or chute, sample is by far the best sample. All workings are studied periodically by an engineer, who makes graphic and detail notes of the geologic structure, as shown in Fig. 1. The daily car tally and assay of each particular working is added to the same sheet opposite the material it represents. These sheets make a permanent record, showing the exact boundaries as well as the grade of ore in all workings.

Jan 1, 1925

By A. T. Peters

DURING an investigation concerning the use of large nozzles for pouring of low-carbon rimming steels, the practical details of which were reported elsewhere, it was noticed that increases of nozzle sizes were generally followed by improvements of slab surface quality. It is the purpose of this note to present the data available and some tentative opinions about this phenomenon. The problem of correlating pouring rates with the metallurgical performance of steels is complicated by several factors. The two most important are; 1) Variations of the steel pouring rate throughout a pour, these being due to the nozzle erosion, which enlarges the bore area, and the dropping ferrostatic pressure in the ladle. The pouring rate is lowest towards the end of a heat when the ladle is nearly empty. 2) Variations in the ingot pouring time due to the different ingot weights poured. Consequently, the use of the average pouring rate of a heat may not be exact, but in large-scale production it is not practical to treat ingots separately according to their pouring rates. The variations of ingot weights and sizes may be overcome by considering the rate of rise of steel in the mold. Hence, the average rate of filling of molds throughout the pour of a heat, inches per second, will be used in this note. Every ingot rolled at Inland is rated at the blooming mills prior to hot machine scarfing as being good, fair, or poor for cracks, scabs, and checking. The latter term refers to the network of breaks or lines associated with overheating or burning in the soaking pits. It is also known that thin-skinned steel is prone to show this defect if the subsurface blowholes are exposed during reheating or rolling. The experiences with the surface quality of slabs rolled from ingots poured at different rates are presented in Fig. 1. The data represent nearly 11,000 ingots. It appears that all three types of defects are in-

Jan 1, 1960

By A. R. Elsea, E. E. Fletcher

This paper describes a metallographic investigation of the influence of tungsten or molybdenum additions upon the transformation and precipitation reactions occurring in Co-rich Co-Cr alloys. It is shown that tungsten has little effect upon the a-ß transformation temperature range, while molybdenum tends to raise it. Both elements tend to promote the formation of ? phase, molybdenum being more potent in this respect than tungsten. HIGH temperature alloys, that is, alloys which have load-carrying ability at elevated temperatures, have been developed at an increasing rate during the past few years. This has resulted from the requirements in the design of modern aircraft engines. Although many alloys of this type are available, they have been developed on an empirical basis. Metallurgists do not have a clear understanding of the phases or structures that are responsible for these high temperature properties. In order to determine why these alloys possess this particular ability, a project was started at Battelle Memorial Institute with the object of learning more about the fundamental factors which promote high temperature strength in alloys. This study was to include a correlation of microstructure and the high temperature properties of Vitallium, an alloy which is widely used for high temperature service. Vitallium is a complex material both from the standpoint of composition and microstructure. Consequently, it was necessary to obtain informa- tion regarding the phase relationships in this alloy. The Co-Cr binary diagram was determined as the first phase of this investigation.' A second paper described the effects of iron, nickel, or nitrogen on the reactions occurring in the Co-rich end of this system.' The present paper covers a continuation of this investigation in which the effects of tungsten or molybdenum on the reactions occurring in Co-rich, Co-Cr-base alloys were determined. Preparation of 'rest Materials Two series of ternary Co-Cr-base alloys, representing Co-Cr ratios of 80:20 and 68:32 ( Cr x 100 =20 and 32 ) , were prepared containing ( Co + Cr = up to 6 pct W and up to 12 pct Mo. Melting stock consisted of electrolytic Co, electrolytic Cr, 99.9 pct pure W, and 99.9 pct pure Mo. Table I lists the chemical analyses of these materials. The melting furnace was a vertical porcelain tube

Jan 1, 1952

By D. Mills, G. B. Craig

The defortnaliotz of zirconicltt single crystals conlaining osygen in the range 740 to 6800 atom parts per nilllion was esanined oc7er the range 77" to 950°K. An anctlsis of the dqfarmaliotz parameters leads to the cotcllsiotr that the rale -cotzfrolling thermally activated dqivr,irrtion process oe-r /he range 77" to 560°K is oc.crco,ling osvgen alotns. A thermally actitaled defor,ilntion process is not found between 600" and 800", but does occur aboz%e 800°K. THE present investigation was undertaken to measure the effects of controlled amounts of oxygen on the deformation parameters of a zirconium single crystals over the temperature range 77" to 950°K and to determine the rate-controlling mechanisms. Although there is no doubt that the mechanical properties of the group IV metals, titanium, zirconium, and hafnium, are strongly influenced by the interstitial impurities oxygen, nitrogen, carbon, and hydrogen, there are many conflicting theories as to the role played by the interstitials during the deformation proess.'- There is general agreement that the mechanisms which control plastic flow in a metal impose characteristic values on such parameters as the flow stress and its temperature dependence, the activation volume, and the activation energies. These parameters will be used to analyze the deformation mechanisms. eltham,' Sargent,16 and ibbs' have shown that the stress relaxation technique allows the activation volume characteristic of the deformation process to be found during the course of a simple tension test. In many cases it is found that the relaxation of stress is logarithmic with time and obeys a relationship of the following form: T-T = AT =S logl0(qt + C) [I] where t, is the shear stress at the start of the relaxation test, t is the shear stress at time t, and S. q, and C are experimental constants, and S is the strain rate sensitivity of the stress t as shown in the appendix. The slope found from a semilogarithmic plot of At vs time is approximately equal to S. The activation volume u, association with the deformation process, is found from the following relationship: The theoretical treatment of thermally activated plastic flow due to schoeck18 shows that the activation volume when combined with the temperature dependence of the flow stress gives the activation energy for the process according to equations: seegerZ3 considers that the flow stress at lower temperatures ld is composed of two parts such that Tapplied = tinternal + Teffective , where Teffective 3 ff , is the stress necessary to overcome the local obstacles to deformation and Tinternal, ri, is the stress necessary to overcome the long-range elastic stress field of dislocations on other planes. ri is considered to be largely elastic in origin and can be estimated from the stress value at the temperature independent portion of the flow stress-temperature curve. EXPERIMENTAL The crystal bar zirconium used in this investigation was supplied by Wah Chang Corp. whose certified analysis gave the following impurity contents in parts per million by weight: oxygen, 150; nitrogen, 10; iron, 180. All others were less than 100 ppm. The oxygen and iron contents were confirmed by neutron activation and chemical analyses, respectively. Single crystals were grown in an electron beam furnace according to the method of Wilson and Pickle-simer'' and ills.'' The orientation of the crystals was such that the specimen axes were located in the lower third of the standard section of the basal plane stereographic projection for zirconium. This orienta-

Jan 1, 1969

By J. S. Kennedy, G. L. Simard, A. A. Lefrew, C. M. Judson, R. B. Booth

DITHIOPHOSPHATE collectors are commonly used in the flotation of sulphide minerals. Studies of the interaction of a typical dithiophosphate collector with galena surfaces have been previously reported from these laboratories.'* These fundamental studies were carried out by employing phosphorus labeled radioactive dithiophosphate. Radioactivity determinations then could be used to measure readily and accurately the small concentrations of dithiophosphate that are present under conditions of flotation processes. Measurements were made on ground mineral, determining the amount sorbed indirectly from the concentrations in solution; and studies were also made with single crystals, determining the amount sorbed directly by counting the crystal surface. The rates, isotherms and reversibility characteristics of dithiophosphate sorption, the competition between phosphate and dithiophosphate for the mineral surface, and the exchange of sorbed dithiophosphate with dissolved dithiophosphate were studied. These studies have now been extended by sorption measurements in flotations with a Fagergren machine. For this work, the selective flotation of galena and sphalerite from quartz was chosen, using ammonium di-(sec-butyl) dithiophosphate as the collector, sodium cyanide as depressant for sphalerite, and copper sulphate as an activator for sphalerite. While the selective flotation of galena and sphalerite using a single dithiophosphate collector is not typical of flotation practice (two different collectors are generally used), it was found that a reasonably good separation could be obtained by using zinc sulphate with the sodium cyanide in the galena flotation and by cleaning the sphalerite concentrate or by carrying out the sphalerite flotation in an alkaline medium. Data of practical importance on the distribution of collector between the concentrates, tailings, and solutions were obtained, particularly with regard to the effect of copper sulphate and sodium cyanide. In addition to the selective flotation of galena and sphalerite from quartz, single flotations of galena-quartz and sphalerite-quartz mixtures were carried out, along with blank flotations on quartz alone. The present paper describes the results of these experiments. As in previous papers, the term sorption is used to designate uptake of collector by the mineral, without implication as to the nature of the processes involved. Experimental Materials: The mineral system was a ground synthetic mixture of galena, sphalerite, and quartz. The galena was from Galena, Kans., and contained 75 pct lead (theoretical 85.6 pct Pb for PbS); the sphalerite, from Ottowa County, Okla., contained 63 pct zinc (theoretical 67.2 pct Zn for ZnS); and the quartz from Klondike, Mo., analyzed as 99.97 pct SiO,. Sulphur labeled radioactive di-(sec-butyl) dithiophosphate was prepared from SS supplied by the Oak Ridge National Laboratory on allocation from the U. S. Atomic Energy Commission. The synthesis consisted of precipitating barium sulphate, reducing the barium sulphate to barium sulphide, acidifying to form hydrogen sulphide, and oxidizing the hydrogen sulphide with iodine to elemental sulphur.

Jan 1, 1953

By J. S. Kennedy, A. A. Lefrew, C. M. Judson, R. B. Booth, G. L. Simard

DITHIOPHOSPHATE collectors are commonly used in the flotation of sulphide minerals. Studies of the interaction of a typical dithiophosphate collector with galena surfaces have been previously reported from these laboratories.'* These fundamental studies were carried out by employing phosphorus labeled radioactive dithiophosphate. Radioactivity determinations then could be used to measure readily and accurately the small concentrations of dithiophosphate that are present under conditions of flotation processes. Measurements were made on ground mineral, determining the amount sorbed indirectly from the concentrations in solution; and studies were also made with single crystals, determining the amount sorbed directly by counting the crystal surface. The rates, isotherms and reversibility characteristics of dithiophosphate sorption, the competition between phosphate and dithiophosphate for the mineral surface, and the exchange of sorbed dithiophosphate with dissolved dithiophosphate were studied. These studies have now been extended by sorption measurements in flotations with a Fagergren machine. For this work, the selective flotation of galena and sphalerite from quartz was chosen, using ammonium di-(sec-butyl) dithiophosphate as the collector, sodium cyanide as depressant for sphalerite, and copper sulphate as an activator for sphalerite. While the selective flotation of galena and sphalerite using a single dithiophosphate collector is not typical of flotation practice (two different collectors are generally used), it was found that a reasonably good separation could be obtained by using zinc sulphate with the sodium cyanide in the galena flotation and by cleaning the sphalerite concentrate or by carrying out the sphalerite flotation in an alkaline medium. Data of practical importance on the distribution of collector between the concentrates, tailings, and solutions were obtained, particularly with regard to the effect of copper sulphate and sodium cyanide. In addition to the selective flotation of galena and sphalerite from quartz, single flotations of galena-quartz and sphalerite-quartz mixtures were carried out, along with blank flotations on quartz alone. The present paper describes the results of these experiments. As in previous papers, the term sorption is used to designate uptake of collector by the mineral, without implication as to the nature of the processes involved. Experimental Materials: The mineral system was a ground synthetic mixture of galena, sphalerite, and quartz. The galena was from Galena, Kans., and contained 75 pct lead (theoretical 85.6 pct Pb for PbS); the sphalerite, from Ottowa County, Okla., contained 63 pct zinc (theoretical 67.2 pct Zn for ZnS); and the quartz from Klondike, Mo., analyzed as 99.97 pct SiO,. Sulphur labeled radioactive di-(sec-butyl) dithiophosphate was prepared from SS supplied by the Oak Ridge National Laboratory on allocation from the U. S. Atomic Energy Commission. The synthesis consisted of precipitating barium sulphate, reducing the barium sulphate to barium sulphide, acidifying to form hydrogen sulphide, and oxidizing the hydrogen sulphide with iodine to elemental sulphur.

Jan 1, 1953

Edward K. Landis, Philadelphia, Pa.: In studying Mr. Thackray's paper it seemed that a critical comparison of the results from different methods therein reported would he of interest. For this purpose Table I. was constructed by grouping all determinations made by the same method, and the probable errors were calculated. In this table all chemists titrating with permanganate (A1, E, F, G and 0 of Mr. Thackray's paper) are classed under "Emmerton;" those titrating with nitric acid (C, J, S and Y) under " Handy; " those re Probable error of result: a, ±0.0008996; b, ±0.000694; c, ±0.00107; d, ±0.00115; e, ±0.000674; f, ±0.000473; g, ±0.003675; h, ±20.0007959; i,0.000.5098; k, ±0.0008303. Probable error of single determination: a, ±0.001989; b, ±0.001547; c, ±0.00214; d, ±0.0023;e, ±0.00116;f, ±0.000818;g, ±0.0019;h, ±0.00224; i, 40.00143; k, ±0.00234. The formula for calculating the probable error is 0.6745, where N (N— 1)' S is the sum of the squares of the differences from the mean and N is the number of determinations.

Jan 1, 1897

By A. S. Venkatadri, H. B. Bell

The equilibrium sulfur distribution between molten iron and Ca0-Mg0-Al203 slags containing iron oxide was investigated at 1550°C. The results were used to derive the iron oxide activities at low iron oxide concentrations in the slag by combining the sulfide capacity data obtained from gas-slag work with the free energies of both the sulfur solution in iron and the iron oxide formation in slag. The derived ferrous oxide activities were compared with values based on Tem-kin's kin's and Flood's ionic models. One difficulty in using these models is that the nature of the aluminate ion in slag is uncertain. Nevertheless, such indirect methods, in particular, those described in the present paper, are of value because of the difficulty of measuring small amounts of oxygen in liquid iron in equilibrium with slag. It is shown that these methods confirm the consistency of thermodynamics data on liquid iron and slags. It is well established that decreasing the iron oxide activity in the slag increases the desulfurization of molten iron at constant slag basicity. This effect is most pronounced at the very low iron oxide activities, characteristic of blast furnace slags. Yet a precise quantitative determination of the significance of low iron oxide contents in slag in blast furnace desulfuri-zation is not possible for the following reasons: a) difficulty of separation of iron "shots" from the slag, and b) errors in chemical analysis of small amounts of iron oxide in slags. In view of these obstacles, one must resort to indirect methods of calculating iron oxide activities. EXPERIMENTAL TECHNIQUE The apparatus for providing the sulfur equilibrium data has been described previously1 and was similar to that used by ell' in connection with the study of slag-metal manganese equilibrium. The procedure consisted of: a) melting about 50 g of Armco iron in a magnesia crucible in a platinum furnace, b) adding a mixture of about 15 g of lime-alumina slag and varying amounts of Fe2O3 and CaS, and c) maintaining the temperature at 1550°C for more than an hour in an atmosphere of argon to enable the sulfur equilibrium to be attained. Several melts were made using lime-alumina slags with basic composition 55, 50, and 45 pct lime. During the experiment the temperature was controlled manually using a Pt/10 pet Rh-Pt thermocouple. After the experiment, the Power was shut off and the flow rate of argon was increased to freeze the melt as quickly as possible. The analysis of sulfur in the metal was carried out by the oxygen combustion method3 using uniform drillings from the top and bottom of the metal button. After crushing and grinding and removal of any iron particles with the aid of a hand magnet, the slag was analyzed for sulfur by the CO2 combustion method.4 The E.D.T.A. method was employed for the analysis of lime5,6 and magnesia,= the ceric sulfate method7 for the analysis of slag iron oxide, and the perchloric acid dehydration method5 for the analysis of silica. The remaining amount was taken to be Al2O3 precipitation with ammonium hydroxide in several preliminary melts had confirmed the propriety of using this simple procedure. RESULTS The activity of iron oxide in binary, ternary, and more complex slags has been the object of numerous investigations, and the two experimental methods for its determination are: 1) Equilibrating the metal with the slag in question and measuring the oxygen content of the metal. The ferrous oxide activity is then given by aFeO L%OJSat where [%0]sat is the oxygen content of the metal in equilibrium with pure iron oxide slag. This method was used by Chipman et al.8,9 2) Equilibrating the slag in iron crucibles with known partial pressures of H2/H2O or CO/CO2 mix-tures.10-12 This method is limited to temperatures between 1265" and 1500°C. The very low oxygen content of the melts in this investigation made it impossible to derive the ferrous oxide activity by the first of these methods. Therefore, the iron oxide activities were computed by means of: Sulfide capacity data from the gas-slag work" Temkin's concept14 Flood's approach15 a FeO from Sulfide Capacity. The method of calculating the aFeO involves the sulfide capacity of the slag (c,), the sulfur distribution coefficient (Ls), the free energy of dissolution of sulfur in iron, and the free energy of formation of iron oxide in the slag. Bell and Kalyanram13 have investigated the sulfur absorption characteristics of lime-alumina slags containing magnesia by the Carter-Macfarlane method16 (based on comparing the sulfide capacity of the slag in question with that of a standard slag of unit lime activity) and have derived lime activity values. The relation between sulfide capacity and their lime activity a'CaO is given by: Cs= 3—: Xa'CaO at 1500°C

Jan 1, 1970

By R. A. Pallanch

Sodium sulfite as a zinc retarding agent in the selective Hotation of complex lead-zinc sulfide ores was discovered by the writer in the summer of 1919 in the testing laboratory of the U. S. Smelting, Refining & Mining Co.'s gravity concentrator at Midvalc. Utah. It proved to be the first reagent to give consistently good results in the laboratory on the cornpanj's Bingham ore. In December, 1919, C. A Lemke, concentrator superintendent, recommended that a flotation unit be added to the existing gravity mill to handle the mill slimes, using sodium sulfite as the zinc depressant Owing to the poor lead and zinc markets and the unfavorable royalty schedules offered by the Minerals Separation Co., the project fell through at this time. In 1921, a number of laboratory tests were made at Midvale. on other ores, among them ore from the Sunnyside mine at Eureka, Chlo. Both sodium and calcium sulfites were used with succcss on this ore. Early in 1923, further tests were made at Eureka, shortly after the Sunnyside company had resumed operations after a two-year shutdown. AS a consequence sodium sulfite was given a trial in the mill. The results showcd sufficient improvement over previous work as to warrant continuous use of this reagent in the lead circuit Exeept for a week or so in 1926 and for several weeks in April, 1927, when sodium cyanide and zinc sulfate were given trial runs in this mill. sodium sulfite has been used ever sinee.. Sodium sulfite was chosen rather than the calcim sulfite brcauscl of its gre1ater sollubility, making it possitdr. to introduee the reagent as a solutiun. This Solution is introdueed into the Marry ball mills along with the original feed of ore,. The consumption of sodium sulfite in the Sunnyside mill varies from 1/4 to 12 lb per ton of ore, the smaller amount probably being nearer the average. In February, 1924, laboratory work at Midvale demonstratcd conclusivcly that good results could be obtaincd on the company's Bingham ore and on most of the custom ores tested by using sodiuin sulfite as the zinc depressant, xanthate as the lead enhancer in the lcad circuit, followed by copper sulfate and additional xanthate to float the zinc Sodium sulfide was used to float the iron pyrite after the lead and

Jan 1, 1928