Search Documents

By John M. Tinsley, Calvin D. Saunders, H. K. van Poollen

In the past few years much con-sideration has been given to the evaluation of the effect of hydraulic fracturing on the productivity of wells. Generally, these studies included the evaluation of fracturing materials, fracture extension and formation damage due to the use of various fracturing fluids. Only little consideration has been given to the characteristics, and in particular the flow capacity, of the fracture itself and its effect on well productivity. This paper presents the results of laboratory investigations pointed toward fie evaluation of the efficiency of various fracrures with special emphasis on the flow capacity of these fractures. Data presented in this paper are the results of both an electrical model study and physical testing. Under consideration are (I) effect of overflush, (2) premature production of well after treatment, (3) "tailing-in" with coarse sand near the end of the treatment, (4) effect of propping agent size and concentration, (5) reduction in effective frac-ture permeability caused by formation caused by formation fines, silt and clays, and (6) effect of various fluids on formation strength and competency. The results of this investigation indicate that the flow capacity of a fracture is affected by any or all of the various parameters mentioned above. The authors believe that a better understanding arid utilization of these factors should result in more efficient formation fracturing. INTRODUCTION Hydraulic fracturing has become almost a standard practice of many companies for stimulating production from old and new wells. Although most companies utilize this service, techniques of application vary widely between companies and areas. Probably too often when a well in an area responds favorably to a particular technique all future wells in the same area are treated in a similar manner. Possibly a modification of the technique would result in a further production increase. Variables, of which many are extremely difficult to evaluate from field results, hamper the selection of procedure changes. Attempts are being made by a number of organizations to analyze statistically treating techniques from production data. This is a very worthy and necessary approach but very possibly laboratory investigations may aid in evaluating some of the variables which tend to affect the results of a fracturing treatment. Some of the factors cannot be studied from practical field experience and only laboratory tests can show the possibilities which might exist. One of the factors which appears to be of major concern today is the flow capacity of the created fracture and how it can be changed. Papers on this general subject have been primarily concerned with the size of propping agent and the extent of fracture. Papers have also been written on the possible permeability damage to formations by fracturing fluids. In addition, it might be possible that another type of flow restriction is prevalent. This would be a restriction of flow through a sand-packed frac- ture caused by foreign materials integrating within the propping agent. This paper presents preliminary data obtained in an attempt to evaluate the effect of some factors affecting flow through sand-packed fractures. No attempt is being made to offer a fracturing technique adaptable to all areas and conditions, but to furnish data tending to show the possible effects which might be caused by variations in procedures and materials. PROPPING AGENT PERMEABLLITIES A hydraulically induced fracture containing sand as a propping agent may theoretically be classified as a packed-sand system. The flow of fluids through such packed systems has been the subject of much research. Although there have been numerous methods proposed for the evaluation of such systems, most writers agree on the general properties affecting their flow capacity or permeability. These properties include porosity, particle size, sphericity and the roughness of the particle. In some methods of evaluation . the particle size and sphericity terms are combined to produce an equation which is a function of the surface area of the particles. In this study the permeability of various fracturing sands was both measured and calculated. The apparatus for the permeability measurements consisted of a 52-in. Lucite tube with a 2.5-in. ID. A screen and drain plug were fitted in the bottom of this tube to retain and hold the sand in place while allowing fluid flow. Two pressure taps consisting of thin, highly perforated

Endurance Properties of Non-ferrous Metals Discussion of the paper of D. J. McADAM, JR., presented at the Syracuse Meeting of the Institute of Metals Division and issued, as Paper No. 1506-E, with Mining AND METALLURGY, October, 1925. H. F. MOORE,* Urbana, Ill. (written discussion).-This paper says that the results of tests of some non-ferrous metals made at the University of Illinois and in the testing laboratories at McCook Field are abnormal when they do not agree with results obtained by the author. The writer can see no inherent reason why results of the type uniformly reported in this paper are any more normal. The knee of the stress-cycle, or S-N, diagram comes at different lengths of life for different metals. For steel, the knee occurs after from 1,000,000 to about 4,000,000 cycles, and for some non-ferrous metals not before 20,000,000 of 30,000,000 cycles. The writer can see nothing inherently abnormal in finding certain nonferrous metals for which the knee of the stress-cycle curve occurs at 1,000,000,000 cycles or higher. The writer has had experience with both the cantilever and the rotating-beam testing machine, and thinks that the chance of whipping action in the cantilever machine is a more serious handicap than the action the author has pictured. Furthermore, the writer questions whether the author has shown the existence of a clearly marked and definite endurance limit for all the non-ferrous metals he has tested including the following: Nickel (CT and A-16, Fig. 1), monel (CS-5.5 and BK, Fig. 2), bronze (F and CK, Fig. 4), aluminum bronze ( BJb-1, Fig. 6).

Jan 12, 1925

By A. M. Gaudin

TEN years ago Taggart, Taylor and Ince1 described a workable, convenient apparatus for the measurement of contact angles be-tween cleaved, ground or polished particles and captive bubbles. Wark and Cox2 and Wark and Sutherland3 have done an im-mense amount of experimental work with this apparatus. Their work has had as principal object the determination of "con-tact curves." Contact curves are Cartesian charts in which pH (or some other variable) is plot-ted against quantity of modifying agent. The rectangular area is broken into two or more curvilinear areas separated by the contact curve. The curve indicates that a sharp demarcation exists between condi-tions that bring about sticking of particles to bubbles and conditions that do not pro-duce sticking, The type curve appears in the TRANSACTIONS as Fig. 1, page 248, volume 112. Wark and Cox offer data to show that the contact angle has a value determined by and characteristic of the agent used. Wark and Cox also make the statement that they believe this value is independent of concen-tration (ref. 2a, p. 209), They say: It is suspected that, given sufficient time and provided that there are no disturbing factors. the full ethyl xanthate angle (corresponding to a complete xanthate film) would be obtained in every case where contact occurs.

Jan 1, 1940

By J. C. Bartlett

The following discussion was suggested by an experiment of Mr. Krom, the Manufacturer of air-jigs, to illustrate the superiority of air over water as a medium of concentration. The paper is written in the interest of no system of concentration, but simply to test the experiment, and, perchance, to add something to the general fund of information on the subject. To speak of testing an experiment by a theoretical discussion, may seem a misuse of terms, but the theories concerning falling bodies and the resistance of fluids are pretty well crystallized into laws, which may properly be used to show where experiments which seem to refute them were improperly performed, and that instead of refuting they only corroborate. It is well known that a sphere of galena & inch in diameter, and a sphere of quartz 1/2 inch in diameter, are equal falling in water ; that is, these two spheres, being placed together in a column of water at rest or in motion, will practically remain together, filling or rising together, or remaining in suspension. Mr. Krom, to show that these

Jan 1, 1879

By H. M. Chance M

The following tables have been compiled from the annual reports of the Inspectors of Mines, to determine the percentages of fatal and non-fatal casualties from roof-falls and explosions of fire-damp. As we cannot assume that every accident has teen recorded by the inspectors ; as many casualties terminating fatally after the lapse of a considerable period, are inevitably recorded as " non-fatal;" and as clerical errors may have crept into the compilation,* the figures of these tables cannot be considered absolutely correct, but the summary is sufficiently reliable to show the features I wish to differentiate. Under the heading " Miscellaneous" are included all accidents not directly attributable to explosions of fire-damp, roof-falls or fails of coal. Prominent among the numerous causes included under this head are premature or delayed explosion of blasts, accidental explosion of powder or cartridges, accidents from mine cam, falls in shafts, machine accidents, sliding of loose coal in pitching breasts, suffoca tion by choke-damp, etc., comprising in all 48 per cent. of the total number of casualties.

Jan 1, 1882

By J. H. Brophy, J. Wulff, H. W. Hayden

The mickel-activated sintering of tungsten occurs in two stages of densification. A kinetic analysis of the second stage has been based on an appropriate model of the process. As in the first stage, the rate-controlling mechanism for the second stage is also the solution of tungsten in the nickel carrier phase. The transition from the relatively rapid first-stage results from the spherozdization of pores and the initiation of grain growth. Finer grain size due to higher-nickel content leads to more rapid and higher degrees of densification 1 HE sintering of tungsten is accelerated by small additions of nickel, cobalt, and iron.' Experimental evidence in detail has shown that nickel-coated, hydrogen-reduced tungsten powder may be sintered to more than 90 pet of theoretical density at l100o C.2, 3 Simultaneously, a kinetic analysis of the process showed that it took place in two distinct stages. In the first stage, nickel evidently served as a carrier phase through which tungsten atoms could move. This stage was kinetically similar to the "solution-precipitation" step postulated when the carrier phase is a liquid,4 although in the Ni-W case, there is no evidence of the existence of a liquid phase either in equilibrium phase relationships or in microstruc-tures at the temperatures under consideration. It has been shown that this stage corresponds to a process which is rate controlled by a phase boundary reaction.3 More recent evidence has been presented5 showing that after the initial rapid stage of sintering, densification continues in the final stage but at a slower rate, although no mechanism for this stage of densification was defined. An analysis of later stages of densification in solid state sintering has been presented,6 but it is not directly applicable in the present case of activated or carrier phase sintering. It is the purpose of this investigation to study the final stage of nickel activated tungsten sintering in greater detail The effect of varying nickel content has been examined, and a possible kinetic mechanism defined. EXPERIMENTAL PROCEDURE AND RESULTS Commercial hydrogen-reduced tungsten powder from Wah-Chmg Corp., having a nominal particle size of1 µ and a B.E.T. specific surface area of 5500 sq. cm per g was mixed with aqueous solutions of hydrated nickel nitrate in proportions sufficient to produce nominal compositions of 0.25, 1, 3, and 5 wt pet Ni. This solution was then evaporated to dry-ness at approximately 150" C for 15 hr. Following evaporation, the resulting powder cake was broken with a mortar and pestle and reduced in hydrogen at 800oC for 1 hr. Following reduction, the powder

Jan 1, 1962

By A. Totani, S. Nakajima, H. Okazaki

The phase diagram for the SnTe-SnSe system has been studied in the temperature range from 300° to 900°C by differential thermal and quenching techniques. The X-ray measurements were made on quenched specimens. High-temperature diffraction was also made to study the phase transition in SnSe. The system is proved to be of a eutectic type in which no intermetallic compound exists. The eutectic point is at the composition SnTeo.55 Seo.45. the eutectic temperature being 755°C. Solid solubility limits are SnTeo.6Seo.r and SnT eo. 3s Seo.6s at the eutectic temperature, and change almost linearly to SnTeo.aaSeo.lz and SnTeo.18 Seo.az as temperature decreases to 300°C. It was shown that the SnSe phase has a phase transition of the second order at about 540°C and that the transition temperature decreases with increase of the SnTe content. THERMOELECTRIC properties of tin telluride (SnTe) and tin selenide (SnSe) have been studied extensively in recent years. The variation of physical properties with composition could be of interest if these compounds form an appreciable crystalline solution. The purpose of present investigation is to confirm the formation of crystalline solution or intermetallic compound, if any, and to establish the phase diagram for this system. The crystal structure of SnTe is NaCl type with a cubic unit cell1 (a = 6.313A). The crystal of SnSe having an orthorh2mbic unit cellz (a = 11.496, b = 4.1510, and c = 4.4437A) is isomorphous with tin sulfide (SnS) which has a distorted sodium chloride structure. It has been known that SnSe has a phase at at 540°C; the transition has been assumed to be of the second order. As far as we know, only two studies on the SnTe-SnSe pseudobinary system have been reported. The conclusion obtained in these papers is that, in the composition regions near SnTe and SnSe, the system forms a crystalline solution of the SnTe structure and the SnSe structure, respectively, and that, in the intermediate region, both phases coexist. However, neither the variation of the solid solubility vs the temperature nor the liquidus and solidus were investigated. Hence present writers have attempted to determine the phase diagram of the system by differential thermal analysis (D.T.A.) and X-ray diffraction. EXPERIMENTAL Sample Preparation. Starting materials, SnTe and SnSe, were prepared by the direct fusion of commercially available high-purity (99.999 pct) elements. Stoichiometric amounts of each couple Sn-Te or Sn-Se were weighed into a clear fused silica ampule. After evacuation to a pressure below 10-3 mm Hg, the am- pule was sealed, and annealed at 900°C for 5 hr. The melt was quenched in water. X-ray analysis confirmed the formation of a single phase of SnTe or SnSe. The other samples, SnTel-,Sex were synthesized from these SnTe and SnSe by mixing them in the required ratio, followed by annealing at 900°C and quenching. These samples were used directly for D.T.A. For X-ray measurements, samples were annealed at 700°, 600°, or 500°C for 100 hr or at 300°C for 150 hr, and then quenched in water. It was found that the lattice constants of the SnTe phase annealed for 150 hr at temperatures above 500°C did not differ from those annealed for 100 hr at the same temperatures. However the X-ray phase analysis showed that at 300°C the annealing for 150 hr was necessary to attain a true equilibrium state. D.T.A. The solid-liquid equilibrium temperature was determined from D.T.A. measurements. The sample was sealed in an evacuated silica tube and molybdenum powders sealed in an another tube were used as a reference material. The sample and the reference tube were placed in a nickel block and were heated from room temperature to 900°C at a rate of 3°C per min and then cooled down at the same rate to 600°C. Thermocouples for these measurements were Pt-Pt. Rh (10 pct) and the error of temperature measurements was within + l0C. D.T.A. curves were obtained on a two-pen recorder and an automatic controller (PID type) was used for the program of heating and cooling. When temperature reaches the solidus from the low-temperature side, there appears an endothermic peak. The solidus temperature was determined by extrapolation of the straight portion of the starting flank of this peak to the base line. In a similar way, the liquidus temperature was determined from an exothermic peak on D.T.A. cooling curve. In the case of supercooling, if any, its degree can be estimated from the magnitude of the abrupt temperature rise. X-Ray . X-ray powder patterns were taken by a diffractometer using CuK, radiation. Since the SnSe crystal is cleaved easily, the powders become flaky when SnSe-rich samples are ground in an agate

Jan 1, 1969

By V 7. 0 / 300 dpi

LAST fall, having a number of ore samples from mine-development work carried on in spite of the "Revolution," I was forced to do my own assaying again, after a lapse of many years. This gave me an opportunity to build a furnace for crucible assaying, using wood for fuel, along lines which had been developing in my mind since the time 20 years ago, when as general factotum at a little mining camp in western Chihuahua, Mexico, I had converted a crucible charcoal furnace into one using the reverberatory principle. Wood-burning furnaces have been described in technical literature, but I believe the present application will prove helpful to those of the profession who are working in out-of-the-way places. The furnace is shown in detail in Figs. 1, 2 and 3. Remembering the trouble caused by stoking my first charcoal furnace too heavily, I fired this one with but a few sticks of wood at a time. By this method I could run out a charge of 12 crucibles in 30 to 35 min., using 50 sticks of ordinary stove wood. Later I fill up the firebox, holding about 40 sticks, get everything ready, put the crucibles into the melting chamber and "fire up." Just as soon as the fire is well started the draft door is closed and the furnace allowed to heat up slowly for 5 min. Then the draft is opened (the door to the ash-pit) and the fire allowed to roar, which it does. In 20 min. from the time the fire is lighted the fire door is opened, the fire stirred along the grates, and 5 or 6 more sticks of wood thrown in. In 25 min. from the start, the draft is closed again, the cover of the melting chamber pushed back and the charges poured. The melts will be found to be perfect, and the crucibles to pour absolutely clean, if everything has gone right, as will usually be the case. A new charge may be put in, and fired with S to 10 sticks of wood at a tine, and be ready to pour within 20 min.; but it is just as well to leave the crucibles in the melting chamber a full 2.5 min. By using 10 sticks of wood to start the fire and adding 5 sticks as often as needed, which will be as soon as the last sticks fed in are in perfect combustion, the smelting can be completed in from 30 to 35 min., using from 35 to 40 sticks of wood. I consider this to be the best method of stoking.

Jan 10, 1914

By G. P. Airey, R. F. Mehl, T. A. Hughes

The coarsening of cementite particles in a ferrite matrix has been studied in a series of steels with 0.15 pct C only and 0.15 pct C plus 1 pct Ni, Mn, and Cr, respectively. Two initial states were employed: quenched nartensite, and quenched and cold-rolled martensite. A series of tempering temperatures between 500' and 700" and tempering times of up to 190 hr were used. The structures were studied by replica and transmission electron microscopy. Particle size distribution curves were determined. From the average size value coarsening curves were obtained. These were plotted in accordance with the Wagner analysis assuming diffusion control. A discussion of the significance of the results is given. L HE reactions occuring upon the tempering of martensite have long engaged the attention of metallurgists. The latter stages, when cementite particles coarsen in a ferrite matrix, have been studied both qualitatively and quantitatively. Studies of such coarsening processes have recently been spurred by the publication of the Lifshitz-Wagner theory1, and the extension of this to the a Fe-Fe3C system by Oriani3 and by Li, Blakely, and einold. Following Wagner the coarsening process is often designated as "Ostwald Ripening". The only quantitative data on the rate of coarsening, except for the work of Hyam and uttin,' in the a Fe-Fe3C system are those of Bannyh, Modin, and odin' for a commercial eutectoid steel and those of Heckel and ereorio" using a pure eutectoid steel. The data of Bannyh, Modin, and Modin have been employed by 0riani3 to derive the a Fe-FeE interface energy. The reaction is one of the most important ones in steel and is worthy of detailed study. This is the purpose of the present study. Laboratory heats were prepared; these were steels with approximately 0.15 pct C, selected so that the num ber of carbide particles would be relatively small and thus so that the overlapping diffusion fluxes would be minimized, presumably a desirable circumstance.'-3 In addition to Fe-C alloys, comparable heats containing 1 pct of Ni, Mn, and Cr, respectively, were included with a view of appraising the effect of alloying elements. This report includes an account of the micro-structures observed, primarily with the electron microscope, and of kinetic data and their interpretation. MATERIALS AND TREATMENT The alloys were prepared from electrolytic iron ("Plastiron") and high-purity graphite; these were melted in a zirconia crucible using a vacuum furnace. The alloy steels were made by adding electrolytic nickel, electrolytic manganese, and "vacuum grade" chromium, respectively, under a partial pressure of argon. Each melt was poured into a mold within the vacuum furnace and cooled in the mold. The ingots were 2 in. in diam. and 8 to 10 in. long. The analysis of the alloys is given in Table I. These ingots were hot-rolled to strip 0.1 in. thick, then cold-rolled to 0.05 in. and each alloy split into two batches. One batch was austenitized at 1200 for 1 min, quenched in cold brine, then cold-rolled to 0.02 in.; samples given this treatment are hereinafter designated as "worked". The other batch was cold-rolled to 0.025 in., austenitized at 1200" for 1 min, and quenched in cold brine; such samples are hereinafter designated as "quenched". These two batches were then tempered, as below. The purpose of the treatment given the first batch was to provide an initial structure of cold-worked martensite, with the expectation that the additional defect structure created by cold work would encourage a higher rate of nucleation of cementite on tempering and hence a more uniform distribution of cementite particles. Individual specimens were sealed in evacuated quartz or Pyrex tubes, then tempered in a muffle furnace. The temperature control was better than 3'C at 700. Tempering treatments wer: performed at 400°, 500°, 550°, 600°, 65o°, and 700C for time periods between 15 min and 190 hr. PREPARATION OF SPECIMENS Specimens for optical and replicalelectron microscopy were mounted, polished conventionally, and etched with 2 pct nital. For electron microscopy, single-stage "formvar" replicas were made, dry-stripped and rotary-shadowed with chromium at an angle of 30 deg. Carbide extraction replicas were prepared from electropolished specimens usirig the method described by Smith and uttin.' Thin foils for electron transmission microscopy were prepared by chemical thinning in an H202-HF bath prior to electropolishing in a chromium trioxide-acetic acid solution. The most

Jan 1, 1969

No phase of the steel industry is more typical of its remark- able progress than is the evolution and development of the modern American blast furnace. The founding of the Institute in 1871 also marked the beginning of a new era in the pig-iron industry. The rapidly expanding westward development of the country, with its seemingly unlimited markets, gave rise to unprecedented demands for blast-furnace products. The manner in which the iron industry responded provides a fascinating chapter in the history of industrial development. Prior to this period, the iron industry of the United States, largely concentrated in the East, was based upon the consumption of local iron ores and local fuels, the latter predominately charcoal and anthracite. Small, isolated furnaces were located near scattered ore and fuel sources, and the completely integrated ironworks and steelworks were yet to be developed. In about 1860 exploitation of the newly discovered rich ore deposits in Michigan and the successful adaptation of blast furnaces to coke produced from coal of the great Pittsburgh seam in western Pennsylvania proved to be major factors in firmly establishing the general westward shift of the industry. But these were largely economic in character, and it was not until about 1870 that the aggressive, individualistic nature of the ironmaster asserted itself in no uncertain manner. No longer limited by relatively inadequate equipment and inferior raw materials, and spurred as well as encouraged by those who supplied capital for these new enterprises, furnacemen began to establish unheard of records in iron production. It is not surprising that Pittsburgh was the center of this new activity. Its tenor is best indicated by the following account :l

Jan 1, 1948

HENRY FAY, Cambridge, Mass. (written discussion *).-Mr. Rawdon has made a distinct contribution to our knowledge of wrought iron, and .perhaps of steel. It will undoubtedly lead to more careful scrutiny of high-phosphorus steels, with perhaps important results. In view of his results, it would seem to be unprofitable to push further any propaganda on the use of higher-phosphorus low-carbon steels until further information is available. As is well known, and as Mr. Rawdon clearly shows, the process of solidification is a selective one, and there is abundant opportunity for those portions of the melt last to solidify to become rich in phosphorus, and the diffusion of this phosphorus-rich area is slow. Hot work does not help the situation appreciably and only serves to concentrate the low-melting material. It is undoubtedly true, as some writers have recently claimed, that the specifications for steels as they. now exist eliminate some perfectly good material. Higher phosphorus in steel may be perfectly safe provided all of the phosphide is completely and uniformly, diffused in the solid solution. If, on the contrary, it is not evenly diffused, and there is a reasonable chance for it not to be, it makes the steel unsafe. Until our knowledge: of the rate of diffusion of phosphorus in steel, and the effect of other elements upon the rate, is more complete, it seems to me unwise, in view of Mr. Rawdon's experiments, to listen to the recommendations for the use of higher-phosphorus steels.

Jan 1, 1918

Discussion of the paper of GEORGE K. BURGESS and SIR ROBERT A. HADFIELD, presented at the New York meeting, February, 1915, and printed in Bulletin No. 98, February, 1915, pp. 455 to 468. ALBERT SAUVEUR, Cambridge, Mass.-There is a definiteness and finality in the investigations that have been conducted by the Bureau of Standards and in the method of presenting the results that is most satisfactory and refreshing.. A year ago Dr. Burgess and his co-workers investigated the question of critical points in carbonless iron, and they settled the question once for all. No one can now claim that the thermal point A2 in carbonless iron does not exist. At the past meeting of this Institute in Pittsburgh, Dr. Burgess showed the worthlessness of the shrinkage clause. To my mind after his demonstration no one can again claim that the shrinkage clause renders any service. He also showed us that it was a practicable proposition to use pyrometers in steel work in order to ascertain the finishing temperatures of rails. No one can again come before this body and make the claim that it is not a practical proposition. And now Dr. Burgess shows us that steel ingots can be made in a commercial way, practically free from pipe, from segregation, aid from blow holes. It places again before us in a very clear manner the question of piped ingots and of segregation, a question which has been debated for 20 years or more. I know very well the attitude of the standpatters in the matter. They claim that most of the pipe is removed in the discard, and that if a little is left it is so thoroughly welded that it does no harm. I for one am not convinced of the soundness of the argument. I do not believe there is any one present who would claim that, given an ingot free from pipe, free from segregation, and free from blow holes, better rails will not be made out of that ingot than out of the ordinary piped or segregated metal which is used by almost all of our steel mills. In my opinion, if we give our sanction to the casting of steel in the shape of piped or segregated steel ingots, we are guilty. If we give our sanction to the rolling of rails from such metal, we are guilty. It is our duty as experts, as steel makers, and as steel consumers to make and to use the best steel obtainable on a commercial basis, for the manufacture of rails. Now, we have been shown that sound ingots can be produced from which superior rails can be made. If we do not insist upon these sound ingots, then we fail in our duty. I think that the art of casting steel ingots has advanced to such a point that the casting of steel ingots piped and segregated ought no longer to be tolerated.

Jan 5, 1915

By Tasuku Fuwa, John Chipman, David H. Kirkwood

Fe-C-Si alloys in silica crucibles were held at 1600°C in a controlled atmosphere of CO and Co2 and the approach to equilibrium was obsertsed. Results were not of sufficient precision to establish the activity and interaction coefficients. Observations 012 the equilibrium provided an average value for the standard free-energy change which differed by + 1.1 kcal from the earlier accepted value. The C-SL relation at other temperatures is calculated and shown graphically. IN the refining of steel in an acid-lined furnace, it is well known that, unlike in basic refining, a very significant amount of silicon may remain dissolved in the metal even when the carbon content approaches a final endpoint. Further, it is known that the residual silicon increases with increasing temperature. The quantitative relation between silicon and carbon can be calculated for equilibrium conditions from data already available on the Fe-C-O and the Fe-Si-O systems. Such equilibrium calculations could show us approximately the limitations within which the reaction would be expected to operate in practice. In the oxidation of a bath containing both carbon and silicon it is well known that at low temperatures silicon is preferentially oxidized first. It can be shown by calculation that at high temperatures carbon will be oxidized preferentially. It is the purpose of this paper to record direct observations on the Si-C relation by means of experiments carried out in an atmosphere of carbon monoxide for Fe-C-Si alloys contained in silica crucibles. When such a system is brought into equilibrium, at a fixed temperature, the composition of the liquid metal is governed by the following equations: Both K1 and K2 are known with a fair degree of accuracy, and may be calculated from the tabulated In general the percentage of CO2 is extremely small compared to that of CO and in the experiments to be described the partial pressure of the latter was generally only slightly below 1 atm. EXPERIMENTAL METHOD The induction furnace employed was the same as that described by Rist and chipman' and by Fuwa and chipman.2 It was modified slightly in view of the change from alumina to silica crucibles. The small silica crucible was surrounded by a thin susceptor of molybdenum sheet which in turn rested inside a zirconia crucible. Since the zirconia was subject to breakage, it was supported inside an alumina crucible. The charge consisted of 30 to 35 g of electrolytic iron along with the required amounts of refined silicon and graphite to produce a melt of required composition. Purified carbon monoxide and carbon dioxide were passed into the furnace through carefully calibrated flow meters. Two separate and independent series of experiments were carried out. In Series I (D.H.K.) the melt was held in the furnace at 1600°C for periods of time up to 6 hr. Samples were taken at intervals in silica tubes and were analyzed for carbon and silicon. The results of the last one or two samples taken from each experiment and the direction in which equilibrium appeared to be approached are shown in Table I. In Series II (T.F.) the silica crucibles were of less satisfactory strength and the melts were held at 1600° C for periods of only 2 to 4 hr. In heats number 29 to 45 inclusive, the metal was cooled in the furnace and the ingot itself served as a sample for analysis. In heat 46 and all subsequent heats, samples were withdrawn in silica tubes at the termination of the heat, and these samples were analyzed. The results of all of these experiments in which equilibrium appeared to be approached are listed in Table II.

Jan 1, 1965

By W. E. Forsythe

WHEN measuring ordinary temperatures, the instrument is generally placed in very close contact with the body the temperature of which is desired. However, if the temperature of the source is continually raised, a point is soon reached where no known substance will, in general, remain constant in any of its temperature-measuring properties if placed in direct contact with the source. Also, it is occasionally necessary to measure the temperature of a source that 'is so small or so situated that it would be very hard to bring the measuring instrument into direct contact with the source. When these conditions exist, advantage is taken of the well-known fact that all bodies, when at sufficiently high temperatures, send out radiation in amounts readily measurable. This radiation has been found to be related to the temperature. The temperatures of very hot bodies have probably always been judged by the color, or the brightness, of the light given off. With practice, one can estimate probably within 50° to 100° C. of the correct value. However, if judgment is left to the eye alone, very much larger errors are sometimes made, due to

Jan 9, 1919

By W. C. Leslie

W. C. Leslie (Edgar C. Bain Laboratory for Funda mental Research)—This investigation, with its com bination of high-purity metal, calorimetry, and metallography, will serve as a model for annealing studies for a long time to come. The evidence for a competition between recovery and recrystalliza-tion is particularly convincing. The demonstration of edge-nucleated recrystallization was so clear that it may obscure the necessity for other types of "nucleation" sites; otherwise, single crystals of aluminum could not be recrystallized after cold work. At least three types of sites have been found to operate in iron: 1) high-angle boundaries, probably in the same manner as in aluminum, 2) matrix sites, 3) inclusions or second-phase particles. In each instance, the cells developed during cold work and perfected during recovery are the "nucle for recrystallization. Observations by ourselves and others of the dislocation structure of cold-worked metals and of the structural changes that occur during annealing have led us to doubt the validity of the basic assumption of the Lucke-Detert theory, and of the modification developed by Gordon and Vandermeer, that during recrystallization of a metal containing foreign elements in solid solution a high-angle boundary is ad vancing into a cold-worked matrix having a random distribution of solute atoms. We contend that an es sential part of the cold-working and annealing of solid solution alloys is the trapping of solute atoms by the low-energy "wells" afforded by individual dislocations and by dislocation arrays. If cells are formed during cold work, the cell walls are stabilized by this concentration of solute atoms. Thus, solutes inhibit recrystallization not only by decreas-ing the rate of high-angle boundary migration, but also by preventing the formation of high-angle boundaries by subgrain growth or coalescence, i.e., solutes can inhibit both "nucleation" and growth. In addition to stabilizing the dislocation Structure, the solute-dislocation interactions may produce clusters of solute atoms which are not as readily assimilated into the recrystallized grains as are individual solute atoms. There is an additional complication. The dislocation structure formed upon cold working a dilute solid solution may not be the same as that formed during cold working of the pure solvent metal. The solute can either enhance or minimize the formation of cells during cold working. Both effects have been observed in binary alloys of iron. The annealing process is inextricably connected with the mechanisms of strain hardening and solid solution hardening. Although the correlation between experimental boundary migration rates and the predictions made from the theoretical equations are impressive, it should be mentioned that in at least four other instances (Pb-Ag and pb-Au,15, Fe-Mn,16, Fe-Mo)17 the agreement was rather poor. In brief, while it is probable that the migration of high-angle boundaries is held back by solutes in the manner described, this is only a partial explanation of the total effect of solutes upon recrystallization of cold-worked alloys. Paul Gordon and R. A. Vandermeer (author's reply)— The authors first wish to thank Dr. Leslie for his compliments of this work. It is perhaps worth pointing out that some of Dr. Leslie's remarks are directed toward subject matter covered in two earlier papers in our work.18,19 We agree with Dr. Leslie's main contention that the exact nature of the metal structure in the vicinity of a boundary should have an effect on the boundary migration. The theory of Lucke and Detert does not take such detail into account, nor does it account for orientation effects on the migration rates. We assume that since our data checks the theory so well, the effects of detailed structure are statistically averaged out by the polycrystalline techniques used just as are the effects of orientation factors.

Jan 1, 1963

By Samuel H. Dolbear

NOT WITHSTANDING the extremely low ebb of business activity, the nonmetallic industries have fared somewhat better than some other branches of mining. The average price level in nonmetallics, although far from satisfactory, has resisted any cataclysmic fall such as has been suffered by copper and other metals. Stocks, also, though too abundant, represent no corresponding overhang of the market, which should result, in some branches, in a more rapid recovery. Research work has continued in some industries with interesting developments.

Jan 1, 1933

By G. J. Benard

In the 1970’s, several plants have been built and others are in the design stage which use solvent extraction for recovery of copper from acid leach solutions. Other plants are presently being built for the recovery of nickel and cobalt from laterite ores by prereduction and ammonia leaching. A review will be given on the materials of construction for these leaching and solvent extraction processes. Many plants have factors in common which permit selection with a greater degree of accuracy. Based on pilot plant corrosion data, effective use of materials of construction includes proper selection of materials, substitution of lower cost plastics for alloys, and selection of materials resistant against chloride stress corrosion cracking.

Jan 1, 1974

One of the best known of the early mining districts of Nevada was that at Eureka, where gold was first produced in 1864. While the most productive period for the district was during the early 1900s, production was maintained until World War II. During this time it is said that the Eureka district produced as much as $200 million from over 3,200 km (2,000 miles) of tunnels and workings. The Windfall Mine was discovered in 1902; and a 100 ton cyanide plant was operated there during the periods 1907 to 1912 and 1932 to 1940. Since 1974, however, Windfall Venture has been operating a unique heap leaching facility on the site of the old Windfall Mine. Gold at the Windfall occurs primarily in the Cambrian Hamburg dolomite which has been "sanded" and in which the original cementing material has been destroyed. The gold is micron sized and is accompanied by anomalous amounts of arsenic and mercury; however, the ore is low in base metals which distinguishes it from the typical Eureka district ores. Mining the ore causes it to break down into very fine sizes, approximately 50% minus 150 microns (100 mesh). Conventional heap leaching by spraying proved to be impossible; and extensive test work on alternate methods, aided by the United States Bureau of Mines, was conducted using 9 m (30 ft) high columns and then large tonnage heaps. The leaching procedure adopted was to build 10.6 m (35 ft) high heaps on a 50 mm (2 in.) asphalt pad covered with a layer of gravel for drainage assisted by perforated pipe drains and gravel-packed sumps. A berm is constructed around the top of each pad and cyanide solution is allowed to “pond” on top of the heap. The resulting percolation is at the rate of 24 liters per sq m per hr (0.6 gal per sq ft per hr), a figure about 2.4 times the average used in other heap leaching operations. The dolomite furnishes its own protective alkalinity and no lime or caustic is used in the solution which contains 0.4 kg per mt (0.8 lb per st) of NaCN. Pregnant solution from the heaps averages about 0.7 g Au per mt (0.02 oz per st) with a cyanide content of about 0. 2 kg per mt (0.4 lb per st) and a pH of plus 9. Addition of NaCN brings the pH of the leach solution up to 11 to 12. Carbon adsorption of the gold was originally done in six enclosed columns mounted in a trailer but five conventional columns have been substituted as the size of the operations has increased. Carbon stripping is with hot caustic, cyanide and 10% ethanol solution. The

Jan 1, 1981

On Apr. 21, the Victory Liberty Loan was offered to the public. This Loan is made necessary by the expenditures incident to closing of the war. As in preceding Liberty Loans, an intensive campaign is being conducted, and this Committee is to obtain and record subscriptions from the Industry of which you are a part. I am sure you feel as I do in wishing the Mining Committee to make as good a showing as possible. By placing or recording your subscription through us will help your Committee to make its proper showing, and, as heretofore, your transaction can he carried out with any bank or trust company you may prefer to designate. Payment may be made in full or in six instalments. In either case, 10 per cent. will be required on or before May 10. Subscription blanks will be mailed to you as soon as available. CHARLES HAYDEN, Chairman.

Jan 5, 1919

By A. F. Witt, A. M. Gaudin, A. K. Biswas

Finite contact angles in the rutile-water-organic liquid system are traceable to contamination or are due to addition of a surface-active agent. Finite contact angles are invariably accompanied by hysteresis.1-7 Besides surfactant concentration and pH, the nature of the organic liquid is found to be a factor influencing the magnitude of contact angle hysteresis. In a recent paper the authors have reviewed principles and applications of measurement methods for contact angles and their hysteresis.22 In this paper, these methods are applied to a system consisting of rutile, an organic liquid (benzene, decane, or dode-cane) and water. Surfactant (dodecylamine hydro-chloride) was used at various concentrations and various pH values. MATERIALS A synthetic rutile crystal supplied by the Linde Co. was used. It is a cylinder 1/2 in. diam, with faces cut perpendicular to the c-axis. The crystal is stated to be alumina-free and to be 99.9% pure. Rutile is a high surface energy solid, its calculated average field strength being 2.7 x 105 e.s.u.,9 its dielectric constant10 is 114. The zero point of charge of rutile was measured11 and found to be at pH 6.0. The atomic distances and bond angles of the tetragonal crystal of rutile have been precisely determined.l2 The organic liquids were specially purified. Reagent grade benzene was repeatedly shaken with concentrated sulfuric acid to remove thiophene, then neutralized with sodium hydroxide solution, rinsed with distilled water, dried overnight over anhydrous calcium chloride and filtered. The refractive index of this chemically purified benzene was 1.4977 (at 25°C) - very close to that of pure benzene (n25 1.4979).13 Both n-decane and n-dodecane were washed with aqueous sodium hydroxide, concentrated sulfuric acid (repeatedly, until the acid layer was colorless) and again with alkali, to free the organic hydrocarbon from fatty acids and unsaturated hydrocarbons. The organic phases were subsequently washed with distilled water and dried over anhydrous sodium sulfate. The filtered hydrocarbons were then distilled under vacuum (9-10 mm pressure). Decane, thus purified, showed traces of unsaturated and of carboxylic compounds. On gas chromatographic analysis the purified n-dodecane showed the presence of two impurities. However, the relative retention times of these components did not change substantially when measured on a polar or a nonpolar column. This indicates that the compounds were probably in the same polarity class, i.e. the components were nonpolar like dodecane. Conductivity water has always been one of the liquids. Conductivity of the water used was 10-6 ohm-' cm". Dodecyl ammonium chloride was prepared from pure amine (supplied by Armour and Co., Chicago), by Li in the MIT Mineral Engineering Laboratory.14 The critical micelle concentration at 25°C is known, 0.0138 mol per liter15 or 3.06 gpl. All our experiments have been done at concentrations lower than the critical micelle concentration. The glass vessels, glass drop holder and the rutile crystal were all cleaned with hot chromic acid followed by distilled water, concentrated hydrochloric acid, and again distilled water, and conductivity water. During the experiments, a nitrogen atmosphere was maintained. For this purpose, commercially purified nitrogen was further purified by passing it over hot copper wire at 450°C, then through columns of acidic chromous chloride solution, concentrated alkali solution and distilled water. APPARATUS AND METHODS Hysteresis was produced by the "captive drop" or constant volume drop method as well as by the "expanding-contracting drop" or variable volume drop method. The image of the drop while it is expanding, contracting or moving is projected on a screen and photographed. The developed film is projected through an enlarger and the contact angles measured with a protractor.

Jan 1, 1964