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Note by the Secretary.-—In the preceding communication of Mr. Rickard, in the present discussion, as printed in Trans., xxiii., the loss of quicksilver at Pestarena, reported on p. 569, as 230 and 234 grammes per metric ton, is stated as equivalent to about 74 pounds per short ton avoirdupois—an obvious error, which escaped correction in my reading of the proofs, and was not discovered until after Vol. XXIII. had left the press. The true equivalent is 0.46 pound or about 7 1/2 ounces (instead of pounds) per short ton.— R. w. R. Philip Argall, Denver, Colo. (communication to the Secretary) : Mr. Rickard's last contribution to this discussion* calls for some reply from me, if only by way of defending myself against the charge (p. 569) that my criticisms of his paper were "unnecessarily hypercritical and occasionally unfair." At the same time I am fully aware that our Transactions are not the place for mere personal controversy, and that the sole object of discussion is to define differences of opinion, and defend opposing views as a means of eliciting the truth. Mr. Rickard disclaims the statement, which he says I attributed to him, that in the slow-crushing Gilpin county mills the pyrites remain longer in the mortar than the other portions of the ore. My understanding of his statement was based on the following passages in his paper: " Particles of ore, which have heen pulverized to a fineness which would permit of their exit through the screen, are enabled to settle towards the bottom of the mortar. It would he expected that the heavy metallic minerals occurring in the ore would, because of their greater specific gravity, be most affected by this feature of the treatment. In practice this is found to be so. The fine slimes contain a large proportion of metallic sulphides, generally valuable on account of their close association with the precious metals, while the coarsest particles to be found in the tailings usually consist of quartz and other minerals forming the less heavy gangue (Trans., xxiii., 139).

Jan 1, 1895

By W. S. Ayres

I. INTRODUCTION. THIS cavern was discovered Oct. 22, 1904, by Mr. Charles H. Deutschman, in company with whom I made, May 29 to June 3, 1905, at the request of Mr. Howard Douglas, Superintendent of the Canadian National Parks, the first exploration of it for the Canadian government. The results were stated in a paper, orally presented, with lantern-views from my photographs, at the British Columbia Meeting of the Institute, Victoria,, B. C., July 5, 1905.* The present paper embodies also the results of a second examination, made Oct. 25 to 29, 1905. The accompanying map, Fig. 1, will serve as a guide to the following description. II. LOCATION. The cavern is situated at snow-line, at the head-waters of Cougar creek, on the west slopes of the Selkirks, about 2 miles north from Ross Peak water-tank, and 5.5 miles west from Glacier House, on the main line of the Canadian Pacific Railway. It was then reached by an arduous climb from the water-tank, up the ravine of Cougar creek, for 8,000 ft. (2,000 ft. of altitude) over rock- and snow-slides, and through a thick tangle of alders. But an easy and very picturesque trail has, during the past summer, been opened by the government from Glacier House. Figs. 2, 3 and 4 represent views, not heretofore published, of the grand scenery of this region, so rapidly becoming the-object of attraction to thousands of tourists from all parts of the world. These views, as well as those shown in. Figs. 5, 6, 7, 8

Jan 1, 1907

The Lornex mine is located in the Highland Valley area of British Columbia, Canada, one of the most,promising districts of low-grade porphyry-type copper mineralization in the world; Lornex is operated by Rio Algom Mines, Limited, a member of the Rio Tinto Zinc Group of London. Exploration from 1965 to 1968 disclosed an ore body of 293 million tons with a grade of 0.43% copper and 0. 14% molybdenum; this led to the decision to construct a 38,000 tpd operation, and production commenced in the fall of 1972. The ore is open-pit mined with 15 cu yd (11 5 m3 shovels, which load 100- and 200 -ton trucks. These trucks dump directly into a 60 in. by 89 in. Allis -Chalmers gyratory from two sides of the 14 ft 6 in. (4.42 m) deep dump pocket and across splitters mounted on the pocket sides. The unlined pocket would hold 1,000 tons level full. The crushedore discharges into a 300-ton surge hopper equipped with an automatic sonic level indicator to prevent over -filling. A 96 in. by 23 ft (2.44 m by 7 m) apron feeder delivers the ore from the surge hopper to a 72 in. (1.83 m) transfer belt equipped with a tramp iron metal detector. The transfer belt discharges to a 60 in. (1. 52 m) conveyor which conveys the ore about 3,000 ft (914 m) to the 475,000 ton ore storage pile located near the concentrator. Four 48 in. (1.22 m) pan feeders transfer the ore to the mill feed conveyors, which in turn supply the two 32 ft by 15 ft (9. 75 m by 4. 57 m) semi-autogenous mills, which easily accept the 10 in. (254 mm) product of the crusher. Each semi- autogenous mill is followed by a secondary ball mill. The unusually large open side setting of the crusher accounts for its 6,300 tph maximum capacity. Concentrator capacity is now 48,000 tpd. Eccentric removal is eased by the design of the door to the crushed ore pocket, which has the cart rails mounted on its outer surface and is lowered to a horizontal position in the pocket by an electric winch. The top of the door rests on wear bar covered concrete piers in the pocket. Another feature is a chute through the floor at the crusher base that extends into the crushed ore pocket. Dust and spills of ore on that floor during crusher repairs are easily swept into the crushed ore pocket. This feature is also used at Bougainville and Palabora and has been added to others after operation has commenced. The design follows the concrete rectangular box concept with four main service and maintenance levels shown in the sectional drawings, although a third additional section has been added at the maintenance

Jan 1, 1978

By D. L. Katz, M. J. Rzasa

The derivations of three methods of computing the static pressure gradients in natural gas wells have been presented to show the assumptions made. Charts were developed from which the pressure gradients may be read when the well-head pressure, the well fluid gravity, depth, and the average well temperature are given. A chart for estimating the well fluid gravity from the condensate content and separator gas gravity is included. The effect of the increased average well temperature after flow on the calculation of the static pressure gradient is discussed. Introduction Reservoir pressures have been calculated from well-head pressures for gas wells for many years. As the pressure measurements become more accurate, the need for a reliable calculation of the static pressure gradient often arises. This paper will develop the several methods for computing the pressure gradient in gas wells and make a comparison between them. The method of calculating static pressure gradients in common use is Eq. I (ref. I) or its counterpart which includes a factor for the deviation of the gas from the ideal gas law. P2 - P1 = P1(e0.0000347GX _ I) Eq. [I] in which P1 = pressure at well head, lb. per sq. in. abs. PP = pressure at bottom of well, Ib. per sq. in. abs. G = gas gravity X = depth of well, ft. An alternate method is to compute the average density of the gas in the well and multiply by the well depth in a manner similar to that used for liquid gradients. Derivation of Formulas A static pressure gradient is a special case of the general fluid-flow equation. Consider a pound of fluid flowing in a vertical column from point I to point 2, Fig. I. By an energy balance for fluid flowing from I to 2: U1 + P1V1 + u12/2g + X1 + q = U2 + P2V2+ u22/2g+X2 +W [2] in which U = internal energy, ft-lb. per lb. P = pressure, lb. per sq. ft. V = volume, cu. ft. per lb. u = average linear velocity, ft. per sec. X = height above datum, fl. q = heat absorbed by fluid, ft-Ib. pcr lb. W = work done by system, ft-lb. per lb. An energy balance on the fluid itself gives: U = ?TdS - ?PdV + etc. [3] in which T = temperature, deg- R- S = entropy, ft-lb. per deg. R. per lb.

Jan 1, 1945

By AIME AIME

NO FEATURE of the annual meeting is considered more important at Institute headquarters than the assembly of delegates from the various local sections and divisions. There the president of the Institute and other officials may learn at first hand what the members are thinking and doing in every part of the country, and the delegates, in turn, may find that head- quarters is not a group of more or less cold-blooded New Yorkers whose primary function is to send out annual bills for $15. This year, the section and division delegates required three sessions to thresh out the matters of common interest: Monday morning and afternoon and Thursday afternoon. They were also guests of the Institute at the Directors' dinner on Tuesday night, and at the Directors' meeting afterward.

Jan 1, 1932

By C. W. Hill, G. P. Luckey

In a previous article1 preliminary experiments were described, indicating the possibilities of a quantitative spectroscopic method for the determination of small amounts of lead in copper, which would be accurate and rapid, and could be carried out in the refining plant by one not skilled in chemical analysis. The present paper deals with the development of the method in the factory, giving the details of apparatus and its standardization, and presenting a comparison of the accuracy of the method with that of the standard electrolytic determination. (For variations and other applications of the method, the reader is referred to the first article.) A carefully weighed sample (0.4 gm.) of the copper to be tested is placed in a cavity in a graphite positive electrode. An arc capable of

Jan 1, 1919

By L. W. Kempf

A BALANCED system of internal stress is set up in any metallic structure by plastic deformation below the annealing temperature. The internal stress induced by cold rolling or other fabricating processes is generally recognized and its magnitude is known to be, within certain limits, a function of the degree of cold deformation. The plastic deformation that may accompany rapid cooling from elevated temperatures may not materially change the form of the product. The internal stresses so induced are not, therefore, so evident and nonrecognition of their presence has at times led to engineering failures. The heat treatment of aluminum alloys is a relatively new art and little information is available regarding the magnitude of stresses induced luring the commercial heat treatment of aluminum alloy products is the industrial use of aluminum increases, it is inevitable that products of increasingly large volume be required. It has become necessary in the present commercial utilization of aluminum to heat-treat castings and forgings weighing hundreds of pounds. One of the factors governing the magnitude of internal stresses arising from rapid cooling at elevated temperatures is that of the, size of the structure being treated. Some of the other factors are: cooling rate, elastic properties of the alloy, thermal expansivity, thermal conductivity, and the presence or absence of phase changes. Practically all aluminum alloys have a high coefficient of thermal expansion and some are capable of developing relatively high

Jan 1, 1934

By John B. Hastings

THE reconnaissance of the Goldfield mining-district, described in this paper, was made in May and June, 1905, and, though this time was too short for a complete report, the work accomplished may serve as a basis for more thorough future research. Dr. Berkey has examined the rocks collected by myself, and I am using his classifications. As a result of further field-work, and Dr. Berkey's examination of the rocks, this paper is an elaboration and correction of my views expressed in the Gold-field Sun, May 12, 1905. The sketch-map, Fig. 1, illustrates the geology of the Goldfield mining-district. Goldfield is an eruptive complex, consisting of alaskite (binary granite), hornblende-andesite, hornblende-dacite, rhyolite, pyroxene-andesite, pyroxene-dacite (sometimes containing, a small quantity of olivine), quartz-felsite, olivine-pyroxene-ande¬site, and basalt. Considering this list to be arranged in the order of eruption, the age-sequence of the rocks conforms to Richthofen's law, formulated in 1868. From his observations in Europe and America, propylite, andesite, trachyte, rhyolite and basalt, occurring together, succeed one another. In a general way, the medium and more acidic rocks precede the most asic-a result supposed by some to have arisen from their relative position beneath the surface, and due to a rude stratification by gravity in the original cooling magma during the older history of the earth, or to the same differentiation occurring during a quiescent (molten ?) period preceding eruption, being aided by the ease with which acidic rocks, mixed with water vapors, become fusible. In effect, the more basic and less re-

Mar 1, 1906

By W. M. Myers

Certain minerals possess inherent color and other properties that make them suitable for the pigmentation of paints, mortar, plaster, concrete, face brick, and other materials. Their production is one of the most ancient of mineral industries and their use by primitive man is well known. These natural pigments have some economic factors in their favor, particularly wide geographic distribution, low cost of production, ease of preparation, chemical stability, and permanence in use so that they continue to form the basis of a small but useful industry. When used in paints such pigments act as a filler and supply body and opacity in addition to color. Natural mineral pigments are prepared for the market by the comparatively simple operations of washing, grinding, blending, and calcining. Any one, or all of these processes may be applied to a single pigment. The development of synthetic pigments and the use of by- product materials have introduced competition with the products of nature and are having a growing influence on the economic position of the mined minerals.

Jan 1, 1949

By Ralph M. Hunter

Until recent years, maintenance of surface coal handling facilities was a relatively simple task. Equipment consisted principally of conveyors, screens and crushers of comparatively simple construction. Electrical equipment consisted of motors and starters, with little, if any, interlocking. In most cases failure of any component affected only the grades of coal loaded so that even a prolonged breakdown did not affect mine operation materially. However, with the introduction of modern cleaning plants, the picture has changed. The equipment is much more complex and therefore more difficult to maintain. In many cases failure of any component of the plant prevents loading of coal. Even if provision is made to bypass, the quality of coal loaded is lowered, affecting markets. In the case of plants designed to permit full seam mining, marketable coal cannot be loaded without operation of the cleaning plant. Under these conditions it is apparent that considerable thought and effort toward better maintenance are justified. In order to assure continuous, efficient and economical operation, maintenance should receive consideration, not only after the plant is in operation, but while it is being designed. It is hardly necessary to say that the designer should strive for sturdi-ness and wearing qualities. It is sometimes not realized, however, that even the best parts will sooner or later require replacement or repair. The designer should, there- fore, give consideration to accessibility. Anyone who has had to do with cleaning plant maintenance is familiar with installations where several hours are required to get at a part that can be repaired or replaced in a few minutes, once it is accessible. As in most cases, experience is the best guide. The men who operate and maintain this equipment know the problems encountered. Whenever available, the opinions of these men should be sought and heeded. As an example, we might consider the refuse elevator on a Chance Cone. Our company is now operating three of these cones, the first of which was installed in 1941, and the latest in 1946. Exact records are not available, but well over 50 pct of delays charged to the Chance Cones have been caused by the refuse elevator. This elevator receives refuse from the cone and carries it to a point above the water level of the cone, discharging onto a dewatering and desanding screen. Since the elevator operates under water and necessarily has close clearances in the lower boot, it tends to jam on large pieces of refuse or tramp iron. The chain, buckets and boot are also subjected to the action of water, sand and refuse, which accelerate normal wear. In case of jamming or chain-breakage it is necessary to drain the elevator and the cone so that even a minor fault in the elevator causes a considerable loss of time for the cone. In our new plant, which will contain two Chance Cones, the refuse elevator has been eliminated. This was accomplished by raising the cone so that the refuse gates could discharge directly onto the dewater-

Jan 1, 1949

By J. WILLIAM WETTER

WHEN the privilege was extended to me to address this meeting I could not help but make a mental review of my own activities and experiences in connection with association work. After having spent about 16 years in the mining engineering field, I entered into the operating branch of coal mining which afforded, about 12 years ago, my first opportunity of attending a meeting of our local Association and sitting in with the "big boys" of the industry. This was quite a thrilling experience because I had heard a great deal about the various operators who belonged to the Association and knew, or at least thought I knew, that a certain group dominated its affairs and that a "clique" was in control of a sizable "roller" which could be "steamed up" at will to flatten out any opposition which might appear upon the horizon or under it, too, for that matter. Now, I was to have the privilege of observing this "clique" at first hand, of seeing a small group making the policies and shaping the destinies of a great industry and planning the activities of an important Association while a large majority of the members would sit by either complacently or otherwise with the full knowledge that the "roller" was in waiting to reduce them to ribbons at the first sign of resistance.

Jan 1, 1930

By W. J. Taylor

FURNACE-MEN who have not taken advantage of the use of dynamite in certain blast-furnace troubles, as explained by Mr. Witherbee in his valuable papers read before the Institute some years since, cannot appreciate the quick relief and great advantage that may be derived at times from its judicious employment. Before giving my experience in the use of high explosives in blastfurnace troubles of certain kinds, I will record a method I have used with marked success in " blowing down." Had I not understood, however, the use of powder, I would have " salamandered " effectually the first time I tried it. Early in my straight-furnace experiments, last summer, at the Chester, N. J., Furnace, I wanted to blow down to within 3 or 4 feet of the tuyeres. To do this with a down-comer not lined, and without putting in any limestone to keep the gases cool enough to do no harm, was not an easy task. We could keep the bell and hopper cool by filling them with water, say 12 inches deep; but before we got the stock down 15 or 20 feet the pyrometer in the gas-flue on top mas up to 1300°, and the clowncomer was red-hot, with the heat still rising. In this emergency my assistant, Mr. N. M. Langdon, urged the trial of a plan lie had often advocated, viz., the introduction of water in some way under the bell in the proper quantity, in order that its evaporation might absorb and reduce the heat of the escaping gases to a point where it would not do any harm. He thought the bell

Jan 1, 1885

By N. S. Stoloff, R. C. Ku, R. G. Davies

The stress-strain behavior of Fe-Co and Fe- V alloys containing up to 25 pct solute have been studied in the temperature range 25° to - 196°C. The microyield stress is independent of temperature for all alloys studied, while the temperature dependence of the ordinary yield stress is large and comparable to that for unalloyed iron. An alloy-softening phenomenon is observed for many alloys relative to unalloyed iron, and appears to be a consequence of removal of inter-stitials from solution and their subsequent agglomeration. The ductile to brittle transition temperature is increased markedly by both cobalt and vanadium. Transmission electron microscopy observations reveal that cross slip and cell formation are restricted with increasing solute, which can account for many aspects of yielding and fracture behavior. IRON and other metals of bcc structure slip on many planes of the (111) zone at moderate and elevated temperatures, giving rise to wavy glide. At low temperatures, however, there is a tendency for slip to be restricted to planes of only one or two crystallographic types; in the case of Fe-Si alloys for example, (110) glide predominates, giving rise to planar slip bands."' Restriction of cross slip at low temperatures in iron has been linked by Brown and Ekvall3 to increased strain hardening in the preyield microstrain region, leading to an apparently large temperature dependence of the yield stress. Support for this view has been provided by Lawley and Gaigher4 from a transmission electron microscope study of molybdenum. They concluded that dislocations at lower temperatures, by virtue of their inability to change planes readily, are unable to interact and annihilate, leading to an increase in internal stress and work-hardening capacity. Restriction of cross slip at low temperatures has also been suggested to be an important factor in determining the ductile to brittle transition of single-phase solids, including metals of bcc structure.5 It is pertinent to note that most solute elements tend to raise the ductile to brittle transition temperature of poly crystalline ferrite,6,7 although in some cases, e.g., Fe-Cr7 and Fe-Al,8 the dilute alloys may actually yield at lower stresses than unalloyed iron. It appears, therefore, that solute elements may have an effect analogous to lowering the test temperature with regard to restricting cross glide. Such an effect has indeed been observed in the ionic alloy system KCl-KBr,9 in which bromine atoms, although causing little misfit and consequently little effect on the yield stress of KC1, have a pronounced effect in restricting wavy glide and inducing brittleness. The purpose of the present investigation was to determine the effects of selected solute atoms on the yield stress and fracture behavior of iron, and to elucidate in turn how the slip character was related to these properties. Since it is known that interstitial atoms exert a strong influence on the mechanical behavior of iron, the solute elements chosen for study were vanadium, which reacts strong with interstitials,10 and cobalt, which does not form highly stable interstitial compounds." EXPERIMENTAL PROCEDURE Four-pound ingots of each of the following alloys were vacuum-melted in zirconia crucibles: Fe-1, 5, 10, 25 at. pct Co, and Fe-1, 4, 10, 20 at. pct V. An ingot of unalloyed iron from the same original stock as that used for the alloy was remelted under similar conditions to eliminate variations in interstitial content arising from differing thermal histories. Chemical analyses of the iron, cobalt, and vanadium melt stock are listed in Table I. All ingots were rolled and swaged, commencing at 850°C, to 1/4-in.-diameter bar. The bars were then annealed at 850°C for 1 hr (except that the 10 and 20 pct V alloys were heated for 2 hr) to give a uniform equiaxed grain size of about 0.05 mm. Tensile samples of 0.125 in. diameter by 0.8 in. gage length were utilized for studies of the ductile to brittle transition. A second set of tensile samples were utilized for microstrain experiments in which strain sensitivity of 1 x 10"6 was achieved by a capacitance method.3 Cylindrical compression samples 0.250 in. diameter by 0.4 in. long also were prepared to study the influence of composition on the macroscopic yield stress, and for metallographic analyses of defor-

Jan 1, 1965

By J. F. Myers, S. E. Sharp

THE safety data presented in this paper are based upon replies to a Questionnaire sent out to representative mining companies. The authors feel that it is a fair cross section of the milling industry, in that the 17 companies, of the United States and Canada, reporting on 22 mills, are scattered from the Hudson Bay to the Mexican border and from coast to coast. These data concern the accident records of the. various plants from 1939 to 1944, inclusive and the six years are divided into two periods. The first period (1939, 1940 and 1941) represents something of a normal operating condition. The second period (1942, 1943 and 1944) represents the period of time that was most affected by war con¬ditions. During the second period there was a high labor turnover, inexperienced workers were numerous, women replaced men in many kinds of work, a labor shortage existed more or less throughout the industry, and supervision was pushed for peak production. All of the companies reporting compiled their accident experiences for these six years in accordance with the standards set up by the American Standards Association (Engineering Societies Building, New York, N. Y.), consequently the tabulated data presented herein are comparable. The authors of this paper feel that the industry as a whole is greatly indebted to the personnel of the companies that furnished these data, which make this study possible for presentation. This survey covers a total exposure of 74,528,880 man-hours, with 105,471 man-days of lost time from 870 accidents. SAFETY RECORDS In Table I, the safety record is shown of the various mills reporting. The severity rate is usually conceded to be the most vital statistical figure in safety parlance, therefore the participating companies are listed in order of their severity rate for the combined six-year period, under size of organization. The table also shows the frequency rate as well as the frequency-severity ratio (F/S). As noted in Table 1, most of the companies suffered an increase in both severity and frequency rates during the second period; only six of the 22 enjoyed an improvement. From correspondence with the various plants, it seems that a few had very little labor shortage or turnover, and these were not greatly affected. A few plants, anticipating the situation, strengthened their training facilities and actually were able to show a better experience during the second period. This gives great credence to the value of organized training in any safety program. The frequency-severity ratio (F/S) shown in the last column of Table I offers

Jan 1, 1946

By E. W. Johnson, M. L. Hill

Cold working of iron-carbon alloys was found to increase greatly the hydrogen solubility and to decrease the diffusivity at temperatures up to 400° C. These effects are increasing functions of both the carbon content and the degree of deformation. The hydrogen behavior is consistent with the idea that cotd working creates "traps", which are concluded to be microcracks in which the hydrogen is chemisorbed. Hydrogen embrittlement is explained by the Petch theory of metal crack surface energy loss due to hydrogen adsorption. HYDROGEN embrittlement of steel has been studied for many years and has been the subject of an extensive literature, but the mechanism of the effect has not been completely understood. The embrittlement is unusual in that the ductility loss is not accompanied by an increase of the yield strength, being primarily a decrease of the fracture strength alone. The loss of fracture strength is usually most severe in the temperature range between 0°and 100°C. Here the solubility of hydrogen in the iron lattice at ordinary H2 pressures is extremely low while the diffusivity is still quite high. From the relationships between the ductility and the hydrogen content, test temperature and strain rate, it is apparent that the hydrogen atoms causing the ductility loss difbse to and concentrate in small regions of the metal which are especially susceptible to the initiation and propagation of fracture. This hydrogen segregation apparently occurs after plastic straining has begun. Below 0°C the ductility loss persists only at low strain rates in confirmation of the view that the embrittlement is diffusion .controlled. The tendency of the embrittlement to disappear above 100°C can be explained by the increasing lattice solubility of hydrogen with rising temperature. A common view of hydrogen embrittlement of steel is that the hydrogen initially dissolved in the metal lattice diffuses to structural discontinuities and there precipitates as H2 gas at very high pressures which assist the external stress in causing premature failure.1,2 The idea of a high H2 pressure in equilibrium with ordinary amounts of hydrogen in steel at room temperature is due to observations of hydrogen behavior in fully annealed material, for which the Sieverts' law constant relating solute concentration to H2 pressure is extremely small. Hydrogen-embrittled steel, however, is always plastically deformed to some extent, and therefore it is important that hydrogen embrittlement be explained primarily in terms of hydrogen behavior in plastically deformed material. Such an explanation is attempted in this paper. Previous studies of hydrogen in cold-worked steel have shown that both the solubility and the diffusion rate are significantly chaned when the steel is cold worked. Darken and Smith discovered that the amount of hydrogen absorbed from acid by cold-rolled steel at 35°C is many times greater than that absorbed by hot-rolled steel. They found also that the hydrogen permeability of the steel is unaffected by cold working. Keeler and Davis4 confirmed the high apparent solubility of hydrogen in cold-worked iron-carbon alloys at temperatures up to and even beyond the recrystallization temperature. They also found that this solubility increase accompanying cold work is a sensitive function of the carbon content, being absent when no carbon is present. The present experimental study was undertaken primarily to obtain an improved understanding of the behavior of hydrogen in cold-worked steel. Data were obtained on the effects of temperature, H, pressure, carbon content, and degree of cold work on the hydrogen solubility and diffusivity in iron-carbon alloys. These data have been helpful in elucidating the nature of the cold-worked steel structure as well as in providing information on the mechanism of hydrogen embrittlement of steel. EXPERIMENTAL Cylindrical specimens for hydrogen absorption and diffusion rate measurements were prepared from three iron-carbon binary alloys and a commercial SAE 1010 steel. The iron-carbon alloys were prepared by vacuum melting electrolytic iron with graphite in a magnesia crucible. The alloys were cast in vacuum as 2 1/2-in. sq ingots weighing about 20 lb each. The ingots were hot rolled (above 1900°F) to 5/8-in.-diam round bars and then cooled in air to room temperature. The resulting metallographic structure consisted of islands of fine pearlite surrounded by free ferrite. Chemical analyses of the materials are given in Table I. The 5/8-in. diam bars were turned to diameters such that cold reduction to the desired final specimen diameters would result in either 30 or 60 pct reduction in area (RA). The machined bars were then cold worked by swaging at room temperature

Jan 1, 1960

By G. R. Speich

The interlarnmelm spacing, growth rate, and degree of segregation that accompany cellular precipitation in four Fe-Zn alloys containing 9.7, 15.2, 23.5, and 30.5 at. pct Zn have been determined in the temperature range 400" to 600°C. The chemical free-energy change for the reaction was calculated from the available thermodynamic data and the known compositions of the phases. The fraction of the chemical free-energy change for equilibrium segregation that is converted into interfacial free energy decreases from 0.43 to 0.08 as the magnitude of this free-energy change increases from 35 to 270 cal per mole. At constant temperature the cellular growth rate is proportional to the cube of the dissipated free energy. At 600°C newly 100 pct of the equilibrium segregation is achieved during cellulm precipitation whereas at 400°C only 85 pct of the equilibrium segregation is attained. During cellular growth, mass transport of zinc occurs by grain boundary diffusion; excess zinc remaining in the a! phase after the completion of growth is removed slowly by volume diffusion. A modified Cahn theory of cellular precipitation predicts the observed interlamellar spacing within a factor of two. In cellular precipitation reactions such as pearlite formation or discontinuous precipitation, the basic problem is to predict the variation of growth rate G, interlamellar spacing S, and degree of segregation P with composition and temperature. To accomplish this we need three independent equations relating these quantities. One of these equations comes from the diffusion solution. To obtain two additional independent equations, some assumptions must be made. cahnl has suggested recently that two plausible assumptions are 1) that growth rate is proportional to the dissipated free energy and 2) that the spacing which occurs is that which maximizes the dissipated free energy. According to the first assumption, this spacing also maximizes the growth rate and the rate of decrease of free energy per unit area of cell boundary. The present work was undertaken to test these assumptions. To test the first assumption it is necessary to study a cellular reaction over a wide range of supersatura-tions to establish a relationship between G and the dissipated free energy at constant temperature. This is possible only in discontinuous precipitation reactions since in pearlite reactions constituents other than pearlite form if the composition of the parent phase deviates even slightly from the eutectoid composition. The Fe-Zn system was chosen for study because 1) discontinuous precipitation proceeds to completion over a wide temperature and concentration range, 2) the degree of segregation within the cell can be measured by lattice parameter measurements,2 and 3) the thermodynamics of this system have recently been determined by Wriedt.3 In this system the cells consisting d alternate lamellae of a and r phases form from supercooled iron-rich a phase. The a phase within the cells is bcc as is the original a phase, cia, but has a different orientation and a slightly lower zinc content than the original a phase. The r phase has a zinc content of about 70 at. pct and a crystal structure isomor-phous with T brass. EXPERIMENTAL PROCEDURE Four Fe-Zn alloys with 9.7, 15.2, 23.5, and 30.5 at. pct Zn were prepared from carbonyl-iron powder (400 mesh, 99.8 wt pct Fe) and zinc powder (200 mesh, 99.99 wt pct Zn). The powders were ball-milled together and cold-pressed under 60,000 psi to discs $ in. thick by $ in. diam. The cold-pressed discs of the alloys with 9.7 and 15.2 at. pct Zn were sealed in evacuated silica capsules and heated slowly to 1100°C over a period of 1 week (3 days at 600°C, then 3 days at 80O°C, then 1 day at 1100°C). The alloys with 23.5 and 30.5 at. pct Zn were treated similarly except that the final homogenization temperatures were 1000" and 85O°C, respectively, to prevent melting. The alloys were quenched in iced brine from the final homogenization temperature. Specimens of each alloy were subsequently aged in salt pots at temperatures of 400°, 450°, 500°, 550°, 600°, and 650°C for times that varied from a few minutes to several hundred hours. At a late stage of this work, an alloy containing 11.2 at. pct Zn was prepared by vapor-impregnation of iron foil with zinc vapor at 890°C. This alloy proved useful for electron microscope studies because it was free of porosity. The homogenization and aging conditions were based on the recent Fe-Zn phase diagram of Stadelmaier and Bridgers4 rather than the earlier diagram of ansen.5 They consist of a homogenization heat treatment in the homogeneous a field followed by an aging treatment in the two-phase a + r field. The aged specimens were metallographically polished and etched in 2 pct nital and the radius of the largest cell in the microstructure determined. This radius plotted vs time gave a straight line whose slope is the boundary migration rate or growth rate G of the cell. To determine the interlamellar spacing, specimens were examined by surface-replica and thin-section electron microscope techniques. Because of the irregular nature of the lamellae within the cell, the average interlamellar spacing S .of the cell was measured by the method of Cahn and Hagel,6 where S is defined by:

Jan 1, 1969

By A. H. Grobe, F. N. Rhines

AT elevated temperatures the oxide of silver is unstable in the air at atmospheric pressure, consequently no external oxide scale forms upon pure silver under conditions of high-temperature annealing When small quantities of certain alloying elements are present in the silver, the formation of a thin external scale is possible' and in addition there may form a subscale composed of the oxide of the solute element precipitated within the body of the silver Norbury2 and Leroux and Raub3 have reported internal oxidation (subscale formation) in alloys of silver with 2, 7 5, and 30 per cent of copper The presence of the subscale is believed to be responsible, at least in part, for the objectionable "fire mark" in Sterling silver' Several other alloys of silver, after oxidizing heat-treatments, are known to exhibit undesirable polishing characteristics that may be the result of internal oxidation Except for the absence of an external scale of silver oxide, it is to be anticipated that silver alloys will prove to be very similar in their oxidation behavior to the alloys of copper, the oxidation characteristics of which have been studied in some detail 5,6 The present research confirms this anticipation The oxidation of a series of 20 dilute alloys of silver has been studied metallographically, some types of subscale not encountered among the copper alloys have been found Instances of internal oxidation in alloys of most of the metals of the I-b and VIII groups of the periodic system are on record, but evidence of this type of oxidation in alloys of the metals of the intermediate groups is lacking A number of the metals of the intermediate group, among them cadmium, lead, tin, and zinc, appear to provide the conditions essential to subscale formation, i e , they form oxides with a relatively low negative free energy of formation, they dissolve other metals that form more stable oxides, and, presumably, oxygen will diffuse through them In a study of 4o alloys of these white metals only a few cases of internal oxidation have been found The probable reasons for this difference in behavior will be discussed presently EXPERIMENTAL PROCEDURE Silver -The silver alloys employed in the oxidation studies were prepared in heats of 30 grams each from high-purity silver (99 993 per cent Ag)* and the purest avail-

Jan 1, 1942

By Ottar Dragge, C. Danielsson, Bo Kalling

DISCUSSION, T. L. Joseph presiding L. F. Reinartz (Armco Steel Corp., Middletown, Ohio) —I would like to know, in the practical application of the Kalling process, what kind of a lining was used, how thick was the lining, and how much metal was treated at one time? S. Fornander (author's reply)—The rotary furnace is lined with a course of fireclay bricks 6 in. thick. This course is backed by 5 in. of insulation. The furnace has a capacity of about 15 tons. Mr. Reinartz—How was the ladle preheated? Mr. Fornander—As pointed out in the paper, the furnace was heated by a gas flame in the beginning of the experiments. During these first tests, however, the desulphurization was inconsistent. We think that this was due to the fact that iron droplets sticking to the furnace walls were oxidized by the gas flame. Now, the furnace is operated without preheating of any kind, and the results are much better. T. L. Joseph (University of Minnesota, Minneapolis, Minn.)—I might add one comment. This furnace was heated with a flame and for a time they had a little difficulty due to some residual metal in the rotating drum that would oxidize in between treatments and they found therefore, that it was very essential to drain the drum completely of metal so that they would not build up any ferrous oxide between treatments and they eliminated some of their erratic heats by maintaining those more reducing conditions. It was interesting to watch this operation. As soon as the drum started to rotate there was considerable flame, at least, at the time I saw it, that came out around the flanges, indicating there was quite a little pressure on the inside of the drum. W. 0. Philbrook (Carnegie Institute of Technology, Pittsburgh)—Is the reaction slag in the Kalling process liquid or solid, and how is it separated from the metal? Mr. Fornander—In the process there is no slag in the usual sense of the word. The lime powder does not melt during the treatment. After the treatment the lime is still in the form of a fine powder. It is separated from the metal by means of a piece of wood of suitable size placed within the furnace before it is emptied. D. C. Hilty (Union Carbide & Carbon Research Laboratories, Niagara Falls, N. Y.)—Dr. Chipman has given us some of his ideas in connection with a specific effect of silicon and silica on sulphur elimination and how silicon might interfere with desulphuriz- ing in the blast furnace. I wonder if he would like to elaborate on the possibility of a similar effect of silicon in the Kalling process? J. Chipman (Massachusetts Institute of Technology, Cambridge, Mass.)—Silicon does not interfere with the Kalling process. Anything that has strong reducing action is good for desulphurization. In these tests where the temperature was low compared to blast furnace temperatures, the silicon that is in the metal is a better reducing agent than the carbon. At high temperatures, carbon is the better. It is not the silicon in the metal that interferes with desulphurization, it is the silica in the slag. Mr. Joseph—I might add that the metal that was tapped from the drum after desulphurization was really at quite a low temperature. It was not measured, but I think it was well under 1300 °C, probably 1200" or a little above that. That was one of the difficulties, and I think there is no question about the fact that the Kalling process—in that it affects desulphurization between powdered lime, solid and liquid iron— is a reaction definitely between the solid lime and the liquid iron. E. Spire (Canadian Liquid Air, Montreal, Canada) — This Kalling process seems very interesting to us and after all it is only a mixing action that is taking place between the iron and the slag. We have attempted to do the same thing in another way. We have placed at the bottom of the ladle a porous plug through which we injected an inert gas. It can be nitrogen or argon. This plug is placed at the bottom of the conventional ladle and gas injected through the plug. That has appeared in our patent. To define this new type of treatment, I use the word gasometallurgy. I do not know if you like it, but it is a way of defining methods of treating metal using gases. What we do is exactly what is done in the exchange process in another way. We have a porous plug at the bottom with a high lime slag on top of the metal. Using this method, we have very good agitation of metal and slag, and with a small flow of gas, we can achieve a very strong agitation. For instance, in the 500 lb ladle, we use only 5 liters of gas a minute. We have an agitation compared to very rapidly boiling water in a pail. Moreover, the agitation can be controlled to create any amount of mixing desired. In a few minutes, with this method, the sulphur dropped from 0.58 to 0.11. These results have been improved since, and we have obtained results like 0.08

Jan 1, 1952

By Sven Fornander

L. F. Reinartz (Armco Steel Corp., Middletown, Ohio) —I would like to know, in the practical application of the Kalling process, what kind of a lining was used, how thick was the lining, and how much metal was treated at one time? S. Fornander (author's reply)—The rotary furnace is lined with a course of fireclay bricks 6 in. thick. This course is backed by 5 in. of insulation. The furnace has a capacity of about 15 tons. Mr. Reinartz—How was the ladle preheated? Mr. Fornander—As pointed out in the paper, the furnace was heated by a gas flame in the beginning of the experiments. During these first tests, however, the desulphurization was inconsistent. We think that this was due to the fact that iron droplets sticking to the furnace walls were oxidized by the gas flame. Now, the furnace is operated without preheating of any kind, and the results are much better. T. L. Joseph (University of Minnesota, Minneapolis, Minn.)—I might add one comment. This furnace was heated with a flame and for a time they had a little difficulty due to some residual metal in the rotating drum that would oxidize in between treatments and they found therefore, that it was very essential to drain the drum completely of metal so that they would not build up any ferrous oxide between treatments and they eliminated some of their erratic heats by maintaining those more reducing conditions. It was interesting to watch this operation. As soon as the drum started to rotate there was considerable flame, at least, at the time I saw it, that came out around the flanges, indicating there was quite a little pressure on the inside of the drum. W. 0. Philbrook (Carnegie Institute of Technology, Pittsburgh)—Is the reaction slag in the Kalling process liquid or solid, and how is it separated from the metal? Mr. Fornander—In the process there is no slag in the usual sense of the word. The lime powder does not melt during the treatment. After the treatment the lime is still in the form of a fine powder. It is separated from the metal by means of a piece of wood of suitable size placed within the furnace before it is emptied. D. C. Hilty (Union Carbide & Carbon Research Laboratories, Niagara Falls, N. Y.)—Dr. Chipman has given us some of his ideas in connection with a specific effect of silicon and silica on sulphur elimination and how silicon might interfere with desulphuriz- ing in the blast furnace. I wonder if he would like to elaborate on the possibility of a similar effect of silicon in the Kalling process? J. Chipman (Massachusetts Institute of Technology, Cambridge, Mass.)—Silicon does not interfere with the Kalling process. Anything that has strong reducing action is good for desulphurization. In these tests where the temperature was low compared to blast furnace temperatures, the silicon that is in the metal is a better reducing agent than the carbon. At high temperatures, carbon is the better. It is not the silicon in the metal that interferes with desulphurization, it is the silica in the slag. Mr. Joseph—I might add that the metal that was tapped from the drum after desulphurization was really at quite a low temperature. It was not measured, but I think it was well under 1300 °C, probably 1200" or a little above that. That was one of the difficulties, and I think there is no question about the fact that the Kalling process—in that it affects desulphurization between powdered lime, solid and liquid iron— is a reaction definitely between the solid lime and the liquid iron. E. Spire (Canadian Liquid Air, Montreal, Canada) — This Kalling process seems very interesting to us and after all it is only a mixing action that is taking place between the iron and the slag. We have attempted to do the same thing in another way. We have placed at the bottom of the ladle a porous plug through which we injected an inert gas. It can be nitrogen or argon. This plug is placed at the bottom of the conventional ladle and gas injected through the plug. That has appeared in our patent. To define this new type of treatment, I use the word gasometallurgy. I do not know if you like it, but it is a way of defining methods of treating metal using gases. What we do is exactly what is done in the exchange process in another way. We have a porous plug at the bottom with a high lime slag on top of the metal. Using this method, we have very good agitation of metal and slag, and with a small flow of gas, we can achieve a very strong agitation. For instance, in the 500 lb ladle, we use only 5 liters of gas a minute. We have an agitation compared to very rapidly boiling water in a pail. Moreover, the agitation can be controlled to create any amount of mixing desired. In a few minutes, with this method, the sulphur dropped from 0.58 to 0.11. These results have been improved since, and we have obtained results like 0.08

Jan 1, 1952

By D. T. Peters

To better understand the Co-Mo interaction in maraging steels, the precipitate reversion behavior of two alloys closely related to the 18 Ni-250 grade has been studied. The reversion experiment is carried out by aging at a low temperature, T1 (preaging temperature), for some period of time and then aging at a higher temperature, T2, called the reversion tetnperature. Aging and reversion tmzperatures used were in the range 679 to 1050°F. Reversion is marked by an increase in resistivity and a decrease in hardness. It teas found that some reversion took place at all cornbinations of T1 and T2 but that pronounced rei3ersion resulfed for an Fe-18 pct Ni-5 pct Mo-8 pcl Co alloy exposed to preagz'ng' temperatures at or below 850°F. A similar alloy not containing cobalt exhibited no such discontinuity in reversion behazior with TI. The results are interpreted in terms of two types of molybdenum-rich precipitates, one nucleated at dislocations and the other in the matrix. The increased supersaturation resulting from the presence oj- cobalt evidently provides sufficient energy to nucleate the matrix phase. Anotnalies in the temperature dependence of the resistivity decrease and peak hurdness in the Fe-18 pct Ni-5 pct Mo-8 pct Co alloy as a junction of aging temperature noted in an earlier study are explained on this basis. SEVERAL investigatorsl-9 have studied the details of the precipitation-hardening reaction of the maraging steels. The great majority of conclusions have been drawn from transmission electron microscopy. Although much has been learned by this method, alternate techniques which will give information earlier in the aging process are needed for a more complete understanding of the series of precipitation steps probably involved in the aging reaction. Peters and cupp'' have recently shown, by measurements of the kinetics of precipitation, that an 18 pct Ni-Co-Mo maraging steel shows a distinct change in precipitation behavior at aging temperatures below 850°F. The results were interpreted in terms of the existence of two types of precipitates at low aging temperatures. Only one precipitate type is present at higher aging temperatures. The low-temperature precipitate was found to be a particularly effective strengthener. No evidence for the additional low-temperature precipitate was found in the 18 pct Ni-5 pct Mo ternary alloy. The object of this investigation was to study further the characteristics of the two types of precipitates and the interaction between cobalt and molybdenum characterizing this system. Some preliminary experiments indicated a difference in reversion behavior in specimens aged above and below 850°F. This suggested that knowledge of the reversion behavior might shed some light on these two questions. Hardy and Heal11 have defined reversion as the loss of hardness, electrical conductivity, or other properties caused by heating for a very short time at temperatures above the aging temperature. The precipitate reversion referred to in this paper is entirely distinct from "austenite reversion" often referred to in maraging steel literature. This latter phenomenon could more accurately be called the diffusion-controlled formation of austenite. Much has been written about reversion in several of the aluminum-base binary and ternary alloys.'2-16 Two explanations for reversion have been advanced. Based on the classical nucleation theory of Volmer-Weber-Becker-Doring,17 Konobeevski18 suggested that reversion was due to the size of the precipitate particles

Jan 1, 1968