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By F. Lynwood Garrison

As the specific gravity of low-carbon steel seems to be attracting considerable attention as a means of détermining the quality and value of the metal, I give here a few of the results of a long series of experiments recently made by me. The object of the experiments not requiring more than approximate correctness in the third place of decimals, the extreme precautions to obtain accuracy which are sometimes used in determining specific gravity were not observed. But each piece of metal was carefully cleaned to remove scale, rust, dirt, etc., thoroughly dried, and then weighed in air, all weighings being carefully repeated. The balance used was one of Troemner's finest, and sensitive to one-tenth of a milligram. Before weighing in distilled water, care was taken to remove, as far as possible, the air enclosed in the pores of the metal. The pieces of metal were suspended by means of fine silk thread, a correction of course being made for the weight of the silk. Care was taken that the water in which they were weighed should he always at the same level, and, as far as possible, at the same temperature.

Jan 1, 1887

By Alexander Knoll, Dwight L. Baker

THE work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those [ ] of high surface tension; i.e., nitrobenzene, diphenylmethane. WETTING PROPERTIES OF GALENA IN NONAQUEOUS FATTY ACID SOLUTIONS When a "captive bubble"1 is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method.* [ ] When pure nitrobenzene' was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell.2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1941

By Dwight L. Baker, Alexander Knoll

The work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those of high surface tension; i.e., nitrobenzene, diphenylmethane. Wetting Properties of Galena in Nonaqueous Fatty Acid Solutions When a "captive bubble"I is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method." When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1943

By Alexander Knoll, Dwight L. Baker

THE work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those [ ] of high surface tension; i.e., nitrobenzene, diphenylmethane. WETTING PROPERTIES OF GALENA IN NONAQUEOUS FATTY ACID SOLUTIONS When a "captive bubble"' is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method.* [ ] When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell.2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1941

By Alexander Knoll, Dwight L. Baker

The work herein reported shows that galena in certain organic solutions of fatty acids becomes coated with lead soaps, and that this coating is not only highly water-repellent but is also repellent to certain organic liquids, particularly those of high surface tension; i.e., nitrobenzene, diphenylmethane. Wetting Properties of Galena in Nonaqueous Fatty Acid Solutions When a "captive bubble"I is withdrawn from a polished, plane galena surface under a nitrobenzene solution of stearic acid, the air bubble shows a decided tendency to "cling" to the mineral surface. The contact angle, therefore, was greater than zero, although it was not large enough to be measured quantitatively by the captive-bubble method." When pure nitrobenzene was substituted for the nitrobenzene-stearic acid solution, no clinging of the bubble was observed; viz., contact angle = zero. Although the contact angle developed in air-galena-nitrobenzene-fatty acid solution was small, the organic solvent repellency of the galena surface was great enough to enable good recovery in a laboratory flotation cell2 In Table I are given the results of flotation experiments using several different fatty acids dissolved in nitrobenzene.

Jan 1, 1943

By Robert A. Haney, Stephen J. Gigliotti, James L. Banfield

A series of investigations were made by the Mine Safety and Health Administration to evaluate the performance of various face ventilation systems as part of a program to reduce frictional ignitions of methane and to develop face ventilation systems that could be used with the line brattice more than 10 feet from the face. Tests were conducted in a full-scale laboratory model of a face area. Systems tested included unassisted blowing and exhaust line brattice, diffuser fan and spray fan systems. Systems were evaluated at air quantities ranging from 1.4 to 7.0 m3/s (3,000 to 15,000 cfm), and brattice-to-face distances from 1.5 to 9 meters (5 to 30 feet.). Tests were designed so that systems could be evaluated for the location of the high-point methane concentration in the face area, methane dilution capacity, and face ventilation index. The methane dilution capacity is the total amount of methane a system can dilute to 1.0 volume-percent. The face ventilation index is the efficiency at which the available face air volume is being used.

Jan 1, 1982

By William E. Bruce

This paper is intended to provide an improved understanding of natural draft (natural ventilating pressure) and the effect of natural draft on underground mine ventilation circuits. Attention is focused on measurement of natural draft pressures during ventilation surveys in mechanically ventilated mines and on different methods for modeling natural draft using the measured data. A number of examples are presented which utilize data collected during absolute air pressure surveys made by personnel of the Ventilation Division of the Mine Safety and Health Administration's Safety and Health Technology Center, Denver, Colorado. Examples are used to illustrate how the data from absolute air pressure surveys may be interpreted to determine whether natural draft pressure is present and what its magnitude is. In addition, two different methods are described for mathematically estimating the magnitude of the natural draft pressure. Comparisons are made of results obtained using the different methods. Different procedures are described for modeling natural draft using the MSHA-modified Penn State computer program. Use of the routines is described and illustrated relative to drafts that aid or oppose the mechanical ventilation system. Tabulations of results facilitate comparison of outcomes obtained using the different modeling procedures.

Jan 1, 1982

By J. C. Bartlett

(Read at the Wilkes-Barre Meeting, May, 1877.) 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 refitting they only corroborate. It is well known that a sphere of galena 1/8 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, falling or rising together, or remaining in suspension. Mr. Krom, to show that these

Jan 1, 1878

By H. I. Smith

The technical and safety press have devoted much space in support of or in opposition to the use of booster and auxiliary fans in coal mines. The Mine Safety Board of the U. S. Bureau of Mines has given the matter consideration, and the Mine Ventilation Committee of the A. I. M. E. is now seeking a discussion of the merits and demerits of such fans to guide it in formulating recommendations. In this paper I will set up some principles on which I believe most engineers will agree and from which we may work toward a decision, though as to what that decision shall be there may be a difference in opinion. Before stating the points on which I believe there is accord, I will distinguish between booster and auxiliary fans. Definition of Booster and Auxiliary Fans In discussing underground fans G. S. Rice1 distinguishes between those used to increase the amount of air passing a given point and those used to augment the ventilation locally. He describes a booster fan as one which is installed to handle the entire air current passing a given

Jan 1, 1927

By J. F. Shea, O. F. Tangel

Battelle Memorial Institute participated in a program for the General Services Administration aimed at developing a nickel-cobalt separation process that could be integrated in the Nicaro nickel plant. At the time the programwas being carried out, the Nicaro process was a straight-through operation, in which the ore was reduced and leached, after which the pregnant solution was boiled to produce a so-called "bulk precipitate" which contained virtually all of the nickel and cobalt which had been dissolved in the leaching step. The weight ratio of nickel to cobalt in Nicaro ore is approximately 15 to 20:l. The weight ratio of nickel to cobalt in the finished product had to be 100:l or higher to meet specifications. Because the Nicaro process embodied no nickel-cobalt separation step, the only way that a bulk precipitate of the specified nicke1:cobalt ratio could be produced was to so adjust roasting and leaching conditions that nickel would be selectively leached and most of the cobalt would be rejected with the tailings. The required selectivity, however, was achieved at the expense of nickel recovery, which was 5 or more per cent less than might have been obtained with the existing equipment, utilities, man power, etc., had selectivity been no object. The over-all purpose of the program was to develop a separation step that could be fitted into or onto the Nicaro facilities and which would permit the manufacture of a product that would meet the desired specifications and still permit the recovery of a maximum amount of nickel. Battelle suggested that this might be accomplished by reprocessing off-specification bulk precipitate and specifically suggested the process based on ammonium sulphate leaching followed by hydrogen reduction of the leach solution according to techniques developed commercially by Sherritt Gordon Mines Limited. Such a process would not only satisfy the objectives of the research but would present two additional advantages. (1) It would produce a separate cobalt product which could be further processed into metal, alloys, oxides, or salts. (2) It would yield nickel in metallic form which might be more generally marketable and command a slightly higher price per unit of nickel than the Nicaro oxide product. DESCRIPTION OF THE PROCESS Figure 1 is a flowsheet of the process. The essential features are: (1) Extraction of about 97 per cent of the nickel and about 85 per cent of the cobalt from bulk precipitate by a principal leach with ainmonium sulphate solution (Step A). Extraction of virtually all of

Jan 1, 1961

By Edwin A. Zink, Gerald P. Zink, John E. Wolgamott

Recent advances in high-pressure water technology can be effectively employed in underground mining. The new equipment is based on standard industrial water cleaning hardware and is compatible with conventional mining techniques. Three viable applications are addressed: rock drilling, hole notching, and rock bolting. Highlights of test results are presented that were obtained in several underground mines during the last two years of development work.

Jan 1, 1982

By A. C. Backeberg

There is no South African code for the design of reinforced concrete headframes, and all those erected have been designed on a uniform basis which, up to the present, has tended to be conservative. With certain exceptions designs have generally conformed with British Standard Code of Practice C.P. 114. In the design of reinforced concrete headframes the following loads are taken into account:

Jan 11, 1961

By Ben B. Sweet

The ongoing controversy over mining and agricultural use of ground water in Arizona underscores the importance of this commodity to both industries. Although the principles presented in this article are fundamental, a method of systematic data collection and interpretation is provided for evaluating a water well by a set of uniform standards common to all areas where ground water is a primary source of supply.

Jan 8, 1978

By W. H. Bassett

W H. BASSETT was elected first vice-president at . the executive session of the new Board on Tues- day afternoon. Karl Eilers, H. Foster Bain, Thomas T. Read, and H. A. Maloney were respectively re-elected as treasurer, secretary, assistant secretary and assistant treasurer. The new Executive Committee will consist of W. H. Bassett, Chairman, and Richard Peters, Jr., H. C. Bellinger, E. De Golyer, Edgar Rickard. The Finance Committee will be J. V. W. Reynders, Chair- man, Henry Krumb and H. G. Moulton. George D. Barron was reappointed Chairman of the Admissions Committee, and F. Julius Fohs put in charge of the Papers and Publications Committee.

Jan 1, 1929

By J. Nagy, D. W. Mitchell, E. M. Murphy

In 1957 research was initiated in the U.S. Bureau of Mines experimental coal mine near Pittsburgh, Pa., to study factors affecting foam generation and transport, to evaluate the effectiveness of high-expansion foam for controlling mine fires, and to develop techniques for applying the method under U.S. mining conditions. These investigations showed that high-expansion foam containing at least 0.2 oz of water per cu ft of foam is effective in controlling experimental underground fires burning coal, wood, and oil. Sometimes the fire was completely extinguished, but more often, it was brought under sufficient control to permit either a direct attack on the fire with a stream of water or loading of the hot material into cars. A progress report' prepared in July 1958 summarized the initial achievements of the USBM experiments. Since then other phases of the foam-plug method for attacking fires have been studied in the laboratory and in the mine. Previous studies by British engineers' of the foam-plug method for fighting mine fires indicated that high-expansion foam was effective in controlling experimental timber fires in an underground passageway. Their subsequent workx-1 pertained to the practical aspects of fighting large fires within a mining area with a foam-plug. CONTROLLING EXPERIMENTAL FIRES In the USBM tests foam was formed by spraying a dilute solution of a foaming agent on a metal or cotton net of 1/8 to 1/4-in. mesh. Air passing through the continuously wetted net forms bubbles of 1/2 to 11/2-in. diam and produces a honeycomb of foam that fills the passageway. Under the ventilating-air pressure, this light-weight plug moves forward through the passageways, around sharp corners, and over obstacles. as illustrated in Fig. 1. High-expansion foam was transported to a wood fire, an oil fire, and 13 coal fires. Figs. 3 and 4 show a typical coal fire before and after attack with foam. In 12 of the 15 experiments the fire was brought under control when the water content of foam was 0.2 oz or more per cu ft. A fire was considered controlled when the flames were quenched and observers could cross the area without wearing breathing apparatus or protective clothing. In the other three experiments, conducted when the water content was less than 0.2 oz per cu ft of foam, the flames were retarded but the fire was not controlled. Coal fires have been attacked successfully by foam introduced at points varying from 155 to 1010 ft from the fire. The time of burning in coal beds 10 in. thick ranged from 11/2 to 5 hrs or more. Most of the experimental fire beds were 15 ft in length. However, in one experiment a floor fire 25 ft long and 5 ft wide was constructed $5 upwind from another fire 15 ft in length; in another instance, the fire was 100 ft long and 5 ft wide. Foam was applied to the fires for periods ranging from 7 to 36 min. The time required for foam application depends on the extent of the fire, time of burning, water content of foam, foam velocity, and degree of fire control desired. In addition to the coal fires, foam was transported to a fire covering 45 sq ft, produced by 15 gal of oil burning in metal trays on the floor. The foam extinguished the oil fire in about 1 min. In one other test, the burning of 1100 lb of dry sawmill slabs stacked in open cribs 4 ft high and 16 ft long was brought under control by foam in 2 min. Composition of Gases in Return Air: In several of the experiments samples of the return air from fire zones were collected; composition of the atmosphere before, during, and after foam application was then determined. Because of condensation in the relatively cool sampling tube, the amount of water vapor was not determined. Analyses showed that concentration of carbon dioxide and combustible gases increased as the foam began passing over the fire. This resulted from the decrease in the volume of air when foam generation started and from the formation of gases when water reached the fire.* The quantity of gases generated would not be greater than that from an equivalent amount of water applied directly to the fire. The highest total concentration of combustibles (CO, CH1, and H2 mixture) obtained during the experiment was about 2 pct; this occurred 6 min after foam reached the fire. This atmosphere was nonex-plosive, but calculations show that if the air flow were reduced to about 5 fpm and if the rate of gas liberation from the fire remained constant, the mixture would be explosive. The use of foam on a fire in all probability would affect the normal ventilation of a mine. If the mine is gassy, this factor must be carefully considered before the foam is applied. APPLICATION OF THE FOAM-PLUG TECHNIQUE IN MINES Equipment and procedures for applying the foam-plug methods must be adapted to the prevailing conditions at a particular mine. Some factors to be considered in developing equipment are: size or extent of the mine, dimensions and number of entries, ventilation system, mining methods, haulage facilities, availability of water, amount of methane liberated, and existing fire-control apparatus. • In most experiments the initial air velocity of 200 fpm decreased to 50 to 100 fpm as the foam plug increased In length.

Jan 1, 1961

By J. B. Clark

In multiphase ternary diffusion studies, plots of the variation bf the composition on the isotherm constitutes one of the most effective methods of presenting experimental results, especially if such plots are made in a manner which relates the composition path on the isotherm with the diffusion layer structure in the couple. Unfortunately, if different conventions for plotting are used serious misinterpretations occur readily, causing apparent disagreement between investigators who actually share the same viewpoint. A common convention for mapping these diffusion paths is needed at this time because with the increasing use of the electron-probe X-ray microanalyzer, a much greater number of ternary diffusion studies can be expected in the near future. In an effort to prevent unnecessary confusion in the future litera- ture, a convention for these plots is proposed, as outlined below. A hypothetical example of the use of these conventions is given in Fig. 1 where the path of composition through the diffusion structure of the 100 pct A/50 pct B, 50 pct C couple is plotted on the appropriate isotherm of the ABC system. The lower case letters relate the region in the diffusion layer structure to the appropriate composition on the ternary isotherm. 1) The diffusion path is plotted on the isothermal section corresponding to the diffusion temperature of the couple. 2) The terminal compositions of the plotted diffusion path are the initial compositions of the couple halves—provided infinite boundary conditions are maintained. If, in either couple half, infinite conditions are not maintained, then the path terminates at the composition of the exterior surface of the couple. If, at this surface, the composition varies with time or if the plotted path is time dependent, then the diffusion time should be noted beside the plotted path. 3) A solid line crossing a single phase field (e.g., line a-b in Fig. 1) denotes an existing layer of that phase in the diffused couple. 4) A dashed line crossing a two-phase field parallel to the tie lines (e.g., line g-h) represents an interface between the two phases with interfacial compositions designated by the ends of the tie-line. The line represents no spatial extent. 5) A solid line crossing a two-phase field so as to cut tie lines (e.g., line b-c or line j-k) represents a locally equilibrated columnar two-phase layer. The solid line should cut those tie lines which correspond to the lateral interfacial equilibria along the columnar

Jan 1, 1963

By Charles W. Merrill

IF we follow the threads of the mining problems, upon which I have touched, we find them all leading to one great fundamental desideratum. The people of this State, of this Nation, and of this world must be brought to a better understanding of the basic nature of our industry-must be made more mineral-minded. It is my belief 'that there is not a man present among this earnest gathering of those interested in the mining industry, who has not a deep-seated and heartfelt desire that the existing unprecedented welfare and prosperity of the whole mass of American people be maintained not merely through our own generation but through the generations of our children and their children. In the decades to come there can be no question of the keenness of the foreign competition which we are doomed to meet, and in this great international contest that Nation which has the best balanced program of development and that broadness of vision in its governmental direction, which recognizes the necessity of a sympathetic attitude toward the upbuilding of such a broad pro- gram will be the Nation which will maintain and pre- serve that welfare of all of its people.

Jan 1, 1929

By Michael Epstein, Daniel E. Rosner

Fume nucleation sufficiently close to vaporizing suvfaces can augment net vaporization rates into cooler environments. Environmental conditions favoring large vaporization rate enhancements are briefly discussed and a previous theoretical treatment of this nucleation phenomenon is generalized to account for the self-regulating effect of condensalion-heat release within the boundary layer. Despite kinetic limitations on homogeneous nucleation, and latent heat release, non-diffusive condensate removal processes appear to make possible large enhancements in steady-state vaporization rates, provided surface temperatures are well below the boiling point. When condensed phases vaporize (or dissolve) into cooler media, the diffusion-limited mass loss rate can be strongly influenced by the process of nucleation/con-densation (or precipitation) within the thermal boundary layer. This condensation process (which typically leads to mists or fumes in the case of evaporation into cooler gases) has the effect of steepening the vapor pressure profiles near the evaporating surface, since the condensation zone acts as a vapor sink. However. the resulting enhancement in the diffusion-limited evaporation rate can be estimated (as first done by Turkdogan1 for the case of molten iron/nickel alloys evaporating into helium) only if one has independent knowledge of the critical supersaturation, sCrit(T), required to homogeneously nucleate the vapor.* In a recent reformulation and generalization of the theoretical model of Ref. 1 it has been shown that, when log sCrit is approximately linear in reciprocal temperature, rather simple expressions can be derived4 for the ratio of the actual rate of vaporization j" to either the minimum (no condensation) rate j"min, or the maximum (equilibrium condensation) rate j"max In the present communication we wish to briefly report on further developments and implications of the formulation of Ref. 4, with emphasis on i) environmental conditions favoring large enhancements in vaporization rate, and ii) the self-regulatory influence of condensation heat release (neglected in Refs. 1 to 4) on predicted vaporization rates. Additionally, we take this opportunity to correct several misprints appear- ing in Ref. 4, and comment on Elenbaas's recent criticism5 of Ref. 1. MAXIMUM POSSIBLE VAPORIZATION RATE IN PRESENCE OF CONDENSATION A nonequilibrium theory is of interest because of the very large difference between the minimum (no condensation) and maximum (equilibrium condensation) vaporization rate. The magnitude of this maximum possible enhancement can be shown quite clearly by combining a result of Refs. 3 and 4 with the fact that for most liquids there is a simple relationship between the molar heat of evaporation, A, and its boiling point, i.e., A/(RTBp) = C, where the constant C, often called the Trouton ratio, takes on values not very different from 11.* More generally, for any substance (including The Trouton ratio (which for water is 13, for methane, 10, and so forth) will be recognized as the ratio of the molar entropy change upon vaporization (at TBP or Ttransf) to the unlversal gas constant R. Its near constancy reflects the fact that the change in atomic order upon vaporization depends only weakly on the kinds of molecules involved. those that sublime under ordinary conditions) we can define a characteristic transformation temperature. Ttransf, by a relation of the form Ttransf =A/(CR), and then examine the maximum possible evaporation rates as a function of how far removed from Ttransf are the surface temperature, Tw, and ambient temperature, T. Subject to the assumptions: 1) equilibrium vapor pressure, pv,eq, everywhere small compared to prevailing total pressure, p, and 2) negligible effect of condensation heat on temperature profile, the maximum enhancement ratio was found (Eq. [17], Ref. 4) to be: where, for most vapors, Nu/NuD (the ratio of heat transfer coefficient to mass transfer coefficient for the same configuration) is a number near unity.* Ex- *An alternative derivation of the Nu = NuD special case of this equation. revealing its validity for arbitrary velocity/temperature profiles in a laminar boundary layer, is given in Ref. 3. amining this result for a "Trouton substance", one obtains the results shown in Fig. 1, constructed for C = 11. Since we are concerned with vaporization enhancements (j'max/J"min > 1) at surface temperatures below Ttransf, this area of interest is shown unshaded. One notes that at a fixed ambient temperature (hence, T/TtranSf) there is a unique surface temperature, 2T , at which j"max/j"min attains its peak value; moreover, the peak enhancement ratio, see dashed locus. Fig. 1, is: (NuA/NuD)(C/4)(Ttransf/T,). Hence, if Nu = NuD, when the ambient temperature is less than 1/4 of TtranSf the peak enhancement exceeds the Trouton

Jan 1, 1969

By W. H. Smith

IN connection with some recent work on the effect of impurities on the ductility of chromium, it appeared desirable to know the solid solubility of carbon in chromium. A literature survey indicated that this information was not available. Although considerable work has been done on the Cr-C phase diagram,&apos;.&apos; previous investigators have been more concerned with the structure and phase boundaries of the carbide phases than with the terminal solid solution. The phase diagram shown in Fig. 1 is taken from the work of Bloom and Grant&apos; and represents the most recent determination. As indicated by the dashed line, the a solid-solubility limit was not determined. Experimental Procedure Alloys of chromium were prepared from hydrogen-treated and vacuum-degassed electrolytic chromium plus spectrographic grade carbon. The oxygen and nitrogen content of the alloys was <0.002 pct. After melting, analysis of the alloys showed them to contain 0.02, 0.08, 0.15, and 0.55 pct C. Pieces of the alloys were heated in a protective atmosphere to various temperatures and then quenched after holding for a time sufficient to insure equilibrium. Microscopic examination of the as-quenched alloys for the presence of a second phase was used as a measure of the solubility limit. The heats were made in a multiple hearth arc-furnace using a zirconium-gettered static argon atmosphere. A zirconium melt was made before each Cr-C heat. Triple melting was used to insure ingot homogeneity as shown by microscopic examination. The alloys were prepared by adding portions of a 4.5 pct C-Cr master alloy to high purity chromium. The carbon contents listed previously were those obtained by analysis. The nitrogen and oxygen contents after arc melting were both <0.002 pct. Sections 1/8X1/4X1/2 in. were cut from the 100-g ingots and a hole drilled in one end in order to suspend the sample from a molybdenum wire. After the surface was carefully cleaned, a sample of each melt was hung in a mullite tube heated externally by a platinum resistance furnace connected to a vacuum system. The lower portion of the mullite tube was sealed to Pyrex and closed off several inches below the furnace. This was filled with sili-cone oil kept cold by circulating cold water around the outside of the Pyrex. Quenching into the oil bath was achieved by melting a fuse wire supporting the sample. It required about 4 sec for the sample to cool from 1400" to 600°C. This severity of quench was considered satisfactory to freeze-in the high temperature equilibrium. For tests made at temperatures of 900" to 1200°C, heating was done in vacuum; for tests above 1200°C, an argon atmosphere was used. The holding time employed ranged from 12 hr at 900°C to 6 hr at 1400°C. Experiments were performed at temperatures of 900°, 1000°, 1100°, 1200°, 1300°, and 1400°C. Microscopic examination for evidence of a second phase was done at X1500. Experimental Result The microstructures of a 0.08 pct C-Cr alloy as-cast and after quenching from 1300°C are shown in Figs. 2 and 3. A 0.15 pct C-Cr alloy quenched from 1300°C is shown in Fig. 4. The data obtained from the quenching experiments is shown graphically in Fig. 5. If the Van&apos;t Hoff equation is obeyed, a plot on a logarithmic scale of the mol fraction of solute vs the reciprocal of the absolute temperature should give a straight line. For dilute solutions the weight percentage can be substituted for the mol fraction without introducing any appreciable error. The Van&apos;t Hoff equation can then be written as where H is the heat of solution in calories per mol. The slope of the straight line on the log pct C vs 1/T plot gives the value of AH. Assuming that the Van&apos;t Hoff equation is obeyed, which is probably justified for the dilute solution of carbon in chromium, the heavy straight line shown on Fig. 5 represents the best fit of the data. This line was obtained as follows. On Fig. 5 the results of the microscopic examination of all alloys following quenching were plotted and designated as to whether one or two phases were seen. Below 1100°C all alloys showed a second phase on quenching. The heavy vertical lines shown in Fig. 5 therefore represent the possible range of the ter-

Jan 1, 1958

By S. A. Lever, R. Hultgren

The solidus is usually the least satisfactorily determined portion of a phase diagram. Cooling curves, which succeed well with the liquidus, show the solidus inaccurately or not at all because of segregation which occurs during freezing. Heating curves of carefully homogenized alloys might be expected to indicate accurately the solidus, but they are seldom used. Dynamic methods involving heating or cooling are never completely satisfactory because of uncertainty as to whether equilibrium is attained. A static method in which the specimen may be allowed hours, days, or even weeks to attain equilibrium is to be preferred. In a static method a solid solution, for example, is first made thoroughly homogeneous, then heated to successively higher temperatures. After sufficient time at each temperature to assure equilibrium, some property is measured which should alter strikingly when melting begins. Microscopic examination can be used to detect the beginning of melting, but the method is tedious since the specimen must be quenched, sectioned, polished, and etched before each examination. Of all the physical properties which change on melting, electrical resistance is probably the most satisfactory to measure. The measurement may be made while the specimen is at temperature without damage to the specimen. It may be repeated indefinitely to ascertain when equilibrium has been achieved. Measurements may be made on a single specimen over the whole range of temperature. Most metals approximately double their resistance on melting. Since an accuracy of a few tenths of a percent is easy to achieve, the method is highly sensitive to the beginning of melting. In spite of these advantages, which have been perceived for a long time,l,2 a reasonable search of the literature has failed to reveal a single case in which the method has been satisfactorily applied in practice to the determination of solidus temperatures. The use of electrical resistance measurements appears to have been confined in practice to changes in the solid state. In the work described in the following pages we have applied the electrical resistance method to the solidus of the lead-tin system. We have found the method to be convenient, reproducible, and highly sensitive. We chose the lead-tin system because it leads to few technical difficulties. Furthermore, a number of determinations of solidus have been made in this system by various methods and results could be checked against them. However, all published results are not in good agreement with one another, so this work should help in determining the solidus more precisely. The Lead-tin Diagram Because of its commercial importance, there have been numerous investigations of the lead-tin diagram. The results of the most recent work on the solidus are indicated in Fig 7, as well as the results of the present work. The works of Honda and Abe3 and of Stockdale4 agree fairly well with each other and with the present work. Jeffery&apos;s5 data indicate the solidus to be about 50°C lower. Honda and Abe3 used differential thermal analysis on both heating and cooling cycles. Stockdale4 used the microscopic method and also differential heating curves. Stockdale&apos;s results were about 4" higher than those of Honda and Abe at low tin contents and lower at higher tin contents. These results also agree with those of Rosen-hain and Tucker.= Jeffery5 used electrical resistance measurements of the alloy as it was being heated or cooled. Apparently he did not attain equilibrium as his results are about 40°C lower than those of Stockdale4 or Honda and Abe.3 MATERIALS AND METHODS The lead and tin used were of high purity. They were supplied by the American Smelting and Refining Co., who gave the following analyses: Lead: silver, 0.0016 oz per ton; copper, 0.0008 pct; cadmium, 0.0007 pct; zinc, 0.0002 pct; arsenic, 0.0003 pct; antimony, 0.0002 pct; bismuth, 0.0005 pct; tin, 0.0001 pct; iron, 0.0020 pct; lead (by difference), 99.995 pct. Tin: antimony, 0.037 pct; arsenic, 0.020 pct; bismuth, 0.004 pct; cadmium, trace; copper, 0.025 pct; iron, 0.004 pct; lead, 0.020 pct; nickel and cobalt, 0.005 pct; silver, 0.0005 pct; sulphur, 0.005 pct; tin (by .-difference). 99.88 pct. One hundred grams of metal with the desired proportions of lead and tin was weighed out to the nearest one-tenth of a milligram. The mixture was placed in a silica crucible, covered with charcoal, and melted in a reducing atmosphere in a gas-fired furnace. The alloy was well stirred. Chemical analysis of two of the alloys checked closely with the weighed portions. The compositions of the remainder of the alloys were taken directly from the weighings, without chemical analysis.

Jan 1, 1950