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By A. English, M. J. Greaves

This paper is a discussion of pelletizing systems developed over the last 15 to 20 years for the agglomeration of fine iron ore concentrates. Five different pelletizing systems are now in commercial use in the U.S., and for the purposes of comparison, estimated operating costs and capital costs for the construction of four of them are included. Capacities of existing commercial plants are examined, together with the anticipated capabilities of plants presently being built or projected. In just 21 years, the art of pelletizing iron ore concentrates has reached maturity with mastery of the separation of finely divided concentrates from low-grade iron ores and their agglomeration into pellets containing about 65% iron. This accomplishment has firmly established an improved feed for the blast furnace, with resulting benefits in faster reduction of burdens and greater economy of operation. The present production capacity of pelletizing facilities in the U.S. is about 20 million tons annually, and it is expected to double by 1970. The rapid expansion of pelletizing in the U. S. has been closely observed in European countries, notably in Sweden and Germany, where pioneer agglomerating techniques were developed early in this century. PELLETIZING PLANTS AND PROCESSES Twelve commercial pelletizing plants are presently in operation in the U. S. and Canada. An equal number are in various stages of engineering and construction, and many others are being considered. The pelletizing systems currently employed include shaft furnaces, horizontal grates using three different airflow arrangements, and grate kilns. The capacity of pelletizing operations in North America is shown in Table I. All of these plants are integrated with the mine, the ore-crushing facilities and the concentrating plant and are equipped with storage and loading-out facilities for the product. Normally, a pelletizing plant is composed of a shuttle conveyor above the receiving bins; balling equipment; a heat-hardening system including the necessary auxiliaries such as furnaces, burners and controls, ducts, fans, meters and instrumentation; fines recovery equipment; and product handling equipment. Also included are the necessary auxiliaries and utilities such as boilers or power plant; oil unloading and storage facilities; coal unloading storage, grinding and distribution facilities; and bentonite or other additive storage and distribution equipment. Shaft Furnaces: Vertical shaft furnaces used in this country are limited to the treatment of natural magnetite concentrates containing minor quantities of residual fluxing elements. Fig. 1 shows a perspective view of the shaft furnace with balling, feeding and pellet-handling equipment. An elevation of a shaft furnace is shown in Fig. 2. A commercial shaft furnace unit is about 45 ft in height with a 6 x 14-ft rectangular cross section and has a nominal production rate of approximately 50 gross tons of pellets per hour. The upper portion of the furnace shaft is constructed of fire brick as protection from the high process temperatures involved. The lower portion of the shaft is lined with abrasion-resistant brick to withstand erosion from the fired pellets. Rectangular-shaped, refractory-lined and insulated combustion chambers are situated on each side of the shaft furnace. Oil or gas is burned to produce high temperature gases which are forced into the furnace through ports located near the top of the combustion chambers. The shaft furnaces operate at a pressure of approximately 6 psi. Pellets are fed into the top of the furnace by a pantographic feeder designed to produce the desired pellet stockline. The furnace is kept filled at all times and pellets are fed and discharged from the furnace at the same rate. In early development, 10 to 12 lb of solid fuel was incorporated in the pellets. However, the main source of process heat is now derived from the combustion chamber gases. In some instances no solid fuel is used. The pellet movement in the shaft furnace is counter-current to the flow of gases. Ambient air is introduced through louvers at the lower end of the furnace, at about 6 psi, cooling the fired pellets and supplementing the heat of the high temperature gases from the combustion chamber ports. The zone of maximum temperature, located above the ports of the combus-

Jan 1, 1963

By H. M. Otte, A. G. Crocker

SLIP, twinning, stacking faults, and precipitates on well-defined planes in a crystal produce traces that are visible on either a polished or an etched surface. The purpose of this note is to establish the usefulness and limitations of the information obtained from such traces when determining the orientation of single crystals or grains in a polycrystal. Attention will be confined specifically to traces produced by octahedral planes in cubic crystals, though most of the remarks can be taken as more generally valid. The problem of determining the crystal orientation is completely solved in principle' and in particular for the special case under consideration.1'2 Tables are available3 in which the orientations can simply be looked up when given the two or three angles between the traces. Thus a quick and simple method is available for obtaining the orientation of a crystal from surface traces. In this note two examples will be given from recently published papers and will show the use of the method with the aid of the Tables, as well as some of the precautions that should be taken in the procedure. As part of an analysis of X-ray Kossel lines, Peters and Ogilvie 4 determined from them the crystallographic orientation of the specimen. They chose a Cu-5.10 wt pct Si alloy that had been partly transformed from the a (fee) phase to the k (hcp) phase. The latter formed as very straight platelets along the octahedral planes of the a phase, and a photograph (Fig. 7 of Ref. 4) was reproduced in the paper4 of the region for which the orientation had been determined from the Kossel lines. Apart from a very small area (about 0.15 mm diam) near the top center of the photograph, the region shown was clearly all of one orientation. Traces in four different directions were readily identified. Starting with the smallest angle and proceeding counterclockwise, the angles between the traces were measured to be 27° 43', 55° 16', 64 3 43 1, and32"26'. These add up to 1802 08 1, indicating a cumulative error of 8'. The correct values should, of course, be taken from the original glass plates, or at least from prints on distortion-free paper, so the precision of the quoted values is actually greater than their accuracy. The solutions can be looked up in the Tables3 in four ways, depending on how the angles are paired, tion for the minutes of arc is required and the solution obtained will be identical for all the four pairs if the values of the angles are not in error. In a practical situation, such as this one, there are several sources of error, so that the four solutions obtained will all be slightly different. An arithmetic average of the four solutions is mathematically incorrect, but may, in special cases, give an answer close to the correct one. A rigorous procedure for refining the orientation has been described by Mackenzie;5 he gives a least-squares method that can be applied, if necessary, to this type of problem. The orientation thus determined can be compared with the one from the Kosel lines and discrepancies larger than the experimental error assigned to nonor thogonality of the X-ray or electron beam to the specimen. Here the example will only be used to illustrate the general procedure for making a very rapid rough check. From measurements on the stereographic projection, Fig. 9 of the paper,4 we can determine that the surface normal is approximately (0.434, 0.704, 0.562). From the Tables3 we find, using 28°, 55" as a good approximation to the first pair (27°43', 55°16'), that the surface normal is (0.453, 0.678, 0.579).* These two values are within 2 deg of each

Jan 1, 1967

By C. O. Lee, R. H. Feierabend, Z. W. Bartlett

DESPITE the fact that American brimstone production has increased 2 times since the prewar period 1935-1939, the demand for sulphur exceeds the supply. To alleviate this situation efforts are being made to increase the production of sulphur and bring the shortage to an end. The most important developments are being undertaken on the Gulf Coast. One new brimstone mine has been put into operation and three others are being developed. These projects are expected to account for a large part of the additional sulphur production now anticipated for the free world.'.' Except for a small amount of byproduct sulphur from sour natural gas and refinery gases, American brimstone is produced by the same process devised by Frasch 60 years ago, consisting essentially of the injection of superheated water at about 325°F into sulphur-bearing formations through wells which are drilled from the surface by standard oilfield methods. Sulphur deposits vary in depth from a few hundred feet to 2500 ft from the surface; in a typical deposit the sulphur occurs as crystalline aggregates in porous limestone and gypsum in concentrations varying from 5 to 40 pct, the thickness of the formation ranging from a few feet to several hundred.3 The deposits are usually surrounded by formations impermeable to the flow of hot water, the top and sides being enclosed by impermeable sediments and the bottom by dense impermeable anhydrite. As the hot water leaves the well bore, it percolates through the formation and transmits its heat to the rock and sulphur. When the sulphur reaches 240°F it melts, separates from the rock, and flows through the hot channels downward to the bottom of the well. Here it is freed from incoming water and from formation water, which saturates the porous rock, by gravity separation, liquid sulphur being 1.8 times as heavy as water. It then is pumped to the surface in a relatively pure state, 99.5 pct or better. Chief contaminants are organic impurities, such as petroleum residues, which are soluble in sulphur and tend to discolor it.' Sixteen deposits of commercial magnitude have been discovered in the Gulf Coast area. Five of these deposits have been depleted and abandoned with production totalling more than 26,886,000 tons. Eight properties are operating and have produced 65,875,-000 tons to Jan. 1, 1952, for a total Frasch-type production of 92,761,000 tons. Three new deposits are under development. Aforementioned deposits are listed in Table I. Each of these deposits has been found in the cap-rock overlying shallow intrusive salt plugs or domes and buried in several hundred to as much as 2500 ft of sediments. All salt domes do .not contain sulphur; only 16 sulphur deposits have been found in a total of 231 salt domes which are known to exist in the Gulf Coastal states of Texas, Louisiana, Mississippi, and Alabama. Ten of the salt domes lie in the Gulf of Mexico offshore from the Texas and Louisiana coasts. Additional offshore domes may be found, but their value as a sulphur potential is questionable owing to the great hazard and high cost that can be visualized at these exposed locations where depths of water reach 50 ft. Marsh operations of Freeport Sulphur Co. are in the southeast section of Louisiana. In general, the country is low, flat, relatively uninhabited marshland broken by many shallow lakes and bayous which extend for irregular distances inland. Geologically, the coastal area is of sedimentary origin, having been built up gradually under the sea by deposition of material carried down by large streams to their deltas. Offshore bars were formed enclosing

Jan 1, 1953

By C. O. Lee, Z. W. Bartlett, R. H. Feierabend

DESPITE the fact that American brimstone production has increased 2 times since the prewar period 1935-1939, the demand for sulphur exceeds the supply. To alleviate this situation efforts are being made to increase the production of sulphur and bring the shortage to an end. The most important developments are being undertaken on the Gulf Coast. One new brimstone mine has been put into operation and three others are being developed. These projects are expected to account for a large part of the additional sulphur production now anticipated for the free world.'.' Except for a small amount of byproduct sulphur from sour natural gas and refinery gases, American brimstone is produced by the same process devised by Frasch 60 years ago, consisting essentially of the injection of superheated water at about 325°F into sulphur-bearing formations through wells which are drilled from the surface by standard oilfield methods. Sulphur deposits vary in depth from a few hundred feet to 2500 ft from the surface; in a typical deposit the sulphur occurs as crystalline aggregates in porous limestone and gypsum in concentrations varying from 5 to 40 pct, the thickness of the formation ranging from a few feet to several hundred.3 The deposits are usually surrounded by formations impermeable to the flow of hot water, the top and sides being enclosed by impermeable sediments and the bottom by dense impermeable anhydrite. As the hot water leaves the well bore, it percolates through the formation and transmits its heat to the rock and sulphur. When the sulphur reaches 240°F it melts, separates from the rock, and flows through the hot channels downward to the bottom of the well. Here it is freed from incoming water and from formation water, which saturates the porous rock, by gravity separation, liquid sulphur being 1.8 times as heavy as water. It then is pumped to the surface in a relatively pure state, 99.5 pct or better. Chief contaminants are organic impurities, such as petroleum residues, which are soluble in sulphur and tend to discolor it.' Sixteen deposits of commercial magnitude have been discovered in the Gulf Coast area. Five of these deposits have been depleted and abandoned with production totalling more than 26,886,000 tons. Eight properties are operating and have produced 65,875,-000 tons to Jan. 1, 1952, for a total Frasch-type production of 92,761,000 tons. Three new deposits are under development. Aforementioned deposits are listed in Table I. Each of these deposits has been found in the cap-rock overlying shallow intrusive salt plugs or domes and buried in several hundred to as much as 2500 ft of sediments. All salt domes do .not contain sulphur; only 16 sulphur deposits have been found in a total of 231 salt domes which are known to exist in the Gulf Coastal states of Texas, Louisiana, Mississippi, and Alabama. Ten of the salt domes lie in the Gulf of Mexico offshore from the Texas and Louisiana coasts. Additional offshore domes may be found, but their value as a sulphur potential is questionable owing to the great hazard and high cost that can be visualized at these exposed locations where depths of water reach 50 ft. Marsh operations of Freeport Sulphur Co. are in the southeast section of Louisiana. In general, the country is low, flat, relatively uninhabited marshland broken by many shallow lakes and bayous which extend for irregular distances inland. Geologically, the coastal area is of sedimentary origin, having been built up gradually under the sea by deposition of material carried down by large streams to their deltas. Offshore bars were formed enclosing

Jan 1, 1953

By C. O. Lee, Z. W. Bartlett, R. H. Feierabend

DESPITE the fact that American brimstone production has increased 2 ½ times since the prewar period 1935-1939, the demand for sulphur exceeds the supply. To alleviate this situation efforts are being made to increase the production of sulphur and bring the shortage to an end. The most important developments are being undertaken on the Gulf Coast. One new brimstone mine has been put into operation and three others are being developed. These projects are expected to account for a large part of the additional sulphur production now anticipated for the free world.1,2 Except for a small amount of byproduct sulphur from sour natural gas and refinery gases, American brimstone is produced by the same process devised by Frasch 60 years ago, consisting essentially of the injection of superheated water at about 325°F into sulphur-bearing formations through wells which are drilled from the surface by standard oilfield methods. Sulphur deposits vary in depth from a few hundred feet to 2500 ft from the surface; in a typical deposit the sulphur occurs as crystalline aggregates in porous limestone and gypsum in concentrations varying from 5 to 40 pct, the thickness of the formation ranging from a few feet to several hundred.3 The deposits are usually surrounded by formations impermeable to the flow of hot water, the top and sides being enclosed by impermeable sediments and the bottom by dense impermeable anhydrite. As the hot water leaves the well bore, it percolates through the formation and transmits its heat to the rock and sulphur. When the sulphur reaches 240°F it melts, separates from the rock, and flows through the hot channels downward to the bottom of the well. Here it is freed from incoming water and from formation water, which saturates the porous rock, by gravity separation, liquid sulphur being 1.8 times as heavy as water. It then is pumped to the surface in a relatively pure state, 99.5 pct or better. Chief contaminants are organic impurities, such as petroleum residues, which are soluble in sulphur and tend to discolor it.4 Sixteen deposits of commercial magnitude have been discovered in the Gulf Coast area. Five of these deposits have been depleted and abandoned with production totalling more than 26,886,000 tons. Eight properties are operating and have produced 65,875,000 tons to Jan. 1, 1952, for a total Frasch-type production of 92,761,000 tons. Three new deposits are under development. Aforementioned deposits are listed in Table I. Each of these deposits has been found in the caprock overlying shallow intrusive salt plugs or domes and buried in several hundred to as much as 2500 ft of sediments. All salt domes do not contain sulphur; only 16 sulphur deposits have been found in a total of 231 salt domes which are known to exist in the Gulf Coastal states of Texas, Louisiana, Mississippi, and Alabama. Ten of the salt domes lie in the Gulf of Mexico offshore from the Texas and Louisiana coasts. Additional offshore domes may be found, but their value as a sulphur potential is questionable owing to the great hazard and high cost that can be visualized at these exposed locations where depths of water reach 50 ft. Marsh operations of Freeport Sulphur Co. are in the southeast section of Louisiana. In general, the country is low, flat, relatively uninhabited marshland broken by many shallow lakes and bayous which extend for irregular distances inland. Geologically, the coastal area is of sedimentary origin, having been built up gradually under the sea by deposition of material carried down by large streams to their deltas. Offshore bars were formed enclosing

Jan 1, 1952

By M. A. Grossman

The harden ability of most steels can be predicted within 10 to I5 per cent provided the complete chemical composition is known, including "incidental" elements; and provided the as-quenched grain size is known; and provided, finally, that the composition and heating temperatures for hardening are such as to result in austenite free from carbide particles. In the method proposed herein, the steel is considered as having a base hardenability due to its carbon content alone (the hardenability of a "pure steel" of the given carbon content, without any other elements), and this base hardenability is multiplied by a multiplying factor for each chemical element present. After multiplying all these together, the final product is the hardenability. Grain size may be taken into account either in the base hardenability or after the multiplication. Hardenability is stated in terms of "ideal critical diameter", namely, the diameter of bar, in inches, that will just harden all the way through (absence of un-hardened core) in an "ideal" quench, and the calculation may also be related to the Jominy test The data bring out certain features rather clearly. For example: i. It is quite useless to attempt to predict hardenability unless all elements, including "incidentals,,) are known; thus an "incidental,, chromium content of 0.20 per cent increases the hardenability by about 50 per cent. 2. The relative effectiveness of different alloys is sometimes unexpected; thus molybdenum when calculated in this way appears to be of the same order of effectiveness as manganese, rather than much more powerful, as would appear to be common experience; observe that an increase from no manaanese to 0.20 per cent Mn provides a multiplying factor of 1.67, and an increase from no molybdenum to 0.20 per cent Mo provides a factor of 1.63, an increase of over 60 per cent in each case. However, if to a steel containing 0.50 per cent Mn there is added "20 points of manganese," the factor is raised from 2.65 (for 0.50 per cent Mn) to 3.35 (for 0.70 per cent Mn), or an increase of only 26 per cent. Thus the fist small addition of an element has a much more powerful percentage effect than an equal further addition when some is already present, and in most cases the effect of molybdenum is considered in relation to a steel in which molybdenum is absent. 3. If two elements are equally effective, a greater hardenability will be obtained by using, for example, 0.5 per cent of each than by using I.o per cent of either of them alone. 4. A knowledge of the as-quenched grain size is essential for precise work, since a difference of only one grain size number (say No. 7 instead of No. 6) makes a difference of almost 10 per cent in hardenability (in these units); this, however, does not apply to certain It should be emphasized that in chromium steels (over 0.30 per cent Cr) and chrome-molybdenum and chrome-vanadium steels, un-dissolved carbides are likely to be present in the steel as quenched, and that in such cases the charts can indicate only a maximum Passible hardenability, whereas the extent of hardening actually obtained may be much less. Thus tests on a number of chrome-molybdenum steels have indicated a degree of hardening amounting to only 50 to 65 per cent of the maximum possible, and in chromium steels from full hardening (100 per cent) down to as low as 70 per cent. On the other hand, when the amount of such elements is small (Cr under 0.30 per cent, Mo up to 0.25 per cent in the

Jan 1, 1942

By M. A. Grossman

The harden ability of most steels can be predicted within 10 to I5 per cent provided the complete chemical composition is known, including "incidental" elements; and provided the as-quenched grain size is known; and provided, finally, that the composition and heating temperatures for hardening are such as to result in austenite free from carbide particles. In the method proposed herein, the steel is considered as having a base hardenability due to its carbon content alone (the hardenability of a "pure steel" of the given carbon content, without any other elements), and this base hardenability is multiplied by a multiplying factor for each chemical element present. After multiplying all these together, the final product is the hardenability. Grain size may be taken into account either in the base hardenability or after the multiplication. Hardenability is stated in terms of "ideal critical diameter", namely, the diameter of bar, in inches, that will just harden all the way through (absence of un-hardened core) in an "ideal" quench, and the calculation may also be related to the Jominy test The data bring out certain features rather clearly. For example: i. It is quite useless to attempt to predict hardenability unless all elements, including "incidentals,,) are known; thus an "incidental,, chromium content of 0.20 per cent increases the hardenability by about 50 per cent. 2. The relative effectiveness of different alloys is sometimes unexpected; thus molybdenum when calculated in this way appears to be of the same order of effectiveness as manganese, rather than much more powerful, as would appear to be common experience; observe that an increase from no manaanese to 0.20 per cent Mn provides a multiplying factor of 1.67, and an increase from no molybdenum to 0.20 per cent Mo provides a factor of 1.63, an increase of over 60 per cent in each case. However, if to a steel containing 0.50 per cent Mn there is added "20 points of manganese," the factor is raised from 2.65 (for 0.50 per cent Mn) to 3.35 (for 0.70 per cent Mn), or an increase of only 26 per cent. Thus the fist small addition of an element has a much more powerful percentage effect than an equal further addition when some is already present, and in most cases the effect of molybdenum is considered in relation to a steel in which molybdenum is absent. 3. If two elements are equally effective, a greater hardenability will be obtained by using, for example, 0.5 per cent of each than by using I.o per cent of either of them alone. 4. A knowledge of the as-quenched grain size is essential for precise work, since a difference of only one grain size number (say No. 7 instead of No. 6) makes a difference of almost 10 per cent in hardenability (in these units); this, however, does not apply to certain It should be emphasized that in chromium steels (over 0.30 per cent Cr) and chrome-molybdenum and chrome-vanadium steels, un-dissolved carbides are likely to be present in the steel as quenched, and that in such cases the charts can indicate only a maximum Passible hardenability, whereas the extent of hardening actually obtained may be much less. Thus tests on a number of chrome-molybdenum steels have indicated a degree of hardening amounting to only 50 to 65 per cent of the maximum possible, and in chromium steels from full hardening (100 per cent) down to as low as 70 per cent. On the other hand, when the amount of such elements is small (Cr under 0.30 per cent, Mo up to 0.25 per cent in the

Jan 1, 1942

By Nestor Torres-Acuña, Fathi Habashi

Metallic copper of purity equal to commercial electrolytic copper is deposited during the anodic dissolution of technically available white metal, Cu2S, in m acidic solution of' copper(II) sulfate as electrolyte and copper sheets as cathodes. The process may be applied on commercial scale since it has the advantage of by passing the converting and poling steps, decreasing pollution problems due to SO, and recovering the sulfur of the white metal in the elemental form. The anodic dissolution is believed to take place in three steps: The working conditions that lead to 98 pct cathodic current efficiency are: 30 gpl Cu2+ and 100 gpl H2SO4 in electrolyte, current density 1.0 amp per sq dm, and tetnperature of bath 40°C'. DURING the smelting of copper, nickel, lead, and zinc sulfide ores, large amounts of sulfur dioxide are produced. Because the release of this gas in the atmosphere causes pollution problems, many attempts were made in the past for its recovery either in liquified form or processed to sulfuric acid. Although these two forms of sulfur are the usual forms that are consumed by the chemical and metallurgical industries, their storage and transport usually raise economic problems. It was realized, long ago, that a process by which sulfur can be recovered directly in the elemental form would be most attractive. Elemental sulfur is easily stored and transported, and is readily converted to SO2, H2S, or H2SO4 when needed. Processes aimed to recover the metals from their sulfide ores, and at the same time by-product sulfur in the elemental form, were recently reviewed.' As early as 1882, Marchese2 patented a process in which a matte having the composition: Cu 15, Pb 14, Fe 41, and S 25 pct was electrolyzed. According to cohen3 the process was applied on a pilot scale by the Aktiengesellschaft fur Bergbau-, Blei-, und Zinkhiitten-betriebe at Stolberg, Rheinland, Germany. The process was unsuccessful, however, owing to the contamination of the electrolyte during electrolysis. Studies in this field were reported by Bernfeld4 and Egli.5 Borchers et a1.6-8 developed the process further by using white metal (Cu 78.2 pct, S 19.6 pct) instead of the matte, and a pilot plant was operated by the Mansfeldschen Kupferschiefer Co. at Eisleben, German~.~ It appears, however, that the process never went into commercial operation. Further studies in this direction were carried out by Russian workers.10-23 The International Nickel Co. of Canada erected a pilot plant at Port Colborne in 1951 to apply the process to nickel matte which is essentially pure nickel sulfide."'- 26 Full-scale plant went into operation at the Thompson Refinery in Manitoba in 1964.27 In this method nickel sulfide matte is melted and cast into anodes analyzing 76 pct Ni and 20 pct S with small amounts of copper, cobalt, and iron. These anodes are then electrolyzed in an aqueous solution of NiS04 at pH 4. Further work on this method was reported in the literature.28-31 In this paper, experiments on the anodic dissolution of white metal in aqueous copper sulfate solution are reported. EXPERIMENTAL White metal, Table I, obtained from The Anaconda Co., was cast in form of anodes 10 by 7.5 by 1 cm, Fig. 1. The anodes are mechanically strong and do not break easily; when polished they gave a shiny gray metallic appearance. From the chemical composition shown in Table I, it can be seen that the atomic ratio Cu:S corresponds approximately to the formula CU2.06S. The copper in excess to the formula Cu2S is most probably present as a separate phase since metallic copper could be seen under the microscope, Fig. 2. Fig. 3 shows the X-ray diffraction pattern of white metal which matches fairly well with that of reagent-grade Cu2S.

Jan 1, 1969

By A. E. Zawadzki

A progress report is presented on the development of a process for the removal of sulfur dioxide from flue gases. Catalytic oxidation of the sulfur dioxide in flue gases, with the production of recoverable sulfuric acid, has been demonstrated to be technically feasible. Problems associated with the process are discussed. The need for an inexpensive and efficient process for controlling sulfur dioxide emissions from utility plant stacks has been accentuated by the ever-increasing public demand for elimination of all man-made air pollutants. I would like to describe the results of an investigation of the development of such a process; more important, I would like to present a discussion of the problems associated with the process which remain to be solved. The research work on the BCR catalytic gas phase oxidation process has been jointly sponsored by the Association of Edison Illuminating Cos., Edison Electric Inst. and Bituminous Coal Research, Inc., since 1958. However, work on SO2-pollution abatement was initiated by BCR in 1953. Tieman and Clymer,1 working with ozone and simulated flue gases, evaluated a gas phase oxidation process for removing SO2 from flue gases. Their experimental data indicated that the use of ozone to oxidize SO2 in flue gas concentrations, with subsequent recovery of H2SO4, did not appear to be economical due to the large ratio of ozone to sulfuric acid produced (2.6 to 1). The cost of the ozone would be 6 to 10 times the cost of sulfuric acid produced. As a result of the ozone study, work on a catalytic oxidation process was developed. The following reactions are the basis for the catalytic oxidation process Reaction [I] normally occurs in the combustion of sulfur-bearing fuels. At the high temperature found in the combustion chamber, 95% to 99% of the sulfur in the fuel is oxidized to SO2 and 1% to 5% is oxidized to SO3. The concentration of SO2 in the combustion gases depends on the combustion efficiency and the quantity of excess air used. A commonly used rule of thumb is 0.1 percent by volume SO2 in the flue gas for each 1% sulfur in the fuel. Reaction [2] proceeds at a wide range of temperatures. The rate of the reaction is rapid above l,000°F; however, the equilibrium conversion drops rapidly above this temperature. 2 Reaction [3] occurs rapidly to completion at temperatures below 400°F; above this temperature some SO3 exists in equilibrium with H2SO4. Complete dissociation of H2SO4 occurs above 650°F.3 The simplicity of the proposed process provided added incentive to the development and evaluation of the various component unit operations. The advantages of the process were considered to be as follows: 1) no raw materials were required, 2) the unit operations were not radically new; and 3) a salable product, sulfuric acid, would be produced. The successful development of the process was contingent upon the solution of several major problems: 1) The development of a catalyst which would provide high catalytic activity at reasonable conditions of gas flow and temperature without causing an unacceptable increase in pressure drop. 2) The development of a high temperature dust collection system to provide clean flue gases to the catalytic reactor. 3) The complete recovery of the sulfuric acid produced in the process; the effluent gas must contain less than 20 ppm by volume of sulfuric acid. As of this date, the complete solution to these problems has not been achieved. EXPERIMENTAL Catalyst Development: The use of platinum and vanadium catalysts for the production of sulfuric acid by the treatment of dry gases containing 5% to 20% by volume sulfur dioxide has been known for many years. The application of the basic idea of catalytic oxidation of sulfur dioxide in flue gas concentrations was

Jan 1, 1965

By G. Sandoz, D. A. Meyn

The fracture surfaces of specimens of titanium a1loys which exhibited susceptibility to subcritical crack growth in a wide variety of environments, including aqueous solutions, alcohols, hydrocarbon gases, carbm tetrachloride, and dry air, were examined. The dominant and characteristic fracture mode was cleavage. which became mixed with an increasing porportion of ductile fracture modes (dimples. and so forth) as the applied KI was increased. The cleavage plane in all the alloys was oriented at 15 deg from (0001) of the a phase. No indices could be assigned to the 15 deg cleavage Plane because of uncertainty as to which zone it belonged to. SLOW crack growth and delayed fracture take place in certain titanium alloys at stress intensity (KI) lower than the critical values for complete fracture (KIc) found in short-time tests for plane strain fracture toughness.' Such crack growth may take place in very dry air on sustained loading if the alloy contains a sufficient amount of hydrogen and if the stress intensity factor is higher than a threshold value designated KIH.2 Similarly, a number of environments such as water, alcohols, and hydrocarbons may cause slow crack growth provided the stress intensity factor exceeds the threshold value KISCC. In this paper it is intended to examine some fracto-graphic and crystallographic details of this subcritical crack propagation process as related to alloy composition, environment, and stress intensity. It has been previously reported that subcritical crack growth takes place in titanium alloys in aqueous environments by cleavage.2"6 The observations to be described here indicate that in the alloys investigated the mode of subcritical crack propagation is more dependent on the stress intensity during cracking than on the environment. The fracture mode is illustrated with photographs of the fracture surfaces at a wide range of magnifications. The crystallographic character of the cleavage mode is also presented and the results discussed. EXPERIMENTAL APPROACH The studies were made on four titanium alloys— Ti-8A1-1Mo-lV, Ti-5A1-2.5Sn, Ti-7Al-1Mo-lV, and Ti-0.350. Of these four alloys the first two were mill annealed and fine grained. The latter two were noncommercial and coarse grained, having been prepared for other experimental purposes. The crystallographic studies required a large-grain size. Consequently the fine-grained alloys were an- nealed in a vacuum at 1950°F and furnace cooled to produce samples for these studies. This treatment did not alter the microstructure significantly except for grain size. All the aluminum-containing alloys showed primary a with a network of ß-phase particles within the a grains; Figs. 1 and 2 show this microstructure for the specific case of fine-grained Ti-8A1-1Mo-1V. The cracks in the figures will be discussed later. Fractographic studies were made on all the alloys, but the electron fractographs displayed herein are from the Ti-8A1-1Mo-1V alloy in the fine-grained condition. Emphasis was placed on this commercial alloy because considerable information was available on the stress-corrosion cracking characteristics in a variety of environments. Sufficient supplementary studies of the alloy after the anneal to produce large grains were conducted to establish that the stress-corrosion cracking susceptibility and fractographic characteristics were not changed significantly. Thus it could be inferred that the crystallographic data obtained exclusively on large-grained specimens would apply also to fine-grained specimens. Fracture surfaces for study were obtained using precracked cantilever beam specimens loaded as described by Brown. The precracked section of a specimen was immersed in the environment of interest. Values of initial stress intensity factor Kli were chosen slightly higher than KISCC in order to obtain a fairly extensive region of slow crack growth. Fracture surfaces representative of a variety of stress intensity levels could then be examined because in the cantilever beam test KI increases as the crack propagates.

Jan 1, 1970

By Bernard S. Borie

THE U-A1 binary system has been studied by Kaufmann and Gordon.' They have shown that three intermetallic compounds occur in the system: UAl², UAl², and a third compound tentatively identified as UA15. UA1³ is simple cubic, a, = 4.26A. Its unit cell contains one formula weight, and it is iso-morphous with AuCu³. UA1² is face-centered cubic, a, = 7.72A, with eight formula weights per unit cell. Rundle and Wilson have shown that it is iso-morphous with Cu²Mg.² A Debye-Scherrer pattern of the Al-rich compound indicated a more complex structure than either UA1² or UA1³. The following is a report of an investigation of the crystal structure of this compound and a determination of its stoi-chiometric formula. A melt of uranium (99.9 pct pure) and aluminum (99.9 pct pure) was prepared which contained about 25 pct U by weight. It was cooled from 950" to 650°C at a rate of 500" per hr and then taken from the furnace and air cooled. An X-ray diffraction pattern of the ingot showed only lines of aluminum and the Al-rich compound. Filings from the ingot were reacted with a solution of sodium hydroxide, producing a fine black powder, the diffraction pattern of which showed no traces of aluminum. A comparison of the Debye-Scherrer pattern of our sample with the data published by Kaufmann and Gordon1 showed that it is identical with the Al-rich phase which they reported. Single crystals were obtained by cooling the melt more slowly (about 50°C per hr). After reaction with sodium hydroxide, the crystals appeared as small black needles attached to the ingot surface. Cell Size, Space Group, and Uranium Positions A series of Weissenberg photographs for rotation about two of the crystallographic axes, taken with copper radiation filtered through nickel foil, revealed an orthorhombic cell of dimensions: a = 4.41 ± 0.02A b = 6.27 ± 0.02A c = 13.71 ± 0.03A Reflections of the type hkl were observed only if: h + k + I = 2n, of the type hkO only if: h = 2n and k = 2n, of the type h01 only if: h + 1 = 2n, and of the type Okl only if: k + 1=2n. Hence, the cell is body-centered with an 001 glide plane. The evidence for the existence of the glide plane is the observed extinction of 23 possible re- flections of the type hkO with at least one index odd. There are only two space groups consistent with these data: C"" — I2ma and D28 2h — Imma.³ he possible sets of atomic positions for these space groups are: 12ma: (0 0 0; ½ ½ ½) + 4: (a) x 0 %; x % % (b) x ¼ z; x ¾ Z 8: (c) x y z; x y z; x, ½ + y, Z x, M - y, z Imma: (0 0 0; ½ ½ ½) + 4: (a) 0 0 0; 0 ½ 0 (b) 0 0 ½; 0 ½ ½ (c) ¼ ¼ ¼; ¾ ¼ ¼ (d) ¼ ¾ ¾ ; ¾ ¾ % (e) 0 ¾ Z; 0 ¾ z 8: (f) x 0 0; x 0 0; x 1/2 0; x ½ 0 (g) ¼ Y ¼; ¾ Y ¾; ¾ y ¼; 1 y ¼ (h) 0 y z; 0; ;; 0, ½ + y, z; 0, l/2 - Y, Z (i) x 1/4 z; x ¾ z; ¼ z; x ¾ z 16: (j) xy z; x y z; x y z; x y z; x, ½ + y, Z; x,½ - y, z; x, ½ - y, z; 11 1, + y,Z Though density measurements on different samples were found to vary somewhat, they were all within the range 5.7 * 0.3 g per cu cm. If it is assumed that the unit cell contains four formula weights of UAl,, it is 6.5 g per cu cm. If there were as many as eight uranium atoms per unit cell, the

Jan 1, 1952

By AIME AIME

NAPOLEON'S dictum that an Army travels on its stomach has not changed in this present war, but the things an Army's stomach calls for would be more than strange to Napoleon. Today one of the main articles of diet for the mechanized army is oil and gasoline, and the chief and most efficient source of 'apply overland is the pipe line. It was a flexible 4-in. pipe line that supplied the voracious appetite of tanks, trucks, jeeps, and planes across the North African desert. and it is the 1800-mile pipe line from Calcutta to Kunming, Yunnan Province in China, the longest in the world, that supplied oil and 100-octane gas for the trucks, tanks, Jeeps, and planes fighting on the Assam-Burma-China front in recent months. Completion of this approximately 1800-mile pipe line to China over rivers that had never been bridged, over hill that towered 9000 ft., and over swamps

Jan 1, 1945

By Edwin B. Eckel

This paper, based on brief field examination and on data supplied by the operators, records the condition of the Italian mercury industry as of March 1945, not long after Italy's collapse. Except for the once-Italian but now Yugoslavian Idria mine near Trieste, virtually all the known mercury deposits are in the Monte Amiata district in Siena and Grosseto Provinces, 75 miles north of Rome. This district contains the Abbadia San Salvatore. the Siele. the Argus, and the Cerreto Piano mines besides numerous prospects and unproductive mines. Under pressure from Germany the principal mines were highly productive during the early part of the war, but production fell off long before its end. All of the mines were damaged in some way at the German withdrawal but by September 1944 the Abbadia had resumed production and several others were only lacking power by the early spring of 1945. The Monte Amiata district is characterized geologically by a thick series of sedimentary rocks that range from Triassic to Eocene in age . and are surmounted on Monte Amiata itself by a thick cap of extrusive trachyte. Bodies of travertine and of landslide detritus, younger than the trachyte, are rather widespread. The structure is complex and little known but most of the ore deposits seem to lie along or near a major, north-trending fault or on associated cross-fractures. Cinnabar is the only important ore mineral and clay minerals are by far the most abundant products of hydrothermal alteration. A southward increase in the amount of stibnite, relative to cinnabar, suggests horizontal zoning. The grade of ore ranges from 0.60 to 3.0 Pet and the reserves, as compared with those in American mines, are enormous. Even in the face of war-time scarcities, the mines are remarkably self-sufficient and labor is plentiful, but the costs of production are estimated to be not greatly below those of the better American mines. Notes on the principal mines, on the mining and metallurgical methods, and on the manufacture of synthetic cinnabar are included in the paper. Introduction With but few brief interludes, Spain and Italy, including the Idria mine near Trieste, which has passed from Austrian to Italian to Yugoslavian hands in the Past 3 decades, have led the world in the production of mercury, or quicksilver, for many centuries. Despite their enviable position with respect to the supplies of a metal so essential in both war and peace, there is a notable lack of up-to-date information in America on the mercury industry of either country. Duschak and Schuette' and Schuettez,3 give by far the best summaries in English known to the writer, but the latest firsthand report cited by them on the Italian mines was published in 1915.' Having been deeply interested in the geology and economics of mercury for several years, the writer naturally felt most fortunate in being the to obtain enough firsthand information on the Italian industry to fill at least a few of the gaps in our knowledge. The opportunity came during the war, soon after this industry, together with the rest of Italy, had capitulated to the Allies. Many of the facts presented here are thus definitely "dated," but others are of less transitory nature, and even the dated facts should be of interest in showing the strength and

Jan 1, 1949

By Edwin B. Eckel

This paper, based on brief field examination and on data supplied by the operators, records the condition of the Italian mercury industry as of March 1945, not long after Italy's collapse. Except for the once-Italian but now Yugoslavian Idria mine near Trieste, virtually all the known mercury deposits are in the Monte Amiata district in Siena and Grosseto Provinces, 75 miles north of Rome. This district contains the Abbadia San Salvatore. the Siele. the Argus, and the Cerreto Piano mines besides numerous prospects and unproductive mines. Under pressure from Germany the principal mines were highly productive during the early part of the war, but production fell off long before its end. All of the mines were damaged in some way at the German withdrawal but by September 1944 the Abbadia had resumed production and several others were only lacking power by the early spring of 1945. The Monte Amiata district is characterized geologically by a thick series of sedimentary rocks that range from Triassic to Eocene in age . and are surmounted on Monte Amiata itself by a thick cap of extrusive trachyte. Bodies of travertine and of landslide detritus, younger than the trachyte, are rather widespread. The structure is complex and little known but most of the ore deposits seem to lie along or near a major, north-trending fault or on associated cross-fractures. Cinnabar is the only important ore mineral and clay minerals are by far the most abundant products of hydrothermal alteration. A southward increase in the amount of stibnite, relative to cinnabar, suggests horizontal zoning. The grade of ore ranges from 0.60 to 3.0 Pet and the reserves, as compared with those in American mines, are enormous. Even in the face of war-time scarcities, the mines are remarkably self-sufficient and labor is plentiful, but the costs of production are estimated to be not greatly below those of the better American mines. Notes on the principal mines, on the mining and metallurgical methods, and on the manufacture of synthetic cinnabar are included in the paper. Introduction With but few brief interludes, Spain and Italy, including the Idria mine near Trieste, which has passed from Austrian to Italian to Yugoslavian hands in the Past 3 decades, have led the world in the production of mercury, or quicksilver, for many centuries. Despite their enviable position with respect to the supplies of a metal so essential in both war and peace, there is a notable lack of up-to-date information in America on the mercury industry of either country. Duschak and Schuette' and Schuettez,3 give by far the best summaries in English known to the writer, but the latest firsthand report cited by them on the Italian mines was published in 1915.' Having been deeply interested in the geology and economics of mercury for several years, the writer naturally felt most fortunate in being the to obtain enough firsthand information on the Italian industry to fill at least a few of the gaps in our knowledge. The opportunity came during the war, soon after this industry, together with the rest of Italy, had capitulated to the Allies. Many of the facts presented here are thus definitely "dated," but others are of less transitory nature, and even the dated facts should be of interest in showing the strength and

Jan 1, 1949

By Charles W. Henderson

THE influence of mineral production on the development of the western United States has been profound. From 1848 to 1860, there was only gold production, the effect of silver began in 1860, and from then on both had a powerful influence. Lead production started in 1863, copper in 1863, and zinc in 1885, but was small until 1898. Gold alone was therefore the stimulus of the early settlement and exploration of the Western States.. But mineral deposits caused neither acquisition of territory nor determination of boundary lines. Arizona, California, Nevada, New Mexico, and parts of Utah, Wyoming, and Colorado were formally acquired from Mexico fourteen days after the actual date of the discovery (January 19, 1848)1.2 of gold at Sutters Mill, near the present town of Coloma, California (a discovery which, with the immediate new discoveries, aroused the world several months later) ; but the acquisition was by treaty (under negotiation for some time but signed February 2, 1848)3 in settlement of a war involving the boundaries of the grassy plains of Texas, an area at that time not known to contain any metals, and to date found to have but few metal deposits.4 The international boundary at 49º latitude for the far northwest states was determined by causes other than mineral deposits.

Jan 1, 1933

By Kenneth K. Humphreys, Joseph W. Leonard, Robert L. Llewellyn, William C. McCulloch

INTRODUCTION The particular field of application of machines utilizing air currents as the primary separating medium is in the cleaning of the fine sizes of bituminous coal. Approximately 25,400,000 tons of bituminous coal were cleaned by air machines during 1965. They have not found any application for cleaning anthracite. Since the development and introduction of the first successful commercial pneumatic oscillating machine for cleaning bituminous coal in 19 16, by the Sutton, Steele and Steele Co, Dallas, Texas, and the American Coal Cleaning Corporation, formerly of Welch, W. Va., seven other successful pneumatic coal-cleaning machines have been developed and introduced to the American coal-mining industry: 1. Peale Davis: "Pneumo-Gravity" machine. 2. Arms "Concentrator," oscillating table. 3. Hey1 and Patterson oscillating table. 4. "Stump Air-Flow," pulsating air jig. 5. "Super Airflow," pulsating air jig. 6. Ridge air jig. 7. Phillip air jig. While not all coals can be beneficiated by air washing, the air washing of coals that are easy to clean can be readily proved advantageous. Of all the preparation methods, pneumatic cleaning is the most acceptable from the standpoint of delivered Btu cost. This is based on the premise that a percent of moisture is just as detrimental as a percent of ash. The principle of dry concentration has never been determined with scientific accuracy. To the present time the study has been more of an art than a science. It is possible to forecast the results of wet concentration from a study of the washability characteristics of the raw coal but only after applying rule-of-thumb methods of interpretation to the specific gravity and size distribution can it be ascertained that the raw coal is amenable to dry concentration. Air as a separating medium dates back to biblical times as exemplified in the winnowing of chaff from the grain. However, the same application of air to coal serves merely to blow the dust away and size the remaining particles. Pulsating air was the solution to the problem and largely eliminated the necessity for close screen sizing which was required on early separators. Because of the low density of air, a medium of sufficient density has to be built with the material itself. Hence there must be some device to impart to the bed the necessary mobility for proper classification. Also, the

Jan 1, 1968

By G. E. Warner

This paper presents a review and analysis of a highly stratified Burbank sand waterflooding project in Osage County, Okla. Permeability values in this reservoir range from less than 0.1 md to nearly 3 darcys, and 90 percent of the permeability capacity is contained in approximately 26 percent of the reservoir volume. To date, the project has recovered 103 bbl/flood-acre-ft since waterflood initiation, which represents 50 percent of the total preflood cumulative and 12 percent of the original stock-tank oil in place (OSTOIP). The outstanding feature of this project has been the economical recovery of a sizable quantity of oil at water-oil ratios higher than those normally considered prohibitive. Nearly 70 percent of the recovery to date has been achieved at water-cut values greater than 95 percent. An ultimate waterflood recovery of 138 bbl/flood-acre-ft, or 67 percent of the preflood recovery and 16 percent of the OSTOIP, is predicted. The ultimate primary and secondary recovery will be 302 bbl/acre-ft and approximutely 40 percent of the OSTOIP. The actual performance is compared with the predicted performance by both the Stiles and the Dykstra-Parsons methods, and applicabiliry of these methods to this particular reservoir is evaluated. The performance of this project indicafes highly stratified reservoirs can be successfully and economically waterflooded when either reservoir or economic conditions preclude the use of mechanical and chemical means of mdbility control. Introduction The concept of the stratified reservoir has been used by reservoir engineers for many years to describe the vertical variations in permeability within a reservoir. Numerous techniques have been advanced to predict the expected waterflood performance of the stratified reservoir, and in most cases they prove reasonably accurate. The advisability of undertaking a prospective waterflooding project is determined, based on these predictions. This paper presents a review of a waterflood project in a highly stratified reservoir that normally would be considered a marginal prospect, at best, when evaluated with any prediction technique properly adjusted for reservoir conditions. This kind of project can be successful if the predictions are used to design a waterflooding system capable of economically recovering an oil cut of 1 to 2 percent. Experience gained in the early stages of the project's development was profitably applied in the later development of the entire reservoir and could prove beneficial to other projects with similar reservoir stratification or fracture characteristics. The East Burbank pool waterflooding operations have been developed in three separate stages, each of which has been a separate project: Mid-Burbank Unit, Flood A, and Stanley Waterflood. When referred to collectively, these projects will be called the Composite Project. The Skelly Oil Co.'s Barber lease — the only portion of the pool not included in the three projects — is operated as a separate facility with a cooperative injection-well agreement. It contains less than 80 productive acres and would not significantly affect the over-all performance picture.

Jan 1, 1969

By J. Murray Riddell, Grover J. Holt, Arthur E. Anderson

Out of the depths of each business cycle we emerge with a stimulus for greater efficiency and a realization of progress in industrial technique. The recent years have not been an exception to this rule, and in retrospect we sense that significant advances have been made in mining practices on the Mesabi Range, with emphasis on speed of production and economy of operation. A survey of such changes does not reveal anything that is fundamentally or basically new, but it is apparent that ideas and machines that have found wide application in industry elsewhere, with necessary modifications, are being put to productive use in mining iron ore. Innovations in transporting and conveying ore from the open pits stand out with greatest prominence, so that, in the main, it will be with these features that this paper will treat, in the review of progress made to this date. The late years have witnessed the development of small deposits for open-pit operation, the cleaning up of pits nearing exhaustion, and in two large operations the approach to the limit for haulage by steam locomotives, owing to grades, making it necessary to recover the ore in slopes, track benches and below the power-shovel limit by a milling and scram operation. For several years small standard-type dump trucks have been used in clean-up or scram operations within the pits, but during the season of 1936 the first effort was made to use heavy truck haulage in the transportation of stripping and iron ore. The new units in use today vary from 15 to 20 tons in capacity, and are equipped with powerful gasoline or Diesel engines and supplemented by trailers or wagons on rubber or crawler treads. The Diesel engine finds favor with most operators because of fuel economy. These units develop upward of 125 hp. in the 15-ton trucks. The speed of these trucks varies from 2 miles per hour in Pow gear to 35 in high gear. The transmission affords 12 speeds forward and 3 speeds in reverse.

Jan 1, 1940

By J. Murray Riddell, Arthur E. Anderson, Grover J. Holt

Out of the depths of each business cycle we emerge with a stimulus for greater efficiency and a realization of progress in industrial technique. The recent years have not been an exception to this rule, and in retrospect we sense that significant advances have been made in mining practices on the Mesabi Range, with emphasis on speed of production and economy of operation. A survey of such changes does not reveal anything that is fundamentally or basically new, but it is apparent that ideas and machines that have found wide application in industry elsewhere, with necessary modifications, are being put to productive use in mining iron ore. Innovations in transporting and conveying ore from the open pits stand out with greatest prominence, so that, in the main, it will be with these features that this paper will treat, in the review of progress made to this date. The late years have witnessed the development of small deposits for open-pit operation, the cleaning up of pits nearing exhaustion, and in two large operations the approach to the limit for haulage by steam locomotives, owing to grades, making it necessary to recover the ore in slopes, track benches and below the power-shovel limit by a milling and scram operation. For several years small standard-type dump trucks have been used in clean-up or scram operations within the pits, but during the season of 1936 the first effort was made to use heavy truck haulage in the transportation of stripping and iron ore. The new units in use today vary from 15 to 20 tons in capacity, and are equipped with powerful gasoline or Diesel engines and supplemented by trailers or wagons on rubber or crawler treads. The Diesel engine finds favor with most operators because of fuel economy. These units develop upward of 125 hp. in the 15-ton trucks. The speed of these trucks varies from 2 miles per hour in Pow gear to 35 in high gear. The transmission affords 12 speeds forward and 3 speeds in reverse.

Jan 1, 1940

By H. N. Treaftis, J. W. Cahn

THE previous determinations of the solvus of tin in solid lead disagree with one another by as much as 40°C or almost 10 at. pct. Even determinations that appear to be careful differ considerably in both the solubility and its temperature coefficient. Recent kinetic workl -3 on the rate of precipitation of tin from lead-tin alloys and thermodynamic work4 on the heat of solution of tin in lead have given some insight into the time necessary to reach equilibrium in this system. As this time is longer than that used in almost all previous determinations of the solvus, these determinations are questionable. Since the interpretation of recent kinetic results requires accurate values of the equilibrium solubility the present work was undertaken. DISCUSSION OF PREVIOUS RESULTS The methods used in previous studies may be placed into three classes: 1) Several alloys covering a range of compositions are allowed to reach "equilibrium" at a certain temperature.5-7 Some property, such as the X-ray lattice parameter of the lead-rich phase or the re- sistivity of the alloy, is then measured as a function of composition. The solubility limit for that temperature is taken to be that composition at which a discontinuity in the property occurs. However, the recent kinetic work has shown that tin precipitates in two stages. The first stage is rapid but leaves the lead still supersaturated. The second stage is very slow, and it seems from the equilibration times quoted by the investigators of the solvus that the end of the first stage of precipitation was usually mistaken for equilibrium. This is especially true at temperatures below 100°C where the first reaction is still quite rapid (from minutes to months), but where the second stage is so slow that very long holding times are required to reach equilibrium. Alternatively micrographic work8 on several alloys of different compositions seems to have given good results if done carefully. 2) The beginning of precipitation in a homogenized alloy is measured as it cools slowly8-10. Since reactions in solids undercool easily, such determinations will always give too low a temperature for the solvus. 3) Some property of an alloy is measured as a function of temperature while the alloy is above the solvus.5,9,11 The range of temperature can usually be extended slightly into the two phase region. Then the alloy is precipitated at a much lower temperature and slowly reheated. The solvus is taken to be the lowest temperature where the property of the reheated alloy is equal to that previously determined for the homogeneous alloy. Usually one also expects a discontinuity at the solvus in the temperature variation of the property for the reheated alloy. The difficulty in this method is the sluggishness of the dissolution process, and this method may give too high a solvus temperature. EXPERIMENTAL The phase boundary or solvus temperature was determined by a modification of method 3 for a series of chemically analyzed high-purity alloys, ranging from 5.1 to 26.4 at. pct Sn. The resistance, as a function of temperature, of a sample of homogenized alloy (which could easily be undercooled) was compared with the equilibrium resistance which that alloy sample attained after precipitation at room temperature followed by long isothermal anneals at various temperatures. Before each anneal the sample was rehomogenized and reprecipitated. The solvus temperature could be located to within 1°C as the intersection of the resistance vs temperature curves for the homogenized and equilibrium alloys. No attempt was made to locate the phase boundary more accurately since the limiting factor was the precision with which the alloys could be analyzed. This precision was ±0.1 wt pct Sn and corresponds to an error of 1 deg in temperature. This use of isothermal anneals differs from some of the previous investigations in which method 3 was used with baths of slowly rising temperatures. It was found early in the investigation that solvus temperatures tended to be high if the latter method was used even at extremely slow heating rates. For example a

Jan 1, 1961