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THE book covers principally the assaying of silver and gold and the determination of these values in ores, sweepings, and base metal. It seems to have been written more for the goldsmith and jeweler than for the primary producer of metals. There were approximately sixty different substances needed in the operations described and not over a dozen different types of raw material (ore, matte, crude or alloyed metal) are mentioned. The methods of separation used were essentially simple and reasonably reliable, though the processes were not sufficiently understood to permit the selection of the simplest effective ingredients, and there was a great tendency to employ complicated fluxes, with unnecessary repetition of long-continued heatings indicative of a leisurely pace of life. Practically all the processes described are based on a few chemical facts: the inability of gold to combine with sulphur, while silver and the base metals form easily fusible sulphides; the ready oxidation of base metals; and the ii- solubility of gold in nitric acid. Fluxes serve to make earthy impurities fusible, and to carry oxidizing or sulphurizing ingredients. Many of the processes of assaying had changed little up to the beginning of the present century. Even as late as 1924, when the writer took a University course in fire assaying, the crucibles, cupels, scorifiers, molds, and tongs were identical with those of the sixteenth century, though the wind furnace had a stack on it and the muffle for cupelling was gas-fired.* The fluxes were purer, but of the same essential composition. That this branch- or twig-of metallurgy had not advanced in any funda-

Jan 1, 1949

By T. S. Lundy, J. I. Federer

Chemically purified Zr95and Cb95 have been used in determining self-diffusion coefficients in the bcc phase of iodide zirconium over the temperature range of 900o to 1750°C. The temperature dependence of the diffusion coefficients could not be described by the usual Arrhenius-type equation over the entire temperature range. Values of the apparent frequency factors (D0)a and activation energies (Q)A for ZR95 varied from 4.8 x 10-6 to 2.5 x 10-2 sq cm per sec and 20,700 to 46,900 cal per mole, respectively, between 900°and 1750°C. Similarly, for Cb95, values of (Do) a and (Q)A varied from about 2.4 x 10'5 to 0.25 sq cm per sec and 26,500 to 56,800 cal per mole, respectively. The data may be described in terms of the a to ß transition temperature of 1136 °K and the absolute temperature of the diffusion anneals by the following eauations: SEVERAL studies on the diffusion of Zr95 in zirconium have been reported.1"5 The values of the constants contained in the usual Arrhenius-type equation for describing the temperature dependence of the diffusion coefficient, D = Do exp [- Q/(RT)], are summarized in Table I. The reported values of Do, the frequency factor, and Q, the activation energy, are seen to vary by factors of about 60 and 1.6, respectively. Examination of the data from any one study indicated reasonable consistency of measurements. The large discrepancies of over-all results, therefore, cannot be explained on the basis of experimental scatter. One possible explanation for the differences in results could be a varying impurity content of the zirconium. Another possibility is that the radioactive daughter, Cb95, influenced the values of some of the determined diffusion coefficients. Therefore, the first of the three purposes of this study was to reconcile the large differences in diffusion results that have been obtained. Several empirical relations have been proposed to relate the diffusion coefficients in solids with physical properties, such as the absolute melting point, the heat of fusion, and the heat of sublimation.

Jan 1, 1963

By W. E. Showalter

This paper discusses some of the results of combstion-drive tests which were made in a test cell using a sand bed 10 in. in diameter x 10-ft long. The test method is illustrated and described. The relationship between the API gravity of the in situ oil and the amount of air required for combustion drive is discussed in detail. Other things constant, the air requirement for combustion drive increases as the APl gravity of the in situ oil decreases. If the test results apply to actual reservoirs, the lowest-priced oils may cost the most to recover by this method. Information is shown which indicates that the effect of pressure on the amount of hydrocarbon burned is not large. A method of predicting air requirements from the API gravity of the in situ oil is presented. INTRODUCTION Combustion drive is the term used to identify the process of interstitial or in situ burning as an oil recovery method. Part of the in situ oil is burned to generate the energy needed to produce the remainder of the oil. Combustion drive as an oil recovery mechanism remains an economic uncertainty in spite of all the work that has been done by the industry in both laboratory and field?-6 This paper will show some of the results of tests which were made in a test cell for the purpose of studying the nature of the combustion-drive process. It will present data which indicate that the API gravity of the in situ oil is a significant indicator of the amount of air required to drive a burning front through oil sand. Air requirement varies inversely as the API gravity of the in situ oil. EXPERIMENTAL The tests were performed in a cell which utilized a cylindrical sand section 10 in. in diameter x 10-ft long. The thin-walled metal pipe which held the sand was wound with twenty external electrical resistance heaters which, by means of an automatic controller, maintained adjacent sections of the wall of the pipe at temperatures equal to the temperatures of the contained sand. Each heater covered 6 linear in. of the pipe. By this means lateral heat loss from the sand section was minimized, thereby causing the sand section to simulate more closely a horizontal increment of a combustion-drive reservoir. Fig. 1 shows a schematic diagram of the test assembly. Thermocouples to measure the temperature in the sand were located every 6 in. along the length of the sand section. The pipe containing the sand was enclosed in a cell designed for an operating pressure of 500 psig. The inlet air pressure was controlled at the inlet, and the gas flow rate was controlled and measured at the outlet of the cell. The oil sand used for the tests was prepared by mixing first water and then oil with the noncon-solidated sand using a closed mixer similar to a cement mixer. Table 1 shows a screen analysis of the sand. Ninety percent of the sand was 100 mesh or finer. This sand was a mixture of 80 per cent No. 120 Nevada White Sand and 20 per cent Tennessee Hi-Fusion Moulding Sand No. 3. The Nevada sand was a clean silica sand. The Tennessee sand con-

By CARLE R. HAYWARDC

BEFORE discussing this subject it is necessary to define somewhat the meaning of the tern metallurgical.. When I was a student at M. I. T. ore-dressing was not thought of as metallurgy in any sense of the word, but it was considered as more closely allied to mining, enabling the miner to market an otherwise unmarketable product, or at least to market it to better advantage. Progress in ore-dressing has gradually allied it more closely with smelting, for at present the raw material received by the smelter is predominantly concentrates and smelting practice has been profoundly affected by the products of the concentrating mill. It is not surprising therefore that in many schools ore-dressing is frankly considered as metallurgy and although there may be some dissenting opinions it will be considered as such in this discussion. Twenty-five years ago at M. I. T. metallography was taught in a few optional lectures. This subject has developed rapidly and been expanded into the new and increasingly important field of physical metallurgy. To many metallurgists the -term metallurgy means only physical metallurgy. They know little or nothing about smelting and leaching and even less about ore-dressing. Having then broadened the scope of the term metal¬lurgy to cover ore-dressing, smelting, leaching and phys-

Jan 1, 1930

By J. B. Dyess

TARNISH films on some of the common metals (particularly on copper and silver) have been of much scientific and commercial concern for a long time, but before the development of the electrical method1 of measuring film thicknesses there was no satisfactory quantitative approach by which to study the separate parts of these complex films. This method has been adapted to the measurement of duplex (cuprous-cupric) oxide films on copper .2 In the present work it has been used to measure tarnish films on copper when they were mixtures of cuprous oxide and cuprous sulphide, and also when they contained cuprous oxide, cupric oxide and cuprous sulphide, each component part being measured at a different potential value. Oxide-coated copper specimens, prepared by heating copper in air at chosen temperatures for given periods, were exposed to moist hydrogen. sulphide in air to form the various oxide-sulphide films studied. The comparative resistances afforded by (1) different thicknesses of oxide films, and also (2) equal thicknesses of oxide and sulphide films, against severe attacks of hydrogen sulphide were measured. The electrical method requires that the time be observed for the cathodic reduction of each part of the film substance, and these respective time values multiplied by the constant current give the corresponding quantities of electricity expended. Then each millicoulomb per square centimeter represents a film thickness of T= MX10 8 2D X 96,494 X 103 (a) where M is weight of oxide (or sulphide) giving one gram-atom of oxygen (or sulphur) for cathodic reduction, D is density of the oxide (or sulphide) and t is the thickness in Angström units per millicoulomb per square centimeter. The value of t for cuprous sulphide (cubical) is 14.27, and is obtained by substituting 5.78 for D and 159.20 for M in equation a. Previous values2 of t for cuprous and cupric oxides (12.36 and 6.39, respectively) were used in the present work.

Jan 1, 1939

By T. Egleston

AT the Dover meeting of the Institute, Mr. F. A. Canfield showed some of the members a machine which he had invented for dressing mineralogical and geological specimens, which he has since modified and brought to such a high state of perfection, that after having used it for several months in preparing specimens for the cabinet of the

Jan 1, 1876

By T. Egleston

At the Dover meeting of the Institute, Mr. F. A. Canfield showed some of the members a machine which he had invented for dressing mineralogical and geological specimens, which he has since modified and brought to such a high state of perfection, that after having used it for several months in preparing specimens for the cabinet of the

By Julius Pohlman

Considering the truly wonderful natural resources of the United States, and the variety and extent of uses for hydraulic cement at the present day, it seems strange that the manufacture of the artificial product called Portland cement has not been introduced here. Possibly the reason may be we have in different States of the Union rock deposits from which a cement can be obtained that is as good, and some claim even better, because of a more uniform quality, than the English product after it has been subjected to transportation across the ocean. One of these natural cement-rock deposits is found in the northern part of the city of Buffalo, and its manufacture has been carried on successfully for the past eleven years by the Buffalo Cement co., Mr. L. J. Bennett, President. The quarries cover an area of about two hundred acres, of which only twenty-five acres have been exhausted up to date; and the supply is assured for years to come. One acre yields on an average 80,000 barrels of cement; hence 12,000,000 barrels is a low estimate of what these quarries will yield before they are exhausted. According to the Geology of New York this cement-rock deposit is called the Water-Lime group, and forms in this section the uppermost member of the Upper Silurian. Its outcrop can be traced along the base of the second limestone terrace of Western New York, but at Buffalo a very large part of the overlying Corniferous limestone has been removed by natural agencies, leaving only about eight feet (six feet of rock and two feet of clay) on the top of the cement-rock, and thus furnishing the conditions for successful quarrying at a minimum expense. This rock is really an impure limestone, a mixture, as it were, of the underlying shales of the Onondaga Salt group with the overlying

Jan 1, 1889

E. T. DUMBLE, Houston, Tex.-This paper is a continuation of one that was published by Mr. Garfias, I believe, in the Journal of Geology, 1912, in which he gave the results of his investigations in Mexico, showing that the basalt extrusions frequently did not come up as cones. but reached the surface as a small neck and then mushroomed out into a sill, penetrating the beds both in limestones and in shales. He has continued his investigations to show that as these basalt protrusions came up they forced the strata into a funnel shape at the top instead of throwing them out altogether. While this may be true concerning these particular beds, there are other places at which the basalt does appear clearly as cones and dories, and there the funnel structure does not exist. We know that the sills are there, because we find them in the wells. In one well that I know of. we found a 2-ft. sill of basalt at about 1600 ft. and oil below it at about 2100 ft.; others have gone through similar beds. We also know that there. are cones, because north of the Ranuco River one well struck basalt at about 800 ft. and continued in it for several hundred feet-did not pass through it at all. This paper of Mr. Garfias will give us considerable help in that oil field. W. E. WRATHER, Wichita Falls, Tex.-I would like to ask for information as to the temperatures of Mexican oils. I have heard a number of conflicting reports about the high temperatures of the water and oil, and the relationship between them.

Jan 1, 1918

By Charles Camsell

MORE than one-third of all Canada is embraced in the federal domain known as the Northwest Territories. Its most northern point, Cape Columbia, on Ellesmere Island, is only 500 mi. from the Pole. It includes parts of the main physiographic divisions of the North American continent. In the West there is a strip of 30.000 sq. mi. lying in the Cordilleran region, where peaks in the Mackenzie Mountains rise as high as 8500 ft. East of this strip and extending roughly to a line through Great Bear and Great Slave lakes to the Arctic coast is a section of the interior plains. This section, known as the Mackenzie Lowlands, contains the great artery, the most striking feature of the Northwest Territories-the Mackenzie and Slave river waterway impressive in its width, almost two miles in places, and in it's navigability for 1357 miles without obstruction to the sea. Adjoining the Mackenzie Lowlands on the East is the greater portion of the mainland of the Territories, which, as well as a large share of the island area, is in the Canadian Shield.

Jan 1, 1937

By Robert S. Dewey

Drilling in West Texas during 1942 was substantially less than in the previous year. In all. 1267 Wells were drilled, as compared with 2325 wells in 1941. Of these 1267 wells, 1052 oil wells, 10 gas wells and 69 dry holes were drilled in proven fields and 36 oil wells, one gas well and 99 dry holes were wildcat operations. Of the 36 wildcat wells completed as oil producers, 16 led to new field discoveries, three found new productive horizons in old fields, and 17 extended the productive limits of established fields. Where semiwildcat drilling took place along established productive trends, there was often no sharp demarcation between wildcat wells that extend field limits and normal development to fulfil lease obligations, other than the arbitrary classification of a well as a wildcat if it was drilled at a distance of 2 miles from a producing oil well. The dry hole drilled on the edge of a field may have proved a more hazardous operation than a semiwildcat drilled several miles from production but favorably located on structure. The percentage of successful wildcatting ranges from 26.5 down to 14 per cent, dependent upon the degree of inclusion of the semiwildcat operations. Irrespective of which figure was used, the West Texas area maintained its better than average exploratory position. No doubt a number of factors may have influenced the extent of the 1942 development. Among those arising from the economic dislocation attendant on the war effort, the following are worthy of note. Owing to inductions into the armed forces and shipyard competition for mechanically trained men, experienced drilling personnel was sharply reduced, thereby increasing drilling costs and well-completion hazards. Replacement labor has not met the same standard of responsibility or workmanship to which the oil industry has grown accustomed. Increased military consumption of aviation gasoline and other crude products, coupled with decreased domestic consumption of lower-octane gasoline, has stimulated the market demand for the types of sweet crude most readily processed with available refinery equipment to meet war requirements, and has depressed the market demand for the sour West Texas crudes. As a majority of the purchasers of West Texas crude normally ship a substantial portion of sour crude to the refineries on the Atlantic seaboard, the loss and diversion of tanker service between Gulf Coast and north Atlantic ports have further curtailed the market demand for this type of crude oil. As some purchasers of crude oil were able to move by pipe line their West Texas trunk-line capacity to Midwestern refining centers, they were not impelled to curtail purchases of West Texas crude. The varying ability of the purchasers of crude oil to market West Texas crude was reflected back to various fields to which they were connected, causing an unequal distribution of production as among fields and operators. The pipe-line runs from the West Texas-New Mexico area decreased from approximately 354,000 bbl. Per day in January to about 265,000 bbl. in December 1942. .Approximately 2,991,000 bbl. of West

Jan 1, 1943

By Robert S. Dewey

Drilling in West Texas during 1942 was substantially less than in the previous year. In all. 1267 Wells were drilled, as compared with 2325 wells in 1941. Of these 1267 wells, 1052 oil wells, 10 gas wells and 69 dry holes were drilled in proven fields and 36 oil wells, one gas well and 99 dry holes were wildcat operations. Of the 36 wildcat wells completed as oil producers, 16 led to new field discoveries, three found new productive horizons in old fields, and 17 extended the productive limits of established fields. Where semiwildcat drilling took place along established productive trends, there was often no sharp demarcation between wildcat wells that extend field limits and normal development to fulfil lease obligations, other than the arbitrary classification of a well as a wildcat if it was drilled at a distance of 2 miles from a producing oil well. The dry hole drilled on the edge of a field may have proved a more hazardous operation than a semiwildcat drilled several miles from production but favorably located on structure. The percentage of successful wildcatting ranges from 26.5 down to 14 per cent, dependent upon the degree of inclusion of the semiwildcat operations. Irrespective of which figure was used, the West Texas area maintained its better than average exploratory position. No doubt a number of factors may have influenced the extent of the 1942 development. Among those arising from the economic dislocation attendant on the war effort, the following are worthy of note. Owing to inductions into the armed forces and shipyard competition for mechanically trained men, experienced drilling personnel was sharply reduced, thereby increasing drilling costs and well-completion hazards. Replacement labor has not met the same standard of responsibility or workmanship to which the oil industry has grown accustomed. Increased military consumption of aviation gasoline and other crude products, coupled with decreased domestic consumption of lower-octane gasoline, has stimulated the market demand for the types of sweet crude most readily processed with available refinery equipment to meet war requirements, and has depressed the market demand for the sour West Texas crudes. As a majority of the purchasers of West Texas crude normally ship a substantial portion of sour crude to the refineries on the Atlantic seaboard, the loss and diversion of tanker service between Gulf Coast and north Atlantic ports have further curtailed the market demand for this type of crude oil. As some purchasers of crude oil were able to move by pipe line their West Texas trunk-line capacity to Midwestern refining centers, they were not impelled to curtail purchases of West Texas crude. The varying ability of the purchasers of crude oil to market West Texas crude was reflected back to various fields to which they were connected, causing an unequal distribution of production as among fields and operators. The pipe-line runs from the West Texas-New Mexico area decreased from approximately 354,000 bbl. Per day in January to about 265,000 bbl. in December 1942. .Approximately 2,991,000 bbl. of West

Jan 1, 1943

By W. H. Eardley

It is increasingly evident that the excellence of blast-furnace operation to a great extent depends upon the preparation of the products fed into the furnace. The preparation of these products is carried on largely in the roasting and sintering departments. Prior to the building of flotation plants in Utah and other western states for the treatment of lead-zinc ores, the gravity concentrates received at the Midvale smelter amounted to about 4000 tons per month, containing 24 per cent. lead and 10 or 11 per cent. zinc. This product was about 20 mesh—that is, 45 per cent. of it would be plus 20 mesh and the balance minus 20 mesh. About 1000 tons of pyrite per month, containing 5 per cent. lead and 10 per cent. zinc, was also received. These products were sent to the multiple-hearth roasters for calcining, after which they were sent to the Dwight-Lloyd machines for sintering with other ores. The sintering charge passed over the machines but once. The first flotation products received consisted of a wet, sticky, muddy mass, containing a large amount of moisture, up to 19 or 20 per cent., and it was almost impossible to feed them with any degree of regularity, if at all, through our standard feeders; but the amount of flotation product received during the first year or so was relatively small and it virtually lost its identity by being mixed with a large amount of jig and table concentrates. As the quantity of flotation products increased, more efficient filtering was accomplished and the moisture greatly reduced. Flotation Products Received At the present time the Midvale plant receives about 4300 tons per month of flotation product running 60 per cent, lead and 4.5 per cent. zinc, 85 per cent. of which is minus 200 mesh and contains about 8 per cent, moisture; and 4000 tons per month of pyrite of similar fineness, running about 2 per cent. lead and 3.5 per cent. zinc, containing about 10 per cent, moisture. The lower moisture greatly reduces the difficulties of handling, making it possible to run a 100 per cent. flotation feed on a multiple-hearth furnace without serious mechanical troubles. The calcine, however, would contain nodules and balls of unroast,ed concentrates, sulfur elimination

Jan 1, 1928

By W. H. Eardley

IT IS increasingly evident that the excellence of blast-furnace operation to a great extent depends upon the preparation of the products fed into the furnace. The preparation of these products is carried on largely in the roasting and sintering departments. Prior to the building of flotation plants in Utah and other western states for the treatment of lead-zinc ores, the gravity concentrates received at the Midvale smelter amounted to about 4000 tons per month, containing 24 per cent. lead and 10 or 11 per cent. zinc. This product was about 20 mesh-that is, 45 per cent. of it would be plus 20 mesh and the balance minus 20 mesh. About 1000 tons of pyrite per month, containing 5 per cent. lead and 10 per cent. zinc, was also received. These products were sent to the multiple-hearth roasters for calcining, after which they were sent to the Dwight-Lloyd machines for sintering with other ores. The sintering charge passed over the machines but once. The first flotation products received consisted of a wet, sticky, muddy mass, containing a large amount of moisture, up to 19 or 20 per cent., and it was almost impossible to feed .them with any degree of regularity, if at all, through our standard feeders; but the amount of flotation product received during the first year or so was relatively small and it virtually lost its identity by being mixed with a large amount of jig and table concentrates. As the quantity of flotation products increased, more efficient filtering was accomplished and the moisture greatly reduced. FLOTATION PRODUCTS RECEIVED At the present time the Midvale plant receives about 4300 tons per month of flotation product running 60 per cent. lead and 4.5 per cent. zinc, 85 per cent. of which is minus 200 mesh and contains about 8 per cent. moisture; and 4000 tons per month of pyrite of similar fineness, running about 2 per cent. lead and 3.5 per cent. zinc, containing about 10 per cent. moisture. The lower moisture greatly reduces the difficulties of handling, making it possible to run a 100 per cent. flotation feed on a multiple-hearth furnace without serious mechanical troubles. The calcine, however, would contain-nodules and balls of unroasted concentrates, sulfur elimination

Jan 1, 1928

By P. H. Delano, Will H. Coghill, G. D. Coe

Data concerning the actual net energy required for pulverizing coal are lacking from the literature on coal pulverization. Power data given in the literature concern gross power and frequently include the power expended on the air blast or product-conveyor system, as well as power lost through friction in the pulverizer itself. Consequently, such data supply no information regarding the net energy consumed in pulverizing or the relative grinding resistance of various coals. In the study of coal pulverizing much work has been done on what is known as " grindability-index numbers," but grind-ability tests have seldom considered the energy input (that is, the "cause" part of the system "cause and effect"). There are many records of the effect, but even these have questionable value because the "grindability" tests did not make a pull'erized product by a method comparabLe with- commercial pulverizers. In many of the tests, only a selected part of the coal was ground, and the remainder continued to be an unknown factor. Furthermore, none of the grindability tests provide the balanced circulating load common to all modern commercial pulverizing. In order to obtain better understanding of the fundamental principles of coal pulvcrizing, the Bureau of Mines is investigating the "cause" phase; that is, the net energy input or net power excluding friction between the moving parts of the machine. As a first step in the investigation,it was necessary to design and construct a laboratory machine in which no friction-loss corrections are involved, which could grind and finish a minus-¾-inch feed, which could be emptied rapidly and completely, which could operate with a continuous feed and finish in an air separator; and, most essential of all, which would be equipped with a measuring device for recording only that portion of the total power consumed in actual pulverizing, hereafter referred to as "net energy input" or "net horsepower-hours." The channel-roller pulverizer hereinafter described is believed to meet these requirements. History oF the Machine The, work started when Ralph W. smith, engineer, St. Genevieve Lime Co., St. Cenevieve, Mo., was appointed one of the consultants of the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama, to develop a machine for testing the abrasiveness of coal. Smith had already developed a machine for testing the abrasive-ness of dentifrices,1 and it was thought the same principles might be applied to coal, Smith's machine had a revolving disk with an annular channel in which the sample was placed. Riding in the channel was a small block or runner of selected soft metal held

Jan 1, 1942

By Will H. Coghill, P. H. Delano, G. D. Coe

Data concerning the actual net energy required for pulverizing coal are lacking from the literature on coal pulverization. Power data given in the literature concern gross power and frequently include the power expended on the air blast or product-conveyor system, as well as power lost through friction in the pulverizer itself. Consequently, such data supply no information regarding the net energy consumed in pulverizing or the relative grinding resistance of various coals. In the study of coal pulverizing much work has been done on what is known as " grindability-index numbers," but grind-ability tests have seldom considered the energy input (that is, the "cause" part of the system "cause and effect"). There are many records of the effect, but even these have questionable value because the "grindability" tests did not make a pull'erized product by a method comparabLe with- commercial pulverizers. In many of the tests, only a selected part of the coal was ground, and the remainder continued to be an unknown factor. Furthermore, none of the grindability tests provide the balanced circulating load common to all modern commercial pulverizing. In order to obtain better understanding of the fundamental principles of coal pulvcrizing, the Bureau of Mines is investigating the "cause" phase; that is, the net energy input or net power excluding friction between the moving parts of the machine. As a first step in the investigation,it was necessary to design and construct a laboratory machine in which no friction-loss corrections are involved, which could grind and finish a minus-¾-inch feed, which could be emptied rapidly and completely, which could operate with a continuous feed and finish in an air separator; and, most essential of all, which would be equipped with a measuring device for recording only that portion of the total power consumed in actual pulverizing, hereafter referred to as "net energy input" or "net horsepower-hours." The channel-roller pulverizer hereinafter described is believed to meet these requirements. History oF the Machine The, work started when Ralph W. smith, engineer, St. Genevieve Lime Co., St. Cenevieve, Mo., was appointed one of the consultants of the Bureau of Mines, United States Department of the Interior, in cooperation with the University of Alabama, to develop a machine for testing the abrasiveness of coal. Smith had already developed a machine for testing the abrasive-ness of dentifrices,1 and it was thought the same principles might be applied to coal, Smith's machine had a revolving disk with an annular channel in which the sample was placed. Riding in the channel was a small block or runner of selected soft metal held

Jan 1, 1942

By B. H. Kear, B. J. Piearcey

The orientation and temperature dependence of the tensile and creep propevties oj Mav-M200 crystals halle been determined. Crystals oriented for single slip exhibit ,maximum ductility, minimum work hardening, and least creep resistance, whereas crystals in multiple slip orientations show nzinimu~n ductility, strongest work hardening, and greatest creep resistance. At 1400" and 1600°F there is a marked improzlenzent in creep strength for orientations approaching [001] and [111], indicating that interactions between dislocations gliding in intersecting octahedral slip systems play an important role in creep resistance. At 1800°F the creep strength is much less dependent on orientation, which is rationalized in terms of slip in cube planes as well as octahedral A frequent mode of failure in high-strength cast nickel-base superalloys is by intergranular fracture, particularly along those grain boundaries oriented transverse to the major stress axis. VerSnyder and ~uard' demonstrated that this problem could be overcome by eliminating transverse grain boundaries through unidirectional solidification. Piearcey and versnyder2 made use of this principle in the development of unidirectionally solidified gas turbine blades and vanes, where the growth direction of the columnar grain structure coincides with the axis of principal stress under operating conditions. The present investigation was undertaken to determine if further improvement in properties may be obtained by eliminating grain boundaries altogether, so as to take advantage of the well-known dependence of mechanical properties of single crystals upon the orientation. 1) EXPERIMENTAL PROCEDURE Single crystals of Mar-M200* were grown from the melt under vacuum by a modified Bridgman method. The melt was poured into a preheated alumina mold, and crystal growth was promoted from one end by appropriate gradient cooling. Tensile and creep specimens (2 in. diam by $ in. gage length) were prepared by a series of operations involving electrical discharge machining, precision grinding, and electropolishing. The orientations of the specimens were determined by the Laue X-ray back-reflection method. Tensile tests were carried out in aWiedemann machine with furnace attachment, using a strain rate planes. In all orientations imzpvouement in the strength charactevistics of the material can be induced by heat treatment. Creep ad stress rupture data for (001) oriented crystals are compared with similar data obtailted previously joy random polycvystalline material, and also columnar grained material having a prejevved (001) orientation. The single-crystal )material exhibits both longer rupture life and lower minimum creep rate at all temperatuves, and the rupture elongation is comparable with that in the columnar grained material. From these results it is concluded that single crystals should and useful application in gas-turbine blades and tanes. The optimum orientation for a blade is considered to be with its axis of principal stvess parallel to (001) ou (111). of 0.0001 sec-'. Load and extension were recorded directly on an X-Y recorder. The strain measuring device consisted of extension arms attached to the grips at one end and leading out of the furnace to an LVDT (linear variable differential transformer) at the other. Creep tests were performed using a standard constant load creep frame. 2) DISCUSSION OF RESULTS 2.1) Structure of Alloy. The structure and segregation in as-cast and heat-treated Mar-M200 has been described in detail else where.~ The main features are as follows: the as-cast material is heavily cored, due to pronounced dendritic segregation during solidification; the dendrites are rich in tungsten and cobalt whereas the interdendritic regions are rich in chromium, titanium, nickel, and carbon. The structure consists of -60 vol pct coherent precipitate of y', basically Ni3(A1,Ti), in a matrix of y (nickel-base solid solution), interspersed in the interdendritic regions with minor MC carbides and -y' eutectic. The y' particles, and y-y' eutectic, contain more titanium, aluminum, and nickel, and less tungsten, cobalt, and chromium than the y matrix. Heat treatment partially removes segregation, eliminates the eutectic, refines the y' dispersion in y, and gives additional partially coherent M23Cs carbide. An as-cast crystal, therefore, is composed primarily of two oriented phases (y + y'), whereas the normally heat-treated crystal consists of three oriented phases (y + y' + MZ3Cs). Typical electron transmission micrographs of the y + y' structure are shown in Fig. 1. Crystals grown in the (100) orientation develop a simple unidirectional dendritic structure, Fig. 2, since (100) happens to be the preferred direction of growth for dendrites in this material. Crystals grown in the {110) and (111) orientations, however, tend to promote equal growth, generally in separate colonies, in the two and three geometrically favored (100) growth directions, respectively. In other orientations of growth, a single (100) dendrite direction generally pre-

Jan 1, 1968

By H. B. Menardi

The history, geology, ore deposits and current mining operations of the Huitzuco district have been described by C. W. Vaupelll and the current mill operations by David Segura.2 This paper completes the story of Huitzuco with a description of the reduction of the flotation concentrates. The predominant ore mineral in the Huitzuco deposit is livingstonite, a rare, mercury-antimony sulphide (HgS.2Sb2S3). Other associated minerals include cinnabar, stibnite and elemental sulphur. The gangue is largely limestone and gypsum. Former operators mined a selected grade of ore, from which the mercury was recovered by an expensive, inefficient operation. A considerable tonnage of rejects and fills, carrying mercury and antimony, was left in the mine. In order to recover both mercury and antimony from these fills and also from newly developed ore, a combination method has been developed, by means of which the livingstonite is concentrated by flotation and the flotation concentrates subsequently reduced to metallic mercury and antimony. An essential part of the flotation treatment, as developed by Segura, is the use of copper sulphate as an activating agent. A typical analysis of concentrates now being produced at the property is as follows: Hg, 7.73 per cent; Sb, 26.40; Fe, 1.20; S, 29.68; CaO, 11.50; MgO, 7.25; SiOz, 1.63; A1203, 0.65. PRocess foR Treatment op Concentrates In the development of a process for treatment of these concentrates, three different methods were investigated: (1) roasting in a Dwight-Lloyd sintering machine with an excess of air; (2) separation of mercury and antimony by distillation in a reducing atmosphere; (3) a third method, which ultimately developed into the present process. The third method involved a slow calcination at a closely regulated temperature with a limited admission of air, which separated the mercury and antimony, the raeroury passing out of the kiln with the furnace gases and the antimony remaining in the calcine or "sinter."

Jan 1, 1944

By Werner Schwartz, Wolfgang Haase

Lead sulfide concentrates, which may include other lead concentrates, are sintered on an up-draught sintering machine without the addition of any diluting agents or fluxes. Subsequently they are melted in an oil- or gas-fired rotary furnace. The sintering and melting processes are based upon the following roast-reaction: PbS + 2 PbO = 3 Pb + SO, PbS + PbSO, =2 Pb + 2 SO, For obtaining a lead bullion free from sulfur, the sintering process is carried out in such a way that the sinter product contains a small amount of excess oxygen above that to react with the sulfides. At the end of the melting process, when the reactions are finished, the remaining small amount of oxide residues is reduced with coal to which a certain percentage of soda ash (about 1 pct of the lead bullion) is added. For the lead smelting process described neither coke nor fluxes—except soda ash—are required. This process is being utilized by a European smelter successfully and with a high lead recovery. The consumption figures for the smelting of 100 tons per day of lead concentrates are indicated. The lead content of the lead concentrates from modern ore dressing plants ranges from 65 pct to above 80 pct. In most lead smelters of the world these concentrates are smelted in a blast furnace. For blast-furnace smelting the concentrates have to be desulfurized and agglomerated by sintering. A requirement for the perfect operation of a down-draught sintering machine and of a blast furnace is a maximum lead content in the feed of 40 to 45 pct. For this reason, some lead concentrates have to be diluted by adding return slags, limestone, and possibly iron oxide and sand. As an example, 100 tons of lead concentrate with 72 pct Pb would contain 13.5 tons of gangue (including the zinc). To produce a perfect sinter with 42 pct Pb it would be necessary to add 70 tons of flux and return slag, more than five times the original weight of the gangue, to the sinter mix and blast-furnace charge. A correspondingly large amount of coke would be required in order that all of these materials reach the heat of formation and the melting temperatures of the slag (1200" to 1400°C) inside the blast furnace. The roast-reaction process presents a possibility for lead recovery without dilution of the concentrates. In this process the concentrate mixed with coal is placed upon a Newnam-hearth and air is blown through nozzles into the heated mix. AS a result metalllic lead and a relatively great amount of so-called .'Grey Slag" with a lead content of 25 to 35 pct are formed. The slag is sintered to eliminate sulfur and, after addition of the requisite fluxes, treatt:d in a blast furnace. Owing to the poor recovery of lead from the hearths and to the unavoidable heavy hand-work plus the risk of poisoning this process is utilized in very few 112ad smelters today. Since in mxny countries of the world coke is expensive and difficult to obtain, it appeared feasible to use the principle of the roast-reaction by modern sintering and melting methods with recovery of the lead in electric, or oil, gas, or coal-fired furnaces. Two processes are utilized on an industrial scale: A) Lead smelting in the electric furnace of the Bolidens Gruv A/B in Sweden, as described by S. J. Walldcn, N. E. Lindvall, K.G. Gorling, and S. Lundquist. B) The self-fluxing lead smelting of Lurgi Gesell-schaft fiir Chemie und Huttenwesen m.b. H., Frankfurt a M, Germany, which is described in this paper. In the Boliden process referred to above the sinter mix is pelletized by enveloping return fines with layers of flue dust, limestone powder, and dried galena concentrate. The roasting and agglomeration are carried out on a down-draught machine, and a slight excess of sulfur is left in the sinter product. During the smelting in the electric furnance the roast-reactions occur and a slag poor in lead and a sulfur bearing lead are formed. This latter is subsequently oxidized in a converter to obtain lead bullion and dross. The Lurgi-process achieves the maximum possible extent of the roasting reaction on the sintering machine. The wet flotation concentrates are blended with return fines (lead content 70 to 80 pet), any existing flue dusts and lead slimes—but without the

Jan 1, 1962

By E. M. Porbansky

DURING the investigation of the electrical transport properties of copper, it became necessary to prepare large single crystals of the highest obtainable purity. In an effort to meet these demands, single crystals of copper have been grown by the conventional pulling technique—as has been used for the growth of germanium and silicon crystals.' Low-temperature resistance measurements made on these crystals show that, as far as their electrical properties are concerned, they are generally of significantly higher purity than the original high-purity material. The use of these pure single crystals with very high resistance ratios has made possible the acquisition of detailed information regarding the electron energy band structure of copper2-' and has stimulated widespread effort on Fermi surface studies of a number of other pure metals. It is the purpose of this note to describe our method of preparing very pure copper crystals by the Czochralski technique. Precautions were taken to prevent contamination of the melt from the crystal growing apparatus. A new fused silica growing chamber was used to prevent possible contamination from previous groqths of other materials such as germanium, silicon, and so forth. A new high-purity graphite crucible was used to contain the melt. This crucible was baked out in a hydrogen atmosphere at -1200°C for an hour, prior to its use in crystal growth. Commercial tank helium, containing uncontrolled traces of oxygen, was used as the protective atmosphere. A trace of oxygen in the atmosphere appears to be necessary for obtaining high-purity copper single crystals. A 3/8-in-diam polycrystalline copper rod of the same purity as the melt was used as a seed. The copper rod was allowed to come in contact with the melt while rotating at 57 rpm. When an equilibrium was observed between the melt and the seed (that is, the seed neither grew nor melted), the seed was pulled away from the melt at a rate of 0.5 mils per sec. As the seed was raised, the melt temperature was slowly increased, so that the grown material diminished in diameter with increasing length. When this portion of the grown crystal was -1 in. long and the diameter reduced to less than 1/8 in., the melt was slowly cooled and the crystal was allowed to increase to - 1-1/4 in. diam as it was grown. By reducing the diameter of the crystal in this manner, the number of crystals at the liquid-solid interface was decreased until only one crystal remained. Fig. 1 shows a typical pulled copper single crystal. The purity of the starting material and the crystals was determined by the resistance ratio method: where the ratio is taken as R273ok/R4.2ok. The starting material, obtained from American Smelting and Refining Co., was the purest copper available. Most of the pulled copper crystals had much higher resistance ratios than the starting material. The highest ratio obtained to data is 8000. Table I is an example of the data obtained from some of the copper crystals. Note that Crystal No. 126 had a lower resistance ratio than its starting material and this might be due to carbon in the melt. The melt of this crystal was heated 250" to 300°C above the melting point of copper. At this temperature it was observed that copper dissolved appreciable amounts of carbon. The possible presence of carbon at the interface between the liquid and the crystal will result in reducing conditions and negate the slight oxidizing condition required for high purity as discussed below. The possible explanations of the improvement in the copper purity compared to the starting material are: improvement in crystal perfection, segregation, and oxidation of impurities. Of these, the latter seems to be most probable. A study of the etch pits in the pulled crystals showed them to have between 107 and 108 pits per sq cm. The etch procedure used was developed by Love11 and Wernick.10 The resistivity of the purest copper crystal grown was 2 x 10-10 ohm-cm at 4.2oK; from the work of H. G. vanBuren,11 the resistivity due to the dislocations would be approximately 10-l3 ohm-cm, which indicates that. the dislocations in the copper crystals would contribute relatively little to the resistivity of the crystals at this purity level. Segregation does not seem likely as the reason for purification of the material, since the resistivity of the first-to-freeze and the last-to-freeze portions are approximately the same, as was observed on Crystal No. 124. On most of the crystals that were examined, the entire melt was grown into a single crystal. If the

Jan 1, 1964