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By B. M. Larsen, T. E. Brower

A perspective is presented of the steel plant sulphur distribution and elimination problem from coal to liquid steel ready for teeming, giving distributions of sulphur over a range of coke sulphur content, and some methods of sulphur control, in the blast furnace, external desulphuriza-tion between blast furnace and open hearth, distribution between fuel, slag, and metal, and methods and limitations of control of sulphur in the open hearth furnace. AS a part of the 1951 AIME symposium on sulphur in steelmaking, it was thought that a discussion of the distribution of sulphur throughout the whole series of operations, from coal and ore to finished steel ingots, might have some value in giving a perspective on the whole problem. The following discussion is an attempt to present such an overall picture. The order is that of the actual plant operations, beginning with a very brief consideration of the coking process. Sulphur in Coal and Coke Since by far the largest source of sulphur entering the steelmaking cycle is in the coal used to make coke for the blast furnace, it would seem reasonable to eliminate some of it, either from the coal, or the coke, or during the coking process. This has appeared impracticable up to the present, at least, for two main reasons: the low activity of the organic sulphur in either coal or coke, and because of price limitations involved in treating a low cost material such as coke. A variable portion, usually M or less, of the sulphur is present in coal in the form of pyrites or similar compounds, and a large part of this sulphur may be removed in the coal washery. Most of the sulphur, however, is normally present as "organic" sulphur, intimately associated with the coal structure. Its distribution prevents any separation by mechanical means. Its low activity makes improbable ' any rapid chemical removal, although hydrogen will remove sulphur from both coal and coke. Thus, prolonged recirculation of coke oven gas in the coking process would tend to leave a smaller percentage of the total sulphur in the coke residue. Table I shows a typical distribution of sulphur from coal into products in the coking process. As the sulphur in the coal increases, the sulphur in the coke tends to increase in about the same proportion. Sulphur in the Blast Furnace The best picture of the situation in the blast furnace is provided by a sulphur balance of raw materials entering, and of products leaving, the furnace. The difficulties in accurate weighing and sampling of the variable solid materials entering this process, and the number of hours required for the raw materials to descend through the furnace under variable operating conditions, make it difficult to obtain an accurate balance. However, balances made over periods of weeks or months tend to average out some of these uncertainties. Table I1 presents three typical sulphur balances similar to a number that the writers have calculated. In most of these the slag volume calculated from the sulphur balance is, in some instances more, and in other instances less, than the value corresponding to the best input and output balances of the other slag constituents (lime, silica, alumina, etc.). Probably the greatest source of error in these calculations is the sulphur content of the slag. Despite some possible inaccuracies the balances of Table II show rather definitely the following points: 1—That 87 to 95 pct of the total sulphur input is in the coke and 95 to 97 pct of the total sulphur output is in the slag. Also, that if any sulphur leaves the furnace with the gas it is relatively small, amounting to a possible 1 pct or less. 2—At the lower sulphur coke level of 0.86 pct the total amount of sulphur charged is 15 Ib of sulphur per ton iron increasing to 26 lb per ton at the higher sulphur, intimately associated with the coal struc-rare burdens containing sulphur-rich ores will the total sulphur burden fail to be nearly proportional to the content in the coke used. 3—The 7 to 9 pct of the total sulphur input from the limestone of furnaces B and C is due to the relatively high sulphur content of the stone, 0.226 and 0.265 pct, respectively. In the case of furnace A, the sulphur content of the limestone was only 0.06 pct which resulted in only 3 pct of the total sulphur input coming from this source. It is rather interesting to compare the sulphur balances of a typical ferromanganese furnace with

Jan 1, 1952

By H. Cecil Spicer

The results described in this article are based on field work conducted during the periods APril-May, 1939, and MaY-JulY, 1940. The United States Potash CO. is mining potash on Government land under a permit from the Department of the Interior and the geophysical investigation mas completed under a cooperative arrangemerit made between that company and the Conservation Branch of the Geological Survey. The writer, a member of the Section of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be applicable, an l was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. Others have made, and reported, resistivity studies over saliferous deposits in different areas. Friedell and Messrs. Schlumberger2 reported geophysical work performed in the disrovery of the salt domes of Alsace; Carrette and Kelly3 described the geology of the same area. Leonardon and Kelly4 published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlum-berger5 in a communication. Messrs. Alty6 described studies 0" salt deposits in which the sing[e-probe method was used. Sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performetl with the ground comparator of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 800 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,ll through the courtesy of Harry Aurand, of the Midwest Refining CO.

Jan 1, 1942

By H. Cecil Spicer

The results described in this article are based on field work conducted during the periods APril-May, 1939, and MaY-JulY, 1940. The United States Potash CO. is mining potash on Government land under a permit from the Department of the Interior and the geophysical investigation mas completed under a cooperative arrangemerit made between that company and the Conservation Branch of the Geological Survey. The writer, a member of the Section of Chemistry and Physics of the Geologic Branch, was assigned to this investigation. Four definite objectives were in mind for the geophysical work in the studies over the salt deposits. The first was to determine the measure of success that could be attained in this type of work with the resistivity methods that were to be employed. These methods had been introduced into the work of the Conservation Branch by Benjamin E. Jones for the investigation of dam sites, and have been used under his direction by the author for such work. If the method proved to be applicable, an l was to be made to contour the top of the salt beds and also the other formation boundaries known to be present in this area. Salt-water aquifers were to be studied in an effort to determine their boundaries, and an attempt was to be made to delineate the potash-bearing beds. Others have made, and reported, resistivity studies over saliferous deposits in different areas. Friedell and Messrs. Schlumberger2 reported geophysical work performed in the disrovery of the salt domes of Alsace; Carrette and Kelly3 described the geology of the same area. Leonardon and Kelly4 published a resistivity curve obtained over the Hettenschlag dome, and a further discussion of this same area was given by the Messrs. Schlum-berger5 in a communication. Messrs. Alty6 described studies 0" salt deposits in which the sing[e-probe method was used. Sinerez7 mentions that electrical methods were tried over salt deposits in Spain. Geoffrey and Charrin8 show a resistivity curve obtained over marl, gypsiferous marl and salt which is similar to that obtained over the New Mexico salt deposits. Kelly9 reported resistivity work performetl with the ground comparator of Zuschlag over the salt deposits near Syracuse, N. Y., where the Salina formation is at a depth of 700 to 800 ft. Some structural studies on the potash basin of Alsace are described by Poldini.10 Another single-probe resistivity study, made over salt deposits in New Mexico, is briefly described by Heiland,ll through the courtesy of Harry Aurand, of the Midwest Refining CO.

Jan 1, 1942

By Earl E. Hunner

At the end of the year 1914, the main North Star incline shaft had reached the 6300-ft. level, and encountered a vein dipping southwest, or exactly opposite to the North Star. Subsequent development failed to find the North Star vein continuing beyond this intersection, so the 6300-ft. level proved to be the bottom level of the North Star vein, and very little ore was found below the 5300-ft. level. The new vein was called No. 1 vein. Development work carried on for the next 10 years discovered a third vein, called No. 2, branching off about 1200-ft. to the east, with a north-south strike and a west dip. No. 1 vein had about 900 ft. of backs above the 6300-ft. level before reaching the boundary line of the property, and No. 2 vein died out about 800 ft. above. During these 10 years, the money spent on development was increased from $54,000 in 1914 to $184,000 in 1924; the ore reserves steadily diminished until it was evident that the mine must close down unless by some means a large tonnage of ore could be developed quickly. Problems and Plans In order to understand what follows, the general layout and equipment of the mine as it was at this time must be briefly described. Fig. 6 indicates the relative positions of the shafts. The North Star (incline) shaft extends from the surface to the 6300-ft. level following the vein, with an average pitch of 26", between limits of 11" to 38. There is at present no hoisting equipment in this shaft between the 2700 and 4000-ft. levels. The Central (vertical) shaft connects with the North Star shaft at the 4000-ft. level, at a vertical depth of 1600 ft. In two compartments of this shaft 4-ton skips made a vertical turn of 15 ft. radius at the 4000-ft. level and ran down the incline to the 6300-ft. level. A cage operated in the third compartment to the 4000-ft. level. Men and supplies were transferred to a truck running on a third track down the incline shaft to the 6300, operated by an electric hoist on the 4000-ft. station. When the shifts changed double-deck cages were substituted for the skips in the vertical shaft, but they stopped at the 4000-ft. station. The truck to 6300 carried 22 men, and it required 8 min. to make a trip down and back. This arrangement was satisfactory as long as a fairly large proportion of the work was

Jan 1, 1930

By J. C. Kerkering, P. M. Daling

This paper discusses a study performed to evaluate the feasibility of transferring formal system safety assessment technology to the mining industry. A representative listing of formal techniques was evaluated to select the most useful methods for the mining industry to implement. Criteria for selecting methods included the interests, needs, and requirements of mine safety officials. This paper describes one of the selected methods, preliminary hazards analysis (PHA), and illustrates the analysis procedure for a mining example. This study also includes an assessment of the adaptability of selected methods to a user-interactive computer system for use by mine safety personnel. This paper includes a description of a conceptual computerized PHA-type safety program that facilitates performance of the safety analysis and can accommodate updates and revisions as necessary.

Jan 1, 1983

By R. J. Stevens

The Roan Antelope Smelter commenced operations in October, 1931. As originally designed, its equipment consisted of one reverberatory furnace, 120 X 25 ft, two Peirce-Smith converters 12 X 20 ft, and one straight line casting machine. Since that time the following additions have been made: One reverberatory furnace 120 ft X 28 ft ('934) One reverberatory furnace 95 ft X 28 ft (1943) Two 12 X 20 ft Peirce-Smith converters (1934 and 1938) One 13 X 30 ft holding furnace (1938) One straight line casting machine and 2 ladle tilting quadrants (1934) The metallurgy of the smelting process is comparatively simple. However, there are several features of operation which are uncommon to most copper smelters: (I) The high grade of concentrate treated; this has always been about 50 pct copper. (2) The high flux burden on the charge. This is necessary because of the deficiency of bases in the concentrate and the high alumina content of the concentrate. (3) The frequent necessity of adding coal to the furnace charge to control the matte grade. (4) The high grade of matte produced. This has led to unusual converter problems. From the commencement of operations, the ore mined has come from the Roan Basin orebody. The concentrate produced from this ore consists mainly of chalcocite and shale with small proportions of other copper minerals. As mining operations extend to the Roan Extension orebody, the proportions of bornite and chalcopyrite in the concentrate will increase with a corresponding decrease in the copper content of the concentrate. Because of the concentrate grade the capacity of the reverberatory furnaces in terms of tons of copper produced per ton of coal burned is high. This ratio is usually over 2.2, and on especially favourable runs has reached 2.6. Reference to Table I shows that the iron content of the concentrate is unusually low. Only part of this iron is available for slag formation, the balance going to the matte. To make up this deficiency in bases, limerock is added to the furnace charge. This flux ensures a slag that is of the correct silicate degree, is suficiently fluid, of low specific gravity, and it counteracts the thickening effect of the alumina present. An ample supply of flux is obtainable from Ndola, 22 miles distant by rail. Although the reverberatory slag has a high copper content, the slag fall is low and the copper loss in the slag now rarely exceeds 1.0 pct of the total copper charged. The blister copper shipped is of such purity that only one fire refining operation has been necessary to produce a wirebar with properties comparable to electrolytic copper. Bismuth has always been the most troublesome impurity and consequently the problem of its control in the finished product has been of prime importance. Practically none is removed in the reverberatory furnace. The bulk of the elimina-

Jan 1, 1949

By K. A. Gschneidner, O. D. McMasters, T. J. O’Keefe

X-ray diffraction, differential thermal, ad rnetallo-graphic methods were used to establish the Dy-Pb Phase diagram. Lead additions lower the 1377°C transformation temperature of dysprosium to 1360°C leading to an inverted peritectic reaction. The 327°C melting point of lead is lowered by dysprosium additions to about 326°C yielding a eutectic reaction. A second eutectic reaction occurs at 13.3 at. pct Pb and 1200°C. The dysprosium-richest intermetallic compound DysPb3 melts congruently at 1695°C and crystallizes in the hexagonal Mn5Si3 (D8,) type structure. The peritectic decomposition temperatures for the remaining compounds are Dy5Pb, at 1555C, DyPb2 at 955C, and DyPb3 at 880°C. A fifth compound near the DyPb stoichiometry exists over a 310°C temperature range decomposing at 1130°C by means of an inverted peritectic reaction and melting incongruently at 1440°C. The crystal structures of the compounds are discussed. A systematic study of the rare earth-lead alloy systems is underway in an effort to supply information concerning the alloying behavior of the rare earth metals. The Dy-Pb phase diagram is the fourth system to be investigated in this study. The Yb-Pb,1 Y-Pb,2 and Eu-Pb 3 diagrams have been published recently. Utilization of the rare earth series of metals as a research tool in this manner should yield a better understanding of alloy formation. EXPERIMENTAL PROCEDURE Materials. The lead used in this investigation was obtained from Cominco Products, Inc., and was specified to be 99.99 pct pure. The dysprosium was prepared in this Laboratory by the calcium reduction of the fluoride followed by distillation of the dysprosium. The major impurities in the dysprosium in ppm are: A1 (<40), Ca (400), Er (<50), Gd (<200), Ho (<200), Mg (<50), Si (30), Ta (400), Tb (<100), Y (<50), 0 (651, H (15), N (not detected), F (430), C (35). Alloy Preparation. Most of the alloys were prepared by melting weighed amounts of dysprosium and lead in sealed tantalum crucibles. The tantalum crucibles were sealed by are-welding in a He-Ar atmosphere welding chamber. Thus the alloys are in contact with He-Ar at about 1 atm pressure. Homogenization was achieved by holding them in the liquid state for about 1 hr, cooling, inverting the crucibles, remelting, and repeating the process at least twice. Since these alloys were prepared in sealed tantalum crucibles, chemical analysis for final composition was thought to be unnecessary. No detectable reaction of these alloys with the tantalum crucible was observed by metallographic examination. Metallographic evidence was also used to confirm the homogeneity of some of the alloys prepared in this manner. The compositions of a few alloys, which were prepared by nonconsum-able are-melting, were corrected for the small weight losses involved by assuming that the weight loss is due to vaporization of lead. The specimens obtained from the alloy samples were prepared under a dry-argon atmosphere because they were rapidly attacked by air and moisture. Thermal Analysis. Differential thermal analysis methods were used to determine the liquidus curves and reaction horizontals of the system. Both Pt vs Pt + 13 pct Rh and W + 5 pct Re vs W + 26 pct Re thermocouples were used to measure the temperature. An X- Y recorder was used to record the specimen temperature and differential electromotive force between the specimen and molybdenum standard. The arrest temperatures were measured potentiometri-cally. The accuracy limits (* values) associated with the reaction temperatures obtained by this method were estimated on the basis of both the reproducibility of the particular temperature value and the accuracy of the thermocouple at a given temperature. Liquidus temperatures were obtained from cooling arrest data while both heating and cooling arrest data were used to establish the horizontals of the diagram. Heat treatments during the thermal analyses of the alloys between 40 and 70 at. pct Pb were necessary in order to approach equilibrium conditions. The samples were held at temperatures between the various peritectic horizontals for l to 2 hr before the thermal analyses were continued. The entire range of compositions was investigated at the expense of a minimum amount of materials by adding appropriate amounts of lead to master alloys. More than sixty alloys were analyzed by this differential thermal method and for each alloy the results given herein are taken from two or three heating and cooling cycles. X-Ray and Metallographic Methods. Slice specimens for metallography and powder specimens for X-ray diffraction were prepared from rod-shaped samples which had been melted in sealed 0.62 5-cm-diam tantalum crucibles. The specimens were heat-treated in sealed tantalum crucibles which were protected by sealing them in argon-filled quartz ampules. Quenching was accomplished by breaking the ampules in ice water after heat treatment. X-ray powder specimens were sealed in 0.3-mm-diam glass capillaries under a dry-argon atmosphere. Copper, iron, and chromium radiation were used to obtain the powder patterns for these alloys. More than 150 powder patterns were obtained for specimens of various compositions and heat treatments. Included in these were several patterns for specimens which had purposely been oxidized. Patterns from specimens which had been accidentally exposed

Jan 1, 1969

By W. D. Donnelly, M. L. Rudee

THE crystallography and morphology of ?-Al3Fe precipitates in an A1 + 0.5 wt pct Fe alloy have been studied by transmission electron microscopy. The alloy was cast in cylindrical ingots, 15 cm in diameter and 60 cm in length, and cooled slowly. The measured composition was 0.527 wt pct Fe, 0.001 wt pct Mg, and 0.003 wt pct Cu. Spectrographic analysis revealed no additional trace impurities. Thin slices were cut from the ingot and reduced by more than 95 pct by rolling to a thickness of 0.1 mm with no intermediate annealing treatments. These thin sheets were then vacuum-annealed for 1 hr at 612°C and air-cooled in their capsules. Thin foils for examination in the electron microscope were prepared by electropolishing. The precipitate is found in the form of oval platelets on the (110) planes of the matrix. The major axes of the platelets are parallel to the (110) directions of the matrix, and vary in length from 1/2 to 2 p. The thickness is about 1/10 µ. Examples of platelets, both in the plane of the foil and normal to the foil, are shown in Figs. l(a) and l(b), respectively. lack&apos; found that ?-A13Fe (more correctly Al13Fe4) belongs to the monoclinic system. Using Black&apos;s structural data and simultaneous electron-diffraction patterns from the matrix and precipitates, the habit planes and directions were determined to be: (001)? 1 (110)Al [100]?|| H [001]Al The orthogonal crystallographic axes of the precipitates are accurately in the habit plane, while the measured coincidences of the directions are only within 10 deg. The major axis of the platelet is parallel to [010] in the 0. This orientation corresponds to the direction of nearest registry of the lattices.

Jan 1, 1964

By C. H. Curtis

HE valuable mineral content of the current feed -*- to the Miami concentrator is as follows: copper, 0.7 pct total; molybdenum, 0.01. Flotation of this ore yields a sulphide concentrate containing: chalco- cite, 44 pct; molybdenite, 0.5; pyrite, 50.0; insol, 5.5. A combination of potassium ethyl xanthate and pentasol amyl xanthate as collectors, and pine oil as frother, are used in this flotation. Rejection of pyrite is encouraged by holding the amount of collectors used to the minimum consistent with copper recovery and by operating at high alkalinity (equivalent to 0.35-0.40 lb CaO per ton solution of pH 11.0). The molybdenum recovery in the sulphide concentrates under the above flotation conditions is approximately 50 pct of that originally present in the ore. Taking into account the acid soluble molybdenum, indicated molybdenite recovery is 75 to 80 pct. The attempt to separate the molybdenite into an acceptable molybdenum product begins with the bulk sulphide flotation concentrate just described. This concentrate is composed of chalcocite, whose floatability has been promoted to the fullest extent possible for the sake of its recovery from the ore, together with the pyrite which has been activated along with the copper mineral. The problem is to deaden the copper and iron minerals, and to float the molybdenite. Obviously in the accomplishment of this end, conditioning and preparation of the pulp, prior to flotation, plays an all important role. The first step is thickening to 50 to 60 pct solids, with milk of lime added to the thickener feed to maintain an alkalinity of the pulp equivalent to a pH of 8.5 to 8.8 during its residence in the thickener. The purpose of the thickening is primarily to reduce the volume of pulp for subsequent treatment. However, the relatively prolonged retention of the pulp in the thickener at the desired alkalinity is known to have a favorable depressing effect upon pyrite. There is a limit for this alkalinity above which a depressing effect upon molybdenite occurs. The thickened pulp (alkalinity: 0.015 lb CaO per ton, pH 8.8), discharges into an agitator, retention time approximately 2 hr, to which additional lime is added to raise the alkalinity to 0.35 to 0.40 lb CaO per ton solution, pH 11.6. This additional lime is required for pyrite depression and can be tolerated without loss of molybdenite because of the limited time of contact in the conditioner tank. The pulp leaving the lime conditioner passes through two successive steaming tanks, which are mechanically agitated, and into which live steam is admitted directly into the pulp near the bottom of the tanks. The temperature of the pulp is maintained as near boiling as possible. The steaming time is approximately 4 hr. The pulp leaving the last steamer has an alkalinity of about 0.04 lb Cao per ton solution, pH 8.7. It is believed that oxidation of the copper and iron sulphides occurs during steaming, the resulting sulphates reacting the calcium hydroxide to calcium sulphate and thus reducing the alkalinity. Since the steamer-feed solution is already saturated with calcium sulphate, the calcium sulphate produced during steaming is precipitated. It is believed that this calcium sulphate is precipitated preferentially on copper and iron mineral surfaces thus decreasing their floatability. Aside from the "lime chemistry" during steaming, pine oil is displaced from the pulp and xanthate decomposed, which has a major effect upon the deadening of the copper and iron sulphides. Following steaming, the hot pulp is admitted to another conditioning tank wherein it is aerated, primarily for cooling, but incidentally for additional oxidation of the copper and iron sulphides. The resulting "deadened" pulp is then diluted to 20 pct solids, a specific collector for molybdenite, ordinary stove oil, is added and the separation of the molybdenite by flotation is undertaken at a pH of 8.5 to 8.8 in standard Miami air-flotation ma-chines. B-22 frother is used when necessary. A re-grind of the thickened rougher concentrates is made prior to the first cleaning operation chiefly for rejection of insoluble in subsequent flotation. The cleaner concentrate is then stepped up to 90 pct MoS, in an 8-cell Denver flotation machine No. 18. Sodium silicate is added to the cleaner circuit. Its effect is to flocculate molybdenite and stabilize the froth. In summary, it may be stated: 1. Separation of molybdenite into an acceptable product from sulphide copper concentrates by flotation involves preliminary preparation and conditioning of the pulp, which is of major importance. 2. This preparation and conditioning consists of several successive steps: (A) Thickening to 50 to 60 pct solids at controlled alkalinity to reduce volume of pulp and to contribute to depression of pyrite. (B) Agitation at high-pulp density for limited time with additional lime to provide for depression of pyrite. (C) Steaming at high-pulp density for decomposition of xanthate and xanthate surface films, evolution of pine oil, and oxidation of sulphide minerals other than molybdenite. The latter involves sulphating of lime with probable precipitation of calcium sulphate preferentially on copper and iron minerals. (D) Aeration at high-pulp density for cooling, and for further oxidation of copper and iron sulphide minerals. (E) Dilution of pulp to 20 pct solids and addition of specific collector for molybdenite, common stove oil. It is hardly necessary to point out that this rather drastic procedure for depression of previously activated copper and iron sulphide minerals, without at the same time depressing molybdenite, is possible due to the inherently high floatability and refractory nature of molybdenite. However, molybdenite is susceptible to depression by excessive lime which must therefore be limited to the amount consistent with satisfactory molybdenite recovery. The steaming procedure is being carried on at Miami Copper Co. under license agreement with Janney, Nokes, and Johnson, holders of letters patent on the process.

Jan 1, 1951

By C. H. Curtis

HE valuable mineral content of the current feed -*- to the Miami concentrator is as follows: copper, 0.7 pct total; molybdenum, 0.01. Flotation of this ore yields a sulphide concentrate containing: chalco- cite, 44 pct; molybdenite, 0.5; pyrite, 50.0; insol, 5.5. A combination of potassium ethyl xanthate and pentasol amyl xanthate as collectors, and pine oil as frother, are used in this flotation. Rejection of pyrite is encouraged by holding the amount of collectors used to the minimum consistent with copper recovery and by operating at high alkalinity (equivalent to 0.35-0.40 lb CaO per ton solution of pH 11.0). The molybdenum recovery in the sulphide concentrates under the above flotation conditions is approximately 50 pct of that originally present in the ore. Taking into account the acid soluble molybdenum, indicated molybdenite recovery is 75 to 80 pct. The attempt to separate the molybdenite into an acceptable molybdenum product begins with the bulk sulphide flotation concentrate just described. This concentrate is composed of chalcocite, whose floatability has been promoted to the fullest extent possible for the sake of its recovery from the ore, together with the pyrite which has been activated along with the copper mineral. The problem is to deaden the copper and iron minerals, and to float the molybdenite. Obviously in the accomplishment of this end, conditioning and preparation of the pulp, prior to flotation, plays an all important role. The first step is thickening to 50 to 60 pct solids, with milk of lime added to the thickener feed to maintain an alkalinity of the pulp equivalent to a pH of 8.5 to 8.8 during its residence in the thickener. The purpose of the thickening is primarily to reduce the volume of pulp for subsequent treatment. However, the relatively prolonged retention of the pulp in the thickener at the desired alkalinity is known to have a favorable depressing effect upon pyrite. There is a limit for this alkalinity above which a depressing effect upon molybdenite occurs. The thickened pulp (alkalinity: 0.015 lb CaO per ton, pH 8.8), discharges into an agitator, retention time approximately 2 hr, to which additional lime is added to raise the alkalinity to 0.35 to 0.40 lb CaO per ton solution, pH 11.6. This additional lime is required for pyrite depression and can be tolerated without loss of molybdenite because of the limited time of contact in the conditioner tank. The pulp leaving the lime conditioner passes through two successive steaming tanks, which are mechanically agitated, and into which live steam is admitted directly into the pulp near the bottom of the tanks. The temperature of the pulp is maintained as near boiling as possible. The steaming time is approximately 4 hr. The pulp leaving the last steamer has an alkalinity of about 0.04 lb Cao per ton solution, pH 8.7. It is believed that oxidation of the copper and iron sulphides occurs during steaming, the resulting sulphates reacting the calcium hydroxide to calcium sulphate and thus reducing the alkalinity. Since the steamer-feed solution is already saturated with calcium sulphate, the calcium sulphate produced during steaming is precipitated. It is believed that this calcium sulphate is precipitated preferentially on copper and iron mineral surfaces thus decreasing their floatability. Aside from the "lime chemistry" during steaming, pine oil is displaced from the pulp and xanthate decomposed, which has a major effect upon the deadening of the copper and iron sulphides. Following steaming, the hot pulp is admitted to another conditioning tank wherein it is aerated, primarily for cooling, but incidentally for additional oxidation of the copper and iron sulphides. The resulting "deadened" pulp is then diluted to 20 pct solids, a specific collector for molybdenite, ordinary stove oil, is added and the separation of the molybdenite by flotation is undertaken at a pH of 8.5 to 8.8 in standard Miami air-flotation ma-chines. B-22 frother is used when necessary. A re-grind of the thickened rougher concentrates is made prior to the first cleaning operation chiefly for rejection of insoluble in subsequent flotation. The cleaner concentrate is then stepped up to 90 pct MoS, in an 8-cell Denver flotation machine No. 18. Sodium silicate is added to the cleaner circuit. Its effect is to flocculate molybdenite and stabilize the froth. In summary, it may be stated: 1. Separation of molybdenite into an acceptable product from sulphide copper concentrates by flotation involves preliminary preparation and conditioning of the pulp, which is of major importance. 2. This preparation and conditioning consists of several successive steps: (A) Thickening to 50 to 60 pct solids at controlled alkalinity to reduce volume of pulp and to contribute to depression of pyrite. (B) Agitation at high-pulp density for limited time with additional lime to provide for depression of pyrite. (C) Steaming at high-pulp density for decomposition of xanthate and xanthate surface films, evolution of pine oil, and oxidation of sulphide minerals other than molybdenite. The latter involves sulphating of lime with probable precipitation of calcium sulphate preferentially on copper and iron minerals. (D) Aeration at high-pulp density for cooling, and for further oxidation of copper and iron sulphide minerals. (E) Dilution of pulp to 20 pct solids and addition of specific collector for molybdenite, common stove oil. It is hardly necessary to point out that this rather drastic procedure for depression of previously activated copper and iron sulphide minerals, without at the same time depressing molybdenite, is possible due to the inherently high floatability and refractory nature of molybdenite. However, molybdenite is susceptible to depression by excessive lime which must therefore be limited to the amount consistent with satisfactory molybdenite recovery. The steaming procedure is being carried on at Miami Copper Co. under license agreement with Janney, Nokes, and Johnson, holders of letters patent on the process.

Jan 1, 1951

By L. Mair

A STUDY by J. R. Low, Jr.1 on the effect of quench aging on the Charpy-impact specimens of semikilled 1020 steel disclosed that a decrease in cooling rate from 1275°F raised the transition temperature. This was demonstrated in his investigation by controlling the cooling rate of impact specimens to duplicate that of a heavier plate and com- paring the properties with air-cooled specimens and quenched specimens. The transition temperature of the samples that had been cooled at a rate estimated to be similar to that of an air-cooled 3/4 in. plate was approximately 45ºF higher than the quenched samples. The transition temperature of the air-cooled series was between that of the slow-cooled and the quenched series. On the basis of this work, it appeared that the cooling rate of plates after rolling in a hot mill would have a bearing on the brittle fracture of the

Jan 1, 1955

By James A. McGurty, Walter J. Koshuba, Samuel G. Gordon, Gilbert E. Klein

ONE of the problems encountered in working with metals at elevated temperatures is the instability resulting from solid-solid diffusion at a -common interface. A determination of the nature and magnitude of this phenomenon is important as related to structural properties of materials potentially useful in high temperature applications. This paper is concerned with the solid state reaction between metallic molybdenum and beryllium at elevated temperatures. In the older literature,&apos; there were no known inter-metallic compounds in the system Be-Mo, and the list of beryllium intermetallics was rather small. New compilations have been made by Smithells&apos; and by Taylor," listing all the then known beryllium binary intermetallic compounds. In addition to these, some new phases have just been reported&apos; in the system Zr-Be and some further compounds of the type MBe,3 have been currently described. The new compound MoBe,, which is reported upon in this paper differs considerably from the above mentioned MBe13 group, and will be discussed in detail. Diffusion Study The nature of the solid diffusion at a Mo-Be interface was determined by sealing a beryllium rod inside a molybdenum capsule and heating at a temperature of 2000°F&apos; (1100°C) for 100 hr. The molybdenum capsule was fabricated from % in. swaged molybdenum rod obtained from the Fansteel Metallurgical Corp. The beryllium metal was obtained from Brush Beryllium Corp. as % in. cold-drawn rod. This material assayed 99.05 pct Be and contained as impurities 0.84 pct Be0 and 0.19 pct Be2C. The molybdenum capsule was % in. in OD x 2 in. long. To prepare it, a concentric hole 0.250 in. + 0.001 in. — 0.000 in. in diam was drilled and reamed in one end of a rod to a depth of 1 &apos;/2 in. A 1 in. long beryllium rod 0.250 in. + 0.000 in. — 0.001 in. in diam was pressed into the molybdenum capsule. A molybdenum plug 0.250 in. & 0.001 in. in diam x 9/16 in. long was then used to seal the beryllium in place. The capsules were placed in a molybdenum resistance furnace and heated at 2000°F (1100°C) for 100 hr. On cooling, the specimens were cut and examined metallographically. Fig. 1 is a micrograph at X250 of a portion of the interface from a transverse section. Four phases are clearly visible, with sharp boundaries between them. Phase A is a section of the molybdenum capsule; phase B is the molybdenum-rich intermetallic composition MoBe,; phase C is the beryllium-rich compound MoBe13; phase D is a section of the beryllium rod. All phases were readily polished to a high metallic luster. The molybdenum-rich phase has a pronounced purple tinge. The beryllium-rich phase (C) is only slightly darker than the pure beryllium. In polarized reflected light, however, it shows striking birefringence between crossed Nicols. The black areas represent flaws or pores in the material. A small representative amount of powdered material from each of the phases was carefully removed under the microscope with a diamond tool. With this material, powder X-ray diffraction patterns were made for the identification of each phase. Table I lists the X-ray diffraction spacings and corresponding indexes characteristic of these intermetallic compounds. Synthesis To establish the formula of the new intermetallic compound, X-ray diffraction patterns were made from powders obtained from solidified melts of known composition. The syntheses were made by

Jan 1, 1952

By R. W. Raymond

There is apparently no end to the doubts, inconsistencies and absurdities in which the courts of our mining States and Territories are involved in their attempts to apply to conditions of ever-increasing complexity the provisions of our anomalous mining law. In previous papers, I have called this statute " the law of the apex," because it based upon that vague, novel and mysterious condition the most important grant of title. But the apex is scarcely a more essential feature than the end-lines and the side-lines; for the rights which it may confer may be limited in various ways by these; so that we have, in many a case, the most ridiculous result that the United States, in return for the money of a citizen, conveys to him with much solemnity, under its broad seal, nobody knows what, bounded nobody can tell how. A decision recently made at Butte by Judge De Wolfe, of the United States District Court of Montana, in the case of King et al. vs. The Amy and Silversmith Mining Company, furnishes a fresh illustration of this criticism. The diagram on the following page, constructed without precise regard to courses and distances, simply to assist in the statement of the essential features of the case, will, 1 hope, make clear the principles . involved : The plaintiff occupies a location (the Nonconsolidated) adjoining on the north the defendant&apos;s location, a b c d (the Amy), and the disputed mining-ground lies, let us say, in depth under the point W, that is, on the dip of the vein, VD, but not under the surfacelocation, a b c d. The defendant has the prior title, and claims this ground under its extra-lateral right. It is admitted that the apex does not cross the end-line, a d, and does cross the side-line, a b. Whether it crosses, at the other end of the location, the end-line, b c

Jan 1, 1889

By R. B. Snow

This paper describes a technique of polishing and etching specimens of open-hearth furnace slags or hearth aggregates for identification of the crystalline constituents —lime (CaO), tricalcium silicate (3CaO.SiO2), dicalcium silicate (2CaO.-SiO2), rnonticellite (CaO.MgO.SiO2), or forsterile (2MgO.SiO2), with especial em-phasis on the mineral merwinite (3CaO.-MgO.2SiO2). With proper standardization, this identification does not require the use of the petrographic microscope. The composition of basic open-hearth slags and furnace bottoms falls, almost without exception, within systems containing CaO, MgO, &apos;IFeO,,, MnO and SiOz, in which the number of basic molecules so greatly exceeds the orthosilicate ratio (two molecules of base to one of silica) that free basic oxides, and combinations between them such as alumi-nates or ferrites, are present in cooled specimens. Orthosilicates of (CaO + NgO) are the most common in such specimens, since in nearly all cases, except premelt slags, the molecular ratio of (CaO + MgO) to SiO, is more than 2 to I. When sufficient lime is available it combines with the silica to form dicalcium silicate (2Ca0.Si02), which contains little, if any, IvfgO, FeO or MnO in solid solution whereas the latter oxides combine to form the oxide solid solution known as periclase. If the lime present is insufficient to form dicalcium silicate (2Ca0.Si02) it combines with Mgo to form either merwillite or moIlticellite (SiOz); these minerals take little if any FeO or MnO into solid solution and the remaining MgO, FeO and hInO combine as periclase. This generalization seems to be valid for basic slags and furnace bottoms, since minerals such as Ca0.MnOSi02 and CaO.FeO.SiOz are found only in slags in which the lime-silica ratio is less than 2 and are not observed in &apos;pecimens from furnace bottoms. The identification of crystalline constituents in such materials, especially of fine crystals in the groundmass, is difficult under the petrographic microscope. They are often masked by their neighbors because of their small size in relation to the thickness of the thin section and because of the presence of Opaque Or colored constituents. The indices of refraction and the optical sign of the mineral are sometimes difficult to determine because of the small size or because Of twinning or of inclusions within the crystal. Moreover, the positive identification of merwinite (3Ca0.Mg0.2Si02) from its optical properties is usually difficult in the presence of dicalcium silicate (zCaO.SiO2). CaO, MgO, jCa0.Si02 and 2Ca0.SiOz in open-hearth &apos;lags have been identified for a number of years in the U.S. Steel Corporation Laboratory by the usual

Jan 1, 1948

By R. B. Snow

This paper describes a technique of polishing and etching specimens of open-hearth furnace slags or hearth aggregates for identification of the crystalline constituents —lime (CaO), tricalcium silicate (3CaO.SiO2), dicalcium silicate (2CaO.-SiO2), rnonticellite (CaO.MgO.SiO2), or forsterile (2MgO.SiO2), with especial em-phasis on the mineral merwinite (3CaO.-MgO.2SiO2). With proper standardization, this identification does not require the use of the petrographic microscope. The composition of basic open-hearth slags and furnace bottoms falls, almost without exception, within systems containing CaO, MgO, &apos;IFeO,,, MnO and SiOz, in which the number of basic molecules so greatly exceeds the orthosilicate ratio (two molecules of base to one of silica) that free basic oxides, and combinations between them such as alumi-nates or ferrites, are present in cooled specimens. Orthosilicates of (CaO + NgO) are the most common in such specimens, since in nearly all cases, except premelt slags, the molecular ratio of (CaO + MgO) to SiO, is more than 2 to I. When sufficient lime is available it combines with the silica to form dicalcium silicate (2Ca0.Si02), which contains little, if any, IvfgO, FeO or MnO in solid solution whereas the latter oxides combine to form the oxide solid solution known as periclase. If the lime present is insufficient to form dicalcium silicate (2Ca0.Si02) it combines with Mgo to form either merwillite or moIlticellite (SiOz); these minerals take little if any FeO or MnO into solid solution and the remaining MgO, FeO and hInO combine as periclase. This generalization seems to be valid for basic slags and furnace bottoms, since minerals such as Ca0.MnOSi02 and CaO.FeO.SiOz are found only in slags in which the lime-silica ratio is less than 2 and are not observed in &apos;pecimens from furnace bottoms. The identification of crystalline constituents in such materials, especially of fine crystals in the groundmass, is difficult under the petrographic microscope. They are often masked by their neighbors because of their small size in relation to the thickness of the thin section and because of the presence of Opaque Or colored constituents. The indices of refraction and the optical sign of the mineral are sometimes difficult to determine because of the small size or because Of twinning or of inclusions within the crystal. Moreover, the positive identification of merwinite (3Ca0.Mg0.2Si02) from its optical properties is usually difficult in the presence of dicalcium silicate (zCaO.SiO2). CaO, MgO, jCa0.Si02 and 2Ca0.SiOz in open-hearth &apos;lags have been identified for a number of years in the U.S. Steel Corporation Laboratory by the usual

Jan 1, 1948

By A. D. Hughes

A relatively small area in Malaya, about 200 miles long by 40 miles wide, is the most important source of tin in the world. Some tin is recovered in other parts of the peninsula. Of the tin mined, 98 pct is recovered from alluvial deposits. From 1935 to 1941 the average annual world production of tin was 190,000 tons. The average annual production from Malaya during the same period was 62,000 tons or about one third of the total. Other producing countries, in order of importance, were the Netherlands East Indies 34,000 tons, Bolivia 30,000, Belgian Congo, Nigeria, Siam, Burma, China, and a few others with smaller amounts. The serious shortage of tin during the war period was due to the fact that the Japanese were occupying Malaya, Netherlands East Indies, Siam, Burma, and China which, together, formerly were producing 65 pct of the world supply. Because of the importance of tin in the world economy, and because of the fact that little is generally known in this country regarding the methods of recovering the tin in Malaya, it is believed that a short description of the industry, as carried on there, may be of interest to many of the readers. In addition you may be interested in the effect of the Japanese occupation, subsequent recovery of the properties and conditions existing at that time. The Malay Peninsula lies at the southeast tip of Asia. Singapore, a British colony, is situated on a small island at the southern end of the peninsula. It is a city of nearly a million population, an important world port, the site of a large British naval base and of one of the tin smelters. The Federation of Malaya consists of nine states, plus Penang, Malacca, and other small areas formerly part of the Straits Settlements, and it now covers the entire peninsula. The civil administration is controlled by the British. A constitution was adopted recently after reaching agreement with the Malay Sultans of the various states, who retain control of religious matters. The Capital is at Kuala Lumpur, a city of about 200,000 population, 250 miles north of Singapore and about half way to Penang. The country covers an area of 51,000 square miles, an area about equal to that of Florida and about one third that of California. It has a population of about seven million consisting of Malays, Chinese, East Indians, and a relatively small number of Europeans. The principal products are tin and rubber. There are over three million acres of planted rubber. The country is not self-supporting agriculturally as about one third of the necessary food supplies is imported. Rice is the principal food of the Asiatic population and some of the recent unrest is caused by a shortage of rice and the consequent high price. Good highways have been built through the settled part of the country. A railway, Government owned, extends from Singapore northward through the entire peninsula. The climate is tropical but health conditions are good for a tropical country. I was in Malaya from 1939 until January 1942, during the time of the simultaneous air attacks on Pearl Harbor, Manila, Hongkong, and Singa-

Jan 1, 1950

By Victor A. Phillips

A series of specimens of a Cu- 3.23 pct Co alloy were prepared with particle diameters from zero to 590A. The samples were then cold-rolled 95 pct and the effects of the particle size on the behavior on annealing for hr at temperatures between 100" and 900°C were studied (by hardness, light, and electron metallography). Particles, particularly for d r 105 to 590A, greatly impeded softening and vecvystallizn-tion, and tended to give elongated grains. Particles deformed fairly homogeneously with the ,matrix, be- IN a previous study by the author,&apos; the growth of cobalt-rich precipitates was followed electron microscopically in Cu-3.12 Co alloy as a function of aging, typically at 650°C. The coherent spherical precipitates grew to 520 + lOOA average diam before spontaneously losing coherency and developing (111) facets. Stretching a few percent after precipitation 2aused loss of coherency to occur sooner at about 220A average particle diam. The particles apparently retained their fcc structure after loss of coherency. coming lau2ellae. For d = 55 to 180A, these lamellae gave streak-contrast effects apparently due to coherency strains , and spheroidized on annealing at 600" to 650°C, forming coherent particles. Particles of d = 250 ov 320A lost coherency during t-olling, giving incoherent lamellae. Recrystallization apparently occured by growth of new grains into unrecrystallized (recovered) material at temperatures below that at which cobalt atoms had much mobility. The present study was undertaken to explore the effect of cobalt-rjch particles of various average sizes from 50 to 600A diam on the isochronal annealing behavior of copper after heavy cold rolling. The previous work&apos; was used as a guide in preparing the two-phase series of prerolling structures. The solution-treated alloy was also rolled for comparison. A further question of interest in the present study was whether dislocation and particle hardening were additive, since the prerolling structures covered the full range unaged - peak aged — overaged, and further precipitation might occur on annealing after cold rolling. Although there have been exhaustive studies of the isothermal2"6 and is~chronal annealing behavior of

Jan 1, 1967

By M. H. Waxman, L. J. M. Smits

A simple physical model was used to develop an equation that relates the electrical conductivity of a water-saturatedshaly sand to the water conductivity and the cation-exchange capacity per unit pore volume of the rock. This equation fits both the experimental data of Hill and Milburn and data obtained recently on selected shaly sands with a wide range of cation-exchange capacities. This model was extended to cases where both oil and water are present in the shaly sand. This results in an additional expression, relating the resistivity ratio to water saturation, water conductivity and cation-exchange capacity per unit pore volume. The effect of shale content on the resistivity index - water saturation function is demonstrated by several numerical examples. INTRODUCTION A principal aim of well logging is to provide quantitative information concerning porosity and oil saturation of the permeable formations penetrated by the borehole. For clean sands, the relationships between measured physical quantities and porosity or saturation are well known. However, the presence of clay minerals greatly complicates log interpretation, particularly the electrical resistivity and SP logs, and considerably affects evaluation of hydrocarbon-bearing formations. The conductance and electrochemical behavior of shaly sands and their relation to log interpretation have been studied by many workers. wylliel and Lunch2 reviewed this work in some detail. Virtually all laboratory measurements of electrical resistivity and electrochemical potential of shaly sands published to date are the work of Hill and Milburn.3 Their measurements were made on about 300 cores covering a large variety of sedimentary rocks, and a wide range of equilibrating NaCl solution concentrations. Hill and Milburn described their conductivity data by an empirical equation in which the shaly sand conductivity Co was expressed as a function of the solution conductivity C and two parameters b and F01 . The quantity b was shown to be a measure of the effective clay content of the rock, being approximately proportional to the cation-exchange capacity of the rock divided by its pore volume. The latter ratio is designated as 9, in this paper and has the dimensions meq/ml or equiv/liter. Qv is identical with the term representing the concentration of fixed charges in the Meyer-Sieved and Teorel15 theory of permselective membrane behavior. F01 is a formation resistivity factor referred to a hypothetical equilibrating solution resistivity of 0.01 ohm m at 25C,* where clay effects presumably are minimized. F01 was correlated to porosity by an Archie-type equation.6 The Hill-Milburn equation describes their data with a standard deviation of approximately 1 percent and a maximum deviation of + 10 percent. Shaly sands behave as permselective cation-exchange membranes, their electrochemical efficiencies increasing with increasing clay content. The electrochemical potential data of Hill and Milburn were expressed graphically, and demonstrate that the membrane efficiency (or cation transport number) of these sands is a function only of the b value (i.e., Qv) and the respective salt concentrations of the two solutions forming the liquid junction in the sand. The diffusion potentials are not dependent on F01 or any parameter relating to the porosity or pore geometry of the rock. The Hill-Milburn resistivity equation correctly predicts a decreasing sand conductivity Co with decreasing solution conductivity C?. However, at some low value of C,, the calculated Co-C, function goes through a minimum; with further decrease in C?, the predicted sand conductivity increases sharply. As pointed out by Hill and Milburn, an increasing value of Co with decreasing C, is physically meaningless. Since this occurs below the range of practical values of C,, the usefulness of the empirical equation is not affected when

Jan 1, 1969

By Robert Rhea Goodrich

This research was done partly in the non-ferrous laboratory of the Department of Metallurgy of Columbia University, under the direction of Dr. Edward I?. Kern, and completed elsewhere. Acknowledgment is due to Prof. Arthur L. Walker, Dr. Edward F. Kern and Dr. William Campbell of the Department of Metallurgy, for their kind advice and for the inspiration derived from their instruction. This report is given under the following heads: Petrographic Description (Microscopic Study); Sampling and Preparing Ore for Treatment; Chemical Analysis; Treatment of Ore. Petrogeaphic DescRiption Texture: variable. Fine to medium mixed aggregate. Original Structure: Obscurc. Secondary structure: Fractured; healed. Mineralogy (Minerds are grouped for interpretation purposes and are arranged, in each group in approximate order of abundance)

Jan 1, 1916

By W. G. Matteson

I. Introduction...................................................... 436 (a) Extent of the Gulf Coastal Plain. (b) History of Important Gulf Coast Oil Pools. 1. Corsicans, Tex. 2. Spindletop, Tex. 3. Sour Lake, Tex. 4. Jennings, La. 5. Saratoga, Tex. 6. Batson, Tex. 7. Humble, Tex. 8. Caddo, La. 9. Vinton, La. 10. Naborton, La. 11. Red River, La. 12. Edgerly, La. 13. Goose Creek, Tex. 14. Damon Mound, Tex. 15. New Iberia, La. (c) Favorable Features of the Gulf Coast Pools. 11. General Topography and Physiography of the Gulf Coastal Plain.....440 111. General Stratigraphy of the Gulf Coastal Plain West of the 90th Meridian......................................................441 IV. Structural Types and their Characteristics.........................446 (a) hnticlinal Structure. (b) Structure of Salt Domes. 1. Domes of the Coast Prairie. 2. Domes of the Wold Region. 3. Recapitulation of Dome Structural Characteristics. V. Methods of Surveying and Prospecting............................. 454 VI. The Development of Salt Domes................- .................458 VII. Origin of Salt Domes...............4.............................461 (a) The Volcanic-plug Theory of Hager. (b) The Contemporaneous Sedimentation Theory of Norton. (c) The Theory of Upward Pressure Exerted by the Force of Growing Crystals, as Developed by Harris. VIII. Source of the Oil in the Gulf Coastal Pools.........................465 IX. Petrolific Value of the Salt Domes of the Wold Region..............467 X. Future Outlook.................................................. 467

Jan 1, 1918