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By G. Krauss, W. Pitsch

The fine structure of the bcc martensite formed in an Fe-33 wt pct ATi single crystal of arrstenite is sho~on by transmission electron microscoPy to consist of combinations of transformation twins, stacking faults, deformation twins, and regular arrays of parallel screw dislocations. These structures constitute evidence for the multiple lattice-invariant deformations which operating during the formation of martensite could produce the real habit-plane scatter measured by a two-surface analysis of the plates formed in the single crystal of this investigation and reported in the literature for other Fe-Ni rnartensites. CRYSTALLOGRAPHIC theories1,2 of martensitic transformation show that the habit plane of martensite in a parent lattice is dependent in part upon an inhomogeneous distortion or lattice-invariant deformation which takes place on a fine scale within a martensite plate during its formation. Several recent theoretical papers3,4 have addressed themselves to an analysis of a wide variety of conceivable lat-tice-invarient deformations and the habit planes which they produce, while experimental investigation have been concerned with either the measurement of habit planes or the description and identification of the martensitic fine structure which reflects the nature of the lattice-invariant deformation operating during transformation. In Fe-Ni alloys with subzero Ms temperatures, the group of alloys with which this paper concerns itself, habit planes have often been found to scatter an amount greater than might be expected from possible experimental errors,5-7 and fine twinning has been identified as a major constituent of the fine structure of martensite.8-11 It has been suggested3,4 that more than one type of invariant shear occurs during martensitic transformation. This possibility has been experimentally supported12,13 by the observation of both dislocation configurations and twinning in a single martensite plate. The purpose of this paper is to report additional evidence for multiple lattice-invariant deformations in martensite and so to account for the real scatter in the habit planes of the martensite plates formed in Fe-Ni alloys. EXPERIMENTAL PROCEDURE The Fe-Ni single crystal was produced by pulling a high-purity iron and nickel charge through a single-crystal vacuum furnace in an alumina crucible. The crystal was double-melted to promote homogeneity and to increase its size by further additions on the second pass. In its final form the crystal was 4 cm in diam and 5 cm long. The nickel and carbon contents were analyzed at 32.9 and 0.006 wt pct, respectively. The austenite of this alloy first transformed to martensite by bursts at about -120°C, and, to preserve as much of the austenite as possible, all transformation was performed just below -120°C. Some observations were made on transformed samples which had been heated for 2 min at 340°C. It is assumed that the features of the martensite of these samples, Figs. 1 and 4, are the same as those of the as-quenched martensite. Orientation of the crystal by X-ray diffraction established 10.735 0.609 0.3161? as the axis of the crystal, an orientation that was checked within 2 deg by neutron diffraction. Further checks by electron diffraction of samples cut normal to the axis confirmed this orientation within the larger limits of error inherent in electron diffraction of thin foils. The X-ray orientation was the one used for the two-surface analysis of the martensite habit planes. A two-surface analysis was performed on the quadrant of the single crystal which had been oriented by both X-ray and neutron-diffraction techniques. Photomicrographs at X50 were made on two surfaces along an edge 2 cm long. Fiducial marks and the fact that many of the plates were almost completely surrounded by retained austenite made good matching of individual plates on two surfaces possible. The habit-plane trace on a surface was taken as the best line parallel to the long axis of a plate. A measure of the accuracy afforded by this criterion was provided by a family of very large plates which appeared at intervals along the entire 2 cm length of the edge. The plates all had habit-plane traces within 2 deg of one another. Many of the plates did not show midribs and, therefore, the use of midribs7 to represent habit-plane traces was not feasible in this investigation. The over-all experimental accuracy is estimated to be better than ±2 deg. Samples for transmission examination in a Siemens Elmiskop I at 100 kv were prepared by cutting 2-mm-thick discs from the single crystal, removing about 0.5 mm by chemical polishing,14 trans-

Jan 1, 1965

By J. J. Frawley, W. J. Childs, W. R. Maurer

The object of this investigation was to determine the growth habit of bismuth and bisrrtuth alloy dendrites as a function of supercooling. To do this, techniques were developed to increase the amount of supercooling in bismuth and bismuth alloys. For pure bismuth, the growth habit was dependent on the amount of supercooling. At low amounts of supercooling, about 10" C, prismatic dendrites were obtained. With increased supercooling, about 20 C, a hopper growth habit was observed. In many cases where hopper growth had occurred, the hopper dendrites were twinned during the growth process. This twinned surface enable prismatic dendrites to nucleate and grow by a twin plane mechanism. When the amount of supercooling was increased to about 25 °C, the growth habit was a triplanar growth. With still greater supercooling, about 3s°C, a branched growth habit occurred. The exposed planes on the prismatic, hopper,, triplane, and branched dendrites have been determined. The growth habit of the dendrites which grew along the crucible wall was found to have the (111) as the exposed plane, with <211> growth direction. It is apparent that dendritic growth of a metal is dependent on its purity and the solidification variables present. One of the solidification variables is the degree of supercooling. Supercooling, although often observed, has not been studied extensively until recent years. For dendritic growth to occur in a pure metal, the metal must be thermally supercooled. After the dendrites grow into the supercooled melt, the heat of solidification raises the temperature of the specimen to the melting point of the material and the remaining liquid will solidify at this temperature. Decanting is the removal of this remaining liquid before complete solidification. This removal of the remaining liquid after recalescence had occurred is a great aid in the study of dendritic growth. In this investigation, decanting was accomplished by a vacuum-decanting technique . Other investigators1-5 have studied the growth characteristics of various low-melting-temperature pure metals and alloys as a function of supercooling. However, large degrees of supercooling were not included. For their study of dendritic growth of lead, Weinberg and chalmersl employed a decanting technique which was achieved by pouring off the remaining liquid, exposing the solid/liquid interface. This method was employed later by Weinberg and Chalmers2 for the investigation of tin and zinc dendrites. The method for obtaining a solid/liquid interface was improved by Chalmers and Elbaum. They employed a triggered spring which was attached to the solidifying section of the specimen. Upon activation, the spring jerked the solid interface away from the liquid melt. In the study of growth from the supercooled state, a metal of low melting point which exhibited a high degree of supercooling was desired. Bismuth gave very consistent supercooling when a stannous chloride flux was employed. The maximum supercooling obtained was 91°C, with an average supercooling of between 65" and 75°C. The consistency of supercooling greater than 50°C was very high. The use of vacuum to aid in the rapid decanting of molten metal has proven to be very successful in this investigation. The vacuum gives a rapid decantation, usually leaving the solidified metal structure sharply defined. The purpose of this investigation was to study the effects of supercooling and the effects of alloy additions on the growth habit of bismuth dendrites. The structure of bismuth has been variously defined as face-centered rhombohedral, primitive rhombohedral, and hexagonal. However, bismuth has only one plane with threefold symmetry, the (111) plane, and the crystal-lographic structure is considered a 3kn structure. MATERIALS The bismuth which was employed in this investigation was obtained from the American Smelting and Refining Co. of South Plainfield, N. J. The accompanying spectrographic analysis data indicated the bismuth to be 99.999+ pct pure. The tin was obtained from the Vulcan Materials Co., Vulcan Detinning Division, Sewaren, N. J. It was classified as "extra pure". Nominal analysis was 99.999+pct. In order to prevent contamination of the bismuth melt from the atmosphere, an anhydrous stannous chloride (Fisher certified reagent grade) was added to each melt. The fluxing action obtained from the use of the chloride provided a large amount of supercooling in the specimen. APPARATUS A 30-kw, 10,000-cps motor-generator set, connected to a 6+-in.-diam air induction coil, was employed to melt and superheat the specimens. The temperatures were recorded by means of a chromel-alumel thermocouple and a potentiometric recorder. The thermocouples were 0.003 in. in diam, and were encapsulated with Pyrex glass to prevent the thermocouple from acting as a nucleating agent and also from contaminating the melt. Fig. 1 illustrates the vacuum-decanting apparatus when a liquid flux was employed. A standard 30-ml Pyrex beaker was placed on top of an asbestos insulating block. A 5-mm-ID Pyrex tube with aA-in. spacer tip attached to its end was used for the decanting tube. The spacer tip contributed significantly to a successful decanting operation. The tip located the opening of the decanting tube about -^ in. from the bottom of the

Jan 1, 1969

By G. M. Yocom

Blowing acid Bessemer converters with oxygen-steam produces steel of below 0.002 pct N2 content. This method of blowing, combined with a dephosphorizing treatment in the steel ladle, results in low-carbon steels of low nitrogen and low phosphorous (under 0.035 pet) contents, which has physical properties equivalent to open-hearth steels of similar analysis. Using a 50-50 mixture of oxygen and steam, the refinitzg rate is increased 25 pct over blowing with natural air, and scrap charge increased from 3 to 10 pet. Bottom life is normal with proper tuyere area and arrangements, fumes are decreased, yields increased, and hydrogen content is normal. THE acid Bessemer plant at the South Works of Wheeling Steel Corp., consists of two 15-ton bottom blown converters with a monthly capacity of 57,000 N.T. The product of the shop is skelp billets for continuous welded pipe and slabs for ordinary drawing and forming quality sheets. Approximately 50 pct of ingot production is regular Bessemer steel of natural Phos content and the remainder is a dephosphorized grade of steel made by a special treatment of the blown metal as it is poured into the steel ladle. The low Phos grade of steel has certain advantages over the higher Phos grade but since both grades were produced by blowing natural air, the N2 content was in the range of 0.015 pct which limited its application. In 1954 it was decided to explore the possibilities of blowing with a steam-oxygen mixture for the production of steel of both low N2 and low Phos contents. The necessary equipment was installed to operate one converter in this manner and early in 1955 an experimental run of 160 heats was made by blowing with a steam-oxygen blast and excluding natural air entirely. During this period the proper operating techniques were established, such as blast pressures, steam-oxygen mixtures, valves and instrumental control equipment, tuyere arrangement in the bottoms, blowing times and production rates, and a thorough study made of the final steel quality. Also during this experimental period the dephosphorizing practice was improved by the use of a tap hole below the lip of the vessel. This provided a clean separation of the acid converter slag and blown metal which made the dephosphorizing treatment more effective. The results of this experimental run dictated further development of this practice and a second run of 720 heats was made in 1957. The quality features and conversion cost results were in line with expectations and accordingly a 400-ton per day oxygen plant is now being installed. The plant is scheduled for completion in September of this year. This will provide sufficient oxygen to operate both vessels on steam-oxygen blast and delete natural air blowing entirely. The steel will then be below 0.002 pct N2 bar content and the dephosphorized grades will be between 0.015 and 0.040 pct Phos. STEAM-OXYGEN BLOWING The steam for the process is fed to the plant at 220 psig pressure through a 6-in. line. The high-purity oxygen is compressed to 200 psig and conducted through an 8-in. line. The oxygen from the main line is valved down to 100 psig and passed through a steam heated heat exchanger. The heat exchanger is regulated to supply oxygen at 300°F to the steam-oxygen mixing station. It is essential that the incoming oxygen be held at this temperature to avoid condensation of the steam with resulting excessive erosion of the clay tuyeres in the vessel bottom. Oxygen is admitted to the mixing chamber by a 6-in. hydraulically operated valve driven by the ratio control regulator on impulse from the flow of steam. Steam is admitted to the steam-oxygen mixture station through a 2 1/2-in. hydraulically driven valve. The ratio control regulator acts to increase or decrease oxygen input as the steam flow increases or decreases with changing positions of the Blower&apos;s control lever. The important point to note here is that steam flow always precedes the oxygen flow as a safety measure. The control valves have sufficient capacity to afford protection should blow pipe trouble develop. A 50-50 mixture for these 15-ton heats demands an oxygen flow of 3800 standard cu ft per min along with 317 lb of steam. The Blower&apos;s stations is provided with an indicating blast pressure gage, and indicating steam and oxygen flow meters. Signal and warning lights indicate the valve positions and line pressures. A control room at the real of the Blower&apos;s pulpit room houses the ratio control and pressure regulators, as well as the various meter bodies. The hand actuated wheels used to change the conditions are mounted on a panel on the front of the meter control house. The recording steam and oxygen meters used for totalizing and accounting purposes are also mounted on this panel.

Jan 1, 1962

By William G. Kranz

Discussion of the paper of WILLIAM G. KRANZ, presented at the San Francisco meeting, September, 1915, and printed in Bulletin. No. 101, May, 1915, pp. 927 to 930. M. PETINOT, Niagara Falls, N. Y. (communication to the Secretary*). -I have read this paper with considerable interest and agree perfectly with Mr. Kranz that steel for castings made in an electric furnace is not necessarily, because of that fact, all good steel, and also that the qualities which he mentions, such as absence of segregation, elimination of `sulphur, great tenacity, etc., can be obtained in an electric furnace if operated under proper metallurgical conditions. An unusually low content of sulphur in steel for castings is not, of course, an absolute necessity and the range of this element usually obtained in steel made in basic open-hearth furnaces is sufficiently low to meet all physical requirements. The main factor in making steel for castings, regardless of the process, is the complete deoxidation of the bath to prevent the formation of

Jan 12, 1915

By N. J. Grant, C. F. Flo, F. B. Cuff

An investigation of the Ti-Cr system has shown the presence of a complete series of solid solutions in the ß phase, with a minimum in the solid us near 50 pct Cr. An intermetallic compound, TiCr2, forms during cooling from the ß solid solution. There is a eutectoid reaction at the low chromium side of the system. IN view of the recognition of the potentialities of titanium and its alloys as important structural materials there has arisen a need for a systematic investigation of various titanium binary diagrams. Of these, the Ti-Cr system was of particular interest because of the improved properties imparted to titanium by small chromium additions. A literature survey disclosed a partial constitution diagram that had been suggested by Vogel and Wenderott,¹ This diagram, shown in Fig. 1, is the result of work done on the Fe-Cr-Ti ternary system. Alloys containing less than 43 pct Cr were not investigated. In addition to this, a study of alloys in the Ti-Cr system was reported by McPherson and Fontana.² Adenstedt3 furnished a number of dilato-meter curves obtained from specimens containing 5, 10, and 15 pct Cr. Very recently, McQuillan4 submitted a proposed diagram covering the complete range of compositions between titanium and chromium. This diagram was in general agreement with the one described here. Experimental Procedure Sponge titanium (99.7 pct) and electrolytic chromium (Bureau of Mines analysis: 99.03 pct Cr, 0.40 pct Fe, 0.53 pct O2) were used for the initial determination of the system. Subsequent refinement of points, particularly for the low chromium side of the diagram, was accomplished by using iodide titanium and high purity chromium (National Research Corp. analysis: 0.050 pct C, 0.045 pct O2). The Ti-Cr alloys were prepared by melting 25 g charges in an enclosed, water-cooled copper crucible using a movable tungsten electrode. The atmosphere was helium, prepurified by first passing it through a drying agent and then through sponge titanium heated to 850°C. Particular care was taken to avoid any large scale segregation resulting from insufficient mixing of the components. Each charge was melted and kept molten for approximately 1 min, allowed to cool, inverted, remelted, and kept molten for an additional minute. In order to ascertain the amount of impurity pickup (oxygen and nitrogen) during the melting procedure, three iodide titanium specimens were melted in sequence and then checked for increased hardness. The specimens in the as-cast condition showed a relatively large hardness increase over the hardness of the as-received iodide titanium. The scattering on these readings was large. However, after the specimens had been homogenized at 840 °C for 2 hr and slowly cooled, the measured increase in hardness over the as-received titanium was small with a corresponding decrease in scatter. The reason for this hardness change is that in heat treating these specimens below the transformation temperature (885°C) there was a conversion from the as-cast structure to the more nearly equilibrium structure of the annealed specimen. The alloys were analyzed for chromium content and although the actual percentage was invariably low the deviation from the nominal composition never exceeded 0.6 pct Cr.

Jan 1, 1953

By D. Watson, T. J. N. Grainger-Allan

A technique for studying the mechanism of the froth flotation process in which continuous froth removal does not take place but, instead, an equilibrium is reached between froth and pulp is described. A flotation cell, specially designed to facilitate equilibration, and froth and pulp sampling procedures are described. The main advantage of the technique is that the ability to measure the steady-state froth height allows froth-stability effects to be separated from pulp-process effects. In the flotation of hematite front quartz, linear relationships are found between airflow rate and froth height and between airflow rate and the ratio at equilibrium of mass of values in froth to mass of values in the pulp. A simple mechanistic interpretation of these results is given. It is suggested that froth-stability effects may play a more important role than hitherto allowed. In particular, the way in which concentration and size distribution of gangue particles may affect overall flotation rate is shown.

Jan 1, 1975

US 4,183,794 - Electrowinning zinc from a zinc sulfate solution produced by leaching zinc ore with sulfuric acid. The leach liquor is subjected to electrolysis in a first cell having an insoluble anode to deposit primary zinc on the common electrode. The coated electrode is transferred to a second cell having an alkaline electrolyte, and electrolysis is effected in the second cell to transfer zinc from the common electrode to the second cell cathode in a spongelike form which is readily stripped. R.H.C.L. Ross. Jan 15, 1980. 10 pp. (204-119). Filed: 12-22-77 (863,190). Same: Canadian 1,051,820, dated Apr. 3, 1979.

Jan 1, 1982

By Frank C. Smith

THE following article covers the history of a metallurgical campaign, commenced in March, 1905, at the mines of the Socorro Gold Co., in the so-called desert region of Yuma county, Arizona. The results obtained were simply a function of necessity, as will be seen from the description of the local economic conditions and the character of the ores treated. The mines and mill of the Socorro Gold Co. are located near the small village of Harrisburg, about 60 miles from Congress Junction, Arizona, which, at the time this work was undertaken, was the nearest railroad station, and from which all supplies were brought by wagon through the desert, at a cost varying from $10 to $15 per ton in addition to the railroad freights. Wood, the only available fuel, cost $7 per cord. Water for all purposes was pumped to the plant from a well in the valley about 4 miles away. Under the Arizona law, a working-shift is 8 hr. Wages were $6 per day for foremen and mill-men, $4 per day for blacksmiths and engineers, $3.50 per day for miners, and $3 per day for shovelers and trammers. The ore consisted of quartz, in which, above the 250-ft. level, the iron-minerals were largely oxidized and some free gold was visible; below that level few traces of oxidation occurred, and pyrite constituted the principal mineralizer in the quartz, together with occasional pockets of galena and a few eccentric specks of covellite. The 20-stamp mill was equipped with plates for amalgamation, and three Standard tables for concentration. The tails from the tables were elevated by a centrifugal pump to a launder, by which they were conveyed to a 60-ton cyanide-mill for further treatment. The cyanide-mill was erected at so great a distance from the stamp-mill that a separate crew of workers and a separate power-plant were necessary. No arrangement had been made for the treatment of the concen-

Jan 1, 1907

By R. J. Schaefer, M. E. Glicksman

Direct, in situ observation of metallic alloys during solidification reveals that in some systems crystal multiplication occurs by means of a dendrite remelt-ing process, without the necessity of independent nu-cleation events. The solidification is observed on optically clean surfaces of supercooled molten alloys. In one system (Sn-3 wt pct Bi) , a fine-grained equi-axed structure is produced by the complete disintegration, via remelting, of transient initial dendrites. In contrast, several other metallic systems show little or no evidence of remelting activity. The behavior of these metallic systems is consistent with that expected on the basis of published observations of dendrite remelting in transparent organic alloy systems. It is concluded that dendrite remelting is an important crystal multiplication process in some metallic alloys, but is velatively unimportant in some other alloys. The detachment of dendrite branches from the primary stem by a remelting process has been observed by Jackson, Hunt, Uhlmann, and seward1 during the solidification of some transparent organic alloy systems. The branches released by this remelting process can drift free of the primary stem and serve as seeds for the formation of numerous independent crystals. This proliferation of new crystals does not require repeated independent nucleation events, but only modification of the initial solidification structure. The mechanism of dendrite remelting, as described by Jackson et a1.1 and by Tiller and O&apos;&apos;Hara,2 is dependent on the transport of both heat and solute and is, therefore, expected to operate only in alloys, and not in pure substances. It was found in the transparent organic alloy systems that remelting occurred primarily in the constricted regions near the base of dendrite branches, where the branches had grown through the solute-rich liquid layer surrounding the primary dendrite stem. It was suggested that impure solid had formed in these constricted regions at a relatively low temperature and had later become unstable as further solidification of purer material raised the temperature. Jackson et al. proposed that the equiaxed zone of metal alloy castings originates from a similar remelting process, and they demonstrated the operation of this mechanism in "ingots" poured from saturated salt solutions. Although these substances were especially selected to show solidification behavior similar to that of metals,3 the remelting mechanism has, until now, been subject to the objection that its operation has not been directly observed in a metallic system. Considering the fact that thermal properties such as diffusivity may differ by as much as two or three orders of magnitude between metals and organic compounds, this objection was considered to be possibly serious. A method has now been developed by which it is possible to make direct optical observations of metals during solidification. This method has revealed transient solidification processes which would not be detected by metallographic examination of totally solidified specimens. In particular, a grain-refinement process in a metallic alloy has been observed to be a direct consequence of the total disintegration of an initial dendritic structure. The influence of an initial, transient solidification structure on the final solidification structure is demonstrated here for the first time in a metallic system. I) EXPERIMENTAL The technique of using a transparent flux to maintain an optically clean metal surface during solidification has been described by us elsewhere.* The

Jan 1, 1968

By J. W. Halley, G. L. Plimpton

Because of the two distinct stages in the solidification of rimmed steel, segregation in the rimmed ingot is more complex than that in the killed or semikilled ingot. In the earlier stage, chemical reactions, resulting in evolution of gas and vigorous stirring of the metal, effect a degree of negative segregation unique to rimmed steel. The composition of this zone constitutes the principal quality advantage of this type of steel. In the later stage of solidification, after the evolution of gas has ceased, the segregation follows the general pattern of a more completely deoxidized steel. However, the composition of the liquid remaining after the first solidification stage varies markedly from that of the original melt, some constituents having been partially removed as reaction products while the concentration of others has been intensified by rejection from the metal solidifying in the first zone. The aim, from the standpoint of segregation, in rimmed steel of high quality is to effect a maximum negative segregation in the rim zone without excessive concentration of undesirable elements at the center of the ingot. To achieve this aim, the composition of the melt may be varied and the furnace and pouring practice may be adjusted within certain limits. It is the purpose of this study to discuss segregation in rimmed steel from the standpoint of the mechanisms that produce it and to survey the phases of open-hearth practice that influence those mechanisms. Mechanisms Producing Segregation The mechanisms that determine the degree of segregation in the rimmed ingot are closely interrelated, making it difficult to select the primary factors and to determine a satisfactory order for presenting them. For instance, the question of sulphur segregation is relatively simple, since sulphur is not directly involved in chemical reactions in the ingot; but its concentration in the rim zone is dependent not only on its original analysis in the melt, its segregation coefficient, and the freezing rate, but also on the rate of its removal from the impure film on the solidifying surface. This washing action involves all the factors (such as freezing rate, the carbon-oxygen product, pressure, etc.) that determine the rate of gas evolution and hence the efficiency of film removal. Sulphur distribution between the rim and core is affected by the volumetric ratio between the two zones, and its segregation in the core is a function not only of the freezing rate of the core but also of all the foregoing factors that determine its concentration in the metal when solidification of the core starts. To simplify the presentation, it is proposed to treat the mechanisms affecting segregation independently in this section, reserving a discussion of their over-all effects for the section in which actual segregation data are given. The factors affecting segregation will be treated in the following order: (I) differential solidification, (2) removal of constituents as

Jan 1, 1945

By William Loblowitz

A simplified system of flotation testing has been developed recently at the Bureau of Mineral Research of Rutgers University. The technique involves the known principle of skin flotation and can be used with minute quantities of sample and reagents in a beaker. A vessel containing the conditioned sample with added water and flotation reagents is held inclined and rotated slowly. Water-repellent particles come in contact with air and float on the surface of the liquid, while wettable particles are submerged. The float is poured off and filtered whereas the nonfloat remains in the beaker. The filtrate may be returned to repeat the process. This procedure can be made quantitative. Separations are obtained and are remarkably complete and repeatable. The effect of different reagents, optimum quantities, pH and other variables can be determined in a fraction of the time required for conventional testing. However, the method gives no information on the effect of frothers and the quality of froth to be expected in a cell, and it is not practical for particles finer than 200-mesh. Unlike other preliminary tests, separate float and nonfloat products are obtained, and their contents can be determined quantitatively by chemical analysis or grain counts. After the optimum reagent combination has been determined, the effect of fines and frothing may be verified in the conventional flotation cell. On the other hand, agglomeration-tabling can be directly duplicated from beaker tests. Procedure: Five to ten grams of sample are weighed into a 100-ml beaker. Flotation reagents and a small initial quantity of water are stirred together; additional water is then added to produce the proper water-solids ratio. The beaker is then tilted to 45" and rotated slowly. After three to five rotations, liquid and float are poured off and filtered; the filtrate may be recycled until the separation is completed. One test generally requires less than 10 min. Reagent concentration and pH remain quite constant because of the recycling of the filtrate. Two to four tests may be made simultaneously, and the effect of varied conditions may be observed by comparison. Considerable time is saved in preparation and handling since small quantities of sample suffice for a series of systematic tests. Repeatability One test was repeated four times under constant conditions. The sample used was a quartz sand containing approximately 24 pct feldspar and some clay aggregates. The +28-mesh grains had been screened out, and most of those finer than 100-mesh had been removed by hydraulic classification. The results are presented in Table I. For comparison, 500 g of the sample were separated by agglomeration-tabling using the same reagent combination and quantities as given in Table I. The weight percent float was 18.3 pct, composed almost entirely of feldspar and with only traces of quartz. Most of the remaining feldspar was recovered in a middling product with 2.2 pct by weight.

Jan 1, 1952

By B. T. Wykoff

This paper describes an important function of mining in Southeast Missouri. The practice is a necessary procedure to prevent disintegration of the pillars. Although the technique is peculiar to this district, it might have application in other mines using room and pillar method. CONSIDERING the subject alone, this paper would cover only a mechanical treatise of pillar roping. Because the St. Joseph Lead Co. originated the practice, it is proper to give a short introduction to the company. It is also proper to describe pillars and discuss their purpose to justify expending large sums of money to preserve them after the surrounding area has been thoroughly mined. Because the St. Joseph Lead Co. originated the practice of back pinning with wedge bolts, patch plates and channel irons, and the pouring of substitute pillars of concrete, these too, are mentioned. The Southeast Missouri Division of the St. Joseph Lead Co. is the largest lead producer in the United States. About 95 pct of the present producing mines are in St. Francois County, which begins 60 miles south of St. Louis. The entire lead ore production of this county, at the present time, is mined and milled by this company, treatment plant capacity being about 22,000 tons per day. This area is also the oldest, lead having been mined at Mine La Motte, in Madison County, in 1723. Estimated production of all the various companies that have mined here is about 7,000,000 short tons of pig lead. Method of Mining The lead occurs in the ore as galena. Galena is found either in the form of disseminated or solid streaks, of varying thickness. Ore stratum is the Bonne Terre dolomite, which is about 350 ft thick, but almost all the ore is in the lower 100 ft. Ore is mined by room and pillar method in open stopes. These stopes vary in height from 7 ft to 200 ft, depending on the thickness of the pay ore in that spot. Back, or roof, is supported entirely by pillars. In a majority of stopes, after the loose scales are mined down, the back has remained solid for many years (fig. 1). Under ideal conditions pillars are spaced to form an equilateral triangle and are as small and as far apart as the height of the stope and the character of the back will permit. They vary in diameter from 10 ft to 50 ft and are from 18 ft to 50 ft apart, measured from the outer edges. In general, the pillars are approximately 12 ft in diameter, and 25 ft apart. The spacing is very uncertain because of the vagaries of the ore trend, the desire to better support breaks in the back, and the attempt to spot out the thinner ore by not placing one in the core of the ore body. Use of Structural Steel Channels In stopes where the back is bad because the overlying formations are thin with wet, weak and shaly

Jan 1, 1951

By B. T. Wykoff

This paper describes an important function of mining in Southeast Missouri. The practice is a necessary procedure to prevent disintegration of the pillars. Although the technique is peculiar to this district, it might have application in other mines using room and pillar method. CONSIDERING the subject alone, this paper would cover only a mechanical treatise of pillar roping. Because the St. Joseph Lead Co. originated the practice, it is proper to give a short introduction to the company. It is also proper to describe pillars and discuss their purpose to justify expending large sums of money to preserve them after the surrounding area has been thoroughly mined. Because the St. Joseph Lead Co. originated the practice of back pinning with wedge bolts, patch plates and channel irons, and the pouring of substitute pillars of concrete, these too, are mentioned. The Southeast Missouri Division of the St. Joseph Lead Co. is the largest lead producer in the United States. About 95 pct of the present producing mines are in St. Francois County, which begins 60 miles south of St. Louis. The entire lead ore production of this county, at the present time, is mined and milled by this company, treatment plant capacity being about 22,000 tons per day. This area is also the oldest, lead having been mined at Mine La Motte, in Madison County, in 1723. Estimated production of all the various companies that have mined here is about 7,000,000 short tons of pig lead. Method of Mining The lead occurs in the ore as galena. Galena is found either in the form of disseminated or solid streaks, of varying thickness. Ore stratum is the Bonne Terre dolomite, which is about 350 ft thick, but almost all the ore is in the lower 100 ft. Ore is mined by room and pillar method in open stopes. These stopes vary in height from 7 ft to 200 ft, depending on the thickness of the pay ore in that spot. Back, or roof, is supported entirely by pillars. In a majority of stopes, after the loose scales are mined down, the back has remained solid for many years (fig. 1). Under ideal conditions pillars are spaced to form an equilateral triangle and are as small and as far apart as the height of the stope and the character of the back will permit. They vary in diameter from 10 ft to 50 ft and are from 18 ft to 50 ft apart, measured from the outer edges. In general, the pillars are approximately 12 ft in diameter, and 25 ft apart. The spacing is very uncertain because of the vagaries of the ore trend, the desire to better support breaks in the back, and the attempt to spot out the thinner ore by not placing one in the core of the ore body. Use of Structural Steel Channels In stopes where the back is bad because the overlying formations are thin with wet, weak and shaly

Jan 1, 1951

By D. Turnbull, J. H. Hollomon

IN the most general sense, solidification refers to the formation of crystalline material from either a gas or a liquid. However, in this symposium, only the formation of crystals from liquids will be considered. Thus, in our present study the problem of solidification becomes that of determining the mechanism of the transition from a liquid to a crystalline solid, and our particular interest is in the transformation of metals from the liquid to the crystalline state. Metal liquids are seldom composed of only one kind of atom. Often solute atoms are added intentionally to make an alloy, or they may be present accidently because of incomplete purification. Furthermore, there may be small solid particles of various other crystals present in the liquid. Such small crystals may persist if their melting points are higher than any temperature to which the liquid is heated. Prior to solidification, the liquid metal usually is poured from one container to another. The second container, called the mold, usually is at a lower temperature than the container, or the crucible, in which the metal is liquified. The first solid that forms upon contact with the mold generally is of a different composition than the liquid, usually containing fewer foreign atoms or dissolved impurities. Heat is evolved upon solidification and is dissipated through the surroundings. Tree-like crystals, or dendrites, grow from the container walls and branch into the melt, enriching the remaining liquid in impurity atoms. In some alloys the remaining, relatively impure liquid continues to solidify until no liquid remains and the branches of the original crystal are cemented together. In other alloys, particles with a second type of crystal structure appear before solidification is complete. First the nature of the liquid and the solid states will be considered and then the mechanism of the initial formation of crystals from pure and alloy liquids. Later the problem of the growth of these crystals and the complexities of solidification in a mold, where the temperatures are not uniform and the composition of the melt changes continuously, will be discussed. LIQUID AND CRYSTALLINE STATES A liquid is an aggregate of atoms arranged with no apparent regularity (over distances of more than a few atom diameters). Nevertheless, any given atom generally has a definite number of nearest neighbors at definite distances, and thus order may be said to exist over a short range. In a crystal, on the other hand, a regular array of atoms continues for many hundreds or thousands of atom diameters, and a long-range order is apparent. Thus, a crystal having long-range order can be reproduced by linear translations for 10-5 cm or more of some fundamental unit possessing short-range order. A crude illustration of the difference between liquid and crystalline structures can be obtained by comparing the possible arrangements of oranges in a crate. If the oranges are simply dumped into the crate haphazardly until it is filled, the oranges will represent a static model of a liquid.

Jan 1, 1951

By Nathaniel Herz

The use of zinc dust for precipitating the pecious metals from cyanide solutions is well established now in many places, and has many advantages over the shavings method of precipitation. Although much work has been done o,n methods of testing zinc dust, as yet. no absolutely positive test has been devised to determine the value of the material. Certain facts are known, but often it happens that results on a working scale are not as expected from the laboratory tests. The purpose of this paper is to record some obscrvations made while testing a large variety of zinc-dust samples in the laboratory. W. J. Sharwoodl has described standard analytical methods, which have been followed, with the changes noted. The regular determinations include zinc oxide, by solution in ammonia and ammonium chloride, lead, and precipitating efficiency. In some cases cadmium was determined by a method similar to that described by J E Clennell.2 I will discuss the precipitating-efficiency test in detail. The procedure is as follows: "A solution of potassium silver cyanide is prepared by dissolving 10 grams of silver cyanide (AgCN) and 5 grams of 99 %&apos; potassium cyanide in a little water and diluting up to 1000 cc. It is then adjusted by addition of a little more XCN or AgCN until the solution indicates from 0.12% to 0.15% free KCN by titration with standard silver nitrate. The titration is best made by using a 10-cc. or 20-cc. sample, adding 1 CC. of 2 % potassium iodide, and a slight excess of ammonia, as the end point is then sharper. Or 15 grams of pure crystallized XAg(CN)2 may be dissolved in a liter of water and 1.5 grams XCN added. " Weigh out 0.5 gram zinc dust into a 300-cc. beaker. Add a few cubic centimeters of watcr and stir until zinc is well mixed, then pour in 250 cc. of the prepared solution, stirring vigorously. See that all lumps are broken up, and continue stirring for fully five minutes. Stir occasionally (at least every 10 minutes) until the end of two hours from the addition of the solution. Then filter upon an 11-cm. filter, wash precipitate thoroughly, sprinkle with test lead, wrap it carefully in the paper, place in a scarifier with about 20 grams test lead, burn paper cautiously in muffle, scorify five minutes, cupel at low temperature and weigh silver. Milligrams silver obtained from 0.5 gram zinc X 0.0606 = percentage precipitating efflciency."³

Jan 1, 1916

By J. D. Lindner, Gene E. Roark

Waterflooding operations in the Langston-Kleiner field. Young County, Tex., are described. Widespread application of formation fracturing has been practiced in both producing and injection wells. Field performance data arc cited which indicate than no detrimental effect on sweep efficiencies and that probable benefits in imectivily have resulted from the fracture treatments. I N T R O D U C I O N This paper is a report on a waterflood operation which is being carried out in the Lanpston-Kleiner field located in Young County, Tex. The oil reservoir aflected by this flood operation occurs in a Strawn sand member at an approximate depth of 3.550 ft subsurl&apos;ace. The operators of&apos; the project are Kleiner Estate. Turncr. Fiske. and West who are hereinafter collectively referred to as the Operators. Although the operation is unusual in several respects, the distinctive feature of this flood has been the widespread application of hydraulic formation fracturing treatments as a means to improve productivity and injectivity of the wells. It shall he the purpose of this paper to present basic information regarding the reservoir characteristics. op- craling practices, and waterflood behavior so that conclusions may be drawn concerning the effects which the fracture treatments have had on the performance of this water flood to datc. DEVELOP MENT Development of the 3,550 ft Strawn sand reservoir occurred during 1951 and 1952. The early development occurred on the Langston and Davis leases which arc in the northern region of the Operators&apos; holdings and the wells were drilled on 20-acre proration units according to the field rules. However, studies of the economics of this program. coupled with the decision to proceed with pressure maintenance by water injection. resulted in the adoption of wider spacing in the later stages of development. This variation in spacing is apparent upon inspection of Fig. I upon which only the 3,550-ft Strawn sand producing and injection wells have been located on the Operators&apos; properties. The development to the north of the operators leases is Ihe Garvey Strawn field and that to the south is the Taylor Strawn field. It wits determined that unitization of the leases to he involved in the waterflood program was not feasihle. Consequently. a system of offset injection wells, or lease line injection wells, was adopted from place to place as required to protect correlative rights in the program. This resulted in a dispersed array of injection and producing wells with relatively close proximity of wells along lease line areas and wider spacing toward

Jan 1, 1956

Discussion of the paper of E. W. Parker, presented at the New York meeting, February, 1913, and printed in Bulletin No. 75, March, 1913, pp. 443 to 451. A MEMBER :-I would like to call attention to the fact that the speaker has failed to indicate where is the center of gravity of the membership of the Institute, while he is dealing with this map. MR. PARKER :-I think you will find that a little further east. CHAIRMAN JAMES F. KEMP :-In connection with Mr. Parker&apos;s paper, I would like to inject a little matter of history into our program here, as regards the founding of the Institute. The credit for the founding of the Institute really applies to miners who were engaged in the anthracite coal region. The three men who signed the circular for the call for the meeting which brought the engineers to Wilkes-Barre in May, 1871, were Eckley B. Coxe, Richard P. Rothwell, and Martin Coryell.

Jan 5, 1913

By Ross E. BROWNE, Ross B. HOFFMANN

IT seems strange that a theory so devoid of value in its application to our practical problems should attract such widespread acclaim. This appears still more remarkable when one considers the foundation on which it is built. The criticism naturally suggested is as follows: First; the special theory of relativity is based on an assumption which is counter to the fundamental conception of relative motion. Second; the theory claims only a slight modification of Newtonian mechanics-a modification so minute that, even if true, it would have no practical value in its application to any visible occurrence here on earth.

Jan 1, 1931

By Robert B. Sosman

ONE of the most neglected fields for physicochemical education as well as for research is that of high-temperature phenomena. Few universities or technical schools give instruction in the physical chemistry of substances at high temperatures. On the contrary such instruction is almost entirely confined to the region between the freezing and boiling points of water. This field should be extended to a much wider range of temperatures, both low and high. Such an extension is logical, sound, feasible, and practical.

Jan 1, 1943

By W. C. Winegard, J. E. Gruzleski

The stages in the development of cells in the Sn-Cd eutectic have been studied by unidirectionally solidifying specimens under known conditions of growth rate, temperature gradient, and impurity concentration. By means of a quenching technique, the shape of the solid-liquid interface during solidification could be observed. Cells are shown to develop from defects or depressions which exist on the solid-liquid interface of even a pure eutectic. Th,e container wall, grain boundaries , and fault lines in the micro structure play an important role in cell development. A two-phase eutectic dendrite found at high impurity concentrations is described. L HE cellular or colony structure formed during eutectic solidification caused much confusion among early workers in their attempts to classify eutectic structure, and a major advance in our understanding of eutectic solidification was made when the colony structure was identified with a cellular interface caused by the presence of impurity elements.1&apos;2 To date, however, no detailed investigation of the stages in cell development in eutectics has appeared, and little work has been done on the cell morphology. The present paper presents the results of such an investigation. EXPERIMENTAL The Sn-Cd eutectic was used in this investigation with lead as the impurity element to promote cell formation. Materials of 99.999 pct purity were zone-refined to an approximate purity of 99.9999 pct. Alloys as close as possible to the eutectic composition, 67.75 wt pct Sn, were prepared using zone-refined tin and cadmium. The alloys were then zone-melted to the exact eutectic composition, as described by Yue and Clark,3 using a total of twenty to twenty-five passes on each eutectic bar. Only those portions of the bars which contained no primary phases were used in subsequent experiments. Master ternary alloys were prepared by melting together the required amounts of lead and the Sn-Cd eutectic in a sealed Pyrex tube under argon, and these alloys were then diluted with pure Sn-Cd eutectic as required. Unidirectional solidification was conducted vertically upward using the two-element resistance furnace shown schematically in Fig. 1. With this apparatus, it was possible to obtain a range of growth rates and temperature gradients so that the cell structure could be studied under different growth conditions. Growth rates in the range of 0.4 to 9.1 cm per hr and temperature gradients from 2.25° to 1475°C per cm were used. To ensure steady-state solidification, power to the furnace was stabilized, and the entire apparatus was enclosed in a large box in which the temperature was controlled to within ± 0.2°C. The apparatus was arranged so that the specimen could be quenched in situ during solidification by pouring a large quantity of water down the central vycor tube. Excellent delineation of the solid-liquid interface at the time of the quench was obtained because of the structural changes accompanying the rapid solidification of the remaining liquid. The quenching rate was always extremely rapid as no evidence of a transition in the lamellar spacing at the interface was ever observed. The alloys to be solidified were contained in degassed, high-purity graphite tubes, 1 cm OD and 0.6 cm ID. The specimens were about 18 cm in length. After the alloy had been cast into the tubes, three 0.8-mm holes were drilled in the tube to the center of the specimen. One hole was placed 1 cm from the bottom of the ingot, and the other holes were placed at 8 and 9 cm, respectively, from the base of the ingot. Thirty-four-gage chromel-alumel thermocouples were sealed in the holes. The lower thermocouple was used to position the solid-liquid interface at the start of each experiment,

Jan 1, 1969