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By C. A. Hansen

The furnace used for experimental work is shown in Fig. 1. One fireclay sagger, or pot, was set within another and the space between the two filled with Silox heat insulation. The hearth is a cast-iron plate with an imbedded ribbon of nichrome wire; this wire heater is connected to a potential regulator, which permits a very close voltage control. A mechanically driven arm is fitted with rabble blades so arranged that a uniformly thick ore bed may be maintained indefinitely. This arm is usually driven at about one revolution per minute but its speed of rotation can be varied as desired. Compressed air is led into the furnace through a meter, and it was found necessary to preheat the air in order to secure the definitely isothermal conditions sought. With this arrangement, it is possible to maintain any desired temperature constant within about 5" C. for any desired length of time and to

Jan 1, 1921

By Walter Miller

PETROLEUM refining, like other industries in the United States in 1940, focused much attention on its duties and opportunities in the field of national defense. In counter-distinction to the situation during the World War; the industry is well constituted as LO existing equipment, processes, and capacity together with planned additions to handle any demands that may be made upon it by the defense program needs. Evident throughout was the growing sense of ability to manipulate oil molecules for the production of materials not hitherto considered as being available commercially from petroleum The development and application of catalytically-induced reactions on a broad front is one of the distinguishing characteristics of refining progress during the year.

Jan 1, 1941

By E. von Maltitz

IN his highly interesting paper on "Piping and Segregation in Steel Ingots,"1 Prof. Howe emphasizes the effect of successive phases of internal pressure in the ingot in the evolution of gas, and the consequent formation of blow-holes. From his statements in other places, it may be inferred that he does not here intend to ignore the other variable factor, temperature, but rather to discuss this one more particularly. At all events, it is my purpose not to engage in controversy with Prof. Howe, but rather to contribute, towards the complete elucidation of this important subject which we all desire, my own views and experience. If, in doing so, I specially emphasize other factors than pressure, I need not be understood as denying what I do not think it necessary to discuss fully. Nor, in presenting my own original conclusions, need I be understood as claiming to be the first who ever reached or announced them. Many things are asserted or suggested upon inconclusive evidence; and to confirm such tentative propositions may be as valuable a service as to overthrow them. In the following passage, Prof. Howe adduces analogies, based upon the behavior of charcoal and of water, respectively, which seem to me questionable "In general, the. solvent power falls as the pressure falls ; and in general it rises as the temperature falls. Thus, to heat a solid, for instance charcoal, may expel part of its dissolved gas ; and a tumbler of water drawn cold from the faucet gradually evolves gas, as it stands and warms up on the sideboard." (p. 238.) Charcoal is a solid body, which has the property not only of absorbing gases in large quantities, but also of expelling the thus absorbed gases upon heating. A comparison between charcoal and iron as to the absorption of gases is scientifically not possible ; the gas-content of charcoal is partly due to the

Sep 1, 1907

By Otto Wartenweiler

AFTER the phenomenal development of the new mine, the United Eastern Mining Co., with Mr. Frank A. Keith as President, decided to install a reduction plant. The character of the ore, closely resembling the product of other mines in the district, did not offer any particular metallurgical problems, since these neighboring mines had been operating milling plants very successfully for several years. Thus, with the general metallurgical treatment fairly well-defined, the matter of next importance was to design and construct a plant as economically as possible, that would give the best results obtainable. The ore consists of a mixture of calcite and quartz in about equal quantities with some decomposed andesite, while the average value of mill heads were calculated to be $20 plus in gold, no silver being present. The tonnage to be treated at ,the start was fixed at 200 tons, but, in view of the favorable condition of the mine, it was considered advisable to arrange facilities, for increasing the capacity to 400 tons. . While it is best in some cases to adopt a distinct independent unit system where future enlargement is contemplated, in this instance the plans worked out differently. Summarized, the treatment adopted consists of coarse crushing, coarse grinding, fine grinding and cyanidation. For coarse crushing the selection of the No. 6 size gyratory crusher was governed not so much by its capacity as by the size of the feed openings to properly receive the run-of-mine material, which was too coarse for a No. 5 crusher. To accomplish the coarse grinding to. best advantage, a careful comparison was made between the modern steel ball mill-the last word in crushing and grinding-and one of its older, and, at that time better-established, competitors, the rolls.' The following conclusion was reached: While it is possible that for the sized plant under consideration the cost of operating rolls might be a little cheaper, it is preferable to use ball mills because a simpler arrangement is possible, and1 because. the handling of, ball mills is preferred by the operator.

Jan 11, 1917

By AIME AIME

THE Petroleum Division will hold its first fall meeting in Tulsa, Okla., Thursday and Friday,' Oct. 2 and 3, preceding the. International Petroleum Exposition that opens there on Oct. 4. Headquarters will be at the Hotel Mayo, and members planning to attend should make reservations promptly because of the large attendance expected at the Exposition. The program for Thursday will feature production engineering problems and that for Friday the unit operation of oil pools. The principal papers planned for the various sessions are as follows:

Jan 1, 1930

By Frances Hurd

WHEN 60:40 brass is heated to 825° C., given a drastic quench to obtain the beta solid solution, and reheated, various changes take place in the structure. Reheating at 200' C. causes a fine, granular, sorbitic structure to appear which has been considered alpha solid solution. These particles coalesce at higher temperatures of reheating, and at 470° C., the alpha forms twins. A further study of these transformations was considered worth investigating.

Jan 1, 1927

By Albert E. Wiggin

PagE I. Early History of Boston & Montana Mill at Great Falls (1891 to 1905). 210 a. Original Mill Built in 1891.........210 b. Coarser Concentration Tried...211 c. Screen Sizing of Fine Jig Feed Introduced..211 d. Installation of Finer Grinding.......211 e. Steam Stamp Tried in Place of Blake Crushers..... 211 j. Mill Increased from Three to Six Sections........ 213 g. Tonnage Increased from 300 to 450 Tons per Section... 212 h. Round Tables Replaced by Wilfley Tables....212 I1. Hancock Jig Replaces Evans Jig...212 a. Description of Hancock Jig...213 - b. Tests Made on- Hancock Jig..213 1. Treating Natural Feed..215 2. Treating Sized Feed..215 3. Treating Classified Feed .215 c. Tests Made on Evans Jig...216 III. Richards Pulsator Classifier System...218 a. Experimental Work.....218 b. Installation of System in Section No. 4,....... 220 IV. Woodbury Classifier and Jig System.............222 V. The Great Falls System................ 222 a. As Installed at Anaconda............ 224 1. Coarse Crushing and Jigging Division...... 225 2. Hancock Jig Division........... 226 3. Fine Middling Division.......... 229 4. Table Division............. 230 5. Slime Division.........230 b. Special Features of Great ails Flow sheet....... 231 1. Development of Hancock Jig Flow Sheet..... 231 2. Development of Finishing Table Flow Sheet.... 232 3. Treatment of Coarse Middling Table Products .. 232 4. Results of Test Made on 500-Ton Section at Great Falls Mill...........234 VI. Comparison of Great Falls and Evans System at Anaconda.... 236

Jan 1, 1914

By Alexander B. Morris

Studies such as the investigations into the solubility of gases in crude oil under various conditions, which have been carried on during the past three or four years, are very interesting from an academic point of view, but this consideration alone is hardly sufficient to warrant the large contributions from the industry necessary to maintain them. Some definite benefit to the industry as a whole should be forthcoming. The purpose of this paper is to direct the attention of company engineers, and company executives, to some of the ways in which the information gained from these studies can be made directly profitable. This work has two principal economic aspects. One affects the investment budget, and through it the financial requirements of the companies. The other affects operations, and through this course is reflected in current earnings. It will be shown that, as a direct result of the investigations into gas solubility, undertaken in the recent past by various investigators, it is now possible: 1. To determine more accurately the amount of reservoir oil originally present. 2. To obtain closer control on operating conditions, to effect more economical recovery. 3. To predict earlier and more dependably when and how much surface lifting equipment will be needed. 4. To reduce, or entirely avoid the very large investment in gasoline recovery equipment now frequently found necessary. 5. To control the gravity of the pipe-line oil so as to secure the greatest possible revenue from the products of the well. 6. To effect the recovery of a large amount of gasoline now wasted while the practicability of a gasoline recovery system is being decided. 7. To plan operations, by comparison with the history of old properties operated without this new information, so as to avoid the mistakes of ignorance made in the past. These points will be discussed in the following pages, though not necessarily in the order stated. There is so much overlapping of the points themselves, and of the data from which they have been drawn as conclusions, that to treat them in any particular order would require

Jan 1, 1935

By R. M. Howe, J. Spotts McDowell

Preparation and Use.—Magnesite is an important refractory in open-hearth, heating, and electric furnaces for steel-making and in many of those employed in the metallurgy of copper and lead. It is sold in the form of brick, finely ground "furnace magnesite" for bricklaying, and dead-burned grains for making and repairing furnace bottoms. The latter are a mixture of granules varying in size from pieces of about 5/8 in. (1.6 cm.) diameter to very fine but sandy particles. Dead-burned magnesite results from calcining the crude or lightly burned mineral at a temperaturc that will not merely drive off practically all the CO2, but will also cause sintering of the particles. During this process the pieces shrink considerably and become hard, dense, and inert to atmospheric moisture and CO2; under-burned material, on the other hand, will hydrate on exposure to the air. A small percentage of ferric oxide seems to be necessary for the production of a satisfactory sinter; from 4.5 to 8 per cent. in the dead-burned grains is considered the most desirable amount. Dolomite has been little used for brickmaking in the United States, but it is prepared for use in the granular condition calcined or "double-burned" and is the principal ingredient of several materials offered for sale under various trade names for refractory purposes. Dolomitic refractories are almost wholly confined to the open-hearth and electric furnaces, where they are used for fettling and as substitutes for magnesite. Much more magnesite and dolomite are used for basic open-hearth steel-making than for all other refractory purposes. The hearth of the furnace is usually built up of magnesite brick and dead-burned grain magnesite so laid that the brick base is protected by a working bottom of the granular material. The latter is sintered into place in layers 1/2 to 1 in: (1.25 to 2.5 cm.) thick to a total depth of 12 to 18 in. (30 to 45 cm.) at the center of the furnace. After each heat, burned dolomite is thrown against the banks as high as it will stick, and all holes in the bottom are Glled. At most plants such holes, at the end of each week, are also carefully filled with dead-burned grain magnesite. For temporary

Jan 1, 1920

By J. C. Trantham, J. W. Marx

From 1955 to 1958 the Phillips Petroleum Co. conducted a series of small scale counterflow combustion field tests in a tar sand about 60-ft deep and 6 to 12-ft thick near Bellamy, Mo. A total of seven different well patterns, including conventional five-spots and seven-spots plus a 15-well line drive pattern and a 10-well radial pattern, were employed. Electric heaters, gas burners and wellbore fuel packs were tested as counterflow ignition devices. Direct drive ignition followed by reversal to counterflow operation was not possible in this case because of formation plugging by the semi-solid tar during the direct drive phase. Sustained counterflow burning was achieved with wellbore fuel packs under conirolled conditions which permitted close correlation of fire front velocity, air velocity, air-oil ratios and yields for a wide variation in process parameters. The tar in place was about 10' APl with a reservoir viscosity greater than 500,000 cp. The composite oil prodlcct was 26' API with a viscosity in the range of 5 to 15 cp. Vertical sweep efficiency in the line drive pattern was essentially 100 per cent, with no evidence of gravity segregation. Original tar in place ranged between 800 and 1,000 bbllacre-ft, specific rock permeability averaged about 800 md before burning and effective air pemeability with residual oil and water in place (at the time of ignition) averaged 250 md. The volume of oil recovered during stabilized line drive counterflow burning represented about 67 per cent of the volume of tar originally in place in the burned out zones. A minimum was found when air-oil ratios were plotted against formation air velocities, and a limiting air velocity existed below which the counterflow fire front reversed and burned back over its own trajectory, using the residual coke left behind. INTRODUCTION Early in 1955 the Phillips Petroleum Co. began preparations to field test counterflow underground combustion as a method for producing oil from high viscosity hydrocarbon deposits, such as bituminous (tar) sands. At that time all published information on the use of underground burning io increase oil recovery was based on the direct drive process, in which the fire front moved through the formatim in the same direction as the injected air stream. Such direct burning is not applicable to many heavy oil sands or to most tar sands because the heat-thinned native hydrocarbon congeals in the cold rock ahead of the fire front forming a gas permeability block which smothers the combustion. Laboratory experiments first demonstrated that this permeability blocking would not occur if the fire front and the air stream moved in opposite directions. In this counterflow (reverse) burning process the heated heavy oil or tar is driven back through the combustion zone. Here thermal cracking produces relatively light hydrocarbon products which pass through the heated rock behind the fire front (largely in the vapor phase) and are incapable of causing a gas permeability block.' Exploratory wring revealed that consolidated bituminous sandstones with a combination of tar saturation, permeability, thickness and depth favorable for experimental field testing existed at several points in western Missouri. By the fall of 1955, a test site for determining technical feasibility of the counterflow process under field conditions had been selected near Bellamy, Vernon County, Mo. — about fifty miles north of Joplin. The pay zone was too thin and too shallow to constitute a commercial prospect, but these same factors permitted controlled experimental operation with a small compressor installation and with a large number of monitor wells. These were needed for adequate observation of the underground phenomena at reasonable cost. RESERVOIR CHARACTERISTICS The reservoir chosen for the experimental field tests was a 124 thick section of tar sand extending from 49 to 61 ft subsurface, with shale and siltstone laminations sealing the top and bottom. This section was part of a larger 30-ft thick tar sand deposit which extended both above and below the test zone. Core analyses showed that the 12-ft sand was effectively subdivided into two approximately equal sections, with the lower zone being consistently more permeable than the upper zone. The most significant laboratory core data are summarized in Table 1. The line drive test which is the principal subject of this report utilized only the lower 6-ft thick zone, with the upper zone regarded as part of the 55-ft overburden. WELL PATTERNS The over-all field test program involved a total of seven different well patterns, including conventional five-spots and seven-spots plus a 15-well line drive pattern and a 10-well radial pattern. In some of the tests the full 12-ft zone was employed; in other cases only the more perme-

Jan 1, 1967

By Ray W. Carpenter, Ralph Hultgren, Raymond L. Orr

Heats of formation of Au-Zn alloys of compositions Au3Zn and AuZn were rneasured at several temperatures by liquid tin solution calorimetry. The data for Au3Zn show that much smaller heat and entropy effects are associated with the a2- a1 transformation than for the a1 - a transformation. This result is consistent with reported X-ray diffraction studies which indicate that the a1 and (a2 phases have ordered structures which only slightly differ, whereas the a phase is disordered. The heat of formation of AuZn(ß') does not change significantly between 322o and 8000 K, confirming that the ß' alloy remains highly ordered to high temperatures. Not many measurements have been made of the energies of order-disorder transformations in alloy phases. In many cases these energies may be conveniently determined by measuring heats of formation as a function of temperature. Many alloy phases approximately obey Kopp's law of additivity of heat capacities; as a consequence their heats of formation do not change with temperature. In ordered alloys, however, a decrease in degree of order with increasing temperature will contribute an endothermic component to the heat of formation. Thus, for ordered phases where other anomalous contributions to heat capacity in the alloy or its pure components are absent, a measured change in the heat of formation may be attributed to the energy of disordering. A portion of the Au-Zn phase diagram1" is shown in Fig. 1. The composition AuZn(ß') has a well-ordered superlattice structure of the CsCl type at room temperature. The alloy is considered to remain ordered to its melting point,1 although, from X-ray diffraction data and electromotive force measurements of zinc activities, Terpilowski3 concluded that considerable disordering began at -673°K. The Au3Zn composition is a disordered fee solid solution (a) at high temperatures. Between 693o and 543oK, the ailoy orders to form the a1 phase, having a structure based on the L12(AuCu3) type, but with a regular distribution of ordering faults in the c direction, making it tetragonal. Below 543oK, the alloy orders further by means of slight atomic shifts, without diffusion, yielding a complex long-period orthorhom-bic superlattice structure, a2.4-7 Heats of formation of Au3Zn(a2) and AuZn(ß') were measured at 363°K by Biltz et al.8 by aqueous solution calorimetry. Heat capacities of several alloys between 14.9 and 38.4 at. pet Zn in the range from 373" to 723°K were measured by Iwasaki ef al.6 Stoichiometric Au3Zn, however, was not included in the alloys measured, the nearest composition being 26.1 at, pet Zn. Also, the heating rate used for the measurements, 2 deg per min, may not have permitted equilibrium to be reached in the neighborhood of the transformations. Heat contents of solid and liquid AuZn were measured between 488o and 1138°K by Kubaschewski.9 It was decided to determine the ordering energies of Au3Zn and to check on the possible disordering of AuZn by measuring the heats of formation of these alloys at several temperatures. The present paper reports measurements by liquid tin solution calorimetry of the heats of formation of the three phases of Au3Zn at temperatures within their regions of stability, and of AuZn at a low (322°K) and a high (800°K) temperature. EXPERIMENTAL Alloy Preparation and X-Ray Examination. Ten-gram ingots of Au3Zn and AuZn were prepared by melting weighed amounts of gold (99.95 pct Au) and zinc (99.99 pet Zn) together in sealed evacuated Vycor tubes at 1060°K, followed by rapid quenching. The resulting ingots were homogenized at 900°K for 10 days. The Au3Zn alloy lost no weight in preparation, the loss from the AuZn alloy was enough to introduce an uncertainty of only 0.1 at. pet in its composition. Filings for X-ray examination were taken from various parts of each ingot and strain-annealed at 723°K for 20 min in vacuo. The Au3Zn filings were quenched rapidly to retain the disordered phase. Diffraction patterns were determined with an X-ray dif-fractometer using copper Ka radiation.

Jan 1, 1968

By HOWARND N. EAVENSON

THE year 1930 resembled the preceding one in the coal industry in continuing the era of falling prices and 'of the abandonment of unprofitable mines. Practically all coal prices fell, and in the steam sizes during the last half of the year this was particularly true, due to the small industrial demand. No new mines of any size were opened in the bituminous coal industry, but there was a steady increase in the number of cleaning plants of all kinds built in all fields. It is estimated that at least nine million tons per year were added to the previous total of washed coal. The largest washing plant started during the year was that of the Buckeye Coal Co., at Nemacolin, Pa., with a capacity of 650 tons per hour. Fig. 1 shows - the mixing-bin, conveyor galleries, washing-plant and skip hoist, and Fig. 2 the 120-ft. Dorr thickener for collecting the 48-mesh material from the wash water. Dryers are used for drying the steam coal product. The following statement by J. R. Campbell shows the effect of cleaning on Pittsburgh coal in Greene County: "With the advent of the 650-t.p.h. efficient washing plant in Greene County at the Nemacolin mine of the Buckeye Coal Co., it has undoubtedly been demonstrated that the potential coking-metallurgical coals of the county can be brought within the pale of the highest grade high-volatile coals for steel manufacture. A few months' operation indicates that 9% per cent ash in the raw coal can be easily reduced to under 7 per cent ash in the washed coal and the sulfur from 1.60 per cent in the run of mine to 1.20 per cent sulfur in the washed coal.

Jan 1, 1931

By G. K. Burgess

(New York Meeting, October, 1913.) 1. COOLING AND HEATING CURVES BY G. V. BURGESS AND J. J. CROWE. § 22. THE results published in Professor Howe's paper 10 of our determinations on the Ac3 and Ar3 points for a series of commercial carbon steels 11 containing manganese in varying proportion, represent the average temperatures found by taking several (4 or 5) heating and cooling curves. The accompanying curves, Figs. 6 and 7, are, for each steel, the first heating and cooling curves as obtained by' the inverse-rate method of Osmond, using a cylindrical chronograph sensitive to -0.1 sec. for recording .time. Simultaneous observations were also taken by the differential method with a platinum neutral and plotted by Rosenhain's derived differential method and gave substantially the same results, the curves having sensibly the same contours in both cases.12. The observations were taken in vacuo on cylinders 5/8 by 1 in. in length bored to center with a 1/8-in. hole to receive porcelain insulated thereto-couple, and inclosed in an out- and in-glazed Berlin porcelain tube heated electrically by, platinum foil wound on the tube. The vacuum was usually better than 0.1 mm. The heating and cooling of the furnace was automatically controlled by a salt-water rheostat with shaped electrodes, giving a uniform rate of heating and cooling.

Jan 6, 1913

Jan 2, 1976

By D. K. Crampton

ON giving thought to the subject of this paper, my first reaction was that many and striking changes have come about as a direct result of the war. However, more careful analysis indicates that few, if any, of these changes can be wholly attributed to it. The actual situation is that all these changes were conceived and most of them at least partially executed in re- cent prewar years, it remaining the role of war to achieve results in a fraction of the time that might normally have been taken, lacking its driving impulse. The further discussion will therefore be with the premise that the individual changes have been greatly hastened rather than directly and primarily caused by any war conditions. Co-operation among copper alloy producers on production problems is agreed to be much worth while. The industry was too long noted for jealousy and secrecy as to equipment, methods, and even materials produced. Gradually, a more open and co-operative policy evolved but even just prior to the war the interchange of ideas was relatively cautious and limited. The need for a great increase in production in record time fostered a more co- operative attitude; exchange of ideas and experience concerning all phases of production increased tremendously to the benefit of the individual participants and thus the war effort, too. This more united effort has undoubtedly led to many specific improvements in process or equipment and these in turn to more rapid and economical operation than could have taken place on an each-for-himself basis.

Jan 1, 1944

By John Chipman, Theodore B. Winkler

IN order to understand more fully the complexities of the reactions occurring between the liquid steel and the slag in the basic open-hearth steelmaking furnace, investigations in this country and abroad have turned to laboratory equilibrium studies. This paper is one of a series of reports on investigations being conducted at the Massachusetts Institute of Technology. The experimental work was completed early in 1942. The slag systems found in the basic open hearth are very complex, being made up of at least eight major components and as many others whose effect might be classified as minor. The first two papers of the series, by Fetters and Chipman,l,2 as well as the paper by Taylor and Chipman,3 dealt with the simplest possible slag system that would resemble those found in the basic open hearth-the slag system consisting of CaO-MgO-SiO2-FeO. (Taylor's rotating induction furnace eliminated the necessity of contamination of the slag by MgO.) Having arrived at some reasonable conclusions regarding the physical chemistry of the reactions between molten iron and the simple slags at equilibrium, the next step was to investigate more complex slag systems. The major purpose of the present investigation was to determine what factors control the distribution of phosphorus between molten iron and the more complex basic slags at equilibrium, and to what extent these factors are influential. The slags used contained CaO, MgO, Si02, FeO, Fe203, P205, MnO, A1203 and CaF2, but not all of the slag samples contained all of these components at one time. REVIEW OF LITERATURE Although a number of interesting papers have been published on the subject of dephosphorization of an iron bath, there are as yet no results from laboratory studies that give thoroughly reliable information on the dephosphorization reaction. Even for the supposedly simple Fe-O-P system involving iron-phosphorus melts and iron oxide-iron phosphate slags, the experimental results are contradictory and no formulas have been established that adequately fit the equilibrium conditions. The Fe-O-P system has been studied by Schackmann and Brings4' von Samson-Himmelstjerna,5 Oelsen and Maetz,6 Bischof and Maurer,7 Diepschlag and Schürmann,8 and Herty,9 and the results of their investigations appear in Table I. A number of different equilibrium constants and distribution ratios

Jan 1, 1946

By William G. Pariseau

Advances in numerical methods of analysis and computer technology during the past decade have brought many formerly intractable ground control problems within easy reach of present day graduate mining engineers. However, the new technology brings with it new problems. The identity of these problems are largely those arising from a lack of familiarity with the capabilities and limitations of the new technology. In this regard, the central problem in ground control planning is the calculation of ground motion associated with mining. The fundamentals of this problem leading to a form suitable for computer programming are therefore reviewed. Solution procedures in the broad sense including the gathering of input data and the interpretation of output are described. Computer program capabilities necessary for ground control analysis are discussed and the steps necessary to implement an analysis are outlined.

Jan 1, 1983

By Barry K. McMahon

Following minor slope failures at the commencement of mining the west wall of the Kanmantoo Mine was redesigned from an overall slope between haul roads of 55° to 46°. This decision was based on a probabilistic analysis which indicated that 46° was the optimum economic slope.

Jan 1, 1983

By W. H. Bassett, C. H. Davis

ALTHOUGH brasses and bronzes have been made for ages, a systematic study of their physical properties has been carried out only during the years of the present century. Among these properties may be included those which are to be detected by means of microscopic examination; in other. words by the science of metallography. The earlier workers in this field, both in this country and abroad, gave their attention to steel. When the senior author explored the situation in 1902, there was little encouragement to be found in undertaking the study of the non-ferrous alloys. A start was made, and the metallography of the brasses and bronzes, as well as of the copper-nickel-zinc alloys developed materially under his direction. Annealing experiments were begun in 1902, and in the succeeding years the effect of temperature, and the influence of previous working, on the grain size of brass were studied. The conclusions so well known and widely published today were largely reached during those earlier years. . In 1905 the first complete annealing series were made. By this it is meant that brass and copper sheet, 5 B & S Nos. hard, was machined into tensile test specimens, then annealed under accurate control for 30 min. at temperatures up to the melting point of the material. Various determinations were made, including tensile strength and elongation in 2 in. There rapidly followed similar series on all of the copper-zinc alloys from 100 to 60 per cent. copper, on the bronzes, cupronickels, and on copper-zinc-nickel alloys. At this point there was published by Grard, in October, 1909,1 the very comprehensive and complete work on the tensile properties of cartridge brass, 90-10 copper-zinc, and electrolytic copper. The excellent photomicrographs in that paper illustrated the changes in structure produced by cold rolling as well as by annealing at different temperatures, but where Grard's work was confined to copper and to two alloys, the investigations in this laboratory have been over the entire fields of the commercial copper-zinc alloys, copper-tin alloys, representative copper-nickel and copper-nickel-zinc alloys as well as aluminum bronzes and others of a more special nature.

Jan 1, 1928

By W. M. Albrecht, W. D. Klopp, R. I. Jaffee, B. G. Koehl

Kinetic studies were made of the reactions of tantalum with oxygen, nitrogen, and air at 400o to 1500°C. The tantalum-oxygen reaction is linear from 500° to 1250°C. The tantalum-nitrogen reaction follows a cubic rate law at 400° to 700°C and a parabolic rate law at 800" to 1475°C. The reaction behavior in air is initially parabolic followed by a transition to linear behavior. In the search for high-temperature materials, considerable interest is being shown in the refractory metal, tantalum. It is the third highest melting metal with a melting point of 2996°C. Also, tantalum has excellent ductility, making it one of the most workable refractory metals. In considering high-temperature applications of tantalum, the oxidation kinetics of the metal must be known. Such information also serves as a basis for the development of corrosion resistant tantalum-base alloys. Therefore, this study was made to investigate the reaction of tantalum with air, nitrogen, and oxygen. LITERATURE Several oxides of tantalum have been reported. The pentoxide, Taz05, is the only oxide of tantalum whose identity has been established. A high-temperature modification, aTa2Os, has been reported by several investigators.1-4 A low-temperature phase, ßTa2O5, undergoes an allotropic transformation at 1320o to 1350oC. 5-8 Four other oxides of tantalum have been reported. The oxides TaO2, TaO, and Ta4O have been reported by schonberg.9 A suboxide Ta2O, was observed by Wasilewski 6. However, the presence of oxides lower than Ta2O5 is questioned by Lagergren and Magneli.7 In oxidation studies, vermilyeal0 and Peterson, et al.,12 reported one possible phase intermediate between Ta and Ta2O5. Only Ta2O5 was formed in the tantalum air reaction, as reported by Michae1.l3 Several studies have been made on the kinetics of the tantalum-oxygen reaction. vermilyeal4 investigated the range 50° to 300°C and found that the rate of growth of a thin adherent oxide film could be described by the Cabrera-Mott theory. Gulbransen and Andrew15,18 studied the reaction kinetics of tantalum in oxygen pressure of 1/10 atm at 250° to 450°C. At all temperatures the reaction followed the parabolic rate law for periods up to two hours. The oxidation behavior in the range 500" to 1000°C was found to be linear at oxygen pressures of 0.2 to 600 psi according to Peterson. et al.l1 At very low pressures (1 x 10-3 to 2 X lo-' mm of Hg) Gebhardt and seghezzi17 reported linear oxidation at 800° to 1500°C. The reaction of tantalum with air is similar to the reaction with oxygen. Studies have been made by Waber, et a1.,12 and Michae1.l3 Two nitrides of tantalum, TaN and Ta2N are known. Their structures have been determined by Brauer and Zapp 18,19 The tantalum-nitrogen reaction kinetics have been investigated by Gulbransen and Andrews. 15, 16 The reaction follows the parabolic rate law at 500° to 850°C at a nitrogen pressure of 1/10 ,atm. At the same temperature, the tantalum-nitrogen reaction is much slower than the tantalum-oxygen reaction. EXPERIMENTAL TECHNIQUES Material— The material used in this study was high-purity, electron-beam-melted tantalum obtained from the Temescal Metallurgical Corp. The hardness of the as received ingot was 76 Vhn. The analysis of the material is given in Table I. Methods—Cylindrical specimens of tantalum approximately 0.9 cm in diam and 0.5 cm in length

Jan 1, 1962