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By Howard Scott, Henry S. Rawdon

The method of demonstrating the structure existing in a metal or alloy at high temperatures, by etching a polished sample after it has been heated to the desired temperature, is quite familiar to metallog-raphists. The usual procedure1 2 is to heat the specimen, previously polished for microscopic examination, to the desired temperature, in a neutral atmosphere (hydrogen or nitrogen), then admit the etching gas (chlorine, hydrochloric acid or similar gas) for a few seconds, and finally, after flushing out the etching gas with the neutral one, cool the specimen in the neutral atmosphere. The pattern produced by etching at a definite temperature is usually taken as a record of the microstructure prevailing at that temperature. It has frequently been pointed out that changes in composition of the surface metal occur during the preliminary heating in the neutral atmosphere, so that the appearance produced by the etching at high temperature may not exactly represent the condition of the interior of the specimen. To overcome this uncertainty, the heating has sometimes been done in vacuo,3 the etching gas being admitted when the desired temperature was reached, then pumped out and the specimen cooled in vacuo. The studies of Rosenhain, Humfrey, and other workers 4, 5, 6, 7, 8 dem-

Jan 1, 1922

By Howard Scott, Henry S. Rawdon

The method of demonstrating the structure existing in a metal or alloy at high temperatures, by etching a polished sample after it has been heated to the desired temperature, is quite familiar to metallog-raphists. The usual procedure1 2 is to heat the specimen, previously polished for microscopic examination, to the desired temperature, in a neutral atmosphere (hydrogen or nitrogen), then admit the etching gas (chlorine, hydrochloric acid or similar gas) for a few seconds, and finally, after flushing out the etching gas with the neutral one, cool the specimen in the neutral atmosphere. The pattern produced by etching at a definite temperature is usually taken as a record of the microstructure prevailing at that temperature. It has frequently been pointed out that changes in composition of the surface metal occur during the preliminary heating in the neutral atmosphere, so that the appearance produced by the etching at high temperature may not exactly represent the condition of the interior of the specimen. To overcome this uncertainty, the heating has sometimes been done in vacuo,3 the etching gas being admitted when the desired temperature was reached, then pumped out and the specimen cooled in vacuo. The studies of Rosenhain, Humfrey, and other workers 4, 5, 6, 7, 8 dem-

Jan 1, 1922

By D. O. Noel

IT is, of course, expected that manufacture of the various metal powders should involve numerous methods adapted to the specific characteristics of the metals themselves. Several methods for powdering a particular metal may be available, but the physical characteristics of the powder as produced by the several methods may be quite different. In the final analysis, the application of the metal powder dictates the physical properties that the metal powder must possess, and this, to a very large extent, will determine which of several possible methods of manufacture is adopted. Sometimes powder of the same metal is produced by more than one method, each powder having specific characteristics that make it particularly suitable for its application. For purposes of classification, the various methods of powdering metals can be grouped as follows: 1. Machining. 2. Milling (by ball mills, stamps, attrition mills, etc.). 3. Shotting (pouring molten metal into water, air, etc.). 4. Granulation (by stirring molten metal while solidifying). 5. Atomizing (disintegrating by steam, compressed air, etc.). 6. Condensation of metal vapor. 7. Reduction of oxide powders. 8. Chemical precipitation. 9. Electrolytic deposition. 10. Sintering (for producing alloy powders). 11. Formation of an alloy followed by dissolving or otherwise remov-ing one of the alloying constituents.

Jan 1, 1938

By Charles Mitke

(San Francisco Meeting, September, 1915) INTRODUCTION THE Copper Queen mine is composed of seven divisions which are operated through the following shafts: Division Shaft Depth, Air Current No. Feet Uncle Sam 600 Downcast (shut clown April, 1914, to 1 curtail production) Southwest 600 Downcast 2 Czar 400 Downcast 3 Holbrook 600 Downcast 4 Spray S00 Downcast (shut clown April, 1914, to curtail production) 5 Gardner 1,000 Downcast 6 1 Dallas 1,400 Downcast 1 Lowell 1,600 Upcast 7 Sacramento 1,700 Downcast " I I The workings of the different shafts are connected by motor-haulage drifts on the even numbered levels. The general location of the orebodies and workings is illustrated by the vertical projection of orebodies of the district as shown in Fig. 1. The Uncle Sam, Southwest, and Czar workings have many connections to the surface through raises and extensive cracks that were caused by moving ground. These divisions are cool and are ventilated entirely by natural means. The Holbrook is ventilated partly by natural and partly by artificial ventilation, while the Spray, Gardner, Lowell; and Sacramento are ventilated entirely by mechanical means. In some of the divisions mentioned above a considerable quantity of air exhausts through shafts of adjoining properties.

Jan 9, 1915

By C. P. Lawhon, J. P. Simpson, W. M. Evans

Recent efforts to design drilling fluids for increased drifting rates have confirmed some laboratory results of other investigators, but have also produced additional data that should be considered. These data were obtained under controlled test conditions using a microbit drilling machine. Clays and some polymers have previously been reported to cause reduction in drilling rate. Recent data have shown that under laboratory conditions, suspensions of a single day or polymer have sometimes given faster drilling rates than when water was used. Measurements have been made of clay suspensions and polymer suspensions comparing filtration (I) under API conditions, (2) while drilling with temperature of 150F and differential pressure of 1,000 psi and (3) under dynamic conditions after drilling. Some correlation between instanraneous filtration (white drilling) and drilling rate has been observed. INTRODUCTION Several papers have been presented that related drilling fluids to penetration rate. Generally, it was found that a decrease in the solids concentration resulted in significant increases in the drilling rate. Of course, this change also resulted in a decrease in the viscosity of the drilling fluid.' Conclusions from investigations by this laboratory are in agreement. Data have shown that of the simple mud measurements commonly made at the drilling rig (density, plastic viscosity. yield point, API filtrate and total solids), only the density and total solids have a significant relationship to the drilling rate in Berea sandstone when attempting to correlate a single mud property individually.' More recent drilling rate experiments have been designed to study (1) effects of individual clays and polymers on drilling rates in Berea sandstone and Lueders limestone, (2) the relationship between drilling rate and dynamic filtration as measured after drilling and (3) the relationship between drilling rate and dynamic filtration as measured during drilling. Data show that drilling rates are dependent upon type and concentration of particles, type of formation and filtration of the individual fluids while drilling. Mud pressure: pressure of drilling fluid as measured after leaving the drilling chamber (Fig. 1). This is taken to be approximately the mud pressure just past the bit and at the face of the formation. Terrastatic pressure: pressure representing weight of overburden. Formation pressure: pressure of formation fluid as measured at outlet of drilling chamber (Fig. 1). This is taken to be approximately the pressure of fluid in the interstices of the formation. Differential pressure: difference between the mud pressure and formation pressure. LABORATORY EQUIPMENT AND TESTING PROCEDURE The drilling equipment was described in two previous publications."' Main components are a drilling chamber, filter-heater, rotary drive and variable-speed circulating pump. Auxiliary pumps supply pressure boosts for the mud, terrastatic and formation pressures. All equipment is designed for 15,000 psi and 500F. Capacity of the circulating system is approximately 7 gal. The mechanical design was facilitated by moving the rock down onto the bit. Data collected with this design should not differ from that obtained by a normal design where the bit moves into the rock. Drilling fluid is pumped through 50 ft of ID pipe coiled in an oil bath, enters the rotary shaft at a right angle and is pumped through the jets on the bit (Fig. 1). Most of the drilled solids are extracted by a screen mounted in the circulating system on the suction side of the pump. Data reported in this paper were obtained by controlling these parameters: mud pressure, 5,000 psi; formation pressure, 4,000 psi; terrastatic pressure, 5,000 psi; force on bit, 1,000 Ib; formation, Berea sandstone and Lueders limestone; flow rate, 7 gal/rnin; bit, 11/4-in. diameter with two 0.078-in jets; mud temperature. 150F; and rotary speed, 60 rpm. Mud pressure was controlled at 5,000 psi, thus giving a differential pressure of 1,000 psi even though the fluid densities varied. Cores of 3%;-in. diameter and 8 in. long were selected from quarry blocks to provide some control of grain size distribution, permeability and porosity. A 2-in. section was cut off each core and a I -in. diameter plug was taken from this section. Permeability to 5 percent by weight sodium chloride solution was determined and the large cores were

By G. A. Parks, C. Kovacs

The xanthate flotation of chrysocolla can be improved by preheating the ore to 500° to 600°C. Addition of water vapor reduces the preheating temperature required. The temperature range of flotation improvement correlates well with the range over which dehydroxylation occurs. This observation is consistent with changes in the structure and properties of the mineral as detected by measurement of solubility, D.T.A., T.G.A., X-ray diffraction, and infrared absorption and with recently proposed explanations of chrysocolla flotation. A brief experiment by one of the authors several years ago showed that exposure of chrysocolla to high temperature water vapor resulted in increased recovery by subsequent xanthate flotation. Recently renewed interest in flotation and thermal properties of chrysocolla1-5 prompted further study of this effect and more detailed reporting.6 This paper explores the response of pure chrysocolla recovery in Hallimond tube flotation tests to the time and temperature of exposure and to changes in the water vapor pressure. Brief attention is paid to the effects of such treatment on accessory minerals. A single experiment with flotation of chrysocolla from an ore is reported. MATERIALS Chysocolla from Inspiration, Gila County, Ariz. was crushed in a porcelain mortar, cleaned of visible and magnetic impurities, and screened to obtain -48 +65 mesh (Tyler) material for flotation test work. The clean material contained 28.5% Cu and was identified as chrysocolla by comparison of X-ray diffraction, D.T.A., and infrared absorption data with that reported for similar materials by others.4,5,7 Samples of malachite and chalcopyrite, prepared in a similar way, were also identified by X-ray diffraction. The sources of these materials are unknown. A sample of chysocolla-bearing oxidized copper ore from Pima, Ariz. was crushed and dry ground for thermal activation and subsequent flotation. PROCEDURES Activation: The apparatus used for exposure of materials to high temperature water vapor is illustrated in Fig. 1. The furnace temperature was controlled to ±5°C Water vapor pressure was controlled by pre-saturating a nitrogen carrier stream with water in an adjustable thermostatted saturator (multiple bubbler). A water manometer and capillary orifice flow meter were used to measure nitrogen flow rates for activation and for subsequent Hallimond tube tests. Gas flow rate and temperature were adjusted prior to introduction of samples. Exposure time was measured from the moment of introduction of the sample to the furnace, hence includes an initial drop below the control temperature. After heating, the samples were removed from the furnace and stored at room temperature in air. Representative samples of activated materials were examined by X-ray diffraction and infrared absorption.

Jan 1, 1967

By R. E. Ogilvie, N. L. Peterson

DURING the past few years there has been considerable effort devoted to the understanding of radiation effects on materials. The concept of the Frenkel defect and other lattice defects suggests that radiation may alter the rate of many metallurgical phenomena, especially those which are diffusion controlled. In 1953 R. R. Coltman and T. H. ~lewitt' found an appreciable effect on the ordering rate of Cu,Au due to fast neutron bombardment. Since then several rather comprehensive theories have been proposed on radiation enhanced diffusion in solids.2"4 If the energy of the radiation is above the threshold energy for the removal of atoms from their lattice sites, Frenkel defects will be produced. These defects can be produced uniformly throughout a relatively thick specimen by high-energy X-rays permitting bulk property studies without the limitation of sample dimensions. In this work high-purity arsenic containing 30 ppm of impurities was allowed to diffuse from the gase- ous phase at 700°C into single crystals of p-type germanium containing 0.1 ppm of indium. As the arsenic diffuses into the P-type germanium, an n-type layer will form in the diffusion zone. At the p-n junction the concentration ratio of the arsenic to the indium is constant. Experimental Procedures—The germanium specimens, 10 mm by 10 mm by 5 mm, were polished and etched to a mirror finish. The specimens were then sealed off in a vycor glass capsule at 3 x 10"5 mm Hg pressure with a sufficient amount of arsenic powder to produce a one-half atm pressure of arsenic at 700°C. Specimens were annealed at 700°C without radiation. The diffusion coefficient determined from these samples agrees within 8 pct of previous work done by Fuller.' Three specimens were given diffusion anneals at 700°C in a small tube furnace centered beneath the target of a 2-mev Van de Graaff generator. The specimens when in the furnace were 10 cm directly below the target of the generator. These specimens were irradiated continuously during the diffusion run with the Van de Graaff operating at 2 mev with a tube current of 225 to 250 pamp. The intensity of the x-radiation at the surface of the specimen inside the furnace was approximately 4.5 x l05 roentgens per hr. The temperature was controlled within m2°C by a chromel-alumel thermocouple throughout this work with no observed temperature change due to the radiation. By careful lapping, the samples were polished at an angle of 5 deg to the diffusion zone, giving a XI0 increase in the visible diffusion zone. The location

Jan 1, 1960

By Ralph Hultgren, David W. Mitchell

MAGNESIUM alloys usually are superheated before casting in order to ensure fineness of grain. Superheat temperatures in common use range from 1600° to 1700°F while the casting temperature, which depends upon the mold shape, is usually 200° to 300°F lower. The process of superheating requires considerable time and seriously shortens the life of the iron pots used. Recently it has been reported' that if acetylene, carbon dioxide or natural gas is bubbled through molten electrolytic A.S.T.M. No. 4 alloy at 1400°F. for 5 min., grain refinement equivalent to that of superheating will take place. Addition of certain solids such as graphite or aluminum carbide accomplishes the same results.2 As will be shown in this paper, it is possible to achieve grain refinement in magnesium casting alloys at low temperatures by mechanical stirring of the molten metal for a short time. This process was developed in the course of research work, supervised by the War Metallurgy Committee under the "Restricted" Project NRC-550, for the Office of Production Research and Development of the War Production Board. This paper, based on that work, has been released for publication by the O.P.R.D. MATERIALS AND METHODS The alloys studied were the most common American sand-casting alloys designated as No. 4 and No. 17 by the American Society for Testing Materials. The magnesium used in these alloys was of both carbothermic3 and electrolytic4 origin. Chemical analyses supplied by the producers are shown in Table I. Each heat consisted of approximately 5 lb. of alloy melted in a Tercod crucible. It was refined by fluxing with Permanente No. 7* refining flux at 1300° to 1350°F. After cooling to 1200' to 1250°F., portions of approximately one pound each were ladled into iron crucibles contained in an electric furnace at about 1250°F. The molten metal was covered with Permanente No. 21† covering flux and then heated to the temperature to be investigated. Normally each of the four portions was given a different treatment. In a typical case one portion was stirred vigorously for 5 min., acetylene gas was passed through a second portion for 5 min., a third portion was superheated to 1600°F for 15 min., then cooled to casting temperature, and the fourth was held for 5 min. at the temperature of stirring or gassing without other treatment. Each portion was then cast into one-inch diameter cylinders in three "nonturbulent" molds of identical shape. One mold was made of cast iron and the other two of baked sand. The cast-iron mold and one of the baked sand molds were heated to 360°F., the other baked sand mold was at room temperature. The freezing times in these molds were

Jan 1, 1945

By E. F. Jr. Young, H. E. Steinman, G. C. Smith

Through a progressive laboratory and pilot-plant program Jones & Laughlin Steel Corp has analyzed and corrected mine drainage pollution problems at all of its coal mines. In conducting this program, the company found no "typical" drainage discharge. Each discharge point at each mine was unique, so that varied approaches were needed to eliminate stream pollution. To illustrate the variety of these approaches, the treatment of drainage from foul, discharge points at three mines in Pennsylvania will be considered here. The flows and critical analyses of the drainage sources and treated effluents arc shown in Table I. Hydrated Lime Works at Thompson Borehole The discharge stream from the Thompson bore- hole at the Vesta No. 5 mine flowed into a small branch creek where it created a "yellowboy" deposit and affected aquatic life. Investigation indicated that hydrated lime would neutralize the acid and precipitate ferric iron without aeration. Treatment of the 150.000-gpd flow, however, created about 4000 gpd of wet sludge for which there was no nearby accumulation site. With State approval, this sludge was deposited through an unused borehole into an abandoned section of the Vesta No. 6 mine several miles away.

Jan 1, 1970

By R. L. Skaggs, R. A. Molsberger

DARKEN1 has pointed out that in most binary liquid metal systems the thermodynamic behavior is relatively simple in the terminal regions. Between the terminal regions. the thermodynamic behavior is more complex. To describe this behavior. he has defined the stability and the excess stability as shown: Qualitatively, an inflection in the free energy of mixing curve results in a change in sign, from positive to negative, of the stability function and is associated with a phase separation. Conversely, a large, positive stability over a narrow composition range is indicative of compound formation. Darken has shown a number of binary systems where the excess stability is constant in the terminal regions and varies sharply in between. The work described in this communication was undertaken to study the variation of stability and excess stability in a binary system as a function of temperature. In addition, this work provides means for the direct comparison of previously existing equilibrium (activity) and calorimetric (molar heat of mixing) data on the Hg-Sn system. Hildebrand2 measured the vapor pressure of mercury over Hg-Sn alloys at 595°K. Calorimetric studies were made by Kawakami3 at 523°K and by Kleppa4 at 423°K. In this work, the equilibrium vapor pressure of mercury was measured over a series of Hg-Sn alloys at 453" and 503°K by use of fused salt manometer with one arm exposed to mercury vapor. Deflections of the fused salt manometer were balanced by argon pressure on the other arm. Argon pressure was subsequently measured with a dibutyl phthalate manometer. Tin activities were determined by graphical integration of the Gibbs-Duhem equation making use of the familiar Darken5 a function. The activities of mercury and tin showed positive deviation from Raoult's law at 453 and 503°K as Hildebrand observed at 595 K. In Fig. 1 are plotted log activity of mercury and tin vs reciprocal temperature. The plot contains activities obtained from calorimetric studies. Hult-gren6 has calculated activities from Kleppa's4 data, and Kubaschewski7 has similarly treated Kawakami's7 data. Presumably. in each case a regular solution was assumed. For regions where a two-phase field

Jan 1, 1970

By Persifor Frazer

The rocks which cover the east flank of the South Mountain are chloritic schists typical in character. A specimen of this rock from near the Bechtel shaft, Hamilton Ban Township, Adams County, Pa., was selected and analyzed in my laboratory by Mr. C. Hanford Henderson, with the following results: Ignition,........2.740 CaO,..........7.040 SiO,,..........41.280 MgO,.......... 7.486 AI,O,,.........18.480 K,O,..........2.208 Fe,Os,.........9.440 Na,O,.........3.523 FeO,......... 8.200 100. As one penetrates the range by moving westvard, these schists are replaced either by epidotie quartz or by orthofelsite. In the former case, a belt of copper-bearing rock is traversed, but not in the latter case. Inasmuch as this junction of the chloritic schists on the southeast and orthofelsite on the northwest, separated by the epidotic quartz, is several times repeated, we find two or three copper belts arranged in general parallelism to the axis of the chain, because the copper horizon is generally at this junction. Thus, in going west from Fairfield, after entering the low spurs on the South Mountain, one is fairly within the chlorite measures. At the " Virginia Mills " a chlorite schist comes in with a dip of S. 1.5 E.-74 Half a mile up Middle Creek, large numbers of fragments of chlorite schist, decoruposed epidotic matter, and quartz are encountered. The former rock, where in place, dips E. 40" S.-57o. About 4000 feet west of the intersection of this road with the so-called Tape-Worm Railroad, near the house of one Singly, large masses of chloritie schist are found loose on the road. A hundred yards farther west, near a triangle in the road, the latter is less in quantity and much epidotic quartz appears, after which a very large display of orthofelsite succeeds on the left bank of Middle Creek. All these last-mentioned rocks, however, are in fragments. Crossing the stream again a few hundred yards farther On, the chlorite fragments at first preponderate, and then large numbers of both rocks

Jan 1, 1884

By J. Bruce Clemmer, P. E. Churchward, Carl Rompacek

The paper describes a cyclic method for processing manganese ores using sodium sulphate as the basic reagent. Sodium sulphate is electrolyzed in a diaphragm cell to give an anolyte sodium sulphate acid and a catholyte containing caustic soda, a part of which is carbonated in a cyclic manner to form soda and reduced ore is leached with the anolyte to dissolve the manganese and the impurities are precipitated by addition of catholyte. Manganese in the pregnant solution is precipitated as synthetic rhodochrosite with a carbonated catholyte, and sodium sulphate is regenerated. Calcining the manganese carbonate site a high-grade product and the carbon dioxide is returned to the carbonation step. the results of laboratory tests using cells equipped with synthetic fiber diaphragms and permselective membranes which permit transfer of using or cations during electrolysis are described. The article from which the above abstract is reprinted appears in Trans. AIME (1955) 203, p. 51; Journal op Metals (January 1955).

Jan 1, 1956

By S. R. Balajee, I. Iwasaki

The interaction between British gum 9084 and dode-cylammonium chloride (DAC) at quartz and hematite surfaces was established from coadsorption studies and streaming potential measurements. The cationic DAC interacts with the somewhat anionic British gum 9084, leading to the formation and adsorption of a binary complex of DAC-British Gum 9084 at the interface. The parallel ability to depress quartz along with hematite as a result of the interaction between DAC and British gum appears to be the main reason for the ineffective depressant action of starches and starch derivatives in the cationic flotation of iron ores. Amines are not particularly selective collectors for the flotation' of siliceous gangue from iron ores and, therefore, a suitable iron oxide depressant is needed for a satisfactory separation. Various starches and their derivatives have been extensively tested with oxidized iron ores,'-3 and it has been empirically established that British gums and dextrins are preferable. However, for the flotation upgrading of magnetite-taconite concentrates from 8 or 8.5% Si O2 to about 5% Si 02, British gums, which have been used so successfully on oxidized iron ores, have been found to have no effect and oftentimes are actually deleterious.4 In previous articles,5-7, starches were shown by adsorption measurements, flotation tests, and floccula-tion tests to interact with calcium ions in solution, and it was thought that a study on the interaction between starches and dodecylammonium ions would be able to shed some light on the anomalous flotation behavior described above. In fact, starches are known to interact markedly with paraffin-chain-type surface active agents and, thereby, to precipitate the starch or inhibit the iodine-starch reaction.8 From X-ray diffraction studies and viscosity measurements, the formation of a helical complex between mylose and a surface active agent has been postulated.9 The interaction with other types of hydrophilic colloids, such as synthetic polymers and proteins, has also been investigated and is usually explained in terms of van der Waals' force interaction and/or ion-ion interaction. In the present investigation, the interaction of British gum and dode cylammonium chloride on quartz and hematite was studied by adsorption and streaming potential measurements in an attempt to establish the mutual adsorption behavior of British gum and dode-cylammonium chloride on mineral surfaces and to clarify the anomalous depressant activity of British gum in the cationic flotation of iron ores. All the measurements were carried out at a natural pH of near 7 because dodecylammonium chloride gives maximum selectivity of flotation separation at this pH2 and to avoid any third parameter in the system. EXPERIMENTAL MATERIALS AND METHODS Minerals: The quartz and hematite samples used for the adsorption tests were prepared as described in a previous paper,"J except that the specific surfaces of the samples were increased to 5,860 and 16,000 Sq cm per gm, respectively. For the streaming potential measurements, the 48165-mesh fractions screened out of the original samples were etched with hydrochloric acid, washed repeatedly with water, and stored under water in Pyrex bottles. Reagents:DodecyIammonium chloride (DAC) was prepared1 1 by bubbling dry hydrogen chloride gas through a benzene solution of high-purity dodecylamine supplied by Armour and Co. British gum 9084, received from Corn Products Co., was solubilized by first dispersing it in water to produce a 0.05% solution and then homogenizing it in a blender for 5 min. Distilled water was used in the preparation of the samples and the solutions and for all test work. Adsorption Measurements: The procedure for the adsorption density determinations was also the same as that described in the previous paper.1° The residual concentrations of the British gum and the DAC in the supernatant solution were analyzed colorimetrically by the phenol-sulf uric-acid and amine-picrate methods, respectively. The validity of the mine-picrate method for the colorimetric analysis of DAC in the presence of British gum and the analysis of British gum in presence of DAC were checked by establishing calibration curves between optical density and concentration. Streaming Potential Measurements: The cell assembly for the streaming potential measurements was similar to that described by Fuerstenau.' The streaming potential

Jan 1, 1970

By J. P. Denny

The constitution of the Ga-In system was determined by thermal methods. An experimentally determined metastable equilibrium line (an extension of the indium-rich liquidus) was obtained. The various alloys were studied metallographically using polished samples obtained by a casting method. These low melting alloys required a special dry-ice assembly to maintain a suitable temperature. RECENT interest in alloys that are liquid at room temperature has led to rather extensive investigation of gallium-base alloys. Widely distributed over the earth, gallium could be produced in substantially larger quantities than at present, if a significant demand existed.' One study' has established its presence in 12 out of 14 zinc blends, in all of 15 aluminum ores, in 4 out of 12 manganese ores, in 35 out of 91 iron ores, and in all of 7 magnetite ores. It occurs as a rule in minute amounts, however, leading to high extraction costs. Recent quotations run from $2.50 to $7.50 per g. During the course of the present investigation, portions of the system Ga-In have been redeter-mined, and the results of this study are presented herein. Thermal and metallographic methods have been employed. Lecoq de Boisbaudran, the discoverer of gallium, conducted the first investigation" on Ga-In alloys in 1885. The temperatures of incipient melting, and of completion of melting, were determined at four alloy compositions. In 1936, Hansen' constructed a eutec-tic-type phase diagram for the system Ga-In, based on . work. The existence of a Ga-In compound was regarded as improbable by Hansen, and subsequent investigations are in agreement. French, Saunders, and Ingle3 conducted a more complete study of the system in 1938, using thermal methods. Their phase diagram is a eutectic type, containing a unique concave-upward liquidus. The solid-solution range of gallium in indium was reported as 9.5 pct by weight, and that of indium as less than 1 pct, at the eutectic temperature. The eutectic composition, determined as being bracketed by the compositions showing a true horizontal at the eutectic temperature (16°C), was reported as 76 5-0.5 pct Ga and 24 i 0.5 pct In. Experimental Procedure The preparation of Ga-In alloys is simplified by the low melting points involved. Various compositions were prepared by melting in pyrex tubes, using a cover of distilled water or parafin to prevent the alloys from wetting the glass wall. In all cases, the melts were homogenized. by stirring. Where possible, both cooling and melting curves were determined. The extensive undercooling of gallium was found to prohibit a satisfactory cooling-curve analysis of gallium-rich alloys, however, and transition points on the gallium side of the eutectic could be determined only by melting curves. The inverse rate method of thermal analysis proved to be most satisfactory and was used to a great extent. Various heating and cooling rates were used, ranging from 0.2" to 5.0°C per min. Low temperature melting analyses were conducted within a constant temperature bath, maintained at about 70 °C. The alloys were solidified (under water or paraffin) within a pyrex tube, using dry ice; the tube was then sealed within a cold Dewar flask, the unit transferred into the constant temperature bath, and periodic temperature readings taken. The high temperature melting-curve determinations and all cooling-curve determinations were made in a vertical tube furnace. At near-eutectic compositions, the furnace was placed within a refrigerated room held at —20°C. Accordingly, the furnace on cooling approached —20°C asymptotically and permitted the determination of those phase transitions occurring below room temperatures. Temperatures were measured with a 30-gage iron-constantan thermocouple, immersed directly in the alloy. To prevent contamination of the melt, the leads and junction were coated with Lucite, applied by painting with a solution of Lucite in ethylene dichloride. Electromotive force measurements were made with a Leeds and Northrup precision potentiometer, type 8662. The couples were calibrated against the boiling point. of water and, at lower temperatures, against a calorimeter thermometer having a Bureau of Standards certificate. The melting points of gallium and indium used in the present investigation were determined as 29.-77° and 156.1°C, in good agreement with previously reported values of 29.78°C° and 156.4"C.' The spec-

Jan 1, 1953

By H. P. Allen

THE Achotla mill of the Cia. Minera de Pe[n]oles is of special interest in that it is one of the few still employing the chloridization process. The ore milled comes from the Suriana mine and consists of both oxide and sulphide, from neither of which can the gold or silver be extracted by a simple cyanide treatment. The mill was built in 1927, after several years of study in the development of the process1, and operated from December of that year until October 1930. Operations were resumed in February 1935, and have been continuous since, treating approximately 5000 tons per month, while the mine is getting up to full tonnage of 6500 tons per month. Transportation Of Supplies The property is in Guerrero, Mexico, some 175 km. by airline southwest of Mexico City. The mill site is at Temisco (Fig. I), 8 km. from the Balsas River and 4.8 km. by aerial tram from the mine. At Temisco are the general office, shops, warehouses and laboratory serving both mine and mill. Here sufficient water is available either from a small creek running through the property or from the Balsas River, also convenient and ample storage space for the tailings. With the exception of the mine timber and a few native building materials which may be obtained locally, all supplies for both mine and mill are brought down the Balsas River from Balsas, the terminal of a Mexican National Railway line out of Mexico City. The method of transportation on the river is interesting. Rapids with very fast water are numerous, prohibiting the use of mechanically propelled boats. Those used resemble large, flat-bottomed rowboats some 22 ft. long by 8 ft. wide (Fig. 2). They are manned by two oarsmen sitting in the bow, each handling one large oar, and usually another man in the stern who, with his oar, assists in steering the boat, especially when the rapids are run. From 3 to 7 tons of freight are carried on each boat, depending upon the stage of the water, which governs also the time

Jan 1, 1937

By J. W. Freeman, E. E. Reynolds, A. E. White

Fram a study of 63 systematic alloy modifications it was found that molybdenum, tungsten, and columbium, added individually or simultaneously, and increases in chromium cause major improvements in 1200°F rupture strengths of Cr-Ni-Co-Fe base alloys. Rupture strengths were a function of the effect of composition modifications on both the inherent creep resistance and the amount of deformation the alloy would tolerate before fracture. THIS paper describes the results of an investigation of a series of alloys with systematic variations of the chemical composition of the following basic alloy: C, 0.15: Mn, 1.7; Si, 0.5; Cr, 20.0; NI, 20.0: Co, 20.0: Mo, 3.0; W, 2.0; Cb, 1.0; N, 0.12; Fe, 32.0 pct. The 62 modifications of this alloy were produced under conditions which minimized all factors influencing properties at high temperatures except composition. Melting, fabrication, and heat treatment were carefully maintained constant. Stress-rupture properties at 1200°F were used as the primary criteria of evaluation of the alloy. The objective of the study was to obtain data for determining the fundamental role of the influence of alloying elements on properties of heat-resistant alloys at high temperatures. In addition the results should be useful in determining optimum chemical compositions, the sensitivity of properties to variations in composition, and the degree to which alloy content could be reduced while retaining worthwhile properties. It is difficult or impossible to develop correlations between properties at high temperatures and systematic variations in chemical composition from published data for wrought heat-resistant alloys developed for gas turbines.' ' The main reason for this is the extreme dependence of the properties on conditions of treatment of the alloys." In most cases variation in final treatments between alloys so influences the properties that the influence of chemical composition is obscured. In addition it is recognized Table I. Basic Alloy and Some Modifications Used Basic AllOy, Variations in Element Pct Composition, Pct C 0.15 0.08. 0.40. 0.60 Mn 1.1 0.03,0.25.0.50,1.0,2.5 S1 0.50 1.2, 1.6 Cr 20.0 10, 30 Ni 20.0 0, 10,30 Co 20.0 0. 10, 30 MO 3.0 0. 1.2.3, 5, 7 W 2.0 0, 1, 5, 1 Cb 1.0 0.2,4,6 N 0.12 0.004, 0.08, 0.18 Fe 32.0 that variations exist between heats of the same alloy which are related to melting practice and that there is a strong possibility that conditions of hot working influence response to final treatments. The development of heat-resistant alloys has been based on the gradual accumulation of data roughly related to composition from extensive testing programs. There is every reason to believe that in most cases the optimum compositions have been achieved by this procedure in the alloys commercially available. There are, however, very little data showing the influence of systematic variations of composition free from the influence of other factors, particularly for alloys of the type investigated. Several investigators of cast alloys have demonstrated compositional effects, notably Grant,1-6 Epremian,t Guy,8 and Harder and Gow.9 Sykes10 eviewed the work on the wrought alloy Rex 78 and the systematic variations of carbon, copper, molybdenum, and cobalt leading to the development of the stronger Rex 337A alloy. From the papers by Wilson11 and Henry12 it is possible to deduce the beneficial effect of substituting cobalt for iron in 0.45 pct C-20 pct Cr-20 pct Ni-4 pct Mo-4 pct W- 4 pct Cb alloys. Wilson mentioned but did not present the extensive compositional studies involved in developing these alloys. Binder" showed optimum properties for 3, 2, and I pct, respectively, for molybdenum, tungsten, and columbium in 20 pct Cr-20 pct Ni-20 pct Co-30 pct Fe alloys for limited systematic variations of these

Jan 1, 1953

By Murray F. Hawkins, W. J. Ainsworth

In all types of subsurface pressure gauges the extension which occurs in the pressure-sensitive element is a function of the difference between the external (well or calibration) pressure and the internal pressure within the gauge, rather than a function of the external pressure only. The internal pressure is near atmospheric and depends upon (a) the quantity of air sealed within the gauge at the time of calibration or measurement, (b) the quantity of moisture (liquid water), if any, sealed within the gauge, and (c) the temperature at which the calibration or well measurement is made. Part of this correction for the change of internal pressure with temperature is taken care of by the customary temperature coefficient of the gauge. However, part of it is not, and while this portion may be only a few psi, it is nevertheless predictable or preventable, and should be considered in precision measurements. ERROR NO. 1 If air is sealed in the gauge at the same temperature and pressure for both the calibration and the well measurements, the usual temperature correction will take care of any difference between calibration and well measurement temperatures. However, if air is sealed within the gauge at temperature T1 and pressure P1 at calibration but at temperature T2 and pressure P2 for a well measurement, because different amounts of air are sealed within the gauge in each case, the internal pressure at. or corrected to, calibration temperature Tr will he different by where all temperatures and pressures are absolute. The calibration temperature is used, and not the well measurement temperature, because the usual temperature correction reduces the well measurements to calibration temperature. The correction term as calculated by the above equation is separate from. and in addition to, the usual temperature correction. Example: T, = 540°R, sealing temperature at calibration P, = 14.7 psia, sealing pressure at calibration T2 = 460°R, sealing temperature at well P2 = 14.7 psia, sealing pressure at well Tr = 660°R, calibration temperature AP = 660 [14.7/460 — 14.7/540] = 3.1 psi While this error is small even under these somewhat maximal conditions, it nevertheless represents a practical situation which did occur, and which as a matter of fact gave rise to this note. Where AP is positive, as above, the correction is added to the measured pressure; where negative, subtracted from the measured pressure. This correction should also be considered in successive calibration runs where the gauge, for example, may be warm from a previous calibration at an elevated temperature. ERROR NO. 2 Where a small quantity of moisture (liquid water) is sealed within the gauge at atmospheric conditions, the increased vapor pressure of the water at higher well or calibration temperatures will cause an increase in internal pressure. This moisture will come presumably from condensation within the gauge following temperature changes, from moisture on the operator's hands, and from atmospheric moisture (rain, mist, fog, etc.). Calculation shows that approximately 0.2 cc of water (three to four drops) is sufficient to saturate the air within an Amerada RPG-3 Gauge at 160°F, at which temperature the vapor pressure of water is about 5 psia. As the vaporization occurs in a sealed volume, the increase in internal pressure will be in excess of this 5 psi. At higher temperatures the pressures will be higher; however more water will be required to saturate the air within the gauge. Some experimental work was carried out with an Amerada RPG-3 Gauge at 200°F fitted with a 1,000 psi element, both with a dry recording chamber and with a small amount of water added. The results directly proved the existence of the error due to the presence of moisture, and, it is felt, indirectly, due to the differences in sealing temperatures and pressures, as both effects may be ascribed simply to an increase in the moles of gas within the recording chamber. SUMMARY In precision measurements the error introduced by sealing the gauge during a well test at a different temperature and pressure from that of calibration may be corrected for by using the equation presented, or it may be prevented by taking care always to seal the gauge at near calibration conditions. The error introduced by sealing moisture in the gauge may be prevented by taking care to keep moisture out of the gauge, or by removing the moisture by either warming or evacuating the gauge. Both of these errors are independent of the range of pressure measurement and the type of gauge, and are in addition to the usual temperature correction. ACKNOWLEDGMENT Appreciation is expressed to W. B. Kendall, Geophysical Research Corp., Tulsa, Okla., who pointed out the error from differences in sealing temperatures during some winter work in Canada. ***

Jan 1, 1956

By H. B. Pulsifer

ABOUT 15 varieties, or modifications, of the best magnesium available were prepared and subjected to etching tests, then examined for microstructure. Of the 30-odd etching reagents that were tried, nearly half, mostly ammonium salts, etched the metal satisfactorily. The surfacing and etching of magnesium is shown to be a very simple and quick operation. The density and hardness of magnesium were determined. The most interesting new observations relate to the finding of the hexagonal etch figures, the crystal laminations, and the fact that the metal is plastic, cold, when restrained or quickly deformed. Under slowly applied pressure cold metal deforms slightly, then shears to fracture without plastic flow. The chief structural features of magnesium are presented in two reduced photographs and 30 photomicrographs. MATERIALS TESTED There are only two sources in the United States from which new metal can be procured: the American Magnesium Corpn. and the Dow Chemical Co. No pronounced structural or property differences in the metals from these two companies were disclosed by the work of this investigation. The following materials were obtained from the manufacturers: 1. Massive crystals of distilled metal (American Magnesium Corpn.). 2. Rods of hot-extruded metal, ½ -in. squares and 5/8-in. rounds (American Magnesium Corpn.). 3. Sheet magnesium, 0.005-in. thick (American Magnesium Corpn.). 4. Cast stick metal, 1 3/8-in. dia. (Dow Chemical Co.). 5. Magnesium-aluminum alloy, hot-rolled plate, ½ in. thick (American Magnesium Corpn.). From these materials, were prepared: 6. Sections from a furnace-cooled ingot made from distilled crystal. 7. Cold-strained pieces from (6), (4) and (2). 8. Pieces cold-squeezed to fracture from (6), (4) and (2). 9. Hammer-struck pieces from (6), (4) and (2). 10. Steam-hammer struck pieces from (6), (4) and (2). 11. Sections from furnace-cooled ingot of the magnesium-aluminum alloy.

Jan 1, 1928

By Cyril Stanley Smith, Earl W. Palmer

A complete discussion of the literature on the subject of the influence of copper on iron and steel will be published elsewhere.' The present paper is concerned especially with the precipitation-hardening of copper steels, and brief mention will be made here only of the work of Kin-near,2,3 Nehl4 and Buchholtz and Koster,5 who alone have studied this phase of the subject. Kinnear found that normalized low-carbon steel castings containing about 1.0 per cent copper on drawing at temperatures in the neighborhood of 530" C. (1000" F.) increased in tensile strength and yield point, with little decrease in ductility. The maximum effect was obtained with about 0.9 to 1.0 per cent copper, and when the copper exceeded 3 per cent no improvement occurred on reheating. Kinnear did not study the effect of time of reheating—an all important factor where precipitation is concerned. Neh1,6 who apparently was unaware of Kinnear's work, recognized the change as due to precipitation and studied the interdependence of time and temperature of reheating, the temperature of the initial solution heat treatment, and the speed of cooling necessary to retain the bulk of the copper in supersaturated solution and to give an increase in hardness and tensile strength on reheating. Nehl found that if the final rolling or forging temperatures exceeded 700" C. (1300" F.) it was not necessary even to normalize the steel, but full precipitation occurred on merely reheating the forged or rolled shapes at 500" C. (930" F.). Buchholtz and Koster7 studied in detail the precipitation-hardening of a mild steel containing 1.0 per cent copper and 0.5 per cent chromium. From data on the electrical and magnetic properties of copper steels, they drew the portion of the equilibrium diagram in Fig. 1, assuming the

Jan 1, 1933

By G. C. Wallick

Since the appearance of the paper, "Solution of the Equations of Un-steady State Two-Phase Flow in Oil Reservoirs," by W. J. West, W. W. Garvin, and J. W. Sheldon,' a two-fold investigation of this subject has been carried out. One objective of the investigation has been to deter-mine the feasibility of solving such problems 7on a medium-size com-puter such as the Datatron*, and the other objective has been to in-vestigate the application of such cal-culations to experimental and theo-retical petroleum reservoir research. In the first Datatron calculations, the fluid and rock properties published by West, et al, were used, together with the published equations describ-ing the system. Details of the formu-lation not given in the original paper are discussed in the Appendix to this note. Reference should be made to the subject paper for the complete equations and defintion of symbols. An unexpected result of this in-vestigation was the discovery that the linear solution published by West was in error. Thus, in addition to describing the Datatron solutions and to discussing certain numerical diffi-culties which will be encountered if one uses the published method of solution, the purpose of this note is to indicate the nature of this error. LINEAR FLOW Since the linear case requires a minimum amount of scaling, a fixed-decimal point Datatron program was written for the one-dimensional flow problem and an attempt was made to duplicate the solution described by West. In the case described, fluid was produced at a constant rate, Q, until such time as well pressure reached 0.04. Production was then continued at constant pressure. From the constants and curves given by West it was determined that the ini-tial constant production rate could be approximated by Q = 0.007. An ini-tial dimensionless time step ?t = 0.434 X 10 - "as used, and each suc-cessive time step was doubled until a value of = 0.444 was reached. This constant interval was then used for the remainder of the solution. In subsequent solutions, several varia-tions in the time schedule were em-ployed, including smaller time steps and slower rates of increase in the time steps. In all cases, almost identical results were obtained regardless of the time schedule employed. However, as described below, it was noted that the time schedule had some influence on the rate of convergence of the solutions. As a check on the accuracy of the solution, the cumulative production at each time step was calculated using the two methods described in the Appendix. Satisfactory agreement was observed with the differences in these two values of the order of two parts in 50,000. It should be noted that the mass balance check as described is of questionable value, particularly with regard to the well pressure and saturation. This is especially true in the radial solution where pressure and saturation values near the wellbore would make only a negligible contribution to the numer-ical integration. It is believed, how-ever, that such a comparison is ot value in determining the over-all accuracy of a solution. In comparing the Datatron solu-tion with that published by West it was discovered that in the later stages of depletion, the pressures near the well declined more rapidly in our solution than in the West solution, and that the limiting well pressure of 0.04 was reached at an earlier time than that originally reported. It thus became evident that it would be impossible to duplicate the production schedule described by West and a constant rate of production was maintained until the well pressure was equal to 0.0. A representative comparison of the results published by West with those obtained in this investigation is shown in Fig. 1, which is a plot of GOR as a function of cumulative recovery. These two curves should be in agreement until a cumulative recovery is reached which corresponds to a well pressure of 0.04 — for the Datatron solution, a recovery of approximately 5.6 per cent. Actually, a major disagreement is evident. Subsequent correspondence

Jan 1, 1958