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By W. Mostowitsch, H. O. Hofman

In our investigation of the Behavior of Calcium Sulphate at Elevated Temperatures with Some Fluxes,' we incidentally studied the decomposition of ferric oxide when heated in a current of dry air. We found that at 1,500° C., with 15-min. periods of heating, Fe²,O³, hardly changed in weight, the greatest loss being 0.23 per cent., and we therefore concluded that the compound remained unchanged at 1,500° C. in a current of dry air. In a more recent experiment we heated Fe²,O³, in a current of dry air and found that there was a decided loss in weight. A new investigation upon the behavior of Fe², O³, using a larger amount of substance and heating for a longer period of time, revealed the fact that a measurable dissocia-

Jan 1, 1910

By William G. Christy

EFFORTS at smoke abatement date back to the year 1273 in England when a law was passed prohibiting the use of "sea cole." The law was not enforced, so King Edward I, 33 years later, appointed a commission "to enquire of all such who burnt sea cole in the city or parts adjoining, and to punish them for first offense with great fines and ransomes, and for the second offense to demolish their furnaces." Many other commissions have since been named to investigate the smoke problem in England, but it still persists in many British cities. In the United States the movement to abate the smoke nuisance started in certain Middle Western cities, and has made considerable progress. Until recently, the coal-producing industry co-operated little in smoke¬abatement programs, taking the attitude that smoke elimination is the dealer's or user's responsibility; and the dealers, in turn placed the responsibility entirely on the user.

Jan 1, 1942

By C. Jardine, D. Freudenreich

The system concept is to minimize costly unscheduled equipment breakdowns by replacing components earlier than their life expectancy. Periodic unit services are scheduled according to preset constraints. Service sheets are generated by matching a job and component master listing based on assigned cyclic component lives. The system can account for all man-hours reported, and history information can be selectively retrieved. By reducing unscheduled equipment shutdowns, this system allows for better manpower utilization and an overall improvement in equipment reliability and availability.

Jan 1, 1982

By Charles Catlett

The terms " developed " and " undeveloped " are necessarily relative and cover a wide range; but the latter is here applied to cases in which the information at hand falls short of a clear demonstration of values, and conclusions must be reached frorn a study of the geological conditions of the particular deposit, interpreted in the light of similar and closely-related deposits. Such an inquiry might be characterized as an effort to reach reliable conclusions from insufficient data. But the engineer

Jan 1, 1909

By S. A. Mahon

AN interesting feature among the mining structures, on the Mesabi. iron range is the iron ore stacker erected in 1934 at the Mesabi Chief washing plant at Keewatin, Minn. It is built of structural steel, and carries a system of belt conveyors which collects the washed product of the plant and places it on a stockpile for subsequent shipment. Although the only one of its kind in the Lake Superior iron district, installations of similar nature have been used elsewhere in the handling of coal and gravel and in earthwork construction. The reasons for stocking Lake Superior iron ores may be as various and diversified as the methods used in building the piles. At the under¬ground mines the existence of the huge piles in evidence at each active shaft is due, principally, to climatic conditions in this north country where the shipping period is much shorter than the operating season. Conversely, at the washing. plants it may be desirable to stockpile washed ores because the shipping season is commonly of longer duration than the period during which the plants may be operated. Washed ores, and mixtures of which washed ores are a component part, have found high favor with the oper

Jan 1, 1935

By John Primrose

Tube stills having demonstrated their usefulness for refining operations, the later developments in their design have been in the direction of improved thermal efficiency. The earlier designs operated with low furnace temperatures and large volumes of furnace gas because the fuel was burned with much excess air. It was quite possible to provide sufficient heating surface to lower the temperature of the flue gas to within 150" of the temperature of the inlet oil, or when inlet-oil tempera-tures were high to have the flue gas escape at 300" or 350" F. by using the heat remaining in the flue gas from the still to preheat the air supplied for combustion. But even so, the thermal efficiency was low because of the large quantity of air used for combustion. The large quantity of excess air was required to burn the fuel in the furnace at a temperature low enough to prevent overheating the furnace walls and overheating of the oil. Supplying heat to the tubes of the heating surface at a rate beyond the capabilities of the oil to absorb, except with a considerable difference between the temperature of the inside of the tube and oil passing through, would result in overheating the tubes and the oil in contact with them. For these reasons it was very necessary in the older types of tube stills to burn the fuel with large quantities of excess air, resulting in low thermal efficiency despite the low flue-gas temperature. Neglecting loss by radiation, the thermal efficiency could be improved only by burning the fuel with less excess air, but it was necessary to accomplish this without upsetting the furnace temperature conditions existing when large quantities of excess air were used. There are several methods of bringing this about, such as controlling the furnace temperature by returning a proportion of the flue gas to the furnace, or by exposing direct to the fire a heat-absorbing surface so located and proportioned that sufficient heat will be absorbed by radiation to prevent excessive furnace temperatures.

Jan 1, 1928

By John Primrose

TUBE stills having demonstrated their usefulness for refining operations, the later developments in their design have been in the direction of improved thermal efficiency: The earlier designs operated with low furnace temperatures and large volumes of furnace gas because the fuel was burned with much excess air. It was quite possible to provide sufficient heating surface to lower the temperature of the flue gas to within 150° of the temperature of the inlet oil, or when inlet-oil temperatures were high to have the flue gas escape at 300° or 350° F. by using the heat remaining in the flue gas from the still to preheat the air supplied for combustion. But even so, the thermal efficiency was low because of the large quantity of air used for combustion. The large quantity of excess air was required to burn the fuel in the furnace at a temperature low enough to prevent overheating the furnace walls and overheating of the oil. Supplying heat to the tubes of the heating surface at a rate beyond the capabilities of the oil to absorb, except with a considerable difference between the temperature of the inside of the tube and oil passing through, would result in overheating the tubes and the oil in contact with them. For these reasons it was very necessary in the older types of tube stills to burn the fuel with large quantities of excess air, resulting in low thermal efficiency despite the low flue-gas temperature. Neglecting loss by radiation, the thermal efficiency could be improved only by burning the fuel with less excess air, but it was necessary to accomplish this without upsetting the furnace temperature conditions existing when large quantities of excess air were used. There are several methods of bringing this about, such as controlling the furnace temperature by returning a proportion of the flue gas to the furnace, or by exposing direct to the fire a heat-absorbing surface so located and proportioned that sufficient heat will be absorbed by radiation to prevent excessive furnace temperatures.

Jan 1, 1928

By AIME AIME

OCTOBER will be western month for the Institute. With meetings at Spokane, Tulsa, Los Angeles, and San Francisco, and with a large number of American Institute of Mining Engineers members and their families in the party sailing out through the Golden Gate to Japan on the afternoon of the tenth, the major activities of the Institute will, for this month at least, be west of the Mississippi. Despite cancellations due to necessity, most of the officers of the Institute will be present and taking part in some one or more of the Western meetings. Prof. Robert S. Richards, our senior past-president, will attend both the Spokane and San Francisco meetings and then go to Japan. President Bradley will preside at the San Francisco meeting and then head the party going to Tokyo. At Tulsa and Los Angeles, the principal officers of the Petroleum Division will be present and active and at all the meetings, directors, ex-directors and -present and past officers will be on the job and keeping things moving.

Jan 1, 1929

By B. D. Harden

FOR over fifty years the Spanish mine, 21 miles northeast of Nevada City, in Nevada County, California, has been one of the Bradley properties. Between 1883 and 1889 it was operated by the late Frederick W. Bradley and P. R. Bradley. The ore averaged only about $1 a ton at that time but the mine was credited with a production of about $900,000 in that period. The property was then closed down until 1922, when the Bradley interests reopened it and continued development for the next nine years, when a 50-ton mill was built. This began operation in April, 1931. This was a selective flotation plant, with the tailing treated on Wilfley tables, and operated on ore from the No. 4 and No. 16 tunnel stopes. This ran from $3 to $6 in gold, 2 to 3 oz. of silver, copper 0.6 per cent, lead 1.5,

Jan 1, 1935

By R. W. Mancantelli, J. R. Woodward

IN 1947 a large low grade deposit of uranium was located in the northwest corner of Saskatchewan, in the Beaverlodge property of Eldorado Mining & Refining Ltd. Most of the values occur as thin seams and as coatings on other minerals, and the ore, which is light and friable, is not amenable to the usual gravity methods of concentration. The acid leaching process developed to retreat the company's Port Radium tailings was also impractical, as the percentage of carbonates is high and the percentage of sulphides relatively low. Construction of the mill building and installation of equipment, both scheduled for 1952, awaited selection of a satisfactory ore dressing process on or before Oct. 1, 1951. An extensive research program on dressing of ores from the Ace mine therefore was undertaken by the Mines Branch in Ottawa, a research team at the University of British Columbia, and an ore dressing group at the company's Port Hope refinery. Pilot plant operations were conducted at the Ottawa plant of Sherritt Gordon Mines Ltd. under the general direction of C. S. Parsons, consultant on metallurgy and ore dressing for Eldorado. In mid-September, having compared results of the several research programs, Dr. Parsons recommended a process employing a carbonate or basic leach. He reported that, while the chemistry of the process had been proved, engineering of the flowsheet was incomplete, and he suggested that under normal conditions further pilot plant work at the Ace mine might be profitable. However, since this would involve a delay of 12 to 18 months in bringing the property into operation, he recommended that design of the concentrator proceed immediately. Concentrator capacity was determined by two considerations: 1) the amount of ore then available and 2) the expectation that continued improvements would be made in the ore dressing process as a result of the intensive research being carried out by the Mines Branch of the Department of Mines and Technical Surveys. As these improvements could affect both the chemistry and the en-

Jan 1, 1956

By R. W. Mancantelli, J. R. Woodward

IN 1947 a large low grade deposit of uranium was located in the northwest corner of Saskatchewan, in the Beaverlodge property of Eldorado Mining & Refining Ltd. Most of the values occur as thin seams and as coatings on other minerals, and the ore, which is light and friable, is not amenable to the usual gravity methods of concentration. The acid leaching process developed to retreat the company's Port Radium tailings was also impractical, as the percentage of carbonates is high and the percentage of sulphides relatively low. Construction of the mill building and installation of equipment, both scheduled for 1952, awaited selection of a satisfactory ore dressing process on or before Oct. 1,1951. An extensive research program on dressing of ores from the Ace mine therefore was undertaken by the Mines Branch in Ottawa, a research team at the University of British Columbia, and an ore dressing group at the company's Port Hope refinery. Pilot plant operations were conducted at the Ottawa plant of Sherritt Gordon Mines Ltd. under the general direction of C. S. Parsons, consultant on metallurgy and ore dressing for Eldorado. In mid-September, having compared results of the several research programs, Dr. Parsons recommended a process employing a carbonate or basic leach. He reported that, while the chemistry of the process had been proved, engineering of the flowsheet was incomplete, and he suggested that under normal conditions further pilot plant work at the Ace mine might be profitable. However, since this would involve a delay of 12 to 18 months in bringing the property into operation, he recommended that design of the concentrator proceed immediately. Concentrator capacity was determined by two considerations: 1) the amount of ore then available and 2) the expectation that continued improvements would be made in the ore dressing process as a result of the intensive research being carried out by the Mines Branch of the Department of Mines and Technical Surveys. As these improvements could affect both the chemistry and the en-

Jan 1, 1956

By Sherwin F. Kelly

THIS is intended as a simple review of the principles and practice of geophysics, so will not be of interest to the geophysicist, who is hereby warned of its elementary character. The engineers for whom it is written are those who, having glimpsed the formidable formulas and discussions of the geophysicists, give all publications on the subject a wide berth. For a few years now the geo-physicists have had a tendency to be ingrowing at their meetings, going deeper and deeper into theory and instrument construction, and forgetting to present the topics that would interest the practicing engineer who desires merely to know how geophysics can help him, not why.

Jan 1, 1934

By R. G. Jones, W. L. Kinney, R. E. Schilson, R. S. Wilson, G. A. Clark, H. Suralo

This paper discusses the results of the Fry conventional or cocurrent in situ combustion test, which was conduct-ed in a 3.3-acre inverted five-spot. The depth of the formation was between 880 and 936 ft; the oil had a specific gravity of 28.6° APl and a viscosity of about 40 cp at the reservoir temperature of 65°F. Preceding the combustion test, air injection tests were conducted which, in conjunction with geological studies, were used to evaluate the characteristics of the reservoir. Combustion was initiated on Oct. 13, 1961, with ignition being accomplished by a 40 kw electrical heater. The test phase of the project ended on Oct. 1, 1963. During the test, the average air injection rate was 1,520.-000 scf/D. Throughout the test, production of all fluids— gas, oil, and water—was monitored. Cumulative oil production credited to the project was 100,586 bbl. The cumulative air-oil ratio was 11,500 scf/bbl oil, and the oxygen uti1ization efficiency was 87 per cent. INTRODUCTION The Marathon Oil Co. conducted a successful in situ combustion test, beginning Aug. 22, 1961, at the Fry unit, Crawford County, 111. The purpose of the project was to test the feasibility of cocurrent in situ combustion as a means of oil recovery in the Fry type reservoir. Interest in in situ combulstion as an oil recovery tool has been stimulated mostly by the existence of large reserves of heavy viscous crudes with low expected recovery, usually less than 10 per cent. These are the so-called unrecoverable reserves, and most combustion tests to date have been conducted in this type of reservoir.1-4 In contrast, the Fry combustion test was conducted in a reservoir with a relatively high gravity oil having a relatively low viscosity. This paper discusses the performance of the test. The geology of the reservoir and the field operations are discussed in separate papers.5 TEST SITE The Fry combustion test was carried out in a 3.3-acre inverted five-spot portion of a lenticular body of Robinson sandstone. Net sand was 50 ft thick, porosity averaged 19.7 per cent, oil saturation was 68 per cent of pore volume, and water saturation was 20 per cent of pore volume. The oil in place was estimated at 1,040 bbl/acre-foot, or 171,600 bbl within the 3.3-acre pattern. The water in place was 326 bbl/acre-foot, or 53,800 bbl. The oil has a specific gravity of 28.7° API and a viscosity of 40 cp at the reservoir temperature of 65°F. AIR INJECTION PERFORMANCE Air injection took place in two phases, the phases separated by ignition of the reservoir. In the pre-ignition phase, air injection tests were conducted in the summers of 1960 and 1961. These indicated that the Fry reservoir was confined, and a high return rate of injected air could be expected. This proved to be an outstanding characteristic of the project, as cumulative gas production was 95.3 per cent of the air injected. The difference between the cumulative air injected and the total gas produced can be largely accounted for by the quantity of air stored in the reservoir. An estimated 16 X 10 cf of air remained in the burned-out portion of the reservoir and an indeterminate amount of gas was stored in the unburned but pressurized reservoir. Hence, a complete material balance of gases would account for nearly 100 per cent of the air injected. At times during the test, the daily gas production rate was 98 per cent of the daily air injection rate. Fig. 1 presents the air injection history of the Fry com-

Jan 1, 1966

By John Tyssowski

In 1925, Harry Howard Stout, then metallurgist for Phelps Dodge Corporation, while investigating the cleaning of cathode copper by various gases at elevated temperatures below the melting point of the metal, observed in the laboratory that particles of pure copper heated in a closed tube filled with hydrogen seemingly "stuck together." By further investigation he found that there was actual crystal growth across the boundaries of the particles of pure metal; in other words, there was a complete new crystal realignment and growth throughout the newly formed copper mass. It was coalescence, not adhesion; the several particles had become one unit. From this discovery has been developed the coalescence process, whereby copper of cathode purity is squirted out in semifabricated form from an extrusion press, by the application of about 3000 tons pressure on a 10-in. piston. Stout decided that cathode copper produced by electrolytic deposition was the logical source of the pure copper required for the coalescence process, but as there was no way of reducing the ordinary tough commercial cathodes to the small particles required he was confronted by a serious problem at the outset. Under his direction, this problem was solved by William H. Osborn and Harry Howard Stout, Jr. They developed the process and technique for producing cathode copper in brittle, friable form, and to them must be given the greater part of the credit for this phase of the development program as well as for that relating to the gas cleaning of the cathode particles. Concurrently, the three metallurgists worked on the problem of effecting a complete union of the cathode particles. Adequate washing was all that was needed to free the particles from electrolyte solution and slimes. A press was designed to produce briquettes of the proper porosity and density, and a method was devised of removing surface oxidation from the particles of cathode, by treatment in an atmosphere of deoxidizing gas at an elevated temperature. The temperature was determined at which the surface cleansing and preheating could be done in one operation, and for this a charging and preheating furnace in which there is maintained a positive pressure of deoxidizing gas atmosphere was designed. And finally, a method of feeding the heated briquettes of deoxidized cathode copper into an extrusion press without contamination from the air was evolved. For the final stage, a press was required because not only heat but pressure was required to obtain complete growth of the new crystals between the cathode particles as well as the elimination of all voids or non-coalesced areas. All essential stages of the process are protected by patents or patent applications in the United States and principal foreign countries, and the copper is produced on a commercial scale.

Jan 1, 1941

By John Tyssowski

In 1925, Harry Howard Stout, then metallurgist for Phelps Dodge Corporation, while investigating the cleaning of cathode copper by various gases at elevated temperatures below the melting point of the metal, observed in the laboratory that particles of pure copper heated in a closed tube filled with hydrogen seemingly "stuck together." By further investigation he found that there was actual crystal growth across the boundaries of the particles of pure metal; in other words, there was a complete new crystal realignment and growth throughout the newly formed copper mass. It was coalescence, not adhesion; the several particles had become one unit. From this discovery has been developed the coalescence process, whereby copper of cathode purity is squirted out in semifabricated form from an extrusion press, by the application of about 3000 tons pressure on a 10-in. piston. Stout decided that cathode copper produced by electrolytic deposition was the logical source of the pure copper required for the coalescence process, but as there was no way of reducing the ordinary tough commercial cathodes to the small particles required he was confronted by a serious problem at the outset. Under his direction, this problem was solved by William H. Osborn and Harry Howard Stout, Jr. They developed the process and technique for producing cathode copper in brittle, friable form, and to them must be given the greater part of the credit for this phase of the development program as well as for that relating to the gas cleaning of the cathode particles. Concurrently, the three metallurgists worked on the problem of effecting a complete union of the cathode particles. Adequate washing was all that was needed to free the particles from electrolyte solution and slimes. A press was designed to produce briquettes of the proper porosity and density, and a method was devised of removing surface oxidation from the particles of cathode, by treatment in an atmosphere of deoxidizing gas at an elevated temperature. The temperature was determined at which the surface cleansing and preheating could be done in one operation, and for this a charging and preheating furnace in which there is maintained a positive pressure of deoxidizing gas atmosphere was designed. And finally, a method of feeding the heated briquettes of deoxidized cathode copper into an extrusion press without contamination from the air was evolved. For the final stage, a press was required because not only heat but pressure was required to obtain complete growth of the new crystals between the cathode particles as well as the elimination of all voids or non-coalesced areas. All essential stages of the process are protected by patents or patent applications in the United States and principal foreign countries, and the copper is produced on a commercial scale.

Jan 1, 1941

By C. A. Stetefeldt

The hacienda Sauceda is one of the largest and finest haciendas in the vicinity of the City of Zacatecas, Mexico, and is said to reduce ores by the Patio process more cheaply than any other establishment. It receives its supply of ore from the San Acacio mine. This mine has been for some time, like most of the Zacatecas mines, out of bonanza, and yields, at present, ore of rather low grade. The silver occurs principally as silver-glance, ruby-silver and native silver, associated with pyrites of iron and copper, and some galena and zinc-blende, in a gangue of pure quartz, which takes the form of amythyst whenever the ore is of high grade. All the ore, as it comes from the mine, is broken by hand into small pieces, and sorted before it is delivered to the hacienda. Here it is first crushed dry in Chili mills, and then ground wet in arrastras to an impalpable powder. The sulphurets not decomposed in the patio process are separated in the settlers from the tailings and concentrated by hand. By roasting them in a reverberatory furnace with carbonate copperores, "magistral" is obtained. All machinery is driven by mulepower.

Jan 1, 1885

By E. E. White

(Cleveland Meeting, October, 1912.) IN, August, 1911, I read a paper before the Lake Superior Mining Institute' on surveying and sampling diamond-drill holes. The present paper gives a more thorough description of these methods, together with a few changes and notes suggested by further experience. Since August, 1911, the methods, used constantly by the Cleveland-Cliffs Iron Co., have been developed to a higher degree of efficiency, and have given great satisfaction. Until a few years ago but little attention was paid to the determination of the actual course of drill-holes, to the accurate sampling and analysis of the material, or to the scientific location of the drill-holes. It has now been common practice for several years in many districts to test the inclination of drill-holes by etching glass tubes with hydrofluoric acid, but the direction of deviation from the vertical has not often been determined. Methods of determining the direction by means of a compass were first developed in connection with drilling in Victoria. The latest method used on the Rand in South Africa has been recently described by John I. Hoffman.2 In the same paper Mr. Hoffman describes an ingenious method of wedging-off a drill-bole so as to start new holes at several successive points. By this means a hole can be deflected in any desired direction, and the curvature can be controlled to a considerable extent, provided the rock is soft enough to permit the hole to be wedged off. Unfortunately, in the Lake Superior district, the jasper iron-formation is so hard that it is very difficult, if not impossible, to do this. I tried to deflect one hole so as to avoid drill-rods stuck in the hole, by using a 1 Proceedings of the Lake Superior Mining Institute, vol. xvi., pp. 100 to 120 (1911). 2 Recent Practice in Diamond-Drilling and Borehole Surveying, Bulletin No. 91, Institution of Mining and Metallurgy (Apr.. 11, 1912).

Nov 1, 1912

By Kenneth Seaver

It is rather gratifying that in the field of the manufacture of refractories, in which, as a whole, foreign practice has surpassed us, the United States stands pre-eminent in the making of silica brick. In some instances European manufacturers have refused point-blank to credit the possibility of making to such specifications as are Common with us, until the actual completed shapes were shipped for inspection. But both the manufacturer and consumer in foreign lands are now frankly learning from us, and benefiting by our advanced practice in this field, as is evidenced by the orders placed here and the efforts put forth abroad to come up to the standard of American-made material. In no metallurgical operation has the employment of silica brick spread with such leaps and bounds as in the building of plants for the carbonization of coal, particularly in the byproduct coke oven. Today, in practically all types of oven, the structure above the floor level (except the facings) is of silica, while in the recuperative and in some regenerative types, its use is extended to that portion of the oven below the floor as well. By reason of the fact that there are a number of classes of refractories of higher silica content than the usual so-called fire-clay brick, there is sometimes a misunderstanding as to the class of material referred to as "silica" brick. We here refer only to a brick having a silica content of 94 per cent. or more and made usually from quartzite rock with a small percentage of lime as a binder. The term "silica" brick is sometimes rather loosely applied to brick from highly siliceous clays, or to a quartzite refractory of mingled fire-clay and quartz rock; but such products are not considered in this discussion. : Materials The rock from which practically all high-grade silica brick are made is a true quartzite or metamorphosed sandstone, variously known as

Jan 1, 1916

"The building stone industry of Utah has developed slowly on account of the limited market offered. The state has large and varied deposits of granite, limestones, marble and onyx.Three cement companies manufacture Portland cement in the Salt Lake valley. Brick clay, fire clay and clay for sewer pipe is found in the vicinity of Salt Lake City and Ogden.Large deposits of gypsum have been found in several localities in Utah. The gypsum deposit near Nephi has been developed to be one of the most important plaster producers in the western country. This gypsum occurs in large quantities and is exceptionally pure.Oil and Oil ShaleVast deposits of rich oil shale occur in the Green River formation of the Tertiary rocks in the Uintah Basin, northeastern Utah. It is estimated by the United States Geological Survey that the basin contains at least 92,159,000,000 tons of shale which will yield as much as 15 gallons of oil to the ton when distilled. These shale deposits indicate that ultimately Utah will be one of the leading shale oil producing states of the country. Some development work and considerable experimental work has been done, but overproduction of petroleum and general low prices afforded little incentive to the oil-shale operator, consequently no commercial production has yet been established in Utah."

Jan 1, 1925

By R. W. Bartlett

The rates of oxidation of tungsten have been determined at temperatures between 1320" and 3170°C and oxygen pressures to 1 amn using a surface -recession measurement technique. Above approximately 2000°C and 10-6 atm the rate is independent of temperature and can be calculated from gas collision theory assuming a constant reaction probability, e, of 0.06. Oxygen molecules react at surface sites where oxygen atoms have previously chemisorbed. This provides a direct pressure dependence at low pressures but at high pressures tungsten oxide molecule s form an adjacent gas boundary layer which lowers the PO2 at the tungsten surface. A correction for this effect using free-convection theory fits the rate data over the entire oxygen-pressure range from 10-8 to 1 atrn as well as data using O2-A mixtures. Below 10-6 atrn and above 2000°C, e decreases with increasing temperature because of desorption of oxygen atoms. Below 2000°C the rate decreases with decreasing temperature at all oxygen pressures following an apparent activation energy of 42 kcal per mole and depending on (Po2)n with n varying between 0.55 and 0.80. MOST of the previous tungsten oxidation studies have employed gravimetric methods and have been limited to temperatures below 1000°C where the weight loss associated with evaporation of tungsten oxides is negligible compared with the weight gain from oxidation.' At higher temperatures, oxygen-consumption rates have been determined from pressure measurements, usually at constant flow rates, by Langmuir,2 Eisinger,3 Becker, Becker, and Brandes,4 and Anderson.5 The sensitivity of this method decreases with increasing pressure and, with the exception of Langmuir's work, these investigations were confined to pressures below 10-6 atm. Above approximately 1300°C, depending on the oxygen pressure, the rate of oxide evaporation is greater than the oxide-formation rate and the recession of the tungsten surface can be measured optically without interference from an oxide layer. This was first done by Perkins and crooks6 who heated tungsten rods in air pressures from 1 to 40 torr at temperatures between 1300" and 3000°C. The present investigation of the oxidation kinetics of tungsten at high temperatures emphasizes oxygen pressures from 10-6 to 1 atm. This is the range of interest for earth atmosphere re-entry applications of tungsten for which little data were previously available. APPARATUS The apparatus is a modification of the type used by Perkins and crooks.' Ground tungsten seal rods, 6 in. long by 0.125 in. diam, were mounted vertically between two water-cooled electrodes, one fixed and the other having free vertical travel. The movable counter-weighted electrode is prevented from undergoing horizontal displacement by three sets of runners mounted at 120-deg intervals. Electrical contact is made by means of a water-cooled mercury pool. A 24-in. vacuum bell jar having a volume of approximately 267 liters was used as the reaction chamber with the sample holder mounted in the middle of the chamber. Power was supplied from an 800-amp dc variable power supply. Temperature readings were made by means of a Latronics automatic two-color recording pyrometer. With this instrument, corrections for emissivity are not necessary provided the spectral emissivi-ties at two closely spaced wavelengths are equal. Supporting measurements were made with a micro-optical pyrometer corrected for emissivity of bare tungsten and window absorptivity. The micro-optical pyrometer was calibrated against a National Bureau of Standards calibrated tungsten lamp and both pyrometers were periodically checked against the melting points of tungsten and molybdenum using the oxidation apparatus. Above 10-6 atm, pressures were measured with an Alphatron gage calibrated against a McCleod gage. At 10-6 atm, a hot-filament ionization gage was employed. A magnified image of the self-illuminated tungsten rod was formed using a 360-mm objective lens mounted outside the bell jar. When the experiment exceeded 1 hr, the image was focused on a ground-glass plate about 10 ft from the tungsten rod at about X8 and the recession of the thickness of this image was monitored with a Gaertner cathe-tometer. When faster rates were encountered, a 35-mm time-lapse cinecamera with a telephoto lens and bellows extension was substituted for the ground-glass plate and cathetometer. Diameter recession rates were determined from the photograph image projected on the screen of an analytical film reader. EXPERIMENTAL PROCEDURE After installing the rod in the apparatus and cleaning it with acetone, the system was evacuated to 5 1 x 10-5 torr. Before oxygen was introduced,

Jan 1, 1964