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By P. F. MINISTER

AT Lime Spur, Mont., the East Butte Copper Mining Co. has been quarrying limestone for twenty years. The quarry is beside the Northern Pacific R. R. in the Jefferson River canyon, 4 ½ miles east of Cardwell, at Lime Spur, Montana. HISTORY This quarry was opened early in 1900 by Dan Morrison of Whitehall, the discoverer of the Morrison cave, to supply a demand for smelter flux. Limestone was sold to the Pittsmont smelter of The East Butte Copper Mining Co. and to the Butte Reduction Works. As no particular effort was made at the quarry to select the rock that delivered to the smelters was unduly high in magnesia and impurities. The East Butte com¬pany, therefore. Bought the quarry. in 1909 and confined operations to the high-grade beds in order to supply rock of the desired purity for its own smelter and the Butte Reduction Works until the latter shut down. It also developed a market for some of its rock with the sugar factories. The latter market increased until in later years all rock, larger than 4 in. in size over a bar grizzly, was being shipped to the sugar factories, and the rock smaller than 4 in. was being used as a flux in the blast furnaces at the Pittsmont smelter. In 1924, the East Butte concluded a contract with the Anaconda company for the treatment of its ores, and the Pittsmont -smelter -was shut down: which made the minus 4-in. rock a useless by-product. Since there was not enough revenue in the sugar rock alone and also because of limited waste room it became necessary, if Lime Spur was to continue to operate, to increase- the proportion of plus 4-in. rock and to develop a market for the minus 4-in.

Jan 1, 1930

By James P. Sloss

WHAT is the likelihood if any-that a real gold mining industry will be developed in the southern Appalachian region? Has the increase in the dollar value of gold from $20.67 to $35 per ounce potency to turn the trick? Suppose it be assumed that the price of gold will, at worst, not recede, and that the cost of digging ore and treating it of which the average level of commodity prices and wages is a fair index-will, at most, not exceed that prevailing in 1926. One may or may not accept these as reasonable assumptions; but one must arbitrarily remove some of the potential variables if one is to get anywhere on a problem like this. As a matter of fact, this article is not going to venture a conclusive answer to the question that has been posed; but it will endeavor to present some of the factors that have a bearing on the problem. The writer spent ten days visiting a dozen properties in Virginia and the Carolinas early in April, 1935, and in doing so got a first-hand slant on mining conditions in the domain of King Cotton.

Jan 1, 1935

By AIME AIME

THE following paragraphs comprise such information as the Secretary has been able to obtain concerning the members and associates whose deaths have been reported. Further particulars or corrections of errors, and biographical data concerning deceased members or associates not already noticed in this way, are solicited. [SECRETARY'S NOTE.-All of these notices have been revised, and some of then have been more or less completely prepared, by me. To those which contain more particularly the expression of my personal feeling, my initials have been appended. The labor of preparing or editing these paragraphs has been in many respects both welcome and interesting, on the one hand, and sorrowful, on the other. In going through the list, I have repeatedly felt like one who, visiting the Morgue, suddenly comes upon the pale face of a dear friend, of whose death lie was not aware ; and, even when this fact was known to me, the work of recording it has brought upon me a flood of recollections, almost preventing the discharge of that official duty. The list for 1907 seems to me to he peculiarly sad, comprising, as it does, so many sudden deaths by violence or accident, so many veterans, removed too soon, and so many young men whose early departure impoverishes the future, even more than the present. Probably, this feeling on my part is largely due to the circumstance that the increased membership of the Institute necessarily in¬volves an increase of the annual death-list. Probably, also, it is connected with the circumstance that during the first years of the history of the Institute-say from 1871 to 1880-it was joined by men of all ages, and that the death-rate is consequently now above the average which would result from the normal annual addition, principally of young men. And finally, I must admit that, as one of the original members of the Institute, and practically connected with it for nearly thirty-seven years as Acting President, President or Secretary, I am peculiarly impressed and depressed by the successive deaths of those who were my associates in the years of its early struggles and triumphs. I do not wish to inflict upon my younger colleagues the melancholy reflections of an increasingly lonesome old man. In fact, my prevailing mood concerning the Institute is not at all melancholy, but triumphant and hopeful. If I may be permitted to preach at all, I would enforce, from the texts given below, a moral which many of them declare so forcibly as to preclude the necessity of expository enforcements-namely, the duty of every one of us, old or young, to give to his brethren, as he goes along, and without waiting for some future occasion for a comprehensive and monumental contribution to technical literature, the results of his observation and experience. When I look at this list of names, my personal sorrow over many of them is drowned in my professional reflection as to each and all-How much has died with

Jan 1, 1908

By ROBERT H. BOOTH

THE happy intra-plant relationships of the Bridgeport Brass Co. are largely attributable to the interest of the management in this important business factor. In furtherance of this development Carl F. Dietz, President of the Company and a member of the Institute, has contributed the novel plan for the objective presentation of business economics, described herein. All of the officers of the corporation are active in its management and they together with many other workers filling both executive and subordinate positions have a substantial financial interest in the enterprise. The viewpoint of this organization is fairly reflected by the following quotation from Roosevelt's "The Foes of Our Own Household."

Jan 1, 1924

By Thomas T. Read

THE benefits derived from stabilization of industry that might possibly be attained through some scheme of centralized economic planning have been much discussed of recent months, and opinions on the subject range from those who believe that some agency like the War Industries Board would be practicable to create and wholly beneficial in effects, to those who are equally convinced that none of the suggestions so far advanced are at all practicable, or likely to be productive of more of good than of evil. The discussion has been on the general topic, but-many of those who have written or spoken on it have introduced economic problems of the pinera1 industry; for example, Newton D. Baker, who referred to the coal industry in his address on economic planning at the Williamstown Institute of Politics on July 31, and then went on to say, "Industrial progress is made by the development of new things, but new things upset the equilibrium of any plan. Who could have planned the industrial effects of the development of the railroads, or the economic changes which you have seen attend the development of the internal combustion engine. Obviously, unless we are prepared to put world economics in a strait-jacket and, like the encyclopedists, write its full history on the theory that further progress is impossible, no such plan could be made for nations which are forging ahead as is entirely rational for nations which are still catching up."

Jan 1, 1931

By R. H. Smith, A. C. Polk

The physical properties of the materials are listed, together with a short explanation of how this material binds the sand grains together without materially reducing the effective permeability of the sand. The chemical can be used in wells with bottom-hole temperatures ranging from 105°F to more than 350°F A description of the equipment required and the techniques used for applying these plastics to the wells is included. Introduction Recovering oil and gas from unconsoli-dated sand formations offers one of the most troublesome of all production problems. These sands generally present no particular trouble while drilling is in progress, but after the well has been completed and a pressure differential has been established across the face of the producing zone, the formation begins to L'slough," resulting in "sanding up" of the well. The term "sanding up" means that sufficient volumes of sand have moved into the well bore or casing to cause a serious reduction or complete halt of all flow of oil, water or gas. In rare cases a well may produce only a small amount of sand and still continue to flow or pump, the sand being carried to the surface in the fluid stream. However, in such instances, the result may be a costly repair bill due to the effect of the sand on surface and pumping equipment. The difficulty of producing petroleum from sands that are loosely cemented has long been recognized by petroleum engineers but only within the last few years has any new approach to the problem been undertaken. This involves the use of plastics that are capable of bonding the individual sand grains in place without materially reducing the effective permeability of a formation. The successful application of plastics for the consolidation of poorly cemented sands is relatively recent but now it is widely used in many of the more difficult areas on the Gulf Coast of Texas and Louisiana. This relatively new use of plastics1 in the oil fields has been preceded by much laboratory and field research on the use of various chemicals2,3 for solving numerous well-completion and work-over problems. Plastics now are being used successfully to control gas-oil and water-oil ratios,4'6 in zone isolation, the repair of casing leaks, the elimination of caving in cable-tool drilling wells6'7 and in the setting of linerss and casing.9 Sand-consolidating plastics, however, are basically different from all others in that they must not form an impervious seal. Field Practices The approach to the sanding-up problem usually has been the mechanical obstruction of the movement of the sand grains.

Jan 1, 1947

By A. C. Polk, R. H. Smith

The physical properties of the materials are listed, together with a short explanation of how this material binds the sand grains together without materially reducing the effective permeability of the sand. The chemical can be used in wells with bottom-hole temperatures ranging from 105°F to more than 350°F A description of the equipment required and the techniques used for applying these plastics to the wells is included. Introduction Recovering oil and gas from unconsoli-dated sand formations offers one of the most troublesome of all production problems. These sands generally present no particular trouble while drilling is in progress, but after the well has been completed and a pressure differential has been established across the face of the producing zone, the formation begins to L'slough," resulting in "sanding up" of the well. The term "sanding up" means that sufficient volumes of sand have moved into the well bore or casing to cause a serious reduction or complete halt of all flow of oil, water or gas. In rare cases a well may produce only a small amount of sand and still continue to flow or pump, the sand being carried to the surface in the fluid stream. However, in such instances, the result may be a costly repair bill due to the effect of the sand on surface and pumping equipment. The difficulty of producing petroleum from sands that are loosely cemented has long been recognized by petroleum engineers but only within the last few years has any new approach to the problem been undertaken. This involves the use of plastics that are capable of bonding the individual sand grains in place without materially reducing the effective permeability of a formation. The successful application of plastics for the consolidation of poorly cemented sands is relatively recent but now it is widely used in many of the more difficult areas on the Gulf Coast of Texas and Louisiana. This relatively new use of plastics1 in the oil fields has been preceded by much laboratory and field research on the use of various chemicals2,3 for solving numerous well-completion and work-over problems. Plastics now are being used successfully to control gas-oil and water-oil ratios,4'6 in zone isolation, the repair of casing leaks, the elimination of caving in cable-tool drilling wells6'7 and in the setting of linerss and casing.9 Sand-consolidating plastics, however, are basically different from all others in that they must not form an impervious seal. Field Practices The approach to the sanding-up problem usually has been the mechanical obstruction of the movement of the sand grains.

Jan 1, 1947

FRank FirmstoNe, Easton, Pa.: The effect of lead on brass seems to have been recognized by Berthier, and the facts published by him as early as 1818 (Ann. des Mines, 1st ser., iii., 1818, p. 347 et seq.). He there says expressly that copper containing lead makes " dry " (see) brass, and that, for the same reason, blast-furnace

Jan 1, 1898

By G. W. LAAiIBOURNE

FEW mines possess a history of more fascinating interest than the Ontario at Park City, Utah. The famous Bonanza's production record of over $50,000,000; the great extent of its workings; the remarkable character of its mineralization; the fact that recent discoveries have shattered preconceived theories of the geology of the camp practically assuring the half-century old property a future as active and as prosperous as the past make the Ontario one of the unique mines of the world. A mere accounting of the wealth created by this historic property not only exemplifies the great profits

Jan 1, 1925

By Simon D. Strauss

Production and consumption of nonferrous metals in the United States during 1950 were at peak levels for the postwar period, as is shown in Tables I, II, and III. The trend of production was upward through most of the year. At the year end, with the possible exception of the Tri-State zinc-lead district, the large mining operations in the country were running at capacity. The absence of serious labor interruptions during the year was an important contributing factor in the increased out-put of metals, since in each of the previous postwar years there had been a number of major strikes which affected production adversely.

Jan 2, 1951

By Joseph P. Kittredge

At the time this matter first came up in 1912, the National Malleable and Steel Castings Co. had seven basic-bottom open-hearth furnaces in its plant at Sharon, Fa., using fuel oil, then costing about 2½¢ per gallon. The fuel was satisfactory but its cost fluctuated widely, therefore the use of pulverized coal, which had been successful in the cement industry and in some metallurgical furnaces, was suggested. After a thorough investigation, and an actual trial on one of the open-hearth furnaces, to be certain that the siliceous ash in the coal would not seriously affect the basic slags, the management of this company approved its adoption and a complete installation was started. The conclusion had been reached that the success of the operation depended on pulverizing the coal to greater fineness than had thus far been accomplished, and all equipment was chosen with this in mind. A coal drier was deemed essential, and one of ample capacity and efficiency was selected, which has done all that was expected of it, working without failure and with very small maintenance cost, and is still in operation. Pulverizers The company demanded a pulverization of at least 90 per cent through a 240-mesh screen, with consistent results, and a machine was chosen that was grinding other materials than coal to the fineness desired. The control of fineness was obtained through a vacuum separator, and was governed by the size of the separator and the number and construction of the valves necessary to expand and direct the air current. These valves can be set to obtain any degree of fineness desired, and the result is consistent. Two machines were installed, each capable of producing 2½ tons per hour, 95 per cent through 240 mesh. These machines have done everything expected of them, have run continuously, and are still in operation. An examination of some of our pulverized coal by elutriation and microscopic measurement disclosed that a 1-lb. lump of bituminous coal,

Jan 1, 1940

By Joseph P. Kittredge

At the time this matter first came up in 1912, the National Malleable and Steel Castings Co. had seven basic-bottom open-hearth furnaces in its plant at Sharon, Fa., using fuel oil, then costing about 2½¢ per gallon. The fuel was satisfactory but its cost fluctuated widely, therefore the use of pulverized coal, which had been successful in the cement industry and in some metallurgical furnaces, was suggested. After a thorough investigation, and an actual trial on one of the open-hearth furnaces, to be certain that the siliceous ash in the coal would not seriously affect the basic slags, the management of this company approved its adoption and a complete installation was started. The conclusion had been reached that the success of the operation depended on pulverizing the coal to greater fineness than had thus far been accomplished, and all equipment was chosen with this in mind. A coal drier was deemed essential, and one of ample capacity and efficiency was selected, which has done all that was expected of it, working without failure and with very small maintenance cost, and is still in operation. Pulverizers The company demanded a pulverization of at least 90 per cent through a 240-mesh screen, with consistent results, and a machine was chosen that was grinding other materials than coal to the fineness desired. The control of fineness was obtained through a vacuum separator, and was governed by the size of the separator and the number and construction of the valves necessary to expand and direct the air current. These valves can be set to obtain any degree of fineness desired, and the result is consistent. Two machines were installed, each capable of producing 2½ tons per hour, 95 per cent through 240 mesh. These machines have done everything expected of them, have run continuously, and are still in operation. An examination of some of our pulverized coal by elutriation and microscopic measurement disclosed that a 1-lb. lump of bituminous coal,

Jan 1, 1940

By J. R. Linney

Demand for eastern magnetite in 1948 necessitated practically all eastern magnetite industries to operate on a six-day week, with the result that over 11,000,000 long tons of crude ore were mined, and the shipping products amounted to approximately 5,000,. 000 long tons. Reports indicate that operating on a six-day week and doing maintenance work on the seventh day was satisfactory and resulted in excellent continuity of operation. In the Port Henry district, Republic Steel Corp. once again set new all-time records for the production of crude ore and total shipping product; 1,868,000 long tons of crude ore were mined, 945,000 from the Old Bed mine, 408,500 from the Harmony mine, and 514,500 from the Fisher Hill mine. Of the 969,000 long tons of shipping products, 663,800 long tons were sinter, 181,000 lump ore, and 115,200 con¬centrates.

Jan 1, 1949

By L. E. Snow, L. F. Pett

AT the Utah Copper Pit of Kennecott Copper Corp. a versatile mobile drill unit has been developed and tested. Through increased drilling speed and additional available drilling time, an improvement of 233 pct in drill performance has been realized. Operators using drill power can quickly and easily convert the unit from a vertical to a toe hole drill. Drilling is done with the machine in line with the unit or at right angles to it. Table I covers the 1950 drill record at the mine, showing the types of machines used and the footage obtained. Development of the new units was prompted by a desire for solution of the following problems: 1—The ever-expanding operations within the Utah Pit, requiring some 65 miles of transmission pipe lines radiating from a central compressed air plant, have now taxed this compressor plant beyond capacity. While 100 lb per sq in. pressure is maintained at compressors, transmission losses from innumerable small leaks result in low terminal pressure at the drills. Fig. 1 illustrates that while terminal pressure varies according to size of air hose and fittings used, the average drill is operating on air pressures within the 60 to 70-lb range. The compressor plant is operated primarily for air rock drills. All drilling is done on day shift, but it is necessary to run two of the three 3720 cu ft capacity compressors during night shift in order to prevent drastic loss of pressure through leaks. On day shift all three compressor units are operated at capacity, so that there is no reserve safeguard available for extensive repairs to any compressor. The calculated volume of compressed air required for operation of 25 drills is but 33 pct of three day-shift compressors. While compressed air is being used to a minor extent for purposes other than drilling, it is felt that satisfactory substitute facilities could be pro- vided in the event that air lines were no longer available. 2—Drill performance has increased beyond the capacity of present 3-in. drifter machines. 3—The installation, maintenance, and moving of air lines in routine mining is a growing problem. The 2-in. level lines are placed outside electrification towers and must be moved to new location upon completion of each shovel cut. In addition to these moves it is often necessary to dismantle level lines so that excessive shovel spillage, or material covering track following a blast, can be pushed in the clear with bulldozers. Where level room is limited, it is often necessary to remove air lines in giving bulldozers room to prepare grades for wagon drills. In spite of precautions taken, many level lines become buried, twisted, and constricted, with excessive air loss resulting. Excessive back break in blasting often leaves several sections of air line suspended in mid-air. Occasionally air lines come in contact with defective electric transmission towers, so that holes are burned through pipe. 4—Rail-handling of drilling equipment such as wagon drills from one location to another requires considerable locomotive crane crew time. Any new unit developed should travel under its own power. 5—Present practice requires accessory material including hose, water pressure tanks, water barrels, drill steel, and bits to be transported by means of push cars when drill locations are changed on any level. 6—In order to supply numerous drill locations with material, many stock piles of new drill rods, drill bits, and other essentials must be left at strategic points, usually in the vicinity of powder magazines. This practice makes for poor housekeeping and contributes to the loss of supplies. Planning the Unit It was felt that a mobile drill unit which would rectify the foregoing problems should meet certain demands: 1—It must furnish compressed air to operate a 4-in. rock drill at a pressure of 90 to 100 lb.

Jan 1, 1953

By L. E. Snow, L. F. Pett

AT the Utah Copper Pit of Kennecott Copper Corp. a versatile mobile drill unit has been developed and tested. Through increased drilling speed and additional available drilling time, an improvement of 233 pct in drill performance has been realized. Operators using drill power can quickly and easily convert the unit from a vertical to a toe hole drill. Drilling is done with the machine in line with the unit or at right angles to it. Table I covers the 1950 drill record at the mine, showing the types of machines used and the footage obtained. Development of the new units was prompted by a desire for solution of the following problems: 1—The ever-expanding operations within the Utah Pit, requiring some 65 miles of transmission pipe lines radiating from a central compressed air plant, have now taxed this compressor plant beyond capacity. While 100 lb per sq in. pressure is maintained at compressors, transmission losses from innumerable small leaks result in low terminal pressure at the drills. Fig. 1 illustrates that while terminal pressure varies according to size of air hose and fittings used, the average drill is operating on air pressures within the 60 to 70-lb range. The compressor plant is operated primarily for air rock drills. All drilling is done on day shift, but it is necessary to run two of the three 3720 cu ft capacity compressors during night shift in order to prevent drastic loss of pressure through leaks. On day shift all three compressor units are operated at capacity, so that there is no reserve safeguard available for extensive repairs to any compressor. The calculated volume of compressed air required for operation of 25 drills is but 33 pct of three day-shift compressors. While compressed air is being used to a minor extent for purposes other than drilling, it is felt that satisfactory substitute facilities could be pro- vided in the event that air lines were no longer available. 2—Drill performance has increased beyond the capacity of present 3-in. drifter machines. 3—The installation, maintenance, and moving of air lines in routine mining is a growing problem. The 2-in. level lines are placed outside electrification towers and must be moved to new location upon completion of each shovel cut. In addition to these moves it is often necessary to dismantle level lines so that excessive shovel spillage, or material covering track following a blast, can be pushed in the clear with bulldozers. Where level room is limited, it is often necessary to remove air lines in giving bulldozers room to prepare grades for wagon drills. In spite of precautions taken, many level lines become buried, twisted, and constricted, with excessive air loss resulting. Excessive back break in blasting often leaves several sections of air line suspended in mid-air. Occasionally air lines come in contact with defective electric transmission towers, so that holes are burned through pipe. 4—Rail-handling of drilling equipment such as wagon drills from one location to another requires considerable locomotive crane crew time. Any new unit developed should travel under its own power. 5—Present practice requires accessory material including hose, water pressure tanks, water barrels, drill steel, and bits to be transported by means of push cars when drill locations are changed on any level. 6—In order to supply numerous drill locations with material, many stock piles of new drill rods, drill bits, and other essentials must be left at strategic points, usually in the vicinity of powder magazines. This practice makes for poor housekeeping and contributes to the loss of supplies. Planning the Unit It was felt that a mobile drill unit which would rectify the foregoing problems should meet certain demands: 1—It must furnish compressed air to operate a 4-in. rock drill at a pressure of 90 to 100 lb.

Jan 1, 1953

By F. C. Smyers, E. W. Merrick

ALTHOUGH the zinc and pyrite concentrates produced at Midvale go to other companies, the United States Smelting Refining and Mining Company smelts and refines its own lead. Refining is the first step of the process that is done at some distance from the mining operations, the plant being at East Chicago, Ind., an industrial center about 25 miles southeast of Chicago. For years it has been notable as being the only lead refinery in the country using the Betts electrolytic process. The original buildings, many of which are still in use, were erected in 1906 when the plant was known as the United States Metals Refining Co. In 1920 the parent company sold its copper refinery at Chrome, N. J., and since the copper refinery was also known as the U. S.

Jan 1, 1948

By John McCoy, Edward Thimons, Kenneth Heller

As the working levels in domestic mines are developed to greater depths and work areas move further from the shafts, maintaining a safe and healthful working environment becomes more difficult. Increased temperature and humidity at greater depths becomes first a factor in productivity and then a threat to the miner's safety. Initially, a miner might develop listlessness leading to reduced productivity and reduced alertness. Continued overexertion can lead to heat stroke and possibly death. Mine ventilation engineers, therefore, must not only provide clean air to work areas, but also must provide cooled air. The following article describes the United States Bureau of Mines (USBM) and Foster-Miller's successful development of a high performance, low maintenance direct water to air contact heat exchanger for mine cooling. While heat problems frequently do not develop until mining operations descend below sea level, problems will arise any time mining penetrates high temperature rock. Hot fissure water will increase the severity of the situation, causing increases in wet bulb temperature - the temperature to which perspiring miners reject metabolic body heat. All energy expended in mining adds to the heat load which must be absorbed by the ventilation air. Just when the cooling capacity of ventilation air is needed most, adiabatic compression (autocompression) of air descending the shaft raises air temperatures 1.3g°C (2.5'F) to 2.94"C (5.3OF)/305m (1000 ft) depending on humidity. Increased temperatures decrease the ability of the air to absorb heat from the mine, and work area temperatures rise. Once forced ventilation air can no longer maintain safe work area temperatures, refrigeration methods must be employed. Many mines now use cooling coils for this purpose. A cooling coil uses refrigerated mine water to cool the air by passing the air through banks of copper tubing filled with cold water. Heat from the air is transferred to the water through the pipe with the aid of fins. Conventional water to air heat exchangers prove troublesome for many mines be- cause of the high levels of dust that are encountered, causing these exchangers to operate at relatively low efficiencies. A more satisfactory approach to work- place cooling is desired - one that offers reduced maintenance and increased cooling efficiency.

Jan 1, 1982

By DIFTIGIHT E. WOODBRIDGE

(Glen Summit Meeting, June, 1911,) DURING April, May, and June, 1910, I was in charge of an examination of the greater part of the Moa iron-ore area in Oriente Province, Cuba, on the north coast, near the east end of the island. My instructions, on arrival at the properties, were to check former estimates of tonnages and grades, and to re-examine the ore comprised in claims covering 44,727 acres. This work included .the running of lines dividing the properties into co-ordinate planes, the boring of many thousand feet of holes spaced at the intersections of these co-ordinates, the taking of samples of the ore penetrated, the analysis of these samples for their various constituent minerals, and the determination of the results as to tonnages, depths, and grades, both for individual properties and for the entire group. Each section of every one of the thousand holes drilled was to be compensated for depth and grade with every other, a series of simple arithmetical calculations of no slight magnitude, the mere mechanical labor of which consumed much time, but finally resulted in giving a complete average of all the essential facts for the entire area of 18,000 hectares. Had it not been for the more than willing, active, and able co-operation of the officers of the Spanish-American Iron Co., from Charles F. Rand, President, and Jennings S. Cox, General Manager, down to the most humble water-carrier, the work would have consumed far more time than it did. Papers prepared by others, and to which my present paper may be considered an addendum, elucidate, more fully than I could hope to do, the origin and geological character of these ores. I will confine myself to the situation, method and expense of exploration, and to probable courses of development and mining, with some attention to the cost of the ore delivered in the United States.

Mar 1, 1911

By A. U. Seybolt

DURING the course of experiments involving oxygen equilibrations with a high-purity Pd-5 at. pct Rh alloy, the appearance of a subscale was noted. Most of the heat treatments in a pure oxygen atmosphere were performed at 900°C. The presence of the subscale was noted when the oxygen partial pressure was in excess of approximately 95 mm, up to 1 atm, the highest pressure used. According to available thermodynamic information' on the free energy of formation of Rh2O3 (the only reliably reported solid oxide of rhodium), this oxide should not be stable under these conditions, nor, of course, any oxide of palladium. Extraction of the subscale from the matrix was affected by treatment with aqua regia, and the resulting X-ray diffraction powder pattern is shown in Table I. This pattern is not that of Rh2O3, nor that of any known rhodium or palladium oxide. It can be indexed on a hexagonal lattice with a. = 5.22Å and co = 6.0Å. In addition to this unknown material, there was a weak Rh2O3 pattern. An X-ray fluorescence analysis of the powder gave 3214 palladium counts per sec and 5381 rhodium counts per sec, thus indicating the likelihood of a double oxide of palladium and rhodium. In view of the fact that the above result was obtained on a single sample, it is perhaps best not to insist upon the above ratio of about 0.6, but possibly to tentatively assume 0.5 or 1/1. The small amount of Rh2O3 in the X-ray pattern might have occurred on cooling, and it seems possible that the double oxide, below some temperature level, is not as stable as Rh2O3. To examine this point, some of the extracted double oxide was heated on a sheet of pure palladium in air at 900°C, and allowed to furnace-cool over a period of several hours. The X-ray diffraction pattern of the powder showed approximately the same intensity of Rh2O3 and the "hexagonal" oxide as before, but, in addition, a rather faint pattern of another crystalline species made its appearance. This finding again suggests partial transformation of the major (double) oxide to other oxides on cooling from 900°C. Application of the phase rule shows that only one equilibrium oxide (subscale) could have been present at temperature. Vacuum-fusion, oxygen analysis of the extracted subscale showed 7.7 ± 0.7 pct O. Combining this information with that of the X-ray fluorescence analysis suggests the formula PdRhO. This compound should have an oxygen content of 7.07 pct, which is within the range of error of the oxygen analysis. However, until a more careful stoichiometric study is made, it is suggested that the formula be written

Jan 1, 1965

By George F. Kunz

Jan 1, 1902