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By Vince Poxleitner, John Delaney

Introduction In the mining industry, comminution typically begins in the mine with a blast of explosive to break rock so that it can be handled by the avail- able equipment. Though the breaking of the rock is essential for material handling in the mine and plant, this is not the only reason for ore reduction in the mineral industry. Comminution is primarily required to liberate minerals from ore so that they can be concentrated into valuable products or to prepare minerals, such as talc, for market as mined. The size of the equipment used for comminution ranges from small to massive. Regardless of equipment size, the power required to reduce the rock is a major expense. Years ago, mineral deposits could be mined more selectively and required less grinding to produce saleable products. However, as richer deposits were depleted, it has become necessary to mine low-grade deposits, with the valuables dispersed throughout the rock. Comminution equipment evolved in physical size and capacities to meet the new mine and process requirements. A modern, modestly sized mining operation, with a capacity of 25.000 TPD may use crushers two stories high weighing over a million pounds, SAG mills 36 feet in diameter driven by dual motors putting out 10.000 horse- power, and ball mills over 16 feet in diameter . Because of the increasing size and weight of modern equipment, the builder is faced with the problems of erecting massive foundations and field assembling equipment on these foundations. As equipment costs and plant construction costs increase, builders are finding that owners are asking for more detailed progress and cost data. Comminution construction projects are generally classified as grass roots plants or expansions or modifications to existing plants. It is estimated that 60-702 of the jobs involve existing plants. Today ' s costs for construction of small, new comminution plants can reach tens of millions of dollars; larger plants can cost hundreds of millions of dollars. Modifications, on the other hand, usually run from a few thousand to several million dollars. Though many problems are common to the construction of both new plants

Jan 1, 1982

By Arthur Mitchell

POSSIBLY in no other of the non-ferrous mining districts of this country has the use and develop-ment of mechanical loaders been carried to such an extent as in the "lead belt" of Southeast Missouri. It has become apparent to the four mining companies in the district that it is imperative to apply satisfactory mechanical methods to the chief remaining stage of the entire operations-mining, milling, smelting and refining-in which manual labor is still largely used to handle material in process. With increasing wages and with the reduction of the metal divisor by the extension of mining into lower-grade orebodies, the shoveling cost per ton of lead produced has become relatively so large that in an effort to reduce it there is ample justification for considerable capital expenditure. Hand shovelers load about 18 tons of ore per shift and the average grade is less than five per cent. lead. Further, the ore is relatively heavy, about 21 cu. ft. to the ton when broken, and is often so coarse and so closely compacted after shooting that it requires much more block-holing, sledging, and muscular effort to shovel than, for example, does the cherty and more granular ore of the Joplin district or the finer ore in the headings of a drift mine. No mining company desires to pay for mere back muscles if it be economically feasible to avoid it, and labor saving machinery should be susceptible of operation by older employees, who are no longer capable of the more strenuous manual occupations.

Jan 4, 1923

By John V. Beall

Cutting costs and increasing safety with new ideas is the byword with The Cleveland-Cliffs Iron Co. on the Marquette Range in Michigan. Among the new ideas being tried out are mechanical shaft mucking, prefabricated lagging to replace timber poles, Carset bits in shaft sinking, and rubber tired guide wheels on the ore skips. Plans are being made to stockpile ore with conveyor belts during the winter. In sinking the Mather "B" Shaft a 3/8-yd clamshell-type bucket is used for mucking. The clamshell is opened and closed by means of a verticallymounted hydraulic ram actuated by 5000 psi oil pressure. An Ingersoll Rand-type hoist is used to raise and lower the clamshell. The hoist is controlled by one member of the crew on the floor of the shaft. When the bucket is raised, the men swing it over the muck pile to the desired position and then it is lowered on to the broken rock. The 1400-lb weight of the bucket causes it to sink into the broken rock and it digs as the ram closes the bucket. The hydraulic ram is operated by a man on the lowest shaft steel set who controls a specially designed oil pump which supplies oil pressure. The clamshell is emptied.

Jan 1, 1949

By W. G. Jewitt

YELLOWKNIFE, the most northerly Canadian gold mining district, is once more in the throes of a boom. Touched off by spectacular and well-publicized diamond-drilling results on the property of Giant Yellowknife Gold Mines, Ltd., mining companies and the general public are competing for mining claims and for the shares of companies owning mining claims in the area, with little regard for values. Such a stock-market boom has various unfortunate consequences but undoubtedly one beneficial result is that considerable amounts of money are made available for serious development. The Yellowknife mining area lies on the north shore of Great Slave Lake, in the Northwest Territories, at a latitude of approximately 62°30' north. The topography is a low-relief phase of that usual in the Canadian Laurentian shield. Roughly, one third of the surface is lake-covered, one third muskeg or overburden, and one third is bare

Jan 1, 1944

By G. E. Johnson

LEAD SMELTERS AND REFINERS in 1932 were confronted with the problem of adjusting operations and costs to curtailed production and consumption at reduced prices, a problem which has been partially solved at least by improvements in operating technique and increased efficiency. At the Mount Isa properties in Australia, a third blast furnace and additional Dwight-Lloyd sintering machines were installed during the year, designed to increase the production to 6,000 tons of bullion per month. The large proportion of lead carbonate in the ores to be treated has presented metallurgical problems. Of the total lead contained in the concentrates to be smelted, two-thirds is Dresent as carbonates and one-third as sulfides. In the iiitial operations, the resulting Dwight-Lloyd sinter was soft, contained an excessive amount of fines, and was easily fusible. When charged to the blast furnaces it developed accretions in the upper part of the furnace owing to the easily fusible lead carbonates softening and fusing at the top of the charge column. This was remedied by the addition to the sinter feed of diluents of higher melting point, granulated slag and crushed limestone. The sinter feed consists of concentrates, Cottrell dust and wind-box cleanings, totalling 57 per cent of the charge; return sinter fines 15 per cent; granulated slag 23 per cent; and crushed limestone 5 per cent. The sinter produced contains 34 per cent lead and 0.5 per cent sulfur. Experiments indicated that double sintering under these conditions was of no advantage, so the original plan of single sinter treatment was retained.

Jan 1, 1933

By K. D. Jacob

IN the decreasing order of the tonnages involved, the uses of phosphates can be grouped conveniently into three general classes, namely, fertilizer; chemicals for military, industrial, and technical purposes; and mineral feed for livestock. The quantity of phosphate used as fertilizer, principally in the form of superphosphate, has always exceeded by far that used for all other purposes, though in recent years a marked increase has occurred in its consumption for the other two general classes of uses. Prior to the present century large quantities of superphosphate, as well as a considerable portion of the production of phosphorus chemicals, score made from bone materials which were plentiful and cheap in some areas and which could be more easily processed than phosphate rock for the manufacture of chemicals. Today, however phosphate rock has almost completely displaced bone as a raw material for the manufacture of chemically processed phosphates in nearly all countries of the world.

Jan 1, 1944

Jerome L. Boyer, Reading, Chairman; William L. Sheafer, Pottsville, Secretary ; Levi Quier, Reading, Treasurer; Robert Allison, Port Carbon; James Archbald, Jr., Pottsville; William Atkins, Pottsville; D. P. Brown, Lost Creek; William McH. Boyer, Rending; Albert Broden, Reading; George Brooke, Birdsboro; Frank Carter, Pottsville; H. P. Cooper, Pottsville ; J. H. Carpenter, Reading; E. S. Cook, Pottstown; B. Halberstadt, Pottsville; Hakon Hammer, Pottstown; J. Hartshorne, Stowe; M. P. Janney, Pottstown; R. C. Luther, Pottsville; N. Muhlenberg, Reading ; W. H. Morris. Pottstown ; George L. Norris, Reading; G. H. Potts, Pottstown ; H. Potts, Pottstown; S. M. Riley, Ashland ; J. S. Robeson, Pottstown ; Jas. P. Roe, Pottstown; A. W. Sheafer, Pottsville; Heber S. Thompson, Pottsville; Bard Wells, Pottsville; E. C.Wagner, Girardville; N. B. Wittman, Birdsboro. Reception Committee.— George Brooke, Chairman; Robert Allison, J. H. Carpenter, Edgar S. Cook, R. C. Luther, W. H. Morris, H. S. Thompson. Hotel Headquarters.—The Neversink Mountain Hotel, near Reading, Pa. All sessions were held in the hotel. The opening session was held on Tuesday evening, October 11. Mr. Jerome L. Boyer, Chairman of the Local Committee, called the meeting to order, and introduced Mr. John F. Daniel], Jr., VicePresident of the Reading Board of Trade, who delivered an address of welcome, in the course of which the industrial and commercial importance of the city was effectively outlined by skilful use of the statistics of leading branches. From this statement the following particulars are condensed for preservation: The Board of Trade has about 300 members. The annual value of the manofttctures (taking mainly the figures of 1891) is as follows: Iron manufactures, about $16,000,000 (including boilers and flues, $323,000; hardware, locks and butts, $1,650,000; pig-iron, wrought-iron pipe and machinery, $8,400,000; beams, bridge-work and steel, $4,000,000; bolts, nuts, rivets, etc., $1,000,000; stoves, $659,000); silk and cotton goods, $1,725,000; boots and shoes (one concern only), $150,000; ropes and cordage, $600,000; fire-brick, terra-cotta and glass, $320,000; wool and fur hats, $3,000,000; cigars (105 millions), upwards of $3,150,000. The street and elec-

Jan 1, 1893

By Ta M. Li

How do you convert a copper-zinc resource into a viable economic mining operation? This problem, unlike most, was complicated by the additional presence of a sub-arctic climate, highest labor costs in the world, low-grade copper-zinc values, depressed market prices, and a complex mineralization.

Jan 12, 1977

By AIME AIME

MEXICO embraces one of the great metal and petroleum producing provinces of the world. In this respect its history dates back to the overthrow of the Aztec empire by a Spanish force under Hernando Cortes between 1519 and 1.521. Even before then, its richness in silver and other minerals was not unknown. But it was a treasure house for the Spanish conquerors until the country became independent in 1821. It has been computed that in the 400 years following 1521, Mexico yielded 1.55,000 metric tons of silver, worth $3,000,000,000, two-thirds of the entire world production. In 1935 the country accounted for 36 per cent of the world's silver output, 14 per cent of its antimony (in 1934), 13 per cent of its lead, 3 per cent of its zinc and copper, and 21/2 per cent of its petroleum. Contrary to the impression of some, its gold output is now comparatively small, though important in the past. Its oil, as well, formerly hulked much larger than now, in 1921 being one-fourth of the world output.

Jan 1, 1936

By F. R. Milliken

EXPERIMENTS, in what has come to be known as flash roasting began some ten years ago. The principle underlying the operation was not a new one, but the experimental work started at that time was the first that was carried through to a logical conclusion, followed by construction and operation of a pilot plant, and then full-scale production. For a short working definition, flash roasting may he considered the instantaneous and complete oxidation of finely ground sulphide particles, partially suspended in air or gas, the oxidation reaction evolving enough heat to make the reaction self-sustaining, or nearly so.

Jan 1, 1937

By Charles R. Holmes

MORE than 70 igneous pipes and dikes are known to occur in Cambrian sediments throughout an approximately circular area of about 75 sq miles in southwestern Ste. Genevieve County and southeastern St. Francois County, Mo., across the southern portion of the Farmington anticline, which is outlined in fig. 1. From evidence obtained from fossil fragments taken from some of the intrusive, and from the similarity in composition of the more basic intrusives to those of known age in surrounding states, these pipes and dikes are believed to be at least post-Devonian and probably Cretaceous in age. As first postulated by Rust, these intrusives are believed to represent explosion tubes, or diatremes, punched through great thicknesses of solid rock by gaseous pressure. The particular intrusive studied is located about 1 mile north of the small town of Avon at an elevation of 880 ft in the EM SES NE% of sec. 2, T. 35N, R. 7E. Outcrop is through the Bonneterre dolomite in two separated exposures. The larger outcrop extends east and west for about 50 ft along a tributary in a small ravine (fig. 2). The smaller exposure occurs as a few scattered patches over an area 20 ft square about 100 ft to the north. The area between the exposures is covered, but scattered patches of the Bonneterre dolomite outcrop throughout the area surrounding the diatreme. Where exposed, contact relations show the surrounding dolomite to be shattered and metamor- phosed to a fine-grained rock for a distance of 15 to 20 ft from the intrusive. The igneous rock occurs as a dark greenish-gray porphyry near the center of the diatreme and as a fine-grained, greenish-gray material containing lapilli and metamorphosed fragments of dolomite near the contact with the country rock. The most abundant original mineral of the porphyritic rock is olivine now largely serpentinized as the result of extensive hydrothermal alteration at time of emplacement. The most common constituent of the fine-grained rock, which occurs near the border of the intrusive, is calcite. Mica is a common constituent of both types of rock, occurring as tufts or

Jan 1, 1950

By John H. Hollomon

A REVIEW of the steps which have been made to increase knowledge in the field of ferrous physical metallurgy during the closing period of World War II brings both pleasure and disappointment. Contributions of great value have been made, to be sure. However, due partly to the stress of the times, researchers in this field have been in the main directing their attention toward the short-range problems involved in the development and production of materiel for war. Furthermore, publication of the results of a great number of studies has had to be delayed. Much of the German work may, indeed, be lost entirely, owing to the efficiency of our bombers, which managed to account for most of the famous Kaiser Wilhelm Institut of Dusseldorf, not to mention the other large laboratories and manufacturing plants throughout that country. It would seem safe to assume, however, that fundamental research in Germany had been forced to give way to the shallow, but more pressing, engineering problems of a country trying to avoid defeat. In Russia the picture has been clouded by the limitations imposed upon comunication; but this much does seem clear: Russia alone among the great nations of the world has maintained her long-range view and has continued to foster research of the most fundamental type. English workers; on the other hand, appear to have been able only to meet the demands of the pressing problems of war, and their studies have been of the short-range variety. That metallurgical research of any sort should have continued in France during this chaotic period in her history would seem impossible, but, amazingly, a small handful of scientists did manage to carry on their work, and it is to be hoped that more will be heard from them in the future.

Jan 1, 1946

By Edward Keller

(New York meeting, February, 1912.) IN a paper, entitled A Uniform Method for the Assay of Copper Material for Gold and Silver,1 A. R. Ledoux invited the assayers of this country to contribute to a symposium, in which the results of their assays of given samples of copper-matte and metallic copper would be made comparable. This symposium 2 appeared about one year thereafter; and through it and its discussion, first became generally known the fact that the ,gold-yield by the all-fire method of assaying is usually higher than by the so-called combination (wet and dry) method, in which nitric acid is employed as a solvent for the copper. In the publication alluded to, the supposed cause of gold-losses in the latter method was declared to be the solvent action of copper nitrate, or of the reduction-products of the nitric acid, upon the gold. Up to a very recent date, gold has been held to be insoluble in pure nitric acid. (The solvent action of any chlorine present in the nitric acid must here properly be disregarded as belonging in the realm of carelessness. Among later allusions to this topic, W. R. Tan Liew 3 ascribes the solution of the gold in the combination-assay entirely to the action of nitrous acid at the high reaction-temperature of copper and nitric acid ; F. B. Flinn 4 a believes the low result in gold to be due exclusively to mechanical losses-finely-divided gold penetrating through the filter-paper-but presents no experimental data confirmative of this belief; and 0. Pufahl 5 attributes the solubility of the gold in some coppers to the presence of selenium-a view which appears to be shared by many as- 1 Trans., xxiv., 575 (1894). 2 Trans., xxv., 250 (1895). 3 Engineering and Mining Journal, vol. lxix., No. 16, p. 469 (Apr. 21, 1900). 4 Engineering and Mining Journal, vol. lxxxvii., No.11, p. 569 (Mar. 13, 1909). 5 Lunge, Chemische Technische Untersuchungs Methoden, vol. ii., p. 229 (1900).

Jul 1, 1912

By Hannon, J. W. G.

Silicosis is today's most important industrial disease and probably dates back to the Stone Age. Since the industrial revolution, increasing attention has been paid to those occupations where mineral dust is present in the air breathed by the workers. For many years it was assumed that the inhalation of all mineral dusts was hazardous. but investigations conducted in several countries pointed the statistical finger of guilt at free silica in any of its numerous physical forms as a dust of outstanding toxicity. Recognition of silica as the chief hazard has resulted in widespread use of the term "silicosis." Depending upon the concentration of finely divided silica dust to which the individual is exposed and the duration of exposure, silicosis may become a disabling condition in from one to thirty years. The structure of the lung and respiratory passages is such that only minute particles of silica can gain entry to the air cells in the lung (5 microns or under are most toxic). When these minute particles gain entry to the lung tissues they stimulate certain protective cells in the lung to multiply at an excessive rate. The cell's undergo inflammatory changes which result in nodular scars and a low-grade inflammation of the lung tissue. These progressive changes in the lung structure gradually encroach

Jan 1, 1949

By M. F. Goudge, R. V. Tomkins

Sodium sulfate is an important chemical raw material that is being used in ever increasing quantities in modem industry. It comes on the market mainly in three forms: (1) Salt cake (Na2SO4), a relatively crude form of the anhydrous salt containing up to 3 pct impurities, and comprising about three-quarters of the North American production; (2) anhydrous sodium sulfate (Na2SO4), a refined form containing less than 0.3 pct impurities; (3) Glauber's salt, the decahydrate (Na2SO4.10H2O) containing 55.9 pct water of crystallization. Competing with salt cake from natural sources is byproduct salt cake from a number of industrial operations. For instance there is Mannheim cake resulting from the manufacture of hydrochloric acid by the reaction of salt (NaCl) and sulfuric acid in Mannheim furnaces; rayon cake, a high-quality product, resulting from the process of making rayon by the viscose process; chrome cake from the processing of sodium chromate to dichromate; phenol cake from the manufacture of phenol; also byproduct sodium sulfate resulting from the conversion of lithium sulfate to lithium carbonate; from the processing of sodium tetraborate to boric acid; from converting sodium formate to formic acid; and in the manufacture of cellophane. Sodium sulfate is also obtained as a byproduct in the manufacture of isosebasic acid. In addition strong competition has resulted from imports of byproduct salt cake from the chemical industries of a number of highly industrialized European countries. However in recent years due to technological changes the output of byproduct salt cake is rapidly diminishing and the natural deposits are becoming the most important source of sodium sulfate used in North America. For instance, the production of hydrochloric acid in Mannheim plants has become obsolete and thus the greatest single source of byproduct salt cake will disappear. Also viscose rayon is meeting strong competition from nylon and other synthetic fibers and production of byproduct salt cake from this source may do little more than remain at the present level. These factors together with increasing demand for sodium sulfate point to increased production from natural sources. In 1958, 36 pct of the total United States production was derived from natural sources and in addition 97,000 short tons was imported so that over 40 pct of the total consumption was supplied by natural sources whereas in 1953 the proportion was only 24 pct. The rapid growth in production is shown in Table 1. Principal Sodium Sulfate Minerals There are many minerals in which sodium sulfate is a constituent but those of commercial importance at the present time, and consisting wholly of sodium sulfate in either the hydrous or anhydrous states, are mirabilite and thenardite. Minerals of potential importance but consisting in part of compounds other than sodium sulfate are glauberite in which sodium sulfate is combined with calcium sulfate, and blödite in which sodium sulfate is combined with magnesium sulfate. Mirabilite (Na2SO4.10H2O) the decahydrate, consists of 24.8 pct SO3, 19.3 pct Na2O, and 55.9 pct H20. It is a colorless to opaque, soft, water-soluble mineral with a slightly bitter taste. It has a hardness of less than 2 and a specific gravity of 1.48. It forms long needle-

Jan 1, 1960

By M. J. Hordon, M. A. Wright

ReCENT work has indicated that the substantial decrease in the rate of fatigue crack propagation for aluminum observed below a critical vacuum level can be attributed to the depletion of oxygen or water vapor from the vicinity of the fatigue crack opening.' At reduced gas pressures, generally below 10-2 Torr with fatigue strain amplitudes in the range *1 to 2 x 10-3 and cyclic loading rates of 25 to 50 cps, estimated rates of oxide or hydroxide monolayer adsorption on newly formed crack surfaces can fall behind the actual rate of crack extension. Changes in the critical pressure required for the transition in fatigue behavior with changes in temperature, strain amplitude, and cyclic frequency can be interpreted from variations in the adsorption and crack growth rates.'" Although the adsorption model generally appears to explain the enhanced fatigue resistance of reactive metals in vacuum, the specific adsorbing gas species and nature of the adsorption mechanism are uncertain. In addition to the direct dissociation and adsorption of O2 on the metal surfaces,3 the dissociation of H20 and subsequent adsorption of H ions have been advanced for aluminum alloys.4 The present note describes some measurements of the fatigue behavior of 1100 aluminum in reduced partial pressures of specific gases including O2, H2O, and H2 in order to provide additional experimental data. Cantilever-type specimens of 1100-H14 aluminum were fatigued in cyclic reverse bending at constant strain amplitude using a multispecimen vacuum apparatus and procedure described previously.' After initial vacuum evacuation to 1 x 10-7 Torr, the appropriate gas species was bled into the system through a calibrated leak valve. The input rate was adjusted to maintain the desired pressure level under continuous evacuation, thus minimizing possible changes in gas composition during testing. High-purity input gases including 99.9 pct O2, 99.999 pct H 2, and water vapor from triply distilled H 2 O were used to provide residual pressures. Trace amounts of contaminant species were limited by passing the Oz and H 2 input gases through liquid-nitrogen-cooled copper coils prior to entry to the test chamber. Care was taken to repeatedly flush the gas lines and valves before testing to minimize the effect of adsorbed contaminants. Residual gas pressures in the range 10-6 to 5 x x3 Torr were monitored by an NRC ionization gage corrected for each gas species. In the higher-pressure range, 5 x 1CT3 to 5 x 10' Torr, an NRC alphatron gage was used. In operation, eight simultaneous fatigue tests were conducted at a constant strain amplitude of *1.2 x 10 at cyclic bending rates of 25 and 50 cps to give an average fatigue life of 6.5x 105 cycles-to-fracture at standard atmosphere and 3.3 x 106 cycles in 1 x 10"7 Torr vacuum. Representative results for the effect of residual O2, H2O, and H2 contents on the fatigue life are shown in Fig. 1 for tests performed at 50 cps. It is apparent that the presence of either O2 or H2O gas in the system at partial pressures greater than 10"3 Torr was noticeably detrimental to the fatigue life. In contrast, the enhanced fatigue resistance typical of high-vacuum environments was retained with pure H 2 through the pressure range up to 1 Torr. For partial pressures of H2 gas above 1 Torr, the fracture life noticeably decreased. The critical Hz

Jan 1, 1969

By Robert L. Haffner

When mining operations of The Eagle-Picher Co. began in the Illinois-Wisconsin zinc mining field in 1949, all underground loading of broken ore and waste was by caterpillar-tracked machines. Beginning in 1956 rubber-tired end-loaders were brought in; ultimately they completely supplanted the tracked units. End-loaders proved to have the mobility needed for the mining conditions and additional merit in auxiliary capacities. Eagle-Picher operates five mines in this area; two are entered by shafts and three by inclined adits. Several ore zones, some of which are attenuated over a considerable distance, are worked from the same entry. Consequently underground haulage roads connecting or following these orebodies have attained great length. In addition, working places are often widely separated because of the character of the mining operations which include pillar recovery and extending haulage connections into old workings. At one mine, the haulage distance is 5000 ft on either side of the shaft, at another the maximum one-way distance is 8400 ft, and at another the present road system of 6800 ft is expected to reach 10,000 to 12,000 ft.

Jan 6, 1962

THE hall of the Western Iron and Nail Associations having kindly been placed at the service of the Institute, the opening session was held at 3 o'clock, Tuesday afternoon, May 13th, with an attendance of about one hundred and twenty-five members. Mr. William Metcalf, of Pittsburgh, read an address of welcome on behalf of the Local Committee of Arrangements, to which President E. B. Coxe responded. The following papers were then read and discussed : Regenerative Stoves; a Sketch of their History and Notes on their Use, by John M. Hartman, of Philadelphia. Some Curious Phenomena Observed on Making a Test of a Piece of Bessemer Steel, by William Kent, of Pittsburgh. On the Use of Determining Slag Densities in Smelting, by Thomas Macfarlane, of Wyandotte, Michigan. After the reading of these papers each member was presented by the Local Committee with a schedule of excursions, a specially prepared map of Pittsburgh and surroundings, and a directory of industrial works, all tastefully bound, and also with a metal badge bearing the seal of the Institute, to be worn on the excursions. The second session was held on Tuesday evening. The following persons, duly proposed for members and associates of the Institute, were, on the recommendation of the Council, unan¬imously elected. (In this list are included those elected at the final session on Friday morning.) George Bartol, - Cleveland, Ohio. Luther S. Bent, - Steelton, Dauphin Co., Pa. Octave Chanute, - New York City. Albert H. Childs, - Allegheny, Pa. Theodore Cooper, - New York City. Andrew Cosgriff, - Brewster, Putnam Co., N. Y. William B. Crocker, - New York City. Henry M. Curry, - Pittsburgh, Pa. Charles Davis, - Allegheny, Pa. Henry F. De Bardeleben, - Birmingham, Ala. Herbert Du Puy, - Pittsburgh, Pa. Charles L. Fitzhugh, - Pittsburgh, Pa. W. S. Franklin, - Ashland, Md. F. G. Fricke, - Pittsburgh, Pa. Paul A. Fusz, - St. Louis, Mo. Ignatius Hahn, . Pittsburgh, Pa. Henry Hargreaves, - South Pittsburgh, Tenn.

Jan 1, 1880

By L. Leibowitz, M. G. Chasanov, L. W. Mishler

A drop calorimeter system is described for use in measuring enthalpies to 3600°K. Data are presented for tungsten between 2800" and 3600°K. The enthalpy of tungsten in cal per mole between 2000° and 3600°K can be represented by the equation HºT- Hº298 = - 1.7622 X 103 + 5.7772T + 8.9861 where T is in degrees Kelvin. A tabulation of com -puted values is presented for heat capacity, entropy, and free energy function. A drop calorimeter has been constructed to carry out enthalpy measurements at temperatures to 3600°K. Samples are heated by induction1 and dropped into a commercial adiabatic calorimeter, modified for this purpose. The experimental temperature is limited by the melting point of container materials and compatibility of the container and its contents. Several high-temperature drop calorimeters have been described in the literature1-5 but none has been used at temperatures as high as those in the present work; our measurements of the enthalpy of tungsten range from 2800" to 3600°K. DESCRIPTION OF EQUIPMENT An overall schematic view of the equipment is shown in Fig. 1. Power for the induction coil is supplied by a 25-kw 250 kHz Ther-Monic generator coupled to an iron core RF transformer. The Sample capsule is suspended in the work coil by 10-mil diam tungsten wires which are wrapped around a horizontal 5-mil diam tungsten wire. The horizontal suspension wire is clamped between two massive copper electrodes which are fixed in an x-y motion device that allows adjustment of the position of the heated capsule from outside the vacuum chamber. The copper electrodes are connected by flexible copper straps to a 1250-joule (5 kv, 100 pfarad) condenser bank. When it is desired to release the capsule, the condensers are discharged through the horizontal suspension wire causing it to vaporize rapidly. Very reliable and precise release of the capsule is achieved in this manner. Experiments have shown that no heat correction is required for this discharge energy. As part of the temperature measuring system, two prism holders have been incorporated in the apparatus. The upper prism holder is in the main vacuum chamber itself, whereas the lower one is in a side arm attached to the drop tube below the gate valve. The upper prism is mounted on a rotary vacuum feed-through, and may be moved under a protective shield when not in use. This prevents deposition of vapors on the prism surfaces when temperature measurements are not being made. Similarly, the lower prism is mounted on a push-pull vacuum feed-through, and when not in use may be pulled into its side tube. The prism mountings are fitted with guides and stops so that they may be moved precisely into the desired position. The aim throughout is to minimize the time the prisms are exposed to vapors from the hot samples. At the high temperatures reported in this paper, only the lower prism was used. The upper prism holder in these cases was fitted with an additional radiation shield. By using a prism and viewport, the lower surface of the samples can be observed by an optical pyrometer. The measurements discussed in this paper were obtained with a Leeds and Northrup 8622-C-S series manual pyrometer which is estimated to be accurate to 0.5 pct. Pyrometer calibrations and prism and window corrections were carried out in the conventional manner6 using tungsten strip lamps calibrated by the National Physical Laboratory, Teddington, England. Prism corrections were rechecked after each use. All work to date has been done in vacuum, and no measurable change has been observed in the prism correction below -2300°K for the upper prism and below -2800°K for the lower one. The total time of exposure of the prisms is about 50 sec per run. At high temperature, the final temperature reading is corrected by using the final A value for the prism; see Ref. 6 for details of this procedure. The calorimeter is a modified Parr Instrument Co. (Moline, lll.), Series 1230 adiabatic calorimeter with automatic jacket control. Other authors5 have used a similar calorimeter with good results. The calorimeter jacket cover and calorimeter cover are attached to the drop tube which contains a radiation shield. This shield is a gold-plated copper disc which can be operated manually from outside the calorimeter. The receiver is attached below the radiation shield and is lined with tungsten. In a typical experiment, the calorimeter and its jacket water temperatures were adjusted to 0.000°K temperature difference. The sample was allowed to equilibrate in the furnace at the desired temperature for about 20 min. The initial calorimeter temperature was then recorded, the sample dropped, and appropriate shutters closed. After about 3 min, the drop tube and receiver were filled with helium to 60 torr. The final calorimeter temperature was recorded after it had remained constant over a 5-min period. The equilibration time in the calorimeter was about 25 min. Thermistor probes are used to operate a hot and cold water supply system to maintain the jacket temperature equal to the calorimeter temperature. For actual measurements of the calorimeter temperatures, a quartz thermometer was used (Hewlett Packard Dymec Thermometer, Model #2801A). This thermome-

Jan 1, 1970

By Bernard Kopelman

THE particle size of tungsten metal powder used to make tungsten wire for use in radio tubes and incandescent lamps must be closely controlled if the highly desirable feature of nonsagging is to be achieved. Our knowledge of factors affecting the particle size of tungsten powder has been limited by lack of any extensive literature on the subject. There are no publications in the English language discussing this problem in any but the most general terms. In this paper the published experimental information on this subject is reviewed. Based on the published data and some experimental data obtained by the author, a general theory of factors affecting the particle size of tungsten metal powder obtained by reduction of the oxides in hydrogen is offered. The various forms of the tungsten oxides and tungsten metal used in the experiments described were those prepared by com¬mercial processes, so that the experimental results obtained on a laboratory scale would be more directly applicable to actual commercial reduction conditions. The effects of time of reduction, temperature, and concentration of water vapor in the hydrogen were observed by counting microscopically the particle distribution obtained. Such a method is very time-consuming, but the data obtained by this method are more reliable and more fundamental than those obtained by any of the several instruments available for measurement of particle size. REVIEW OF THE LITERATURE Until the year 1912, tungsten powder was prepared commercially by reducing tungstic oxide in the presence of carbon or one of its compounds (such as glycerin or ethylene glycol), usually by firing the mixture in a closed fire-clay crucible. The resultant powder contained about 95 per cent tungsten.1 When reduction of tungsten oxides by H2 was introduced commercially, 2.1 several investigators became concerned with the equilibria between tungsten metal and its several oxides in an atmosphere of hydrogen and water vapor.4-13 While these many investigations were in fair agreement on the equilibria there arose considerable controversy as to the chemical composition of the oxide between W03 and W02, because of very poor agreement on the equilibrium constant of this intermediate oxide reduction reaction. The controversy on this intermediate oxide has been in progress for more than 10o years. Thus Malguti,14 in 1835, decided it was W02.56. In 1857, Riche" proposed the formula W308. Usler,16 in 1865, confirmed the existence of W308 and further proposed W4O11. In 1897, Desi17 agreed upon W308 but also found W5014.

Jan 1, 1946