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United Engineering Trustees, Inc. GEORGE D. BARRON ARTHUR S. DWIGHT R. M. ROOSEVELT The Engineering Foundation H. C. BELLINGER E. DEGOLYER J. V. N. DORR

Jan 1, 1932

By Janshi Sen

VERTICAL-INTENSITY magnetometers, such as the Hotchkiss Superdip and the Askania vertical field balance, are now [ ] widely used, because vertical-intensity charts give definite information for the location of upper pole, dip and strike, and approximate shape of the deposit. Again, a slow and steady increase of dip over a large area indicates a large deep-lying deposit, while a large dip limited to a small area and falling away rapidly suggests a small and shallow one. The complication comes more from the richness of the ore. A large body of lean ore near the surface might produce the same vertical-intensity chart as a rich ore at depth. This paper presents a method for calculating the maximum depth of a single-pole deposit and another for a two-pole mineral body, by utilizing data of both vertical and horizontal intensities as obtained by a Thalen-Tiberg magnetometer. As shown on the left side of Fig. 1, lean ore, rich ore and a single pole produce the same magnetic field. The depth of the pole, [ ] h, can be calculated from the following relation: [h=a=tan¢=G-F h=aXFy] where G is the vertical intensity at point A due to the pole; F, the horizontal intensity of the same; and a, the distance from the point of maximum vertical intensity or the vertical projection of the pole on the surface to the point of observation A. If an entirely covered deposit is indicated by magnetic measurements and boring cost estimated from the calculated depth is so reasonable as to encourage drilling, the ore should be struck somewhere within the limit of the calculated depth by the borehole. A number of such points as A should be taken for calculation, erratic results should be rejected and the average figure used for cost estimation.

Jan 1, 1944

By VERITAS

THE most concentrated industry of major character in the United States is that of the Ford Motor CO., which is to say Henry Ford. Its sole function is to supply the public with a cheap motor car which it does to the extent of two million or so per annum. In doing this, a relatively small profit per unit is multi- plied to an enormous aggregate per annum and has resulted in the creation of one of the greatest industrial fortunes of the world. The industrial and sociological consequences of .this are bound to be immense. On the physical side the production of two million automobiles means the consumption of two or three million tons of materials, chiefly metals, in the 'direct form of the finished product', and a huge additional tonnage of coal and other things that ,are consumed en route, and also the labor of many thousands of men. In the development of a business on this scale it was but natural that the Ford Motor ,Co. should seek to supply itself with the raw 'materials it needs, and they being so largely coal and metals the company is brought into close contact with the mining and metallurgical industries. It is a huge consumer of - steel. It is the fourth largest consumer of copper. It is a large consumer of lead, tin, aluminum and zinc. The mining and metallurgical industries have, therefore, good reason to learn to know Henry Ford, his personality, his thoughts and his policies.

Jan 1, 1924

By Howard Willey

MINING operations of the Charcas unit at present are limited to the Tiro General mine at Charcas, in the State of San Luis Potosi, Mexico. The Tiro General mine was first operated during the Spanish occupation of Mexico for rich silver ores in an oxidized zone along the outcrop of the principal vein. In depth the ore is a complex sulfide with widely varying proportions of sphalerite, argentiferous galena and chalcopyrite; and until recent years, it was economically impossible to carry on mining otherwise than irregularly in sections of the veins richest in galena and chalcopyrite. The advent of selective flotation brought the orebody as a whole within the field of economic interest, and a flotation mill of 650 metric tons daily capacity was constructed in the year 1925. The mining of partly worked-out sections of the mine, as well as the very heavy ground in most of the stopes opened in virgin ore, presented an unusually difficult problem. This -paper describes the so-called "filled top slice" stoping method finally adopted as the standard system.

Jan 1, 1930

By Oscar Weiss

An aerial magnetometer survey was carried out by the author's geophysical organization over the Vredefort dome, where Witwatersrand beds are wrapped around a granite plug 25 to 30 miles in diameter. The well- known magnetic shales of the Lower Witwatersrand system (to be referred to as LWW) give strong negative anomalies over the out-cropping portion of the dome. This is unusual as these same shales -cause positive anomalies over large areas near Johannesburg and along a strike of 130 miles between the East Rand and Klerksdorp. It is suggested that the negative polarization is caused by heat and stresses connected with the doming. This negative polarization of sedimentary beds, which usually cause positive anomalies, is a good example of how "magnetic lows" can be caused by "structural highs." Significant magnetic anomalies should be tested by gravity and seismic methods irrespective of the sign of the anomalies.

Jan 1, 1949

By AIME

D R. GILLSON, who was born in Evanston, Ill., in 1895, is another one of those geologists who received his early inspiration and foundation in his science from that great teacher at Northwestern University, the late Professor U. S. Grant, and then went on to give his time and interest to Institute affairs-like those other Northwestern men, Arthur Blair, Gilbert Cady, Charlie Behre, Evan Just, Ian Campbell, Clayton Ball, and many others. After serving in the Navy in the first World War as, of all things for a geologist, a commissary officer on a transport, he went on to MIT and took his doctor's degree under Waldemar Lindgren in 1923. He even assisted in mineralogy at Harvard and thus had training under another great teacher, Charles Palache. He taught mineralogy and petrography at MIT from 1923 to 1928. After several summers of field work as an assistant in the U. S. Geological Survey, Dr. Gillson joined the staff of the du Pont company.

Jan 1, 1947

By W. M. Parris, P. D. Frost, H. A. Robinson

The effects of hydrogen content and strain rate on the static tensile and notch-rupture properties of the Ti-3Mn-complex alloy heat-treated to differed strength levels were investigated. The extent of embriulement was found to be proportional to the amount of hydrogen present and the strength to which the specimens were heat-treated. The research suggests the possible necessity of specifying lower hydrogen limits than are now allowed when titanium alloys are heat-treated to higher strengths than are presently used. The research also supports a hypothesis advanced earlier for a mechanism of hydrogen embrittlement. MUCH attention has been focused on the effects of hydrogen in in Most of the published in- formation has dealt with the effects of hydrogen on alloys in the annealed or lowest-strength condition. The work of Kotfila and Erbin3 is one of the few exceptions. In view of the fact that heat-treatments are now being used to produce high strength in titanium alloys,' it is necessary that more attention be given to the effects of hydrogen on these alloys in the heat-treated condition. Research was initiated to establish the effects of hydrogen on the properties of the Ti-3Mn-complex alloy at various strength levels. This research, which supplemented that of Kotfila and Erbin, was started because it was found that high-strength tensile specimens of this alloy were strain-rate sensitive. The essential results of the research are summarized in this paper. MATERIALS AND EXPERIMENTAL PROCEDURES Material for this investigation was a 41/2-in.-diam bar forged from a single commercial heat of the Ti-3Mn-complex alloy having the composition given in Table I. The as-received forging was reduced further by forging at 1750°F to 3/4-in. square bars. About one fourth of this material was vacuum annealed at 1400°F for 24 hr to obtain a base hydrogen content of 25 ppm. The remaining bars were hydrogenated to levels of 90, 140, and 260 ppm in a large Sievert's apparatus in the following manner: Four 3/4-in. square bars, 5 in. long, were placed in the reaction chambzr. The chamber was evacuated, heated to 1400°F, and a measured amount of hydrogen was introduced. When absorbtion was complete, as indicated by the drop in pressure, the reaction tube was cooled and the bars removed. Each batch of bars was then sealed in individual evacuated Vycor containers and heated for 24 hr at 1400°F in order to distribute the hydrogen homogeneously. After vacuum-annealing or hydroge nation, the bars were rolled at a temperature (1400°F) below the ß-transus to 1/2 - in. - diam rounds. Groups of the rolled specimens representing each of the hydrogen levels were given the following heat-treatments: 1) One hr at 1300°F, water-quenched. 2) One hr at 1300°F, water-quenched, and aged 8 hr at 1100°F. 3) One hr at 1300°F, water-quenched, and aged 4 hr at 1000°F. 4) One hr at 1300°F, water-quenched, and aged 48hr at 800°F. Heat-treated bars were machined into standard 0.250-in.-diam tensile specimens having 1-in. gage lengths. Throughout the processing and testing of this material, hydrogen analyses were made by vacuum-fusion methods to check for accuracy of hydrogen additions, homogeneity, and possible losses during processing. A summary of these analyses is given in Table II It may be seen that the actual hydrogen contents were reasonably close to the desired levels. In addition, it was noted that the variation in hydrogen content within any one bar did not exceed

Jan 1, 1959

By N. S. Wagner, R. S. Mason

The production of lightweight aggregates in Oregon is a new industry, and, like all new enterprises, it is suffering from growing pains characterized by numerous, small operations some of which flourish for a short time and then cease altogether. Norinally all industrial mineral products are produced in a highly competitive atmosphere. At the present time this condition does not exist to a very marked degree in the state because as yet producers have not saturated the constantly expanding market. This paper has been prepared with the intention of outlining very briefly the current status of the various products now heing used as lightweight aggregates in Oregon. The present piche will surely change, perhaps quite radically within even a short space of time. Lightweight Aggregates Used in the Northwest PUMICE Interest in Oregon pumice is not new. Deposits are abundant. Successful development, however, dates only from 1946. During 1948 a total of nine operations was engaged in full or part-time production of aggregate. The postwar building boom and increased public consciousness regarding the value of insulation are the immediate reasons behind the current development. Just how firmly this production of pumice aggregate may be established is something which cannot be foretold at the present time. Much will depend upon how successfully the pumice aggregate construction already installed stands the test of time. Some fine pumice aggregate products have been made and it seems probable that because of its unique properties a certain demand for pumice aggregate will continue in the future. Fire-proof, rodent-proof, decay-resistant properties supplement the lightness in weight and insulation properties of pumice aggregate products in rendering them particularly ideal for many types of construction. In addition there has been fabrication in the form of reinforced fence posts, street markers, and similar products of a specialized-product nature and these are not to be overlooked in terms of future production. Also pertinent to how soundlj pumice aggregate production is established will be possible future competition with other lightweight aggregates. However, this situation will be governed largely by competitive costs of production and marketing. For its present use, which is almost exclusively limited to the manufacturing of building blocks, the market for Oregon pumice aggregate has been extended from the mining area around Rend and Chemult to points as far distant as San Francisco and Seattle. Naturally enough the bulk of the production goes to the Portland and eastern Oregon consumers. Shipments are made by both rail and truck. Early in 1947 the State Department of Geology and Mineral Industries made a canvass of all pumice producers in the state. The production for 1956 amounted to 26,614 cu yd and was valued at $13,649 at the plants. The United States Bureau of Mines estimates the production for 1947 as 33,240 short tons valued at $111,380. This is roughly 65,000 cu yd. No data are available for the 1948 production but it is understood to exceed that for 1947. The Oregon pumice occurrences originated largely from the eruption of Mount Mazama, the name of the formerly active volcano and the location of Crater Lake. Other lesser volcanoes throughout the area contributed to the present occurrences, however, and it has been estimated by Moore' that the pumice deposits cover an area of some 3500 square miles. This area lies east of Crater Lake between Bend and Klamath Falls and embraces the southern portion of Deschutes County, the northern part of Klamath County, and the northwest corner of Lake County. Thickness of the pumice ranges from thin skims to local thicknesses of as much as 30 to 40 ft. Fragment size also varies greatly. Any attempt to describe the situation by giving screen analyses would be confusing because of the wide variations to be found in all area of this size. The picture can best be summed up by stating that places showing great variations in fragment size can be found if a search for extremes is made. For mining purposes in connection with aggregate production, it call be stated that miles and miles of pumice exist in which the fragrnent sizes range from an inch or so downward. The usual color of the pumice is a light gray to off-white. A typical pumice analysis shows a silica content of about 69 pct, alumina 15 pct, and sodium oxide about 5 pct. Potash, lime, and water are the next three most abundant constituents, running just a little over 2 pct each. Iron oxides are fairly constant at 2.75 pct. Titanium, manganese, magnesium, and phosphorus occur in amounts of less than 1 pct. All of the foregoing substances are combined as a glass exhibiting cellular structure. The weight of crushed but otherwise pit-run (undried) pumice runs around 1100 Ib per cu yd according to figures furnished by various producers. The minimum and maximum weights per cubic yard reported are 1050 and 1400 lb, respectively. The 1400 lb per cu yd pumice contrasts with the pumice from most of the other

Jan 1, 1950

By Robert L. Gower, John H. Cash

Interconnections for integrated circuits operating at rnicrowaue frequencies rzust be formed as microwave transmission lines. This paper describes the fabrication of one type of microwave transmission line known as microstrip, which can be fabricated on momlithic integvated circuits by deposition of 0.1- to 2.0-mil-thick metal and dielectric films. A microstrip line consists of a narrow conducting strip separated from a gvound plane by a dielectric material. Thick films of good conducting materials are required for low loss at high frequencies. Vacuum-evaporation methods for depositing aluminum and silver films are described. The narrow conducting strip forming the top conductor is defined by photoresist-etching techniques after the thick rnetal film is deposited. Gold plating with a photoresist-masking technique is also used to forrrz thick metal conductors. The microstrip dielectric layer is formed by deposition of suitable dielectric films 0.1 to 2.0 mils thick. Several deposition techniques were investigated. Electron-beam evaporation of quartz is described. Electrical characteristics of deposited microstrip lines at microwave frequencies are included and the microwave power attenuation as a function of conductor and dielectric thickness is given. It is concluded that the deposition of microstrip transmission lines is a practical way to achieve low-loss interconnections in monolithic integrated circuits. CONNECTIONS between devices in low-frequency and digital circuits are usually made by connecting the devices with a length of conductor such as a metal lead oi- a wire. If this method were applied to microwave integrated circuits, the reactance of the connection due to the series inductance and parasitic capacitance would be very high, in fact too high to permit successful circuit operation. In addition, resonance and antenna effects would occur at high frequencies, especially when the connections approach the wavelength.' Connections which are sections of transmis- sion line will overcome these difficulties. The electromagnetic field is confined to the volume of the transmission line, parasitic effects are not present, and circuit design utilizes familiar transmission-line techniques. TRANSMISSION LINES One type of transmission line geometrically adaptable to integrated circuits is known as micrstri. A microstrip line can be generated from a coaxial line as shown in Fig. l(a). The outer conductor of the coaxial line is distorted into an ellipse (b) and finally separated at the extremities of the ellipse to form the strip transmission line shown in (c). One of the ground planes is then removed, leaving a conducting ground plane and a narrow conducting strip separated by a dielectric. Two configurations of the microstrip line were considered in this investigation, Fig. 2. Type (a) is fabricated from a semiconductor slice with the ground plane and top conductor deposited on each side of the slice. The semiconductor slice serves as the die lec-

Jan 1, 1967

THE IRON HUNTER. By Chase S. Osborn, pp. 316, Ills. 10. The MacMillan Company, New York. 1919. An autobiography, the story of a Hoosier boy who fought his way to manhood and power through early misfortune and poverty, from street urchin and newsboy, to editor and author; from lumberjack and dock walloper to statesman and Governor of Michigan. The reader has the measure of the man in the first chapter, a dramatic recital of how the fighting boy editor cleaned up a lawless mining camp of 40 years ago. The thread of the narrative is the author's life-long devotion to outdoor living, ex-ploration and travel. Residing in Sault de Sainte Marie, Mich., in the heart of the Lake Superior country, he took his delight and, incidentally, found his fortune in prospecting the north woods for iron ore; eventually, extending his travels to the continents and many of the islands of the world, he discovered what, he believes-to be a great iron range in Madagascar. In this book there is plenty of anecdote, a great deal of wholesome social and po¬litical philosophy and some interesting sidelights on the characters of some of the author's prominent contemporaries in the political life of Michigan. The style is direct and animated, flavored and illuminated with the vernacular of Hoosierdom and the woods country of the North. The author levies on the vocabulary of the sciences and the classics for many a noun and adjective and, with Rooseveltian license, now and then coins a word. The reader's interest will be gripped from cover to cover, albeit he may occasionally need a dictionary. R. C. A.

Jan 11, 1919

Organization Place Date 1917 American Institute of Architects Philadelphia,.,; Pa. Dec. 26-29 American Society of Mechanical Engineers New York City. Dec. 26-29 American Mining Congress State Chapter Phoenix, Ariz. Dec. 26-29

Jan 11, 1917

By C. G. Rhodes, D. Kramer

The kinetics of precipitation of transient a phase during the transformation in U-16 wt pct Mo between 400° and 550°C were studied using quantitative metallography and electrica1 resistiuity measurements. The volume percent of a phase goes through a maximum in time, corresponding to a critical degree of progress of y' formation. prior to its re-solution after prolonged annealing. The fastest rate of a precipitation oc-cuvs at 500°C with a concomittant lowest peak of 9.5 vol pct a. At 450°C, 14 vol pct a, greatest fov any temperature, was observed after 24 hr witlz an associated slowest rate of formation. a precipitation at 400°C ceases after approximately 160 hr and the amount of a present remains unchanged after long times at temperature; no y' was observed metallographically at this temperature. IN the U-Mo system at 16 wt pct Mo, an ordering reaction takes place below 600°C, see Fig. 1, whereupon the random bcc solid solution, y, transforms to the ordered bct phase, y'."2 The new unit cell is constructed of three old unit cells somewhat distorted. While attempting to study the kinetics of this transformation it was observed that an unexpected phase was precipitating out early during the transformation anneal reaching appreciable amounts before disappearing after long times. The y' appeared in the presence of this new phase and after long times constituted the whole sample. Owing to the high optical activity of this unexpected phase under polarized light, it was suspected to be the a phase. Subsequent X-ray powder pictures confirmed this belief. The kinetics of a phase formation and disappearance is the subject of this paper. EXPERIMENTAL PROCEDURE A) Alloy Preparation. Alloys for this study were prepared by vacuum induction melting normal reactor grade uranium and 99.5 wt pct Mo pellets in thoria crucibles. Two ingots were prepared, and sections of the top and bottom of each ingot were chemically analyzed for uranium and molybdenum content. The results of the analyses appear in Table I. B) Metallography. Samples of 16M were wrapped in tantalum foil, sealed in evacuated (5 X 10"6 mm of Hg) quartz capisules, and annealed at 1110"C prior to being transferred directly to the transformation temperature. They were examined metallographically after increasing times to determine the progress of the transformation at 400°, 450°, 500°, and 550°C. The samples were prepared for metallographic examination by mechanical polishing with diamond paste and electrolytic polishing with a solution of glacial acetic acid and chromic acid. Since the y' phase is tetragonal, its presence can be detected by viewing the sample in polarized light. To increase the contrast between y' plates, the samples were electro-etched in a 10 pct oxalic acid solution. To reveal a phase in bright field (it can be seen in polarized light in the "as-polished" state), the samples were electro-etched in a solution of citric acid and nitric acid. To determine the vol pct a phase, a variation of the one dimensional systematic point count method as described by Hilliard and cahn3 was used. The

Jan 1, 1962

By W. R. Atkins

The Negaunee mine is at the east end of the Marquette Range, in the city of Negaunee, on the Upper Peninsula of Michigan. Iron ore was first discovered on this property in 1883 by diamond drilling. A shaft was sunk soon afterward. and the mine has been worked continuously ever since. The total shipments from 1887 to Jan. I, 1945, were 20,417,587 long tons. The mine was taken over by the present operators, The Cleveland-Cliffs Iron Co., in 1903. During the past four years, 1941 to 1944 inclusive, the property has produced an average of nearly a million tons a year, and has employed more than 400 men. Geology The ore body at the Negaunee mine lies in a large syncline dipping about 15° to the west, the ore coming to ledge at the east end of the trough. The ore occurs in the Negaunee formation of the middle Huronian age, which consists of ferruginous cherts and slates through which intrusions of diorite have occurred. Although these intrusions of diorite have an important bearing on the formation of ore on the range, they are not important in this ore body. Some faulting has taken place along the diorite intrusions, or dikes as they are called locally, and also other faults are known to exist across the formation. These faults do not complicate either mining or development of the ore body. The footwall consists of jasper underlain with Siamo slate; the hanging wall is jasper and ferruginous chert. Fig. I shows a typical cross section of the ore body. The ore body is quite regular, about 120 ft. thick in the middle of the syncline and thinning out toward both sides of the fold. Its width ranges from 400 to 800 ft., the average being about 600 ft. The footwall is uniform in dip and strike, but irregular lenses of ore often extend 50 to 75 ft. up into the overlying jasper capping. Method of Mining Ore in the Negaunee mine has been mined by top slicing almost exclusively since 1903 This method of mining has been employed because it is especially adapted to the size and shape of the Negaunee ore body, and to the soft, sticky nature of the ore as well as the generally soft, broken jasper capping. Development The ore body has been developed from six different levels with intervals varying between loo and 125 ft. On the average, the dip causes a horizontal offset of 350 ft. per level, and under these circumstances it has been necessary to carry on considerable development in rock to make available the ore lying along the north and east footwalls. This is not as disadvantageous as might be supposed, because of reduced pressure and the accompanying saving in maintenance costs. The development of the

Jan 1, 1949

By W. A. Rachinger, C. Graeme-Barber, R. L. Bell, R. C. Gifkins, T. G. Langdon

R. L. Bell. C. Graeme-Barber, and T. G. Langdon (Imperial College. London)— The internal-marker technique developed by Ishida, Mullendore, and Grant has enabled them to make some interesting observations on the role of grain boundary sliding in creep. Certain of their conclusions are supported by our own similar experiments on Magnox AL80 (Mg-0.8 pct Al) specimens containing several markers, full details of which will be published shortly. In particular, we would agree that: 1) Using the internal-marker method, there is little difference between Egb, the contribution made by grain boundary sliding to the total strain, measured at the surface and in the interior of a specimen. 2) The measurement of the change in grain shape during creep leads to an underestimation of the grain strain, and hence an overestimate of Egb.. However, the discrepancies between the values obtained by this method and those obtained using markers are not as great as Tables IV and V of Ishida, Mullendore, and Grant would suggest; see below. The authors' Eq. [I] which is used to compute Egb from the transverse displacement ITt of longitudinal marker lines is not given in the reference quoted,'' where in fact only relations for Egb in terms of the longitudinal displacements of markers were developed. As first pointed out by Gifkins and Gittins,12 a problem arises in the use of longitudinal markers. and we will show that Eq. [1] underestimates Egb in the interior by a factor of 2. In Fig. 12, two grains X and Y have become displaced by the vector AC which lies in the plane of the grain boundary ABCD separating them. A longitudinal marker has been split by this displacement into the two parts LA and CAW. If these were surface grains the transverse displacement, Ut. could be obtained by viewing normal to the "top" surface. If interior, a section through CD parallel to the top surface would show the same result, provided the longitudinal internal markers delineated planes normal to the top surface. (This is an essential feature of the markers not pointed out in the paper.) The important point is that the quantity Ut tan B (=BE=DF) only gives the elongation due to the one component AB of the sliding. The elongation V/tan 8 (=GD) due to the component AD must be added to produce the total elongation resulting from the boundary displacement AC. If the grain boundaries in a poly crystalline specimen are randomly oriented with respect to the stress axis it follows that In the interior of a specimen the two sums depend for any difference simply on the definitions "top'' and "side". On the surface it is possible that the two sums could differ somewhat. In either event it is clear that the authors' Eq. [I] underestimates Egb, and in the interior, and perhaps at the surface also, the appropriate formula is given by The suggested modification probably makes little difference to the comparison between surface and interior values of Egb where both were obtained from marker measurements. For the estimation of the correction becomes extremely important where the boundary contribution is large. In our own work on magnox, for example, we have obtained values of as large as 70 to 80 pct, under conditions of high temperature and low strain rate. The use of planar markers transverse to the stress axis would simplify the comparison between surface and interior behavior, because measurement of the longitudinal offsets Us of these markers could be summed to give the total elongation di-

Jan 1, 1965

By W. E. Wrather

DURING the war the mineral industry, and metal mining in particular, extended itself more than any other to attain the limit of its productive capacity. Likewise, probably no other industry went quite so far toward jeop¬ardizing its own economic future through depletion of material reserves. Once we looked to Europe for most of the manufactured goods we needed. Our own limited mineral requirements were easily supplied from mines near the Eastern seaboard. With expansion and industrialization, our mineral needs increased in proportion, and the centers of mining activity moved westward to Michigan, Wisconsin, Minnesota, and the Tri-State district, where seemingly inexhaustible high-grade deposits of iron, copper, lead, and zinc ores were opened and rapidly developed.

Jan 1, 1946

[†AARONSON, ALFRED E., Vice-Pres., Mid-Co. Petroleum Co., Mid-Co. Bldg., Tulsa Okla. '18 ABADIE, EMILE R., Min. Engr Box 927, Porterville, Cal. '76 ¦ABADILLA, QUIRICO A. Student, Colorado School Of Mines, Golden, Colo. '20 ABBOTT, CLARENCE E., Gen'l Supt. Iron Mines Div., Tenn. Coal, Iron & R. I. Co., 1405 Minnesota Ave., Bessemer, Ala. '04] [ ]

Jan 1, 1925

By L. D. Jaffe, R. K. Pitler

IT would clearly be advantageous to produce molten titanium, suitable for alloying and casting, directly from the relatively inexpensive tetra-chloride, without using a metallic reducing agent. Accordingly, a preliminary investigation has been made of the production of titanium by hydrogen reduction of the tetrachloride in an electric arc furnace. For the reaction: TiCl4(g) + 2H2(g) ? Ti(s) + 4HCl(g), Lockhart and his colleagues' have calculated equilibrium constants at 800" to 1500°K, based on tables of Brewer.' Extrapolating these data on the assumption that the heat of reaction varies linearly with temperature, and using Brewer's value for the heat of fusion, there is obtained for the reaction: TiCl4(g) + 2H2(g) ? Ti(l) + 4HCl(g) an equilibrium constant at 2100°K (100" above the melting point) Kp = (PHCl)4/pTlcl4 (Ph2)2 = 0.167 atm. If this is correct, starting with hydrogen saturated with TiC14 at 25°C, where the vapor pressure of the latter3 is 12.6 mm, and maintaining the overall pressure at 1 atm, 99 1/4 pct of the TiC14 would be reduced to Ti at equilibrium. An arc furnace designed for the melting of titanium and lined with water-cooled copper was used for the preliminary experimental check. Its inside diameter was 2 7/16 in. and height 6 in. The water-cooled electrode was tipped with 3/4 in. diam tung-sten. In the one run carried out, the furnace was charged with a starting batch of 293.35 g of scrap titanium,' analyzing 99.24 pct Ti. After the system was twice pumped out and flushed with argon to remove air, the arc was struck in argon and kept at 400 amp dc, electrode negative, for 1 min to melt the starting batch. Commercial tank hydrogen, dried by passing over silica gel and bubbled through technical grade TiC14 at room temperature, was then admitted to the furnace. The inlet tube directed this gas downward toward the arc and melt; the gas outlet was at the top of the furnace. The quantity of gas passed through was not measured accurately but is estimated to be about 50 liters per min at a few mm of mercury above atmospheric pressure. The arc was held in the H2-TiC14 mixture at 400 amp with little difficulty. After 10 min the arc burned through the copper lining above the melt, admitting water and ending the run. (This had happened frequently in straight melting runs under argon, and is not thought due to the atmosphere used.) In the furnace were found an ingot, several small pieces, and a little metallic powder, evidently formed when water entered the hot furnace. Some titanium also clung to the electrode. The portions were weighed and separately analyzed for titanium. Their total weight was 321.76 g of 94.82 pct overall purity. Much of the impurity consisted of tungsten broken off when the titanium was removed from the electrode. No detailed impurity analysis was made because the starting materials were impure and flooding the furnace introduced further contamination. Thus, the metal recovered contained 305.08 g Ti, as compared to 291.12 g in the starting batch. Titanium could not have been carried over from previous melting runs in the furnace, as the interior was sandblasted and the electrode ground clean before the run. Evidently at least 13.96 g of Ti were produced from TiCl4. Since this would require complete reduction of 430 liters of TiCl, gas at 12.6 mm of Hg, the efficiency of the process must have been rather high. Experimental work is continuing. No reason is seen why the process could not be scaled up to the size of a 30-ton steel-melting arc furnace. In a large unit there would be a large molten pool from which liquid metal could be withdrawn for alloying and casting. The problems of electrodes and power supply are similar to those arising in arc furnaces for melting titanium. Unreacted TiC14 and the HC1 in the exhaust gases could be recovered; unreacted H2 could be dried and re-used. The melt would be saturated with hydrogen, whose solubility in liquid titanium is unknown. Small amounts of hydrogen seem to have little effect on the properties of titanium.5 If the amount introduced was so large as to impair properties or cause casting difficulties, it could be reduced by holding the melt under an inert gas or by pumping on it, prior to casting. Acknowledgment The authors would like to thank I. Preble and M. Goldman for their valuable aid in the experimental work and the thermodynamic calculations, respectively. References 1R. J. Lockhart, J. J. Ward, M. J. Hussey, and J. W. Clegg: In unpublished report, "U. S. Air Force Project Rand. Titanium and Titanium Base Alloys." Battelle Memorial Institute (1949) 37-44. 2 L. Brewer et al: Chemistry and Metallurgy of Miscellaneous Materials—Thermodynamics. Ed. by L. L. Quill. pp 13-39, 60-192. (1950). McGraw-Hill Book Co. 3 K. Arii: Scientific Reports. Tohoku Imp. Univ. (1933) 22, 182. 4 R. S. Dean, J. R. Long, F. S. Wartman, and E. L. Anderson: Transactions AIME (1946) 166, 369-381; Metals Technology (Feb. 1946) TP 1961E. * R. I. Jaffee and I. E. Campbell: Transactions AIME (1949) 185, 646-654; Journal of Metals (Sept. 1949) TP 26813.

Jan 1, 1951

By R. H. Jacoby, M. J. Rzasa

Experimental equilibrium vaporization ratios were obtained for nitrogen, methane, carbon dioxide, ethane, and hydrogen sulfide in natural gas-condensate systems. Two different overall mixture compositions were investigated over the pressure range 500 to 4,000 psia at 100°, 150°, and 200 °F. Partial phase diagrams of the mixtures were obtained; one of these showed a critical point at 204°F and 3,875 psia. These and earlier data' were compared with the Kellogg correlation' at! 100°F and 1,000 psia. INTRODUCTION The authors' have presented equilibrium vaporization ratios for nitrogen, methane, carbon dioxide, ethane, and hydrogen sulfide in complex mixtures, such as natural gas-crude oil and natural gas-absorber oil. Since mixtures of the natural gas-condensate type also occur widely in petroleum reservoirs and often contain the non-hydrocarbons mentioned, it would be useful to have appropriate K data for calculating equilibrium vaporization conditions. Roland, Smith, and Kave-ler' obtained K's for methane and the light hydrocarbons in gas-condensate mixtures; and Poettmann and Katz3 obtained K's for carbon dioxide in a gas-condensate system. The data presented in this paper extend this coverage to include K's for nitrogen and hydrogen sulfide and phase diagrams for the experimental mixtures. EXPERIMENTAL WORK The equipment and experimental procedure was essentially as described previously, except for analysis of the vapor samples. The vapor sample bombs were filled at the pressure and temperature of the run. Immediately after sampling, a portion of this sample was flushed from the bomb into a 650 cc glass bulb, filling it to near atmospheric pressure. The sample in the glass bulb was then analyzed by the mass spectrometer. Some checks were made on this analytical procedure to find the accuracy of measurement of the C + content of the vapor samples. The modifications tried were complete fractionation of the vapor sample and the use of several liquids (depropanized condensate and retrograde liquid from several vapor samples) as calibrating materials for the mass spectrometer. The results obtained from these various checks differed by about 10 per cent relative and this is believed to be the order of accuracy of the vapor C+ concentrations.

Jan 1, 1953

By S. C. Sun, A. M. Gaudin

This paper presents the results of a. study of the relationship of the electrokinetic or zeta potential to flotation phenomena. The relationship is established on the experimental evidence that mineral behavior in flotation and in cataphoresis is generally governed by the chemical properties and amount of the reagents adsorbed at mineral surfaces. Cataphoresisl-5 or electrophoresis is the name given to the movement of a charged particle in a liquid medium under the influence of an applied electric field. Mineral behavior in cataphoresis, as indicated by the magnitude and sign of its ionic charge, can be represented by the term zeta potential. In this paper, the zeta potential represents the difference in potential between the immovable liquid layer attached to the surface of a solid particle and the movable liquid layer in the body of the liquid, and is the result of the tendency of ions on the surface of the particle and within the liquid boundary layer to establish a condition of equilibrium. A high positive zeta potential means that the mineral surface is dominated by cations, a high negative zeta potential indicates domination by anions, and a low zeta potential indicates that the surface is influenced almost equally by cations and anions. In terms of observed quantities the zeta potential is given by the relation _ 4µ(300)² Z= kx in which z is the zeta potential expressed in in volts, µ the viscosity of the solution in poises, u the velocity of particles in centimeters per second, x the impressed potential gradient in volts per centimeter, and k the dielectric constant of the solution in c.g.s. units. A convenient source for the derivation of the equation is the book by Thomas. The term zeta coefficient is an expression coined to denote the difference between the magnitude of the zeta potential of a mineral suspended in solution A, and that of the same mineral suspended in solution B, which consists of solution A and an additional chemical agent, but is at the same pH. For example, the difference between the zeta potential of galena particles in distilled water and that in any chemical solution at the same pH is a zeta coefficient. Or, when the zeta potential of a mineral particle is measured first in distilled water, then in a mixture of water and copper sulphate, and finally in a mixture of water, copper sulphate and xan-thate, we can calculate the zeta coefficient

Jan 1, 1947

By A. M. Gaudin, S. C. Sun

This paper presents the results of a. study of the relationship of the electrokinetic or zeta potential to flotation phenomena. The relationship is established on the experimental evidence that mineral behavior in flotation and in cataphoresis is generally governed by the chemical properties and amount of the reagents adsorbed at mineral surfaces. Cataphoresisl-5 or electrophoresis is the name given to the movement of a charged particle in a liquid medium under the influence of an applied electric field. Mineral behavior in cataphoresis, as indicated by the magnitude and sign of its ionic charge, can be represented by the term zeta potential. In this paper, the zeta potential represents the difference in potential between the immovable liquid layer attached to the surface of a solid particle and the movable liquid layer in the body of the liquid, and is the result of the tendency of ions on the surface of the particle and within the liquid boundary layer to establish a condition of equilibrium. A high positive zeta potential means that the mineral surface is dominated by cations, a high negative zeta potential indicates domination by anions, and a low zeta potential indicates that the surface is influenced almost equally by cations and anions. In terms of observed quantities the zeta potential is given by the relation _ 4µ(300)² Z= kx in which z is the zeta potential expressed in in volts, µ the viscosity of the solution in poises, u the velocity of particles in centimeters per second, x the impressed potential gradient in volts per centimeter, and k the dielectric constant of the solution in c.g.s. units. A convenient source for the derivation of the equation is the book by Thomas. The term zeta coefficient is an expression coined to denote the difference between the magnitude of the zeta potential of a mineral suspended in solution A, and that of the same mineral suspended in solution B, which consists of solution A and an additional chemical agent, but is at the same pH. For example, the difference between the zeta potential of galena particles in distilled water and that in any chemical solution at the same pH is a zeta coefficient. Or, when the zeta potential of a mineral particle is measured first in distilled water, then in a mixture of water and copper sulphate, and finally in a mixture of water, copper sulphate and xan-thate, we can calculate the zeta coefficient

Jan 1, 1947