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Executive Committee, Board of Directors Howard C Pyle, Chairman, J L Gillson, Vice¬Chairman, A W Thornton, Elmer A Jones, Augustus B Kinzel Finance Committee, Board of Directors J S Vanick, Chairman, John P Hammond, J W Woomer Investments Gail F Moulton, '60, Chairman, Andrew Fletcher, '62, John M Lovejoy, '61, C R Dodson, ex off as AIME Treasurer, J S Vanick, ex off as Chairman of Finance Committee Endowment Andrew Fletcher, Chairman, N G Alford, W J Coulter, Harold Decker, J V N Dorr, R B Gilmore, J B Haffner, Kenneth Hill, 0 H Johnson, J D MacKenzie, D H McLaughlin, J R McMillan, W S Morris, L F Reinartz, H DeWitt Smith, Wilfred Sykes, J R Suman, C E Weed Honorary Memberships C E Reistle, Jr, '60, Chairman, Grover J Holt, '61, Augustus B Kmzel, '62, (ex off as Past Presidents of AIME) M L Haider, '60, D H McLaughlin, '61, John M Lovejoy, '62, L F Reinartz, '63, Howard C Pyle, ex off as President of AIME

Jan 1, 1959

By W. V. Kuster

The investigation described in this report is part of a survey by the Federal Bureau of Mines of the titanium resources of the United States. The purpose of this project was to study a typical coastal deposit of beach sands in the Middle Atlantic States, particularly in the area surrounding the Delmarva Peninsula. The field investigation consisted of a reconnaissance survey of the Eastern Shore of Maryland, followed by surface sampling and drilling of the sands on Assateague Island, off the Atlantic coast of Maryland. The study covered the period January-December 1957. Detailed analyses were made of 5-foot sections of eight drill holes along the Maryland section of the island. The heavy-mineral fraction of these samples was separated by sink-float tests, using acetylene bromide as the heavy liquid. The minerals comprising the heavy fraction were examined microscopically, and mineral counts were made on selected samples.

Jan 1, 1959

By A. S. Nowick, W. A. Goering

INspite of considerable interest in the kinetics of ordering of the alloy Cu3Au there is no direct information available on the activation energy for atom movements in this alloy, such as that obtainable by radioactive tracer-diffusion studies or by internal friction measurements. Accordingly, this alloy was examined to find out whether it displays an internal friction peak resulting from stress-induced ordering, similar to that studied extensively in other alloy systems.1-3 Measurements of the internal friction as a function of temperature were made in a torsion pendulum similar to that described by Ké.8 Wire specimens 0.032 in. diam and 11 in. long were used. The wire, obtained in the cold-drawn condition,* was annealed at 900C in a quartz tube to obtain a large grained sample, and then mounted in the torsion pendulum furnace. Internal friction is reported here as the lag angle, 4, which is equal to the logarithmic decrement divided by .ir. Fig. 1 shows the internal friction at three frequencies (the frequency given for each curve is the value measured at the peak). The data for these curves were obtained on cooling one specimen from 460C to just above the critical temperature for long-range ordering, which is about 390C for this alloy. In this way, the internal friction is measured under conditions where the alloy is in the disordered condition throughout the run. The curves obtained at frequencies of 2.15 and 1.29 cps show peaks in the range of measurement. The corresponding peak for the 0.78-cps curve is estimated, from the shift of this curve relative to the others, to be located slightly below the critical temperature (at 385C). The fact that the peak can be observed above the critical temperature is good evidence for the belief that it is a stress-induced ordering phenomenon similar to that which is observed in other disordered alloys. The fact that the peaks in Fig. 1 are not the same

Jan 1, 1959

By A. C. Rice

This report describes a chemical process for preparing solutions of trivalent rare-earth chlorides from sulfate solutions obtained by treating bastnasite concentrate. The chief impurity in the final solution is cerium, and this element is less than 1 percent of the rare-earth oxides. The solution is used directly in the separation of rare-earth elements by ion-exchange methods. The attractive features of the process are that the chemicals are inexpensive and the steps few. The process starts with precipitating the rare-earth hydroxides from sulfate solutions with caustic soda. After the hydroxides are dried to oxidize the cerium, they are treated with dilute hydrochloric acid to dissolve away the trivalent rare-earth elements, leaving the tetravalent cerium. Details for controlling the leaching step are described. The process shortens older procedures by omitting the usual oxalate or double-sulfate-precipitation step.

Jan 1, 1959

By G. C. Fryburg, H. M. Murphy

ThE rates of oxidation of metals are usually obtained by heating the metal specimens in furnaces. Such a procedure is satisfactory for most metals. However, there are several metals that oxidize according to the reaction.

Jan 1, 1959

By R. E. Delavault, H. V. Warren

In normal soils there are usually 10 to 50 parts of copper in every million parts of .soil. Only 0.2 to .5 pct of this copper can be found by any simple cold chemical attack. Now, with rubeanic mid reagent paper, a prospector or field geologist can detect as little us 4 ppm of readily available copper ill soil. This degree, of sensiticity is enough to determine the presence. of copper anamalous an as and, ecentually, to discouer copper mineralization. Circumstances determine whether it is better to make analyses in the field or in a permanent laboratory. The rubeanic acid test described in this article has been designed primarily for field use: it is simple and virtually foolproof, and it requires a minimum of field kit." It is sensitive, easily de- • Ed. Note: Persons Interested in purchasing kits suitable for rubeanic acid prospecting can obtain information by writing Eldrico Geophysical Sales Ltd., 633 Hornby Street. Vancouver 1, B.C. The University of British Columbia does not produce these kits for sale and has no financial interest in their production tecting 4 ppm of readily extractable copper in a soil. This is by no means a quantitative test, but it is accurate enough to provide a valuable indicator of copper anomalous areas for both prospectors and field geologists. The easiest method for detecting metal deposits that do not produce visible float or stains is to make a simple chemical test for the metal in overlying soil, or in the silt of a stream that may have picked up metal farther upstream. In Brief: Testing for copper may be done easily by shaking a soil sample with strong acetic solution in a small test tube and pouring the mud into a small filter, the tip of which rests upon a strip of reagent paper impregnated with rubeanic acid (di-thio-oxamide). When copper is present—and only when it is—a blue spot develops. The more copper, the darker the spot. If the copper content is merely the small amount present everywhere, there is a pale blue or hardly visible spot; if it is abnormally high, the spot will be dark. There are, of course, intermediate cases where the experienced geochemist cannot tell offhand whether a medium-strength spot represents rich agricultural soil, weak copper mineralization, or distant rich copper mineralization. Reagents and material are inexpensive; the test may be readily done on the spot with a simple kit easy to pack and handle. Anyone interested in general problems of soil sampling as applied to prospecting may refer to an article recently presented to the AIME. In exploration work it is the contrast between the metal content of anomalous and background areas that is important; absolute values become of greater interest when an anomalous area is being investigated in detail. With specific reference to copper, it has been the authors' experience that the amounts of metal extracted from anomalous and normal soils with buffer solutions of decreasing pH show better contrast if an acid reagent is used. This contrast tends to increase with increasing acidity until 3 to 4 pH is reached. Using a short cold attack on unheated soil, it has been found that further increases in acidity do not produce better results, and only increase the hazards involved in carrying strong acids. An acidity of about pH 4 is satisfactory for direct determination of copper by dithizone. But dithizone itself introduces some problems: it must be made up fresh at frequent intervals, and with some soils, notably those with much ferric iron, oxidation mag take place before all the copper has reacted with the dithizone. Rubeanic acid keeps its strength unimpaired for long periods, is unaffected by oxidation, and is practically specific for copper at pH 4. Consequently it seems an ideal reagent to use in prospecting for copper. History and Background: Rubeanic acid (systematic name: dithio-oxamide (SC-NH2) has long been known as a spot test reagent for some heavy metals with which it gives a number of compounds. Only copper and some metals of the platinum family are believed capable of providing any ru-beanate compounds under conditions of moderate

Jan 1, 1959

By Clyde N. Garman

The Homestake-New Mexico Partners consist of Homestake Mining Company of Lead, South Dakota; Rio de Ore Uranium Mines, Inc; United Western Minerals Company; White, Weld and Company; J.H. Whitney; San Jacinto Petroleum Corporation; and Clyde Osborn, Homestake Mining Company is the general partner, the others are limited partners. The Rio de Ore Uranium Mines, Inc. has. a mine in the Ambrosia Lake area; this was the first mine to go into production in this area. The United Western Minerals Company also has a mine in the Ambrosia Lake which is operated as a "farm out" from the San Jacinto Petroleum Corporation. These mines are the principal sources of ore for the mill. This group was the first to obtain a contract with AEC to make uranium concentrate from Ambrosia Lake ores and the first to have a mill in operation specifically for these ores. With Clyde Osborn as the sparkplug and co-ordinator holding the ore suppliers of, this group together, a contract with AEC was agreed on as to its essential points by mid-summer, 1956, At that time, there was no general partner and no financing, so me formal contract could be signed. By December, 1956 when the contract was signed and the present partnership officially formed, much of the basic engineering was done and purchasing of main elements of the mill waited on the formalizing of agreements, at the specifications and sizes agreed on previously. Ground for the mill was broken in April, 1957. The sampling plant went into operation in October and ore was first fed to the ball mills on February 5, 1958, ten months after construction actually started. Filling of the circuit with sodium carbonate bicarbonate solution had begun a week before that.

Jan 1, 1959

By V. F. Zackay, W. A. Goering

ALLOYS of iron and aluminum up to 35 wt pct aluminum are single-phase solid solutions, and are of potentially wide applicability.1-3 In spite of early and continued interest1-4 little progress has been made until recently in the preparation and evaluation of sound alloys containing more than 6 wt pct aluminum. Vacuum-melting techniques for the production of ductile Fe-A1 alloys have been described recently.1-7 A. procedure for air melting these alloys is presented here. Low-carbon iron is induction melted without a slag in a rammed magnesia crucible. At the beginning of melt-down, aluminum pig (99.95 pct Al), charged in a clay-graphite bottom-pouring crucible is placed in a pot furnace at 1800°F. The primary deoxidation of the molten iron after melt-down is effected by the addition of 0.1 pct aluminum and 0.5 pct manganese. (Hilty and Crafts" have reported a significant increase in the deoxidation efficiency of the aluminum and manganese combination over that of the aluminum alone.) A more drastic deoxidation designed to reduce the oxyen content to the lowest possible level is accomplished by plunging metallic calcium to the bottom of the melt. This is done by wiring small cubes of the metal to a steel rod. A circular shield larger than the diameter of the crucible opening is attached to the rod so that any spa'ttering of the molten metal will not endanger the operator. Since the temperature of the molten metal is above the boiling point of calcium, the bath is vigclrously purged by calcium vapor. It is believed that the calcium-vapor treatment permits a homogeneous distribution of calcium in the melt. Owing to the vigor of the reaction the temperature of the molten metal should be kept below 2900°F prior to the calcium addition. A total of 0.05 pct calcium is added in two stages in this manner. The second calcium deoxidation is made just before charging the molten aluminum into the iron, in order that an excess of calcium be present for the remainder of the melt. The aluminum, which has been removed from the holding furnace, is then hydrogen degassed by bubbling chlorine through a quartz tube immersed in the molten aluminum. The hydrogen-chlorine reaction is an exothermic one preventing the solidification of the aluminum during the 5-min chlorination. Approximately 0.1 pct calcium, based on the amount of aluminum, is then added to the aluminum. A further excess of calcium is introduced into the melt in this manner. The oxide dross is removed, fluorspar is added to the molten iron, and the molten aluminum is poured through the fluorspar slag. The fluorspar should be dried thoroughly prior to its use, as any water present will react with the aluminum. Aluminum oxide formed during the pouring operation reacts with the fluorspar slag to form gaseous aluminum fluoride and calcium oxide. A forced-draft ventilating system is required for this operation as aluminum fluoride is toxic. As soon as the molten aluminum has been added, vigorous manual stirring of the melt is required because the slag-aluminum oxide reaction is highly exothermic and tends to take place near the top of the melt. The combination of high temperature and the slagging action of the fluorspar quickly erodes the crucible at the slag line if the aluminum is not stirred uniformly into the melt. It has been found that at least 4 min of manual stirring combined with induction stirring are necessary to ensure homogeneity. The power is shut off 1 min prior to pouring to allow metal and slag to separate. As much slag as possible is removed from the melt, which is then poured directly into cast-iron molds. A mold wash of aluminum oxide is used to prevent ingot sticking. For slab ingots which are to be rolled into sheet, a carbon-tetrachloride vapor atmosphere or a chlorinated-pitch mold wash is desirable, as the aluminum oxide formed in the pouring operation is subsequently removed by the chlorine in the presence of carbon." As in vacuum melting, a pouring temperature of about 2900°F is recommended. Adequate hot-topping is important as iron-aluminum ingots are subject to very deep piping. Ingots are removed from the molds and buried in vermiculite, where they are allowed to cool slowly to room temperature. The ingots are radiographed,

Jan 1, 1959

By D. Turnbull, H. N. Treaftis

Precipitation of tin from Pb-Sn alloys (lead-rich) occurs by the nucleation and growth of hemispherical cells which consist of tin lomelloe interspersed in the depleted solid solution. Nucleation and growth of these cells and the tin interlamellar spacing at various compositions and temperatures have been investigated. The interlamellar spacing increases approximately as the reciprocal of the logarithm of the supersaturation ratio. For constant initial tin concentration the concentration of cell nuclei increases with decreasing temperature to a limiting temperature-independent value. The kinetic results support the view that the cell growth rote is governed by the diffusion of tin along the cell boundary. In the main, the results confirm the authors' earlier deductions, drawn from resistometric and calorimetric data, about the precipitation mechonism. IT has been shown1, 2 that tin (ß) precipitates from lead-rich (a) PbSn solutions by the nucleation and growth of cells (cellular or discontinuous precipitation). These cells consist of tin lamellae, with a spacing 1, interspersed in a depleted a solution. Reorientation of a also accompanies cell growth. The kinetics of cellular precipitation of tin from lead have been measured by resistometric2, 3 and ca1orimetric1, 3 techniques. The time-transformation isotherms (t equals time; x, volume fraction of specimen transformed) of the initial rapid precipitation, which drains about 60 pet of the tin from solution, have been described by a kinetic law having the form x = 1 —exp (—bt n) [I] where n usually has the value 3.0. It was shown" that this law and the other kinetic facts can be explained satisfactorily if it is assumed that the cells grow at a constant rate and that all the cells nucleate in a time negligible in comparison with the period of cell growth before impingement. Thus, for hemispherical cells b = (2/3)pNG3 [21 where G is the rate of cell growth in cm per sec, and N is the number of cell nuclei per unit volume. The rapid rate of cell growth at low temperatures can be accounted for"' if it is assumed that the dissolved tin drains to the lamellae edges by diffusion along the sweeping cell boundary rather than by diffusion through the a crystal (volume diffusion). For cell growth governed by cell boundary diffusion it was shown, approximately G=2(X° - X° / X° ) DBA / l2 where A equals the thickness of the cell boundary; D R, the coefficient of diffusion of tin atoms within the boundary; and X° and X, are the atom fractions of tin in the supersaturated and saturated solutions, respectively. Zener8 had already shown that, where

Jan 1, 1959

[Adams, Frank E U.S. Steel Corp., 919 Kearns Bldg., Salt Lake City, Utah Alger, Van Kaiser Steel, Sunnyside, Utah Allan, Andrew Thompson Creek Coal &Coke Corp., Glenwood Springs, Colo. Allen, Earl W Mine Safety Appliances Co., 257 Rio Grand St., Salt Lake City, Utah Allen, Thomas Chief Coal Mine Inspector, Colorado, Argonaut Hotel, Denver 2, Colo. Anderson, Merlynn D U.S. Fuel, P.O. Box 5022, Dragerton, Utah Anderson, Nephi W Book Cliffs Coal Co., Dragerton, Utah Ankeny, Marling J Bureau of Mines, 5308 Roosevelt St., Bethesda, Md. Arentzen, E. M Lee-Norse Co., Charleroi, Pa. Arentzen, L. E Lee-Norse Co., 2975 18th St., Boulder, Colo.]

Jan 1, 1959

By C. F. Cornell, R. C. Emmett, D. A. Dahlstrom

FOR many years the disk-type and cloth-covered drum filters have found widest application in liquid-solids separation, which uses continuous filters. The disk type is less expensive, occupies less floor space per square foot of filtration area, and requires negligible down time for filter media changing. However, because filter cloth is billowed out by the blowback in the cake discharge, it is very short-lived if the scraper blades are set too close. Consequently cake weight is very important in assisting cake discharge, which normally necessitates a minimum cake thickness of 3/8 to ½ in. Also, the vertical position of the disks eliminates the possibility of efficient cake washing for removal of soluble values. The disk-type filter is generally limited, therefore, to applications that require no cake washing and form relatively thick cakes within the normal range of filter cycle times. The conventional cloth-covered drum filter is a more flexible unit, permitting wider variation in the percentage of cycle time devoted to cake formation, dewatering, or washing, as required by the application. Thinner filter cakes can be discharged because a horizontal line across the filter medium at the location of the scraper blade is equidistant from the edge of the blade at all points. The scraper blade therefore may be set a short distance from the filter medium or, where wire winding is not used, a floating scraper can be utilized so that the contour of the cloth can be followed. The drum filter is generally employed when there are difficult filtering slurries with resultant thin cakes or when cake washing to recover soluble values must be practiced. Difficulties sometimes encountered in continuous filter operation can be summarized in the following four categories: 1) Low filtration and/or washing rates due to blinding of the filter medium. 2) Poor cake discharge resulting from sticky cakes, filter medium blinding, or too thin a cake for the particular type of filter. 3) High filter media costs caused by short life and frequent down times for cloth changing. This results from blinding or from abrasion by the scraper blade when cakes are thin. 4) Blowback of filtrate at cake discharge because not enough air passes through the cake to purge the drainage area and filtrate lines during dewatering. To reduce or eliminate blinding tendencies several modifications have been tried, for example, cover-cleaning showers, blowback under the feed slurry, and snap-blow cake discharge. In many cases, however, this simply retards the rate of blinding, since the filter medium is kept clean at its outer surface only by these methods. As blinding usually occurs within or on the back of the medium, the operator is finally forced either to remove the cloth and scrub the medium intensively with a cleaning solution or acid-rinse it on the filter—all resulting in down time, short cloth life, and additional costs.

Jan 1, 1959

By W. S. Hyler, L. W. Berger, R. I. Jaffee

Hydrogen additions of 390 ppm to A-55 titanium and 368 ppm to Ti-8 pet Mn have no deleterious Hydrogenadditionseffect on the unnotched and notched rotating-beam fatigue properties of these materials. 'These amounts of hydrogen, however, are sufficient to cause severe notch-impact thesematerials.embrittlement in A-55 titanium and pronounced loss of tensile ductility in Ti-8 pet Mn. The lack of embrittling effect in fatigue in the latter alloy is consistent with the postulated strain-aging mechanism of hydrogen embrittlement in a-ß alloys. There is a significant strain-agingincrease in the unnotched endurance limit of A-55 titanium with the addition of hydrogen. This increase may be explained as the result of internal heating effects which would dissolve the hydride and cause solid-solution strengthening. TITANIUM and its alloys may be seriously embrittled by relatively small amounts of hydrogen. The form which this embrittlement takes has been shown to vary with alloy type. The a alloys, for example, suffer most strongly from loss of notch-bend impact toughness' when sufficient hydrogen is added, and this effect has generally been associated with the presence of hydride phase in the micro-structure. In a-ß alloys, on the other hand, hydrogen is most detrimental to tensile ductility in slow-speed tests,2-1 and the embrittlement may be detected in a most convincing manner by means of rupture tests at room temperature. This particular kind of embrittlement has not been associated with a change in microstructure, but has been classified rather generally as associated with a strain-aging type of mechanism.' In the present paper, the effect of an embrittling amount of hydrogen on the rotating-beam fatigue properties of both an a and an a-ß titanium alloy is covered. For this study, annealed commercially pure (A-55) titanium was chosen as an a alloy, and equilibrated and stabilized Ti-8 pet Mn as representative of a typical a-ß alloy. Nominal hydrogen levels of 20 and 400 ppm were evaluated, the latter amount having been shown previously to be severely detrimental to the impact toughness of commercially pure titanium and to cause pronounced strain-aging embrittlement in the Ti-8 pet Mn alloy. The only report of the effect of hydrogen on the fatigue properties of titanium is given by Anderson et al.,° in which a push-pull type of fatigue test was conducted on as-received commercial-purity titanium sheet. Much scatter was found in the results, but generally the presence of hydrides slightly decreased the fatigue strength of unnotched specimens in the longitudinal direction. The results of notched tests were masked too greatly by scatter to be significant. Experimental Procedure Preparation of Materials—Analyses of the A-55 titanium and the Ti-8 pet Mn alloy used in this investigation are given in Table I, which indicates the 8 pet Mn alloy to be more nearly a 6 pet Mn alloy. This alloy will be referred to as Ti-8 pet Mn, however, since this is the commercially designated composition. Both alloys were received in the form of5/8-in. diam rod and, after suitable surface preparation, 5-in. lengths were vacuum annealed at 820°C. Half of the rods for each material were then hydrogenated at 820°C to a nominal hydrogen content of 400 ppm. The hydrogenated and vacuum-annealed A-55 rods were hot swaged at 700°C from 5/8-in. diam to 1/4-in. diam, and then annealed 1 hr at 800°C and air cooled prior to preparation into test specimens. Fabrication of the Ti-8 pet Mn alloy was by hot swaging to 3/8-in. diam at 760" and then 1/4-in. diam at 704°C. This material was then annealed 1 hr at 704", followed by furnace cooling to 593"C, and finally air cooling to room temperature. Evaluation—In order to examine more completely the effects of hydrogen on the particular materials studied, slow-speed tensile and notch-bend impact properties were determined in addition to fatigue data. Tensile specimens were of the standard ASTM type with a reduced section of 1/8-in. diam and a gage length of 1/2 in. A subsize cylindrical Izod specimen was used for impact tests. These specimens had a 45" notch with a 0.005-in. radius and a 0.150-in. root diam, and the stress concentration factor of this notch in bending was Kr = 3. Both the ten-

Jan 1, 1959

By Elliot Gillerman

The title of this paper implies the presence of silver, nickel, and cobalt minerals at, the Alhambra mine. Perhaps this should be amplified to include uranium, as pitchblende also occurs, possibly in mineable quantifies. A brief history of the Alhambra mine is of interest, both from a historical angle and as pointing up the importance of geology in the-present development. The Alhambra is one of several mines in the Bullards Peak or Black Hawk dis¬trict, ass it is more familiarly known, in southwestern. New Mexico, which was mined for silver in the 1880?s and 18901s, Silver valued between $500,000 and $1,000,000 was extracted from the mine in the 10 years prior to 1893, when operations ceased. Almost all the silver mined was native silver, although a small quantity of argentite was produced. Nickel and cobalt were recognized in the ores, but they were thought to be of no consequence.

Jan 1, 1959

By Richard H. Mote, W. C. Schroeder

The endlessly changing pattern of mineral supply and demand offers opportunity to the alert and can bring disaster to the unwary. The discovery of ore bodies, the invention of extractive processes, the provision of new transport facilities, the political stabilization of underdeveloped areas, and many other changes can increase supply dramatically. Such new outpourings of mineral wealth from ore bodies bring fortunes to their developers, and consumers frequently find their competitive positions decidedly improved by new and cheap sources of supply. On the other hand, operators of marginal properties can find competition from newly opened high-grade mines intolerable. Consumers that have depended on the products of nearby, high-cost mines may find new, remote, low-cost supplies advantageous only to their competitors. The invention of new prospecting methods can have spectacular effects. Shortly after World War I the discovery rate of petroleum pools began to decline. The leading prospecting technique of that day, the projection downward of surface reflections of geologic structure, was proving less rewarding. Prophets foretold an oil shortage in the near future. But at that very moment scientists were perfecting the application of seismic waves to reveal underground oil-bearing geologic structures. As these geophysical methods were put into commercial use the whole outlook changed-the problem of the 1930's became how to cope with the surplus from discovery, not how to meet the ever rising demand. Many lead mines were being abandoned as unprofitable about this same time because the penalties charged by smelters for the zinc in the ores and concentrates more than counterbalanced the payments for lead and silver. Then selective flotation (at the time called differential flotation) appeared,

Jan 1, 1959

By Robert L. Montgomery

Heats of solution of samarium (III) oxide and chloride in hydrochloric acid and of samarium (III) oxide, sulfate, and hydrated sulfate in sulfuric acid were measured. The heats of solution of this hygroscopic oxide are larger than those from the literature, probably because of more complete removal of water in the present study. From the literature value for the heat of combustion of samarium, the heats of formation of samarium (III) chloride and sulfate are -244.18 ± 0.41 and -928.5 ± 1.6 kcal./mole, respectively. The heat of hydration of the sulfate is -34.7 ± 1.0 kcal./mole. The heats of formation of other samarium com-pounds have been recalculated, using the new data.

Jan 1, 1959

By L. C. Weiner

For zinc single crystals, xo = 3o, a surface coating raises both the cleavage and yield strengths over a large temperature range. The "brittle temperature," associated with slip after completion of twinning, does not coincide with the point of intersection of the flow and cleavage curves, which is associated with twinning. A surface film has no effect on the brittle temperature, while it lowers the intersection temperature some 20°. For crystals, yn = 83o, a coating decreases the cleavage strength, making it temperature independent, as well as increases the brittle temperature or its equivalent, the intersection temperature, 20°. These observations are described on the basis of a dislocation-pile-up-at-a-barrier model for brittle fracture; in crystals x,, = 3o the number and distribution of twins play a vital role. IN a recent investigation on the effects of solid environments on the brittle fracture of zinc single crystals,' it was demonstrated that the presence of a surface film changes the cleavage strength of these crystals, either increasing or decreasing it, depending on the crystal orientation. An increase in cleavage strength of some 43 per cent was found for coated crystals oriented x, — 3o K = 28",* while a decrease of 48 per cent was observed with crystals X" = y» — 83". Moreover, these effects were found

Jan 1, 1959

By J. H. Wernick, J. E. Kunzler

HIGHLY pure metals are needed for low-temperature electron transport studies in progress. Recent improvements in purification techniques, such as zone refining, have made it possible to obtain metals with improved purity. For some metals, the improvement has been to the extent that ordinary analytical techniques are inadequate and special methods are needed.1 For other metals purification is more difficult, so that simple but rapid analytical methods are desirable as an aid in evaluating the effectiveness of purification procedures. Furthermore, it is desirable to be able to determine the impurity level of the sample or ingot with the minimum of physical disturbance of the material. In order to aid in the preparation of purer metals, techniques involving the measurement of electrical resistance at liquid-helium temperatures have been devised for studying impurity distributions in zone-refined ingots and other bulk samples without destroying the ingot or its geometry. The method yields information on the variations in purity along the length of the ingot or sample and provides a measure of the overall purity of the material. Compared with ordinary analytical methods, the resistivity method is rapid, sensitive, and does not require significant physical disturbance of samples with reasonable shapes. It has the disadvantage that resistance measurements are not specific, i.e., they do not identify the impurity. However, this disadvantage is offset by the advantage of being able to establish a measure of the overall purity so far as electrically active" impurities are concerned. METHOD AND ITS BASIS The method is based on the well-known fact that the resistivity, at Liquid helium temperatures, of a reasonably pure metal containing no regions with additional phases decreases with increasing chemical purity or a decrease in the number of physical defects. It is convenient to separate the total resistivity into three parts: where is the resistivity due to the scattering of the conduction electrons by the lattice vibrations or phonons, p is the contribution due to physical defects, and originates from the effect of chemical impurities in the metal. Insofar as Matthiessen's rule is obeyed,2 pphys and pchem are independent of temperature. Except possiblyin the very purest metals, ptherm is negligible at liquid helium temperatures and For zone-refined metals, which normally are well annealed and consist of large grains, at the chemical purity levels thus far attained the available data indicate that pphys is negligibly small or at least constant throughout the ingot. Assuming that the effect of physical defects is negligible for isotropic metals, This assumption appears consistent with most of

Jan 1, 1959

By Joseph A. DeCarlo

THE TOTAL VALUE of sales of coal-chemical materials in the 10-year period 1948-57 increased 34 percent or at an average annual rate of approximately 3.5 percent. According to the Chemical Industry Facts Book, third edition, 1957, published by Manufacturing Chemists' Association, Inc., the production of industrial chemicals since 1939 "has grown at au average rate of about 10 percent" a year (p. 7). The rapid growth of the chemical industry increased requirements of chemical raw materials at a faster pace than could be supplied by coal carboniza¬tion, and view sources of supply became necessary. The petroleum industry in the past decade increased tremendously the flow of chemical raw materials to the chemical industry through the processing of crude petroleum and natural gas. Whereas coal carbonization supplied most of the raw materials for manufacturing synthetic organic chemicals before World War 11, coke ovens supplied only about 40 percent of the total used in 1957. Although the proportion of chemical raw materials supplied to the chemical industry by coke-oven operators declined, this source of supply is large and important to our economy. In 1957, the value of coal-chemical materials sold, including surplus gas used by producing companies, totaled $358 million, compared with $267 million in 1948. Major factors that contributed to this gain were (1) increased production of all coal chemicals and (2) higher prices for tax and light-oil products. Gains in output of coal chemicals resulted principally from expansion in carbonizing capacity of coke plants owned and operated by the iron and steel industry, as yields of the basic coal¬-chemical materials (tar, ammonia, light oil, and gas) varied only slightly during the 10 years under review.

Jan 1, 1959

By S. A. Spachner

An analysis of the powder patterns of the omega transition phase in three binary titanium alloys containing 8 pct Cr, 13 pet Mo, and 15 pet V, respectively, showed that all could be indexed on an orthorhombic unit cell. The unit-cell dimensions were all quite similar. There is evidence for the occurrence of more than one transition phase in Ti-Cr and Ti-V alloys. FOLLOWING the discovery of a new brittle phase in certain titanium-chromium alloys by Frost, Parris, Hirsch, Doig, and Schwartz,' named ? by these investigators, much interest has developed concerning the identification of alloy systems in which this phase exists, kinetics of the transformation in such systems, and the crystal structure of the ? phases appearing. Omega has been found in alloys of titanium-manganese, titanium-molybdenum, titanium-iron,' and titanium-vanadium.' In the present work, a study was made of the powder patterns of the ? phase occurring in alloys of Ti-8Cr, Ti-13Mo and Ti-15V in an effort to obtain a basis of comparison for ? phases appearing in these different alloys. Comparison of Alloys for ?-Phases Two hundred mesh powders of Ti-8Cr, Ti-13Mo and Ti-15V were prepared. A portion of powder sufficient for three x-ray powder specimens was placed in a Vycor tube, evacuated to less than 0.1 µ pressure, filled with argon, and sealed. The tubes were then heated to 900°C, held at this temperature for 30 min, and water-quenched. Following this transformation to the ß phase, the specimens were quenched in lead or solder pots, held at the desired temperature for varying lengths of time and water-quenched. The heat-treatments used and the phases identified are listed in Table I. The intermediate water quench was used in lieu of direct downquenching from 900°C to the bath temperature desired to circumvent the possibility of transformation of the powder specimen from ß to (ß + a) while it was being moved from the homog-enization furnace to the lead bath. To check the possibility that upquenching to the bath temperature might bring into play a different mechanism than downquenching to this temperature, resistivity measurements were compared on Ti-8Cr rod specimens which were transformed isothermally at 400°C by downquenching from the solution-treatment temperature and those which were transformed at 400" C by upquenching ß specimens from room temperature. The results are shown in Fig. 1. No difference in transformation mechanism was noted. It soon became apparent that sufficiently detailed Debye-Scherrer photograms of the ? phase in the alloys which were to be used could not be obtained by the use of copper radiation. Although satisfactory photograms of ß and ß + a phases were obtained with this radiation, the ? phase appeared to exhibit mild fluorescence, making interplanar spacing computation virtually impossible. Molybdenum radiation appeared to offer promise in cutting down this fluorescent effect, the mass absorption of titanium for molybdenum radiation being 23.7 in contrast to 204 for copper radiation. The reduction in the accuracy in determining the location of the photo-gram lines caused by the shorter wave length of molybdenum characteristic radiation did not appear to be a significant factor. Utilizing a camera of 57.3 mm radius, best results were obtained for exposure times ranging between 30 and 40 hr. Tube potential

Jan 1, 1959

By L. O. Brockway, W. C. Bigelow, J. A. Amy

Specimens of Inconel-X alloy solution-treated at 2050°F and aged for periods of 1, 10, 100, and 1000 hr at 1200°, 1400°, and 1600°F have been examined by electron microscopy and by electron and X-ray diffraction. Four minor phases were identified: titanium nitride, niobium nitride, an M23C6 complex carbide, and the intermetallic ? phase. The two nitrides were found in all of the aged specimens and in the solution-treated alloy, the y' phase formed at all aging temperatures, while the M23C6 carbide formed only on aging at 1200° and 1400°F. Variations in the hardness, rupture strength, creep strength, and yield strength of the alloy have been shown to be related to variation in the size and distribution of the particles of the y' phase within the matrix grains of the alloy, with maximum values of these properties occurring when there is a maximum amount of the phase present and a fine state of dispersion of the particles prevails. THE nickel-chromium alloys containing titanium and aluminum are widely used in applications requiring high strength at elevated temperatures. Studies on relatively simple ternary and quaternary alloys'-4 have indicated that the favorable high-temperature properties of these alloys are related to the precipitation of an intermetallic ?'-phase having a structure based On that of the Ni3A1 phase of the nickel-aluminum system. The present investigation was undertaken to identify the minor phases and to study the microstructural changes occurring in one of the more complex commercial alloys as a result of aging in the service temperature range, with particular emphasis on investigating the role of the ?' -phase. The microstructural changes were studied by electron microscopy and the minor phases were identified by X-ray and electron diffraction. MATERIALS AND METHODS Inconel-X alloy was selected for this investigation because the previous studies of Frey, Freeman, and white6 provided extensive information on the variations in metallurgical properties of this alloy resulting from high-temperature aging treatments. Specimens aged 1, 10, 100, and 1000 hr at 1200°, 1400°, and 1600°F were made available for the present use. These were taken from 1-in. round-bar stock of a commercial heat having the following weight composition: 0.04 C, 0.56 Mn, 6.59 Fe, 0.007 S, 0.38 Si, 0.03 Cu, 73.22 Ni, 14.97 Cr, 0.78 Al, 2.38 Ti, and 1-02 Nb. They were solutjon-treated at 2050 for 4 hr and then water-quenched prior to aging. Powder X-ray diffraction patterns were obtained from insoluble minor phases which were separated from the alloys by digestion in the reagent of Mahla and Nielsen.6 Back-reflection patterns were obtained from electrolytically polished surfaces of the bulk search to detect the ?'-phase' Cu-K a radiation was used in both cases. In the electron-diffraction studies, the general method developed by Heidenreich, Sturkey, and

Jan 1, 1959