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By J. E. Elliott, K. O. Miller

Solubility studies were carried out to establish the phase distributions for various Fe-Ni-Pb-C alloys at temperatures where the metallic components exist as liquid solutions. Temperature us composition diagrams for the Ni-Pb, Fe-Pb, Fe-Ni-Pb, and Ni-Pb-C systems are derived by employing various approximations in conjunction with the data. Results are summarized for 1550°C in a quaternary phase diagram of the Fe-Ni-Pb-C system. BECAUSE surprisingly little information has been published on the phase diagrams of the Ni-Pb, Fe-Pb, Fe-Pb-Ni, and Fe-Ni-Pb-C systems, a study of these systems was undertaken to ascertain the important phase relationships in the temperature range of 1300" to 1550°C. Measurements were also made on the carbon-saturated systems in the hope that they would assist in the interpretation of the systems without carbon. This paper reports the results obtained from the simple equilibration of the various liquid and solid phases. EXPERIMENTAL PROCEDURE The experimental technique involved holding appropriati quantities of the metals in an alumina crucible, or in a graphite crucible when saturation of the melt with carbon was desired, for sufficient time at the desired temperature to ensure equilibrium. Then a sample of each liquid phase presen was drawn into a small-bore silica tube. This sample was withdrawn quickly from the furnace, cooled, and sent to the chemical laboratory for analysis. The cell assembly used is shown in Fig. 1. Durin the work on the Fe-Pb-Ni system, it was placed in a furnace wound with 20 pct Rh-80 pct Pt wire. This furnace eventually failed and subsequent studies were carried out between 1350" and 1475°C in a tube furnace heated by silicon-carbide resistance elements. A protective atmosphere of argon with approximately 10 pct hydrogen was supplied to the cell assembly at a gage pressure of 1 in. of water. Hydrogen was passed over palladized alumina and then anhydrous calcium chloride for purification. Argon was purified of oxygen and water vapor by passing it over copper gauze at 550°C and then through a calcium chloride drying column. The gases were mixed and redried before they entered the equilibration cell. Temperature was measured by calibrated Pt/Pt-10 pct Rh thermocouples and a Rubicon Type B potentiometer. The thermocouples were standardized against the melting points of pure nickel

Jan 1, 1961

By D. H. Shaffer, W. F. Harris, W. M. Hickam, M. H. Loeffler

Experiments have been performed on the quantitative addition to niobium of enriched isotopes 018 and 017 at the 0.1 - 40 micro-gram level and their subsequent recovery. A measured quantity of molecular oxygen of known isotopic concentration is added to niobium metal by oxidation. Recovery of the enriched isotopes as carbon monoxide is by the vacuum fusion technique. Quantitative determinations of the enriched isotopes are made in standard volumes at constant temperature using accurately calibrated micromanometers and the mass spectrometer as pressure measuring instruments. THE presence of low concentrations of nonmetallic impurities in metals can often adversely affect the physical properties of the metal. The increase in hardness and the embrittlement of refractory metals due to oxygen is well known. In metallurgical studies dealing with the diffusion rates or the effect of oxygen on the physical properties of refractory metals, it is often necessary to add small quantities of oxygen to the metal and later recover the total quantity present. It is desirable, therefore, to establish the accuracy with which microgram quantities of oxygen can be added to niobium and recovered by vacuum fusion. The successful addition of microgram quantities of oxygen to metals by the usual manometric techniques and the subsequent recovery by vacuum fusion is difficult because of the uncertainty in the accurate determination of the quantity of oxygen originally present in the metal and because of the chance of contamination by atmospheric oxygen. In order to minimize these uncertainties earlier workers have added quantities of O16 at levels much higher than the oxygen concentrations that are of interest.'-3 In order to eliminate the uncertainty associated with the O16 additions to metals at low microgram levels, experiments have been performed on the quantitative addition of oxygen highly enriched in O17 and O18 at the 0.1 to 40 pg level to niobium and the subsequent quantitative recovery of the isotopes by vacuum fusion. Since the natural abundance of O17 is 0.04 pct and of 0" is 0.2 pct this enriched oxygen provides a uniqueness from interference not achieved in earlier work.'-= A measured quantity of molecular oxygen of known isotopic concentration is diffused into the metal. Recovery of the isotopes in the form of carbon monoxide is by vacuum fusion. The total quantity of gas is determined in standard volumes at constant tempera- ture using accurately calibrated Consolidated Electrodynamics micromanometers and the mass spectrometer for pressure measurements. The molecular and isotopic composition is determined mass spectrometrically. APPARATUS A schematic of the oxygen addition apparatus is shown in Fig. 1. Take-offs are provided for the attachment of the isotope container and for sample bulbs which are used to transfer samples to the mass spectrometer. Metal valves are used throughout the system including the sample bulbs in order to achieve a vacuum of 10"6 mm Hg. Evacuation is accomplished with a 3-stage oil-diffusion pump backed by a mechanical pump. A liquid nitrogen trap is used to remove condensables and to prevent oil vapor from entering the system. A micromano-meter is used for pressure measurements. The furnace assembly is shown in Fig. 2. It consists of a quartz tube joined to the apparatus through a 40/W joint with Apiezon W low-pressure wax. The furnace cap, also a 40/W pyrex joint, is provided with a pyrex hook. The sample is suspended from this hook with a platinum wire. The total volume of the furnace section is 435 ml. All volumes were determined by expanding a known volume of gas at a known pressure into the evacuated system and re-measuring the pressure. Both the micromanometer used on the oxygen addition system and the micromanometer used on the mass spectrometer were compared to a precision

Jan 1, 1961

By A. Alonso, J. Daubenspeck

In the nickel extraction process at Nicaro, Cuba, dried and ground nickel bearing laterites are reduced at 1300-1400F in multiple-hearth furnaces. Nickel is leached from the reduced ore by aeration in an aqueous solution of ammonium carbonate. Nickel carbonate is precipitated from the liquor and calcined to yield nickel oxide. The following are the more important modifications of the Nicaro process since plant rehabilitation and expansion. Ten percent increase in tonnage was achieved without decreasing the fineness of the ore by minor mechanical modifications of the grinding plant. Another five percent increase in tonnage was attained by intentionally overloading the ore prepration and leaching circuits in an effort to control cobalt extraction. Modifications at the sintering plant allowed it to handle the entire output of the expanded plant. A fifty percent increase in leach liquor cooling facilities alone provided an increase in nickel production of five percent. Stronger fresh leach liquor for increased nickel washing efficiency was obtained through improved distribution of water to the ammonia absorption towers. Advantage was taken of the reduced calcine's capability to precipitate cobalt, and modifications in the leach liquor circulation provided controlled cobalt solubility with minimum harm to nickel extraction. Several process changes at the drying plant brought about a ten percent reduction in the fuel oil consumption at this pint. Controlled air addition to the reduction furnaces' upper hearths burned formerly wasted combustibles thereby reducing oil consumption by twenty percent. The nickel extraction process successfully emplayed on the extensive but lowgrade lateritic ores of Eastern Cuba at the U. S. Government owned Nicaro plant, has been previously described in various publications. The large mine and plant operated by the Nickel Processing Corporation, located on the northeastern shore of Oriente Province, have been recently expanded to a yearly capacity of about 50 million pounds of nickel. Essentially, the operation involves open pit mining of a limonite-serpentine ore mixture containing 1.3 to 1.4 percent nickel and 34 to 38 percent iron. The comparatively lumpy, wet (25 to 30 percent moisture) ore is first dried and ground prior to chemical treatment, to which the entire 7,000 tons per day feed must be subjected. In the initial chemical action the dried and ground ore is reduced with carbon manoxide and hydrogen at 1300-1400° in multiple-hearth furnaces. The resulting metallic nickel is selectively leached from the reduced calcine by aeration in an

Jan 1, 1961

By S. H. Ward

Since the advent of the first airborne electromagnetic system, it has been evident that such systems were inherently limited to shallow depths of exploration of the orderof 100 to 200 feet. Hence in 1948 the author and his associates commenced a study of the feasibility of applying natural audio frequency magnetic fields to investigation of the electrical properties of the subsurface in order to provide a system capable of overcoming this limitation. This research culminated, in the summer of 1958, in the development of a new airborne prospecting device — AFMAG. This device has detected surface massive sulphide bodies while flown at heights as great as 3000 feet. Hence, by inference, it is deduced that it could find similar sulphide bodies if they were buried 2500 feet below surface and the aircraft flown at 500 feet. Thus a considerable improvement over conventional airborne electro-magnetic systems is obtainable with AFMAG. Airborne exploration in mountainous terrain involving deep valley fill now becomes possible. Examples are presented of the results of actual airborne AFMAG test surveys over known deposits of massive sulphide mineralization. Interpretation of the data is discussed with particular reference to the knowledge of size, dip, depth, depth extent, and conductivity of causative bodies as deduced from the flight records. The possibility of mapping major geologic structures, for both mining and oil exploration purposes, is discussed with the aid of examples of airborne AFMAG data. INTRODUCTION Electrical prospecting with natural audio frequency electromagnetic waves as a source has, within the last three years, become a practical reality. Both airborne and ground survey instruments under the trademark "AFMAG" (for audio frequency magnetics) have been used successfully in the search for conductive mineral deposits. It is the object of this paper to discuss the principles of airborne AFMAG and to illustrate its application by means of examples obtained over known geological situations. WHY AFMAG? In view of the large number of good airborne electromagnetic systems available for purchase or contract surveying, one may well ask, "Why another new system?". Primarily the answer lies in the fact that AFMAG does not suffer from the very limited depth of exploration available with, and inherent in, any conventional airborne electromagnetic system. AFMAG is not conventional insofar as an artificial transmitter is not required. Only a receiving and detecting device is employed. The electromagnetic fields measured are those from millions of electrical discharges in the atmosphere (e.g;..- lightning strokes). Their random distribution in time and space make these fields difficult to employ and it is only with recent advances in the electronics of geophysical instrumentation that this has become possible. A second reason for AFMAG and one of its

Jan 1, 1961

By W. T. Swensen

The Anaconda Company, through its wholly owned subsidiary The Anaconda Company (Canada) I,td., has investigated, optioned and partially developed a large tonnage of iron ore amenable to magnetic concentration. The reserves are located in north central Ontario and occur within a twenty-two mile belt of layered and intricately folded metamorphic rocks, close to the north contact of an igneous complex of granite and pegmatite. There are two main ore deposits. Briarcliffe is a steep to vertically dipping body 100 to 500 feet wide and over a mile long. The Two Mile Lake deposit is flat dipping and confined to an open, asymmetrical syncline; it is approximately a mile wide and 250 to 4.00 feet thick. On its flat easterly plunge, it is saucer-like in shape and is amenable to open-pitting for an east-west distance of several thousand feet. Magnetometer surveys, confirmed by drilling, indicate at least a three mile eastward extension of this deposit. Location and Access: The property is located in the Kowkash Mining District of northwestern Ontario, roughly forty-four miles north of the community of Nakina on the main line of the Canadian National Railroad. (Fig. 1) Access during the exploration period was entirely by airplane from Nakina. (Fig. 2) More recently, Nakina itself was connected to the highway network in the Longlac-Geraldton area. The property is roughly 190 miles by existing and proposed railroad from the Great Lakes waterway system. The Trans-Canada pipeline moving natural gas from western to eastern Canada passes through Geraldton roughly 70 miles south of the property. Topography: The surface features in the area are typical of a sizeable portion of the Precambrian Canadian Shield area. Many lakes, low swampy areas, and glacial moraine-type features are common in this recently glaciated area. The average elevation is between 800 and 900 feet above sea level, and the relief is probably less than 100 feet with the greater portion of the area less than 50 feet. The topographic "highs" are formed either by outcrops that were resistant to glacial erosion or by moraines, eskers and drumlins which were deposited upon the recession of the glaciers. The better mineralized zones, composed chiefly of quartz and magnetite, commonly form ridges resistant to erosion and weathering. Previous Work: Because of the obvious outcrop of the magnetite-rich beds and knowledge gained from early developments within the general region, it is conceivable that the presence of the iron formations has been known for a good many years. The area is included in studies made by L. F. Kindle* in 1929 and 1930 for the Ontario Department *Kindle, L.F., Kowkash-Ogoki Gold Area, Ontario Department of Mines Annual Report, Vol. XL, Part IV, 1931; map 40f

Jan 1, 1961

By J. L. Gillson

Joseph H. Birman (Chairman, Dept. of Geolcgy, Occidental College, Los Angeles, Calif.) Many thanks to J. L. Gillson for so comprehensive a survey of the titanium sand deposits of the world. Over the past two years, the writer studied rather carefully some of the Cretaceous ilmenite deposits in New Mexico and Colorado, including the Sanostee deposit shown in Gillson' s map, Fig. 6. The deposits were geologically mapped and sampled, surveyed by magnetometer, and the Sanostee deposit was drilled. Moat of the genetic interpretations made by Gillson concerning the recent sedimentary ilmenites can be clearly read in the Cre-taceous deposits in New Mexico. The deposits are in marine regressive members of the Mesaverde group. The deposits trend within a few degrees of N 55° W and persistence of this trend through both distance and time (the deposits are in different members of the Mesaverde group) implies that the deposits are offshore bar accumulations. Heavy mineral content ranges from about 10 pct to more than 50 pet. Thicknesses are from 4 ft to as much as 20 ft, widths range from 150 to 600 ft, and lengths range from a few thousand feet to a few miles. All are locally or completely overlain by carbonaceous shale and thin coal. The deposits are strongly altered, and from X-ray diffraction the principal titanium alteration product appears to be anatase. Drilling of the Sanostee deposit shows that the alteration is not related to the present erosion surface but took place at the site of deposition and before burial by the overlying sediments. Iron oxide derived from the alteration cements the grains and is the chief coloring agent in the immediately overlying shales. In the Sanostee deposit, there is virtually no feldspar, the gangue mineral being almost exclusively quartz. Sorting is excellent, but the quartz grains are subangular to angular. Petrographic examination reveals that the angularity is not due to overgrowths. Therefore, short distance transport is implied. The mineralogical composition suggests a low relief granitic terrane as the source area. Feldspar may have been decomposed by weathering at the source, but an alternative preferred by the writer is that each of the deposits represents a long-term concentration site (for example a large sand bar) which was continually being deprived of light minerals by wave action and selective transport. Feldspar may have been mechanically reduced in size more quickly than the quartz, and thus its rate of removal may have exceeded that of quartz. Concentration of heavy minerals would thus occur until the marine regression removed the zone of maximum wave energy from the site. Chemical alteration would then become the most important process until burial by encroaching swamp deposits.

Jan 1, 1961

[James C. Gray, President W. B. Stephenson, President-Elect A. B. Cummins, Past-President E. G. Fox, Eastern Regional Vice-President H. C. Weed, Western Regional Vice-President Donald W. Scott, Central Regional Vice-President John Cameron Fox, Secretary 29 W. 39 Street New York 18, N. Y. After September 7, 1961 345 East 47 Street, New York 17, N. Y. D. R. Tone, Assistant Secretary Nathaniel Arbiter, Treasurer]

Jan 1, 1961

By W. L. Phillips

The plastic properties of lithium fluoride and magnesium oxide under compression were investigated in the temperature range 25° to 1000°C. At the higher test temperatures, the critical resolved shear stress and the rate of work-hardening of both materials decreased. At the same time, the number of stress lines decreased and the individual stress lines became wider. The density of dislocations decreased for a given strain the higher the test temperature for lithium fluoride. The decrease in the critical resolved shear stress as a function of temperature could be fitted by the equation 7 = Toe-KT. THE influence of temperature on the stress-strain curves of a variety of metal single crystals has been studied for a wide range of temperature.1"5 In general, it has been found that both the critical resolved shear stress and the rate of work-hardening decrease rapidly with increasing temperature and fall to a value of essentially zero well before the melting point is reached. AS the test temperature is increased, the density of slip lines has been found to decrease, while the width of the individual lines increases. Recently, Gallagher,' Graf et al.,7 and Pate1 and Alexander8 have found that single crystals of germanium and silicon, which have a covalent bond, can be plastically deformed at elevated temperatures. In compressing germanium it has been found that the strain-hardening coefficient decreased very rapidly as the temperature was increased. The coefficient did not tend to zero, however, as the melting point was approached. The plastic properties of ionic crystals at elevated temperatures have not been extensively investigated. In the only work previously reported Tamman and salge9 and Theile10 have shown that the yield point of sodium chloride single crystals tested in tension and compression decreased slowly with increasing temperature, falling to zero at the melting point. As the temperature was increased, they found a substantial increase in the amount of plastic deformation that could be sustained before fracture; and at temperatures above 400°C in tension tests there was an obvious necking which produced local extensions of up to 3000 pct. The purpose of the present work is to extend the knowledge of high-temperature deformation to the ionic crystals, lithium fluoride and magnesium oxide. The following were investigated: 1) The gross shape of the stress-strain curve at several temperatures. 2) The change in the critical resolved shear stress as a function of temperature. 3) The appearance of slip bands and the density of dislocations as a function of strain and temperature. EXPERIMENTAL TECHNIQUES The lithium fluoride and magnesium oxide used in this investigation were purchased from the Harshaw

Jan 1, 1961

By W. E. Dunn

CHLORINATION of titanium ores and slags is the source of TiCl,4 intermediate between ore and metal. A number of chlorinators are operating in the United States using a wide diversity of ores. These chlorinators vary in design to accommodate the ore source, but all use chlorine and carbon.

Jan 1, 1961

By D. P. Seraphim

Single crystals of bee Li-Mg solid solution were grown and their internal friction was measured as a function of temperature, A peak of the Zener type was found in the damping spectrum. The activation energy for the relaxation process is 21.5 ± 1 kcal per mole and the frequency factor is 1015.7 ± 0.7 sec-1. ZENER internal-friction peaks which are observed for a wide range of solid solutions are attributed to stress-induced changes in local order.' In the present work a Zener internal-friction peak, the first reported for a solid solution of an alkali metal, is

Jan 1, 1961

By H. H. Klepfer, M. E. Snyder

UNTIL very recently, the commercial availability of the rare earths as metals has been very limited. Fabrication of mill products from these metals has not been studied in most cases. This note reports the results of the development of fabrication techniques for thulium. Thulium has a melting point of about 1550°C and a hexagonal close-packed crystal structure. It oxidizes in air to give a black oxide (TmzO,). The procedures for producing thin thulium foil were developed on one ingot weighing about 220 g and were subsequently applied in processing about a pound of metal to foil. Several alternates for the various fabrication steps were investigated and will be discussed. The metal fabricated was in the form of commercial chill-cast ingots 1 in. in diam and 2 in. long weighing approximately 220 g. Impurities in the ingots were reported by the vendor to be 4000 ppni tantalum, 2000 ppm calcium, 200 ppm nickel, 100 to 200 ppm iron, 100 ppm europium, and less than 100 ppm copper, lutetium, and ytterbium. In addition to these impurities, several salt-like inclusions as large as l/8 in. in diam were revealed along the center line of the one ingot sectioned. Preliminary tests indicated that small wafers cut from the as-cast ingot would not fabricate readily by rolling. Forging of copper-jacketed wafers was therefore attempted. At 1550"F forging was satisfactory but an apparent reaction of copper with thulium demanded investigation of lower temperatures. Therefore, the remainder of the test ingot was forged at 1450°F—with only minor cracking. All ingots forged were inserted into copper tubes of 1 in. 1D and 0.125-in. wall thickness. The jackets were sealed by flattening the ends of the tubes and welding under helium. Heating time at 1450°F was 30 min. Press forgings of 1/8 in. per pass were used, followed by 10 min reheats. When the ingots had been squared and reduced to 0.250 in. in thickness, the original copper jacket was stripped off and replaced by a new jacket in preparation for hot rolling. Hot rolling at 1450" F without edge cracking was readily accomplished after forging. Excellent results were obtained with 10 pct reductions of thickness followed by 5 to 10 min reheats. After reduction of thickness from 0.250 to 0.100 in. the copper jacket was removed. It was found, in fact, that hot rolling in air was possible. A tenacious black oxide similar to that seen on zirconium was formed during 3 min reheats at 1450°F. Reduction in air to 0.010 in. foil was possible taking 10 pct reductions per pass. The oxide coat formed during hot rolling in air could best be removed by sand blasting and pickling. Common pickling solutions containing polar solvents were found to attack the metal too rapidly and a concentrated nitric-hydrofluoric acid mixture attacked neither the oxide nor the metal. The most satisfactory pickling solution was 52 vol pct concentrated nitric acid-48 vol pct glacial acetic acid. After forging to 0.250 in., vacuum annealing and cold rolling was found to be another satisfactory alternate to hot rolling in copper jackets. After forging. a hardness of Rockwell B76 was found. Annealing in vacuum (2 X l0-5 mm of Hg) for 1 hr at 1200"F did not alter this value. Annealing at 1470"F for 1 hr brought the hardness down to R;]63. With cold rolling (5 pct per pass) the hardness returned to about R,1:76 after 20 pct reduction and edge cracking became noticeable. However, cold rolling to a total of 40 pct reduction in thickness (RI,,83) was possible before edge crack propagation became serious. Good surface finish was obtained, and the metal loss due to oxidation was minimized by cold rolling and vacuum annealing. Using this procedure the yield of 1.25 in. wide by 0.010 in. thick foil from a 1-in. diam ingot was about 40 pct.

Jan 1, 1961

By O. K. Riegger, L. H. Van Vlack

The median angle of relatively few two-dimensional observations provides a satisfactory value for dihedral angle determinations. Those data that contain bimodal or non-equilibriated dihedral angle distributions are readily detected. THIS paper is concerned with a statistical simplification for determining dihedral angles in solids. Microstructures are partially controlled by relative energies of interphase boundaries and grain boundaries. smith1 has shown rather conclusively that such boundaries may be equilibrated to give a vectorial balance at grain and phase edges. Thus if an accurate measurement is made of the dihedral angle associated with grain and phase edges, an accurate calculation of the relative energies may also be made. The accurate measurement is difficult because the dihedral angle involves two planes in three dimensions, and only a two-dimensional cut through the dihedral angle is usually observed. Such a two-dimensional cut is statistically random provided there is no preselection or orientation. Harker and parker2 have shown that the mode of the frequency distribution of observed angles is within 5 deg of the true angle if the true dihedral angle is 120 deg. smith1 had calculations made to show that the same generalization could apply to dihedral angles of 30, 60, 90, and 150 deg. This procedure of requiring the determination of the statistical mode is time consuming because experience has shown that more than 200 angle observations are necessary before the mode is clearly indicated. It is possible to determine the dihedral angle with equal accuracy with only 25 angle observations if the median angle is used in place of the mode angle. Use is made of Harker and parker's2 basic equation tan =2 sin x cos

Jan 1, 1961

By C. G. Dunn, J. L. Walter

Secondary recrystallization to the (110) [001] texture in high-purity silicon iron occurs if low-oxygen material is annealed in a nonoxidizing atmosphere. Any departure from these conditions results in a growth of (100) oriented grains. The nature of the matrix and secondary recrystallization structures and textures and the nature of grain boundary interactions during growth show that the low gas-metal interfacial energy of the (110) surfaces provides the driving force for growth of these grains. A type of grain growth, characterized by a driving force which derives from energy differences of {hkl} surfaces at the gas-metal interface, has been treated in recent papers.&apos;-7 Secondary recrystallization to the cube text!:: in high-purity silicon iron provides one example. The present paper also deals with a surface energy driving force but the texture that results by secondary recrystallization is not the cube texture; it is a texture in which the (110) plane is in the plane of rolling and the [001] direction is in the direction of rolling. The phenomenon described in this paper is different from the impurity (dispersed phase)-controlled secondary recrystallization process in which the (110) [001] oriented grains grow under the action of grain boundary driving forces.8-12 It is also different from tertiary recrystallization,2 which also produces the (110) [001] texture in high-purity silicon iron, since the matrix textures and grain sizes are different. Finally, it is unlike any other form of secondary recrystallization reported in the literature. The possibility of obtaining the (110) [001] texture in high-purity silicon iron became clear in a study of the effect of impurity atoms on the energy relationships of (100) and (110) surfaces. In this study Walter and Dunn6 observed the migration of (100)/(110) boundaries, i.e., boundaries between two grains, one of which has a (100) plane and the other a (110) plane, respectively, parallel to the plane of the sheet specimen. At 1200°C the (100)/(110) boundaries advanced into (100) grains in a vacuum anneal, then reversed their direction and migrated into (110) grains in a subsequent anneal in impure argon. Finally, the direction of migration reversed once again with (110) grains growing into (100) grains in a second vacuum anneal. These results were explained in terms of a change in concentration of oxygen atoms at the gas-metal interface during the anneals. Thus, oxygen atoms were added to the surface during the anneals in impure argon to the point where ?100, the specific surface energy of the (100) oriented grains, was lower than ?110, the surface energy of (110) oriented grains. In vacuum, however, the oxygen concentration at the surface was lowered to the point where ?110 < ?100. Concerning the possibility of secondary recrystallization in high-purity silicon iron with a low initial oxygen concentration, the observed effect of adsorbed oxygen atoms has indicated6 that a good vacuum anneal would favor the rapid growth of matrix grains with the (110) plane in the plane of the sheet much more than grains in the (100) orientation. The growth of only (110) oriented grains of course would depend upon y110 being less than ?hkl, where hkl refers to any plane different from (110). The present paper is concerned with the application of the above ideas to secondary recrystallization to the (110) [001] texture in high-purity silicon iron. The matrix and secondary recrystallization textures and structures are defined and discussed. Observations of growth of nuclei for secondary recrystallization and of boundary interactions are included to provide direct information on the surface energy relationships between (110) and other (hkl) surfaces. EXPERIMENTAL PROCEDURE As before, 2,4-6 high-purity iron and silicon were melted and cast in vacuum to provide an alloy containing 3 pct Si with less than 0.005 wt pct impurities. The oxygen content of the ingot was lower than in previous ingots, being approximately 3 ppm (by weight). The carbon content of this ingot may have been slightly higher than was found for previous ingots. The same rolling and annealing schedule used previously2 was followed in this study to obtain samples 0.012 in. (0.3 mm) thick. These samples were electropolished prior to annealing. After rolling and polishing, the oxygen content of the material was approximately 6 ppm; material used in the previous studies contained about twice this amount of oxygen.

Jan 1, 1961

By E. T. Hunter

Surrounded by the 13,000-ft high peaks of the San Juan Mountains in southwestern Colo., the town of Silverton is the site of the extensive development operations initiated 20 months ago by Standard Metals Corp. Appropriately termed the Silverton Project, Standard&apos;s operation has now passed the half-way point in its program to reopen two mines that were once sizeable producers of copper, lead, and zinc ores.

Jan 1, 1961

By B. S. Blakeney, E. P. Abrahamson II

The effect of the transition elements in binary solid-solution additions upon the recrystallization temperature of iron has been investigated. All these elements immediately raised the temperature, the majority having their greatest effect in less than 0.10 at. pct. A correlation is noted between the rate of change of recrystallization temperature with atomic percent solute and the electron configuration of the solute element. THE work of Abrahamson and rant&apos; on binary chromium-base alloys indicated that a correspondence existed between the effect of each solute element on the brittle-to-ductile transition temperature of chromium and the ground-state electron configuration of the element added. This was felt to be a bonding phenomenon and would be expected to be observed in measurements of other properties involving the breaking or exchange of atomic bonds. From this work it was postulated that a like correspondence should be found for other properties of binary alloys, such as recrystallization. This study is an effort to check this postulation using binary solid-solution iron-base alloys. Previously, the majority of recrystallization studies were carried out on steels. However, Tammann2 investigated the recrystallization of iron as effected by Co, Ni, Si, Mn, Mo, and Cr and stated that elements with the same crystal structure at room temperature as iron appeared to be more effective in raising the recrystallization temperature. Austin, Luini, and Lindsay3 studied the effects of Ni, Cr, Mn, Co, Si, and Mo on cold rolling and annealing, but noted no trend. Abrahamson and rant,&apos; in their work on the effect of both substitutional and interstitial elements upon the brittle-to-ductile transition of chromium, have shown that the outer electron configuration in the ground state of the solute element appears to be the prime determinant of the transition temperature. PROCEDURE All alloys were made using 99.95 + pct Fe with 0.02 wt pct 0, 0.004 pct C, and 0.001 pct N. All alloying elements were 99.9 + percent pure. Metal-lographically the alloys, out to at least 0.1 at. pct, appeared to be in solid solution. Though several published phase diagrams tend to dispute this.4 All alloys were arc melted six times and cast into square 400-g ingots under an argon atmosphere.

Jan 1, 1961

By K. Sallmann

Spurred by a variety of factors, coal flotation is making headway among the preparation plants of West Germany. The author gives some statistics on German coal flotation plants and information on the properties of the feed and quality of the derived products. Types of machines and reagents used, dewatering practices, tailings disposal, and thickening operations are covered. There is special emphasis on the many-sided problems that confront German coal preparation engineers. The coal mining industry of West Germany is concentrated in three coalfields: the first on the Ruhr and the Rhein rivers, the second on the Saar river, and the third near the frontier between Germany and the Netherlands, around the towns of Aachen and Erkelenz. The total run-of-mine production of these three coalfields amounts to 736,000 tpd which come from 145 collieries. There are 121 washeries, 43 of them with a flotation plant. The total throughput of these 43 washeries is 280,000 tpd, out of which 26,000 tons (9.3 pet of the washery feed coal) are cleaned by flotation. The capacity of the individual flotation plants varies within relatively wide limits, the average being 40 tph and the capacity of the largest flotation plant being 120 tph. During the last few years, the number and size of flotation plants have been steadily increasing, although flotation must be looked upon as an expensive and rather complex cleaning process. The considerations which have led to the widespread application of flotation may be summarized as follows: 1) In making coking coal, it is seldom possible to add uncleaned fines to the coke oven charge, as their ash content is too high. If, however, the ash content of the fines is reduced to a maximum of 7 or 8 pet, they can be admixed to the washed and crushed small sizes without difficulty. This means, naturally that revenue is increased since the price of coking fines is always higher than the price for dust or uncleaned wet fines. 2) To prevent silicosis and pneumoconiosis, water infusion and spraying of the coal are practiced much more today than ever before. As a result, moisture content of run-of-mine coal has markedly increased and the washery feed coal contains more and more slurry instead of dry dust. The price of slurry, how- ever, is very low, and in many cases it is impossible to sell filtered raw slurry with a moisture content of 20 to 25 pct and, at the same time, 20 to 25 pct of ash. Reduction of the ash content of these slurries improves the possibility of dewatering them and, in this way, also enhances the marketability of this product. 3) The new severe laws and regulations against pollution of air and rivers make it necessary to de-dust coal better than in the past and to reduce the quantity of the waste water from coal preparation plants and their solids content to a minimum. 4) Even if there were no compulsory reasons to clean the fines, flotation will often lead to an increase in the overall yield. Although not the only application, it appears that the treatment of coking fines is the primary field for the flotation process in coal preparation. It must not be overlooked, however, that a series of arguments may be advanced against flotation: 1) Flotation is an expensive process because, in addition to the cleaning operation itself, the dewatering of the froth and the disposal of the tailings is very costly. 2) Operation of a flotation plant requires well trained personnel. 3) Filtered froth has about a 20 pct moisture content and, therefore, if mixed with the cleaned small coal it causes an undesirable increase in water content of the coke oven charge. For this reason it is necessary to take additional measures for dewatering washed small coal and this, of course, entails additional expense. 4) Disposal of flotation tailings involves very difficult problems, particularly in the highly industrialized regions. An investigation covering 32 flotation plants of Western Germany shows the following composition and properties of their feed:

Jan 1, 1961

By Barbara A. Thompson

A previously reported high-resolution method for the location of boron-rich areas in metallurgical and biological specimens was been adapted for general use on a routine basis. The rnetlzod utilizes neutron activation and autoradiograpizy. Alpha-particles emitted by boron nuclei upon neutron capture are recorded on a photographic emulsion. The resulting a-particle tracks show the location of boron-rich areas. Experimental techniques, interferences, and limitations of the method are discussed in detail. The method is most useful where there is marked segregation of boron. In this type of sample, the segregation can be observed when the nominal boron concentration is as low as 0.0006 pct. THE positive identification and location of boron-rich areas in metals is frequently of great interest in metallurgical work. Unequivocal identification is often difficult to make by conventional metallo-graphic methods. Recently, a method has been described which accomplishes this objective by neutron activation and autoradiography.l-3 The method can be described briefly as follows. Upon neutron capture, a -particles are emitted by boron nuclei according to the following reaction: ,Blo + n - ,a4 + 3Li7 + 2.4 mev The energy is dissipated as kinetic energy of the products. By irradiating a boron-containing sample in contact with a photographic emulsion and subsequently developing this emulsion, a-particle tracks are obtained whose location corresponds to the location of boron-rich areas in the sample. Two factors combine to make the reaction extremely specific for boron. The first is the unusually high (755 barns) cross section of boron for thermal neutron capture. The second is the higher neutron energy required to produce (n, a ) reactions in essentially all other nuclei except lithium. These two factors make the method specific for boron by six to seven orders of magnitude when a predominantly thermal neutron source such as the Brookhaven reactor is used. The reported limit of detection of this method is of the order of 0.01 pct B., The present work was originally undertaken to determine whether this limit could be lowered by use of a thinner emulsion. However, initial experiments showed that in order to use the method at all, it was necessary to reestablish the optimum experimental conditions in terms of the available irradiation facilities. It is the purpose of this paper to describe these experimental conditions in detail, to discuss the factors influencing sensitivity, and to evaluate several techniques for increasing sensitivity. EXPERIMENTAL A) Preliminary Experiments—The first measure-ments were made using samples of crystal oriented silicon steel containing various concentrations of boron. In the later experiments, samples of various high-temperature alloys such as M-252, hcoloy 901, Nichrome V, and so forth, were used. Faraggi, et al.,2 reported that the lower limit of sensitivity in this type of sample was about 0.01 pct B using nuclear emulsions of 50- u thickness. but that it should be possible to extend this limit by the use of thinner emulsions. Accordingly, we first used Kodak Auto-radiographic Stripping Film (Permeable Base) which has an emulsion thickness of only 5 µ. This was mounted on the metallographic specimens according to the technique described by Boyd.4 The emulsion remained in contact with the metal surface throughout exposure and development. Since the emulsion is transparent after development, the autoradiograph and metal surface can be viewed simultaneously and any correlation between film blackening and structure of the metal can be made directly with no problems of realignment. Because the silicon steel is readily attacked by moisture alone, it was necessary to apply a protective coating to the metal surfaces before mounting the emulsion. The coating was made extremely thin in order to absorb as few a-particles as possible. Boyd4 and Gomberg5 have discussed various plastics used for this purpose; however, none was sufficiently impermeable to prevent chemical attack of the steel during the developing process. This attack resulted in the production of gross chemical artifacts in the emulsion. It was, therefore, necessary to use the method of Wolfsberg and John6 as follows. A very thin (approximately 1 µ) coating of Plexiglas II was applied by dipping the sample in a 2 pct solution of Plexiglas II in dichloroethylene. Then, because the emulsion will not adhere to Plexiglas 11, a thin coating of Parlodion was applied in a similar manner using 2 pct Parlodion in iso-amyl acetate. No protective coating was necessary with the high-tem-

Jan 1, 1961

By W. A. Riggs

In a single year the total transportation cost equals nearly 30 pct of the value of mineral commodities, the largest single cost from the deposit to consumer. The magnitude of this economic factor calls for more complete understanding of cost and operational problems between producer and carrier than now exists. Details are given of the costs of providing transportation as well as freight rates for selling transportation. In 1958, transportation of mineral commodities in the United States required 600 billion ton-miles to move 1 3/4 billion tons of products of mines comprising solid fuels, crude oil, industrial minerals and rocks, and ores. Possibly 17 pct was handled by more than one mode of transport, since combinations of several modes of transport may, at times, achieve better service/cost results than any single mode. Total transportation cost of nearly $5 billion equaled roughly 30 pct of the value of the mineral commodities, the largest single cost from the mineral deposit to the consumer. The tremendous magnitude of this transportation undertaking demands much more complete understanding than now exists between mineral producers and carriers about the economic and operational problems of each other. A substantial portion of the daily work of the writer is spent in trying to act as a combination interpreter and catalyst between potential shippers and carriers, hoping to direct both to points of mutual understanding and advantage. For the purpose of this paper, it is necessary to ask mining people to accept some terminology and to try to appreciate the mental approach of the freight rate making people of the carriers. This paper will consider costs of providing transportation as well as freight rates for selling transportation—although these are fields of limited certainty. There are no accurate statistical breakdowns for all modes of transport and types of carriers indicating commodities, volume of traffic, distances, costs, and rates. Much information is available for railroads, and some for the regulated portions of air, motor, pipeline, and water transportation. Unregulated carriers, handling about half of the transportation of products of mines, are not required to report, and very little is known of their activities. Figures used herein are national in scope, unless otherwise indicated, and have generally been derived from Interstate Commerce Commission reports and files. Tonnage figures have been reduced to net tons of 2000 lb. The very generalized comparison of average mileage freight rate levels for various modes of transport provided by Fig. 1 affords advantageous perspective for the entire field of transportation costs. Dashed guide lines show cents per ton-mile, and dotted guide lines show percentage of first class railroad freight rate. While costs of other than railroad transportation more nearly follow constant cents per ton-mile functions, costs of railroad transportation show characteristic taper, or decrease in cents per-ton mile with increasing length of haul. This fundamental difference in cost is due largely to the fact that railroads and pipelines provide their own fully taxed roadway facilities while highway, waterway, and air carriers use government-provided tax-free roadway at no cost other than fuel, license, and certain excise taxes. Thus railroad and pipeline transportation might be said to carry heavy threshold costs in addition to those transportation costs which are directly variable with ton miles of transportation produced. The original basis of railroad freight rate structures lies in the classification of all articles of commerce into railroad class ralings ranging from 7 to 40 pct of first class (100 pct) rate level, dependent on value, hazard, loading characteristics, service requirements, and whether carload or less than carload. Classification tables and mileage-based (but arbitrarily grouped), rate scales are published as tariffs subject to approval by regulatory bodies. Used together, these determine class rates in cents per 100 lb between points in the U. S. Where local commercial or operating conditions render it advantageous for carriers to depart from

Jan 1, 1961

By B. N. Das, P. A. Beck

THE o phases have a complex tetragonal structure with Lo/ao = 0.52 and 30 atoms per unit cell.1 A large number of such phases are now known to occur in various binary systems of the transition elements and they exhibit the following typical features: 2,3 The composition of binary o phases is variable, ranging from approximately A4B to ABI. With only a few exceptions, in the o phases the A-ele-ment comes from the V- or Cr- group of the periodic table, while the B-elements are from the Mn-, Fe-, Co-, or Ni- group. In the first long period the corresponding o phases of the V- and Cr-series have approximately the same compositions. However, as the B-element changes from Mn to Fe to Co to Ni, the mean composition shifts monotonously toward higher A-contents.2-4 For example, if the mean compositions of the various o phases with vanadium are compared with each other, the composition shift mentioned above becomes plainly visible: V 30Mn0 80 Vo.45Feo..,, Vo .,Coo. 45 and Vo.5Nio.3. Similiar composition shifts, although not the same composition values, were observed in u phases formed by second and by third long-period transition elements.3&apos;4 This behavior, very characteristic of o phases, is in rather sharp contrast to the usually quite well-behaved stoichi-ometry of the Laves phases. In the latter, the AB2 stoichiometry predominates, with A the large atom and B the small atom.= The p phase occurs in the four binary systems of Mo or W with Fe or Co. On the basis of their crystal structure determination, Arnfelt and westgren6 ascribed to the p phase in the Co-W system the ideal composition W,Co7. Since all four binary pphases have nearly the same composition, it would seem quite plausible that some definite stoichiometry such as A6B7, might be characteristic of this phase, as AB2 is of the Laves phases. On the other hand, it has been noted,7 that the phases occur at average electron concentrations near to those at which the various cr phases are found. Also, it has been pointed out by Shoemaker and associates8 that structurally the a phases and the p phases are somewhat related to each other; both of these structures may be described in terms of suitable stackings of quasi-hexagonal layers&apos;of atoms. By studying a suitably chosen ter- nary phase diagram, one might expect to be able to find out which one of the two conditions, the analogy with the o phase or the constant ratio between the number of large atoms and the number of small atoms in effect governs the behavior of the p phase. Several isothermal sections of ternary systems containing o phases have been investigated. In all cases where two binary o phases occur, these were found to be connected b a more or less straight ternary o phase field.7&apos; &apos;10 Such elongated o phase fields were also found in ternary systems in which only one of the limiting binaries is known to contain o phase. In this manner a latent o forming tendency could be detected and the virtual composition of a "binary o phase", which does not actually occur as such was approximately determined by extrapolation. The behavior of the phases, including their composition shift, is analogous to that of the classical electron compounds, as described by Hume-Rothery.11 In order to decide whether the p phase is essentially a "size compound" like the Laves phases, where a fixed stoichiometric ratio is quite generally maintained between the "large atoms" and the "small atoms", or whether the p phase is typically an "electron compound" in the same sense as ois, it was decided to investigate an isothermal section of the Mo-Mn-Co system. The Mo-Co system12 and the Mo-Mn system13 each are known to have a binary o phase. It could be therefore expected that a ternary o phase field will connect these two binary cr-phase fields. The p phase is known to occur in the Mo-Co system. If the p phase should turn out to form an elongated phase field extending deep into the ternary system, the following considerations mighto apply. The atomic radius of manganese (1.314for C.N.12) is between the va,lues for Mo (1.40Afor C.N.12) and for Co (1.26Afor C.N.12). If it is assumed that p is a "size compound", and that Mn is substituting for the smaller Co atoms in the p-structure in the ternary system, the y-phase field might be expected to extend parallel to the Mn-Co binary line. If Mn is substituting for the large Mo atoms in the p-structure, the p-phase field may be expected to extend parallel to the Mn-Mo binary line. On the other hand, if the p-phase turns out to be an "electron compound" like o, the ternary p-phase field should extend parallel to the ternary o -phase field connecting (Mo,Mn)owith (Mo, Co) a

Jan 1, 1961

By L. Adler

Analysis of a mine roof can be based on fixed-end beam behavior. The author here analyzes the effects of zero restraint at deflecting beam supports. Formulae are given for determining permissible support deflections. Analysis of a mine roof in a bedded deposit usually follows the assumption that the behavior of the roof is analogous to a beam with both ends fixed. Yet it is recognized that the end restraint itself varies with the thickness of cover, so that at shallow depth the restraint is minimum, and at great depth, maximum.&apos; Consequently, an analysis on the basis of fixed ends or full restraint represents only one extreme in the possible range of conditions. Since the actual amount of restraint is difficult to ascertain, a more rational approach is to consider the two extreme cases of end restraint. Such situations regarding uncertainty of the restraining effects of supports are not uncommon in structural analysis, and are handled in a like manner.&apos; Since previous studies9)4 have dealt with full restraint, this paper will analyze the effects of zero restraint at deflecting beam supports. In such a case a mine roof with several intermediate supports becomes analogous to a uniformly loaded continuous beam on simple supports, as shown in Fig. 1A. Such a structure is statically indeterminate to a degree equal to the number of intermediate supports, n. Therefore, with the three equilibrium equations, n additional equations are needed. A number of methods exist to analyze this problem, but The Theorem of Three Moments is Simplest. The continuous beam is divided at each support into a sequence of simply supported single span beams, with the unknown end moments, as appears in Fig. 1B. Continuity requires that the common ends of adjacent beams have the same slope (Fig. 1C). eiB= B(i+l)~= ei(i+l)and MiB= Mti+I)A= Mi(i+i). [1I A Glossary of all terms is given in Table I. Furthermore, if we first consider that the supports do not deflect, the slope at a support is the sum of the slopes due to each of the individual loads shown in Fig. 2, yielding:

Jan 1, 1961