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By J. J. Demeter

Experiments were conducted in 2- and 4-inch-diameter standpipes to evaluate the effectiveness of standpipes as pressure seals. During the experiments, these standpipes conveyed Alan-Wood magnetite (60 to 230 U.S. standard sieve mesh) by gravity flow from one vessel to another of relatively higher pressure. The information obtained has been helpful in a Federal Bureau of Mines investigation of how to make either synthesis gas or hydrogen by a modified steam-iron process employing a continuous recycling stream of granular iron-iron oxide at temperatures of 600° to 900° C. In this process the mixture of granular material flows by gravity from a reduction vessel at low pressures to an oxidation vessel at higher pressures. Data from the 2- and 4-inch-diameter standpipes indicate that it would be practical to use a standpipe as a pressure seal between the reductor and oxidizer. Investigators found that, by gravity flow, the standpipe could convey the Alan-Wood magnetite against pressure gradients up to 1.07 pounds per square inch per foot of column height.

Jan 1, 1961

By McKenzie A. M

The Corridor ore body is so named because it occurs in an east-west zone or corridor of schist bounded on the north by the siliceous conglomerates of Mount Lyell, and on the south by similar conglomerates of the Tharsis ridge (Fig. 1). It was discovered after the geophysical prospecting methods described below had defined a target zone for diamond drilling.Since the proving of copper mineralisation by drilling, the corridor orebody has served the vital function of a convenient known target body for the orientation of more recently developed geophysical methods. Traversing of the orebody by these new methods has provided experience for the evaluation of anomalies elsewhere.Some of the methods applied had not been used in Australia before, and were introduced to the west coast of Tasmania through the undertaking there of modern regional exploration programmes. The authors feel that the information gained could be of assistance to others engaged in geophysical prospecting.HISTORY OF DISCOVERYProspecting in the Mount Lyell district has been more or less continuous since 1881. The first geological report was published by Thureau (1886).In 1934, Blazey and Douglas (1934-38) commenced geophysical surveys at Mt. Lyell using the equipotential method.They obtained anomalous indications in several discrete zones and actually detected the south-east half of the corridor orebody but their work never became the basis for...

Jan 1, 1961

By Charles E. Whieldon

The importance of producing more oil from known petroleum reserves has placed increased emphasis on the application of secondary-recovery methods. Recently published reports3 4/ describe the results of waterflooding in Roane and Pleasants Counties, W. Va. (see fig. 1.) This report describes the Barron Kidd Oil Co.?s Santee waterflood project, Maxton sand, Burton field, Church district, Wetzel County, W. Va. (See fig. 2.) The Federal Bureau of Mines hopes that these reports will stimulate interest in improved waterflooding techniques, thereby discouraging premature abandonment of oil leases.

Jan 1, 1961

By F. Petkovich, M. P. Sudbury

Development of a new method of treating flotation concentrates for the preparation of feed suitable for direct charging to blast furnaces or converters is described. The method takes advantage of the fact that pyrrhotite contained in the concentrates can be made to undergo exothermic reactions which, under properly controlled conditions, result information of oxidation products that serve to cement the concentrate particles together. Thus green concentrates either in the form of pellets or briquettes containing 5 to 8 pct moisture not only were hardened, but also completely dried autogenously by continuous countercu,vrent shaft treatment with air. The process was developed through pilot plant operations ranging from 35 1b per hr to 2.5 tph, culminating in products evaluation tests on a railway-car scale. Falconbridge Nickel Mines Ltd., Falconbridge, Ont., have practised sintering, on a travelling grate machine, for many years to prepare a pyr-rhotite-bearing Cu-Ni sulfide flotation concentrate for blast furnace smelting. In recent years the development of new mines, and the construction of concentration plants some 40 miles from the smelter has increased the quantity of concentrate shipped, and encouraged the search for a method of producing dry, hard pellets or briquettes suitable for direct charging to a blast furnace or converter, and capable of withstanding considerable handling. The cementing properties of pyrrhotite oxidation products were discovered during a search for a suitable agglomeration method for sulfide concentrates, and were exploited in a process subsequently developed for autogenously drying and hardening pellets and briquettes of pyrrhotite-bearing Cu-Ni sulfide flotation concentrate. EARLY TEST WORK The production of hard, dry pellets of concentrate filter cake was attempted in the drying plant of one of the new concentrators. While soft pellets were produced containing 5 pct moisture, attempts at further drying resulted in disintegration of the pellets and intolerable dusting. The plant therefore was controlled to produce a concentrate containing about 6 pct moisture. The partially dried concentrate, which was shipped to Falconbridge for sintering, tended to heat spontaneously in transit. An at- tempt to briquette the moist concentrate at Falconbridge, in a plant incorporating a muller, a 20-in. roll briquetting press, and a steam-heated travelling grate oven, was more successful, although the equipment corroded rapidly due to the acid nature of the concentrate after spontaneous heating had occurred. LABORATORY STUDIES OF SPONTANEOUS HEATING OF CONCENTRATE The spontaneous heating of partially dried concentrate was studied in the laboratory. Moist concen-

Jan 1, 1961

By W. L. Dare

This report is one of a series published by the Federal Bureau of Mines to describe methods and costs of mining uranium on the Colorado Plateau. The Navajo Uranium Division of Kerr-McGee Oil Industries, Inc., mines uranium from several deposits of carnotite-type ores, which lie buried in the Lukachukai Mountains on the Navajo Indian Reservation, Apache County, Ariz. The country is rugged and isolated Constructing and maintaining roads has been a continuous task. The ore bodies occur within the Salt Wash member of the Jurassic Morrison formation and are similar to other such deposits on the plateau. The current mining activity in the Lukachukai Mountains is a result of uranium-ore discoveries in 1949, although the Navajos undoubtedly knew of the outcrops of yellow uranium minerals long before that time. The ruggedness of the country and the heavy soil cover over much of the surface hampered prospecting, but probably the main reason the ore was not found sooner is that no one took the trouble to look for it in the Lukachukai Mountains.

Jan 1, 1961

By H. Linder, W. H. Dennen

The graphitic carbon content of soils may be used to detect and delimit subsurface graphitic zones. Spectrographic measurement of carbon in C horizon soils from several areas in the northeastern United States shows good correlation with known graphitic bodies. Bodies of graphite and sulfides are readily located by electromagnetic prospecting methods, but these methods cannot generally discriminate between them. Usual practice, therefore, requires follow-up work on electrically anomalous areas by trenching, drilling, or soil sampling in order to determine the mineralogical nature of the conductor. The efficiency and cost of such follow-up is consequently an important factor in prospecting. The presence of buried sulfide deposits is often reflected in concentrations of metals in the superincumbent soil. Simple chemical tests for such metal concentrations have been developed and applied with considerable success. Bodies of graphite or mixtures of graphite and sulfides are, however, very common and a means whereby buried graphite could be detected by soil testing should provide valuable additional information in the search for ore sulfide and graphite deposits. Graphite is a notably stable substance and should persist in soil above graphite-rich horizons. Microscopic examination of soil samples high in carbon, however, failed to reveal any recognizable graphite fragments indicating a grain size in the clay range. Presumably such small particles would have some mobility in a soil by a translocation mechanism similar to that proposed for the movement of clay particles in a soil profile. Experimental data supports this idea since the boundary between background and anomalous soils carbon values is quite sharp, but the anomalous zone is slightly broader than the graphitic source rock. A simple spectrochemical technique for the determination of carbon in geological materials has been described by Dennen,1 and may be directly applied to soils. A modification of this technique which employs an arcing chamber through which nitrogen is passed is recommended to decrease contributions from atmospheric carbon dioxide. Tests indicate that soils over graphitic zones may be strongly enriched in carbon. The spectrochemical determination of carbon depends upon the formation of the cyanogen molecule (CN) from carbon in a sample and atmospheric nitrogen, under the high temperatures associated with a dc arc. Samples for analysis are dried, lumps broken, and screened. A small portion of the -100 mesh fraction is packed into a copper electrode and excited as the cathode of a dc arc. The band spectra of cyanogen are recorded photographically and the density of the bandhead CN 3883A is measured. The limit of detection of the method is about 0.01 pct C and its coefficient of variation is about 15 pct. Soils, of course, contain carbon in other forms than graphite, and the amount of interference from such sources was examined. The C horizon of several soils from Massachusetts, Maine, and Pennsylvania were found to have a carbon content of 0.3 to 0.5 pct by weight. This content is chiefly due to the presence of carbonates and vegetable matter in the sample and may be readily eliminated, or at least

Jan 1, 1961

By P. K. Guerrero, N. Arbiter

The correlation of power consumed by a tumbling mill with the dimensions, speed, and load has been attempted by three principal methods. One of these, the torque formula, has been reviewed critically elsewhere.' This approach, while analytical, disregards the individual motion and speed of the tumbling bodies and assumes that the gross geometry of the entire load is sufficient to establish the power requirement. A more general approach, using dimensional analysis, has been applied in this laboratory by the present authors1'1, and more recently by Rose.3 This disregards the internal conditions within the mill entirely and in effect is an empirical procedure for correlating data. Finally, the complete analysis of tumbling mill dynamics as first made by Davis' attempts to develop the power requirement from individual ball and rod paths and velocities. Although Davis' result is applicable only at a single speed for a given size and load it could be useful, since his optimum speed is at the upper limits of conventional tumbling mill practice. Where power values predicted by the Davis equation were compared with actual mill requirements, they were found too low for small mills and much too high for the largest mills. This suggested that the agreement with actual intermediate range requirements might be fortuitous, and the development of the equation was examined critically. The probable source of error was found to lie in an erroneous assumption made by Davis in converting the energy of ball or rod motion to power. With the same approach, but with different assumptions, a modified equation has been obtained which predicts results that are usually consistently high. This is to be expected, since it is assumed that there is no slip between load and shell and no interference among tumbling bodies. Both these effects should account for the difference. Development of Equation: When a cylindrical shell charged with a substantial weight of rods or balls is slowly rotated about a horizontal axis, the load surface first assumes an inclination that gradually increases to a maximum. Continued rotation results in failure within the load, characterized by a sliding of the top layers down the slope and a reduction in the angle of inclination. Further rotation again increases the angle, and the cycle repeats. If the speed is increased, there is continuous load failure and build-up and a continuous stream of rods or balls descends over the upcoming mass, which moves in circular arcs. At higher speeds the up-

Jan 1, 1961

By J. R. Nettle

The purpose of these studies by the Federal Bureau of Mines was to determine the feasibility of refining low-grade hafnium by an inert-gas-shielded molten-salt electrorefining technique to produce a hafnium metal meeting reactor specifications. The techniques were adapted from those used success-fully for titanium electrorefining. Three electrolytes containing hafnium chlorides were developed from which deposits having a Brinell hardness of 170 or below were recovered. A KC1 + NaC1 + HfC14 electrolyte produced deposits in the hardness range of 140 to 165 Brinell. Deposits with a hardness range of from 132 to 152 Brinell were pro-duced from an electrolyte composed of KC1 + LiC1 + HfC14. A third electrolyte composed of NaC1 + K3HfC17 produced deposits with a hardness as low as 139 Brinell. In a fourth electrolyte, composed of NaC1 + K2HfF6, a measure of refining was accomplished, but under the test conditions no metal meeting specifications was recovered; none was softer than 174 Brinell. A number of metallic impurities were reduced in quantity by the electro-refining process, notably iron, which normally was reduced from 250 p.p.m. to less than 50 p.p.m. Magnesium generally was reduced from 680 p.p.m. to less than 80 p.p.m. Manganese content was also reduced by the electrorefining process. Sponge containing 90 p.p.m. Mn yielded deposits containing a maximum of 50 p.p.m.; some deposits contained only 10 p.p.m.

Jan 1, 1961

By J. F. Shea, O. F. Tangel

Battelle Memorial Institute participated in a program for the General Services Administration aimed at developing a nickel-cobalt separation process that could be integrated in the Nicaro nickel plant. At the time the programwas being carried out, the Nicaro process was a straight-through operation, in which the ore was reduced and leached, after which the pregnant solution was boiled to produce a so-called "bulk precipitate" which contained virtually all of the nickel and cobalt which had been dissolved in the leaching step. The weight ratio of nickel to cobalt in Nicaro ore is approximately 15 to 20:l. The weight ratio of nickel to cobalt in the finished product had to be 100:l or higher to meet specifications. Because the Nicaro process embodied no nickel-cobalt separation step, the only way that a bulk precipitate of the specified nicke1:cobalt ratio could be produced was to so adjust roasting and leaching conditions that nickel would be selectively leached and most of the cobalt would be rejected with the tailings. The required selectivity, however, was achieved at the expense of nickel recovery, which was 5 or more per cent less than might have been obtained with the existing equipment, utilities, man power, etc., had selectivity been no object. The over-all purpose of the program was to develop a separation step that could be fitted into or onto the Nicaro facilities and which would permit the manufacture of a product that would meet the desired specifications and still permit the recovery of a maximum amount of nickel. Battelle suggested that this might be accomplished by reprocessing off-specification bulk precipitate and specifically suggested the process based on ammonium sulphate leaching followed by hydrogen reduction of the leach solution according to techniques developed commercially by Sherritt Gordon Mines Limited. Such a process would not only satisfy the objectives of the research but would present two additional advantages. (1) It would produce a separate cobalt product which could be further processed into metal, alloys, oxides, or salts. (2) It would yield nickel in metallic form which might be more generally marketable and command a slightly higher price per unit of nickel than the Nicaro oxide product. DESCRIPTION OF THE PROCESS Figure 1 is a flowsheet of the process. The essential features are: (1) Extraction of about 97 per cent of the nickel and about 85 per cent of the cobalt from bulk precipitate by a principal leach with ainmonium sulphate solution (Step A). Extraction of virtually all of

Jan 1, 1961

By Dale W. Richardson

Ductile hafnium was not obtained consistently by the conventional Kroll process. The bimetal reduction modification produced a more ductile hafnium by lowering the impurities, especially oxygen, in the sponge metal. Hafnium oxide was chlorinated in the presence of carbon to form anhydrous hafnium tetrachloride, which was reduced by sodium and magnesium in an inert atmosphere to produce sponge hafnium metal. After vacuum distillation to remove the byproducts, the sponge was arc-melted into ingot and rolled into strip. Metallic impurities were decreased by evaporating the hafnium tetrachloride from a fused salt. An excessive amount (over 1,200 parts per million (p.p.m.)) of aluminum was contained in some of the hafnium oxide, much of which remained as aluminum chloride in the hafnium tetrachloride during chlorination. Evaporation of the hafnium tetrachloride from a fused NaCI-KCI mixture during the Mg-Na reduction greatly lowered its aluminum content, as most of the aluminum and some of the other metallic impurities were retained by the fused salt.

Jan 1, 1961

Jan 1, 1961

By Maurice J. Peterson

The applications of optical spectrochemical methods of analysis for determining trace impurities in metals are described, and the need for developing analytical procedures capable of accurately determining fractional parts per million of impurity elements in metals is stressed. Factors which determine sensitivity of detection and means to extend sensitivity levels in spectrochemical methods are discussed. Examples from the current literature illustrate the diversity of spectrochemical techniques that have been applied to the analyses of varied sample types, Many of the methods use preconcentration procedures to increase sensitivity limits. A bibliography containing abstracts of recent methods in included. Optical spectrochemical analysis is based upon the measurement of radiant energy emitted by atoms of the elements to be determined when a sample is subjected to a suitable source of excitation. The behavior of the valence electrons during excitation, usually by an arc, spark, or flame, produces radiant energy of specific wavelengths. This is recorded as spectral line images on a photographic film or plate by the spectrograph; for direct-reading instruments, the spectral lines are detected with photomultiplier tubes. The spectral lines result from the excitation of atoms in the sample. Each variety of atom produces its own characteristic set of lines, thus serving to identify the elements in the sample. Increased concentrations of elements in the excited sample results in increased blackening of the spectral line images.

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

By W. L. Hunter

The research on this report was conducted to obtain information on the feasibility of producing ferro chromium of varying silicon and carbon contents from domestic chromite. Concentrates from the Mouat deposit were chosen because they typify the chromite found in the Stillwater complex, the largest domestic reserve, and are similar in composition to other extensive North American and foreign deposits. Batch-smelting tests designed to produce high-, medium-, and low-carbon ferrochromium were made in single phase and three-phase, electric-arc, steelmaking furnaces. Agglomeration studies were made in a rotary kiln. Continuous smelting tests were made to yield data on the production of high-carbon ferro chromium and low-carbon ferrochromium-silicon. The carbon content of high-carbon ferrochromium was lowered to the medium-carbon range by oxygen injection. Mouat stockpile concentrates were nodulized in a gas-fired rotary kiln using quartz, limestone, and fluorspar additions in the proportion necessary to flux the slag. The nodules were smelted in a continuous test using coal, coal char, and mixtures of the two consecutively as reductants.

Jan 1, 1961

By Eugene T. Sheridan

The Bureau of Mines annually canvasses the fuel-briquet and packaged-fuel producers in the United States and publishes economic data on these industries, based upon reports submitted voluntarily by producers. This publication lists all producers that reported commercial production to the Bureau for 1960 and presents data on individual plants. The companies named herein represent virtually all producers of processed minerals fuels. A few small plants may not have been canvassed or failed to respond to the survey because some of the smaller plants operate intermittently and the survey is voluntary. All plants that reported commercial production were included; regardless of size. Specifically excluded were plants that manufactured briquets from wood charcoal. Fuel briquets and packaged fuel are manufactured solid fuels, produced by mixing fine-sized mineral fuels with binding materials and compressing into small individual shapes, Briquets are produced in pillow-shaped and cylindrical form, are 2 to 4 inches long, and weigh 2 to 4 ounces. Packaged fuel consists of 3- or 4-inch cubes; 6 or 8 of which are wrapped together in heavy kraft paper to form a package weighing 10 to 15 pounds, Briquets are durable and may be stored and handled as bulk fuel; packaged fuel breaks easily and must be stored indoors to prevent it from deteriorating. Whereas briquets are consumed in many areas as a general residential fuel, packaged fuel is more of a specialty item, used at times to supplement other fuels. Packaged fuel is burned without re-moving the paper and is referred to as the "white glove" fuel.

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 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.3'4 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'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' '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