Search Documents

By W. A. Tiller, J. P. McHugh

HE majority of liquidus and solidus surfaces in phase diagrams have been determined by the conventional cooling- and heating-curve techniques.' These techniques have two main shortcomings: 1) the solidus may be in considerable error due to the difficulty involved in completely homogenizing the solid and 2) the determination of liquidus and solidus in more than a two-component system does not enable one to determine tie-lines connecting the specific equilibrium solid and liquid compositions. However, in a recent paper by one of the authors,' a method was suggested whereby the liquidus and solidus surfaces plus tie-lines in an n-component system may be determined. This method utilizes a controlled solidification technique and assumes that interface equilibrium exists during freezing. The present work was undertaken with a twofold purpose; first, to determine the liquidus and solidus lines in the pseudo-binary system Bi2Te3-Bi2Se3 by heating- and cooling-curve techniques and, second, to determine the partition coefficients of Te and Se in the BizTe3-,Sex system by controlled solidifica- tion techniques. The two sets of results can be compared to test the accuracy of the controlled solidification method. EXPERIMENTAL I—The starting materials for this study were 997999 pct Bi, Te, and Se, obtained from the American Smelting and Refining Co. The compounds BizTe, and Bi2Se3 were each prepared by melting together stoichiometric amounts of the elements, followed by twelve zone-refining passes. This produced homogeneous bars of the compounds for use in the phase-diagram studies. The apparatus used to obtain heating and cooling curves is illustrated schematically in Fig. 1. The alloy samples were located in a graphite crucible placed in a stainless steel canister. The canister was supported in a heavily lagged pit furnace by a device which oscillated the canister about its vertical axis at a frequency of about 3 cycles per sec during heating and cooling-curve runs. The graphite crucible was designed to minimize the thermal coupling of the sample to the furnace. A thin graphite sleeve separated the alloy sample from the stainless steel tube that housed the thermo-

Jan 1, 1960

By D. Kramer

HASEN1 has published a phase diagram for the zirconium-nickel system. This phase diagram has been redetermined by Hayes, Roberson, and paasche2 in the range 0 to 50 at. pct Ni. Recently, Smith and Guard3 have published a tentative diagram for the

Jan 1, 1960

By Raymond B. Ladoo

Wollastonite is a calcium metasilicate, with the formula CaSiO3; containing theoretically 48.3 pct CaO and 51.7 pct Si02. It is one of many natural and synthetic silicates with varying CaO/SiO2 ratios, with and without water of crystallization. While it is a very common mineral, deposits of sufficient size and purity to be of commercial interest are unusual. There is only one producer (1958) of wollastonite for industrial use in the United States, Godfrey L. Cabot, Inc. at Willsboro, New York. There has been a small production of surface material for ornamental use from near Blythe, California. Carload tests have been made on California wollastonite for making mineral wool and a commercial plant for this purpose was projected in 1957. Properties Wollastonite is monoclinic and commonly occurs in masses or aggregates of bladed or needle-like crystals. It has a perfect cleavage parallel to the long prismatic axis. It is rather brittle and some types grind easily to a very finely fibrous product, but other types, due to interlacing of fibers, are tough and difficult to grind. Mobs hardness is 4.5 to 5; specific gravity 2.8-2.9; index of refraction 1.616 to 1.631; melting point 1,512°C. Color when pure is a brilliant white, but when less pure it may be gray or brown. Luster is vitreous, transparent to translucent. Common mineral associates are garnet (several varieties), diopside, calcite and quartz. The nature of the mineral impurities determines to a large degree the commercial value of a deposit. At Willsboro, New York, the impurities consist chiefly of iron garnet and iron diopside which are both magnetic and so are easily removable by magnetic separation, yielding a nearly theoretically pure product. Some deposits in California contain calcite and quartz which cannot be removed cheaply, thus limiting market possibilities. Occurrence Wollastonite is a contact metamorphic mineral occurring in most places within or associated with impure limestones. The deposits at Willsboro, New York1,2,3,5 consist of two or more beds dipping 15-50°E and striking NW-SE. The main bed, 30 to 70 ft thick, may be traced on the surface for at least 2 ½ miles. In this belt, the Pre-Cambrian Grenville limestone has been injected and partially replaced by the more liquid portions of an anorthositic magma. Buddington and Whitcomb3 have described the rock as "Mixed gneisses, pyroxenite and garnetiferous gneisses and skarns." Prospecting revealed the wollastonite at ten different places in the belt, overlain in most places by a garnet rock. Diamond drilling has proven several million tons with probable reserves around 15 million tons. Interbedded with the wollastonite are beds of garnet from a few inches to several feet in thickness. In the wollastonite ore itself the chief and almost only associated minerals are garnet (mostly almandite but some andradite and grossularite) with small amounts of green hedenbergite. Inasmuch as the almandite and diopside are magnetic they are easily separated from the wollastonite in high intensity magnetic separators. If grossularite should occur in quantity other means of separation would be needed. Wollastonite has been reported at 35 localities in California12 but only those in the Big Maria and Little Maria Mountains, 16 to 20 miles north of Blythe, Riverside County, are

Jan 1, 1960

By A. A. Bauer, M. S. Farkas, F. A. Rough

An investigation of the d-phase relationships between the uranium-zirconium and uranium-molybdenum systems was conducted. A ternary cut joining U-31.5 at. pct Mo to U-74 at. pct Zr is presented on the basis of differential thermal analysis, metallographic and X-ray diffraction data. HyDothetical isothermal ternary sections, inferred from the determined d-phase relationships, are presented for the uraniztm-zirconium-molybdenum system. A ternary eutectoid, at 454ºC, was found in zirconium-rich alloys. Its composition, based on metallography and electron-beam micro-analysis, is estimated as U-61.7 at. pct Zr-7.1 at. pct Mo. URANIUM binary systems have been studied extensively in the past to supply basic information needed in reactor-fuel development. Alloys of uranium with zirconium, molybdenum, and titanium are of particular interest because, in these binaries, extensive or complete solid solubility between the body-centered-cubic forms of these elements and y uranium exists. In addition, an intermediate phase of limited solid solubility forms in each of these systems by transformation of the high-temperature ?-uranium phase. Previous investigation of the phase relationships existing between the intermediate 6 phases in the uranium-zirconium-titanium and the uranium-molyb- denum-titanium ternaries have already been reported.1,2 The results of an investigation of the phase relationships existing between the 6 phases in the uranium-zirconium-molybdenum system is reported here. The phase equilibria that occur in the solid-state portions of the pertinent binary systems are shown in Fig. 1. Phase nomenclature appearing throughout the report is as shown in these diagrams. The crystal structure of the phases in this system are given in Table I. EXPERIMENTAL PROCEDURES Alloys were cast and fabricated to 1/4-in.-diam rod. Specimens were heat treated and examined by metallographic and X-ray techniques. Thermal-analysis data were obtained.

Jan 1, 1960

By D. Gupta, S. Weinig

This investigation comprises the study of dislocation-oxygen interactions in a! titanium and its effect on the ductile to brittle transition in titanium. Internal friction techniques using a low-frequency lorsion pendulum were used to study the oxygen atom interactions with dislocations in "superpurity" titanium. A calculation of the interaction energy between an oxygen atom and a dislocation, based on the "breakaway" strain resulted in a value of 0.015 ev as compared to theoretical values of 0.022 and 0.035 ev for edge and screw dislocations, respectively. Both the saturation of the room temperature decrement and the transition from ductile to brittle behavior occurred at 1.5 at. pct 0. It was proposed that the embrittlement was due to oxygen atoms immobilizing the dislocations. It was possible to increase the ductility of the Ti-0 binary alloys by decreasing the oxygen pinning. The increase in uniform elongation was 30 pct for an increase in the preanneal temperature of 300°C. ThE room-temperature ductility of a titanium is significantly affected by interstitial solutes. Although oxygen has a solid solubility of 15.5 pct by weight, the room-temperature ductility extends only to 0.6 pct.' The ductility precipitously falls at this concentration and the fracture characteristics change from ductile to brittle.2 The small effective bulk composition of solute required to destroy the room-temperature ductility of the titanium must be indicative of an in-homogeneous distribution of solute atoms. Internal friction techniques were used in this investigation to

Jan 1, 1960

Jan 1, 1960

By H. J. McQueen, G. C. Kuczynski

ThE useful properties of k6-Alfenol and the thermenol alloys (summarized by J. E. Nachman and W. J. Buehler') have encouraged research into those alloys which, having compositions near 25 at. pct Al, 75 at. pct Fe, undergo an ordering transformation between 500° and 550°C. The equilibrium diagram of the iron-rich iron-aluminum alloys was first determined by Bradley and Jay.2,3 They distinguished three structures: the disordered, which is bcc; FeAl, which is simple cubic with one Fe atom and one Al atom per lattice site; and Fe3Al, which is fcc with three Fe atoms and one Al atom per lattice site. This last structure may be conceived as eight body-centered cubes with Al atoms at the centers of alternate ones, so that Al atoms have only Fe as first and second nearest neighbors. Later, Osawa and Murata4 determined the boundaries of the different superlattice regions in the iron-rich Fe-Al solid solution by dilatometric and X-ray methods. Two of the six phases, which they found between 0 and 50 at. pct Al, were never identified by other workers. A. Taylor and R. M. ones,' concurrently with and independently of this research, redetermined this diagram by measuring lattice parameters at temperature. Further reference will be made to their results. EQUILIBRIUM DIAGRAM A) Experimental Procedure—The alloys were prepared from NRC gas-free iron (99.9 pct Fe) and 99.99 pct Al. They were melted in alumina' crucubles under vacuum in an induction furnace. If the ingots were unsound or showed more than a 3 pct weight loss, they were rejected. The ingots were homogenized at 1100°C for 24 hr before hot-rolling at 700" to 900°C from 1 in. to 0.25 in. thick. It is interesting to note that alloys containing more than 28 at. pct Al were able to take an 80 pct reduction of area in the ordered FeAl region. The dilatometer specimens and specimens for chemical analysis were cut from these plates. A Leitz dilatometer was used to measure the coefficient of linear expansion as a function of temperature. The specimens were slowly cooled from 900" to 300°C where they were annealed for 10 hr before slowly cooling to room temperature. The expansion was recorded photographically as the alloys were heated and cooled at 1.5oC per min between 100" and 1000°C. The magnetic measurements determining the Curie points were performed on the dilatometer specimens in the dilatometer, by using direct current in the furnace windings both to heat the specimen at 1.5°C per min and to serve as the primary coil. The regular specimen holder was replaced by a thin alundum tube on which was wound, as a secondary, a closely spaced coil of fine copper wire. A reversal of current in the furnace windings produced, in the secondary, an emf which was proportional to the induction in the specimen, and which could be detected on a galvanometer. In this way, it was possible to determine the Curie points of alloys to within * 5°C. B) Results and Discussion—The coefficients of linear expansion, as obtained from the dilatometer curves, are plotted as a function of temperature and composition in Fig. 1. Since in many cases the heating and cooling curves were superimposed, it was decided to measure slopes of heating curves only. Definite high peaks, due to the transformations, were observed on each curve between 400" and 520°C, and, for alloys containing more than 23 at. pct Al, a second set of smaller peaks at temperatures above 660°C. The sharpness of the peaks indicates that ordering to Fe3Al is a first-order reaction. The compositions and the temperatures of these peaks are listed in Table I. When these temperatures are plotted as a function of the composition, the result is the constitution diagram presented in

Jan 1, 1960

By C. G. Kirkland

An apparatus for determining trace impurities in Grade-A helium by mass spectrometer methods was designed and built by the Federal Bureau of Mines. Grade-A is the designation for helium commercially produced by the Bureau. Its nominal purity is 99.995 percent. The device, following a suggestion by Deaton, concentrates the impurities in the helium by freezing them out in a coil-and-trap assembly cooled by liquid helium. A known volume of helium is passed through the trap, the concentration ratio determined, and samples of the concentrated impurities are analyzed by mass spectrometer methods. The apparatus has been in service for approximately 20 months and has satisfactorily met all requirements. Over 200 analyses were made of helium contained in conventional cylinders, obtained from the Amarillo, Exell, Otis, and Navajo Helium Plants, during the 6-month period ending March I, 1959. Total impurity concentrations, in parts per million, were as follows: Amarillo, 19.1; Exell, 17.1; Otis, 11.3; and Navajo, 6.6. Neon and nitrogen were the major impurities. Complete data are shown in table 4 in the body of this report.

Jan 1, 1960

By C. Land, R. Hultgren

Heat contents of four Cr-Ni alloys were determined in a diphenyl ethev calorimeter. Aside from ferromagnetic effects, Kopp's law of additivity of heat capacities is approximately fol-lowed, in disagreement with earlier results of A. W. Foster. In 1934 Foster1 reported heat-capacity measurements of dilute solutions of chromium in nickel, primarily as a study of the effect of alloying on the ferromagnetic Curie temperature. He found that, apart from the Curie temperature effect, the general level of heat capacities was reduced 10 pct by the addition of 1 pct Cr; 20 pct by the addition of 2 pct Cr. His measurements of pure nickel essentially agreed with accepted values. These results indicate that small amounts of dissolved chromium cause an increase in the Debye temperature of nickel, presupposing a change of frequency of interatomic bonding vibrations which is much larger than should be expected. If Foster's results were verified, therefore, they would have important implications for bonding theory. The only other heat-capacity measurements in this system seem to be those of Taylor and Hinton,' who studied anomalies which they attributed to super-lattice formation at 25 at. pct Cr. At temperatures above the anomaly, Taylor and Hinton found heat capacities at this composition were quite normal, approximately obeying Kopp's law of additivity. EXPERIMENTAL WORK In order to verify or disprove the remarkable results of Foster, the heat contents of four dilute solid solutions of chromiunn in nickel were measured in a diphenyl ether calorimeter. This instrument, described elsewhere,, operates on the principle of the Bunsen ice calorimeter, but uses diphenyl ether as the working substance. Diphenyl ether melts at the convenient temperature of 26.S°C and supplies a more sensitive measure of heat than ice. The hot sample, in an atmosphere of argon, is dropped from a furnace at a measured temperature into a chamber which is surrounded by a mixture of solid and liquid diphenyl ether. The heat from the hot specimen melts some of the solid without chang- ing the temperature of the calorimeter. The amount of solid melted, and therefore the number of calories released by the specimen, is measured from the increase of volume of the mixture, which pushes mercury down a graduated capillary tube. The apparatus has been standardized against the known heat content of pure platinum. Heat loss during the dropping of the specimen was estimated by comparing the heat content of an empty platinum capsule with a solid platinum ball of the same radius and degree of polish of the surface. Repeated tests demonstrate the precision of measurement to be closer than *0.3 pct. Smoothed experimental results are listed in Table I. The tabulated values for pure nickel are taken from kelley, several measurements were made which agreed closely with this tabulation. For chromium, however, no similar agreement was found. The values tabulated were taken from a thorough study of chromium with the diphenyl ether calorimeter which will be published elsewhere.= Suitable plots of the data showed the expected ferromagnetic anomalies in the low-chromium alloys, while the 11 pct alloy shows no ferromagnetic anomaly, but a different, small anomaly below 900°K. This is perhaps the same anomaly found in CrNi, which was once attributed to superlattice formation,' but is probably due to some other cause, such as antifer-

Jan 1, 1960

By W. M. Lehrer

RECENT development of high-temperature brazing alloys has required information regarding the eutec-tic temperature and composition of the Pd-rich section of the Pd-B system.. Literature on this subject was found to be scanty with no complete system yet determined. Buddery and welch1 report an inter-metallic compound occurring in the Pd-B system at 6.33 wt pct B (PdsBz). Another source, Sieverts and Bruning,2 indicates that after annealing at 700°C, a 1.6 and a 2.0 wt pct B alloy were two phase whereas a 0.75 pct B alloy was single phase. Recent work3 using a hot-stage microscope has proposed a eutectic temperature of 743OC. This method utilized the observation of the onset of incipient melting at grain boundaries. The eutectic composition, however, was not determined. METHODS AND PR0CEDURES Five alloys were prepared by triple inert arc-melting high-purity palladium (95.98 pct) with additions of 2 to 6 pct purified amorphous boron. The alloys were crushed within a hardened steel mortar with a steel pestle. The 2 pct alloy, however, was too tough to be crushed in the above manner so was crushed by successive reductions through a rolling mill. Approximately 17 to 18 g of the crushed alloy was used in the thermal analysis. The alloys were melted in pure quartz crucibles. The thermocouple protection tubes were also of quartz and fused along the inside wall of crucibles to prevent floating of the thermocouple. This was an expediency as centering of the thermocouple in the melt would have been preferable. Melting was done in a tube furnace with a slow flow of tank helium maintained as a protective atmosphere. Heating and cooling rates were maintained at 3.5OC per min through the critical temperature ranges by means of a synchronous motor hook-up to a furnace controller. All specimens were heated to 100°C over the indicated liquidus on heating prior to reversing to the cooling cycle. Specimens emerged from the furnace with mirrorlike brightness attesting to the protective quality of the helium atmosphere. Thermal arrests were detected by the differential thermocouple technique using chrome l-alumel couples and nickel as the reference specimen. Arrests were recorded on a Leeds-Northrup automatic X-Y recorder. The specimen temperature and temperature difference were read to + 7.5OC and ± 1.5OC, respectively. These readings were well within the sensitivity of the instrument amplifier. Chromel-alumel couples were used in lieu of Pt-Rh as very few arrests were contemplated in excess of 1200" to 1300°C, the approach of instability. No standardization was performed on these thermocouples subsequent to their use. RESULTS The thermal arrest temperatures obtained are plotted in Fig. 1 as a function of wt pct B. The composition function was obtained by chemical analysis of portions of the specimens after the thermal analysis was completed. The 2 to 6 pct nominal alloys were found to have 1.80, 2.35, 3.65, 4.18 and 5.90

Jan 1, 1960

By H. F. Weaver

The 18th National First-Aid and Mine Rescue Contest was held in the Memorial Auditorium, Buffalo, New Vork, October 5, 6, and 7, 1959. The meet was sponsored by the Federal Bureau of Mines and the Joseph A. Holmes Safety Association, in cooperation with State mine inspection agencies, management and labor of the mineral extractive industries, and other safety minded groups. The Arrangements Committee, as authorized by the General Committee, made a11 the necessary arrangements for conducting the 1959 contest. Members of the Arrangements Committee were: Harry Gandy, Jr. (chairman), National Coal Association; James B. Benson, Southern Coal Producers' Association; Charles Ferguson, United Mine Workers of America; George C. Trevorrow, Bituminous Coal Operators' Association; and James Westfield, Federal Bureau of Mines.

Jan 1, 1960

By H. D. Hess

This report describes in detail a unique occurrence of fersmite, (Ca, Ce, Na) (Cb, Ti, Fe, Al)2 (0, OH, F)6, which occurs as small anhedral inclusions and intergrowths with a tantalum-free columbite found in the metamorphic complexes of Ravalli County, Mont. Chemical and crystallographic data along with the physical and optical properties agree in general with those given in the original description of fersmite from the Ural Mountains of Russia. X-ray diffraction data not given in the original description and more specific optical data have been determined. The Montana fersmite, now established as the second occurrence of this rare calcium-columbate mineral, was discovered during a routine Bureau of Mines mineralogical examination of a prospector's sample.

Jan 1, 1960

President W. K. Dennison, Jr., called the final session of the Rocky Mountain Coal Mining Institute to order, and introduced H. A. Cornell, Portland Cement Association, Ft. Collins, Colorado. Mr. Cornell explained that the Portland Cement Association was not a sales organization, but is supported by the major manufacturers of portland cement. The research laboratories of the association are constantly endeavoring to improve the quality of cement, as well as promote new markets, new uses, and new ideas. The association works with engineers, contractors and universities, making available to them the results of their research. Mr. Cornell stated that numerous booklets and bulletins were available on request for any phase of construction with concrete. Mr. Cornell presented a film, "How to Make Quality Concrete," to the members of the Institute. D. W. Lyke, General Electric Apparatus Service Shop, Denver, Colorado, was introduced by President Dennison, who presented a film, "A-Hunting He Would Go." Following the film, Mr. Lyke stated that his firm was not confined to electrical equipment, but to all types of equipment, and asked the members to feel free to call for assistance at any time. These two films concluded the Manufacturer's Hour, and President Dennison opened the final business meeting of the session. Robert F. Bowie, of the Auditing Committee, read the Treasurer's Report, and complimented Mr. Whiteside on the commendable state in which the books were found. The Treasurer's Report is as follows:

Jan 1, 1960

"M bed, Matanuska valley, Alaska, coal carbonizingproperties B 510M spectral lines, low-energy, study RI 5538Mab shaft, Leadvile district, Colo., investigation RI .1518Maberry process, for aluminum chloride TP 321"

Jan 1, 1960

By C. R. Ross

"THE ASSESSMENT of pneumoconiosis-producing dusts in mines and other industries is usually undertaken for one or more of three reasons: (1) To compare dust exposures at particular operations with standards of permissible dustiness in order that hazards may be evaluated and preventive procedures initiated where required.(2) To study particular operations with the objective of improving dust control devices or procedures by locating dust sources. (3) To obtain data which, along with the results of medical investigations, may assist in understanding the causes of dust-induced diseases or aid in the establishment of permissible standards of dustiness. Most dust measurements are made for the first of these reasons -to evaluate dust hazards so that they may be controlled. For this purpose, four quite different assessment techniques have been in widespread use for many years. One of these is based on the konimeter, an instrument familiar to most .Canadian mining men; a second on the impinger, which is also widely used in Canada, and almost exclusively so in the United States; a third on the thermal precipitator, used extensively in Britain and South Africa; and a fourth on the tyndallometer, a light-scattering instrument used in Germany."

Jan 1, 1960

By R. E. Reed, R. D. Leggett, Paxton, H. W.

TECHNIQUES have been developed for growing monocrystals and bicrystals of Fe-20 Cr, Fe-20 Cr-20 Ni, and Fe-18 Cr-8 Ni alloys by both the strain-anneal and the Bridgeman techniques. None of the techniques are new but since they are simple and many people have expressed interest, they are described here quantitatively as they could be modified for other single-phase "commercial" materials of high melting point. CRYSTAL GROWTH BY STRAIN ANNEAL Flat tensile specimens with a tapered gage length were initially studied to deduce the approximate critical strain. Normal flat tensile specimens were then used. The optimum procedure for the austenitic steels (Fe-Cr-Ni) deduced from a variety of cold reductions, recrystallization treatments, tensile strain, and growth anneals was as follows: cold reduce 70 pct, recrystallize (after machining tensile specimens) at 1000°C for 1 hr, strain in tension 2.5 pct, and then heat to 1350°C as rapidly as possible. A time of 100 hr at 1350°C is usually sufficient to pro-

Jan 1, 1960

By J. W. Rutter, K. T. Aust

The motion of individual grain boundaries under a constant driving force was investi,qated for zone-refined lead, with and without solute tin additions. The rate of boundary migration was found to depend strongly on tin content and on the orientation relationship between the adjacent grains. The results are compared with the theory of impurity-controlled grain boundary miqration developed by Lucke and Detert. Evidence was found that grain boundaries separating grains which have the Kronberg-U&apos;ilson orientation relationships of 38 and 22 deg about <Ill> and 28 deg about <100>, correspond to boundaries of high mobility. The results are discussed in relation to the formation of annealing textures in metals and the structure of high-angle boundaries. It is generally known that small amounts of impurities in solid solution greatly influence the re-crystallization behavior of metals. For example, the addition of 0.005 at. pct of tellurium to copper,&apos; or 0.005 at. pct of silver to lead,2or 0.01 at. pct of manganese or nickel to aluminum3 greatly decreases the rate of recrystallization of these metals. However, this effect may be the combined result of a decrease in the rates of both nucleation and growth; recrystallization experiments do not separate these two factors. Bolling and winegard4 determined the effects of small quantities of tin, silver, and gold on grain growth in polycrystalline zone-refined lead.

Jan 1, 1960

By R. O. Williams

A recent article by Chernock, Singer, Mueller, and Beck 1 which supports the use of the integral of I sin $ d$ for comparing fiber texture data does not settle what happens to I sin ø as ø approaches zero, where I is the diffraction intensity for poles oriented 0 deg from the fiber axis. They indicate that they believe that it should approach some constant value (that is, I increases without bound) and the fact that in reality it does not was a result of the diffraction

Jan 1, 1960

By W. J. Wenger

THIRTY-FOUR analyses of crude oils from the fields of the Four Corners Area of Arizona, Colorado, New Mexico, and Utah are presented and compared. The samples, taken from formations in four geological time periods, have high gravity and low-sulfur, -nitrogen, and -asphalt content. Generally, the oils are paraffinic in the low-boiling fractions, with increasing naphthenicity in the higher-boiling fractions. Oils from Cretaceous formations resemble other Cretaceous oils in the Rocky Mountains, but oils from Permian and Pennsylvania formations are unlike other oils of these ages in the Rooky Mountains. The differences in the oils are minor and cannot be used to distinguish between fields or between producing formations. With minimum special processing, the oils should yield large amounts of good-quality motor fuels. INTRODUCTION The only place in the United States where four States have a common junction is known as the Four Corners Area. This area (fig. 1) includes the northeast corner of Arizona, the southwest corner of Colorado, the northwest corner of New Mexico, and the southeast corner of Utah. It includes three major geological basins: The Black Mesa, the San Juan, and the Paradox. Major oil developments have occurred in both the San Juan and Paradox basins, but no discovery of commercial importance has been made in the Black Mesa basin.

Jan 1, 1960

By H. H. Heady

A naphtha obtained by destructive, recycle hydrogenation of crude shale oil, produced by gas-combustion retorting of Colorado oil shale, was found by the Bureau of Mines to contain 49.1 percent paraffins, 20.3 percent cycloparaffins, 7.8 percent olefins, and 22.8 percent aromatics. The naphtha contained only minor amounts of sulfur, nitrogen, and oxygen compounds. Compounds containing less than 5 carbon-atoms per molecule were removed by distillation before analysis. The paraffins where predominantly straight-chain compounds; n-Hexane was present in the largest quantity, and the other straight-chain paraffins decreased in amount as the molecular weight increased. The cycloparaffins, which contained both cyclopentanes and cyclohexanes, were evenly distributed throughout the boiling range. Although the naphtha had been produced by hydrogenation, it contained a small quantity of olefins. Straight-chain olefins with a terminal double bond comprised about two-thirds of these compounds. Among olefins with an internal double bond, those having trans configuration were present in three times the quantity of those in the cis form. In the aromatics all but one of the alkylbenzenes having nine or less carbon-atoms per molecule were identified; toluene was present in the greatest quantity. Only a few of the higher molecular-weight homologs were identified. The composition of the naphtha was computed from analyses of 105 narrow¬boiling distillation fractions. Volume, density, refractive indices, bromine number, and an ultraviolet spectrum were determined on each fraction. From these data the hydrocarbon-group composition of each fraction was estimated. A silica gel adsorption analysis was used to check the values of nearly one-third of the fraction calculated from physical-property data. Mass and infrared spectra were obtained on some fractions for identifying individual compounds or types of compounds, such as terminal olefins.

Jan 1, 1960