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By M. M. Gilkey

Pegmatites in Colorado occur for 150 miles along the Front Range (eastern-most range of the Rocky Mountains) from Larimer County on the north to Canon City on the south, and west into the Gunnison area. Many of the deposits have been classified. Minerals found in the various dikes include beryl, scrap and possibly punch mica, lithium-bearing minerals, columbite-tantalite, feldspar, and several rare minerals. Pegmatites are abundant in the Crystal Mountain district in Larimer County. About 5 miles south of the Crystal Mountain district and often identified with that district is the Hyatt pegmatite area. The Hyatt Ranch deposit has attracted particular attention because of the comparatively high beryl con-tent of the upper part exposed in opencut workings.

Jan 1, 1960

By James S. Browning

Heavy liquids have been used to separate minerals of different specific gravities for many years.4 5 6 7 8 9/ The method permits substantially quantitative evaluation of a variety of minerals and requires much less time than the usual methods of chemical analysis. This Bureau of Mines investigation was conducted to determine the applicability of heavy liquid mineral separation to the evaluation of certain spodumene and kyanite ores, prepared mixtures, and plant products. After careful standardization of the particular mineral and associated gangue, estimates of chemical analyses could be obtained from results of heavy liquid separations.

Jan 1, 1960

By Raymond O. Dannenberg

The gas-combustion retort developed by the Federal Bureau of Mines at the Rifle Oil Shale Project near Rifle, Colo., is a continuous, gravity-feed retort. The heat required to convert the kerogen in the oil shale to liquid oil is generated by the combustion of product gas and carbonaceous residue remaining on the retorted shale after the kerogen has been converted to oil, gas, and residue. A study of the effects of the process variables on retort operation, product yields, and product properties is important to the successful solution of the problems encountered in the development of a satisfactory process. Statistical methods were used to design the experiments and analyze the effects of the rate of shale throughput, the composition of dilution gas, the height of the shale bed above the air entry, air-gas distributor design, shale size range, and the ratios of the flow rates of the various gas streams entering the retort to the rate of shale throughput.

Jan 1, 1960

By D. E. Redmon

Exploration of hidden mineral deposits becomes increasingly important as known ore reserves are depleted. The primary objective in any exploratory program is to obtain enough reliable information to evaluate accurately the potential of the mineral deposit. Constant improvement in equipment and technique has established drilling as one of the most valuable methods of exploration. This paper presents the results of studies of several drilling methods currently used in the search for uranium deposits in sedimentary formations from surface drill sites. Also presented is a description of drilling with wire-line equipment from an underground location in metamorphic rocks. The studies were conducted in the Colorado Plateau area and in northwestern New Mexico and Wyoming. Statements of a general nature pertain to conditions or situations existent in those areas.

Jan 1, 1960

By D. C. Fleck

This report describes a method of using sodium for reducing titanium tetrachloride, developed at Boulder City, Nev., as part of the Federal Bureau of Mines effort to improve the extractive metallurgy of titanium. Finely divided titanium metal, titanium lower chlorides, or a mixture thereof was produced in a continuous operation at temperatures between 105° and 205° C. by the reaction of molten sodium and vaporized titanium tetra-chloride in an agitated bed of finely divided inert solids (powdered sodium chloride or the reaction products). Composition of the product was controlled by varying the relative quantities of sodium and titanium tetrachloride used. A description of the operations and analytical data of the reaction products are given.

Jan 1, 1960

By R. L. Montgomery

Heats of solution of yttrium chloride and oxide in hydrochloric acid were measured by Bureau of Mines researchers. Using the heat of combustion of yttrium mentioned in the literature, the Bureau calculated the heat of formation of yttrium chloride to be -239.16 + 0.50 kcal./mole. The Bureau experiments gave evidence that the heats of solution of yttrium chloride from the literature are mostly too low because of water and/or oxychloride impurities. Heat of combustion of yttrium (8)3/ and its heat of solution in hydrochloric acid (2, 14) have been measured. The earlier heat of solution measurement (2) is unreliable because of possible potassium contamination (4). Heat of solution of yttrium chloride has been measured by three researchers (3, 9, 15), who obtained widely different results. Spedding and Flynn (14) report the heat of formation of yttrium chloride as -232.69 kcal./mole from their solution studies. The present work was designed to check the reported heats of solution of yttrium chloride and to determine the heat of solution of yttrium oxide. The latter measurement would allow the results of solution and combustion data for yttrium to be intercompared.

Jan 1, 1960

By F. E. Block

This investigation was made as part of a larger program to develop basically new methods for preparing yttrium metal in high-purity form. It was performed under a cooperative agreement between the U.S. Atomic Energy Commission (AEC) and the Federal Bureau of Mines. Laboratory-scale tests were made to devise methods for preparing high-purity, anhydrous yttrium trichloride, for reducing the yttrium trichloride with sodium or lithium, and for consolidating the resulting yttrium sponge into ingots.

Jan 1, 1960

By C. M. McKinney

Bureau of Mines routine crude-oil analyses of 42 samples from 37 fields in the major producing areas in Mexico are presented in this report. Table 1 includes information on the source and general characteristics of each sample. Table 2 gives a summary of analytical and computed data. A map (fig. 1) shows approximately where the samples were obtained. ACKNOWLEDGMENTS Grateful acknowledgment is made to Alfonso Barnetche, manager of production, and Ing. Francisco Inguanzo, assistant manager of production, both of Petroleos Mexicanos, who supplied the crude-oil samples and furnished information concerning their sources.

Jan 1, 1960

By G. M. Carr-Harris

"THE SUBJECT of permanent molding has received a great deal of attention in the technical press as illustrated by the many excellent articles in the bibliography which follows. In general, this covers the period 1940-1958 and is merely representative of what is available. Numbers in •brackets refer to items in the bibliography.It may be desirable at the outset to give a few definitions covering those terms directly related to this subject. The following is a definition of permanent-mold casting as given by J. W. Meier in a paper, ""The Non-Ferrous Metals and Alloys"", read before the Ottawa Valley Chapt.er of the American Society for Metals:""Permanent Mold Casting is used where a large number of castings of the same part are required and higher mechanical properties, greater density and closer tolerances are essential. Since metallic mold s are very expensive, the number of castings must be sufficient to, defray, at least partially, the added expense. Molds are usually made from a good quality cast iron, 1but other mold materials, such as the aluminum and copper alloys, graphite, ceramics, etc., are being used in certain cases. Important factors in permanent mold casting are the mold temperature; the proper mold dressing; and, as in all other casting methods, the mold geometry, that is to say, the design of spruces, gates, risers and vents""."

Jan 1, 1960

By R. A. Hemstock

"Simple classification systems are now being used which will describe adequately the surface vegetation, the topography and the peat for any muskeg condition. Good progress is being made in determining some of the mechanical properties of muskeg and it is apparent that the science of soil mechanics will apply largely to these studies. Correlation is also indicated between shear strength as determined by the shear vane tester and vehicle performance. Several tracked vehicles are now available which perform well in muskeg and advances in this field have come rapidly in the past few years. Testing is under way on the largest of all muskeg vehicles -the thirty-five ton Musk Ox. This vehicle will fill the last gap for the oil industry and will make possible the movement of large drilling rigs at any season of the year."

Jan 1, 1960

By P. Chiotti, G. R. Kilp

Thermal, metallographic, vapor pressure, and X-ray data were obtained to establish the phase diagram for the zinc-zzrconiz~m system. Five compounds corresponding to the stoi-chiometric formulas ZrZn, ZrZn,, ZrZn,, ZrZn,, and ZrZn14 were observed. All these compounds, with the exception of ZrZn2, which melts congruently at 1180°C under constrained zinc-vapor conditions, undergo pexitectic reactians. The temperature at which the zinc vapor pressure is I atm for a series of alloys was determined from vapor-pressure measurements. The data obtained are summarized in the construction of a I-atm-pressure phase diagram and a phase diagram corresponding to a pressure of less than 10 atm. THE purpose of this investigation was to establish the phase diagram for the zinc-zirconium system. Thermal, metallographic, vapor pressure, and X-ray data were employed in determining the phase regions. Partial investigations of this system have been conducted by Gebhardt1 and Carlson and Borders.' Carlson and Borders studied the high-zirconium region and established the existence of a eutectic at 69 wt pct Zr with a melting point of 1015°C. The terminal phases of the eutectic horizontal were shown to be an intermetallic compound ZrZn and a solid solution of ß zirconium containing 21 wt pct Zn. The ß solid solution decomposes into ZrZn and a zirconium at 750°C. The eutectoid composition is given as 15 wt pct Zn, and the solubility of zinc in a zirconium at temperatures below 750°C is indicated to be negligible. Gebhardt studied the zinc-rich region and observed a lowering of the melting point of zinc from 419.5" to 416°C and temperature horizontals at 545" and970°C. Some preliminary observations by Chiotti, Ratliff, and Kilp were reported by Hayes.2 pietrokowsky3 has reported the compound ZrZn2 to have a cubic MgCu2 structure with ao = 7.396A. MATERIALS AND EXPERIMENTAL PROCEDURES The metals employed in the preparation of alloys were Bunker Hill slab zinc or Baker analyzed reagent granulated zinc, both 99.99 pct pure and hafnium-free iodide-process crystal bar zirconium obtained from the Westinghouse Electric Corp. The zirconium contained 200 ppm Fe, 200 ppm Si, 100 ppm C, and minor amounts of other impurities. The zirconium was milled or machined into thin chips or shavings. These were cleaned with a nitric-hydrofluoric acid solution, rinsed with water, and acetone, and dried just prior to their use in alloy preparation. The granulated zinc was similarly cleaned using dilute nitric or hydrochloric acid. Weighed quantities of these materials, 20 to 30 g total, were mixed and pressed at 20,000 to 70,000 psi to give relatively dense compacts. During the early part of this investigation the pressed compacts were placed in MgO-15 wt pct MgF, crucibles which were then sealed inside of quartz ampules. The compacts were given various prolonged heat treatments prior to their use for thermal analyses, or vapor-pressure measurements. Because of expansion of the compacts and the relatively high zinc vapor pressure it was difficult to heat to the melting temperatures of the alloys without failure of the quartz ampules. Homogenization at temperatures below the melting temperature gave brittle, porous alloys unsuitable for metallographic examination. It was also difficult to prevent condensation and segregation of zinc on the colder parts of the quartz ampules during heating and cooling operations. These problems were eliminated to a great extent by the use of tantalum crucibles. Tantalum proved to be a satisfactory container with little or no reaction between the alloys and the tantalum. Small tantalum thermocouple wells were successfully welded in the bottom of these crucibles. Pressed compacts were sealed inside the tantalum crucibles by welding on preformed caps under an argon atmosphere. Heat treating and differential thermal analysis were combined into a single operation. The experimental sample assembly is shown in Fig. 1. This assembly was enclosed inside a stainless-steel tube heating chamber which could be evacuated and filled with an inert gas. The thermocouple leads were brought out of the heating chamber between two rubber gaskets used to provide a vacuum seal for the water-cooled head. Most of the compounds in this system undergo peritectic decomposition. After heating above the temperature of a particular peritectic horizontal the sample was cooled to just below the peritectic temperature and held at temperature for several hours. The sample was then reheated through the peritectic temperature and the size of the thermal arrest, if still present, compared with the one previously obtained. If the thermal arrest was not characteristic for the alloy composition being investigated its magnitude diminished and repeated cycling and annealing eventually eliminated it. The peritectic thermal arrests characteristic of a particular composition were established in this manner.

Jan 1, 1960

By R. D. Pehlke, J. F. Elliott

The equilibrium pressure of nitrogen gas over pure silicon metal and silicon nitride has been measured in the temperature range 1400° to 1700°C. From the experimental data, the standard free energies and enthalpies of formation of Si3N4(a) have been calculated as functions of temperature over the above temperature range. Utilizing data in the literature and the results of this investigation, the specific heat, molar enthalpy, molar entropy, standard enthalpy of fornation, and standard free energy of fornation are estimated for the temperature range 298° to 1400°C. THE high-temperature thermodynamic properties of many metallic nitrides are not well established at present. This is a serious deficiency because nitrogen and nitride-forming metals are important alloying additions to steels, and knowledge of the interaction between nitrogen and these elements is essential to a better understanding of the behavior of steels. Metallic nitrides also are used as refractory materials. Consequently, the investigation reported here was undertaken to provide more complete information on the standard entropy and free energy of formation of silicon nitride. The experimental technique provided a direct measurement of the equilibrium pressure of nitrogen gas in the range of 1413 to 1700°C for the reaction: 3 Si(1) + 2N2 (g) = Si3N4 (a) [ 1 ] and below 1413oC for the reaction: 3Si(c) + 2N2(g) = Si3N4(a) [2] APPARATUS The experimental system consisted of a crucible assembly, a reaction chamber, and a gas supply and vacuum system. The Crucible Assembly which contained the equilibration specimen and molybdenum radiation shields with a susceptor for induction heating is shown in Fig. 1. Two covered, high-purity alumina crucibles, one nested within the other, contained the susceptor, shields and specimen. Central openings in the upper shield and crucible covers permitted on optical pyrometer to be sighted into the central cavity of the specimen. The specimen itself was a 5/8 OD by 1-in.

Jan 1, 1960

By J. S. Berber

Bastnasite is a natural fluocarbonate of the cerium group and affords an abundant and high-grade source of the lighter rare-earth elements. As part of a broad research program in rare-earth element technology, the Federal Bureau of Mines directed extensive experimental work to separating and purifying the rare-earth elements in bastnasite. By the use of a combination of techniques--classical chemical, ion exchange, and solvent extraction--the processing of a bastnasite concentrate to obtain the individual rare-earth elements, or groups of elements, was accomplished. A bastnasite concentrate, containing about 60 percent rare-earth oxides, was sulfated with concentrated sulfuric acid to eliminate the carbon dioxide, fluorine, and silica. Calcination at 1,200° F. made the gangue matter insoluble, thus permitting the separation of the soluble rare-earth sulfates. Essentially 100 percent of the rare-earth elements were recovered by this procedure. Since the rare-earth sulfate solution contained only trace amounts of nonrare-earth elements, subsequent separation procedures were simplified.

Jan 1, 1960

By D. W. Frommer

Mineral dressing research was conducted by the Federal Bureau of Mines under a cooperative agreement with the St. Joseph Lead Co., on three samples of iron ore from the Pea Ridge deposit in central Missouri. The objective was to provide information on how to upgrade these submarginal ores and produce marketable concentrates. Samples were prepared from drill-hole cores of similar composition and character to produce (1) a medium-grade mixed hematite and magnetite, (2) a high-grade mixed hematite and magnetite, and (3) a high-grade magnetite. In all three ores phosphorus and sulfur constituted objectionable impurities; excessive amounts of silica were also present in the medium-grade ore.

Jan 1, 1960

By R. L. Stanton

"The present contribution is complementary with a preceding one on the field association of the conform-able ""pyritic"" deposits. It considers the more important features of their mineralogical constitution and their microtextures, re-examines the present interpretations of these, and of-fer-some alternative explanations. The term ""pyritic"" for these de-posits is m many cases a misnomer, as two quite distinct ore types are inuolve. One is a banded pyritic sphalerite-galena-chalcopyrite ore (for which the term '•pyritic"" is in-deed quite suitable), while the other is non-banded and is composed essentially of pyrrhotite and chalcopyrite. In addition to these constitutional differences, each is distinctive in general appearance and texture. The occurrence of two such consistent but clearly distinguishable ore types is attributed -rather than to difference in source material and pressure-temperature conditions of deposition -to the contribution of similar source material to dissimilarly oxygenated environments of sedimentation. Textures in the banded ores generally thought to be indicative of replacement or of high-temperature exsolution are explained by slow, law-temperature segregation in situ during compaction, folding, and regional metamorphism."

Jan 1, 1960

By Leonard Obert

THIS REPORT presents methods and principles useful in designing underground mine openings and pillars in competent rock formations. Two types of formations are considered: (1) Massive formations, in which openings are generally mined with an arched roof, and (2) bedded formations, in which openings are generally mined with a flat roof. Design principles for openings and pillars in massive formations are obtained by considering the maximum tangential stresses developed around single and multiple openings for stress fields of various types. Design principles for openings and pillars in bedded formations are obtained by considering the average stress in pillars and the maximum stresses in roof layers. Experimental procedures for making stress, strain, and in situ physical-property measurements in underground mines to check design calculations are outlined and the results discussed.

Jan 1, 1960

By T. Fekete, D. L. Flocks, R. T. Hart

The plugging effect of bacteria was investigated by injecting various concentrations of dead bacteria cells though sandstone cores. Pressure profiles along the cores were recorded periodically during the injection cycles. The plugging effect was analyzed using a plot of the ratio of reduced permeabilities to the initial permeability versus input volume. Results indicated that Tock permeability has little effect on plugging, but that the concentration of bacteria in the injection water has a significant effect on plugging characteristics. The pressure profile curves showed that bacteria penetrated several inches through the core but that the greater portion of the bacteria accumulated at the in-put end of the core.

Jan 1, 1960

By G. H. Agnew

When water floods are initiated after gas-oil ratios have increased, the transition period from the start of injection until" the gas-oil ratios are returned to the solution gas-oil ratio may be important for either economic or technical reasons. The transition period is longest, and consequently most critical in water floods where injection is equal to withdrawals. This paper describes a theoretical basis for predicting the behavior of such a system and outlines a procedure for making the necessary calculations. The calculation procedure is illustrated for two actual cases: a line drive water flood and a five spot water flood. In each case there is a reasonable similarity between the actual and calculated performance.

Jan 1, 1960

By T. C. Atchison, W. I. Duvall

Over the past ten years a series of investigations have been conducted to determine some of the pnysical processes involved in breaking rock with confined concentrated charges. Detailed discussions of many of these investigations have been published elsewhere.1-6 Laboratory experiments made by other investigators using Hopkinson pressure-bar techniques have shown that solid materials are fractured in tension by the reflection of an incident compressive stress pulse at a free surface.7-12 In these tests a small charge of explosive is placed in contact with one end of a bar. Detonation produces some plastic flow and crushing of the bar near the charge and generates a compressive stress pulse that travels along the length of the bar. At the free end of the bar the compressive stress pulse is reflected back into the bar as a tensile stress pulse. If the tensile strength of the bar is exceeded during this reflection process, a tensile fracture normal to the length of the bar is produced, and the broken end of the bar moves forward with a constant velocity equal to the average particle velocity trapped in the broken fragment. The new surface formed by the fracture becomes the new free end of the bar that reflects the remaining portion of the incident compressive stress pulse. This process is repeated any number of times until all of the incident stress pulse is reflected. Hino has demonstrated this kind of breakage for three rock types—marble, granite, and sandstone." He has defined a blastibility coefficient, B, as the ratio of compressive strength, C, to tensile strength, T, thus: C The quantity B is the maximum number of slabs that can be produced by reflection breakage. Normally fewer slabs are produced because of loss of energy as the stress pulse travels through the rock. Fig. 1 illustrates reflection-type fracture for a triangular compressive stress pulse. The number of slabs produced by the reflection breakage process is the first whole number less than the ratio of the peak stress of the incident pulse to the tensile breaking stress of the solid. Thus the number of slabs is given by the thickness of each slab is given by and the total length of rock broken is given by N = number of slabs S - peak stress in incident pulse T = tensile strength of the rock F = fall length of incident stress pulse h = thickness of each slab D = total length of rock broken During the reflection process the particle velocity at the free surface is twice the particle velocity in the incident stress pulse. Thus the velocity with which the broken fragments move forward is given by where v, = velocity of broken fragment, and v = average particle velocity contained in that portion of the incident pulse trapped in the broken fragment. Results of these laboratory experiments cannot be applied directly to rock blasting where the explosive charge is placed in a drillhole. In laboratory tests the charge is unconfined and in contact with the rock in only one direction. In a drillhole additional confinement is offered by the rock surrounding the charge and by the stemming placed above it. This additional confinement may be enough to allow the explosive gases to do additional work on the rock during their expansion. Other writers have discussed possible effects of gas expansion'on rock breakage.13-10 However, very few experimental data are available to determine to what extent expansion of the gases is responsible for rock fragmentation. The USBM has studied the physical processes involved in breaking rock with confined concentrated charges by using simple crater tests breaking to one free surface. Crater tests have been performed in four rock types: granite, sandstone, marlstone, and chalk. Table I gives some physical properties of these rocks. Fig. 2 shows plan and section drawings of two typical crater tests and illustrates some of the test variables measured. For these tests the charge was placed at the bottom of the drillhole and primed with an electric cap. The hole was stemmed to the collar with sand and the charge detonated. Size and shape of the crater were measured after it was cleared of broken rock. As a given charge size was buried deeper in a drillhole, the crater depth usually was equal to or

Jan 1, 1960

By R. Hendricks

"IT IS a pleasure for me to appear before yon today and to have this opportunity of reviewing with you recent developments in the world lead and zinc industry. To provide essential background material, I propose reviewing the period from 1950 to the present, a period which has undoubtedly been the most hectic in the long history of the industry.In capsule form, the pattern for this period is one of repeating cycles of boom and recession, of failure through research to develop adequately new markets and new uses for lead and zinc, of surplus production and growing inventories, of price instability, and lastly, of an abdication in some sections of the industry of responsibility for control of its own destiny by turning to governments for support in time of stress. This is not a pretty picture but, as the 1950 decade ends, there are signs of a new maturity and of a growing determination on the part of the industry to put its own house in order.The difficulty suffered by the world's lead and zinc industry in the current decade originated with the support extended to it in 1950 by the U.S. Government at the time of the Korean conflict. Recalling the shortage of base metals in World War II and fearing that the Korean conflict might develop into World War III, the U.S. Government in 1950 adopted a policy to encourage the production of lead and zinc, both domestically and abroad by means of development loans and long-term floor priced purclu.se contracts."

Jan 1, 1960