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By J. H. Field

Synthesis of hydrocarbons by the Fischer-Tropsch reaction in a hot-gas- recycle system was demonstrated to be technically feasible. This project was undertaken, by the Bureau of Mines, to determine if the system was operable and to ascertain the optimum conditions for the production of gasoline. Carbon steel turnings packed with a void volume from 88 to 90 pct. were satisfactory catalysts, but steel catalysts with greater void volume, either turnings or steel wool, were not as active. Good temperature control with a pressure drop of less than 0.5 pounds per square inch (p.s,i,) per foot of catalyst bed of turnings was obtained by operating with a recycle to fresh feed ratio of 20 and by splitting the total gas flaw and injecting portions into the reactor at different entry ports.

Jan 1, 1961

By A. E. Bibb, F. W. Kunz

A platelet form of zirconium hydride was found in zirconium and ZY-1 wt pct U single crystals containing hydvogen in the range of 50 to 100 ppm. The habit planes for the hydride plateletg in the zirconium crystals were found to be {1012}, {1121}, and (1122) while the habit planes in the ZY-1 wt pct U crystals were {1121), {1123}, and (1.231). With the exception of the {1231} plane, these have been identified as the twin planes in zirconium. The different effect of hydridc on the mechanical puoperlies of zirconium at high and low strain rates has been explained in terms of the defornzation mechanism and the habit planes of the hydride. ZIRCONIUM and zirconium-base alloys are considered for many nuclear reactor applications, where the pick-up of hydrogen is a distinct possibility, if not an unavoidable occurrence. An excellent example of this is the absorption of hydrogen by zirconium and its alloys during aqueous corrosion, where as much as 30 pct of the hydrogen produced by the corrosion reaction is picked up by the metal. Under the proper conditions, the absorbed hydrogen would precipitate as zirconium hydride and consequently alter the mechanical and physical properties of the zirconium-base alloys. The knowledge obtained from a study of the crystallographic aspects of the hydride precipitation is necessary for the interpretation of the observed changes in the mechanical and physical properties. The deleterious effect of hydrogen on zirconium-base materials is not always observed in normal slow tensile loadings at or above room temperature, but becomes immediately obvious under impact loading, where the energy absorbed decreases with increasing hydrogen content,' and in notched specimens where triaxial loadings are attained.2 This effect is of serious consequence in the applications of Zr where shock loads or high strain rates are experienced. The purpose of this investigation was to determine the crystallographic planes of the Zr and Zr-1 wt pct U matrices upon which zirconium hydride will precipitate and to correlate these with the observed mechanical property data. PROCEDURE Crystal Growth—Single crystals of Zr and Zr-1 wt pct U alloy were used in this investigation. The Zr crystals were made from sponge that had a typical analysis as shown in Table I. Large grains were grown in this material by rapid cooling an arc-melted charge in a button furnace. This operation undoubtedly lowered the volatile impurity concentration below those listed in Table I. Back-reflection Laue patterns of these large grains showed the presence of considerable substructure and lattice distortion within each grain. It was found that an 18-day anneal in an argon atmosphere at 840°C (a high a heat-treatment) followed by furnace cooling, resulted in the further growth of the large grains and removed the detectable substructure ana lattice distortion. Equiaxed crystals with a cube edge of approximately 1/4 in. were produced in this manner. Large crystals of Zircaloy-2 (1.5 wt pct Sn, 0.15 wt pct Fe, 0.1 wt pct Cr, 0.05 wt pct Ni) also were produced by this technique but the large amount of substructure formed could not be removed by annealing. The Zr-1 wt pct U solid solution crystals were produced from an alloy rod consisting of Westing-house-Foote hafnium-free crystal bar zirconium and depleted uranium. The chemical analysis of the alloy is also given in Table I. Three-inch sections were cut from an 0.120-in.-diameter alloy rod and tapered to a fine point on each end. The samples were sealed in evacuated Vycor tubes, homogenized for 5 hr at 1000°C in the ß-phase field, and slowly lowered in a gradient furnace into the a phase (800°C), annealed for 60 hr at this temperature to produce grain growth and furnace cooled. This technique produced large grains approximately 1/2 to 3/4 in. long over the entire cross section of the rod, which were free of observable substructure. Metallographic examination up to X1000 did not show the existence of any second phase in these grains. Crystal Orientation—All crystals were abraded on fine emery paper to produce two flat surfaces 90 deg to each other. The crystals were analyzed by the standard Back-Reflection Laue technique to obtain the crystal orientation with respect to the abraded surfaces. The Back-Reflection Laue Photograms of all crystals used were clear and sharp indicating that the crystals were free from any substructure that could be detected by these means. Hydriding—Only samples containing four to five grains were used for hydriding. Samples that exhibited fine grained patches were discarded. The samples were hydrided using the following technique. After etching in 48 vol. pct HNO3, 48 vol. pct H2O, and 4 vol. pct HF (48 pct) solution, the specimens

Jan 1, 1961

By Greaves M. C, Amos M. D

A study was made of the instrumentation and technique of atomic absorption spectroscopy developed by Walsh of the Commonwealth Scientific and Industrial Research Organisation (C.S.I.R.O.), Australia.The method was evaluated for the determination of silver in lead sulphide concentrate. The precision of the procedure developed is equal to that of the uncorrected fire assay method and the accuracy is greater.Brief mention is made of the use of this technique for the determination of silver and other elements in ores and concentrator products.INTRODUCTIONThe fire assay method, although accepted on a world-wide basis as the umpire method for the determination of silver in ores and concentrates, is freely recognized as yielding results which are lower than actual due to unavoidable losses.King (1934) investigated the influence of the cupelshape, size and material on silver losses during cupellation. Using 100 mg silver prills he recorded silver losses ranging between l. and 10 per cent under extreme conditions and averaging approximately 2 percent under conditions which might be considered normal. Guerin (1957) made a detailed study, under carefully controlled conditions in a furnace similar to that described by Esdaile (1952), of the effect of temperature on silver losses during cupellation. He concluded that if cupellation were carried out at 840°C., then the amount of lead retained by the silver prill was insignificant and that the silver losses were governed by the equation: Y = 0·055 XO.74where X = the final weight of the silver priIl (mg)and Y = the silver lost (mg)

Jan 1, 1961

By Perry G. Cotter

The borides of the transition metals in Groups IV and VI exhibit, in addition to a certain degree of hardness, considerable resistance to heat and oxidation. They have high melting points (1,850°-3,060° C.) and low coefftcients of thermal expansion and can be bonded with other materials and hot-pressed to desired shape (cermets). Suggested uses for the borides include use in rockets and jet engines, as thermocouple protection tubes, as containers for molten metals in die casting, as flame-plated coatings on less refractory compositions to prevent erosion by hot gases, and as control rods and neutron shielding material in nuclear engineering, The Federal Bureau of Mines investigation of zirconium diboride started in 1950 at the Boulder City Nev,, Metallurgy Research Laboratory, Its purpose was to reduce the cost of raw materials for the production of zirconium diboride.

Jan 1, 1961

In general, the metallurgical industry has so far been slower than the chemical industry to adopt ion exchange materials for industrial processes. The atomic energy industry presents a marked exception to this general situation, and the literature shows a rapidly increasing use of ion exchange techniques for the recovery of atomic energy metals on scales ranging from the ultra micro up to that of the largest mining operations. In many cases, the processes used would be equally applicable to more common metals and it is hoped that this review will be of interest to metallurgists outside the specialised atomic energy field. The review is intended to describe developments of ion exchange processes made during the last three years. Earlier studies have been summarised by Kunin and Preuss (1956) and Roland (1957). In order to restrict the number of references discussed, purely analytical procedures have been omitted and only those processes which have been conducted on a reasonably large scale or which, from their nature, areclearly capable of being upscaled, have been considered. The paper is divided into five main sections concerning respectively:Water treatment and effluent disposal.Metal recovery and purification.New ion exchange materials.New ion exchange equipment.Membrane cells.WATER TREATMENT AND EFFLUENT DISPOSALA high proportion of atomic reactors, and particularly those of American design, are cooled by water which is...

Jan 1, 1961

By Fred C. Bond

The perennial subject of comminution is deserving of a fresh approach if one can be found. This is attempted here by directing attention primarily to principles rather than to theories. While theories attempt to explain how a certain process acts, principles delineate the laws which the action-must follow. Comminution may be defined as the progressive separation of particulate matter. At the present time this is accomplished commercially by applying energy in the form of compressive and, shearing forces. Such forces strain and distort the particles they contact. When-the applied stress locally exceeds the breaking strength at the weakest flaw in the particle, a crack tip forms. The surrounding strain energy flows to the crack tip, which rapidly extends through the particle as a break. The minute changes in shape and the resulting energy flow cause the failure of other highly stressed flaws, with the consequent formation of a progeny (1) of new smaller particles out of its destroyed progenitor. The applied mechanical energy is transformed into strain energy as the particle is distorted, and then into heat when it fails. Only a tiny fraction of the order of 1/1000 of the applied energy necessary for breakage appears as new surface energy in the product particles. The comminution problem is the relationship between, energy input and product particle size. Its solution is of great-economic importance,

Jan 1, 1961

By R. W. Van Dolah

An important function of stemming used to confine explosives in shot holes in underground coal mines is to minimize the chance of ignition of firedamp or coal dust by the detonation products. Until 1952, the Bureau of Mines approved only the use of fireclay or similar incombustible material for stemming permissible explosives. At least 2 feet of stemming were required except in holes less than 4 feet deep; in such short holes the stemming was required to be half the depth of the hole. Over the years, several special stemming devices have been proposed in the United States as substitutes for fireclay. Many economic and safety advantages were claimed for these devices, but only one approved device has been marketed in this country. Bureau requirements for stemming explosives in coal mines were modified at that time to permit the approved stemming device to be used as a substitute for the required fireclay.

Jan 1, 1961

By Ruth F. Brinkley

This report is the 18th of a series of reports originally issued annually, and more recently bienially, to acquaint the public with the work of the Federal Bureau of Mines in explosives technology. Part I reviews briefly the overall activities during fiscal years 1957 and 1958.4/ Part II presents in abstract form the publications prepared by the Bureau that appeared during the period.5/

Jan 1, 1961

By Max J. Spendlove

The secondary copper industry is comprised of numerous enterprises which collectively employ many of the recovery and refining processes now used in primary plants as well as many other processes that are unique to the industry. Effective methods are used for identifying and segregating all types of scrap according to widely accepted standard classifications. Segregated scrap and waste materials usually require some preliminary processing to remove both valuable and deleterious associated constituents. Smelting, melting, alloying, and pyrorefining are common methods used for producing secondary metal, but operating techniques usually differ from primary metal operations because of the difference in physical and chemical properties of the respective raw materials. Some copper scrap is converted to copper chemicals rather than to refined metals or alloys. Recovery efficiencies of all processes are reasonably high, and the quality of products meets rigid specifications.

Jan 1, 1961

By Kenneth H. Johnston

Records show that waterflooding was tried in Osage County as early as 1934, but it was not economically important until a large unitized flood in the North Burbank field was begun in 1950. Development was rapid and by the end of 1960, there were 70 active water flood projects and 16 active pressure-maintenance projects in the County. The locations and status of the water-flood and pressure-maintenance projects in Osage County on December 31, 1960 are shown in figure 1, and information pertaining to these projects as of July 1, 1960 is given in table 1. For the past several years, Bureau of Mines petroleum engineers have arranged tours of selected waterflooding projects for the spring meeting of the Kansas-Oklahoma Water flood Association. These tours are conducted to demonstrate unique operating methods and new field equipment and to provide additional opportunities for exchanging information. Each of these tours has been supplemented by a published report describing in detail the projects visited. This report has been prepared for distribution during the 1961 spring tour of three waterflooding projects and a pressure-maintenance project in Osage County, Okla. (fig. 2).

Jan 1, 1961

By E. H. T. Whitten

Fundamental principles of trend surface analysis are briefly reviewed. Recent analyses of several granite masses illustrate the method of estimating the quantitative regional composition and also variation trends. Mineralogi-cal, bulk chemical, and other quantitative variates can be employed. Such results should improve gravimetric surveys (etc.) relying on correction terms based upon estimated rock composition. For the first time realistic estimates of the mean composition of rock bodies can be made with the aid of trend components. Deviation maps hold promise for delimitation of disseminated mineralized areas. Deviations comprise residual "anomalies" after removal of trend components. In petrogenetic work such deviations have been shown to reflect local influences (e.g., contamination of magma by assimilation of xenoliths or country rocks of the envelope). Similarly, mineralization should be reflected as deviations standing out from background trends. Actual examples are given. Present results largely involved projection of data onto a horizontal plane, but if sufficient data are available use of three spatial coordinates increases accuracy for prediction in "unexposed" areas. Regression analysis shows that statistical correlations between variates for regionally distributed specimens are often strong (particularly with percentage data). Hence, in preliminary surveys more easily determined variates may sometimes be employed to gain first estimates of the distribution of components more economically significant. The sampling plan is of paramount importance. Unless a suitable sampling plan is devised and adhered to rigorously during collection of the samples, all subsequent analysis is liable to strong bias and to yield spurious estimates of the truth. For a wide variety of purposes it is becoming necessary to assess the quantitative composition and variability of rock masses and mineralized zones of various types. In petrology and petrography this is something of a break with tradition, because virtually all descriptions heretofore have been qualitative. Although vast amounts of qualitative data have been compiled, little is known about the quantitative behavior of rock components. However, if variability of rocks could be understood and expressed with sufficient accuracy, there would be considerable advantage to both economic and petrogenetic problems. For example, if, on the basis of a limited series of observations, the three-dimensional geometry of a disseminated orebody (or ore-bearing formation) could be predicted accurately, it would be possible to extrapolate with confidence the structure into unexposed areas. The following example based upon the geometry of an igneous cone sheet illustrates the point. The significant rock-unit gives outcrops at a number of points on the exposed surface ABCD (Fig. 1A). Study of n exposures may enable a geologist to predict that the rock-unit is circular in form and thus indicate where the unit can be expected in unexposed terrain. Such observations are made at sites with u, v coordinates, but, if subsurface information is available at sites with uvw coordinates, it will eventually become possible to predict accurately the three-dimensional form of the rock mass. Geologic rock masses or mineral deposits are not generally as regular and symmetrical in geometric form as the body illustrated in Fig. 1A. However, even where the broad limits of a major rock mass are known, a more acute problem arises in attempting to obtain detailed quantitative estimates of its internal variability; it is difficult to predict the variability of a mass from a limited number of observa-

Jan 1, 1961

By K. K. Kershner

This report describes an investigation by the Bureau of Mines designed to provide background data for extending and improving the applications of chlorine metallurgy in extracting metals from ores. Optimum conditions are given tor chloridizing galena, sphalerite, and chalcocite by contact with chlorine gas. Petrographic and chemical analyses of the sulfides used in the experiments are listed. Graphs are furnished showing the extent of chloridization of each metal sulfide over the temperature range of the observations. In each case, the first tests were made with the reaction chamber at room temperature. This temperature was increased by regular increments in succeeding tests until the temperature was reached at which quantitative conversion of the sulfide to chloride was observed. The data are also plotted for screen-size fractions of the sulfide minerals investigated. Data show that the extent of metal chloride formation was affected by chloridization time, particle size of the sample, and usually, the temperature of the reaction chamber. At 300° to 400° C. an anomaly was noted for both galena and sphalerite. The temperature at which this anomaly was observed varied according to the particle size of the mineral. Comparisons are made between the chloridizing characteristics of the mineral sulfides and their chemically prepared counterparts.

Jan 1, 1961

Drill cores from Section 62, New Broken Hill Consolidated Ltd., were used to study the petrology of rocks associated with the zinc lode. The distribution of the rock types in relation to the lode structure was determined. The distribution of the gahnite-bearing rocks was shown to be only partly conformable with the structure.It was concluded that large scale metasomatism was not widespread, that the rocks associated with the lode (except, perhaps, the quartz-gahnite-garnet rocks) were formed by metamorphism of sediments, and that rocks and lode were contemporaneously metamorphosed.INTRODUCTIONThis investigation was undertaken in order to study the rock types associated with the zinc lode of the Broken Hill orebody, and their relationship to the structure of the ore horizons. The work was confined almost entirely to the laboratory, and is therefore limited in its scope. It is hoped, however, that the information gained may throw some new light on the genesis of the lode.Certain inferences which are drawn from this work are at variance with the ideas of a number of earlier workers.In particular, the idea of large scale metasomatism developing many of the rocks associated with the lode, especially those containing manganese, is questioned. On the contrary, the rocks associated with the lode are more simply explained as highly metamorphosed sediments, in some cases modified by water introduced from surrounding rocks into zones of strong folding and faulting. As a corollary, a metamorphicsedimentary origin for the lode material, either as a concentrated sulphide deposit, or somewhat disseminated...

Jan 1, 1961

By G. V. Sullivan

This report summarizes the results of metallurgical investigations by the Federal Bureau of Mines of manganese oxide ore, averaging 23 to 25 percent manganese, stockpiled at the Butte-Philipsburg depot of General Services Administration (GSA). The oxide ores were stockpiled in two general classifications, straight oxide ore and mixed oxide-carbonate ore. Continuous-circuit flotation tests at the Albany (Oreg.) Metallurgy Research Center of the Bureau of Mines showed that each of these ore types could be concentrated by an oil-emulsion scheme to produce a concentrate that could be sintered to meet program specifications. About 88 percent of the manganese was recovered in the concentrate from the straight oxide sample, with the sintered concentrate containing 48 percent Mn. The sintered concentrate from the mixed oxide-carbonate sample contained 41 percent Mn with a recovery in the concentrate of 95 percent.

Jan 1, 1961

By R. F. Mehl

Jan 1, 1961

By M. E. Tyrrell

Despits its high melting point (2,135° C.), resistance to attack by molten metals, and its hardness (8), spinel (MgO?Al203) synthesized by the fusion of alumina (Al 2 0.) and magnesia (MgO) is not used on a large scale as a commercial furnace lining, mainly because of the prohibitive cost. This investigation by the Federal Bureau of Mines was prompted by the possibility of producing synthetic spinel from inexpensive raw materials by methods outlined in U.S. Patent 2,029,773, "Process for Obtaining Products Containing Spinets," dated February 4, 1936. In this patent Ture B. Haglund described a process for recovering crystalline spinels from melts in the system Mg0?Al203-2CaO-SiO2, a system well suited to the use of starting materials such as dolomite CaMg(C03)2, olivine [2(Mg?Fe)0.Si02], and bauxite (Al203?2H20) which are abundant in the southeastern United States. Compositions, ranging from a low content in the eutectic mixture of 35 percent spinal and 65 percent dicalcium silicate (2 CaO?SiO2) to a high of 75 percent spinel and 25 percent dicalcium silicate, were fused in electric furnaces of the arc-resistance and internal-resistance types. So long as members of the system were in proper chemical balance, "dusting" slags could be produced over the entire range of spinel concentration.

Jan 1, 1961

By A. A. Bauer

The ?-to-? transformation has been studied in zirconium alloys containing 22 to 70 wt pct U. In this range of compositions the ? phase can be retained by quenching. Transformation to ? occurs by a nucleation-and-growth process. The diffusion of atoms to preferred lattice sites to yield a partially ordered structure apparently controls the rate of reaction. Alpha uranium and a zirconium precipitate from the supersaturated E phase initially formed in alloys outside the equilibrium E phase composition limits. ZIRCONIUM-Uranium alloys have long been of interest for reactor-fuel applications because of the low thermal-neutron cross section of zirconium. Considerable information is available on the various properties and behavior of these alloys1 although there had been a number of areas where information was incomplete. As part of a program to provide more detailed knowledge in these areas, the presently reported investigation was undertaken. The constitutional diagram of the zirconium-uranium system is shown in Fig. 1.' The system is distinguished by a region of complete solid solubility between the body-centered cubic ß-zirconium and ? uranium phases and the existence of an intermediate phase in the vicinity of 50 wt pct U. This intermediate phase, designated as E, is reported3 to have a primitive hexagonal structure with a = 5.03 and c = 3.08A. The structure is partially ordered with zirconium atoms at the 0, 0, 0 position and zirconium and uranium atoms located randomly at the 1/3, 2/3, 1/2, and 2/3, 1/3, 1/2 positions. While the E phase may be nominally designated as of UZr2 stoichio-metry, the random distribution of uranium and zirconium atoms permit a considerable range in composition. Of interest in the research performed were alloys in the range from 20 wt pct (10 at. pct) to 70 wt pct (47 at. pct) U. In this range of compositions the body-centered-cubic ? phase can be retained either completely or partially on quenching. The nature and kinetics of transformation of the ? phase were the subject of study. Proceeding concurrently with the presently reported work was an investigation by Kearns4 which has since been reported. Kearns studied alloys containing 50 to 60 wt pct U prepared from sponge zirconium. While the work reported here is for alloys prepared from crystal-bar zirconium and the techniques of study are to some extent dissimilar to those employed by Kearns, general agreement so far as results and interpretation can be reported. Experimental Techniques—Alloys were prepared and the transformation of the ? phase studied during interrupted-quench and quench-and-temper isothermal heat treatments by means of hardness measurements and X-ray diffraction and metallographic techniques. The isothermal transformation of the ? phase on quenching and tempering was investigated further employing dynamic-modulus measurements. Electrical resistivity and limited Hall coefficient measurements were also obtained as part of the study. Alloy Preparation and Heat Treatment— Alloys containing 15, 20, 22, 30, 40, 45, 50, 55, 60, and 70 wt pct U were prepared from as-reduced uranium and crystal-bar zirconium. The alloys were double arc melted by consumable-electrode are-melting techniques. The final ingots were forged and rolled at temperatures between 790" and 840oC to 1/4-in. rod and 1/8-in. sheet. Chemical analyses of the fabricated alloys were

Jan 1, 1961

By A. W. Decora

Gas-liquid chromatography has been applied to separating basic nitrogen compounds, such as pyridines and amines. Close-boiling compounds have been separated by exploiting structural and polarity differences, using selective liquid substrates dispersed on specially prepared solid supports. Development of these special supports was necessary in order to obtain symmetric peaks for basic nitrogen compounds; solution of this problem was important in applying gas-liquid chromatography to the analysis of basic nitrogen compounds found in shale oil. Attempts to analyze shale-oil tar bases by conventional gas-liquid chromatographic techniques, using Chromosorb4/ or Celite 545 as the support for a nonpolar liquid substrate, resulted in asymmetric peaks. These asymmetries were caused by adsorption of sample vapors on the solid support. Symmetric peaks were obtained when strongly polar liquid substrates were used on either Chromosorb or Celite. However, a solid support giving symmetric peaks only with strong polar substrates restricts the choice of substrate, and frequently, desired separations cannot be achieved.

Jan 1, 1961

By Robert K. Jones

Filter media can be defined as that material which effects the removal of finely divided solids from a fluid. Thus the removal of dust from air or turbidity from water, for example, can be the result of passing the fluid through a properly supported filter media. Since filtration in one form or another has been practiced since pre¬historic times filter media have been made from an extremely wide variety of materials. Vegetable and synthetic fibers (used loose, or formed into papers, felts or cloth) sand, ground coal, diatomite, perlite, wire cloth, porous metal, and bonded aluminum oxide are among the more important materials used today.

Jan 1, 1961

By T. A. Sullivan

The work described in this report was undertaken to evaluate and develop techniques for determining the oxygen content of titanium and titanium alloys. Early investigations of volatilization techniques involving halogenation were unsuccessful. Later efforts were concentrated on evaluating vacuum fusion and inert-gas fusion techniques. Two vacuum fusion methods and an inert-gas fusion method were found to be satisfactory in the 0.02 to 1.00 pct., oxygen range. These methods are described in detail. The coefficient of variation by any of the three methods is approximately 5 pct, While the main portion of this paper is devoted to the vacuum and inert-gas fusion methods, a resume of other suggested methods for analyzing titanium for oxygen also is given. INTRODUCTION The Federal Bureau of Nines has conducted research on titanium metal since 1938. This research included development of the Kroll process for the production of titanium (2)4, various sodium reduction processes for making titanium metal and lower valent titanium chloride-sodium chloride mixtures (17), and a fused salt electrolytic process for Me production of high-purity titanium metal and the recovery of titanium by electrorefining from off-grade materials (20).

Jan 1, 1961