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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

By K. P. Gupta, P. A. Beck, N. S. Rajan

By determining the a phase boundaries in the following ternary systems: V-Fe-Si (at 1175oC), V-Co-Si (at 1175°C), V-Ni-Si (at 1175oC), Cr-Mn-Si (at 1000°C), Cr-Co-Si (at 1175°C), Cr-Ni-Si (at 1175°C), V-Fe-A1 (at 1175°C) and Cr-Co-A1 (at 1175°C), it was found that Si exerts a stabilizing effect on these a phases, while A1 tends to destabilize them. Si atoms in solid solution occupy sites D in the a structure, The co/ao ratio increases with increasing Si-, Mn- or Fe-content. The volume of the unit cell decreases with increasing Si-content. THE stabilization of certain metal silicides (the Nowotny phases) by the addition of relatively small

Jan 1, 1961

By David M. Gullikson

Since publication of the paper on the composition of California oilfield waters by Jensen (6)3/ in 1934 the only other information on the subject was published recently by Chave (4). To supply needed information on the composition of California waters in areas of current drilling activity, the Federal Bureau of Mines collected formation water samples for analysis. Thirty-eight samples from oil-and gas-producing formations in 12 fields located in Ventura, Kern, Glenn, and Colusa counties were analysed by the Bureau's San Francisco Petroleum Research Laboratory. The samples were selected particularly from fields where the water composition was not well known or where interpretation of electrical logs has been difficult and the interpretation may be affected by unusual composition of the water. These samples were obtained from rocks ranging in geologic age from Cretaceous to Upper Pliocene. Fifteen constituents of these waters were determined including sodium, potassium, calcium, magnesium, strontium, barium, lithium, chloride, iodide, bromide, carbonate, bicarbonate, sulfate, borate, and residual acidity. These analyses are the first to be published on California oilfield waters in which determinations for potassium, strontium, bromide, iodide, boron) and naphthenates were made on a significant number of samples. The electrical resistivities of tae samples were determined at 75° F. and 175° F.

Jan 1, 1961

By I. H. Warren, Forward F. A

The reduction of aqueous slurries of uranyl carbonate at elevated temperature with compressed hydrogen m the presence of metal catalysts and certain organic promoters has been shown. to yield uranium dioxide. The reduction takes place in a sequence of steps. The purity and sintering properties of the dioxide make it of interest as a starting material for fuel element production. Simple control can be exercised over the surface area and oxygen/uranium ratio of the product during reduction. URANIUM dioxide for fueling atomic power reactors 1s conventionally produced as a powder by simultaneously decomposing and reducing ammonium diuranate with hydrogen in a furnace at high temperature. Fuel elements are then generally made from this powder by compacting and sintering ( 1). In order that elements approaching theoretical density may be obtained,

Jan 1, 1961

Jan 1, 1961

By M. R. Geer

The use of the cyclone as a dense-medium cleaning device was first described by Driessen6/ in 1945, after development of the process in the Netherlands during the German occupation of World War II. A pilot plant was built in the Netherlands soon thereafter, and the first commercial plant was built in 1948. By 1958, 18 plants were operating or under construction.7/ Thus, economic factors in Europe, where the high cost of coal places a premium on efficient cleaning, dictated rapid adoption of the cyclone. American reception of the process differed. The Bureau of Mines presented the results of its own small-scale cyclone experiments in 1946;8/ showing a sharp separation between coal and impurity; adoption by industry now is taking place. There is now much greater emphasis on the efficient cleaning of fine coal, and the first American cyclone plant has begun operating; others are planned or under construction. With the present interest in improved treatment of fine coal, the Bureau of Mines felt that additional performance data on the cyclone would be helpful to industry. Therefore, a complete, open-circuit pilot plant was built to make cleaning trials on American coals covering a wide range of washability characteristics. Five raw coals and one middling product were included in the investigation, and each was cleaned at several densities; 17 cleaning trials are reported.

Jan 1, 1961

By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By William J. Campbell

This study was a part of two programs: The first, to develop and evaluate high-temperature refractories; the second, to investigate reaction-rate kinetics and phase equilibria in the sinter step of the lime-soda process for the recovery of alumina. High-temperature X-ray diffractometer techniques are to be used extensively in both programs. This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines. A more detailed description of the equipment and its calibration is planned in a future paper on thermal expansion and phase inversion of rare-earth oxides.

Jan 1, 1961

By C. N. Adams

The purpose of this investigation was to evaluate the physical and mechanical properties of high-purity titanium made by two processes. Sodium-reduced metal with 58 Brinell hardness number (B.h.n.) and electrorefined metal with 60 B.h.n. and 70 B.h.n. were used. Titanium of these hardness levels did not work-harden excessively, and beyond 40 percent cold work the hardening effect was not great. Rapid softening occurred when the metal was annealed at temperature between 300° and 600° C. Full annealing, as determined by property and microstructure studies, was accomplished after 30 minutes at 700° C. A recrystallization diagram is presented which is based on determinations of annealed grain size as a function of rolling reduction and annealing time. For reductions of less than 20 percent, exaggerated grain growth occurred during annealing; for reductions greater than 20 percent, the variation in grain size for each annealing temperature was minor.

Jan 1, 1961

By K. K. Kershner

The purpose of this research by the Federal Bureau of Mines was to investigate the recovery of tin from mine-run ores and low-grade concentrates. Over 95 percent of the total tin in such materials was volatilized to tin chlorides at temperatures ranging from 520° to 565° C. Gaseous mixtures of hydrogen and hydrogen chloride were used for reducing cassiterite to stannous oxide and for converting this compound to tin chlorides. The chlorides were swept from the reaction zone of an oscillating kiln by a rapid flow of reactant gases and collected in a condensing system. Losses of tin that occur in current metallurgical processing were prevented. Approximately the same time of treatment was required for minus 35-mesh mine-run ores and low-grade concentrates. In a continuous process, the circulating gases would require some enrichment.

Jan 1, 1961

By H. D. Kline

This publication describes mining and milling methods and costs at the Madison mine of National Lead Co., St. Louis Smelting & Refining Division, in the Fredericktown district of southeast Missouri and is one of a series prepared by the Federal Bureau of Mines on methods, practices, and costs of mining and milling throughout the United States. The are bodies of the Madison mine are known for the complexity and diversity of their are minerals. Sulfides of copper, nickel, and cobalt occur in commercial quantities with lead sulfide, which is the most valuable metallic mineral in are bodies of the Bonne Terre formation in southeast Missouri. Several attempts were made by various operators to mine the complex ores and separate the sulfide minerals before 1927 when National Lead Co. became interested in the Fredericktown district. Operating then as the St. Louis Smelting & Refining Co., the company began mining and milling ores from the Madison mine in 1944 and has operated continuously since then. A recently built refinery produces copper, nickel, and cobalt metal from a concentrate containing iron sulphides and small quantities of copper, nickel, and cobalt sulphides.

Jan 1, 1961

A spectrographic procedure applicable to the semiquantitative determination of 29 elements in tungsten is presented. The method is designed to give estimates of impurity concentrations up to 500 p.p.m. Limits of detectability range from 0.3 p.p.m. for the more sensitive elements to 100 p.p.m. for the less sensitive ones. Tungsten metal samples varying in particle size from minus 300-to 30-mesh are excited in the presence of 5 percent germanium with a direct current arc. Germanium acts to stabilize the arc, minimizes the volatilization of tungsten, and serves as an efficient carrier to sweep impurities from the tungsten into the excitation zone. Curves are presented that show the volatilization behavior of germanium, tungsten, and impurities in tungsten at different concentration levels. Data obtained were used as guides in establishing the method of analysis. In the absence of established reliable analytical procedures for determining many impurities in tungsten in the parts per million concentration range, the spectrographic method described here should prove to be helpful in evaluating high-purity tungsten.

Jan 1, 1961

By W. S. Sanner

Anthracite was used extensively as a fuel in iron metallurgy from 1840 to 1880. In 1874, 226 of the 680 blast furnaces in the United States were operating on anthracite and producing almost one-half of the Nation's pig iron. However, by 1890, railroad expansion, the development of western iron-ore reserves, and the growing use of coke decreased the importance of anthracite as a metallurgical fuel. As a result, the last blast furnace designed exclusively for anthracite use was built in 1891. Because of the increased energy requirements of our expanding national economy, the abnormally high demands during national emergencies, and the proximity of anthracite deposits to eastern steel-producing areas, interest has grown in again using anthracite in iron metallurgy. Estimates of anthracite reserves indicate a 300-yr. supply at a production rate of 30 million tons per year. These large reserves dictate the development of an adequate technology for the use of anthracite by the metallurgical industry.

Jan 1, 1961

The paper outlines the development of a solvent extraction process for the recovery of scandium, yttrium, thorium, and heavy lanthanides from waste sulphate liquor at the Port Pirie uranium treatment plant. A summary is given of known solvents for these elements, including the recently developed alkyl-phosphoric acid esters which are applicable to sulphate solutions.A kerosene solution of di- (2'-ethylhexyl) phosphoric acid (EHPA) has been suggested by some workers as a suitable solvent for fractionation of the lanthanides. Experimental work with this solvent showed that it could be used for initial recovery of the above elements from low concentrations in the complex sulphate liquor. In particular, scandium could be recovered as a high grade product by extraction with 0·lM EHPA, followed by a purification strip with 9N sulphuric acid, and final stripping of scandium with sodium hydroxide solution.To enable alkaline stripping to be used successfully, the kerosene solution of the reagent was modified by the addition of a small proportion of nonanol. Experimental work included laboratory scale batch tests and small pilot scale continuous tests.A proposed extension of the process for the separate recovery of individual heavy lanthanides, yttrium, and thorium is described.INTRODUCTIONAt the Port Pirie uranium treatment plant of the South Australian Government, large volumes of "barren liquor", free from 'uranium, are at present run to waste. This "barren liquor" results from sulphuric acid leaching of Radium,Hill uranium concentrate, followed by separation of solid residues and removal of uranium from the clear solution by ion exchange. The mineral davidite, from which the uranium is derived, contains other potentially valuable components, notably vanadium, chromium, thorium, yttrium, scandium, and the lanthanides. These constituents are...

Jan 1, 1961

Present roof bolting practices in the collieries of Australian Iron and Steel Pty. Ltd. are outlined. Roof support has been improved since introducing roof bolts and it is hoped to increase the reliability of the bolts still further.Expansion-shell, and split and wedge roof bolts five to eight feet long are placed by "Atlas Falcon" and "Fletcher" roof bolters. Both anchorage and tightening have presented some problems.Good panel supervision is required if systematic roof bolting is to be properly co-ordinated with coal production without unnecessary delay to either. Successful roof bolting can only be the product of conscientious men and supervisors who are all convinced of its value. A rigid operational code should be established early and maintained.INTRODUCTIONRoof bolting is a method of support which is permanent and reduces or eliminates the need for other support; The method was pioneered in America and was first experimentally investigated in Australian collieries at Elrington in 1949 (McKensey, 1953). Pneumatic installation methods were employed. Subsequently, a method of using standard hand-held electric coal drills was developed at John Darling Colliery (Horseman, 1954). Pneumatic roof bolting equipment was first operated in the collieries of Australian Ironand Steel Pty. Ltd (A.I. &. S.) in 1951. Since then various hydraulically operated mobile machines have been installed in Australian collieries and these, together with improved pneumatic equipment, form the two present basic methods of placing ,roof bolts. Roof bolt anchorage is achieved by either split and wedge or expansion-shell bolts.The two broad types of roof bolting are 1. consolidation of strata, and 2. suspension support.

Jan 1, 1961

By R. J. Leary

Significant improvements in surface conditions or mechanical properties of steels have been attributed by several investigators to ladle additions of small quantities of rare-earth metals or their oxides. To investigate systematically these effects in wrought and in cast plain carbon and alloy mechanical steels containing approximately 0.35 percent carbon, heats of four representative compositions were melted by the Bureau of Mines in a 4-ton open-hearth furnace. Each heat was cast into three sets of ingots to exemplify respectively, treatments with (1) rare-earth metals, (2) rare-earth metal oxides, and (3) an untreated set as a control. The development of melting, casting and rolling practices is described and discussed. Lance injection of oxygen shortly after melt raised the temperature of the metal immediately as much as 500° F., principally because mechanical agitation exposed the high-carbon metal to the flame and furnace root. An exceptional degree of superheat in the metal at the termination of the refining period was attributed to oxygen injection during the refining period. Bath temperatures higher than industrial practice were permitted by the all-basic furnace lining. Rates of carbon elimination as high as 0.036 percent carbon per minute were achieved by oxygen injections.

Jan 1, 1961

By Beverly W. Dunning

The effect of vacuum melting on the elimination of gases and nonmetallic inclusions for six low-alloy steels was investigated. The purpose of these studies was the analysis and comparison of differences in gas content and inclusions in air-melted and vacuum-melted steel. Data obtained from melts of 1-1/4 to 20 pounds indicate that vacuum melting decreases the number and size of nonmetallic inclusions and at the same time increases the degree of dispersion of the remaining inclusions. These improvements are undoubtedly related to the elimination of approximately 80 percent of the nitrogen and 90 percent of the oxygen as well as most of the undesirable metallic trace impurities.

Jan 1, 1961