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By B. C. Allen, W. D. Kingery

Surface tension and its temperature dependence have been determined for pure liquid Fe, Cu, Co, Ni, and Sn and for Fe-C, Co-C, and Ni-C alloys. The temperature coefficient of surface tension is negative for all these liquids. The surface tension and wetting behavior of tin and tin-titanium alloys on A120,, Si,N,, MoSi,, and Sic, as well as the behavior of titanium-containing nickel alloys on A1 20, have been determined over a wide temperature range. For all the solids investigated titanium additims markedly lower the contact angle. Some limits for the solid-surface energies have been calculated from liquid surface tension and wetting behavior. SURFACE tension and interface energy are important variables in a number of metallurgical and ceramic phenomena, and have been discussed at some length in connection with determining micro-structure of polyphase systems,' solid-state sintering,' thermal etching of grain boundaries, heats of solution and fine powders,'1 grain-growth phenomena,' the mechanical behavior of fine foils and fibers, nucleation, soldering and brazing,' and other phenomenz of academic or practical interest However, until recently few quantitative data have been available for high-temperature systems. Among available data are some indicating positive temperature coefficients for the surface tension of liquid copper,*,11,'2 cast iron,l3 and iron-carbon14 alloys. Although carbon was found to be not surface active in iron at 1570" some preliminary studies had indicated the possibility of a positive temperature coefficient for the eutectic composition at lower temperatures.16 One part of the present study has been largely concerned with determining the temperature coefficient of surface tension for several metals at elevated temperatures, In addition to surface-tension studies, the wetting behavior of alloys containing titanium has been investigated over a wide temperature range. Previous measurements indicated that titanium was selectively adsorbed from nickel at a liquid nickel-solid alumina interface,17 and the use of titanium hydride or titanium-alloy techniques for metal-ceramic soldering is well known. In the present study, previous data have been extended to new alloy systems, and measurements have been carried out with other oxidation-resistant ceramics. EXPERIMENTAL The sessile-drop method was employed to measure liquid surface tension and contact angle between liquid and solid, utilizing apparatus and techniques which have been described previously.'g The shape of a sessile drop depends on equilibrium between forces of surface tension tending to form a spherical surface of minimum area and forces of gravity tending to flatten the drop. Typical sessile drops are shown in Fig. 1. From precise measurements of maximum drop diameter and drop height the surface tension and drop volume were calculated. Four solid materials were employed as supporting plaques for the liquid-metal drops. Aluminum oxide (99.9 pct, J, T. Baker, reagent grade) was pressed and sintered at 1800°C. Molybdenum-disilicide powder (99.0 pct, Electro Metallurgical Co.) was pressed and sintered at 1650°C. Plaques were cut from silicon carbide (99.4 pct, hot-pressed at Alfred University) and silicon nitride (95.1 pct, with Al, Fe, 0 as major impurities, Norton Co.) rods. All plaques were polished, cleaned, and dried prior to use. A number of metals and alloys were employed. Chemical analyses of vacuum-melted ingots of iron, nickel, cobalt (National Research Corp.), commercial nickel-base alloys, electrolytic copper (International Smelting and Refining Co.), and tin (Mal-linckrodt Chemical Works) are given in Table I. Alloys were prepared in the laboratory by vacuum melting the base metal with either titanium hydride (Metal Hydrides, Xnc.) or spectroscopic-grade carbon (National Carbon Corp.). Nickel-titanium alloys contained between 0.001 and 0.005 pct oxygen and the ferromagnetic metal-carbon alloys contained 0.001 pct. Cylindrical metal specimens (1 to 2.5 g) were machined and bevelled at the bottom to insure a uniform advancing contact angle on melting. Before use the samples were acid-etched, cleaned with acetone, and rinsed in petrol ether.

Jan 1, 1960

Flue dust from the sintering of base metal sulphides was leached to remove cadmium and arsenic. Leach liquor contained cadmium, zinc and small amounts of other base metals as chlorides. Results are reported of the use of a cation exchange resin Zeocarb 225 to separate the base metals from the arsenic. The resin was eluted with sodium chloride or sulphate to give a solution of relatively concentrated cadmium suitable for recovery by zinc cementation. The limited solubility of sodium sulphate presented some practical problems which were investigated. Another problem was the precipitation of lead sulphate in the resin during elution.INTRODUCTIONWhen lead-zinc sulphides are sintered prior to smelting, the gases passing to the flue are mainly uncondensable but contain a certain proportion of sublimates and dust particles which deposit in the flue or are carried, after condensation in the gas stream, to some form of dust extraction equipment.The recovered dust is a complex mixture of base metal sulphates, sulphites, sulphides, chlorides and oxides, the composition depending on the original concentrates. A large proportion of the cadmium and some of the arsenic originally in the concentrates finds its way to this flue dust, the treatment of which can be a convenient means of removing these elements and controlling their concentrations in the main lead-zinc smelter circuit. However, disposing of this material represents an appreciable waste of base metals as well as a serious toxicity hazard.Sulphide Corporation Pty. Ltd. was faced with this problem in planning the flow sheet of the new lead-zinc smelter at Cockle Creek, N.S.W. From a test run carried out on a pilot plant at Avonmouth, U.K., using a mixture of lead and zinc concentrates, a sample of dust was obtained for...

Jan 1, 1960

By A. N. May

"This paper describes the present approach of the Mines Branch to the problem of measuring the stress condition in the interior of rocks surrounding underground openings. An instrument, which will be referred to as a stressmeter, has been developed at the Mines Branch to measure un-directional stress changes in absolute units. There are two modes of operation of this stressmeter. It can be regarded as a fixed instrument, in which case it is installed at the end of a diamond drill hole and left in position to record any subsequent stress changes taking place. Alternatively, three of the stressmeters can be used in conjunction with a trepanning opera-tion to allow the existing stress condition to be determined. The initial laboratory work and subsequent experiences in the field with the stressmeter are described. All the field development work on the stressmeter was made possible through the co-operation of Canadian Refractories Limited, Kilmar, Quebec."

Jan 1, 1960

By R. W. Coburn

The results of field experiments on wells which required stimulation indicated that engineered well-completions will cause an increase in ultimate recovery at reduced costs. Techniques and tools have been developed which can be used to establish well conditions most conducive to successful stimulation. Cementing, perforating and treating are bound together so completely that the success of one phase is completely dependent on the .effectiveness of the preceding phase. A method of determining the efficiency or effectiveness of any given well-stimulation treatment has been derived. Pressure behaviour during a treatment can be analyzed to yield the total percentage of the formation which has been treated.

Jan 1, 1960

By M. Smutz, C. J. Baroch, E. H. Olson

IN 1949 an orebody containing some 10 billion lb of recoverable rare earth metals was discovered in the Mountain Pass district of San Bernardino County, California.' The following year Molybdenum Corp. of America purchased a number of claims at the deposit and a mill on the property which had been constructed to process the district's gold ores. Average composition of ore from the San Bernardino deposit is less than 0.1 pct Tho2, 25 to 35 pct calcite, 10 pct rare earth oxides, 15 to 20 pct silica, and 30 to 40 pct barite.' Rare earth content of the ore analyzes 50.7 pct CeO2, 4.2 pct Pr6O11, 11.7 pct Nd2O3;, 1.3 pct Sm2O3,, and 34.3 pct La2O3 and others.' By floating the barite and depressing the bastna-site, Molybdenum Corp. of America produced a concentrate that contained 60 to 70 pct rare earth oxides. More than 25 pct of the rare earths, however, was lost in flotation. It seemed likely that a more economical method could be found. At the present time most of the rare earths in the concentrates are converted to rare earth chlorides, which are either fed to ion exchange columns for separation of the individual rare earths or reduced to misch metal. Current investigation shows that solvent extraction may achieve this separation more economically than ion exchange. The study reported here was undertaken to develop an economical method of preparing a pure rare earth nitrate mixture from California bastnasite ore. Results indicated that more than 98 pct of the rare earths could be recovered. Several possibilities were considered for processing bastnasite ore, but only the method outlined in Fig. 1 was investigated. This involved leaching the calcined ore with nitric acid. The nitric acid process is discussed under the following headings: 1) calcination of the ore, 2) leaching of calcine, 3) filtration studies, 4) solvent extraction, and 5) nitric acid recovery. Calcination: Since California bastnasite ore contains 25 to 35 pct calcite and about 10 pct bastnasite, calcination was needed to reduce the violence of reaction with nitric acid. Weight losses of 26 to 30 pct were obtained by calcining the ore at 900°C for I hr or at 800°C for 4 hr. Longer periods resulted in no further weight loss. Leaching the Calcine: When the bastnasite calcine was leached with 30 pct nitric acid for 8 to 10 days, rare earth recoveries of only 45 to 50 pct were

Jan 1, 1960

By J. P. McGee

As part of a joint U.S. Atomic Energy Commission-Federal Bureau of Mines program for using nuclear energy to supply process heat, a simulated nuclear loop has been constructed to test components. This loop has been operated for more than 1,800 hours at 100 p.s.i.g. Of this period, 23 hours were at 2,500° F. and higher; 540 at 2,000° to 2,500° F.; 840 at 1,500° to 2,000° F.; 200 at 1,000° to 1,500° F.; and 260 below 1,000° F. Leakage at flanges and welds was not a serious problem. A helium-recycle system with gas temperatures of 2,300° to 2,500° F. and a static pressure of 250 p.s.i.g. appears feasible. Difficulties were encountered with the recycle compressor due to thermal distortion of the impeller and shaft. The use of sealed bearings limits compressor operation to the life of the bearings.

Jan 1, 1960

By W. M. Nabors

As part of a program to promote conservation and efficient utilization of petroleum resources, Bureau of Mines engineers at the Morgantown (W. Va.) Petroleum Research Laboratory are studying secondary oil-recovery projects in the Appalachian region. The increasing demand for petroleum and its products and the increasing cost of exploratory drilling tend to emphasize the importance of improving the recovery of oil from known petroleum reserves. Published reports setting forth the pertinent facts of these operations may help others to profit by the experience. This report presents the results of a study of secondary-recovery methods used in West Virginia by the Piedmont Oil and Gas Co., the Ryan Oil Co., and Water floods , Inc., on their Roane County leases in the Walton and Clover Rush Run pools. The principal oil-producing horizon underlying the area studied is the Big Injun sand, at approximately 2,000 feet. The sand is often referred to as blanket sand because it underlies much of the State and is oil-productive in many localities. Most of the pools in the area were discovered during 1907 to 1910 and were similarly developed and operated.

Jan 1, 1960

By V. A. Nieberlein

This paper presents the results of research undertaken to recover titanium and columbium by low-temperature chlorination of low-grade columbium-bearing ilmenite concentrates, and to simultaneously remove chlorinated impurities from the volatile chlorides without resort to distillation. Coke-reduced ilmenite was chlorinated at 400° to 500° C., and the resulting TiC14 was free of most impurities before condensation. A heated purification column was used wherein various packing materials reacted chemically or physically with the impurities which passed through them in the vapor phase. A nearly water-white TiC14 product was obtained directly. The principal impurities in the titanium tetrachloride were: 0.02 percent Fe, 0.01 percent V, 0.05 percent A1, 0.04 percent Si, and 0.07 percent Cb. This is a less pure product than commercial TiC14. Most of the columbium was recovered as crude CbC15, requiring further refining.

Jan 1, 1960

By Charles T. Baroch

RESEARCH strengthened the position of cesium as the preferred material (commonly but erroneously called "fuel") for ionic propulsion engines. Its use as an element of the plasma thermocouple for generating electricity also seemed more likely. Domestic Production.-No domestic ore of cesium and rubidium was produced. San Antonio Chemicals, Inc., San Antonio, Tex., and Maywood Chemical Works, Maywood, N.J., continued to produce cesium and rubidium compounds including carbonate, chromate, hydroxide, nitrate, sulfate, and all four halides. Rocky Mountain Research, Inc., Denver, Colo., began producing various cesium and rubidium salts. American Potash & Chemical Corp., Los Angeles, Calif., offered cesium and rubidium for sale.

Jan 1, 1960

By N. P. Titkov

This paper presents the results of laboratory and pilot plant investigations for the development of efficient methods of beneficiating hematite ores from the Krivoi Rog, Kursk Magnetic Anomoly, Olenogorsk, and other localities. The tests included gravity, magnetic (in a high intensity field), flota¬tion, and magnetizing roasting methods. It was possible to develop efficient beneficiation methods depending on the mineral composition of the ore and degree of dissemination of ore and gangue minerals. The paper shows the relationship between the iron silicate and quartz content of the ore and the technologic indices of the various beneficiation methods. Some of the conclusions based on these investigations and the technical and economic computations related to the cost of one ton of pig iron produced from concentrates obtained by the various beneficiation methods are: 1. If the hematite ore is not disseminated uniformly, it is expedient to use a combined gravity and flotation process. Ore particles up to 50 am. in size are beneficiated by gravity (heavy suspension, jigging, and others) and yield a lump concentrate. The middlings from this process are recrushed and floated; 2. Finely disseminated hematite ores, containing small quantities (less than 5 percent) of iron silicates, are most effectively beneficiated by flotation. Anionic (sulphate soap, tall oil emulsion with various foam depressors) as well as cationic collectors may be used. Depending on the mineral and chemical composition of the ore, it is possible to obtain concentrates containing up to 65 percent iron with an extraction up to 94 percent; 3. Finely disseminated, mixed hematite-magnetite ores may be beneficiated by flotation or a magnetic separation-flotation process; 4. Finely disseminated hematite ores, containing large quantities of iron silicates and earthy hematite ores are most efficiently beneficiated by the magnetizing roasting method. This method will yield concentrates containing up to 68 percent iron with extractions up to 90 percent. Although beneficiation by the magnetizing roasting process is costly, it will nonetheless, when employed on this type of ore, yield the least expensive pig iron.

Jan 1, 1960

By Alla D. Mah

THERMODYNAMIC data for manganese and its inorganic compounds have not been critically surveyed since the work of Maier (31) 3 in 1934. At that time data were lacking or inadequate for many of the important metallurgical compounds. Experimental work, conducted during the intervening years, has supplied so many new thermodynamic values that it is again desirable to examine the available data and compile them into a single publication for handy reference. This paper consists of three main sections. The first summarizes the basic metallurgical thermodynamic data for manganese and its compounds, including heat capacities, entropies, heat contents, temperatures and heats of phase changes, vapor pressures, and heats and free energies of formation. All data available to May 1959 have been considered. The second section contains heats, free energies, equilibrium pressures, and equilibrium constants of reactions of manganese compounds, with special emphasis on metallurgical reactions. The third section supplies basic thermodynamic data for other elements and compounds encountered in metallurgical reactions of manganese, thus making it possible for the reader to conduct thermodynamic calculations without recourse to other literature.

Jan 1, 1960

By Walter W. Fowkes

Leonardite is a coallike substance, similar in structure and composition to lignitic coal and believed to be derived from lignitic coal by the process of natural oxidation. Leonardite is little known outside lignite-producing areas and has been developed commercially only to a minor extent. The higher oxygen content and less compact structure of leonardite, compared with lignite, make it undesirable as a fuel but indicate that it has potential as a source of chemicals and for other nonfuel uses. It is a convenient source of humic acids. The United States has a large natural reserve of leonardite; furthermore, it can be produced in the laboratory under controlled conditions. The significant elemental difference between leonardite and lignite is the oxygen content (leonardite, 28-29 percent; lignite, 19-20 percent). The higher oxygen content of leonardite is due entirely to a Larger number of carboxylic acid groups. This fact explains the 17-Cold increase in alkali solubility of leonardite. Spectral studies indicate that the material is mixed salts of humic acids.

Jan 1, 1960

By C. A. Frenzel

Extensive spectroscopic data are needed in making reliable vibrational assignments for use in calculating thermodynamic functions of polyatomic molecules. The fundamental vibrations of organic molecules may be observed at any wavelength from 2.5 to 200 microns (micron = µ = 10-4 centimeters), but most often in the region from 3µ to 50µ. Raman spectra generally cover the range in which fundamental vibrations occur, but equally important infrared spectra usually are not measured at wavelengths longer than 25µ. This limitation results because most infrared spectra are determined for analytical purposes, which seldom require information outside the region 2µ to 25µ. Measurements of infrared spectra in the range 15µ to 35µ recently were begun by the Bureau of Mines to obtain data needed in making vibrational assignments. This report presents the spectra of the following thirteen compounds: Tetrahydrofuran, 1-methylpyrrole, piperidine, 2-methylpyridine, 3-miuthylpyridine, 2-propanethiol, cyclopentanethiol, 2-methyl-2-butanethiol, 3,3-dimethyl-2-thiabutane, cyclohexanethiol, cyclopentyl-l-thiaethane, 2,4-dimethyl-3-thiapentane, and hexamethyldisiloxane.

Jan 1, 1960

By T. E. Gray

This report describes preparation characteristics of the significant coalbeds in Marion County, W. Va., as determined by the Bureau of Mines. It is one in a series telling what coals are suitable for producing metallurgical coke, either as mined or after beneficiation. Over 9.4 million tons of coal was produced in Marion County, W. Va., in 1958, of which almost 6 million tons was cleaned mechanically in nine cleaning plants. All of the coal mechanically cleaned came from the Pittsburgh bed. The Bureau of Mines estimated that 1,578 million tons of recoverable coal remained in the county in beds 28 inches or more thick as of January 1, 1955.

Jan 1, 1960

By Jack D. Ramsdell

The objective of this investigation was to make a preliminary evaluation of titanium-vanadium-zirconium, alloys using room-temperature tensile properties as criteria for selecting promising alloys for future critical studies. Arc-melted titanium-vanadium-zirconium alloys ranging in composition from 5 to 20 a/o (atomic-percent) vanadium and 5 to 30 a/o zirconium, were investigated to evaluate hardness, hot workability, and room-temperature tensile properties. Metallographic examination coupled with hardness measurements were used to follow structural changes and aging response. Room-temperature tensile properties were criteria for evaluating mechanical and engineering properties of the alloys.

Jan 1, 1960

By J. D. Ramsdell

To obtain information on the effects of cobalt on microstructure and tensile properties of titanium-vanadium-cobalt alloys, the composition ranges of 4 to 16 percent vanadium with 1 to 4 percent cobalt have been studied. The beta phase was not completely retained with vanadium additions up to 16 weight-percent or in the same alloys containing up to 4 percent cobalt.

Jan 1, 1960

By John C. Machisak

INJURY DATA and experience at coal mines in the United States for 1957 are presented in this bulletin under the following general sections: (A) General injury experience: Tables 1-6: Current data on number of fatal and nonfatal injuries, frequency and severity rates, and average severity. (B) Selected injury experience: Tables 7-36: Current data on causes of injuries, distribution of injuries by part of body injured, days of disability, extent of hand and machine loading, experience by employ¬ment and production groups, and various other operating factors and physical conditions related to the occurrence of injuries at the Nation's coal mines. (C) Injury experience, by States: Tables 37-41: Data on injuries, injury rates, employment, causes of injuries, and severity rates. (D) Major disasters: Table 42: Data on major disasters from 1948 to 1957. A major disaster is defined as a single accident in which, or as a result of which, five persons or more are killed instantly or die at any time thereafter. (E) Historical coal-mine-fatality experience: Tables 43-47: Data on fatalities and their causes at bituminous-coal, lignite, and anthracite mines from the earliest records through 1957.

Jan 1, 1960

By W. R. Hardwick

This information circular describes mining methods and practices at New Cornelia Branch, Phelps Dodge Corp., Ajo, Ariz. It is one of a series being prepared by the Bureau of Mines on mining methods, practices, and costs in various mining districts of the United States. The New Cornelia mine (fig. 1) is at Ajo, a town in southwestern Arizona (fig. 2) on Arizona State Highway 85 in the western part of Pima County. The [oncentrator] and smelter are near the mine (fig. 3). Copper ore is mined, crushed, ground, and concentrated, and the concentrates are smelted. Copper is cast in anode form and sent to the Phelps Dodge Corp. refinery in El Paso, Tex.

Jan 1, 1960

By Henry G. Dorsett

This report is a description of equipment and test procedures used by the Federal Bureau of Mines in laboratory studies on the explosibility of dusts. The principal tests concern ignition temperature, minimum explosive concentra¬tion, minimum electrical energy for ignition, limiting oxygen concentration, pressure, and rates of pressure rise. As new materials often present unique problems, variations in the general procedure and special tests performed are indicated, The general procedures for handling a dust sample from its receipt at the laboratory to the preparation of the report are described. The repro¬ducibility of the respective tests are shown. A brief history of laboratory studies on dust explosions by the Bureau of Mines and a description of current equipment and test procedures used are presented in this report. Its purpose is to facilitate interpretation of data previously published and those proposed to be published on the numerous mineral, agricultural and industrial dusts that have been studied. Through understanding and interpretation of the laboratory data obtained for the parameters of explosibility, preventive measures can be adopted for alleviat¬ing the hazard of dust explosions arising in manufacturing and processing industries.

Jan 1, 1960

By C. S. Gibson

"MOST of the mines in the Province of Ontario in Canada are multi-level operations in steeply dipping veins; yet there is an appreciable number whose de-posits are relatively flat-lying, ranging up to 45° inclination.The veins vary in width up to several hundred feet and may or may not be branching systems. The depths of mines range from a few hundred to 8,000 feet, approximately. The primary products of the underground group are asbestos, gold, silver, cobalt, copper, nickel, iron, uranium, talc, fluorspar, gyp-sum and salt.There are a few open-pit mines. The majority are temporary in type because, as the outcrops are removed, mining is continued be-low surface. Primary products of the open pits are copper, nickel, iron, magnesium and nepheline syenite.The industry as a whole employs about 50,000 persons, approximately 60 per •cent of whom have dust-exposure occupations. The definition of a dust-exposure occupation and the requirements for •dealing with same are set forth in The Mining Act of Ontario.Results of extensive and continuing studies on the incidence and progression of silicosis have been reported periodically for years past, in annual reports of the Mines Accident Prevention Association of Ontario and in papers presented at Conferences sponsored by Mcintyre Research Foundation of Toronto, all of which have been published. The information provided therein proves the effectiveness of the means being used to prevent silicosis and allied disorders."

Jan 1, 1960