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By R. W. Stahl

An award is a form of recognition given for superior performance in a special field of endeavor. Each year awards are given by the Joseph A. Holmes Safety Association and the National Safety Council to mineral industries' mines, quarries, and plants that have worked a specific number of man-hours without a lost-time injury. These awards have a dual significance in that they prove that efficiency can be attained without injury to persons. Safety awards do not result from luck or good fortune but do result from sincere desire coupled with sufficient effort and cooperation to achieve a desired goal.

Jan 1, 1963

By G. W. Healy

Activities of oxides in the ternary FeO-MnO-SiO system are calculated from data on the binaries, using the Gibbs -Schuhmann method. These activity data are used, together with thermodynamic relations, to calculate the contents of oxygen, silicon, and manganese in liquid iron, and the composition of the corresponding oxide phases in equilibrium with it. Excellent agreement was found between calculated and experimental metal compositions, indicating that thermodynamic methods, such as those presented, can supply useful data on slag-metal equilibria, and are therefore capable of wider application. When molten steel containing oxygen is treated with a deoxidizer, the product of the reaction is composed of the oxides of the deoxidizing elements together with more or less iron oxide. This assemblage of oxides is presumably very close to equilibrium with the melt since it is formed directly from elements dissolved in it. Therefore, it is likely that metal analyses corresponding to a given oxide phase composition are calculable with considerable precision where sufficient information is available on activities in both phases. The present study was made to test this hypothesis in the case of deoxidation by silicon and manganese. Here experimental data on the relationship among oxygen, silicon, and manganese in the metal phase are available, as are activity data for the MnO-SiO2, FeO-SiO2, and FeO-MnO binary systems. A further objective was to demonstrate in a specific example how gaps in the data may be filled by judicious interpolation, and how the Gibbs-Schuhmann method is applied to obtain activities in ternary systems. The rigorous derivation of the latter, requiring considerable facility in handling partial differential equations, tends to mask the real simplicity of the method, and repel the very engineers and experimenters who would benefit the most from its use. I) GENERAL PROCEDURE Deoxidation of steel with silicon and manganese results in the formation of two phases, metal and oxide. The number of components is four—Fe, Mn, Si, and 0. The phase rule then gives the number of degrees of freedom: If temperature and pressure are fixed, 2 deg of freedom remain. Consequently, it suffices to fix the concentration of two of the components of the system for all the concentrations to be determined and, at least in principle, calculable. The practical problem is then to discover a straightforward method of calculation with a minimum of trial and error solutions. The type of reactions to be dealt with are like the following: Si (in steel) + 2 O(in steel) = SiO2(in oxide phase) The standard free energy of this reaction is readily obtained from the literature, so that the equilibrium constant can be calculated by the expression: Since the metallurgist is concerned with percentages rather than activities, a real solution requires information that will permit activities to be converted to concentrations. This information is fairly adequate for the elements dissolved in molten steel, but is not available for the FeO-MnO-SiO2 oxide system. Therefore, the first step in this study was to find the relation between activity and concentration for the three oxides making up the system. The next step was the calculation of slag and metal compositions that are in equilibrium with one another. As shown by the phase rule, it is sufficient to assume the values of two composition variables in order to calculate the rest. But which two are picked makes a vast difference in how difficult the calculation turns out to be, so that it is necessary to make preliminary trial of several routes to find the easiest one. A convenient method is to begin with the slag, and to pick FeO concentration and that of one of the other oxides. Starting with the relation between oxygen dissolved in the liquid steel and FeO in the slag permits a good first estimate to be made of the oxygen content of the steel in equilibrium with FeO, because the iron content being fairly close to 100 pct, Fe has an activity close to unity. Using this first estimate of oxygen activity, approximate values of the manganese and silicon contents of the melt are readily calculated from the appropriate equilibrium constants. A minor correction for the depar-

Jan 1, 1963

By John C. Machisak

INJURY EXPERIENCE AND EMPLOYMENT DATA on all stone quarries and associated plants in the United States are presented in this publication for the calendar year 1959. Such related operations as the manufacture of cement and lime and rock dressing are included. Data on clay and sand and gravel operations are not included and will be found in other Bureau publications on injuries and employment. The Bureau is authorized to make requests for such data and the information voluntarily submitted by the operators contributes to the promotion of safety in the quarrying industry. Every effort has been made to make this canvass as complete as possible. Data for production workers and office employees at the quarry site are included.

Jan 1, 1963

By John C. Machisak

INJURY EXPERIENCE AND EMPLOYMENT DATA on all stone quarries and associated plants in the United States are presented in this publication for the calendar year 1959. Such related operations as the manufacture of cement and lime and rock dressing are included. Data on clay and sand and gravel operations are not included and will be found in other Bureau publications on injuries and employment. The Bureau is authorized to make requests for such data and the information voluntarily submitted by the operators contributes to the promotion of safety in the quarrying industry. Every effort has been made to make this canvass as complete as possible. Data for production workers and office employees at the quarry site are included.

Jan 1, 1963

By A. A. Berk

Other Federal agencies have been coming to the Bureau of Mines for help with the purchase and utilization of fuel, largely coal, almost since the day the Bureau was created in 1910. The requests covered a wide range of fuel-economy problems and included boiler-water treatment after it became apparent that water-formed deposits on heating surfaces acted as insulators, decreasing heat transfer and impairing fuel efficiency. Dr. Ralph E. Hall, a Bureau of Mines physical chemist determined the reactions that cause adhering scale to form in boilers (7)2 and went on to introduce scientific principles into water treatment for scale prevention (8). Widespread publicity of these achievements increased the requests for help from Federal steam-generating plants. Since no other Federal agency (even those which were more directly concerned with testing water) wanted to provide boiler-feedwater service, the Bureau decided to continue to give requested help to Federal agencies, Later, the Congress endorsed such agency cooperation as an economy measure,

Jan 1, 1963

By F. D. Stevenson

A metal diaphragm pressure relay system was constructed to measure vapor pressures of the metal halides, oxyhalides, and other substances at temperatures up to 700° or 800° C. The vapor pressure of arsenic (III) oxide (As2O3) was determined to verify the reliability of the apparatus for such measurements. The data for the liquid AS2 Os (2820 to 4830 C) are represented by the equation, log Pmm = 6.875 - 2,929/T, from which the normal boiling point was calculated to be 461° C. The heat of vaporization calculated from this equation was 13.40 ±0.09 kcal/g mole As4OS and is essentially constant over the interval studied. The melting point of the octahedral arsenic (III) oxide was determined to be 278° C from the inter-section of the solid and liquid vapor pressure curves, A thermal analysis apparatus is also described by which melting and transition temperatures could be checked by a method independent of vapor pressure data. The melting points of the monoclinic and octahedral forms were determined to be 314.4 ±1.4° C and 278 ±5° C, respectively.

Jan 1, 1963

By Nicholas J. Grant, William H. Ferguson, Bill C. Giessen

Ta-lr alloys have been examined over the complete range of compositions using metallographic and X-ray techniques. The terminal solid-solubility limits, solidus temperatures, and intermediate phases were determined. There are four inter-mediate phases: o, tetragonal, analogous to a (Fe-Cr); 0,. orthorhombic; az, tetragonal; and a TaZr,, cubic, AuCu, structure. Of these, o and a, melt peritecticaLly, a, decomposes peritectoidally, and a TaIrs has a congruent melting point. Three peri-tectic and one eutectic reactions occur. 1 HE Ta-Ir phase diagram has not been treated in the literature. Intermetallic phases and terminal solid solubilities have been described and estimated.'-4 The previous findings have been confirmed in this work. A complete diagram with additional phases and solidus curves is presented. EXPERIMENTAL METHODS Starting materials were tantalum powder of 99.8 pct purity, supplied by the National Research Corp., Cambridge, Mass., and iridium powder of 99.9 pct purity, supplied by the Bishop Co., Malvern, Pa. Both powders were -200 mesh. Table I lists the analyses as given by the suppliers. A standard procedure was employed in making the alloy buttons, which was described in detail in Refs. 5 and 6, and which included repeated arc-melting of powder compacts and determination of the composition by the weight-balance method. This is especially justifiable due to the similar vapor pressures of tantalum and iridium. In the critical parts of the diagram, a spacing of 1/2 at. pct was used, based on premelted master alloy material. The observed structures and X-ray spectra were consistent with the composition sequence of the alloys. Table II lists the final alloy atomic percentages with the calculated percent error of composition. Cross sections representative in grain size and composition were selected for the study, as described in Ref. 5. Based on prior experience, no contamination from the tungsten electrode was considered. Temperature measurements were obtained using a Leeds and Northrup optical pyrometer and have been described extensively in Refs. 5 and 6. All heat treatments were made in the high-vacuum tantalum tube furnace mentioned in Ref. 5. Samples annealed in tantalum containers cooled from 1800" to 1000"~ in 5 sec; those annealed in ceramic crucibles cooled over the same range in 15 to 30 sec. The thermal treatments are listed in Table 111. All specimens were homogenized at 1735°C for 24 hr. Tantalum-rich compositions were treated in tantalum buckets. Iridium-rich compositions were annealed in tantalum buckets below the eutectic temperature of 1950°C; up to 2200°C, tungsten-lined tantalum baskets were used; and above 2200°C thoria crucibles were used. It was found that refractory oxides (in early stages of the investigation alumina crucibles were used up to 1800°C and thoria crucibles were used to 2400"~) give off minute amounts of oxygen and thereby influence the microstructure considerably, or react directly with the alloys.

Jan 1, 1963

By B. C. Allen

Liquid surface tensions of copper and 18 Group IV-A to VIII transition metals (Ti, Zr, Hf, V, Cb, Ta, Mo, W, Re, Ru, Rh, Pd, Os, Ir, Pt, Fe, Ni. Co) have been measured by the static pendant-drop and dynamic drop-weight methods on the same rod sample. The drops were formed by electron-bombardment heating in high vacuum. Application of necessary corrections enabled determination of surface tensions to k2 pct and agreement between methods to * 1 to 4 pct for all the metals studied. Evidence is presented that the liquid surface was well screened by metal vapor, suggesting negligible adsorption of gaseous impurities and that the surface tensions measured are characteristic of the metals involved. Correlations between liquid surface tension and melting point, molar volume, heat of vaporization, and atomic number are presented and discussed. Temperature coefficients of surface tension were calculated using Eötvös' law. SURFACE tension and interface energies of metals are the result of incomplete atomic coordination resulting in a force perpendicular to the boundary, tending to minimize its area. These energies are important in many phases of metallurgy, including microstructure, sintering, joining, electronic emission, and lubrication, which in turn affect many physical and mechanical properties of metals. Liquid surface tension refers to the interface between the liquid and its own vapor or nonreactive atmosphere, and is considered a physical property of the liquid. Since equilibrium shapes can be readily obtained with liquids, the units of surface tension (force per length) and interface energy (energy per area) are interchangeable. Thermo-dynamically, the surface tension ?LV is given by the change in free energy F with surface area A at constant pressure P, temperature T, and composition N: for commercially important refractory metals, vanadium, columbium, tantalum,13,14 molybdenum,14 and tungsten,l5 and none for the rare platinum-group metals and rhenium. Measuring the surface tensions of transition metals is difficult because of their high reactivity and melting points. Of the many techniques available,16-18 the pendant-drop 19-21 and drop-weight methods17,22 are considered superior because they can be modified to eliminate persistent sources of contamination such as supports and capillaries necessary in the popular sessile drop, capillary rise, and maximum-bubble-pressure techniques. The necessary modification is to melt a drop on the tip of a vertical rod, which provides support through a solid of the same composition.13,15 The object of the work was to study the surface-tension behavior of copper and transition metals, having reasonably low vapor pressures. Liquid surface tension of each pure metal was systematically determined by using a combination of the static pendant-drop and dynamic drop-weight methods on the same rod. Liquid drops were formed by electron-bombardment heating in high vacuum. EXPERIMENTAL WORK As indicated in Table I, the metals studied were high purity and generally were obtained in rod form. The exceptions were titanium and zirconium, which were machined from crystal bars, and molybdenum (tot 11, osmium, and ruthenium, which were sintered and arc cast into rods. All the metals were ground or swaged to desired sizes between 1- and 7-mm diam, and centerless ground round and smooth to a finish better than 50 µ in., rms. Each rod was thoroughly cleaned with steel wool, degreased, acid etched, and dried. In a typical run, the rod was vertically clamped in a modified floating-zone electron-bombardment furnace designed after Calverley23 and Carlson.24 The specimen was outgassed and maintained positive at several kilovolts in a dynamic vacuum of 10-5 to 10-7 mm. The bottom end was enclosed by a tantalum pillbox and heated by electrons emitted from a hot concentric tungsten filament mounted on a movable bracket. The bombardment power was slowly raised until melting was observed. Power requirements ranged from 30 w for copper to 1300 w for 4-mm tungsten. The stabilized and out-gassed drop of near-maximum size was photographed at 4. 1X on panchromatic film at desired time inter-

Jan 1, 1963

By Henry E. Perlee

Air compressor explosions that are caused by the ignition of combustible vapor mixtures cannot be explained by a single reaction mechanism or sequence of events. Explosions have been caused by the sudden release of large quantities of lubricating oil, by the rapid vaporization of oil that had accumulated slowly in high-pressure piping, and by the production of decomposition products from carbonaceous deposits. Ignitions can be caused by the heat produced in a catalytic reaction, in a compression process, or when a shock wave is propagated through a combustible vapor-air mixture. The frequency of these ignitions can be minimized by establishing proper maintenance and cleaning schedules. Further study is needed to satisfactorily correlate the various factors involved in compressor explosions.

Jan 1, 1963

By Richard Quirk

This report describes methods and techniques employed by The Glidden Co. of Cleveland, Ohio, in explorating an ilmenite-bearing sand deposit in Ocean County, New Jersey, during 1960 to determine ore reserve potential and the feasibility of mining and establishing a milling plant on the property for the production of ilmenite concentrate. The property covered approximately 1,250 acres. Comprehensive sampling by water-jet drilling indicated the deposit averaged 20 feet in thickness and contained 4.5 percent heavy minerals, of which 80 to 85 percent was ilmenite and leucoxene. Average depth of the water table as determined by auger boring was 16.8 feet. Pilot plant tests indicated that circular concentrators in combination with spiral concentrators would recover at least 80 percent of the heavy mineral content of the sands. It was estimated that sufficient ore reserve tonnage had been developed to supply the company's Baltimore chemicals division, pigments department, with a suitable grade ilmenite concentrate for a period of 20 years at the present rate of pigments production. The property was designated as Lakehurst mine and plans are in progress for mining development and plant construction.

Jan 1, 1963

By Frank A. Peters

A series of evaluations is being made to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. These evaluations include the estimated operating and capital costs as well as recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The three processes considered in this evaluation are designed to leach alumina as aluminum sulfate from calcined clay with sulfuric acid and to remove the silica residue by filtration. The filtrate from leaching is then purified by one of the following methods: Removal of iron in electrolytic cells using mercury cathodes; removal of iron by chemical precipitation through the formation of an iron-manganese complex; or precipitation of the alumina from an aqueous-ethanol solution, leaving iron in solution. Both the operating and capital costs for these processes are higher than those for the Bayer process. For plants producing 1,000 tons of alumina a day, the estimated operating costs per ton of alumina are: Electrolytic iron-removal process........... $81.35 Chemical iron-.removal process............... 82.08 Ethanol purification process............... 86.17 The investment in mercury is not part of the operating cost since this cost is considered equivalent to catalyst cost which would not be shown. The estimated capital investments for 1,000- ton-per- day plants on a Marshall and Stevens chemical equipment index basis of 240.0 are: Electrolytic iron-removal process...... $116,775,500 Chemical iron-removal process............... 99,418,900 Ethanol purification process................ 94,210,200 These investments include the working capital but not the land for each of the processes. Included in the electrolytic iron-removal process is an investment of $4,859,400 for mercury. Investigation of other methods for removing iron, of the decomposition operation, and of the leaching operation could reduce these costs.

Jan 1, 1963

Jan 1, 1963

By Harold Rees

[This report supplements and brings up to date a paper prepared earlier this year for presentation at the Eleventh Pan American Railway Congress to be held in Mexico City, October 18 to 31, 1963. In order to acquaint the reader with the background of this project practically all of the first paper is included in the report.]

Jan 1, 1963

By J. H. Schulman, M. H. Buckenham

R. W. Christy (Manager of Sales, Sanitary Engineering Equipment, Link-Belt Co.) and C.D. Rubert (Barrett, Haentjens & Co.) — Messrs. King and Schepman have presented an excellent paper which outlines the general practice in the design of thickener mechanisms. Lifting devices, controls, special applications and underflow pumping arrangements have been reviewed in detail. Pumping arrangements were illustrated which eliminate the need for an expensive tunnel beneath the thickener floor. Most of those illustrated have the common feature of a relatively long underflow suction line extending from the hopper floor to the pump located on the bridge at the periphery of the tank. The authors limit these arrangements to comparatively dilute or thin slurrys. It is implied that dense and coarse concentrates, which are difficult to pump, cannot be handled unless a tunnel is constructed. Fig. 1 shows an underflow pump arrangement which negates the need for a tunnel but which permits the operator to convey a heavy dense slurry. The pump is mounted directly on the fixed hoist platform and the impeller is located at the base of the steel center column. Priming water is not needed. The column

Jan 1, 1963

By John C. Machisak

The Nation's mining and quarrying industries have again met the annual challenge to their ingenuity--that of reducing disabling work injuries among their employees. The effectiveness of management in facing this problem and in meeting this responsibility from the results of the 1961 National Safety Competition. Three hundred ninety-three or 45.3 percent of the mines and quarries participating in the competition established a new record number of participants operating throughout the competition year without a disabling work injury. Another record established in the 1961 contest was the number of participants (868) enrolled in the competition. This annual safety competition was begun in 1925 and is conducted by the Bureau of Mines, U.S. Department of the Interior. It provides for six bronze Sentinels of safety trophies which are awarded each year to the winning participant in each group. Since its inception, the competition has exerted a strong influence in the field of safety promotion. The statistical record of its accomplishments over the years gives strong support to the theory that well-organized and well-administered safety programs are effective tools to be used to reduce the number of disabling work injuries. It stimulates and holds the interest of employees and management in accident prevention. Because of this, mines and quarries participating in the contest have a more favorable safety record than those operations not enrolled.

Jan 1, 1963

By Howard M. Stainer

Published X-ray mass absorption coefficients were compiled and tabulated. These coefficients are required for various X-ray analytical techniques. Values obtained from 28 authors are listed for 87 elements with both experimental and calculated points included; the wavelengths range from 4.01 to 68 A. Representative graphs are presented for six elements (lithium, nitrogen, iron, silver, holmium, and uranium. A 37-item supplementary bibliography is also included.

Jan 1, 1963

Calculations of the temperatures of metal, coke, and gas at any level in the cupola furn~ce can be carried out by means of heat balances, using data obtained from experiments with an 18 in. experimental cupola. The results can, to a certain extent, be verified by means of heat transfer calculations.The curves thus obtained, showing the variation of temperature with height in the cupola, provide a valuable picture of the heat transfer processes in a shaft 'furnace.INTRODUCTIONThe Brown Coal Research Laboratory, of the University of Melbourne, has been engaged in recent years on a programme of iron-melting tests in an experimental cupola furnace.Although the ultimate aim of this work is to develop brown coal char as a cupola fuel, most of the experimental work so far has been with conventional coke. The testing programme was designed to provide information on the effect of variables such as blast rate, metal-coke ratio, and coke size on the overall melting process, e.g. melting rate, temperature of metal tapped, and stack gas composition.However, in many cases data were obtained on conditions inside the furnace by measuring temperatures and gas compositions. The aim of the work described in this paper was to qevelop a method for using this data to obtain information on the processes taking place in the cupola.Very little research has been done on the combustion of fuels in shaft furnaces. Early work on this subject, as well as the initial stages of the Brown Coal Research Laboratory's programme, has been discussed by Evans (1959). The use of probes for obtaining information on conditions in the interior of a shaft furnace was pioneered by Belden (1913)...

Jan 1, 1963

By James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous selective flotation tests of barite-fluorspar ores from two deposits near Marion, Ky., to determine the technical feasibility of recovering commercial grade fluorspar and barite concentrates. The lignin sulfonate-sodium fluoride method of floating the fluorspar successfully produced acid-grade fluorspar concentrates. Flotation of the barite from the fluorspar tailing using petroleum sulfonate collector yielded concentrates suitable for use in compounding oil-well drilling mud. The fluorspar and barite recoveries were about 82 and 85 percent, respectively.

Jan 1, 1963

By H. L. Burmeister

This report describes the mining and milling practices used by the Eastern Magnesia Talc Co. at its Johnson, Vt., operation. The report also contains a description of the local geology and all available information on cost and performance data. Since 1925 the mine has produced continuously at an average annual rate of 54,000 tons, and the ratio of ore hoisted to finished product is roughly 2 to 1. Ore is stoped by a combination of shrinkage and sublevel methods. In any 24-hour period the mill produces an average total of 14 grades of finished talc product, 9 by dry grinding and air classification and 5 by wet grinding and flotation methods. The mine operates one shift per day, 5 days per week and the mill operates on a 3-shift, 5-1/2-day-per-week basis. Operating costs for 1958, on a percentage basis, were mining, 22.34; milling, 54.77; ore haulage, 2.89; and all other, 20.00 percent.

Jan 1, 1963

By C. Chiou, D. P. Seraphim

The effect of clustering on the superconducting properties of Al-Zn alloys has been studied by the ballistic induction techniques. The superconducting critical temperature, T,, changes when zinc-rich clusters are formed. The change in T, depends on the concentration and may be positive or negative, but always correlates with an effective decrease in the solute concentration of the alloy. Reversion after clustering effectively returns a 5 at. pct Zn alloy to the quenched state. These methods might be use&lly extended to the Al-Mg system, where X-ray data are difficult to obtain. In very dilute Al-Zn alloys, as in other tin,' indium, aluminum,2 or tantalums base solid solutions, there is a decrease in the superconducting critical temperature, Tc, roughly proportional to the temperature independent resistivity, i.e., -0.2°K per pS2cm. With increasing solute concentration, the T, generally reaches a minimum and then increases4 to a value well above that for the pure solvent. The change of T, with solute concentration follows an empirical formulation involving two constants which correlate with the scattering cross section of the impurities. As will be shown below, the Al-Zn alloys more concentrated than 1or2at. pct do not follow the empiricism, probably because they are unstable even when rapidly quenched.5 However, it seems possible to study at least the later stages of solute clustering by precise measurements of the 1', following various thermal treatments. A few experiments on quenched alloys, aged alloys, and tests on reversion are reported here. The heat treatments selected for obtaining the quenched and aged states were mainly deduced from the work of Dash and Fine.6 For the quenched state, specimens were homogenized at 480°C, quenched to -160°C, and immediately transferred and mounted in liquid nitrogen. Measurements on the superconducting properties and residual resistivities were then made at helium temperatures, after which the specimens were aged at room temperature for 3 to 5 hr, i.e., much longer than the time required for clustering to be essentially completed. The superconducting properties and residual resistivities were once again examined. To reach the reverted state of the A1-5at. pct Zn alloy, the aged specimen was heated for 5 min at 200°C and then tested as above.

Jan 1, 1963