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By J. G. Donaldson

A bench-scale method for recovering lead and zinc from slimes and mill tailings from the Tri-State District of Missouri, Oklahoma, and Kansas was developed by the Bureau of Mines. Dilute hydrochloric acid, containing sodium chloride, and chlorine gas were used to decompose the mineral constituents. Lead was electrolyzed from the pregnant acid solution, and zinc was precipitated from the depleted electrolyte by neutralization with lime. Up to 98 percent of the lead was recovered in an impure lead electro- deposit assaying approximately 85 percent lead. Zinc recoveries up to 90 percent of the total were attained in a precipitate assaying approximately 40 percent zinc.

Jan 1, 1963

By E. J. Karges

[For reasons well known to Mining Engineers, fine grinding in the wet form is quite universal inn plants engaged in the traction of metallic values from crude ore In the processing, of non-metallic and industrial minerals, however, fine grinding in dry form is the more common method. The crude materials generally contain less moisture than required for wet grinding, and the products are usually marketed or used in the dry form, most of them as powders. To grind wet would therefore entail the addition of water and the expense for drying the product, which is not justified. This paper will concentrate on the particle size reduction or fine grinding of materials to produce a dry powder]

Jan 1, 1963

By L G. White

During 1958, prospecting parties working for the Mackenzie Syndicate in the Flat River area of the Mackenzie mountains, Northwest Territories, identified tungsten mineralization and located the property now being developed by the Canada Tungsten Mining Corporation Ltd. Scheelite mineralization, associated with pyrrhotite and minor chalcopyrite, occurs in lime silicate skarn replacement zones within a limestone-chert-argillite series intruded by granitic dykes originating from the ? main batholithic mass underlying the sedimentary beds. The results of surface outcrop sampling and 15,000 feet of grid-pattern diamond drilling have been combined to outline an orebody estimated to contain 1.32 million tons, grading 2.51 per cent WO after applying a 10 per cent dilution factor for mining purposes. T HE property of Canada Tungsten Mining Corporation Ltd. is located in the upper Flat River area of the Mackenzie mountains, Northwest Territories. Skarn-type replacement deposits containing scheelite mineralization are .situated between elevations of 4,500 and 5,500 feet above sea level along the east flank of the mountain range forming the boundary between the Yukon Territory and the Northwest Territories. The nearest supply center for the area is Watson Lake, Yukon Territory, located at Milepost 635 on the Alaska Highway.

Jan 1, 1963

By Walter Kawa

The hydrogenation of phenyl ether, benzyl ether, and phenyl sulfide in the presence of iron catalysts was studied by the Bureau of Mines to gain a better understanding of the role of iron catalysts in the hydrogenation of coal. The carbon-oxygen and carbon-sulfur bonds in these compounds may be similar to some of the carbon-oxygen and carbon-sulfur bonds in coal which react during the early stages of liquefaction by hydrogenation. Experiments were made in batch autoclaves for 4 hours; hydrogen was at a pressure of about 540 atmospheres. In the hydrogenation of phenyl ether at 400° C, metallic iron catalyzed both hydrogenolysis (splitting-hydrogenation) and nuclear hydrogenation (addition of hydrogen to aromatic rings) reactions, Products were principally benzene and cyclohexane. The activity of metallic iron was decreased by adding carbon monoxide or a reactive sulfur-containing organic compound. Ferrous sulfide catalyzed the conversion of phenyl ether to benzene, phenol, and small amounts of cyclohexane. Hydrogenolysis of benzyl ether was catalyzed by metallic iron and to a lesser extent, by ferrous sulfide at 250° C. No nuclear hydrogenation was observed with either catalyst. Conversion of phenyl sulfide to benzene was nearly quantitative in experiments made at 250° C with equimolar quantities of phenyl sulfide and metallic iron or iron as ferric oxide. Conversions of metallic iron and ferric oxide to ferrous sulfide were nearly stoichiometric. No reaction of phenyl sulfide occurred in the presence of ferric oxide and water, and very little occurred in the presence of metallic iron and water. Ferrous sulfide also catalyzed the hydrogenolysis of phenyl sulfide to benzene, but conversion was lower than in experiments with metallic iron or ferric oxide. The activity of ferrous sulfide was increased by adding water and decreased by adding hydrogen sulfide. The results of this study suggest that ferrous sulfide is an active form of iron when iron is used as a catalyst for the hydrogenation of coal.

Jan 1, 1963

By Donald P. Schlick

This report presents a representative cross section of methods success- fully used to ventilate continuous-miner places as well as various factors that should be considered when selecting auxiliary ventilating equipment. Line brattice can direct fresh air to the active face reasonably well, provided that adequate area for installation is available. Continuous mining equipment, however, often restricts clearances to such an extent that proper installation of line brattice is impossible. Consequently, in many instances face ventilation is inadequate; therefore, many methods of auxiliary ventilation for continuous-mining equipment have been developed and have been discussed in this study.

Jan 1, 1963

By J. J. Pye, J. B. Drew

Mzasurements of the surface diffusion coefficients of metals have been made. Diffusion profiles for the Ag-Ag system were obtained by means of a radioactive point source and a precision auto-radiographic technique. The activation energy for silver self diffusion (=8.1 kcal per mole) is lower than that previously reported (-10 kcal per mole) on poly crystalline wire by Nickerson and Parker. The bresent data indicate an effect due to parasitic volume diffusion at temperatures above 500°C. RELATIVELY few measurements have been made of the surface self-diffusion coefficients of metals. Nickerson and arker' measured the diffusion of silver over the surface of poly crystalline wires and estimated that the activation energy was 10.3 kcal per mole. Winegard and chalmers2 carried out measurements on both polycrystalline and single crystal surfaces but did not report a value of the activation energy. They found, however, that at temperatures between 250" and 400°C the diffusion coefficients were on the order of lo-' sq cm per sec and that there was an acceleration of the migration of silver on the polycrystalline sample when a change of surface shape occurred. Winegard and Chalmers used an autoradiographic technique, hereafter designated ARG, and Nickerson and Parker used a surface scanning geiger counter in order to determine the diffusion profiles. More recently, Hackerman and simpson3 measured the surface self-diffusion coefficient of copper at a single temperature (750°C), and the value of the diffusivity (- 10-5 sq cm per sec) is in agreement with that given by jostein from his thermal grooving measurements. This paper reports the results of an investigation of the surface self-diffusion coefficients of silver over a large temperature range and describes the adaptation of autoradiographic (ARG) techniques for the determination of diffusion profiles obtained from a radioactive point source. EXPERIMENTAL PROCEDURE The experimental procedure is a modification of the method employed by Hackerman and simpson3 in their measurements on copper. A brief description of their technique is as follows: A radioactive needle which sinters to the surface during the diffusion an- neal serves as the source of diffusing atoms. After the diffusion run the needle is removed and the surface is scanned with a shielded counting arrangement. The diffusion profiles reported in this paper were obtained by a modification of the above procedure which employs a precision ARG technique. Previous investigations in this laboratory and elsewhere51B have shown that under carefully controlled developing conditions and by the use of calibration sources a linear relation exists between the concentration of the isotope and the photographic density for values below unity. The use of ARG under these conditions has advantages over the counter scanning method in that cumbersome shielding and requirements for great mechanical precision of the scanner are eliminated. Also the ARG gives a complete picture of the surface which is advantageous in studies of anisotropic diffusion. A recording microdensitometer having a 0.1 p wide slit was employed. At low temperatures the disturbing effects of subsurface radiations are negligible. The diffusion anneals are carried out in the cell shown in Fig. 1. The needle is formed by grinding down a 1.0 mm rod of high-purity silver until a tip of 0.2 mm radius or smaller is formed. This tip is plated withA"' which becomes the source of the diffusing atoms that are detected by ARG. The needle carrier and the crystal holder, Fig. 1 are constructed of quartz and ports are provided in the holder pedestal which allow free vapor circulation ((2.0 oz) and the carrier apron fits snugly over the crystal holder cap, insuring that the needle does not move and scratch the surface. Temperatures are provided by a stabilized tubular furnace which can be quickly positioned around the cell, thus bringing the crystal up to temperature in a time that is short compared to the diffusing times. The diffusion anneals range from 2 hr for the high-temperature samples to about 25 hr for those at the lowest temperature. The possibility of vapor transport of the radioactive metal as a contributing factor in the diffusion profile was investigated in two ways. One method was to suspend the needle directly over a dummy sample, raise the temperature, for periods of time equal to the diffusion times, and then take an auto-radiograph of the surface. Negligible radioactivity appeared. In the second method a thin slot in the crystal face on one side of the source provided a "cong path" for surface diffusion. If evaporation was the primary source of surface atoms the region of radioactivity around the source would be symmetrical. This was not the case. The profile dipped abruptly at the edge of the slot but on the other side of the source the usual diffusion profile appeared.

Jan 1, 1963

By William C. Miller

This report describes investigations by the Bureau of Mines designed to establish the noise level and spectrum of various types of pneumatic rock drills and to furnish information that would be useful in conducting sound measurements in mining environments and in reducing the noise generated in pneumatic drilling. These investigations show that (1) the noise generated by the drills in the frequencies below 100 cps is caused by the impact of the piston and drill steel, in the frequency range between 100 and 2,000 cps by the exhausting of air from the ports, and in the frequencies above 2,000 cps by the resonant frequencies of steel drill parts and of drill steel; (2) satisfactory instruments and instrumentation systems are available for field and laboratory measurements; (3) reliable sound measurements can be made in mining environments; and (4) devices can be developed that will abate the noise.

Jan 1, 1963

By James Westfield

This publication covers the work of the Division of Coal Mine Inspection, Bureau of Mines, as performed under provisions of the Federal Coal Mine Safety Act. It presents background information and data since 1952 when the Act became effective and includes up-to-date statistics for the calendar year 1962. During that year, approximately 9,704 coal mines were active in the United States, and the Bureau made 12,810 regular inspections. BACKGROUND The Federal coal-mine inspection program was established to carry out the provisions in Public Law 49, 77th Congress, (H. R. 2082) approved May 7, 1941. This act has since been amended as Title I, Advisory Powers Relating to Health and Safety Conditions in Mines, under Public Law 552, 82d Congress, approved July 16, 1952, which also included Title 11, Prevention of Major Disasters in Mines. Public Law 552 is known as the Federal Coal Mine Safety Act.

Jan 1, 1963

By R. F. Zaffarano

Reservoir oil in the Greater Aneth area, Utah, part of the Paradox basin, was studied to detect variation in oil characteristics within the reservoir and to determine its relation to age of accumulation and fluid equilibrium. At least three subsurface oil samples were obtained from each of the four largest of five field divisions comprising a producing area of 45,000 acres. Height of the oil column in the Pennsylvanian Desert Creek zone is about 230 ft. In general, the oil characteristics were found to be uniform across the area, and averages were developed for use in engineering applications. Average saturation pressure was 1,780 psia; the oil was undersaturated at the initial reservoir pressure, 2,200 psia. Variation in saturation pressure shows a lack of complete fluid equilibrium and continuing diffusion of solution gas from the main body of the reservoir to two extensions linked by narrow arms. By assuming early accumulation, the time involved in this diffusion process was calculated to be about the same as the age of the reservoir formation. Cause of the concentration of gas in the main body is attributed to differential entrapment during accumulation of oil and gas from an exterior source.

Jan 1, 1963

By A. S. Peck

This report presents the results of a cooperative study between the Bureau of Mines and the University of Utah to define the mechanism involved in the adsorption of oleic acid and sodium oleate on fluorite, calcite, and barite, using an infrared spectrophotometer for identifying and measuring the adsorbed reagents and reaction products. Fluorite, calcite, and barite react with oleic acid and sodium oleate in a water system, forming chemisorbed and solution products. The chemisorbed species is a surface mineral cation-collector anion salt, Chemical analysis of solution resulting from the adsorption reaction indicates that the adsorption process causes displacement of mineral anions, namely, fluoride, carbon ate, and sulfate from the surface of these minerals.

Jan 1, 1963

By L. F. Engle

There continues to be a certain magic attached to the word "Automation". When properly planned for, engineered, installed, and operated, the magic truly does take place - witness certain publicized mineral processing, metallurgical, and chemical plants. They operate successfully with few people, instead of previous dozens as in similar facilities not automated. Production quality has improved. Maintenance costs have been lowered. When such welcome results are achieved, it's proved to be a function of method and procedure in establishing criteria for choosing the intelligence and control systems followed by skilled choice of the specific elements used. The criteria, the bases for decision, are associated with design, construction, startup, operations, and maintenance. How to go about automating any process system to achieve the optimum profit depends on attention to all those aspects of a project. None of them can be forgotten if maximum satisfaction is to be gained. Control loops that look wonderful on an equipment. Piping, and Instrumentation diagram can suddenly turn into costly and. annoying problems in the field if there has been too little coordination of design. Panel boards that are literally works of art just before startup can become the largest of white elephants if an air header is inadequately sized and the pneumatic control circuits are sluggish. Conveyor belt replacement costs can skyrocket if a critical discharge chute far away from immediate operator attention lacks a simple yet effective clog-chute switch. Planning, execution, and followup of the work, the skills, and function of-the automating material can make any new project a success. An integrated owner contractor, producer-engineer approach is the key.

Jan 1, 1963

By M. Schmellenkamp

By comparing two longwall operations, one begun in 1956 and the other in 1960, the author is able to demonstrate the increases in production and performance made possible by longwall mining. These achievements have been brought about by continuous development of longwall mining equipment and associated roof supports. Because of this progress, longwall mining is able to provide, under proper conditions, high production per man-shift, remarkable cost savings, dependable roof control, safe working conditions and truly continuous production. It may seem odd that the title of this paper is not simply "Longwall Mining" but instead "Progress in Longwall Mining." However, the word "Progress" definitely has its place in longwall mining. If it had not been for progress in the development of longwall mining equipment and roof supports, the longwall mining method would not be able to compete in production and performance with modem coal mining machines. The longwall mining method was practiced at the beginning of the century and there were several successful operations in coal fields in Illinois. In those early days of longwall mining, the coal was undercut by hand 2 to 2.5 ft at the bottom of the seam and packwalls were built in the gob to support the roof. The roof eventually subsided and the weight of the subsiding roof was used to ride the face and break the undercut coal. Utilizing natural weight to soften the coal face is still practiced in modern longwall mining; however, the packwalling method has been replaced by the caving method and the roof is now supported by yielding steel roof supports and forepoling steel headers. The purpose of these yielding-type roof supports is to provide a safe working area for the crew along the entire longwall face, to permit continuous mechanical mining across the prop free face, and to provide a strong resistance for the roof by forming an even breaking line at the gob for the roof to cave. Roof supports and associated forepoling headers should be kept as close as possible to the face in order to prevent a caving between face and supports, especially under friable roof. This means that the coal should be extracted in small slices, allowing only a narrow roof area to be exposed and unsupported. The coal planer with its relatively high cutting velocity of 75 ft per min provides such an extraction of coal and has proved its high performance under difficult mining conditions. Since 1951, several longwall faces in southem West Virginia and Pennsylvania which have been equipped with the coal planer and friction-type manual roof supports have been successfully operated. Compared to today's longwall mining, these longwall faces required such a large crew, primarily to handle the roof supports, that the actual high production per shift was charged with too high a labor cost, thereby decreasing the tons per man. Yet, even then the longwall faces outperformed the conventional mining system under the same conditions. In order to demonstrate the progress that has been made in the development of longwall mining, a comparison will be made between a longwall face in Arkansas which was installed in 1956 and a modemized longwall face started in 1960 in southern West Virginia. LONGWALL MINING IN 1956 The 320-ft longwall face was developed in a 32-in. thick coal seam near Greenwood, Ark. The method of mining the 320-ft coal block was the advancing system in which three entries on either side of the face were driven ahead of the advancing longwall face. The face was equipped with a coal planer and a Panzer conveyor; timbering was done with wooden timbers and cribs. The roof supports were set without any pattern. The crew to operate the planer and to handle the roof supports (timbers and cribs) consisted of 15 men per shift. During a period of approximately eight monthsof single shift operating time, the average tonnage produced in this relatively low seam amounted to about 263 tons of clean coal per shift. To show the development in the coal plow from then until now, it should be pointed out that the standard plow was used in this operation. The plow was equipped with rigid bottom bits which could not be adjusted if the plow started to climb, thereby leaving bottom coal to be recovered by pick hammers end causing delays in production. The height of the plow

Jan 1, 1963

By M. Mohan Rao

A Sievert ' technique was used. The few determinations made on 10 per cent and 20 per cent V alloys did not show any deviations from Sieverts' law up to I>N2 = 1 atmosphere. The same held true for alloys of 0.2 per cent Ti. Nitrogen absorptions in Fe-Ti alloys, containing from 0.50 to 0.77 per cent Ti at 1,600°C, follow Sieverts' law at low PN2 values, but, due to the formation of a delta titanium nitride phase, deviate from this law beyond critical values of PN2? There is evidence that this phase is Ti1.1N. The behavior observed can be described by the followmg equations: Ti,.,N(o) = 1.7Ti + N K = (fT; ? % Ti)1?7 (f;;.? %~_) = 0.0020 K = fN. %~ = 0.042 '\)-:>N 2 I NTRODUCTJON Nitrogen's solubility in liquid iron-vanadium alloys was investi-gated briefly by Brick and Creevy ( 1), and more extensively by Kash-yap and Parlee (2) and by Pahlke and Elliott (7). Nitrogen's solubility in liquid iron-titanium alloys

Jan 1, 1963

By Charles Prasky

This report describes and appraises recent progress in the development of a differential sulfatizing process for recovering a ferrograde manganese oxide from low-grade manganiferous ferruginous materials in the Cuyuna range. Individual process steps were carried out successfully using a 20-inch-diameter shaft for continuous countercurrent sulfatization of the manganese, a multiple-compartment rotary drum for leaching the water-soluble manganese sulfate, a submerged-combustion evaporator for the recovery of monohydrate crystals of manganese sulfate, and a shaft furnace for the thermal decomposition of sulfate crystals for production of a ferrograde manganese oxide and a sulfur dioxide gas suitable for sulfatization of fresh are. Of the two general kinds of Cuyuna manganiferous materials--the carbonate slates and the oxidized ores--only the slates were studied at pilot scale.

Jan 1, 1963

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 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 W. P. Evans, R. W. Buenneke

Warren and Averbach's multiple order, Fourier method was applied to solid specimens of SAE 1045 steel. The material was hardened to three hardness levels and specimens of each hardness were shot peened to three intensities. Particle size, root-mem-square strain, mean strain, md macro residual stress were determined for each. Microstrains caused by either hardening or peening varied markedly over microregions. In general, increasing the hardness or peening intensity increased the rms strain and decreased the particle size. Similar effects were observed by varying hardness and peening intensity independently. At a Rockwell hardness of C 50, peening had little effect on line broadening, but both mean strain and macro residual stress increased. Mean strain was independent of column length. Induced macro residual stress by peening was affected most by initial hardness, but not by specific peening intensity. The purpose of this work is to establish the state of residual strain and particle size by X-ray diffraction in hardened and cold-worked plain carbon steel and attempt to relate these X-ray measured parameters to fatigue performance. X-ray line broadening (and its micro implications), along with X-ray residual stress (and its macro implications), may be basic indicators of the inherent fatigue resistance of the material. X-ray line broadening is caused by variable lattice strains and small particle size. Both are a result of plastic deformation which accompanies hardening or cold working processes. Therefore, X-ray line broadening is a good measure of both. warren1 has recently reviewed the Warren and Averbach2,3 Fourier analysis of line broadening. Strain and particle size effects can be separated because broadening due to particle size is independent of order of the diffraction peaks, while broadening due to strain is not. Microstrain is obtained as a root-mean-square strain averaged over discrete distances within the crystals causing diffraction. These distances are quite small, varying from 10 to 10081, and may be interpreted as the gage length over which the strains are averaged. Because of their variable nature, the X-ray line is broadened. The plot of rms strain vs distance (or column length) within the specimen gives a measure of their variability. Small particles also cause X-ray line broadening as already mentioned. A particle is interpreted as a region within a crystal or grain which diffracts X-rays coherently. This region is one of given orientation and may be bounded by a small angle grain boundary, dislocations, a twin boundary, or a stacking fault. The present work covers measurement of X-ray line broadening and macro residual stress on an SAE 1045 steel, quenched and tempered to various hardnesses. Various amounts of cold working were produced by shot peening the surfaces to various Almen intensities. Particle size, root-mean-square strain, and mean strain were calculated from the Fourier coefficients of the X-ray diffraction profiles in a direction normal to the peened surface. No effort was made to separate the various causes of particle size broadening. Macro residual stresses were reported in directions parallel to the peened surface. I) X-RAY METHOD The Fourier coefficients were determined for the 110 and 220 X-ray profiles. They were corrected for instrumental broadening by the method of Stokes,4 using an annealed reference specimen of similar geometry presumed to be free from broadening due to small particles and distortions. The nth Fourier cosine coefficient, A,, is related to a particle size coefficient, Ap, and a distortional coefficient, ADn, by the equation:

Jan 1, 1963

By John L. Burnett

Field criteria are needed to help the prospector recognize a potentially expansible shale, clay, or slate. Certain criteria have proven useful in California even though the physical-chemical mechanisms of expansion are not thoroughly understood. Three conditions must be satisfied before expansion can take place, The raw material must partially fuse at a low temperature (1800-2000°F.), Concurrently a gas must form. The raw material must be sufficiently impermeable to trap the gas within the particle. Low temperature melting, which is controlled by bulk chemical composition, is difficult to assess in the field but most common shale, clay, and slate is suitable in this respect, The presence of organic carbon, the most common source of an expanding gas, is indicated by dark color of the rock, A large proportion of clay-sized particles promotes impermeability; fine grain-size is indicated by conchoidal fracture, The shape of the expanded particle is commonly indicated by the texture of the raw material. Rocks with well-developed slatey cleavage produce accordion-shaped particles; massive rocks tend to form rounded particles. Undesirable materials commonly present with expansible shale include: weathered shale; sandstone and other coarse-grained sediments; and limestone, Weathering, which is indicated by color, reduces or eliminates expansion; therefore, surface samples seldom are representative of the shale found at depth. Sandstone does not expand and will increase the average weight of the finished product, Limestone or particles of carbonate minerals can be actively harmful because they are converted to free lime (CaO) during the firing process, If free lime is present in concrete, hydration will cause expansion of the lime particles which result in surficial ?popouts.?

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