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By R. H. Richman, F. Borik

A 0.3 pct C-12 pct Cr-6 pct Ni steel was rolled to 93 pct reduclion in area as austenite at 510°C, and then partially transformed as desired to ~rlartensite by qnenching to - 196°C. Pole figures for the austenitic matrix and for the martensitic product were separately determined by an X-ray transmission method. The deforitration texture of' the warm-worked austenite is characlerized by (110)(225) components, and is thus closely similar to those produced in a brasses. The pole jigure of the martensite in partially transformed material agrees well with that which can be constructed by transfortnation of the {110)(225) orientations according to either the Kuvdjuniov- Sacks or the Nishi-yatuu relatiotship. Howeuer, an important result of this construction is that me-third of the predicted orientations are missing. A graphical analysis can then be used to show that in deformed austenite certain crystallographic variants of martensite (related to the most probable austenite slip systems) are suppressed, resulting in this preferred transformation. The evidence for preferred transformation is corroborated by the measured elastic anisotropy of warm-rolled and fully transformed H-11 steel. EXTENSIVE plastic deformation of a polycrystal-line aggregate in a manner that causes flow predominantly in one direction results in a preferred orientation of the constituent crystallites. The particular orientations that are produced depend upon the crystal structure and composition of the material, as well as upon the temperature, mode, and degree of deformation; in any case, the preferred crystallo-graphic orientations, or textures, are reflected in directionality of mechanical properties. Although such anisotropy may be exploited in certain specialized applications, it is more commonly diminished or eliminated by heat treatment lest it interfere undesirably in subsequent forming operations or in structural design. In the recently developed thermomechanical treatments that significantly enhance the strength of some steels,1,2 considerable deformation of the metastable austenite prior to the martensite transformation is essential to the strengthening process. If the austenite is textured by the deformation, and if the transformation to martensite proceeds according to one of the relationships established for transformation in annealed austenite, then it must be expected that the martensite will also possess a preferred orientation even though the multiplicity of martensite orientations possible in a given austen- ite crystal will tend to restore some degree of randomness. The existence of a residual anisotropy, both mechanical 3-6 and crystallographic,' has been substantiated. In the latter crystallographic investigation, preferred orientations were determined for the martensitic structure of an SAE 4340 steel rolled 72 pct as austenite at 833°C and then quenched. However, the choice of a composition that transformed almost completely to martensite during the quench to room temperature did not permit direct measurement of the prior austenitic texture. In fact, when the "ideal orientations'' associated with well-known fcc rolling textures were converted, alone or in combination, to martensite according to the Kur-djumov-Sachs (K-s)' or Nishiyama8 relations, the agreement obtained with the observed martensite texture was only fair at best. Recently a pertinent aspect of the austenite to martensite transformation was reported by Bokros and parker,10 who found that certain habit-plane variants of martensite were suppressed by tensile deformation of Fe-31.7 Ni single crystals prior to the necessary subzero cooling. It might be anticipated that the consequences of such preferred transformation are sustained during the formation of martensite in warm-worked austenite that has a well-developed deformation texture. The present investigation was undertaken first to establish more firmly the relation between preferred orientations in plastically deformed austenite and in the resulting martensite, and second to examine the textures for evidence of deformation-induced preferred transformation. EXPERIMENTAL PROCEDURES An alloy containing 0.3 pct C, 12 pct Cr, 6 pct Ni, and the balance iron, was selected because the mar-tensite-start temperature (M,) of about -100°C allowed convenient experimental manipulation of either austenite or martensite at room temperature. Furthermore, this composition can be readily deformed as metastable austenite at moderately elevated temperatures without intervention of appreciable isothermal or athermal decomposition products. The alloy was austenitized at 1150°C, aircooled to 510°C, rolled unidirectionally at this temperature to 93 pct reduction of cross-sectional area, and finally oil-quenched to room temperature. Partial transformation to martensite was accomplished by quenching to -196°C as needed. The rolled stock was reduced in thickness from 0.067 to 0.010 in. by etching in a solution of 5 pct HC1, 45 pct HNO3, and 50 pct water, and further thinned by careful mechanical polishing to maintain the two sides of the sheet parallel within 0.0003 in. After mechanical polishing to 0.005 in., electropolishing in 1:9 perchloric-acetic acid solution produced a final thickness of 0.002 in. The preferred orientations were determined from

Jan 1, 1968

By Thomas Fraser, David R. Mitchell

THE primary purpose of the loading plant is to transfer the finished product from the preparation machines to the railroad car, truck, or barge in which it is to go to market. Secondary purposes of the loading plant are: to prevent excessive degradation of sizes during loading, to reduce segregation as much as possible, and to prevent excessive quantities of very good or off-grade coal from entering any one car. Nonuniformity of consignments is one of the chief sources of com- plaints by consumers and coal merchants. A properly designed loading plant will do much to reduce complaints and ensure uniformity, not only from shipment to shipment but also in each individual consignment along the length of the car and in cross section. DEGRADATION IN STORAGE, LOADING AND SHIPMENT The object in loading is not only to handle the coal without breakage and segregation, but also to produce a well-trimmed load that will ride to its destination without spillage or breakage en route. The small sizes present in a car of prepared coal as received by the purchaser consist of: missed small sizes not screened out in the preparation plant, breakage during loading, and breakage caused by handling en route. For domestic sizes of anthracite shipped from the Pennsylvania anthracite field to Atlantic coast cities, the dealers' loss because of break- age in loading and shipment amounts to from 2 to 5 per cent and for anthracite shipped to Middle West cities, the loss is 8 to 9 per cent. This difference is in part because dealers in the Middle West rescreen their coal more thoroughly than is usual in the East. One dealer handling Illinois No. 6 coal shipped from southern Illinois mines to Chicago reports an average size loss of 10 per cent when lump coal is unloaded with a fork. This runs as low as 5 per cent for carefully loaded coal and as high as 15 per cent for carelessly loaded coal.

Jan 1, 1943

By John P. Harmon

This paper was written with two objects in view: (1) To describe in detail what has been done toward the ventilation of the main unit of the Portovelo mines and the results; (2) to give information that may be useful to anyone who may have to make a preliminary mine ventilation survey, with recommendations for the improvement of the existing system and finally the maintenance of the improved system. General Description The mining operations of the South American Development Co. at Portovelo, Province of El oro, Ecuador, are described here only briefly, as a full discussion does not fall within the scope of this paper. The orebodies are of the steeply dipping, gold quartz vein type, averaging about 2.0 meters wide. As shown in Fig. 1, the ore chutes are relatively far apart, making considerable development work necessary before connecting raises can be driven between the levels. Faulting' on a large scale and a parallel vein system have made long dead-end drifts and many crosscuts necessary in the exploration of veins. The ventilation of these dead ends is described under Auxiliary Ventilation. The method of mining2 is the filled rill stope method, similar to the method that is largely employed at the Butte mines. The main shaft of the mine is in the Amarillo Valley, on either side of which mountains rise abruptly to a height of several hundred feet above the collar of the shaft. Entrance is made to the mine: (1) Through the American shaft, which extends vertically from the surface to a depth of 1100 ft., of which only the first 700 ft. are in active use at the present time; (2) levels are driven from the American shaft at intervals of 30 m. (100 ft.), of which only the third, fifth and seventh levels need be considered in the ventilation problem; (3) adits at intervals of 30 m. (100 ft.), with a few exceptions, above the collar of the American shaft.

Jan 1, 1931

By R. F. Mehl, J. T. Ransom

For many years the Metals Research Laboratory of Carnegie Institute of Technology has been concerned with the statistical nature of the engineering properties of steel from an experimental viewpoint, particularly those properties representing ductility.' In the past three years new work has been directed toward evaluating the statistical nature of the endurance properties. It has been shown that both the fracture curve and the endurance limit in fatigue are markedly statistical in nature. The S-N curve (and the endurance limit) of ferrous materials is often determined with specimens which number as few as ten. The common procedure is to test the first specimen at a stress well above the expected endurance hmit. Each succeeding specimen is then tested at a progressively lower stress, until, after five or six tests, a specimen runs ten million or so cycles without failing. Two or three more specimens are then used to find the highest stress at which failure will not occur; the limiting stress determined in this way is called the endurance limit. It has now been found, however, that the variability in the fracture curve and in the endurance limit in heat-treated alloy forging steels is so great that S-N curves must be drawn on the basis of distribution curves which can be appraised only by statistical methods. Two methods have been adopted in this study: (1) straightforward statistical studies of cycles to fracture of a number of specimens at each of a series of stress levels, and (2) a new abbreviated statistical method, known as "staircase testing."2 The latter corisists in testing a series of specimens, one by one, with the test stress for any given specimen automatically

Jan 1, 1950

By Frederick Laist

(Butte Meeting, August, 1913.) WHILE remodeling No. 1 section of the concentrator at the Washoe Reduction Works of the Anaconda Copper Mining Co. during the summer of 1912, for the purpose of ascertaining what additional metal recoveries could be made by improvements in concentration practice which had been developed by the staff of the Boston & Montana Reduction Department, at Great Falls, it was deemed advisable to carry on some experiments on the treatment of the regular mill tailings by roasting and leaching, to see whether the losses of metal values might not be still further decreased. In the course of these experiments about 5,000 tons of tailings were roasted, and of the resulting calcine about 200 tons were leached. The results were so satisfactory that it was decided to continue the work on a larger scale, particularly as regards the leaching end of the process, and construction work on an 80-ton roasting and leaching plant was accordingly commenced during the latter part of February, 1913, and is being pushed as rapidly as possible. 80-Ton Leaching Plant. This plant will consist of one 20-ft. roasting furnace of the MacDougall type, specially adapted to the work of roasting for leaching; two leaching tanks, .32 ft. in diameter by 12 ft, deep, together with the necessary solution tanks, air lifts, precipitating launders, etc. It has been decided to precipitate the copper from solution on scrap iron, so as not to hamper the roasting and leaching departments by any weakness that might develop in the precipitating department. It is, however, the intention to experiment with a number of different methods of precipitation ; for example, by electrolysis and by hydrogen sulphide.

Jan 7, 1913

By L. C. Brown, S. K. Behera

The diffusion rate in Ag-Sb couples is sensitive to con~pressive load with the width of Ag3Sb, the only phase present in the diffusion zone, increasing with stress up to 800 psi and remaining constant above this. Kirkendall marker experiments show silver to diffuse much faster than antimony in Ag3Sb and incipient porosity may therefore develop at the Ag/Ag3Sb interfnce restricting the transfer of atoms from the silver into the diflusion zone. Application of compressive stress reduces the tendency for porosity to develop and so increases the growth rate. In a recent paper Brown et al.1 observed a significant increase in the thickness of Cu2Te in Cu-Te diffusion couples on application of a compressive stress as low as 20 psi. Similar stress effects have also been observed in the Fe-A1,2 Al-u,3 arid cu-sb4,5 systems. It has been suggested that the increase in growth rates of intermetallic phases in these systems is due to a decrease in the amount of Kirkendall porosity with applied stress. In the present paper, results are presented of the effect of compressive stress on diffusion in Ag-Sb, together with a detailed examination of the Kirkendall effect. The Ag-Sb phase diagram6 shows that antimony has a moderate degree of solid solubility in silver, 5.7 at. pct at 350°C, but that there is essentially no solubility of silver in antimony. There are two intermediate phases— (hcp7) from 8.8 to 15.7 at. pct Sb and Ag3Sb (orthorhombic8) from 21.8 to 25.9 at. pct Sb. EXPERIMENTAL Diffusion couples were prepared from fine silver of 99.95 pct purity and from antimony of 99.7 pct purity. Both the silver and antimony were produced in the form of discs 1/2 in. in diam by approximately $ in. thick, with surfaces ground flat to 3/0 emery paper. Diffusion anneals were carried out in the apparatus previously described.1 A compressive load was applied to the diffusion couple through a lever arm system, with a reproducibility estimated to be ±10 psi. All runs were carried out in a protective hydrogen atmosphere. Following the diffusion anneal specimens were sectioned and polished and the width of the diffusion zone was measured metallographically. Composition profiles were measured using an electrostatically focused electron probe with a spot size of 10 , counting on Sb L radiation. Corrections for matrix absorptiori and fluorescent enhancement9 were not required. S. K. BEHERA, formerly Graducate Student, Department of Metallurgy, University of British Columbia, is now Postdoctoral Fellow, Whiteshell Nuclear Laboratories, Atomic Energy of Canada Ltd., Pinawa, Manitoba. L. C. BROWN, Junior Member AIME, is Associate Professor, Department of Metallurgy, University of British Columbia, Vancouver, B.C., Canada. Manuscript submitted June 14, 1968. IMD RESULTS Fig. 1 shows an electron probe traverse of a typical diffusion zone. In all couples examined only one intermediate phase was observed and the composition of this phase, 23 wt pct Sb, was in good agreement with the composition of Ag3Sb, 23 to 28 wt pct Sb. The presence of this phase was confirmed by X-ray diffraction of filings taken from the diffusion zone. The probe traverses showed no detectable solid solubility in either the silver or the antimony although the phase diagram indicates that some antimony, up to 6.5 wt pct pct Sb, should be in solid solution in the silver. However the width of this portion of the diffusion zone would be expected to be very small in view of the low diffusion coefficient in the silver, 4 x 10-l6 sq cm per sec at 350°C, 10 compared with that in the Ag,Sb, estimated as 3 x 10-8 sq cm per sec in the present work, and this region would therefore not be expected to be seen in the probe traverse. Application of stress resulted in a significant increase in the width of the diffusion zone, Fig. 2. At 350°C, the thickness of Ag3Sb increased from 250 at 0 psi to 400 p at the limiting stress of 800 psi, indicating an apparent 150 pct increase in the diffusion coefficient. Similar behavior was also observed at 400°C, indicating that the stress effect is not characteristic of just one temperature. The growth of Ag3Sb at 350°C and at various stresses is shown in Fig. 3. In every case the growth rate was parabolic indicating diffusion control. The kinetic curves all passed through the origin showing that delayed nucleation of Ag3Sb was not responsible for the stress effect and that it was a real growth effect. A series of tests were carried out in which diffusion was allowed to take place at a lower stress following an initial high stress diffusion anneal. Speci-

Jan 1, 1969

By C. G. Dunn, F. Lionetti

The energy associated with grain boundaries in polycrystalline aggregates is believed to play a major role in grain growth processes and, when growth ceases, to determine the final equilibrium grain boundary angles. Further, the energy of grain boundaries of recrystallization nuclei is a factor in nucleation processes. It is important to know, therefore, how the energy per unit area of a grain boundary, that is, the grain boundary surface tension y, depends on the difference in orientation of the two lattices of the grains producing the boundary. Although the problem is important, surprisingly little has been done toward a quantitative evaluation of the effect of orientation difference on grain boundary energies. C. S. Smith1 recently has discussed this problem and in addition to showing effects of orientation difference on equilibrium angles has shown a variety of interesting effects of surface tension on the appearance of microstructures. Fig 1 and the following relations expressed in Eq 1, which connect equilibrium grain boundary angles and surface tensions, illustrate equilibrium conditions which are believed to hold true in metals. ?l2 _ ?23 _ ?l3 [1] sin ?3 sin ?1 sin ?2 Clearly any two of these surface tensions can be expressed in terms of the third when the equilibrium angles ?1, ?2, and ?3 are known. Applied to the present problem for solid state equilibrium of three grains, the angles ?1,?2 and ?3 must be measured in a plane perpendicular to the line of junction of the three grains. Normally a direct determination of these angles from random microsections is impossible. Consequently Harker and Parker2 and Smith1 (except for some measurements on flat specimens) resorted to a statistical method to determine equilibrium grain boundary angles. Smith reported that grain boundaries meet the surface of a piece of metal nearly perpendicularly. He reported also, in connection with direct angle measurements on flat specimens with grains extending through the thickness, that angles varied appreciably from 120" and concluded that there was a measurable effect of orientation difference on surface tension. Another direct way of determining equilibrium angles and a method adaptable to studying particular configurations, recently suggested by Dunn,³ is to use a three-grain flat specimen with orientations of grains so chosen that the junction line of the three grains will be straight throughout the thickness and perpendicular to the surface of the specimen. Choice of orientations is possible when individual grains of each group can be grown to predetermined orientations through the reorienting and growth of " seed crystals " as described.³ Not only is it possible, for example, to have grains with the same crystallographic plane in the plane of the specimen, but a given orientation difference between two grains can be made a common factor to an unlimited number of three-grain groups while a series of orientation differences is investigated. Any effect of anisotropy of gas-solid surface tension due to grain orientation should be minimized by having all gains oriented the same with regard to crystallographic plane in the plane of the specimen. Another feature of the three-grain group is the notched grain boundaries as shown in Fig 2 for one specimen (S4). The notches serve to anchor the end positions of the grain boundaries (especially at high temperatures) while the central and junction point of the grains moves toward an equilibrium position. Final equilibrium should produce straight grain boundaries if the notches are very narrow and if changes in orientation* of the grain boundary do not alter the surface tension.† If one assumes the straight line condition and no change of surface tension with small changes in grain boundary orientation and finds the equilibrium configuration by a minimization of the grain boundary energy, one obtains the relations given in Eq 1. The approach to straight line boundaries or to minimum energy configurations in specimens containing large grains, such as those used in the present investigation, may be very slow compared with the approach to equilibrium conditions for the grain boundary angles. It may be desirable, as proved to be the case in the present investiga-

Jan 1, 1950

By W. D. Robertson

The effect of a tensile stress in accelerating the corrosion-cracking of certain alloys of aluminum, magnesium and iron is widely recognized. The literature is extensive and it is only necessary to cite the recent ASTM—AIME Symposium,l There are, however, no experimental data conclusively showing the effect of an applied compres-sive stress. It has been inferred, from the generally accepted mechanism postulated for the acceleration of corrosion by an applied tensile stress, that a compressive stress would inhibit corrosion. Furthermore, it is observed that corrosion cracks invariably start on the tension side of a specimen bent as a simple beam. This observation has led to the suggestion that shot-peening of the surface would inhibit or eliminate stress-corrosion cracking in magnesium alloys and aluminum alloys. However, the degree of inhibition produced by shot-peening does not appear in the literature except for the above qualitative references which are unsupported by experimental data. Moreover, while peening undoubtedly imposes a surface compressive stress, the alteration of the surface by the severe cold-working involved complicates the interpretation of the results with respect to the effect of a compressive stress alone. If corrosion proceeds along preferential paths produced by precipitation from solid solution, it is easily understood how a component of tensile stress normal to these paths will accelerate the corrosion and lead to ultimate failure. On the other hand, if the metallurgical conditions are such as to create preferential corrosion paths, then it is difficult to understand how a compressive Stress, produced by shot-~eening Or any other method, can inhibit corrosion except in the sense that the accelerating factor is removed. Thus, if the basic corrosion mechanism remains unaltered, there should be little or no inhibition resulting from the application of a compressive stress if inhibition is defined as the reduction of the degree of corrosion below that experienced in the unstressed state. The experiment described below was performed to isolate and evaluate the effect of a compressive stress on the corrosion and stress-corrosion cracking of a high strength aluminum alloy (24-S); and, by a Comparison of the corrosion rate of 'pecimens subjected to an applied tensile stress, compressive stress and in the unstressed state, to clarify the role of stress in intergranular corrosion. Experimental Procedure The experiment was conducted with the aluminum-copper-magnesium alloy known as Duralumin 24-S.* Specimens, 0.064-in. thick, in the form of I-in. wide strips sheared parallel to the rolling direction,

Jan 1, 1949

By W. W. Anderson, D. G. Girton

The photoluminescence of Pr, Nd, Ho, Er, Tm, and Yb in CdS, and Ho, Er, Tm, and Yb in ZnSe has been observed from crystals Prepared by diffusion using rare earth metals and an excess chalcogen pressure. For a given temperature, time, and chalcogen pressure the spectral characteristics were very reproducible from run to run, and the emission intensity for Nd, Er, and Yb in CdS was as high or higher than the best vapor phase doped crystals we have grown. For a few rare earths it was found that certain conditions of diffusion tend to yield optimum rare earth emission intensity with respect to the background lattice emission. Photoluminescence measwements of Yb in CdS as a function of depth gave a profile which was neither a Gaussian nor complementary error function. Part of the profile appears to arise from a fast component of the diffusion and the other part from a slow diffusing component. At 960°C and 33 atm S pressure, a com -plimentary error function approximation of the slow diffusing component gave a diffusion coefficient of D = 1.3 x 10-9 sq cm per sec. MOST of the studies of emission from rare earth ions in II-VI compounds have been reported on crystals doped during growth,1,2 although Kingsley and Aven prepared ZnSe:Er by diffusion for paramagnetic resonance and fluorescence studies. Pappalardo and Dietz prepared CdS:Yb by diffusion, but they made optical absorption measurements., We know of no study on the properties of rare earth diffusion in the II-VI compounds. To date we have diffused Pr, Nd, Ho, Er, Tm, and Yb into CdS, and Ho, Er, Tm, and Yb into ZnSe and observed the rare earth emission spectra. For a given temperature and chalcogen pressure, the emission characteristics are very reproducible from run to run and for Yb, Nd, and Er in CdS, as good as the best crystals we had prepared by doping during vapor phase growth.2 The emission of Pr, Ho, and Tm has been observed in CdS prepared by diffusion for the first time. Previous attempts2 to prepare these later three materials by vapor phase growth were unsuccessful. The problem of obtaining reproducible characteristics in II-VI semiconductor compound work is well known.5 Not only is it difficult to reproduce results from one laboratory to another but it is sometimes difficult to reproduce results from one growth run to another under ostensibly identical conditions within one laboratory. This situation has been particularly bothersome in research on the luminescence of rare earth activated ZnS1 and Cds2. Crystals from one vapor phase growth run would show very strong rare earth line emission while crystals from a nearly identical run would show no rare earth emission. It was also observed on occasion that the intensity of the rare earth emission was not constant over the entire volume of a single crystal. MATERIAL PREPARATION AND INSTRUMENTATION Vapor phase grown boules of CdS were supplied by Dow Corning. This material was characterized by a free electron concentration of n - 3.5 x 1015 cm-3 and Hall mobility of 350 sq cm per v sec at room temperature. There were microscopic voids and decorated precipitates in some samples. The precipitates annealed out at diffusion temperatures but the voids remained. Single crystal rectangular samples of mm dimensions were sawed from the boules. The ZnSe was polycrystalline, UHP grade from Eagle-Picher. Poly-crystalline samples were sawed from the ingots. The samples were lapped, polished on one side, etched in a solution of 0.5 M K2Cr2O7 in 16 N H2SO4, and thoroughly washed in distilled water. A sample, excess sulfur (or selenium), and 5 mg of rare earth metal (turnings) were sealed in a 3.6 cm3 quartz ampoule at about 2 X 10-5 torr. The high chalcogen pressure used (1 to 30 atm) prevented thermal etching of the crystals and affected the diffusivity and solubility of the rare earth ions in the crystal lattice. For meaningful or reproducible results, it is thus necessary to specify the vapor pressure at which the diffusion was carried out. It is assumed that a negligible amount of the chalcogen was used in the formation of rare earth sulfides or selenides Our sulfur vapor pressure calculations are based on data assuming S2, S6, and S, molecules only in which case the equilibrium constants are given by6 where the pressures are expressed in torr. Selenium vapor consists of a mixture of Se2, Se4, Se6, and Se6 molecules. The selenium vapor pressure was calculated using equilibrium constants given by The status of the rare earth source during diffusion is unknown, i.e., the partial pressures of the rare earth metal and of the rare earth chalcogenides has not been determined. All emission spectra were recorded at 77°K on a Perkin-Elmer model 98-G spectrometer using a 640 line per mm grating. No correction was made for the spectrometer and detector spectral sensitivity. Excitation was by means of an XBO 1600 w xenon arc

Jan 1, 1970

By J. S. Wakeman

The techniques of testing the physical properties of green pellets produced in a batch balling test are described. It has been found that these physical properties, i.e. drop resistance, wet compressive strength, and plastic deformation under load, are generally related to the moisture content of the wet balls. A "criterion" method of analyzing data from a series of batch tests is discussed. This method facilitates the comparison of results of various test series. A time-sharing computer program, which correlates the test data from a batch series, generates the "criterion" values for subsequent comparison and analysis, and produces X, Y plots of the various moisture-strength relationships, is presented. Examples of computer output and use of the "criterion" evaluation method are given.

Jan 1, 1973

By Chase Palmer

INTRODUCTION. WHILE the reducing action of organic matter, of ferrous sulphate, and of hydrogen sulphide has frequently been invoked to account for the deposition of native gold and silver from ore-forming solutions, the high efficiency in this respect of certain of the metallic minerals which form the ore itself has not been sufficiently recognized. If a little finely powdered chalcocite is placed. in a test-tube and 2 or 3 cc. of a dilute solution of gold chloride are poured over it, two or three shakes of the tube suffice to remove all the gold from the solution. The color of the solution changes from yellow to pale green, showing that copper is dissolved simultaneously with the precipitation of metallic gold. If a piece of chalcocite is hung in a dilute aqueous solution of silver sulphate (1 normal), a coating of silver begins immediately to form on the mineral, and within a few moments a beautiful silver tree has developed, similar to that formed when metallic zinc is immersed in a similar solution.

Jan 5, 1913

By J. J. Forbes

'"THE Federal Coal Mine Safety Act (public Law T. 552. 82nd Congress) was approved oil July 16, 1952. It incorporates, as Title I, the Coal Mine Inspectio1.1 and Investigation Act of May 7. 1941 (Public Law 49, 77th Congress), which gave Federal inspectors only the right to enter. coal mines for inspection and investigation purposes but no power to require compliance with their recommendations. Title 11 contains the enforcement provisions of the act; its purpose is to prevent major disasters in coal mines from explosions, fires. inundations. and man-trip 01. man-hoist accidents. At this point a brief account of events that preceded the enactment of the Federal Coal Mine Safety Act seems appropriate. The hazardous nature of coal mining was recognized by the Federal Govermment as long ago as 1865, when a bill to create a Federal Mining Bureau was introduced in Congress. Little was done, however, until a series of appalling coalmine disasters during the first decade of this century provoked a demand for Federal action. As a result an act of Congress established a Bureau of Mines in the Department of the Interior on July 1, 1910. The act made it clear that one of the foremost activities of the Bureau should be to improve health and safety in the mineral industries. One of the first projects selected by the small folce of engineers and technicians then employed was to determine the causes of coal-mine explosions and the means to prevent them. By investigations aftel mine disasters the fundamental causes and means of prevention were soon discovered, and the coal mining industry was informed accordingly. However, despite this knowledge and the enactment of State laws and the Federal Coal Mine Inspection and Investigation Act of 1941, mine disasters continued to occur with disheartening frequency and staggering loss of life. The devastating explosion at the Orient No. 2 mine on December 21, 1951, resulted in the death of 119 men. The Orient disaster rekindled the memory of the Centralia. Ill., disaster of March 25. 1947, which caused the death of 111 coal miners. These two tragedies ultimately brought about enactment of the Federal Coal Mine Safety Act. The act is a compromise measure. Senator Matthew M. Neely of West Virginia and Congressman Melvin Priec of Illinois introduced almost identical versions in the 82nd Congress, but they were considered too drastic. The final version was introduced by Congressman Samuel K. McConnel, Jr., of Pennsylvania, after considerable discussion and amendment in committee hearings. It was passed by the Congress and became effective when signed by the President on July 16, 1952. The act is somewhat limited in scope because it applies only to approximately 2000 coal mines in the United States and Alaska that employ regularly 15 or more individuals underground. It exempts approximately 5300 mines employing regularly fewer than 15 individuals underground and all strip mines, of which there are about 800. Moreover, it covers only conditions and practices that may lead to major disasters from explosion, fire, inundation, or man-trip or man-hoist accidents. According to Bureau records, such accidents have resulted in less than 10 pct of all the fatalities in coal mines. It is important to mention that the law is not designed to prevent the day-to-day type of accidents that have caused the remaining 90 pct or more of the fatalities, because it was the specific intention of the Congress to reserve the hazards which caused them to the jurisdiction of the coal-producing states. Many who opposed any Federal legislation that would give the Federal inspectors authority to require compliance with mine safety regulations claimed that such legislation would usurp or infringe upon States' rights. To assure that the principle of States' rights would be preserved, the act provides for joint Federal-State inspections when a state desires to cooperate in such activities. The Director of the Bureau of Mines is required by the act to cooperate with the official mine-inspection or safety agencies of the coal-producing states. The act provides further that any state desiring to cooperate in making joint inspections may submit a State plan for carrying out the purposes of this part of the act. Certain requirements are listed: these must be met by a state before the plan can be accepted. The Director of the Bureau of Mines, however, is required to approve any State plan which complies with the specified provisions. The Director may withdraw his approval and declare such a plan inoperative if he finds that the State agency is not complying with the spirit and intent of any provision of the State plan. When this paper was prepared, agreements for joint Federal-State inspections had been entered into with Wyoming and Washington. A few other states have indicated their desire to submit a State plan and negotiations toward that end are now under way. Reluctance to enter into such agreements may be due to the mine operators' knowledge that in the states that adopt a cooperative plan they are prohibited from applying to the Director of the Bureau of Mines for annulment or revision of an order issued by a Federal inspector and must appeal directly to the Federal Coal Mine Safety Board of Review for such action. Experience has proved that review by the Director as provided in the act is a less expensive and time-consuming procedure to all concerned than applying to the Board. Reluctance also may stem from the fact that joint Federal-State inspections somewhat restrict the movements of the State mine inspectors and tend to reduce the number of inspections of mines. Where a State plan is not adopted, the Federal coal mine inspector is responsible under the law to take one of two courses of action if he finds certain hazardous conditions during his inspections. The first action involves imminent danger. If a Federal inspector finds danger that a mine explosion, mine fire, mine inundation, or man-trip or man-hoist accident will occur in a mine immediately or before the imminence of such danger can be elim-

Jan 1, 1955

By E. Beril

This may be a most unnecessary paper—from what does crude oil come and how was it formed. Many people, inside and outside of the petroleum industry, believe that we have actually enough oil, and that we can easily produce very important products from this extremely valuable raw material. The writer believes, however, that the answer to this question concerning the parent material and the formation of oil is of broader interest, because it may be that from the answer to these problems it would be possible to get answers to other important industrial questions. Therefore, a study in this line seems to be justified, and the writer will submit some of the results which he has collected during more than ten years with many very capable collaborators, to whom his thanks may be expressed on this occasion. Older Theories There is no doubt that plants were the parent material of coals, but opinion is divided as to the parent material of crude oil and asphalts. One group of specialists believed that they were formed from dead fish. The hydrocarbons of crude oil were formed by the splitting off of CO² from fatty acids formed by the saponification of the fat (glycerides) of fish. Enormous quantities of crude oil are present in many places on the earth, very often in several nonconnected horizons at the same location. This could hardly be explained by the so-called "catastrophe theory," which states that fish died through the entrance of salt water into fresh water, and vice versa. Furthermore, this theory cannot explain the presence of aromatic hydrocarbons, which can be found in nearly all oils, especially in the oil of the Netherlands Indies, which has more than 50 per cent of aromatics. Geological and chemical observations both lead to the belief that the temperature of formation of asphalt, crude oils and coals, perhaps with a few exceptions, did not exceed 200° C. Chlorophyll and haemin derivatives, which decompose above 200° C., have been found in all these materials by Treibs and others. Thermodynamic considerations show that the temperature necessary for the conversion

Jan 1, 1938

By Clarence E. Sims, Donald W. Williams, George A. Moore

INTRODUCTION DURING the past several years the steel casting industry has made studies of heavy castings in which the test bar has been taken from heavy sections rather than from attached or separately cast coupons. It has been noted that the ductility properties of these heavy sections are often lower than those normally expected. Such lowered ductility is usually accompanied by a spotty test bar fracture and the ductility values often can be greatly improved if a low-temperature aging treatment is given to the casting. A loss of ductility of this type is considered "abnormal," since it is not accompanied by an increase of tensile strength or hardness, and "temporary" when the ductility can be restored by aging. The cure of such an abnormal condition represents a real improvement in the quality of the steel. Some hundreds of previous investigations, largely qualitative in nature, have established beyond reasonable doubt that hydrogen is normally present in newly manufactured steel and that this gas, in small amounts, can cause a temporary abnormal loss of ductility. The commonly observed association of high gas content and low ductility has given strong evidence for the presumption that hydrogen, possibly assisted by other gases, is the primary cause of the low ductility observed. Accordingly, the Steel Founders' Society of America has, since Nov. 1, 1944, sponsored investigations at Battelle Memorial Institute whose primary objective is to obtain quantitative information on the relation of the amount of hydrogen and nitrogen in steel, together with associated methods of steelmaking and treatment, to low-ductility effects and porosity. In order that these investigations might proceed on a quantitative basis, hydrogen analyses of a precision considerably higher than any previously reported in the literature were necessary. The method chosen was selected entirely on the basis that it had the highest probability of freedom from uncontrollable errors and will be described in detail in another publication.1 Briefly, the method used consisted of the hot extraction of solid pieces of steel weighing from 45 to 50 g in a highly evacuated quartz tube maintained at 1050°C (1925°F) for a period 0f approximately 40 hr. The greatest precautions were taken to eliminate blanks and insure a sound gas-collection system. Vacuum and temperature conditions were maintained automatically. Mercury-filled risers were used for the introduction of samples in order that the system could be degassed thoroughly in

Jan 1, 1948

By F. J. Lecznar

An investigation of the problem of separating two minerals by a moving inclined plane has revealed that only minerals with considerable difference in sliding friction coefficients separate readily; that it is possible to separate two minerals when only one of them has a rolling friction coefficient; that difference in geometrical shape of the minerals is important to separation which improves as grain size increases; and that the thickness of the stream falling on the belt influences the grade of separation - the thinner the stream, the smaller the interference between the grains of the minerals to be separated and the higher the degree of separation. The problem of separating two minerals with different friction coefficients and shapes by a moving inclined plane has been investigated. Friction separators can be used to separate two materials that differ in shape and in friction coefficient. 1,3 Gladkov has presented some theoretical aspects of using a moving plane to clean corn and podded seeds; this method, however, did not result in practical application. When considering the separation of minerals, only those with considerable difference in sliding friction coefficients can be taken into account. Furthermore, it is possible to separate two minerals when only one of them has a rolling friction coefficient. The difference in geometrical shape of two minerals is also important to separation. It has been found that the separation of two minerals improves as the grain size increases. For example, coal and slate over 2 in. in grain size separate much better than materials of smaller grain size. As Table I indicates, the slate grains smaller than 25 mm gradually lose their flat shape with decreases in size and are more rounded than larger grains, which are almost flat. The smallest grains of slate in first and second fractions slide down the belt since their friction coefficients decrease and approach the value of the rolling coefficient. The percentage of separation of the first fraction is, therefore, low. Thickness of the coal stream falling on the belt also influences the grade of separation; the thinner the stream, the smaller the interference between the grains of the two minerals to be separated and the higher the degree of separation.

Jan 1, 1963

By C. B. Auel

THE subject of this paper involves the crux of the industrial safety problem. It is not overstating the fact to say that "a plant can be made as safe as the management and the workers want it to be;" if such desire is not in evidence and it is not possible to maintain interest in the work of safety, there can be practically no headway beyond the first few steps. These first steps may be said to embrace simply the mechanical or equivalent guarding of tools and equipment and may be taken in a more or less perfunctory manner; but, it has been estimated, they will not effect a reduction of more than 25 to 35 per cent. in the accidents likely to occur in an unguarded plant. The question therefore may be pertinently asked, "Whose interest is meant in the title of this paper, employers', employees?, or both?" It has been repeatedly stated that no safety work of any importance can be carried on: in a plant unless the employer believes in the value of such work. Such statements are true, but have become threadbare with constant repetition and the public is led to believe, that employers differ from ordinary human beings, that their sympathy for their fellowmen has become dulled, and they can be awakened to a sense of the fitness of things with respect to safety, health, sanitation, working hours, etc. only by legislation. There will undoubtedly be found an employer, now and again, who measures down to such specification; but the speaker, in a number of years of close contact with large employers (and his experience has been duplicated by many others) has found that the employers are usually far in advance of the general public in matters affecting the welfare of their employees, including their safety, and not from a selfish viewpoint, but from the humanitarian, economic, etc. If, at times, there is an apparent lack of headway in the solution of some problem connected with employees' welfare, it is not so much due to indifference or a failure to be awake, on the part of the employer, as it is to a lack of knowledge of the way in which to proceed to its successful accomplishment. Further, employers are, only human and cannot follow. every one of the innumerable matters connected with an industry down to their minutest details; they must delegate certain individuals as their representatives, clothing them with the necessary authority to act. These representatives should be looked upon as the Management in their respective fields and the

Jan 6, 1925

Jan 1, 1967

Jan 1, 1967

By E. E. Donath

THE coal hydrogenation process is well known as a means for the production of liquid fuels -from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aromatics and of tar acids and tar bases. The relative amounts of heavy and middle oil-boiling above and below, e.g., 325°C-can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.1 Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydro¬gen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catch-pot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1952

By B. R. Hollebone

The chemical action of molten anhydrous pyridinium chloride (pyridine hydrochloride) on oxy salts and ores of some Group IV and V metals are discussed-in particular zirconium, hafnium, niobium (columbium) , and tantalum. Laboratory-scale experiments are described whose results suggest that this reaction might provide a practicable means of converting ores of these metals to the anhydrous metal chlorides. Experimental results are given which provide some insight into the nature of the reactions and some of the compounds which could be present at intermediate stages. The treatment of ores of the more refractory metals is difficult and expensive and often demands the use of gaseous chlorine, hydrogen fluoride, or other reagents which are, if nothing else, expensive and dangerous to use. This situation is, of course, due to the strong metal-oxygen affinity resulting from the high charge and the small size of the metal ion which combine to produce such high lattice energy in the metal oxide as to defeat standard reduction methods. Thus, the characteristic of these metals which leads to one of their most important properties—corrosion resistance—is the main hurdle in obtaining the metal. Many common methods' for treating ores of zirconium and niobium (columbium), for example, proceed as directly as possible to the preparation of anhydrous halides. These halides are purified by now standard processes of solvent extraction, fractional distillation, and so on. This paper reports on preliminary stages in the development of a method of treating these ores—particularly of niobium—so as to prepare the anhydrous, volatile halides by the use of chemical reagents which are much more easily handled than those used at present. CHEMICAL PRINCIPLES The solvent action of aminium halides has been referred to periodically in the literature over several decades. The chemistry of pyridinium chloride has been discussed particularly by Audreith2 and Starke.3 However, since this is not familiar chemistry in its nonaqueous setting, it is perhaps well to point out some general metallurgical principles and applications. One can use, as point of departure, the fact that HC1 dissolved in pyridine is an acid very much the same as aqueous HC1. It thus gives essentially all the reactions of the HC1 with which we are familiar. However, when the ratio of HC1:pyridine reaches 1:l (a ratio far higher than is possible with H2O) the solution becomes solid C5F5NHC1, pyridinium chloride.* Inter- estingly, the acidic properties of HC1 persist in this medium, although they are manifest only in the molten state of the compound. Some typical reactions of divalent metal compounds which we have carried out in our laboratories are the following: 2PyHCl + Zn — (ZnCl2) + H2 + 2Py 2PyHCl + MnO — (MnCl2) + H2O + 2Py 2PyHCl + CuS — (CuCl2) + H2S + 2Py 2PyHCl + CaCO3 — (CaCl2) + H2O + CO2 + 2Py In these equations, the parentheses indicate a solvated compound which in water would be predominantly a hydra ted cation but which in molten PyHCl will more likely be a complex chloro-anion of the type MC14-. Some important physical properties of pyridinium chloride (PyHCl) are given in Table I. One sees from the data in Table I that at the temperature of molten pyridinium chloride both water and pyridine will boil away. Thus the system will be kept anhydrous. For this reason the reaction 2NbCl5 + 5H2O— Nb2O5 + 10HC1 has no counterpart in molten PyHCl. Instead, the chloride is made even more stable by the formation of a hexachloro complex: Nb2O5 + 12PyHC1 — 2PyHNbC16 + 5H2O + 10Py One interesting property of these complexes is their thermal instability which for the case of niobium can be illustrated as PyHNbCl6 — PyHCl + NbCl5 With a view to possible use of this chemistry in ore treatment, we have attempted to dissolve Pyrochlore (essentially FeO - Nb2O5) and recover the NbC15 from it.

Jan 1, 1968