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By Enrique Hauser

FIRE-DAMP is a mixture of methane with other inert gases or combustible gases. The inert gases in question are carbonic acid, water vapor, nitrogen, etc. The combustible gases are hydrogen, ethane, etc. The study of the properties of fire-damp, therefore, becomes a study of the properties of methane and the influence on its properties of the different gases we have mentioned. Characteristic Properties of Methane 1. Respirability.-Methane being a paraffin is characterized by its weak chemical affinities. From the physiological, point of view one could substitute it for nitrogen of the air at least momentarily, without experiencing any difficulty in breathing the mixture consisting of 21 per cent. 02 + 79 per cent. CH4. I .have tried this on myself, making the gas exhaled -from the lungs burn subsequently in a Bunsen burner.1 From the chemical point of view, this weak affinity permits the gas to be burned in certain circumstances with hydrogen and oxide of carbon in an oxygenated mixture, with the result that the last two gases achieve only a fractional combustion. This practice has been utilized with success in the methods of analysis which I have perfected and which I describe later in this paper. 2. Retardation of Flashing Point.-A characteristic property of methane is its retardation of flashing point, noted by Davy in 1816 and studied by Mallard and Le Chatelier in 1883.2 Taffanel and Le Floch have recently confirmed these results.3 Let us recall the nature of this retardation:

Jan 2, 1916

By C. D. Woodward

PrioR to 1902, the tramming of ore from the stopes to the shafts, in the Butte mines, was done by man or animal power, but the demand for greater tonnage and the need for more improved methods of tramming the ore resulted in the installation of the compressed-air locomotive in a few mines. Some of the objections to animal haulage were thus eliminated, but this locomotive was not generally adopted, because of a number of limiting features. It was superseded by the electric trolley locomotive. The early types of trolley locomotives were not satisfactory from the operators' viewpoint, but they had many economic advantages and after a number of years, in which improvements were constantly made in the structural details, they became dependable, so that the use of animals for main haulage in the mines has now been practically abandoned. There are now operating in the Butte mines of the Anaconda Copper Mining Co., 185 trolley-type locomotives, each of which has replaced five animals. It cost approximately $50 per month to keep an animal, hence the economies that resulted fully justified the expenditure of electrifying the haulage systems. The haulage conditions in this company's mines possess many advantageous features that arc not always found in underground mine workings. The drifts and crosscuts are large, approximately 5 ft. (1.5 m.) wide by 71/2 ft. (2.3 m.) high, and have curves of no less than 18 ft. (5.5 m.) radius; and the roadbeds of the drifts and crosscuts have a uniform grade of 0.5 per cent. toward the shaft, or in favor of the loaded trips. In all of the mines, except two, the track gage is 18 in. (45.7 cm.): and all tracks in the main haulageways are laid with 25-lb. (11.3 kg.) rails. The stations at the shaft are large, well-lighted, clean, and cool. The average temperature of the stations, however, is about 75" F. (24" C.), while the average temperature in some of the drifts and crosscuts is 92" I?. (33.5" C.). As the orebodies lie at varying distances from the hoisting shafts,

Jan 1, 1923

By C. D. Woodward

PrioR to 1902, the tramming of ore from the stopes to the shafts, in the Butte mines, was done by man or animal power, but the demand for greater tonnage and the need for more improved methods of tramming the ore resulted in the installation of the compressed-air locomotive in a few mines. Some of the objections to animal haulage were thus eliminated, but this locomotive was not generally adopted, because of a number of limiting features. It was superseded by the electric trolley locomotive. The early types of trolley locomotives were not satisfactory from the operators' viewpoint, but they had many economic advantages and after a number of years, in which improvements were constantly made in the structural details, they became dependable, so that the use of animals for main haulage in the mines has now been practically abandoned. There are now operating in the Butte mines of the Anaconda Copper Mining Co., 185 trolley-type locomotives, each of which has replaced five animals. It cost approximately $50 per month to keep an animal, hence the economies that resulted fully justified the expenditure of electrifying the haulage systems. The haulage conditions in this company's mines possess many advantageous features that arc not always found in underground mine workings. The drifts and crosscuts are large, approximately 5 ft. (1.5 m.) wide by 71/2 ft. (2.3 m.) high, and have curves of no less than 18 ft. (5.5 m.) radius; and the roadbeds of the drifts and crosscuts have a uniform grade of 0.5 per cent. toward the shaft, or in favor of the loaded trips. In all of the mines, except two, the track gage is 18 in. (45.7 cm.): and all tracks in the main haulageways are laid with 25-lb. (11.3 kg.) rails. The stations at the shaft are large, well-lighted, clean, and cool. The average temperature of the stations, however, is about 75" F. (24" C.), while the average temperature in some of the drifts and crosscuts is 92" I?. (33.5" C.). As the orebodies lie at varying distances from the hoisting shafts,

Jan 1, 1923

By R. E. Barnes

An overall view of the perlite industry is concisely presented. The geology, mining, milling, processing, and applications of perlite, as well as the present status of the perlite industry are treated. Perlite, in strict petrological usage, describes a specific variety of volcanic glass in which strain, incident to cooling, yielded a concentric structure of fracturing which may be visible either to the naked eye or under a microscope. In commercial usage, the term perlite includes any naturally occurring acidic glass of volcanic origin that will expand when heated to a suitable temperature. The name perlite is a derivation of perlstein which originally defined "certain glassy rocks (hyaloliparites, hyalo-rhyolites) with numerous concentric cracks, from the fancied resemblance of broken out fragments to pearls."1 While perlite has been known to geologists for many years, it was not until 1941, while investigating perlite for use in enamel, that an assayer in Superior, Ariz., noted the unusual expansion characteristics of the ore. Further investigations were delayed until following World War II when many small plants were built and experimentation in the treatment and uses of perlite began. The Perlite Inst. was organized in 1949 to promote the development of the new industry, establish commercial standards through research, and to explore new uses and markets. The Institute, located in New York, represents some 50 producers in the U.S., Canada, Australia, England, France, Germany, Greece, Japan, Mexico, and New Zealand. In 1949, 71,l002 short tons of crude perlite were produced, sold or used by U. S. producers, and this figure increased to 325,0003 short tons by 1959. Such a rate of increase indicates the rapid and continuing growth of the perlite industry. GEOLOGY Perlite ore in its crude form has been found in seven of the mountainous western states, since un-devitrified siliceous volcanic rocks are limited to this section of the U. S. Commercially operated perlite deposits are normally of Eocene and Oli-gocene age.4 These deposits are often several hundred feet thick and may extend over hundreds of acres. In 1959, 13 companies in six states produced crude perlite, although the output in New Mexico comprised 79 pct of the total domestic crude output. Other states in order of their production were: Nevada, Arizona, California, Colorado, and Utah.5 Foreign deposits of perlite which are either producing or under exploration are Australia, Canada, Greece, Hungary,6 Iceland, Ireland, Japan, Mexico, New Zealand, and Sardinia. The ore may exhibit a variety of characteristics depending partially on its water content and eruption history and may range through many shades from black to white. While these characteristics may vary slightly among deposits, perlite ore from a particular source is normally quite uniform. Available chemical analyses of perlites from a large sampling of domestic deposits were recently assembled by the Technical Committee of Perlite Institute and are presented in Table I. While the ranges given do not apply to a particular perlite, they are an indication of the chemical analysis which may be expected from any presently commercially operated deposit. The specific gravity of the perlite ore ranges between 2.2 and 2.4, and its bulk density when crushed and sized is 75 to 90 Ib per cu ft. MINING AND MILLING Perlite ore is quarried from open pits by conventional power equipment, although blasting has been occasionally employed. The rock is then stock-piled until needed. While the milling of perlite may seem a simple process compared to that required for basic metals, or even other nonmetals, the need for accurate control of particle size becomes extremely important in further processing. The first step in this operation is the primary crusher, which is normally a jaw crusher. Following crushing, the material is dried, if necessary, in a rotary dryer and conveyed to a secondary grinder which may be a rod mill, hammer-mill, or cone crusher. However, the crushing characteristics of the perlite, caused by incipient cooling fractures, requires it be removed from the grinding operation once it is reduced to the required size so as to prevent overgrinding. Following the grinding operations, various size screens are used to separate the ore according to particle sizes required for particular uses. Most plants use two or more stages of crushing with perhaps four stages of screening.

Jan 1, 1961

By M. M. Rao, P. G. Winchell

The growth rates of bainitic plates were measured at 400°C in Fe-Ni-C alloys containing 0.10 atom-fract~on nickel and 0.0012 to 0.0075 atonz-fraction carbon. The growth rates are adequately represented by where xc is nearly the atom fraction carbon of the bulk austenite and PXCy is nearly the carbon atom fractlon in the ferrlte of radiids p In equilibrium with austetzite. The form of the equation is that predicted by a model in which carbon diffusion in austernite controls the gvowth, but the numerical constatnt is two orders of magnitude below that suggested by the model. THE growth of bainitic plates in steel is often assumed to be controlled by the diffusion of carbon away from the advancing plate tip. This hypothesis predicts that the growth rate will increase as the carbon content of the austenite, xCz, is reduced toward the carbon content of the saturated ferrite comprising the plate tip, PxCY The growth rate should vary approximately as (xCg- pxCy)-1. Experimental observation of the growth behavior at low carbon levels should provide a significant test of this model. An alloying element in addition to carbon is required so that low-carbon austenite can be experimentally observed while undergoing bainitic transformation. Nickel was selected. The presence of nickel complicates the interpretation of the data in two ways: First, diffusion of nickel during the transformation would make analysis very difficult. Nickel is assumed immobile during the transformation. Second, nickel affects the solubility of carbon in ferrite and austenite in equilibrium. This effect has been evaluated.' At the completion of our experimental work Goode-now et al.2 published data in essential agreement with the observations to be reported here. Since their discussion is abbreviated and their data are scanty in the region of interest, we believe the present work is of significance. I) THE MODEL OF BAINITIC PLATE GROWTH The rate of lengthening of a plate is assumed to be controlled by the diffusion of carbon from the advancing ferrite-austenite interface into the surrounding austenite. The precipitation of carbides is assumed to be a secondary process. For ease of analysis the carbon-atom ratio,* pxCy, of austenite in equilibrium with ferrite which is convex with minimum curvature radius p, and the carbon-atom ratio, PxCY, of that ferrite in equilibrium with austenite are assumed independent of location on the ferrite-austenite interface. Since these carbon contents vary with the radius of curvature of the ferrite, p, their assumed positional independence must be held as an approximation. The consequences of these assumptions have been developed approximately by zener3 and Hillert,4 and the resulting equation for a platelet has been applied to bainite by Speich and cohen5 and Kaufman, Radcliffe, and Cohen.8 The Zener-Hillert equation* for plates is: The analysis of Hillert is supported by that of Hor-vay and cahn7 which involves no mathematical approximations but does include the assumption that the a/y interface coincides with an isoconcentration line. The solutions of Horvay and Cahn for elliptic paraboloids are replotted in Fig. 1. The shape of the paraboloid is expressed in terms of the ratio of the principal radii of curvature at its tip, A =p1/p2, which is also the ratio of the minor to the major axis of the elliptic cross section. The Zener-Hillert equation for plates is also plotted. The agreement is within a factor of two for (pxyaCr - xyC )/(xyC - PxCaY) between 0.5 and 100. This is the range of interest here and in most other work on bainite. The original form of the Zener-Hillert equation was the form given above with the right-hand side replaced by (pxCya -xCy)/(PxCya). This replacement is not appropriate here. 11) THE EXPERIMENTAL PROCEDURE Alloys were prepared and three kinds of experiments carried out. Continuous-cooling-transformation experiments were carried out on wires by measuring temperature and resistance during continuous cooling. Isothermal-transformation experiments were carried out on wires by measuring electrical resistance as a

Jan 1, 1968

By D. H. Davis

HAND picking was the earliest form of coal preparation, first practiced to improve the outward appearance of the coal being loaded and to remove any pieces that might appear objection- able to the buyer. It is still extensively practiced on the plus 1-in. sizes and particularly on the plus 4-in. and larger sizes. The percentage of ash reduction that can be obtained by hand picking depends entirely upon the amount of free impurity occurring in the coal. In a particularly dirty seam, where a considerable quantity of rock occurs with the coal as mined, hand picking produces sizable reductions in ash. If the coal is prepared clean at the working face hand picking is a final check; in some cases, on the smaller sizes, it is practiced only to show that an effort is being made to prepare a clean product. Because of the variety and different methods of handling coal, the early plants were not always adapted for efficient hand picking. At most mines an attempt is made to remove the visual impurities at one or more of the following places in the surface plant? (1) in the tipple during screening; (a) on picking band, belt, or shaking conveyors;*(3) during the loading of the coal as it goes into the railroad car. Whatever the physical arrangements of the plant may be, the usual practice is to run the coal over the screen, picking table or boom at such a rate that each piece of impurity is exposed to the view of the picker. Coal should be uniformly sized and spread out on the table so as not to exceed one particle in depth. The flow should be even in tonnage and the speed of travel should be from 30 to 60 ft. per minute and not exceed 80 ft. per minute. The dirtier the coal, the slower the speed required for a fixed number of pickers. Actually, picking capacity depends on the number of particles per minute that can be picked out and rejected. The percentage of impurity removed is determined by this and the average weight of piece rejected. Handling a mixture of sizes from nut to the largest lump over the same picking table or conveyor is not conducive to efficient separation by hand picking because the lump hides the smaller

Jan 1, 1943

By Stephen Burke

THE oxidation of pyritic sulphur associated with coal is important for the following reasons: 1. It is the predominant cause for the formation of acid mine drainage issuing from bituminous coal seams. This drainage pollutes the streams in coal regions, making the water unfit for industrial purposes and causing the disappearance of fish and wild life. As a consequence the movement of industry and especially recreational industry, so important to the population of these areas as an alternative means of livelihood, is impeded. 2. It is instrumental in effecting a series of reactions, which bring about the degradation and ultimately result in the spontaneous combus-tion of bituminous coal in storage. 3. It contributes to the breaking and shattering of the coal structure and is one of the causes of roof falls and floor lifts in mines. 4. It is the primary cause of the many nuisances associated with gob piles and the refuse of cleaning plants. 5. Its proper control and application might possibly be employed in the preparation of coal to reduce the inorganic sulphur content. The research that has been conducted on the oxidation of the various forms of iron sulphides is extensive and the literature voluminous. Nevertheless, few efforts have been made to determine experimentally and with some precision the mechanism of the reaction under the condi-tions of its occurrence in bituminous coal mines. It has generally been accepted that the oxidation of pyritic sulphur proceeds according to the reaction 2FeS2 + 21120 + 702 --> 2FeSO4 + 2H2S04 [1] The ferrous sulphate in the drainage streams is further oxidized by air to produce ferric hydroxide and more acid. Yet the literature fails to dis-close any pertinent investigation on the mechanism of this reaction. The present contribution is concerned primarily with this aspect of the problem and while the work to be reported is not yet complete, it has yielded results from which interesting and significant conclusions may be drawn.

Jan 1, 1937

By S. F. Shaw

In 1913, the Tiro General mine, at Charcas, S.L.P., Mexico, which had been making from 125 to 150 gal. of water per min., was allowed to become flooded, after all the pumps had been removed, and in 1918 the problem of unwatering it came up for solution. There are two vertical shafts, the Tiro General, 1390 ft., and the San Fernando, 1225 ft. in depth, with five connecting levels between them. The San Fernando shaft had been partly retimbered, while the Tiro General had been newly timbered from the collar to 1090 ft. in depth. It had been possible to place guides in only one compartment of the Tiro General, from the collar to the seventh or 850-ft. level, to which it was necessary to lower the water before station pumps could be installed. Soundings indicated that compartments in the Tiro General were open to 1082 and 428 ft., and in the San Fernando shaft to 471, 488, and 586 ft. The water had risen to a point 140 ft. below the collar of the Tiro General shaft.. Pumping Equipment The steam plant at the Tiro General shaft includes one 300-hp., one 150-hp. and one 100-hp. Erie City water-tube boiler, and two 160-hp. Heine water-tube boilers. All but one of these boilers were supposed to be in good shape, but it was soon discovered that six years of idleness in a climate that is foggy for several months of the year had left them in poor condition. The compressed-air plant comprises one Nordberg cross-compound compressor with piston displacement of approximately 2500 cu. ft.of free air compressed to 96 Ib. per sq. in.; and another Nordberg cross-compound with piston displacement of 1235 cu. ft. of free air, to the same pressure. The main pump station is on the seventh level where had been installed a Prescott pot-valve plunger pump with capacity of 200 gal. per min.; also a Gould triplex plunger pump with capacity of 135 gal. per min., driven by a 6 1/2 by 10 by 12 in. steam engine. From the lower levels, the water had been raised to the seventh level by small station pumps and sinking pumps.

Jan 1, 1920

By W. O. Philbrook, K. M. Goldman, G. Derge

EQUILIBRIUM conditions for steelmaking reactions have been studied extensively over the past two decades by a .number of investigators, with gratifying results. Equilibrium data are essential to the understanding of any process, and such knowledge has the practical utility of placing a limit beyond which control measures cannot succeed. When, however, the driving rate of an industrial process is so fast that there is not time for reactions to reach equilibrium, it then becomes necessary that the factors which control the rates of reaction be known in order to establish full control of the process. The desulphurization of molten pig iron by slags within the iron blast furnace is one such process in which the actual degree of sulphur absorption by the slag does not approach the equilibrium distribution obtained for similar slag-metal systems in the laboratory.' A study of the rate-controlling factors governing the desulphurization of iron by slags is becoming increasingly important as the sulphur content of raw materials increases with depletion of higher grade ores and coal. Following up an initial study on kinetics,' this paper reports some results of a continuing laboratory investigation on the mechanism of sulphur transfer between molten iron saturated with carbon and slags of the CaO-SiO,-A12O3 system. Laboratory experiments cannot reproduce in detail the conditions which prevail in the hearth of a blast furnace, but they will contribute to an understanding of the smelting reactions and perhaps will explain some apparent inconsistencies in the factors controlling the equilibrium distribution of sulphur between iron and slags under reducing compared with oxidizing conditions. The mechanism of a reaction—that is, the individual steps and the sequence in which they occur to produce the overall reaction which is ordinarily observed—must be elucidated to learn which steps are the slow ones, or "bottlenecks," that fix the pace of the process as a whole. In the desulphurization reaction, for example, the overall rate might, in principle, depend upon the rate of diffusion of sulphur in the metal or in the slag, upon the speed of some homogeneous reaction taking place entirely within one of the phases, or upon some heterogeneous reaction taking place across the slag-metal interface. Even some side reaction or the back reaction might have some influence. Evidence on all of these points will be presented in this paper. The rate of diffusion of sulphur in both iron and slag is so slow that it seems necessary to assume that convection provides the mechanism of carrying

Jan 1, 1951

By Kenneth Robertson

THERE is probably less known of this subject than of any other connected with the metallurgy of iron. In all the books that treat of this matter, there ore given analyses of slags, their chemical formulae, the loss of iron, etc. ; but few, if any, give the character of the iron mode at the time; none give analyses and physical characteristics of the ores and limestones used, and they present merely isolated examples from various furnaces, and consequently one is more frequently puzzled than enlightened after reading them. During two years I have had occasion to analyze the slags and many of the pig-irons from two furnaces, and for this article I hove made analyses of all the different grades of pig mode by them. A

Jan 1, 1873

By G. T. Hahn, C. N. Reid, A. Gilbert

An evaluation is made of the possible cautsal relationship between twinning and fracture in molybdenum. For both single and poly crystalline material no instance of twin-induced fracture was observed. Instead brittle fracture was found to be slip-induced at heterogeneities. For single-crystal material, the yield stvess in compression and the fracture stvess in tensiow obey a similar angular- relationship which follows approximately a 1/cos2 ? law. where 0 is the angle between the specimen axis and the nearest (100) plane. This sittlilarity between yield and fracture behavior casts doubt on the interpretations made previoltsly that a 1/cos2? relationship supports a critical normal fracture stress criterion. SINCE fracture in brittle materials takes place at stresses an order of magnitude lower than the theoretical strength of the lattice, it must be postulated that some stress-concentrating effect is operative during the fracture-initiation process. Several mechanisms have been proposed whereby the necessary stress concentrations could be produced. The well-known Cottrell mechanism1 describes a dislocation interaction which can lead to the formation of an incipient cleavage crack on a cleavage plane, and both zener2 and stroh3 have discussed models which predict the stress concentration at the intersection of a slip band with a grain boundary. When twinning occurs twin/twin intersections and twin/grain boundary intersections represent another possible means of fracture initiation. Although still controversial, the concept of twin-induced fracture is supported by a weighty mass of evidence, which has been reviewed in a recent paper.4 This investigation was conducted in order to assess the extent to which the brittleness of molybdenum can be ascribed to this cause. Emphasis was placed on seeking direct metallographic evidence for twin-induced fracture such as arrangements of twins located at the fracture origin. EXPERIMENTAL PROGRAM Materials. The experimental materials are described inTable I. From the chemical analyses and estimates of the amounts of interstitials likely to be retained in solution,5 it is concluded that all were mul-tiphased systems. X-ray diffraction experiments6 showed no evidence of preferred orientation in the polycrystalline materials. Single crystals were grown from Molybdenum X and Y using the floating-zone technique,' in a vacuum of better than 3 x 10-5 Torr. However difficulties were experienced with Molybdenum X due to violent gas evolution from the molten zone, and additional crystals (Crystals 3 to 6) were produced by annealing for 5 1/2 hr at 2300°C under a vacuum of 10-4 Torr. Techniques. A series of tension, compression, and bend tests was conducted. Tension tests were used to demonstrate brittle behavior, to measure brittle-fracture stresses, and to provide fractured specimens for metallographic inspection. Compression tests were employed in order to obtain some ductility and a measure of the yield stress. Furthermore, it was considered that compression loading would permit the study of crack nucleation in the absence of propagation. The bend tests were conducted to facilitate identification of the fracture origin, which would be expected to be at, or near, the tensile surface of the sample. Tests were carried out at temperatures between 78" and 298°K attained by means of a liquid-nitrogen evaporator of modified Wessel design.' Specimens were fashioned by mechanical grinding, and, prior to heat treatment, were electropolished at 10 v in a 3:l mixture of ethyl alcohol and sulfuric acid, using a stainless-steel cathode. Except where noted, a strain rate of 4 pct per min was used. All specimens had a gage section 0.75 in. long; diameters of 0.10 and 0.20 in. were adopted for the tension and compression specimens, respectively, the former of single shoulder design, the ends being gripped in split collets with a conical bearing surface. In the bend test, electropolished specimens measuring 0.080 by 0.25 by 1.25 in. were deformed at 78°K by four-point loading. The bending device had spans of 1 in. between the outer and 4 in between the inner fulcra; it was stressed between the compression anvils of the Instron machine at a constant deflection rate. EXPERIMENTAL RESULTS Polycrystals. Tension and Compression Tcsls. It is apparent from Fig. 1(a) that above 170°K fracture of Molybdenum X takes place at stresses equal to or greater than the compressive yield stress whereas

Jan 1, 1967

By D. W. Levinson, L. F. Mondolfo, N. A. Gjostein

MANY investigations are reported in the literature on the age hardening of Al-Mg-Zn alloys but most of them are concerned mainly with mechanical property changes. The present investigation was started to determine the structural changes in an AlMgZn alloy. The alloy composition was chosen in the existing phase diagram" so as to lie on the quasi-binary section Al-(AlZn)Mg Actually, it was found that the diagram as published was inexact at the lower temperatures and that the phase in equilibrium with aluminum at the lower temperatures is not the ternary compound. Technique The alloy used for the investigation was prepared from high purity materials and the resulting composition as determined by chemical and spectro-graphic analysis was: Zn, 6.17 pct; Mg, 2.13 pct; CU, 0.03 pct; Si, 0.009 pct; Fe, 0.005 pct; and the remainder, aluminum. An ingot -in. thick was cast, homogenized, hot and cold-rolled to strip 0.064-in. thick for dilato-metric and powder work, and to foil 0.005-in. thick for single crystal work. Solution treatment temperature for all specimens was 475°±5°C for periods of at least 1 hr, either in air furnaces or lead baths. Aging was done in oil or Pb-Bi baths controlled to within ±3°C. The aging was investigated at the following temperatures: room (30°), 130°, ZOO0, 260°, and 300°C. For the dilatometric study, the length changes were measured continuously, at temperature, using strips of alloy 10 in. long, shaped as channels to eliminate undesirable deflection due to bending. To compensate for thermal expansion and contraction due to the variations in the temperature of the aging baths, the dilatometers were built of the same alloy as the one being tested, with the same shape and size, but with material fully annealed. Gages on which 0.0005 in. could be read and 0.0001 in. estimated were used to measure the dilation. Length changes were also measured at room temperature. Strips approximately 10 in. long were solution-treated, quenched, and measured in a supermicrome-ter in which 0.0001 in. could be read and 0.00001 in. estimated. The specimens were immediately aged for a given time, remeasured, and then the cycle was repeated, including the solution treatment. The error of measurement with this technique was somewhat larger, but the results confirmed those obtained by continuous measurements. The sheet used for the dilatometric work was checked to determine grain orientation. Both X-rays and etching methods revealed a rather coarse grain size but only a negligible amount of preferred orientation. Thus, volume changes calculated from length changes are not invalidated by preferential orientation effects. Pieces of the sheet used for the dilatometric work were also used for the metal -lographic work. Filings for the powder X-ray study were produced from a homogenized piece of sheet. These filings were magnetically purged of iron, screened to 200 mesh, sealed in a Pyrex tube containing an argon atmosphere, and solution-treated. When quenching, the glass tube was broken, so that the powder dropped directly into cold water. After drying with alcohol, the powder was sealed into capillary tubes containing an argon atmosphere and then aged for the required times. In spite of all these precautions the three strongest lines of a( Al2o) appeared in all patterns, and were used as internal standards. By the use of these standards, accurate corrections for film shrinkage were obtained. For the back reflection patterns, annealed nickel powder was mixed with the specimen to act as internal standard. A preliminary investigation was made in small (57.3 mm diam) powder cameras. From these patterns the changes which took place in the solid-

Jan 1, 1957

By Donald E. Ackerman, Norman B. Pilling

The solubilities of a series of experimental alloys covering the range 0 to 100 per cent. Ni, 0 to 30 per cent. Cr have been studied under conditions of complete submersion in several fully aerated acid solutions, and in solutions containing sulfurous acid. In nonoxidizing, hydrogen-discharging acids, if the nickel content is below a certain critical amount, chromium increases the rate of solution and nickel decreases this rate; this critical content of nickel is about 13 per cent. Alloys containing more than this corrode at a constant minimum rate independent of iron, nickel or chromium contents. Austenitic chrome-nickel steels may thus have a resistance to these acids equal to that of nickel-chromium alloys. In nitric acid and in unaerated sulfurous acid rather sharp limits of attack occur which are principally dependent on chromium content. In the former the limit of attack is not related to a particular chromium content but varies continuously with acid concentration. The action of sulfurous acid on these alloys is highly dependent on the presence of small amounts of other substances in solution, and many sulfurous acid mixtures rapidly attack alloys to which the pure acid is wholly inert. The observed effects are not compatible with Tammann's theory relating corrosion resistance to lattice structure but are believed to be concordant with current views of the electrochemical nature of corrosion. Introduction The discovery, development and engineering application of iron alloys resistant to corrosion may well claim a place among the important developments in metallurgy of the past two decades. The varied demands of industry coupled with the skill of the metallurgist have resulted in the production of an extensive group of steels and alloys ranging from the now familiar "stainless " chromium steels of the kitchen to special alloys of great chemical complexity for particular, exacting needs. Any adequate description of the important properties of these-— physical, chemical and economic—would be a formidable undertaking.

Jan 1, 1929

By Donald E. Ackerman, Norman B. Pilling

The solubilities of a series of experimental alloys covering the range 0 to 100 per cent. Ni, 0 to 30 per cent. Cr have been studied under conditions of complete submersion in several fully aerated acid solutions, and in solutions containing sulfurous acid. In nonoxidizing, hydrogen-discharging acids, if the nickel content is below a certain critical amount, chromium increases the rate of solution and nickel decreases this rate; this critical content of nickel is about 13 per cent. Alloys containing more than this corrode at a constant minimum rate independent of iron, nickel or chromium contents. Austenitic chrome-nickel steels may thus have a resistance to these acids equal to that of nickel-chromium alloys. In nitric acid and in unaerated sulfurous acid rather sharp limits of attack occur which are principally dependent on chromium content. In the former the limit of attack is not related to a particular chromium content but varies continuously with acid concentration. The action of sulfurous acid on these alloys is highly dependent on the presence of small amounts of other substances in solution, and many sulfurous acid mixtures rapidly attack alloys to which the pure acid is wholly inert. The observed effects are not compatible with Tammann's theory relating corrosion resistance to lattice structure but are believed to be concordant with current views of the electrochemical nature of corrosion. Introduction The discovery, development and engineering application of iron alloys resistant to corrosion may well claim a place among the important developments in metallurgy of the past two decades. The varied demands of industry coupled with the skill of the metallurgist have resulted in the production of an extensive group of steels and alloys ranging from the now familiar "stainless " chromium steels of the kitchen to special alloys of great chemical complexity for particular, exacting needs. Any adequate description of the important properties of these-— physical, chemical and economic—would be a formidable undertaking.

Jan 1, 1929

By Harold Margolin

The Ti-Al system certainly merits the investigative attention it has been receiving and this latest contribution by Blackburn is therefore to be welcomed. The titanium-rich end of the phase diagram shown here, as well as the diagram by crossley,17 Clark et a1.,18 and Tsujimoto and Adachi,29 reveal no other intermediate phase than Ti3A1, although a previous work by Ence and Margolin20 had reported an additional intermediate phase. Since then, Buerger Precession pictures of single crystals of 10.5, 11.5, and 12.5 wt pct A1 were made at New York university21 and the extinctions were found to be typical of a D6h a Ti structure. Some superlat-tice spots and/or streaks suggesting the presence of an Mg3Cd structure, i.e., Ti3Al, were also found. Since these specimens had been quenched from the y region20 and had revealed a Ti, it was concludedz1 that y does not exist and the structures interpreted as m + y could not be so considered. The absence of normal two-phase behavior in these structures had been indicated in the paper. Accordingly, the two-phase region y + 6 becomes a + Ti3Al and there is some agreement between the results of Blackburn and of Ence and Margolin20 as to both shape and existence above 900°C of an a + Ti3Al field. Crossley 17 proposed that Ti3Al is a line compound which decomposes congruently at 900°C. It is difficult to discount entirely the fact that clear two-phase structures, varying in amount with position in the two-phase field, could be detected above 900°C by Ence and Margolin.20 Precipitation during quenching could not have been so regular and the twin-phase syndrome17 does not apply. The heat treatment and quenching technique was essentially the same as was used by Crossley, whereas Blackburn, who used a rapid quenching procedure, also showed a two-phase a + Ti3A1 field above 900°C. If the two-phase field exists above 900° C, it is easy to picture a two-phase field which could account for the data of Crossley below 900°C without invoking a line compound existence of Ti3A1. All that would be necessary would be an 0 + Ti3Al/Ti3Al boundary which curved sharply to higher aluminum contents below 900° C. It is clear that the controversy must be solved by techniques which obtain data at elevated temperatures without quenching. It is conceivable that the difference in width of the a + Ti3N fields reported by Blackburn and by Ence and Margolin is due to the longer annealing times used by the latter investigators. The criterion for establishment of equilibrium in our work20 was the

Jan 1, 1969

By Clemens Jones

THE analytical history of phosphorus in its relation to the metallurgy of iron is an interesting study, the progress of which runs parallel with the development of the greatest industry in the world. Without the means of finding out how much phosphorus crude pigiron contained, the Bessemer steel process would have been impossible. To do this was originally tedious and slow work. On the other hand, the " direct" process of to-day, as well as the various special processes for steel or iron, have demanded the utmost rapidity in the operations of analytical chemistry. In general, any rapid process for the conversion of unrefined metal into a product of standard composition depends upon the rapidity of some accurate means employed to control it. Moreover, in our modern practice, it is not improbable that the differences in physical properties among the various makes of iron or steel are affected, if not produced, by the use of different methods of analysis. Recourse is always had for correction to the ((standard methods," but I incline to think that these methods are susceptible to error. It is very certain that the system of duplicates would not be resorted to, if the fact were otherwise. Even when duplicated, under the most careful and skilful manipulation, these standard methods produce disagreements. In proof of statements like these, which may sound. heretical, I hope, further on, to cite some evidence worthy of attention. I do not now mean to lay claim to the distinction of discovering the ultimate corrective. That result will come, no doubt, in. time, as the product of the experience of many workers. In the case of phosphorus, as of the other ingredients of iron or steel, a great deal has been done to accommodate the methods of analysis in rogue to the growing necessity for more rapid procedures: Much of this work has concerned what might be called the incidents of method. There is no better example of the accumulation of these incidental improvements than the work done on phosphorus; and I

Jan 1, 1890

By Raymond C. Boettner

The present work had for its purpose: 1) the identification of crack nucleation sites in AISI 4340, quenched to martensite and tempered over a range of 'temperatures; and 2) the comparison of fatigue processes in AISI 4340 with processes observed previously in pure metals From constant def1ection-bending fatigue tests, martensite boundaries were identified as the favored crack nucleation sites in quenched and tempered AISI 4340. It, also, was concluded that the fatigue processes operating- in this lous-alloy steel were similar to Processes observed in pure tnetals. ALTHOUGH much engineering data has been accumulated on the fatigue properties of quenched and tempered martensitic steels,' fatigue as a process is not as well understood in martensite as it is in pure metals.' Important features of the fatigue process, such as the identity of the nucleation sites, have not been determined in the commercially important high-strength low-alloy structural steels. The present work had for its purpose: 1) the identification of crack nucleation sites in a low-alloy steel, i.e., AISI 4340, which had been quenched to martensite and tempered over a range of temperatures; and 2) the comparison of fatigue processes in the AISI 4340 with processes observed previously in pure metals. This comparison of the fatigue processes in the different tempers was restricted to the high-strain low-cycle part of the S-N curve. Under these test conditions, previous work on a number of metals has shown that a large number of cracks are nucleated in less than 30 pct of the fatigue life.3 Furthermore, crack nucleation sites are not restricted to inclusions but are also associated with intrinsic structural characteristics of the metal. MATERIAL A 20-lb ingot of vacuum-melted AISI 4340 (for composition see Table I) was hot-rolled to 1-in.-diam rod and then cold-rolled to a 1-in.-wide strip, 0.08 in. thick. Fatigue specimens, see insert of Fig. 1, were machined from the strip with the long dimension parallel to the rolling direction. m this orientation, the stringers of 1 to 2 p inclusions present in the sheet lay parallel to the stress axis in the specimens. The specimens were austenitited at 2050°F in order to obtain a large prior austenite grain size, i.e., 2 mm, which facilitated the subsequent identification of the prior austenite boundaries. A helium atmosphere was used to minimize decarburization. After austenitiza-tion at 2050°F, the specimens were transferred to a 1450°F furnace so that specimen distortion was held to a minimum in the subsequent oil quench. Previous work4 indicated that refrigeration in liquid nitrogen prior to tempering reduced the percentage of retained austenite in the quenched specimens to less than 5 pct. Tempering was carried out in air over the temperature interval of 200°to 800°F to produce a range of mechanical properties, Table I. The preparation of the fatigue specimen was completed by grinding about 0.005 in. from each surface and electropolishing in a chrome trioxide-acetic acid solution for 30 min. Examination of etched cross sections of specimens prepared in this fashion showed the foregoing specimen preparation to be adequate for the removal of the decarburized layer present after the heat treatment. Transmission electron microscopy showed that the as-quenched microstructure of this alloy consisted of a mixture of martensite plates containing either a high density of dislocations or microtwins. Previous work5'6 indicated that in the course of oil quenching autotem-pering resulted in the formation of E carbide on the martensite and microtwin boundaries. Tempering for 2 hr at temperatures up to about 400°F resulted in further precipitation of the E carbide. Finally, at about 400°F, cementite began to replace the E carbide on the martensite and microtwin boundaries in addition to forming a Widmanstatten structure within the plate matrix. EXPERIMENTAL S-N curves were obtained using electropolished specimens cycled at 1800 cpm as cantilever beams in fully reversed bending at selected constant deflections. The deflections were translated into surface strains by means of a calibration curve obtained through the use of strain gages. An argon atmosphere was used to minimize environmental effects. To investigate the development of fatigue slip bands, the specimens of the different tempers were unidirec-tionally bent to a surface strain of 0.005 to 0.007, photographed to record the location and appearance of slip bands so introduced, and then cycled to failure

Jan 1, 1968

By H. M. Otte, A. L. Esquivel

A new leasl-squares method is Presented for determining lattice parameters of hexagonal or tetragonul structures. The method is adapted for use on electronic computers and involves a reiterative procedure. The correction factor employed raries linearly with the lattice parameter, a (determined from the Brag, angle). In contrast, Cohen's method and recent modifications of it use a correction factor that varies incersely as the squure of the lattice paramneter, a. While the recent modifications attempt to improve the precision of the extrapolated lattice parameter, a, (or-cu). by stressing the importance of the weighting factor. the present approach emphasizes the need for choosing the correct extrapolation function. A comparison between the present method (the Linear method) and Cohen's method indicates that the Linear method may be more appropriale in certain cases. through a priori no critertion appears to he available for making a chorce between the methods. The size of hexagonal and tetragonal crystal lattices is determined by two parameters, a, and c,. Although in principle the two lattice parameters can be determined independently from reflections for which h - k = 0 and 1 = 0, respectively, in practice this may be inconvenient (because of the angular positions at which these reflections may occur) or not easily possible (because of low intensity). Furthermore, if a high precision or accuracy is required, the limited number of reflections of this type available, particularly in the high-angle region, is not sufficient for the necessary corrections (mainly due to absorption) to be determined with accuracy. Several methods1-7,11-13 have been proposed employing all reflections, to obtain the optimum values, a. and co, either by a trial and error procedure or a least-squares fit. Of the latter method, cohen's5 is the best known one since it provides explicit expressions for the optimum a. and c,. However, Cohen's method is only strictly valid if an extrapolation function is used that varies linearly with l/a2 or lie2 (see Section 3), a requirement that does not appear to be generally appreciated. On the other hand, all the better known and more widely used A recent trial and error method was proposed by Massalski and King8,7 who computed extensive auxiliary tables of axial ratios vs the functions A = [(4/3)(h2 + hk +k2) + l2+(a/c)2] and C = A(c/a)2 used in computing a and c values from the observed Bragg angles. These values of a and c were then plotted against a function which permitted linear extrapolation. As a criteria; for the "optimum" values, Massalski and King rely upon a visual fitting of the line through points representing reflections of low 1-index points to compute the extrapolated value of ao and high 1-index reflections to obtain CO. The successive computations and graphical plotting required to reach the "optimum" value are quite lengthy and tedious even on a desk calculator and no quantitative assurance is obtained of having in fact selected the optimum value.* If the method of Massalski and King is used on an electronic computer, then their published tables become redundant and a least-squares fit becomes a natural selection for the choice of optimum values. Such an approach will be called the Linear method. For work now in progress on the effect of certain physical variables on the lattice parameters of hexagonal crystals, it has become essential to determine the confidence limits of small changes in the lattice parameters. Since extrapolation functions that varied linearly with a and c actually also appeared to vary linearly with l/a2 or l/c2 when tested against published as well as our data, a comparison of Cohen's method and the Linear method was considered desirable (Sections 3 and 4). For the latter method an electronic computer was required since a reiterative procedure to obtain the optimum ao and co values had to be employed. The purpose of this paper is to describe the principles of the Linear method, illustrate its application, and compare it with Cohen's method. 1) THE LINEAR METHOD The standard practice in obtaining the lattice parameters in the Debye-Scherrer method is to

Jan 1, 1965

By John C. Calhoun, Raymond G. Loper

Theoretical calculations for the decline of pressure and the variation of instantaneous producing gas-oil ratio with increased cumulative production have been made for reservoir systems under various producing drawdown values and for various spacings. These variables have been included by a modification of previously Published techniques. This consists essentially of utilizing a radial system flowing gas and oil in a succession of steady state calculations. The results of the calculations do not show any variation in the predicted behavior of the internal gas drive reservoir when either the drawdown or the spacing are changed. The prediction of performance on an internal gas drive reservoir has been presented by various authors. ',"' These predictions are in the form of a pressure decline and an instantaneous producing gas-oil ratio as a function of cumulative oil withdrawal. In making these predictions a basic assumption has been that the saturation of the reservoir is uniform throughout at any time, or that the pressure differential imposed on the reservoir system is zero. Because of these assumptions the validity of such predictions has been questioned. Their application to actual systems, where saturations are not uniform and where producing differentials exist, has been a hazardous procedure. The authors cited have used different methods of approach to the derivation of equations for making their predictions and for arriving at a solution of both equations, but basically the same relationships are utilized in each case. In all instances the instantaneous producing gas-oil ratio is calculated from the equation: In utilizing this equation an average reservoir pressure and an average reservoir saturation must be known, the former to define ß, v, s, and uo/ug and the latter to define kg/ko. Predictions can be made, therefore, only for the conditions of a uniform reservoir saturation and a uniform reservoir pressure. This restriction of requiring a uniform oil saturation can be resolved by applying two-phase steady state flow for the radial system to the reservoir's history. Radial steady state flow is defined when the ratio of phases flowing,

Jan 1, 1949

By John C. Calhoun, Raymond G. Loper

Theoretical calculations for the decline of pressure and the variation of instantaneous producing gas-oil ratio with increased cumulative production have been made for reservoir systems under various producing drawdown values and for various spacings. These variables have been included by a modification of previously Published techniques. This consists essentially of utilizing a radial system flowing gas and oil in a succession of steady state calculations. The results of the calculations do not show any variation in the predicted behavior of the internal gas drive reservoir when either the drawdown or the spacing are changed. The prediction of performance on an internal gas drive reservoir has been presented by various authors. ',"' These predictions are in the form of a pressure decline and an instantaneous producing gas-oil ratio as a function of cumulative oil withdrawal. In making these predictions a basic assumption has been that the saturation of the reservoir is uniform throughout at any time, or that the pressure differential imposed on the reservoir system is zero. Because of these assumptions the validity of such predictions has been questioned. Their application to actual systems, where saturations are not uniform and where producing differentials exist, has been a hazardous procedure. The authors cited have used different methods of approach to the derivation of equations for making their predictions and for arriving at a solution of both equations, but basically the same relationships are utilized in each case. In all instances the instantaneous producing gas-oil ratio is calculated from the equation: In utilizing this equation an average reservoir pressure and an average reservoir saturation must be known, the former to define ß, v, s, and uo/ug and the latter to define kg/ko. Predictions can be made, therefore, only for the conditions of a uniform reservoir saturation and a uniform reservoir pressure. This restriction of requiring a uniform oil saturation can be resolved by applying two-phase steady state flow for the radial system to the reservoir's history. Radial steady state flow is defined when the ratio of phases flowing,

Jan 1, 1949