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By A. H. Larson, L. G. Twidwell

The influence which Au, Ag, Sb, Bi, Sn, and Cu have, both individually and collectively, on the activity coefficient of sulfur in liquid lead at 600"C zuas studied by circulating a H2S-Hz gas wlixture over a specific lead alloy until equilibrium was attained. Subsequently, the H2S concentration in the equilibrium gas mixture and sulfur concentration in the condensed phase were deterruined. The elements gold, silver, and antinzony (above 8 at. pct) increased the activity coefficient of sulfur. Bismuth had no apparent effect. Tin (above 3 at. pct) and copper decreased the coefficient. The influence of an individual element, i, on sulfur is best reported as the interaction parameter, riS, which is defined as The values o these first-order interaction zus are: ESzu = —55.0. These interaction parameters are used to predict the activity coefficient of sulfur in six fouv-component alloys and one seven-component alloy. Comparisons are made with direct experimental determinations. INTERACTIONS in dilute solution have been studied by many investigators. Most of the experimental work has been confined to solute-solvent interactions in simple binary systems and solute-solute interactions in ternary systems. Dealy and pehlke"~ have summarized the available literature on activity coefficients at infinite dilution in nonferrous binary alloys and have calculated from published data the values for interaction parameters in dilute nonferrous alloys. Interaction parameters are a convenient means of summarizing the effect of one solute species on another in a given solvent. Only a few investigators have studied interactions of the nonmetallic element sulfur in a metallic solvent. They are as follows: Rosenqvist,~ sulfur in silver; Rosenqvist and Cox,4 sulfur in steel; chipman, sulfur in alloy steels; Alcock and Richardson,% ulfur in copper alloys; Cheng and Alcock,' sulfur in iron, cobalt, and nickel; Cheng and ~lcock,' sulfur in lead and tin. The only reported work on the Pb-S system in the dilute-solution region is that of Cheng and Alcock.' Their investigation involved a study of the solubility of sulfur in liquid lead over the temperature range 500" to 680°C. The results may be summarized by the following relationship: S (dissolved in lead) + Pb(1) = PbS(s) log at. %S = -3388/T + 3.511 Experimentally, it was found that Henry's law was valid up to the solubility limit of sulfur in lead, i.e., at 600°C up to 0.43 pct. Their investigation did not include the study of sulfur in lead alloys. More accurate calculations could be made in smelting and refining systems if activity coefficients of solute species could be accurately predicted in complex solutions. One of the objectives of this study was to compare the experimental data with the values calculated from the equations derived from models for dilute solutions proposed by wagner9 and Alcock and Richardson. A temperature of 600°C was chosen as the experimental temperature to attain reasonable reaction rates and to minimize volatilization of the condensed phase. EXPERIMENTAL Materials. The Pb, Au, Ag, Sb, Bi, Sn, and Cu used for preparation of the alloys were American Smelting and Refining Co. research-grade materials. All were 99.999+ pct purity except the antimony and tin which were 99.99+ pct. The initial alloys prepared for this study consisted of twenty-one binary alloys, eleven ternary alloys, and one six-component alloy. The constituent elements were mixed for each desired alloy and were placed in a crucible machined from spectrographically pure graphite. The crucible was placed in a vycor tube which was evacuated with a vacuum pump and gettered by titanium sponge at 800°C for 8 to 12 hr. After the gettering was completed, the chamber containing the titanium was sealed and removed. The remaining sample chamber was placed in a tube furnace at 800°C for 2 hr and quenched in cold water. The final operation consisted of homogenization of the alloy for 1 to 2 weeks at a temperature just below the solidus for the individual system. The resulting master alloys were sectioned into small pieces and a random choice made for individual equilibrations. Cobalt sulfide (Cogs8) used to control the gas atmosphere in the circulation system was prepared by passing dried HzS for 24 hr over a Co-S mixture heated to 700°C in a tube furnace. This material was then mixed with cobalt metal to give a two-phase mixture which, when heated in hydrogen to a particular temperature, produced a desired H2S/H2 gas atmosphere in the circulation system. A Cu2S-Cu mixture also used in this study was prepared in a comparable manner. Apparatus for Equilibrium Measurements. The experimental technique of this study required apparatus

Jan 1, 1967

THE paper on "Specific Efficiency of the Blast Furnace" by Richard Franchot, which was pub-lished in the September issue of MINING AND METALLURGY, was presented for discussion at the Pitts-burgh meeting. The session opened with a discussion among S. P. Kinney, Mr. Franchot, and J. N. Reese as to the methods and results in sampling for cyanides in the blast furnace. This is covered in detail in writ-ten discussion below. T. T. Read objected to the use of the term specific efficiency as likely to be confusing. The blast furnace has to perform the function of reducing Fe, 03 to Fe as well as that of fusing the metal and, since the reduc-tion of Fe, 0? involves a CO equilibrium, it seems mis-leading to calculate efficiency on the basis of burning the , all carbon to CO? since it is not possible. Mr. Franchot replied that he used the term in the sense defined by Richards in his "Metallurgical Calculations;" but a subsequent search failed to reveal the term in Richards, who says (page 245, 1st edition): The practical conclusion is that a blast furnace generates in itself not much over 40 per cent of the calorific power of the fuel used, and rejects nearly 60 per cent; by using part of the waste gases to heat the blast, however, some of this rejected heat, to an amount representing net 5 to 10 per cent of the calorific power of the fuel used, is returned to and injected bodily into the furnace, thus rendering available for the purpose of running the furnace about 50 per cent of the calorific power of the fuel as a maximum. The efficiency with which the furnace applies this 50 per cent usefully to the objects of the reducing and smelting is another question for investigation.

Jan 2, 1927

By E. H. T. Whitten

Fundamental principles of trend surface analysis are briefly reviewed. Recent analyses of several granite masses illustrate the method of estimating the quantitative regional composition and also variation trends. Mineralogi-cal, bulk chemical, and other quantitative variates can be employed. Such results should improve gravimetric surveys (etc.) relying on correction terms based upon estimated rock composition. For the first time realistic estimates of the mean composition of rock bodies can be made with the aid of trend components. Deviation maps hold promise for delimitation of disseminated mineralized areas. Deviations comprise residual "anomalies" after removal of trend components. In petrogenetic work such deviations have been shown to reflect local influences (e.g., contamination of magma by assimilation of xenoliths or country rocks of the envelope). Similarly, mineralization should be reflected as deviations standing out from background trends. Actual examples are given. Present results largely involved projection of data onto a horizontal plane, but if sufficient data are available use of three spatial coordinates increases accuracy for prediction in "unexposed" areas. Regression analysis shows that statistical correlations between variates for regionally distributed specimens are often strong (particularly with percentage data). Hence, in preliminary surveys more easily determined variates may sometimes be employed to gain first estimates of the distribution of components more economically significant. The sampling plan is of paramount importance. Unless a suitable sampling plan is devised and adhered to rigorously during collection of the samples, all subsequent analysis is liable to strong bias and to yield spurious estimates of the truth. For a wide variety of purposes it is becoming necessary to assess the quantitative composition and variability of rock masses and mineralized zones of various types. In petrology and petrography this is something of a break with tradition, because virtually all descriptions heretofore have been qualitative. Although vast amounts of qualitative data have been compiled, little is known about the quantitative behavior of rock components. However, if variability of rocks could be understood and expressed with sufficient accuracy, there would be considerable advantage to both economic and petrogenetic problems. For example, if, on the basis of a limited series of observations, the three-dimensional geometry of a disseminated orebody (or ore-bearing formation) could be predicted accurately, it would be possible to extrapolate with confidence the structure into unexposed areas. The following example based upon the geometry of an igneous cone sheet illustrates the point. The significant rock-unit gives outcrops at a number of points on the exposed surface ABCD (Fig. 1A). Study of n exposures may enable a geologist to predict that the rock-unit is circular in form and thus indicate where the unit can be expected in unexposed terrain. Such observations are made at sites with u, v coordinates, but, if subsurface information is available at sites with uvw coordinates, it will eventually become possible to predict accurately the three-dimensional form of the rock mass. Geologic rock masses or mineral deposits are not generally as regular and symmetrical in geometric form as the body illustrated in Fig. 1A. However, even where the broad limits of a major rock mass are known, a more acute problem arises in attempting to obtain detailed quantitative estimates of its internal variability; it is difficult to predict the variability of a mass from a limited number of observa-

Jan 1, 1961

By R. R. Webster, H. T. Clark

The side-blown converter has been investigated as a possible commercial process for the production of low nitrogen steel. During this work, two converters of 3-ton and 22-ton capacity were operated on a pilot plant basis for a total of 214 heats. The steel made in these converters was low in nitrogen and possessed good cold working properties. Some problems of converter operation remain to be solved. IN plants operating with a high iron capacity, sev-eral different refining methods are used in the conversion of the molten pig iron to steel. These include various ore practices in stationary and tilting open-hearths, the duplex process employing the Bessemer converter and open-hearth, and the Bessemer process. At J&L, a considerable part of the iron produced is handled by the Bessemer process, either alone or in conjunction with duplexing, and therefore an appreciable portion of the steelmaking research effort has centered about the method. This paper covers research work on the development of the side-blow converter for the commercial production of low nitrogen ingots and includes descriptions of the operation of a 3-ton and a 22-ton experimental converter at the Aliquippa Works. The refining of iron to produce steel requires the removal of a large portion of the carbon and silicon and the control of manganese, phosphorus and sulphur which are present in the iron in varying amounts. The first large-scale means of refining iron was the acid Bessemer process which was brought into use almost 100 yr ago. This method, using compressed air as the refining medium, accomplishes substantially complete removal of carbon, manganese and silicon. Phosphorus and sulphur are not affected but, by choice of an iron composition sufficiently low in these elements, a commercial product can be produced. Since the process will handle large tonnages rapidly, operates without external fuel and with a minimum of additional equipment, it quickly became the major tool in the early expansion of the steel industry. Later, the basic open-hearth process, by affording control of phosphorus and sulphur and by consuming the large quantities of steel scrap that were becoming available, forced the acid Bessemer process into a secondary position in the industry. During the past two decades the demand for steel to be used in cold forming and drawing operations has gradually increased. Bessemer steel, because of its work hardening and aging characteristics, is not as suitable for these applications as basic open-hearth steel, consequently the decline of the process was accelerated. More recently, because of changing economic conditions, this long range trend appears to have been arrested or perhaps reversed. Ingot production data for recent years furnishes only an incomplete picture of the importance of the converter in the American steel industry; open-hearth furnaces utilize large tonnages of blown metal for which no published statistics are available. Metallurgical Aspects The fundamental difference between Bessemer and open-hearth steels apparently lies not in the method of manufacture but, rather, in the differences in chemical composition of the two steels. It is further believed that the principal features distinguishing Bessemer from open-hearth steel are the higher nitrogen and phosphorus contents of the former. Evidence supporting this position is supplied by tests on laboratory induction furnace heats that were made to contain varying amounts of phosphorus and nitrogen but were otherwise similar to normal low carbon silicon-killed steels. Fig. 1, 2 and 3, summarizing the test results, are taken from G. H. Enzian's paper titled, "Some Effects of Phosphorus and Nitrogen on the Properties of Low Carbon Steels."' Fig. l indicates that phosphorus has a marked effect on the cold work embrittlement of steel as shown by the work brittleness test of Graham and Work.' In the low nitrogen steels, which as a group have the better cold working properties, the effect of phosphorus variations is the more pronounced.

Jan 1, 1951

By Arthur Glance

MINE safety is of the utmost importance to all operators and most operations have a safety organization, or safety inspector, whose job it is to be continually on the alert to detect and correct the hazards of mine operation. Reports from the Bureau of Mines show that next to roof falls, gas presents the greatest hazard in mining. The Bureau of Mines Information Circular 6680 shows that 162 explosions occurred in the United States during the five-year period ending June 30, 1932. Deaths resulting from these explosions amounted to 984, with a great many disabled and disfigured. A fatality rate of 6.07 persons shows the ex¬treme severity of this hazard to the industry. Various mine appliance companies have put on the market instruments for methane detection, which record in direct percentages the amount of methane present in the atmosphere. Unfortunately, few mining companies are using these instruments, however. Those available include the Burrell methane detector, the Wolf, the Martienssen, the Mine Safety Appliance detector, and the Union Carbide Company methane detector, which last I have used extensively in making mine inspections.

Jan 1, 1936

By Linn Bradley, W. W. Strong, H. D. Egbert

Marked differences of opinion have been expressed by engineers interested in cleaning iron blast-furnace gases for use in hot-blast stoves and under boilers, in reference to the advantages of a hot-dry method over a cold-wet method. One point at issue involves the sensible heat energy in the moisture contained in the gas. Some advocates of the cold-wet methods claim that the condensation and resultant removal of the greater portion of this contained moisture by wet scrubbing, spraying or similar methods, results in a saving of some of this sensible heat energy, by reason of the fact that water vapor has a high capacity for sensible heat energy and may carry from the exit of a hot-blast stove, for example, more heat units than are sacrificed or lost when the gas is cleaned by this cold-wet method. Other advantages claimed for the latter method are: That gas burns more readily when it is free from moisture in any form; that because gas is made denser by cooling and removing the moisture it has a higher calorific value than hot gas carrying moisture; and that higher flame temperatures are obtained when the gas is cleaned by the cold-wet method. A search through the available literature fails to disclose any extensive calculations or records of conditions obtained in practice, bearing upon these phases of gas cleaning. This paper deals with these problems from the standpoint of the economy of using a gas of higher flame temperatures, of improved stove design, and of economy in the gas-cleaning department. Calculations have been made which show that by cleaning the gases by a cold-wet method the sensible heat energy of the blast-furnace gases is greatly reduced; and, in general, this loss of heat energy is far greater than that lost from the stoves or boilers due to the sensible heat capacity of the water vapor if carried away by the exit gases. By making use of the

Jan 1, 1917

By d&apos, L. Berenbaum, F. Heurle, R. Rosenberg

The structure of aluminum films obtained by evaporation was studied by electron microscopy, mostly by replica techniques and X-ray diffraction. The resistivities and stress conditions of the films were also determined. Film properties were studied as a function of source selection, substrate type, residual pressures of oxygen and water vapor, substrate temperature, and rate of growth. The formation of abnormal localized growths and whiskers resulting from annealing treatment subsequent to deposition was investigated. Films deposited onto single-crystal substrates were found to be epitaxially 0riented; for such films, relative orientations between films and substrates were determined. ALTHOUGH wide use has been made of evaporated aluminum films for the formation of conducting lines on semiconductor devices, relatively little has been reported concerning the structural characteristics of such films.1"9 The purpose of this study was to obtain an overall view of the dependence of these characteristics on film deposition and subsequent annealing conditions, which were similar to those used in silicon planar technology. Accordingly, most of this study was carried out using oxidized and bare silicon wafers as substrates, although some work was also done using alkali halide, magnesium oxide, and mica substrates. However, the main concern remained pragmatic. Emphasis was given to the study of the effects of deposition and annealing conditions on film characteristics such as structure, resistivity, and stress. I) EXPERIMENTAL PROCEDURES The films which were investigated in this study were deposited in 18-in.-diam glass chambers which were connected to the usual type of trapped diffusion pumps filled with silicon oil. Through the use of liquid-nitrogen-cooled Meisner traps and titanium sublimation pumps placed inside the deposition chambers, the pressure could be lowered to the lower portion of the 10- I Torr range and little increase in pressure would occur during the deposition cycle. Unless described otherwise, the substrates were 1-in.-diam p-type silicon wafers having a resistivity of 10 ohm-cm. The wafers were oxidized in wet oxygen at 975°C followed by a short dry-oxygen exposure at the same tempertture to a total oxide thickness of approximately 6000A. The wafers, backed by a layer of gallium, were mounted onto molybdenum discs brazed to a copper block.10 The latter was heated by imbedded commercial cartridge heaters. The substrate temperature could be maintained to within +10°C of a prescribed temperature during film deposition. The search for a satisfactory source for the controlled evaporation of aluminum has led to the use of 1-in.-diam crucibles" machined from rods of a commercially available, refractory composite* of Bn and

Jan 1, 1969

By Jasper L. Stuckey

PYROPHYLLITE, first identified as soapstone,' later as agalmatolite,2 and finally as pyrophyl-lite, has been known to occur in North Carolina for more than 130 years and has been produced intermittently in commercial amounts for the past 100 years. Pyrophyllite mining, however, has become a major industry in North Carolina only during the past 25 years. North Carolina and California are the chief producing states. Current annual production averages 125,000 tons, of which slightly more than 90 pct comes from North Carolina. Distribution and Geologic Setting: All known pyrophyllite deposits in North Carolina are associated with rocks of the Carolina Slate Belt,' which is composed of a vast series of metamorphosed volcanic and sedimentary materials, occurring as two zones extending in a northeast-southwest direction across the state. The larger of these zones, lying in the central Piedmont region, varies from 8 to 50 miles wide. The smaller zone lies along the eastern edge of the Piedmont region and is partly covered by coastal plain sediments. The rocks in both zones consist of a great volcanic-sedimentary series, composed of air-laid and water-laid tuffs and breccias, lava flows, and slates. On the basis of composition, they may be classed into three groups: 1) tuffs, breccias, and lava flows of acid or rhyolitic composition; 2) tuffs, breccias, and lava flows of a basic or andesitic composition; and 3) water-laid slates composed of fine grained materials derived chiefly from the acid tuffs and breccias and

Jan 1, 1959

By J. T., Norton

As cold working is an important feature in a great many of the fabricating processes now applied, this paper presents some ideas on the nature and results of the plastic deformation produced in this operation. The art of manufacturing metal for practical uses is very old and has undergone very great development. The science of metals has- also developed very rapidly recently and the various processes to which metals are submitted are much better understood now than they were even a short time ago. All the knowledge that can be obtained on this subject is useful because it promotes efficiency in converting metal into finished articles.

Jan 1, 1927

By Roger M. Zimmerman

The G-Tunnel heated block experiment is being conducted on the Nevada Test Site (NTS) as part of the Nevada Nuclear Waste Storage Investigations project (NNWSI). The purpose of the ambient temperature testing ph se is to evaluate rock-mass mechanical properties of a block (- 8 m3) under biaxial stress changes up to 7.5 MPa above an initialization in situ value of 3.1 MPa. Results indicate that the modulus of deformation ranges from 9.7 to 17.0 GPa and Poisson's ratio ranges from 0.21 to 0.33. In general, the higher values of the modulus and Poisson' s ratio were influenced by fracture propagations parallel to the compressive stress field. Other measurements indicated that cross-hole compression (p) wave velocities and single fracture permeability values were relatively insensitive to stress changes above the in situ value.

Jan 1, 1984

By S. Whinery

In these times of sharp rivalry, both as to price and quality, among the makers and venders of engineering explosives, it is often desirable to be able to determine the relative energy or value of the various explosives offered for sale, in order to purchase intelligently ; or, having contracted for a large amount of an explosive of a certain standard quality, to be able to ascertain if the manufacturer keeps his product up to the specified standard. The simple and inexpensive apparatus described below was devised by the writer while engaged on the improvement of the Tennessee River, at MuscleShoals, under the direction of' Major W. R. King, U. S. Engineers, in the summer of 1879. It answered the purpose so well that it is thought that a brief account of it may be of interest to other engineers. It consisted, essentially, of an old blacksmith's anvil and a common striking hammer, such as is used for driving rock-drills. The anvil was placed face downward on solid, level ground. In what was then the top of it, a vertical hole, one and one-fourth inch in diameter and about one arid three-fourths inch deep, was made with a ratchetdrill. The surface of the anvil immediately around the drill-hole was made as true and smooth as possible with a file. Next, a new striking-hammer, weighing nine pounds, with a turned and true face, was selected ; and a handle, eleven feet long and about one and a half inches in diameter, was fitted into it so that it

Jan 1, 1886

By F. George, W. Tice, M. Salkind

It was found that Al-A13Ni could be readily cold rolled perpendicular to but not parallel to the whiskers. Reductions of more than 98 pct were achieved without cracking by rolling perpendicular to the whiskers, whereas extensive edge cracking was noted after only 15 pct reduction when rolling parallel to the whiskers. The longitudinal and transverse tensile strengths were nearly doubled, and the longitudinal yield strength more than tripled by cold rolling 50 pct in a direction perpendicular to the whiskers. The whiskers exhibited some waviness (elastic bending) as a result of cold rolling, but at very high reductions (greater than 75 pct) whisker fracture and misalignment became significant. A fine dislocation substructure in the matrix consisting of cells attached to the whiskers was pro -duced by cold rolling. Most of- the substructure was readily removed by a 1-hr anneal at 500°C. Cold rolling was found to substantially reduce the thermal stability of the microstructure at 610°C but did not affect the stability at 500°C. FIBER and whisker reinforced composite materials promise significant improvements in properties over conventional materials. Before they find wide use, however, it will be necessary to understand the response of these highly anisotropic materials to common metalworking processes. Most of the nonmetal-lic fiber reinforced materials have very low elongations (a few pct or less) in the direction of fiber alignment. Thus, metalworking techniques such as rolling and forging would not be as broadly applicable to these materials. This investigation was initiated to determine how a composite system consisting of Al3Ni whisker reinforced aluminum responded to rolling, what changes in the microstructure occurred, and the effect of deformation on the mechanical properties. The composite material studied was produced by unidirectional solidification of the A1-Al3Ni eutectic alloy'-7 and consisted of 10 pct by volume of aligned whiskers of Alai in a matrix of aluminum. It should be pointed out that this system is not representative of all composite materials, and the results will therefore not be universally applicable. The A1-Al3Ni system is characterized by: 1) A strong fiber-matrix interfacial bond 2) A ductile matrix 3) A sufficiently low fiber content to allow significant plastic flow between fibers 4) Strong, completely elastic whiskers (tensile strength 400,000 psi, elastic modulus = 20 X 106 psi.1 These factors allow the material to be readily rolled perpendicular to the fibers. If the fiber-matrix bond were not strong, such a weak interface could fail during rolling. A measure of the ability of a composite to be rolled in the transverse direction can be obtained from noting the transverse tensile behavior. In the case of Al-Al3Ni,2 there is considerable ductility (15 to 30 pct). In the case of boron filament reinforced aluminum, for example, the transverse elongation is less than 1 pct,8 and the material could probably not be cold rolled as readily in that direction. EXPERIMENTAL PROCEDURE 3-in. diam ingots of A1-A13Ni eutectic were unidi-rectionally solidified in graphite crucibles. The starting materials consisted of 99.99+ pct pure nickel and aluminum, and the pure eutectic ingots were made with 6.2 wt pct Ni. The unidirectional solidification process (described in detail elsewhere1-3) consists of preparing a master heat of eutectic composition, remelting, and withdrawing the ingot vertically downward through the heat source at a controlled rate so that plane front solidification proceeds upward at a constant velocity. The resulting microstructure consists of 10 pct by volume of whiskers of very high aspect (length to diameter) ratio. The fiber lengths have not been measured because of the difficulty of detecting fiber ends9 but exceeds 104. There is some possibility that the fibers may be continuous within one grain. Flat sheet specimens 2¾ in. sq and approximately 0.2 in. thick containing whiskers parallel to the plane of the sheet and to one edge were used for this study. A1-A13Ni exhibits either a rod-like (high solidification rates) or a blade-like (low solidification rates) whisker morphology,1,3 and both types were studied. Rolling was accomplished using a two-high rolling mill at a speed of approximately 10 fpm. The rolling direction was either parallel to or perpendicular to the direction of growth (direction of whisker alignment). Reductions of from 0.002 to 0.03 in. per pass were used with the most common value being 0.005 in. per pass. Cold rolling of Al-Al3Ni to more than 98 pct reduction in thickness was accomplished with no intermediate anneals. In addition. a series of speci-mens was cold rolled 97 pct with a 1-hr, 500°C anneal in air after each 50 pet reduction. Tensile testing was accomplished using a Tinius-lsen four screw testing machine. Flat sheet specimens + in. wide and between 2 and 2; in. long with the thickness dependent upon rolling reduction, were used. The gage section was in. wide and 1 in. long. Strain was measured using a clip-on LVDT extensome-

Jan 1, 1970

By Milton E. Wadsworth, John N. Ong, W. Martin Fassell

The temperature and oxygen concentration dependence on the reaction of sphalerite in oxygen at pressures from 6 to 640 mm Hg have been investigated in the temperature range 700° to 870°C. Sphalerite has been found to oxidize linearly over this entire temperature and pressure range. At higher rates, considerable self-heating was observed. The dependence of the oxidation rate on the oxygen concentration may be expressed by: Rate = k' where k' is the specific rate constant and 0 = K1[O2]/(1 + KI[O2]), where K1 is the equilibrium rate constant for the adsorption of oxygen on sphalerite. Values of the activation energy and the enthalpy of adsorption were found to be 60.3 and —59.6 kcal per mol, respectively. Data have been presented that indicate conditions under which either a sulphatizing or an oxidizing roast may be obtained. ROASTING processes have been employed in the metallurgy of a great number of basic metals in use today. Until recently, however, little attempt has been made to deduce the fundamental mechanism by which oxidation takes place. Structural changes upon oxidation have been investigated1 = and thorough work has been performed with regard to the reaction products and the thermodynamics of the oxidation reactions. The objective of this investigation was to determine the rate of oxidation of sphalerite and to apply the absolute reaction rate theory in the theoretilcal interpretation of the experimental results." "O Description of Apparatus The apparatus contains the following features: 1—a furnace with gas system, 2—an autographic weighing system, and 3—a temperature control system. Furnace With Gas System—The furnace was mounted by a yoke on each end and was free to travel up and down on steel guide rods, permitting the introduction and removal of samples from the apparatus with minimum difficulty. The furnace was heated by three sections of Kanthal wire wound externally on a zirconia tube and insulated with Fiber-frax. Pure gases or mixtures of gases were introduced into the lower end of the furnace through two flowmeters, a mixing chamber, and a gas-tight sparger, Fig. 1. The gaseous products of the reaction and the unused gases were prevented from escaping to the atmosphere by maintaining a small negative pressure on the system. This procedure permitted air from the outside to enter through the small an-nulus around the quartz suspension fiber and prevented the escape of the internal gases. Autographic Weighing System—The autographic weighing system consisted of an adapted gold balance, a photoelectric circuit, and a weight recorder, Fig. 2. The sample was suspended from one end of the balance beam by means of a platinum chain outside the furnace and a long thin quartz fiber on the inside of the furnace. On the other end of the balance beam, the necessary weights were added to counterbalance the sample. In addition, a calibrated chain was added to the balance which was linked directly to the weight recording unit. Control was effected by means of a photoelectric circuit." A parallel beam of light from a strong source was directed onto a small front-surfaced aluminum mirror mounted in the middle of the balance beam and then to a front-surfaced mirror mounted on the ceiling of the room. The beam was then reflected onto a front-surfaced right prism at a distance of 9 ft from the balance

Jan 1, 1957

By CYRIL W., William Campbell, Henry M. Howe

THIS paper gives the results of an investigation of the behavior of the argentiferous cobalt-nickel arsenides of Temiskaming, Ontario, in roasting, made in the metallurgical laboratories of the School of Mines, of Columbia University in the City of New York. The ore was kindly given by the owners of the La Rose and Trethewey properties at Cobalt, Ontario, and Mr. E. J. Hall, Tutor in Assaying in Columbia University, has helped us much. I. OBJECT OF THE INVESTIGATION. The object of the investigation was to learn:- 1. The temperature at which the arsenic is most rapidly expelled; 2. The thoroughness with which it is expelled by prolonged roasting at this temperature; 3. The effect of adding charcoal (a) near the end of the roast and (b) at the beginning of the roast. II. NATURE OF THE ORE. The important ores mined in the Temiskaming deposits are native silver-with small amounts of dyscrasite (Ag6 Sb), argentite (Ag2S), pyrargyrite (Ag3SbS3)-smaltite (CoAs2), chloanthite (NiAs2) and niccolite (NiAs). Mispickel (FeAsS) and cobaltite (CoAsS) also occur in smaller quantities. The average composition of the ore shipped from this district for the first six months of 1905 -was: silver, from 4.1 to 4.8 per cent.; cobalt, from 6.9 to 8.2 per cent ; nickel, from 3 to 4.7 per cent ; and arsenic, from 30.9 to 34.6 per cent. The ore which we treated consists chiefly of smaltite ; In our laboratory-work

Jan 1, 1907

By J. H. Swisher

The rate of internal sulfidation of austenitic Fe-Ti alloys in H2S-H2 gas mixtures is controlled primarily by sulfur diffusion, with counterdiffusion of titanium playing a minor role. At temperatures below 1100°C, enhanced diffusion along grain boundaries becomes important. The rate of internal sulfidation at 1300°C is approximately equal to the rate computed from the sulfur diffusion coefficient. The diffusion coefficient of titanium in y iron has been determined from electron microprobe traces in the base alloy near the subscale interface. The solubility of sulfur in Fe-Ti alloys has been measured in the temperature range from 1150° to 1300°C. The equilibrium sulfur content is found to increase with titanium content, due to the large effect of titanium on the activity coefficient of sulfur. The Ti-S interaction becomes stronger as the temperature decreases. TITANIUM as an alloying element in stainless steels is an effective scavenger for interstitial impurities, carbon in particular. Titanium is known to form stable sulfides; however extensive thermodynamic data on the Ti-S system are not available. Schindlerova and Buzek1 have shown that the Ti-S interaction in liquid iron is moderately strong. There have been no previous studies of the Ti-S interaction in solid iron. Internal sulfidation of Fe-Mn alloys was the subject of a recent investigation by Herrnstein.2 He found the rate of internal sulfidation to be an order of magnitude greater than predicted from available solubility and diffusivity data. A satisfactory explanation for the discrepancy could not be given. In the present study, the solubility of sulfur in austenitic Fe-Ti alloys was measured using a standard gas equilibration technique. Fe-Ti alloy specimens were also internally sulfidized. The rate of internal sulfidation was measured as a function of temperature and alloy composition. Supplementary electron micro-probe measurements were made to provide additional information on the nature of the internal sulfidation process. EXPERIMENTAL The starting materials were alloys containing 0.12, 0.24, 0.38, and 0.54 wt pct Ti. The alloys were made in an induction furnace by adding titanium to electrolytic iron that previously had been vacuum-carbon-deoxidized. The major impurity in the alloys as determined by chemical analysis was carbon. The carbon content of the alloys averaged about 100 ppm; metallic impurities were presented in concentrations of 50 ppm or less. Specimens were made in the form of flat plates, 0.03 by 2 by 4 cm for the equilibrium measurements and 0.5 by 1.5 by 3 cm for the rate measurements. The experiments were performed in a vertical resistance furnace wound with molybdenum wire and containing a recrystallized alumina reaction tube. In the gas train, flow rates of the reacting gases were measured using capillary flow meters. The source of H2S was a mixture of approximately 2 pct H2S in H2, which was obtained in cylinders from the Matheson Co. A chemical analysis was provided with each cylinder. The H2-H2S mixture was diluted with additional hydrogen to obtain the desired ratio of H2S to H2, and the resulting mixture was diluted with 30 pct Ar to minimize thermal segregation of H2S in the furnace. Argon was purified by passage over copper chips at 350°C and subsequently over anhydrone. Hydrogen was purified by passage over platinized asbestos at 450°C and then over anhydrone. The H2-H2S mixture was purified by passage over platinized asbestos and then over Pas. The samples used in the solubility measurements were analyzed for sulfur by combustion and iodometric titration. The subscale thickness in the internally sulfidized samples was measured on a polished cross section, using a microscope with a micrometer stage. Electron microprobe traces for titanium in solution were made on several samples that had been internally sulfidized. A Cambridge microanalyzer was used, and the known titanium content at the center of the specimen was used as a calibration standard. The procedure for the microprobe measurements will be described further when the results are presented. RESULTS AND DISCUSSION Equilibrium Data. Fig. 1 shows the sulfur concentration as a function of gas composition for three alloys equilibrated at 1300°C. The dashed line is based on data published by Turkdogan, Ignatowicz, and pearson3 for pure iron. The breaks in the curves are the saturation points for the alloys. The fact that the initial slope decreases with increasing titanium content indicates that titanium interacts strongly with sulfur in solution. To obtain information on the composition of the precipitating sulfide phase, the measurements described in Fig. 1 were extended to higher sulfur partial pressures. These results are shown in Fig. 2. (The initial portions of the curves are reproduced from Fig. 1.) The highest PH2s /pH2 ratio used is believed to be below the ratio required for the formation of a liquid sulfide phase. Time series experiments were used to study the approach to equilibrium in the samples. It was found that equilibrium with the gas phase was reached in less than 4 hr at 1300°C.

Jan 1, 1969

HARD as it is at any time to provide more than three million tons of coal each year for power plants, the task really gets rugged in the wintertime when the fuel freezes solid in the cars. At the Marysville plant of the Detroit Edison Co. the problem of unloading cars of frozen coal was severe because there was an unloader over only one of the two tracks in the coal unloading house. Moving downward by their own weight, with no driving force to aid them, the spuds of this old unloader were unable to break through the crust on a frozen coal car. 20,000 Lb Force To meet this problem, a new mechanical car unloader was installed over No. 2 track and placed in service in December 1947. It is a Kenney type unloader built by Heyl & Patterson, Inc. of Pittsburgh, Pa., a modification of equipment originally designed to unload iron ore cars. The major advantage of this unloader is the force with which it can drive the sharp spade on the end of its ram down through the pockets of a frozen coal car. The unloader consists of the following major units: 1. A traveling bridge structure. 2. A traveling trolley. 3. A retractable and oscillating ram. 4. The operators cab and controls. The bridge is provided with safety hooks to prevent its being lifted from the rails by the upwards push of the ram. The bridge will travel 190 fpm and has sufficient traction on its four wheels to move three loaded 70 ton cars. The trolley runs on tracks supported by the bridge girders and also has upper tracks to control the push from the ram. Two of the single-flange trolley wheels are driven by a one and a quarter hp dc motors equipped with magnetic brakes. The ram is raised and lowered by a 20 hp dc motor equipped with a magnetic brake. A full stroke of a little over 14 ft is given the ram through its rack and pinion drive and the spade can be pushed down into a loaded car with a force of about 20,000 lb. A 15 hp dc motor with a magnetic brake is applied to this drive and is able to swing the ram 45º either side of the vertical. The usual procedure in emptying a coal car is first to drive the sharp spade down through the coal until the pocket is opened and the coal starts to run out the hopper. When all the hoppers are open, the sweeping action of the ram and spade is used to move the remainder of the coal in the car over to the open hoppers. The travel of the trolley permits cleaning the sides of a coal car with the edges of the spade, using the sweeping motion of the ram. It is still necessary to clean out the corners of the car by hand. Final Clean-Out This unloader was a new development and there were improvements to be made before it was completely satisfactory, such as reduction in speed and conversion to ac drive motors. However, it helped at Marysville and unloaded many frozen cars that would have taken a lot of heating to thaw out enough for the old unloader to handle. The mechanical coal unloader described above was a considerable improvement but still left a job to be done by hand-the final cleaning out of the coal cars. The ram had the ability to open a hole through the hopper cars, but did not meet required unloading speed. To eliminate hand cleaning a car shakeout, manufactured by Hewitt Robins, Inc. was added to the installation. This equipment is used to clean the coal car out after the unloader has provided an

Jan 1, 1952

By R. H. Lee

WITHOUT doubt, one of the most frequent and serious annoyances connected with the practical running of a blast-furnace, especially in single-furnace plants, is caused by low steam, in spite of the fact that all boilers at blast-furnaces have grates for burning coal, and that coal is more or less continuously burned upon them, from three to a dozen men being pretty constantly engaged around the boilers as firemen or coal- and ash-handlers. At times, when the furnace is ? tight," all available men are put on to assist the regular firemen; yet sufficient steam cannot be got to keep the engines up to their regular number of revolutions, while the stoves, deprived of the gas which has been sent to the boilers, run cold, so that, when the furnace loosens-up and resumes the regular rate of driving, the blast is very considerably below normal temperature, and a.' cold," or at best a " high-sulphur," east is the result. Again, it often happens that a furnace, running at its best, becomes temporarily a little too hot; the pressure rises; the amount of gas made' is diminished; the steam soon commences to go down; and a small scaffold is likely to form before the furnace has been brought back to the proper rate of driving, and thus enabled to take its regular amount of blast. The usual remedy is either to "jerk" the furnace by a sudden, brief intermission in blowing, or to cool the furnace by lowering the heat of the blast; but if the lower blast-temperature be maintained too long, the hearth and descending stock may be cooled below the " critical temperature " mentioned by Mr. .Johnson, and the furnace may go to the other extreme, and become cold. This is especially the case when coal or coke, high in sulphur, is used:

Jul 1, 1906

By E. A. Stevens

IT has been ascertained in recent years that certain rocktypes, geological formations and structural conditions may be used as fairly reliable guides, when prospecting in recognized mineral belts or mining districts, with a reasonable certainty of discovering "pay-ore;" and that such is considered as a practically established conclusion may be inferred from a perusal of the recent reports of the U. S. Geological Survey and the literature of the several scientific societies discussing minim, geology, and kindred subjects. Cripple Creek is no exception to this conclusion, and the rock-type or association, rather than the structural condition, is the most infallible guide.† These guides consist of four, possibly five, dike-rocks, three of which are extremely basic, while the fourth is an acid rock of an entirely dissimilar character. The basic rocks are nepheline-basalt, limburgite, feldspar-basalt and tephrite. There are grounds, however, for believing that the two latter are subdivisions of one type, and therefore will be described under one head. The acid rock is quartz-porphyry. Nepheline-basalt is-a rock encountered in but few localities elsewhere on this continent, and occurs in narrow dikes cutting various formations. When typical‡ it is composed of

Jan 1, 1913

By S. N. Singh, M. C. Flemings

Results are presented of a detailed study on the combined influences of ingot dendrite am spacing and thermomechanical treatments on the structure and solution kinetics of high --purity cast and worked 7075 alloy. Solution kinetics were found to depend sensitively on ingot dendrite am spacing and on details of therrnomechanical processing, including amount of reduction and extent of&apos; solution treatment before reduction. An approximate analysis is given for rate of solution of nonequilibrium second phase in the cast and worked structres; results of the analysis are compared with experiment. MICROSEGREGATION in high strength aluminum alloys manifests itself as "coring" (composition differences within the primary aluminum-rich phase), and as interdendritic second phase. The mechanism of formation of the microsegregation is understood, and approximate prediction of the amount of second phase is possible for simple binary systems.1,2 When alloy elements or impurities are present in amounts less than their solid solubility at solution temperature, any phases forming from these elements are termed "nonequilibrium" and can be dissolved by appropriate solution treatment. The rate at which the nonequilibrium phases are removed depends sensitively on their spacing (dendrite arm spacing in the cast material, or band spacing in wrought material). When alloy elements or impurities are present in amounts in excess of their solubility at the solution temperature, second phase particles form an "equilibrium" second phase that does not dissolve in heat treatment and may, in fact, coarsen in such treatment. Usual commercial, high strength, wrought aluminum alloys contain nonequilibrium second phases that were not fully dissolved during ingot processing. They also contain equilibrium second phases resulting from impurities present in amounts greater than their solubility. As has been shown by Antes, Lipson, and Rosenthal,3 and will be demonstrated further in a subsequent paper by the authors,4 significant improvements in mechanical properties of high strength alloys can be achieved by reduction or elimination of these second phases. Methods of elimination are 1) to employ high purity materials to minimize amounts of equilibrium second phase, and 2) to employ suitable thermomechanical processing techniques to fully eliminate nonequilibrium second phases. Work reported herein comprises a study of selected thermomechani- cal processing treatments, and of their influence on solution kinetics of wrought high purity 7075 alloy. EXPERIMENTAL PROCEDURE Melting and Casting. The bulk of the work reported was performed on a single ingot of high purity 7075 alloy. The ingot was 4 in. by 4 in. by 8 in. high, uni-directionally solidified following a procedure previously described.5 The mold was heated to 1350°F before pouring the melt. The bottom chill was carbon coated stainless steel. Water was circulated through the chill after the melt was poured. The 7075 alloy was prepared from high purity virgin material (aluminum, zinc, magnesium) and from master alloys (Al-50 pct Cu, A1-15 pct Cr, A1-5 pct Ti). Final measured melt composition (wt pct) was: Zn Mg Cu Cr Ti Fe Si Al 5.70 2.28 1.35 0.18 0.15 <0.002 <0.012 bal Melting was done in a silicon carbide crucible; all tools were coated with zircon wash to minimize iron contamination; degassing was by bubbling chlorine through the melt. che-rmomechanical Treatments. Detailed studies were made on material taken from a location approximately 13 in. from the chill and 51/2 in. from the chill (i.e., from 1 in. thick slices taken between 1 and 2 in. from the chill and between 5 and 6 in. from the chill). Solution treatment was done at 860°F in an air-circulating furnace with a "bottom drop" arrangement to achieve minimum delay time between solution treatment and quench. Samples solution treated in this way were 2 in. by 2 in. by 1 in. Temperature of the quench water was approximately 10°C. Mechanical reduction was by cold rolling. Samples 11/2 and 51/2 in. from the chill were treated for 12 and 24 hr, respectively, before cold rolling. Reduction by cold rolling was then 4/1, 16/1, and 35/1. In each case, several intermediate anneals (1/2 hr at 860°F) were used to permit reaching the final thickness without cracking; two such anneals were used for the 4/1 reduction, five for 16/1, and six for 35/1. After working, materials were again solution treated for various lengths of time from 0 to 48 hr and quenched in water. Structural Measurements. Secondary dendrite arm spacings were measured using procedures previously described.&apos; For each measurement reported, five photomicrographs were first made at X75. Measurements were made of dendrite arm spacings in at least 20 different grains (grain structure was equiaxed). Grain size measurements were made by running a number of random traverses across photomicrographs of the samples and obtaining the mean lineal intercept. Measurement of the volume percent of second phase and porosity was done by quantitative metallography. A two-dimensional systematic point count was used

Jan 1, 1970