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By N. H. MacMillan, W. M. Mularie, R. E. Jackson, A. R. C. Westwood

The initial results of a study of the environment-sensitive microhardness and diamond rotary drilling behavior of granite and its constituent minerals quartz and feldspar (microcline)1 have established that many similarities exist between the environment-sensitive mechanical (chemomechanical) behavior of these materials and that of the simpler solids such as periclase, soda-lime glass, and alumina4 studied previously, at least as far as n-alcohol (straight-chain alcohol) environments are concerned. The results of this study (hereafter designated study I) also suggested that the rate of drilling of granite in these environments is controlled by the chemomechanical behavior of its quartz constituent, and is greatest in those environments which impart a zero l-potential to this phase, thereby maximizing its hardness. Now, cationic surface-active species strongly influence the l-potentials of silicate minerals. For this reason they are widely used in mineral separation operations. In particular, dodecyl trimethyl ammonium bromide (DTAB) was found in study I to produce f 0 for quartz at a concentration in water of 107 to 10-4 moles per 1. Accordingly, the influence of dilute aqueous solutions of this surfactant on the drilling behavior of granite also was examined in study I. This revealed that granite could be drilled three to four times faster in 10-° molar aqueous DTAB than in water, and confirmed by experiment the suggestion that granite is most effectively drilled with a diamond core bit in environments which impart a zero l-potential to quartz. According to O'Connor and Buchanan' however, the isoelectric point for quartz in aqueous DTAB solutions occurs at a concentration of .•.•2 x 10-° moles per 1, rather than [101 to 10-1] moles per 1. To confirm the results of study I, therefore, a more comprehensive investigation of the [ ]-potentials of quartz, microcline, and Westerly granite in aqueous DTAB environments has now been undertaken. At the same time an examination has been made of one of the basic assumptions of the current conceptual understanding of chemomechanical effects. In this view, although hardness changes occur essentially instantaneously following wetting of the solid, they are confined to a surface layer at most a few micrometers (µm) deep. Hence, to maximize the influence of chemomechanical effects on bit penetration rate only shallow cuts should be taken. Practical penetration rates are then obtained by increasing bit rotation speed. Experimental l-potentials were determined by the streaming potential technique using an automated rapid-cycling apparatus recently developed by Martin Marietta Laboratory from a design by Somasundaran and Kulkarni. The drilling studies employed 3.2-mm-OD 120-grit diamond-loaded core bits with a wall thickness of ~0.7 mm, and bit rotation speeds of 2200 and 25,000 rpm. The load applied to the bit was independent of the depth drilled in both cases. The 2200 rpm measurements employed the same drill press and puddle drilling technique as used in study I. The higher rotation speed was obtained using a water-driven dental turbine drill. In the case, the surface active fluid was pumped down the axis of the bit to ensure efficient wetting and flushing of the drilling debris from the hole. In both cases drilling rate was measured by the parameter D(200), defined as the average rate of bit penetration during the interval from 150 to 250 sec after drilling commenced.

Jan 1, 1976

By O. A. E. Jackson

In all three principal dunite dikes, minute disseminated grains of pyrrhotite are to be seen in the fresh rock in amounts less than 1 pct. Traces of nickel have been reported from many such specimens. Nickeliferous pyrrhotite is the principal nickel-bearing mineral, although olivine contains very minor amounts of nickel in solid solution, substituting for magnesium and iron. Such occurences are of no economic significance. Nickel analyses of possible economic significance (up to 3 pct Ni) have been returned from samples taken near the margins of the two large western dunite dikes. These samples were from schistose zones along and within the dike walls. The mineralized shear zones, up to 30 ft wide, strike N 30 W and dip from 65" to 90" west. They consist of layers of hard, fresh, green-gray dunite, mineralized with finely disseminated pyrrhotite. These layers alternate with layers of soft, black, oxidized schistose dunite up to 1 ft wide, well mineralized with pyrrhotite and tabular-fractured pentlandite in crystals up to 1/4-in. diam. Sulfides identified in polished sections were chiefly pyrrhotite and pentlandite, with much smaller amounts of chalcopyrite. There are two varieties of pyrrhotite. One develops a fine polish and conforms to published descriptions. The other is slightly darker and browner, does not polish as well, and displays flamelike growth or intergrowth structure when etched with nitric acid fumes. Pyrrhotite and pentlandite crystallized contemporaneously in the form of veins in the olivine and as fillings of the interstices of euhedral olivine crystals. Chalcopyrite replaces the other sulfides. The most striking feature of the deposits is their occurrence in intimately fractured and schistose zones in the dunite where faulting has been localized along the contacts of the sediments and the dunite dikes. Though far too little detailed work has been done to be certain, there appears to be a higher concentration of sulfides in the shear zones along the margins of dike apophyses, sediment reentrants, and strike and dip irregularities. Much more study would be required in order to submit a plausible theory of formation of the nickel deposits, supported by laboratory and field evidence. Results of the present study, especially localization of the metals by fracturing, certainly indicate that the nickel concentrations were brought about by precipitation of nickel sulfides from fluids that used the fractures as a means of ingress. Studies of nickel sulfide deposits throughout the world have demonstrated that such sulfides were deposited at considerable depths and at temperatures of several hundred degrees. This would rule out the possibility of groundwater as the transporting medium. The two possible sources of hot nickel-bearing fluids are quartz diorite and gabbro. The first possibility is that large volumes of fluids, expelled from the quartz diorite magma during its crystallization, obtained a supply of nickel by altering the nickeliferous olivine of the dunites. The likelihood of this process is lessened by the recognition that, although the dunites show some alteration to serpentine, talc, and trem-olite, they are for the most part remarkably fresh outside the schistose zones. The worldwide association of nickel with basic rocks, together with the presence of pyrrhotite in thin films on joint planes of the gabbro on Jumbro Mountain, favors the gabbro source. The writer extends thanks to C. Phillips Purdy, Jr., project chief of American Metal Climax Inc., for giving him the opportunity to study these deposits. He is also indebted to the officers of American Metal Climax Inc. and Discovery Mines Inc. for permission to publish this article.

Jan 1, 1961

By F. Keller, E. H. Dix, R. W. Graham

Aluminum alloys containing relatively small amounts of magnesium and silicon are of commercial interest because they are readily workable in the annealed form and may be hardened and strengthened by suitable heat treatment. An intermediate temper can be produced in these alloys by quenching after a Solution heat treatment and the alloy in this condition can be formed easily. Artificial aging is required to obtain the maximum mechanical properties but this aging does not cause distortion nor require elaborate heat-treating equipment. The hardening of the alloys after quenching is attributable in part to the retention of the compound Mg²Si in solid solution, while the maximum hardness obtained by subsequent artificial aging is attributed to the fact that the solid solubility of the compound Mg²Si in aluminum decreases with decreasing temperature. Considering the importance of aluminum alloys susceptible to heat treatment, it is surprising how few fundamental investigations have been carried out on the aluminum-magnesium silicide alloys. This paper deals principally with the solid solubility relations of the compound Mg2Si in aluminum and is the sixth paper of a series1 from the laboratories of the Aluminum Co. of America reporting the results of investigations of equilibrium relations in aluminum-base alloys made from high-purity aluminum."

Jan 1, 1931

By A. F. Taggart

OLIVER C. RALSTON, Salt Lake City, Utah (communication to, the Secretary*).-This paper has appealed to me as being one of the most lucid, well-connected and complete papers on this subject which has been published. To be sure, the concepts called upon in an explanation of the flotation process by these authors are mostly old ones which have been more or less discussed in previous literature, but they have nevertheless been assembled in a most constructive and suggestive manner. We find a new contribution to flotation theory in the effect of fine particles increasing the viscosity of the interfacial film between a liquid and a gas. This phenomenon has been variously hinted at but never definitely stated in accepted scientific terms. The discussion of "contact angles". is very clear and will doubtless be welcomed by those who have not had the opportunity to investigate the literature on this subject, but it is unfortunate that the "hysteresis of the contact angle," observed by Sulman and reported some years ago, is not mentioned or explained. A few other points need discussion in order to call attention to the fact that, while this paper is the best discussion of the subject which has yet appeared, all of the truth has not yet been told.

Jan 12, 1916

By D. H. Newland

CERTAIN observations from the field and laboratory suggest the need for recasting some of our ideas about gypsum as a rock-forming mineral and in relation to supplies for industrial use. Until about 25 years ago, the use of gypsum was confined almost entirely to agriculture. During the past quarter century, though, its usefulness has been greatly developed, particularly in the building trades, which now absorb most of the gypsum produced. In 1919, according to the U.S. Geological Survey, the output of crude gypsum was 2,240,163 tons, a gain of 912 per cent. in 25 years. About one-half of this production was mined in New York, Ohio, and Michigan, where the proved supplies can hardly be regarded as over-large when viewed in relation to the rapid expansion of industrial requirements. The occurrence of gypsum in the United States is treated by R. W. Stone and others.1 The deposits of Canada are described by L. H. Cole.2 Several states, including Kansas, Oklahoma, Iowa, Michigan, and New York, have had special surveys made their of gypsum deposits, but the reports, as a rule, refer to conditions as they existed from 15 to 20 years ago.

Jan 9, 1921

By S. M. Brisbane

THE life of refractory linings in rotary cement kilns can be shortened by uneven or inadequate support of the kiln and its shell and by variations in the conditions of operation. Alteration of these factors may, according to their nature, bring about mechanical deterioration of the lining or promote chemical attack. Chemical attack has been described elsewhere.1-4 The distortion of cement kilns has been discussed in a general manner by Rochow,6 ho indicates the amount of distortion which may occur in an unlined shell, and by Rosenblad: who states that the deformations of the shell are greatest above the trunnions. The present article indicates the extent of the distortion of a kiln to an oval shape in certain selected positions and the deviation from a straight line of the kiln along its length between two supports. The cement kiln is a long, hollow, rotating cylinder consisting of steel plates which may be either welded or riveted together. This shell is supported on tires, frequently 60 ft apart, which roll on trunnions. The large mass of the kiln causes distortion of its cross-section; it becomes slightly oval, i.e., diameters lengthen as they become horizontal and shorten as they become vertical. There is also a tendency for the shell to bow between supporting tires; this bowing may be upwards or downwards depending on the position of the weight forces and the supports. The extent of the deviations from the ideal kiln shape was investigated. Observations described in this paper were made on the shell of the clinkering zone between the first and second tires of two of the kilns at the Geelong works of Australian Portland Cement Pty. Ltd. The kilns were both 400 ft long and 10 ft diam with a welded enlarged burning zone 11 ft 6 in. diam. The shell was fabricated from mild steel and in this section its thickness was 1 in. It was lined with 41/2 in. of chemically bonded magnesite-chrome bricks which were jointed with mild steel plates. The kilns operate on a 4 pct slope and the speed may be varied between 0.75 and 1.68 rpm. The wet process is used; kilns are coal fired and are fitted with integral coolers. Temperatures within the kiln are difficult to determine with any accuracy because of the absence of black body conditions, but surface temperatures are probably in the range 1420° to 1470°C. Average shell .temperatures at the two positions at which the deformation studies were made were 370°C and 355"C respectively. Methods: In determining the ellipticity it was necessary to measure the lengths of the vertical and horizontal diameters while the kiln was in operation; data obtained from a stationary kiln would not have the same practical significance. For this purpose the four points V, W, X, and Y at the ends of two mutually perpendicular diameters were marked on one kiln. The point X is shown in Fig. 1. For the measurement of the length of the vertical diameter a vertical column, to which a horizontally aligned telescope was attached, was placed 10 ft from the kiln. The telescope could be racked up and down in a vertical plane. Two sets of readings were taken, one set when each of the points V, W, X, and Y was at its maximum height above the

Jan 1, 1957

By E. T. Cox

WHILe engaged, in the year 1856, in determining the oil-bearing properties of some bituminous coals from Western Kentucky, by subjecting them to dry distillation in an iron retort, which held about a pint;, and to the neck of which were attached several bottles, for collecting the carbon oils, and washing and measuring the gas, I observed that there was a very great gain in the weight of coke thus made, over that obtained from the same coal when charred in a platinum crucible, as is usual in the laboratory for making the proximate analysis of coal. It was thought at the time that the increase of coke, by the former mode of treating the coal, was due to the pressure which the retarded gas exerted upon the solid carbon, and the possible fixing of a portion of the carbon from the volatile hydrocarbons. For the purpose of obtaining a more definite idea of the effects of pressure on the coking of coals, a series of experiments were made this spring under my direction, by my assistant, Dr. G. M. Levete. The results are highly instructive and full of interest, since they point out some peculiarities in the nature of bituminous coals which

(Butte Meeting, August, 1913.) IN metallurgical circle it is. known widely, but somewhat vaguely, that the ease of reduction of metallic .oxides. depends largely on the way they have been prepared. It is likewise known that. different forms of carbon have different and greatly varying reducing powers. It is the purpose of, this paper to show somewhat more definitely and scientifically these facts. Sonic years ago the writer published an account of pyrometric determinations of the reduction temperature of zinc oxides variously prepared and of several kinds.1 In said paper it was shown that the temperature at which zinc oxide evolves zinc according to the equation, ZnO+C? Zn+CO depends upon the nature of -the two reacting bodies. The determinations bad a range of accuracy of from 2°to 6°C.,whereas differences were found to, amount to an extreme of 90° C. So the differences are real ones and must have a definite cause. The equation of boiling water, (H2 O)4 = 4 (H20) has a fixed temperature for? equilibrium of 100° C. at 760 mm. pressure. In general, all equations reacting in the liquid or the gaseous phase have well-defined constant physical conditions which govern the equilibrium point and reaction velocities.

Jan 7, 1913

By Donald Jaffe, Michael B. Bever

The solidification of Al-Zn alloys (2 to 70 pct Zn was investigated at different rates of solidification. The resulting structures were studied; the amounts of nonequilibrium eutectic were measured and compared with the amounts calculated on the assumption of no diffusion in the solid. The compositions of the cored primary constituent were investigated by quantitative autoradiography after activation of the zinc by neutron irradiation. These compositions were also determined from microhardness values. IN a recent investigation of the soltdification of aluminum-rich AI-Cu alloys,' the amounts of non-equilibrium eutectic were measured and compared with the amounts calculated on the assumption of no diffusion in the solid. The compositions of the cored primary constituent were investigated by quantitative autoradiography. The work reported here extends the investigation of nonequilibrium solidification to the Al-Zn system in the range from 2 to 70 pct Zn. In addition to autoradiography, microhard-ness values were used to determine compositions on a micro scale. Solidification Experiments The alloys contained approximately 2. 6, 12, 20, 30, 50, and 70 wt pct Zn and the balance aluminum. According to published diagrams the eutectic reaction occurs at 382°C between the eutectic liquid (95 pct Zn), a (82.8 pet Zn), and $ 498.9 pct Zn). Solid-state reactions at lower temperatures (due to the miscibility gap between 350" and 275"C, the eutectoid at 275'C, and the precipitation from supcrsaturated a) did not affect this investigation. Even if they occurred to any appreciable extent, they did not alter the evidence pertaining to the solidification structures. The alloys had to be of high purity to avoid radioact~ve contamination during activation. The aluminum analyzed 0.015 pct Si, 0.009 pct Fe, less than 0.004 pct Cu, and less than 0.006 pct Mg with traces of sodium and titanium; the zinc was reported to be at least 99.99 pct pure with traces of iron and magnesium. The alloys were prepared under argon in an induction-heated, bottom-pouring furnace, and poured into a coated steel mold, which could be preheated to temperatures up to 700°C in order to control the rate of solidification. The pouring temperatures ranged from about 40" above the liquidus for 2 pct Zn alloys to about 130°C above the liquidus for 70 pct Zn alloys. As soon as the melt entered the mold, the readings of a thermocouple placed % in. above the bottom of the mold were recorded by a recording potentiometer. Cooling at the rate induced by the initial temperature of the mold was continued to a temperature 100°C below the liquidus; the mold with its contents was then quenched in icy brine. Quenching from a fixed interval below the liquidus was used to provide a standardized procedure, since the solidus and liquidus temperatures and the interval between them vary greatly over the composition range investigated. The temperatures from which the samples were quenched were below the equilibrium solidus, but under nonequilibrium conditions some liquid was still present. This residual liquid solidified during the quench. The samples measured 314 in. diam and 11, in. height. Drillings for chemical analysis were taken

Jan 1, 1957

By D. T. Peters

To better understand the Co-Mo interaction in maraging steels, the precipitate reversion behavior of two alloys closely related to the 18 Ni-250 grade has been studied. The reversion experiment is carried out by aging at a low temperature, T1 (preaging temperature), for some period of time and then aging at a higher temperature, T2, called the reversion tetnperature. Aging and reversion tmzperatures used were in the range 679 to 1050°F. Reversion is marked by an increase in resistivity and a decrease in hardness. It teas found that some reversion took place at all cornbinations of T1 and T2 but that pronounced rei3ersion resulfed for an Fe-18 pct Ni-5 pct Mo-8 pcl Co alloy exposed to preagz'ng' temperatures at or below 850°F. A similar alloy not containing cobalt exhibited no such discontinuity in reversion behazior with TI. The results are interpreted in terms of two types of molybdenum-rich precipitates, one nucleated at dislocations and the other in the matrix. The increased supersaturation resulting from the presence oj- cobalt evidently provides sufficient energy to nucleate the matrix phase. Anotnalies in the temperature dependence of the resistivity decrease and peak hurdness in the Fe-18 pct Ni-5 pct Mo-8 pct Co alloy as a junction of aging temperature noted in an earlier study are explained on this basis. SEVERAL investigatorsl-9 have studied the details of the precipitation-hardening reaction of the maraging steels. The great majority of conclusions have been drawn from transmission electron microscopy. Although much has been learned by this method, alternate techniques which will give information earlier in the aging process are needed for a more complete understanding of the series of precipitation steps probably involved in the aging reaction. Peters and cupp'' have recently shown, by measurements of the kinetics of precipitation, that an 18 pct Ni-Co-Mo maraging steel shows a distinct change in precipitation behavior at aging temperatures below 850°F. The results were interpreted in terms of the existence of two types of precipitates at low aging temperatures. Only one precipitate type is present at higher aging temperatures. The low-temperature precipitate was found to be a particularly effective strengthener. No evidence for the additional low-temperature precipitate was found in the 18 pct Ni-5 pct Mo ternary alloy. The object of this investigation was to study further the characteristics of the two types of precipitates and the interaction between cobalt and molybdenum characterizing this system. Some preliminary experiments indicated a difference in reversion behavior in specimens aged above and below 850°F. This suggested that knowledge of the reversion behavior might shed some light on these two questions. Hardy and Heal11 have defined reversion as the loss of hardness, electrical conductivity, or other properties caused by heating for a very short time at temperatures above the aging temperature. The precipitate reversion referred to in this paper is entirely distinct from "austenite reversion" often referred to in maraging steel literature. This latter phenomenon could more accurately be called the diffusion-controlled formation of austenite. Much has been written about reversion in several of the aluminum-base binary and ternary alloys.'2-16 Two explanations for reversion have been advanced. Based on the classical nucleation theory of Volmer-Weber-Becker-Doring,17 Konobeevski18 suggested that reversion was due to the size of the precipitate particles

Jan 1, 1968

By P. Dayal, L. S. Darken

THE migration of carbon in austenite under the influence of an electric current has been observed qualitatively several times.14 Lebedev and Guterman5 recently have reported quantitative measurements; their method consisted of welding a low-carbon to a high-carbon wire, passing current, and later estimating the carbon distribution metal-lographically. We believe the method reported in this paper is superior in principle since electrolytic migration and ordinary diffusion are not necessarily coupled as in the weld method; also for the first time the extent of migration is determined by combustion analysis for carbon. A uniform tubular specimen (S.A.E. 1045 or 1095) was mounted as illustrated in the figures. the whole assembly being in an atmosphere of purified nitrogen. Direct current (129 to 226 amp at 0.65 to 1.0 v) served as source both of heat and of potential gradient for carbon migration. The duration of experiment was 7.5 to 12 hr, during which time the temperature was controlled (±10°C) manually. The experimental conditions are indicated in the first five columns of table I. With this experimental arrangement, the temperature initially has a maximum value at the central plane. Also, in this vicinity (by virtue of the symmetry), the carbon entering any volume element is equal in quantity to that leaving; the loss or accumulation of carbon occurs near the electrodes since the carbon moves uniformly near the center and is "frozen" at the cold ends. Hence, providing the time of experiment is not sufficiently long to seriously influence the conditions at the central plane, carbon crosses this plane only under the influence of the electrical potential gradient and not under the influence of temperature or concentration gradient. The amount of carbon which has crossed this plane was determined by combustion analysis of the two halves of the specimen. The results of these analyses are shown in the sixth and seventh columns of table I. It will be noted that substantial amounts of carbon migrated from the anode portion to the cathode portion (except at 920°C, which temperature was too low to exhibit the effect in the allotted time). In spite of precau-tions taken, considerable decarburization occurred as may be seen by comparing cols. 8 and 5. In three cases (indicated by asterisks in table I) the specimen was ground on one side, polished, and examined metallographically before analysis. One specimen was normalized and re-examined. Micrographs of selected areas in specimens 4 and 6 are shown in figs. 1 and 2, respectively. Evidence of carbon migration from the anode toward the cathode is quite apparent. Fig. 2 shows abundant graphite as well as cementite in a region near the cathode. The temperature of this zone is estimated at about 800°C. In fig. 1, particularly in the micrograph on the extreme right (the right side of which is of unaltered carbon content), there is evidence of slight depletion of carbon in the immediate vicinity of the cathode as contrasted to the general increase in carbon of the cathode half of the specimen. Although this may be attributed in part to decarbur-ization, it is believed that it is occasioned also by thermal diffusion—migration (of carbon) from a cool to a hot zone4—a phenomenon superimposed upon the electrical migration. Evidence of carbon migration was visible particu-larly during the course of the high-temperature,

Jan 1, 1951

By H. C. Fiedler

Heats of high purity iron containing 3.1 pct Si and be -tween 0.0003 and 0.0295 pct N were prepared by vacuum melting ad then pouring while in a nitrogen atmosphere with the pressure between 0 and 90 psi. Strip from a heat with 0.0184 pct N underwent complete secondary recrystallization during the final anneal. Heats with less nitrogen had too few Si3N4 particles to restrain normal grain growth, and the heat with higher nitrogen had too many particles to allow complete secondary recrystallization. In the hot-rolled structure, Si3N4 precipitates only at the grain boundaries, with the consequence that annealing after hot-rolling diminishes the ability to subsequently undergo secondary recrystallization. In contrast to this behavior, ALNprecipitates uniformly in the hot-rolled structure. Under 1 atm of nitrogen, Si3N, in 3.1 pct Si-Fe dissociates between 900" and 950°C; the solubility of nitrogen increases from 0.0010 pct at 900" to 0.0030 pct at 1200°C. The solubility of nitrogen in Si-Fe has been the subject of many investigations. Corney and Turkdogan1 heated a 2.83 pct Si alloy in nitrogen and found the solubility, under 1 atrn of nitrogen, to be 0.0019 pct at 900°C. They claimed that Si3N4 did not form in the alloy above 705°C in 1 atrn of nitrogen. Fryxell et al.2 heated samples of 3.25 pct Si-Fe containing 0.0025 pct N over a range of temperatures and then analyzed for total nitrogen by vacuum fusion and for nitrogen in solution by a modified Kjeldahl technique. At 900°C, they reported the solubility of nitrogen in equilibrium with Si3N4 to be 0.0011 pct. pearce9 found the solubility of nitrogen at 900°C under 0.95 atrn of nitrogen to be 0.0017 pct in a 3.06 pct Si alloy. He reported that Si3N4 does not form above 770°C in 1 atrn of nitrogen. Although internal friction measurements have given somewhat higher values for the solubility,4-6 if the solubility of nitrogen is as low as has been reported by most investigators, and if Si3N4 is stable up to at least 945°C at 1 atrn pressure of nitrogen as reported by Seybolt,7 a small amount of nitrogen in properly processed Si-Fe should be effective in promoting secondary recrystallization. The requirement is that in the final heat treatment there be enough small, well-dispersed particles of Si3N4 to restrain normal grain growth. Fast8 has obtained secondary recrystallization by nitriding high-purity 3 pct Si-Fe after hot-rolling to a thickness of 0.118 in., followed by processing to 0.012 in., and annealing. A large amount of nitrogen, 0.076 pct. was introduced during the nitriding heat treatment, but he has since reported9 that "a few hundredths of a percent" is sufficient. Small amounts of aluminum10 or vanadium" nitride are capable of promoting secondary recrystallization. Heats containing as little as 0.010 pct A1 or 0.042 pct V and from 0.006 to 0.009 pct N underwent complete secondary recrystallization at final gage, whereas heats with lesser amounts of aluminum or vanadium did not.l2 To be reported is the behavior of nitrogen in high-purity 3.1 pct Si-Fe, and the relation of this behavior to the ability to undergo secondary recrystallization. PROCEDURE Ingots weighing 1 lb were made by vacuum melting high-purity electrolytic iron (A104, Glidden Co.) and high-purity silicon (Monsanto Co.). The latter was used in preference to ferrosilicon to insure a low aluminum content. The design of the melting furnace permitted pouring with the furnace atmosphere either below or above atmospheric pressure. Accordingly, at the completion of melting, nitrogen was admitted to the desired pressure and the heat then immediately poured. The ingots were sound, with no indication of porosity. In Table I are listed the heats investigated, the nitrogen pressure at pour, and the nitrogen and oxygen contents as determined by vacuum fusion with a platinum bath at 1850°C, a procedure which insures measurement of the total nitrogen.13 In addition, all heats contained 3.1 pct Si and not more than 0.002 pct C, 0.003 pct S or 0.005 pct Al. It was subsequently found that the quantity of nitrogen contained in the heats in Table I does not necessarily represent that obtained under equilibrium conditions. For example, the ingot poured immediately after 1 atrn of nitrogen was admitted to the chamber contained 0.0093 pct N, whereas an ingot poured 3 min after the nitrogen was admitted contained 0.021 pct N and another poured after a 6-min delay contained 0.029 pct N. While some bleeding of the hot top occurred in the latter instance, the ingot when examined in cross section appeared sound. The ingots were heated to 1325°C in hydrogen and rapidly rolled to 0.080 in. in 3 passes. The roll speed of the final pass was reduced so as to increase the quenching effect of the rolls. The hot-rolled pieces were processed both as-hot-rolled and after heating for 3 min at 900°C in hydrogen. After cold-rolling to 0.026 in., the strips were heated for 2 min at 900°C in hydrogen, then cold-rolled to the final gage of 0.012 in. The loss of nitrogen in going from the ingot to cold-rolled strip was no more than 10 pct. The final heat treatment, which was for the purpose of develop-

Jan 1, 1970

By Eugene A. Stephenson

In November, 1932, Dr. Lacey, of the California Institute of Technology, presented before the American Petroleum Institute some of the results of his research under Project 371. The investigations described dealt particularly with changes in the physical properties of petroleum that result from the solution of natural gas therein. The solubility of Santa Fe Springs dry gas, containing 87 per cent methane, 8 per cent ethane and 5 per cent propane, had been determined in various crudes at 100' F., and 2000 lb. pressure per square inch as shown in Table 1 and Fig. 1 herewith. Originally the computations were made in terms of cubic feet per barrel, but' for a more uniform basis of comparison the results are also shown as cubic feet of gas2 per cubic foot of oil.

Jan 1, 1935

By H. C. Rogers, B. W. Roberts

Vanadium foils and wires, either cold-worked or recrystallized, show a ductile-brittle-ductile fracture sequence with temperature. At about 150°C the hydrogenated vanadium wires are found to be ductile. At room temperature the wires show brittle fracture, and at liquid nitrogen temperature the wires are again ductile, although to a lesser extent than found at 150°C. Hydrogenated cold-rolled vanadium foils have been found to fracture in unusually straight lines along the [100] texture directions. The hydrogen content required to show this [loo] texture fracture is limited to a few atomic percent in range. Hydrogen content above this range causes fracture to occur in random directions. PRELIMINARY experiments with hydrogenated vanadium foils indicated that the embrittling effect of the hydrogen on the vanadium, which was severe at room temperature, was reduced at both lower and higher temperatures. In order to investigate more quantitatively the ductility changes with temperature, vanadium wires were tested in tension at three temperatures. The reduction of area was measured and the fractures examined. Specimen Preparation—The material used was kindly supplied by A. U. Seyboltl in the form of M-in. rod. The nominal analysis was: 99.2 pct V assay, 0.2 pct C, 0.01 pct Si, 0.01 pct Fe, 0.015 pct Ca, 0.02 pct O,, 0.01 pct N2, and 0.003 pct H,. The specimens were 0.035-in. diam wires. These were prepared by cold-swaging the supplied rod to the final diameter without intermediate anneal. They were finished with long-bearing dies. The surface was then given a light polishing with 0 emery paper and degreased in trichlorethylene. An X-ray check indicated that the cold-swaged wire had a fairly strong [110] fiber texture. The wires were then recrystallized in vacuum in continuously pumped quartz tubes at two temperatures to give two different grain sizes. One group of wires was given 45 min at 800°C; another, 60 min at 1000°C. The microstructures in Fig. 1 show the wires after they have been electropolished and elec-troetched in 10 pct HCI. After the 800°C anneal, the vanadium grains had a diameter of 1 to 2p and there appeared to be a tendency to elongation in the longitudinal direction. However, the latter may be an etching effect. After the 1000°C anneal, the grains appeared to be equi-axed, but there was a very large spread in grain size, probably due to some impurity segregation in the wire, Fig. 1, right. The grain diameters varied between the limits of 1 to 150p. The small particles shown particularly clearly in Fig. 1, left, are also visible on the polished surface of all samples before etching and are undoubtedly carbides and nitrides of vanadium. An X-ray check indicated these annealed wires had a strong [110} recrystallization fiber texture. The hydrogenation was carried out in an iron retort with dry hydrogen flowing through it, the retort and contents being heated in a tube furnace with a hydrogen atmosphere. The hydrogenation temperature was approximately 500°C. The hydro-genation times chosen were approximately those which would be just enough to cause the vanadium to be brittle at room temperature and thus allow the greatest chance for ductility to occur at the other two temperatures. Part of the fine grained specimens were hydrogenated for 21/2 min at 490°C. Part of the coarse grained specimens were hydro-genated for 11/2 min at 515°C.

Jan 1, 1957

By H. Foster Bain

Jan 1, 1910

By D. Y. Geng, S. S. Peng

Surface subsidence of two longwall panels, one with a private residence and the other with an arch bridge, was monitored over a period of 1 to 1' ½ years. Surface subsidence data were analyzed in terms of zone of advance influence and delay angle of maximum subsidence velocity. The variational characteristics of both features coincide with the periodic weighting at the advancing longwall face. Surface heaving in the subsidence process can also be attributed to periodic weighting. It was found that residential damages occurred when subsidence velocity exceeded 4.5 mm/day (0.15 ft/day). The effects of locating structures on the panel center and near the gob edges are illustrated. The effect of mining on ground water was also discussed. Finally, methods of reducing structural damages are recommended.

Jan 1, 1984

By L. J. Erck, T. E. Ban

A discussion of laboratory procedures used to determine pellet quality and to simulate handling and firing conditions. Strength-temperature relationships in pelletizing; effect of chemical additives on agglomeration; and crushing, abrasion, and impact resistance of the pelletized products are discussed with respect to five different iron ore concentrates. IN most routine experimental work on products and processes, method:; of operation and product evaluation are established from accurately controlled laboratory tests. With particular emphasis on the pelletization of fine iron ore concentrates, standardized procedures of laboratory production and product testing have been established at Cleveland-Cliffs Iron Co. Research Laboratory at Ishpeming, Mich. A program of this nature was used for investigating the agglomeration characteristics of various iron ore concentrates. The factors which control the process were studied and subsequently controlled for these investigations. Pelletizing as applied to iron ore agglomeration involves the preparation of spheroidal masses from a fine moist concentrate, followed by high-tempera-ture firing to produce a final product. The preparation of moist spherorids is generally designated as balling. This produces the so-called green pellets or balls. After, these have been fired they are called pellets. Balling is accomplished by rolling moist concentrates in a revolving drum until small spheroids form by a snow-balling action. These balls are then heated in a shaft furnace, or a modification of this device, to a temperature high enough to cause agglomeration within the individual balls while they descend countercurrent to hot oxidizing gases. By this process the lour strength balls are converted through various chemical and physical-chemical processes into hard pellets. With correct balling and firing, the pellets are strong, resist abrasive action and handling treatments, and provide a suitable blast furnace and open hearth feed. In 1950 Tigerschiold and Ilmoni developed a working hypothesis to explain the formation and stability of green pellets.' Their work was presented on the basis of geologists' discoveries concerning the soil-water system and C. V. Firth's early postulates of green pellet formation.' Fundamental reactions oc-curing within fired pellets have been described by Cooke and Ban, who showed the microstructure changes caused by different firing temperatures." All these investigators have provided scientific clarifications of agglomeration by the pelletizing process and have opened avenues for greater development. Mineral grain growth and ceramic bond formation are the two basic phenomena imparting coherency to particles within a fired pellet of iron ore. Each of these is established by the transfer of thermal energy to the mineral particles. Grain growth mechanisms are chiefly physical reactions wherein smaller particles consolidate into larger ones, with resulting decrease in surface energy conforming with the second law of thermodynamics. Ceramic bond formation is a chemical reaction usually between basic and acid metallic oxides of the gangue and ore minerals. CaO, MgO, A1203, and FeO of Fe3O4, react in varying proportions with SiO, or Fe2O3, to form a great series of compounds or amorphous solid solutions. These product bond iron mineral particles together by a bridging action or by direct reaction with the surfaces of the particles. The result of the grain growth-ceramic bond formations is a consolidated, coherent compact of gangue and iron minerals formerly held together by much weaker bonds of interstitial water and forces common to dry, unconsolidated particles.4 With respect to iron ore agglomeration, these high temperature bonding reactions have been described by Schwartz, who referred to the bonds in sinters," and by Cooke and Ban, who referred to the bonds in fired pellets." The extent of the bonding phenomena and the consequent strength of fired pellets is governed by

Jan 1, 1954

INTERNAL The year 1976 was another outstanding year in the operation of the Institute and in the success of its varied activities. Total AIME membership reached 59,773 for a gain of. 6.4 percent. Total revenue increased to $5,111,2 10, up 22.4 percent, and balance sheet assets increased to $8,479,612, up 12.2 percent from the previous year. AIME and its constituent units conducted 30 technical meetings during the year, and attendance was up at most of them. Publications issued by the Constituent Societies continued a healthy growth. During the year 9 new local Sections were established, and at the end of the year the Institute had 150 Sections, with 19 of them overseas. Details on all of these operations are on pages 2 and 3 of this report.

Jan 4, 1977

By Peter L. Langsjoen, Kenneth L. Maloney

Ten small and intermediate-sized (4.5 Mg/hr to 113 Mg/hr steam--10,000 to 250,000 lb per hr) coal-fired boilers in the upper Midwest have each been tested on both a bituminous eastern coal and a subbituminous western coal. The purpose of this study was to determine the feasibility of substituting western subbituminous coal for eastern bituminous coal as a means of reducing the SO, emissions from this class of boiler and to demonstrate the feasibility of greatly expanded western coal utilization as a means of reducing the use of oil and gas. The scope of this study was such that the representative boiler types were tested on both eastern and western coal for a period of time sufficient to completely characterize their individual emission and operational characteristics.

Jan 1, 1978

The mining of coal, phosphate, oil, gas, and sodium on the public lands of the United States has, during a long period of years, been prevented by the failure of Congress to legislate, notwithstanding the fact that each successive Congress has vainly attempted to enact a law. Disagreements among members of Congress, many of which have related to non-essential matters, have prevented the passage of a bill, the failure at the last session having been due to a fillibuster in the Senate against the conference report led by Senator LaFollette of Wisconsin. Seven bills covering this subject have been introduced into the present Congress, four of which are identical in nearly all essential respects and follow either precisely or closely the conference agreement of the last Congress. These bills are too long to permit of review in this column. In general they provide for the leasing of lands or privileges to mine or to recover the various minerals above mentioned under terms and conditions as to the amount of land that may be leased by any one applicant, the diligence with which the work must be prosecuted, the return or royalty demanded, and the term of the lease and extensions thereof.

Jan 8, 1919