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By Howard Martens

HARDNESS behavior of commercial titanium alloys following various heat treating processes has been studied for some time. However, the hardness of such alloys following a definite measured cooling rate from the single phase region has not been reported. Therefore, a series of experiments was conducted on the three alloys: 150A, 130A, and 130B. The manufacturers gave the following compositions for these alloys: Ti 150A: 0.045 pct C, 0.069 pctN, 1.32 pct Fe, and 2.68 pct Cr; RC 130A: 0.13 pct C, and 7.9 pct Mn: RC 130B: 0.11 pct C, 3.5 pct Mn, and 3.2 pct Al. A method similar to that described by Greninger was used, and the cooling rate varied from 6" to 9200°F per sec. The cooling curves were recorded on a Speedomax or a recording oscillograph, and the hardness was measured on a Tukon hardness tester using a Knoop indentor with a 500 g load. The curves of Fig. 1 show the variation of the Knoop hardness with the cooling rate for these three alloys. The alloys 150A and 130B behave in a similar manner, as shown by the curves. In neither of these alloys was it; possible to retain the high temperature ß phases, even by the most rapid cooling rate. The slow cooling rates produced a typical ß structure in these two alloys. As the cooling was increased, these phalses became more finely dispersed and the hardness increased. This increase in hardness with cooling rate continued for the 150A alloy until a rate of approximately 1000°F per sec was reached. At this cooling rate, the structure showed the result of the dif-fusionless transformation of the ß solid solution to the supersaturated a solid solution which is referred as a'. At higher cooling rates, the structure showed no change and the hardness showed no great change, as indicated by the dotted portion of the curve in Fig. 1. The increase in hardness with cooling rate for the 130B alloy continued until a rate of approximately 300°F per sec was reached. At this rate the structure was produced and the maximum hardness was reached. Higher cooling rates caused no marked changes in hardness or structure. The alloy 130A behaved in a different manner, as shown by the curve of Fig. 1. The structure produced by the slow cooling rates was a typical a+ß structure, which became finely dispersed as the cooling rate increased. The hardness increased with cooling rate and reached a maximum at approximately 120°F per sec. At this maximum hardness, the structure showed the result of the decomposition of the ß phase into the ß + phase structure. As the cooling rate was increased, smaller amounts of the at phase were formed and the alloy became softer. For cooling rates of 3000°F per sec and above, the high temperature ß phase was retained and the hardness of the alloy did not change markedly. Acknowledgment This paper presents the results of one phase of research carried out at the Jet Propulsion Laboratory, California Institute of Technology, under Contract No. DA-04-495-0rd 18, sponsored by the Dept. of the Army, Ordnance Corps.

Jan 1, 1957

By W. W. Krysko

In order to calculate the critical particle size of lead oxide entrapped in lead, Stoke's Formula may be applied. All data were available except figures for the density of lead oxide at elevated temperatwes. The density of lead oxide was determined by means of dilatometmetrc and volumetric methods up to 1010°C. Graphs of the density of lead and lead oxide as well as the viscosity of lead are given and discussed, with the conclusion that the most unfavorable region for the separation of lead oxide from molten lead lies just above the melting point of lead. DURING previous investigations, particularly on the dedrossing of lead with aluminum1 and the oxygen solubility in lead,' the critical particle size of lead oxide which could be entrapped in solidifying lead was estimated by calculation, and it was shown that high values found for the oxygen content of lead may be due to the method of sampling and the entrapped particles of dross. Unfortunately, due to lack of data, an exact mathematical solution was not possible. The particle size which will separate under a given condition can be estimated from Stoke's Law, which states that where: d = diameter of the critical particle size ¦q = viscosity of lead in Poise V = constant velocity in cm sec-I g = 981 cm sec-2 61= specific gravity of lead 62= specific gravity of lead oxide The depth of the lead bath and the time before solidifying define the velocity. The viscosity of molten lead is known from earlier work by Krysko and is given in Table I. The specific gravity of lead is also known, see Table II. These values are according to Hofmann. A careful survey of literature revealed no values for the density of lead oxide at elevated temperatures. The present investigation was therefore conducted to provide this information. RESEARCH INVESTIGATIONS The density of lead oxide was determined from the following experiments: 1) Determination of the density of lead oxide at room temperature. 2) Dilatometric investigations on the same samples. 3) Determination of the shrinkage at the liquid-solid trans£ormation. 4) Density determinations on liquid lead oxide. 5) Time temperature curves during cooling. 1) The samples for the determination of the density of lead oxide in the solid state were prepared in the following manner. Molten lead oxide was cast into I hot mold which could be opened along the longitudinal (vertical) axis. The cast samples were cylinders of approximately 10 mm diam and approximately 80 mm length. The cylindrical hot mold was open at both ends and was placed on a large copper chill plate shortly before casting. The solidification of the lead oxides proceeded upwards without any formation of internal cavities. The sample was carefully checked with respect to density and crystalline appearance, and only the lower portions which were crystalline and free from porosity were used. The density was determined in a specially made pyknometer-like container, where the surplus liquid was squeezed out through an orifice approximately 1/10 mm in diameter. Mercury or water was used as the liquid. The densities of the samples were calculated from the weight, volume, and mean specific gravity of eight samples was 9.62 * 0.05 g cm"3 at 22"~. 2) The samples were machined to approximately 1 1/2 in. in length and fitted into a dilatometer. A

Jan 1, 1962

By B. C. Craft, Murray F. Hawkins, John R. Rayne

A reservoir mechanism of sulfur recovery by the Frasch process is presented. Improving the economic, of recovery appears to be largely a well, rather than a reservoir problem. A most important factor is the limitation of the lateral extraction of .sulfur about the wells due to the almost vertical .flow of the injected hot water. Model studies are described which confirin the mechanism of sulfur recovery by presently used methods. Studies on a five-spot system indicate improved econo171ics regarding recovery, recovery rate, therinal efficiency, and well spacing. INTRODUCTION Sulfur mining by the Frasch process is one of the most important methods of sulfur production. Developed by Herman Frasch in 1894, it enjoyed a rapid growth and presently supplies 40 per cent of the world's sulfur and about 80 per cent of the U. S. sulfur." The Frasch process of mining the underground native sulfur deposits involves melting the sulfur in place by introducing super-heated water into the sulfur bearing formations, and producing the sulfur as a liquid. Many problems are encountered in mining these native sulfur deposits, and sulfur production depends chiefly upon the nature of the sulfur deposit and the underground thermal efficiency of the heat transfer system. THE RECOVERY MECHANISM Sulfur is typically found in salt dome cap rock as crystal aggregates occurring within the cavities, seams, and pores of limestone and gypsum formations.' Sulfur-bearing limestone is typically cavernous, vugular, and fractured. Porosity averages about 20 per cent and sulfur saturation averages approximately 25 per cent by weight.1,15 Vhe sulfur bearing formations are very heterogeneous in nature and physical characteristics vary widely within small distances. Total cap rock thickness may vary from 50 to more than 1,000 ft, and net productive thicknesses from a few feet to a few hundred feet. In most cases the upper portion of the limestone formation is barren of sulfur, varying from 5 to 200 ft in thickness.1,15,33 The immediately overlying sediments and the underlying dense anhydrite formation provide permeability barriers to the flow of water from the cap rock section.'" Sulfur wells are drilled with conventional oilfield drilling rigs. Fig. 1 illustrates the casing program of a completed sulfur well. The cap rock sections are drilled with core bits and continuous core logs are recorded. After coring, the cap rock section is underreamed to a diameter of 9 7/8 in. The bottom of the 8-in. casing is welded closed and rests on the bottom of the drill hole, which extends through the cap rock to a few feet above the bottom of the sulfur-bearing formation. The 8-in. pipe contains 5 ft of 3/4-in. perforations on 6-in. centers and 15 ft of 1-in. perforations on 1-ft centers. The 20-ft perforated section is set opposite the lower 20 ft of the sulfur-bearing formation. The 4-in. sulfur pipe is set inside the 8-in. water line on a seat ring at the top of the 5-ft section of 3/4-in. perforations. The mining water, heated to about 330°F under a pressure of 250 psi, is forced down the annulus between the 8-in. and 441-1. pipes and through the 1-in. perforations to the sulfur-bearing formation. Compressed air, at 400 psi pressure, is supplied through a 1-in. air line near the bottom of the well to provide air-lift of the liquid

Jan 1, 1957

The high-grade orebody at Miami was mined successively by top-slicing, shrinkage, stoping and under caving. The method described in this paper was developed to enable the low-grade orebody (36,000,000 tons assaying 1.06 per cent copper) to be mined at a low cost without further dilution of the grade. The method is clearly described and illustrated by drawings and photographs, and the original paper should be consulted as it is impracticable to abstract it, beyond noting that the mining cost is just under 40 cents per ton and the average grade of ore now being produced yields less copper than the mill tailing of 1915, the tons mined per day having increased from 4000 to 18,000 in the same period. Vertical and Incline Shaft Sinking at North Star Mine By Arthur B. Foote, Grass Valley, Calif. (Tech. Pub. No. 324: Class A. Metal Mining, No. 36) THE main shaft of the North Star mine is an inclined one following the main vein at an average dip of 26 deg., a vertical shaft intersects it at the 4000-ft. (incline) level, the incline continuing to the 6300-ft. level. At this point the vein was found to give out and a new vein, called the No. 1, was found to dip in exactly the opposite direction.

Jan 1, 1930

By O. J. C. Runnalls, L. M. Pidgeon

Some observations on the kinetics of the iodide process are reported. The deposition rate is geometry-sensitive in a system containing a finely divided titanium charge. Further, results indicate that the iodine diffusion rate influences the velocity of the process. The nonvolatile iodide, Til,, forms in the hot filament zone, thus removing iodine from the cycle. TITANIUM metal of 99.9 pct purity may be prepared using a refining technique originated by Van Arkel and de Boer.' The purity of this metal, commonly called iodide titanium, exceeds that produced by any known process. In a recent application, the method was employed by Gonser et al.² to prepare titanium rods up to 2 to 3 cm in diam. In the Van Arkel-de Boer system, the relative influence of the fundamental mechanisms: l—production of titanium iodides, 2—gaseous countercurrent diffusion, and 3—decomposition, on the deposition rate have not been clearly established. Blocher and Campbell" have indicated that the controlling step in the process under practical conditions of operation may be the reaction rate of iodine with the crude metal. Fast' reported that crude titanium metal reacted with iodine rapidly, even at room temperature, in his apparatus. Little has been reported on the effect of gaseous diffusion or decomposition on the deposition rate. It is these aspects of the process about which this investigation is centered. An attempt has been made to separate these latter effects from those due to the formation of the iodides at the crude metal surface by a division of the experimental program. Reaction of Iodine with Titanium Apparatus: In the investigation of gas-metal reactions of this type, the chemical reactivity of the halogen and halide vapors dictates the use of all-glass apparatus. In such a system standard techniques for measuring reaction rates are difficult to employ. Here, a simple apparatus was devised (Fig. 1) so that some indication of the reactivity of titanium powder with iodine vapor could be obtained. A stream of iodine gas was evolved from a bulb of controlled temperature and passed over a sample of titanium powder heated in a horizontal tube furnace. The product of the reaction, TiI4, volatilized and was condensed outside the furnace in a series of four glass bulbs, each cooled to room temperature in turn. Preliminary experiments indicated that distillation was retarded in a sealed evacuated system due to a pressure build-up in the condensing end of the apparatus. Hence, the system was pumped continuously using a mechanical pump and two oil diffusion pumps in series, through a liquid air trap. The iodine bulb was made large and a capillary restriction was inserted between the titanium bulb and the condensers so that the iodine pressure over the metal would approach the equilibrium pressure over solid iodine crystals. The effect of this restriction on the evaporation rate of TiI4, was determined separately. The iodine bulb was heated in an oil bath controlled to ±2°C. The titanium bulb temperature was automatically controlled to ±5°C. Procedure: About 200 mg of —30 mesh titanium powder, weighed to 0.1 mg, was placed in the reaction bulb after part B had been joined to part A. The powder was tapped into a long (5 cm) shallow mass along the bottom of the tube. Two chromel-alumel thermocouples were inserted into the magnesium radiator which was clamped to the reaction

Jan 1, 1953

By J. E. Lamar

THAT Illinois is an important mineral producing state is well known. A value of over $237,000,000 for the mineral products in 1926 indicates the magnitude of the industries. Coal mining is the largest mineral industry, and the value of its product was about 63 per cent of the total mineral production of the state. Oil and gas constituted about 8 per cent and the non-metallic minerals about 29 per cent. This 29 per cent represents the production of a varied group of mineral industries of wide geographic distribution through the state.

Jan 1, 1929

By A. U. Seybol

Eight binary iron alloys were examined after ion nitriding experiments to determine the behavior of the following elements: Al, Mo, Mn, Si, Ti, V,Cr, and C. Only Al, Cr, Ti, and V additions caused hardening in binary iron alloys. A few steels were examined to see the effect of Cr, Cr + Al, Cr + Ti, and Cr + V. It is suggested that a useful new class of ni-triding grade steels might be those containing about I pct V. The nitriding of steel, first described by Fry1 about 45 years ago, rapidly attained commercial application with very little knowledge of the fundamentals involved. While Fry,' in describing the status of nitriding in 1932, apparently correctly postulated hardening by precipitated nitrides, the details of the nitriding process were not understood, nor has the situation changed much since that time. It is also interesting to note that the compositions of some typical nitriding steels given by Fry at that time have changed little in the intervening years. Currently used nitriding steels owe their surface hardening to either chromium (as in 4340 steel) or aluminum plus chromium as in the Nitralloy grades, where both CrN and AlN appear to contribute to harden ing. Titanium additions have been studied experimentally, but thus far titanium steels have not won wide commercial acceptance. This subject will be expanded later. The orthodox ammonia nitriding process has been reviewed very adequately many times as in Jenkins3 and Case and VanHorn,4 and their is no need to outline the process here. Ion nitriding is not as well-known, although there have been several descriptions5-9 of the process given, sometimes with comparisons with the ammonia process. Most of these papers are primarily concerned with a description of the equipment, or of the physics or electrical engineering aspects of ion nitriding, but Noren and Kindbom9 gave the results of a metallurgical investigation using both processes. In brief, ion nitriding is carried out in a vacuum chamber from which the air is exhausted and replaced by a N2-H2 mixture, typically containing 10 to 20 pct N2, at about 5 to 10 torr pressure. While ammonia gas has also been used in ion nitriding, there is no evidence that ammonia makes any improvement in the ion nitriding process. A few hundred volts dc is applied between the grounded container wall (positive) and an insulated center post supporting the work (negative) to be nitrided. A glow discharge is created in the ionized gas, accelerating positive nitrogen ions to the work. These ions contain enough energy to form the normally unstable Fe4N "white layer", thus establish- ing surface nitrogen solubility characteristic of the a Fe/Fe4N equilibrium. This creates a substantial concentration gradient, driving dissolved nitrogen into the steel. The temperature employed is in the same range (around 500" to 550°C) as in ammonia nitriding, but because of factors which are not understood at present the nitriding time is ordinarily considerably reduced in ion nitriding. Other advantages have been cited,9 but it is not the purpose of the present work to contrast the two processes. The present objective was to examine the behavior of binary iron alloys during ion nitriding with respect to the microstructure, hardness level, and depth, and to examine some of these factors in steels as well. In this way it was hoped to be able to find out something about the individual role of these elements in steels. While all the work was done by ion nitriding, there seems to be no reason why any conclusions reached would not equally apply to ammonia nitriding, excepting only the kinetic aspects of the process. Another objective was an exploration of the critical-ity of the ion nitriding variables: gas composition, pressure, temperature, and time. EQUIPMENT AND MATERIALS The equipment used was substantially as described by Jones and Martin.8 The vacuum tank was about 12 in. in diam by about 18 in. high, and consisted of water-cooled stainless steel, with a single small window at the top for viewing inside. This sat on a heavy mild steel base equipped with the main pumping port, pressure control port, and vacuum gaging. A series of variable resistances was interposed between the glow discharge and a large-capacity -40 amp variable primary transformer feeding a 1000-v transformer, but 600 v were about the maximum ordinarily used. With the small l-in.-round, 4-in.-thick discs used for nitriding, the electrical load was usually about 500 v at 0.8 amp. The specimen temperature was controlled by a stainless-steel sheathed chromel-alumel couple, whose junction was in the steel stool upon which the flat discs were placed. These were ground through 400 Sic paper. Cycling of the temperature controller caused -0.2 amp variation in ion current, providing an ample control band. The binary iron alloys were made from vacuum-melted hydrogen-deoxidized electrolytic iron and alloys of 99.9 pct purity. Cast ll-lb-square tapered ingots were forged and hot-rolled to about 11/4-in.-diam rounds. Discs of 1/4 in. thickness by about 1 in. diam were machined from the rods for nitriding specimens. The following alloys were prepared: 1 pct each of Mn, Mo, Cr, Ti, Al, V, Si, and an Fe-0.8 pct C alloy. EXPERIMENTAL VARIABLES Of the variables total gas pressure, nitrogen partial pressure, temperature, and time, only nitrogen partial pressure was found to be critical to the operation. A critical nitrogen partial pressure was found corre-

Jan 1, 1970

By W. J. Parton

THE efficient recovery and preparation of small sizes of anthracite called No. 4 Buckwheat (3/3 2 by 1/3 2 in.) and No. 5 Buckwheat (1/3 2 in. by 0), present a difficult problem to the anthracite operators. In many instances preparation of these sizes, particularly No. 5 anthracite, is extremely inefficient. In many of the older preparation plants, inadequate facilities, and often none at all, were provided as an integral part of the plant for cleaning this fine anthracite. Consequently, much of the material smaller than s, 32 in. was discarded. As the demand for these sizes increased, facilities for preparing the fine sizes were often crowded into existing structures with consequent sacrifices of capacities and efficiency. In addition to this condition, the methods of preparing the finest sizes are being developed in an attempt to improve their efficiencies. Because the demand for small sizes of anthracite still is increasing, many operators would benefit by investigating and improving the cleaning equipment employed on these sizes.

Jan 1, 1949

By Roy A. Anderson, Roger H. McConnel

The Metaline district from 1906 through 1965 has produced nearly 16 million tons of ore yielding 400,808 tons of zinc and 178,062 tons of lead. The sediments, ranging from Precambrian into the Devonian, are schist, phyllite, conglomerate, greenstone, quartzite, limestone, dolomite, and carbonaceous slates. Quartz monzonite and granodiorite of the Cretaceous(?) Kaniksu batholith are exposed over a large area beginning a few miles south of the district. There is minor Tertiary conglomerate and basalt. Abundant glacial deposits obscure much of the bedrock. Northeasterly trending folds, having steep to overturned northwesterly limbs, and thrust faults, striking northeasterly and dipping southeasterly, characterize the deformation of the Precambrian and Paleozoic rocks. Recent drilling indicates that the Slate Creek fault, too, is also a southeasterly dipping thrust fault. This new evidence suggests that the Valley Block, like the other major structural blocks, may in part be a thrust plate rather than a graben, and that thus the district may have greater structural unity with the surrounding region than has heretofore been apparent. The Cambrian Metaline Formation of limestone and dolomite contains essentially all the lead-zinc mineralization. Most of the ore mined to date has come from a carbonaceous and irregularly siliceous breccia of sedimentary and diagenetic origin, locally called the "Josephine Horizon," that makes up the top few to 200 feet of the formation. The Josephine Unit is a breccia of gray limestone, coarse light gray dolomite, very thin-bedded, dark gray siliceous dolomite, and "zebra rock" believed to be of algal origin, embedded in a matrix of black dolomite or black jasperoid or some mixture of these two. The jaspcroid fragments and irregular blobs embedded in the black dolomite matrix and the jasperoid laminae in the very thin-bedded dark gray dolomite suggest that jasperoid was formed at the same time as the breccia matrix and as the laminated dolomite. So too, the marked tendency of sphalerite and galena to be disseminated mainly in the dark breccia matrix and their tendency to be most abundant in the jasperoid laminae of the very thin-bedded dark gray dolomite, even where the mineralized and laminated dolomite is fragmented and engulfed in black dolomite breccia matrix, suggests that in these ha bits the sulfides also were deposited contemporaneously with the sediments. Yet very commonly, veins and vague veinlets and patches of white quartz, usually carrying rather coarse sphalerite and sometimes galena crosscut all rock types. These contradictory relationships throughout the Josephine Unit suggest that both the black jasperoid and the sulfides were original constituents of the Josephine Unit but that, locally, they later were remobilized and deposited as white quartz and coarser grained sulfides. Possibly, at least in part, this "metamorphism" is one of the effects produced during or shortly after the intrusion of the Kaniksu batholith.

Jan 1, 1968

By A. H. Larson, R. J. McClincy

ALTHOUGH arsenic has a very high vapor pressure and vacuum distillation appears to be a likely method for its removal from lead, the published literature contains virtually no information concerning the vacuum removal of arsenic from lead. Caldwell, Spendlove, and St. Claire1 mention arsenic in their investigation of the removal of volatile metals from lead by vacuum distillation. They do not, however, give any data for arsenic removal or refer to any actual experimental work involving arsenic dissolved in lead. Moriyama, Kozuka, and Miura2 have determined the activity of arsenic in dilute As-Pb alloys in the temperature range from 450" to 600°C using a closed galvanic cell. They found that the activities of both arsenic and lead showed a positive deviation from ideality at 600°C. In view of the lack of experimental data regarding the vaporization of arsenic from As-Pb alloys, a limited vapor pressure study was made on liquid alloys containing from 0.5 to 3.3 wt pct As in lead at 703°C. The pressure of As4(v) above the alloys studied was determined from weight-loss data collected by means of the inert-gas saturation method. The experimental apparatus and procedure used were similar to that discussed by Alcock and Hooper9 with modifications as described by the authors., The technique involved was one of passing a known volume of inert gas over the alloy to be studied in a known amount of time and determining the loss in weight of the sample. Because of the low vapor pressure of lead at 703"C, the observed weight loss could be attributed solely to the vaporization of arsenic as the tetratomic molecule AS43 Measurements of the apparent vapor pressure were repeated at different inert-gas flow rates until from three to five values were obtained which were independent of inert-gas flow rate. This value of the apparent vapor pressure was taken to be the equilibrium vapor pressure of the alloy under consideration. The vapor pressures measured in this investigation have been converted to the activities of arsenic in As-Pb alloys, Table I, by use of the data compiled by Elliott and Gleiser5 for the vapor pressure of pure arsenic. The standard state for arsenic was chosen as the pure, hypothetical, supercooled liquid. The activity of arsenic was calculated from the fourth root of the ratio PAs,/PAS,. The low magnitude of the vapor pressures given in Table I explains the difficulty en- countered by earlier workers in successfully vacuum distilling arsenic from very dilute As-Pb alloys. The data shown in Fig. 1 indicate that the As-Pb system behaves ideally. The apparent outlier represented by the alloy containing 1.43 mol pct As is a result of the fact that the pressure of As, above the alloy was barely detectable by the experimental procedure used in this investigation. Because of this, the apparent vapor pressure determined for this alloy could be in considerable error. Moriyama, Kozuka, and ~iura' have reported that arsenic shows a positive deviation from ideality in dilute solution in lead. However, details of their results have not been made available. This research was made possible by a grant from the National Science Foundation (GK-196) for which the authors are very appreciative.

Jan 1, 1970

By S. Shapiro, J. A. Ford

The crystallo graphy of several grains of the lamellar Ni-Ni3 B eutectic solidified under conditions appvoachirt equilibriun has been examined.. A preferred interlace relationship has been observed in this system which may be described as: A detailed study of this interface by means of an atomistic model reveals the interface Plane to be puckered and more accurately describable as: Analysis of the atomic configuration on these planes reveals that this interface conforms to the orientation criteria proposed for directionally solidified lanzellar eutectics. In addition, a model is proposed to help explain the growth of a "puckered" interface. DURING the past several years an increasing number of unidirectional solidification experiments on eutectic alloys have been reported in the literature. The primary emphasis, in most cases, has been the effect of growth variables on microstructure. Some authors have, however, studied the crystallographic orientations and interfacial relationships resulting from these experiments. Four crystallographic studies have been published;'-4 in each of these there is a factor which tends to prohibit the extension of the observations beyond the particular system. In the Al-CuA12 system, the approximately equal volume fractions of the phases have resulted in sorrie controversy as to which phase constitutes the matrix. In the Mg-Mg,Sn eutectic the presence of several interconnecting lamellar systems2 complicates the analysis. The two remaining eutectics. 1nSb-b and Al-Ali, are both rodlike (the latter exhibits a plate morphology at low solidification rates): the matrix in each of these alloys is the simpler (fcc) phase. Studies of nucleation in eutectic alloys indicate that the more complex constituent is the nucleating -.phase.' For the purpose of an analysis of interface crystallography it was deemed desirable to study a lamellar system in which the matrix was the more complex and, presumably. the nucleating phase. Recently it has been shown that there is a eutectic in the Ni-B system between Ni3B and i; preliminary investigation by the authors indicated that the matrix in this eutectic is the boride phase. The structure of Ni,B is reported to be orthorhombic, the compound being isostructural with cementite. This eutectic is therefore analogous to that between austenite and cementite. Furthermore, the Ni-B system is not susceptible to a competing eutectic reaction as occurs in the Fe-C alloys; nor does it exhibit a eutectoid decomposition. For these reasons the study of the interfacial relationship in the Ni-Ni3B eutectic was undertaken. PROCEDURE Ingots of nominal composition 3.5 and 3.6 wt pct B were induction-melted in boron nitride crucibles within a graphite susceptor under a boric oxide slag; a dynamic argon atmosphere was maintained over the melt to prevent rapid oxidation of the susceptor. The raw materials used were 99.97 pct Ni from Huntington Metals Division of International Nickel Co. and 99.8+ pct B chips supplied by the United Mineral and Chemical Co. The analyses of the starting materials are listed in Table I. The melt was held at 1500cC for 2 hr to insure complete reaction and allowed to cool to room temperature. The castings were chemically analyzed for boron and were metallographically examined for uniformity. The metallographic samples were mechanically polished through 0.1 p A1,0, and etched with Carapella's reagent. Each master casting was cut up to make several specimen blanks which were remelted, in boron nitride crucibles, to form ingots of 1/2 to 3/4 in. in diarn by 7 in. long. These ingots were unidirectionally solidified using a modified vertical Bridgman technique. The rate of solidification was assumed to be equal to the uniform rate at which the crucible-susceptor assembly was withdrawn from the induction coil. This rate was varied from 1.18 to 2.21 cm per hr. In order to perform these experiments it was found necessary to redetermine the eutectic composition. This was accomplished by the zone-melting technique described by Yue and lark.' An ingot of 4.5 wt pct B was zone-melted in a horizontal boron nitride boat 7-1/2 in. long with a 112-in.-square cross section. A

Jan 1, 1967

The plans for the activities of the Petroleum Division for the coming year do not differ materially from those of the past several years. The fall meeting is scheduled for Oct. 12 and 13 and is to be held at Tulsa, Oklahoma. The Division, of course, will take part in the annual meeting of the Institute at New York. A fall meeting will also be held in California at approximately the same time as the meeting at Tulsa. A number of papers are to be presented at the two meetings simultaneously. The various committees are at work arranging the programs. The Division will continue to be active in its various fields of endeavor, such as stabilization, production reviews, and economics, but special stress is to be laid on the engineering and research fields. In the past the Division has served as a forum for open and frank discussion of problems confronting the engineers in the oil industry. It is hoped that it will continue to function in this capacity. Papers presenting original ideas and extending the boundaries of knowledge and understanding in the field of petroleum production will be welcomed. Members who have interesting information to contribute should not wait until called upon by one of the Committees, but should offer a paper at the earliest opportunity. The past year has seen a decided strengthening of the control over production, with prospects of even more rigid control in the future. It is essential that production programs under such control be carefully planned and it is highly desirable that petroleum engineers take an active part in the planning, to insure efficient production of oil and minimize the waste of this natural resource. At a time like this, when it is difficult to keep the production of oil within reasonable limits, it may seem unnecessary to improve the efficiency of production methods, but, as has been aptly said, the trouble is not that we have too great a reserve of oil but that we are producing tomorrow's oil today. Therefore it behooves those who are entrusted with the engineering and scientific phases of production to learn how to get the greatest yield economically possible from the present and future fields in order that we may enjoy the advantages of petroleum products for a long time to come.

Jan 1, 1934

By J. G. Thompson

PROJECT 8411 of the U. S. Bureau of Standards, sponsored by the Iron and Steel Division of the A.I.M.E., is an attempt to define more concisely than has been possible heretofore the accuracy and the Limits ' of usefulness of the ' various methods now in use for the determination of oxygen as it exists in ferrous materials. It originated in correspondence between John Johnston and other metallurgists, and was brought to the attention of the Iron and Steel Division of the Institute at the Annual Meeting in February, 1933. As reported in MINING AND MET,ALLURGY, Vol. 14, page 152, March, 1933, "Dr. Johnston introduced, and those present adopted, a resolution that the Iron and Steel Division of the A.I.M.E., believing that a careful comparison of the several methods now in use for the analysis of steel for nonmetallic elements such as oxygen is highly desirable, heartily endorses the proposal that the U. S. Bureau of Standards act as a clearing house " in this matter, undertaking the final preparation and allocation of identical samples to those laboratories willing to collaborate in this important question, and collate the results re- ported back to the Bureau.'"

Jan 1, 1934

By Charles Janin

(San Francisco Meeting, October, 1911.) THE first successful bucket-elevator dredge to operate in California was put in commission at Oroville in March, 1898. There had been numerous previous attempts at dredging, but none of the earlier boats proved a success. The gold-miners in California early conceived the idea of a machine to dig gravel from the beds and bars of auriferous streams that were inaccessible by the methods then employed, and it was only a few months after the discovery of gold in California that such a machine was. shipped around Cape Horn from New York to San Francisco. This was, however, but the forerunner of many failures in gold-dredging, and was soon at the bottom of the Sacramento river. During succeeding years many other unsuccessful attempts were made, and it was not until 1897 that a dredge of the single-lift bucket-elevator type was floated on the Yuba river. This dredge was built by the Risdon Iron Works for R. H. Postlethwaite, and would probably have been a success if it had been operated on some of the rich Oroville ground instead of in a turbulent stream, where the dredge was wrecked during a flood, and was not repaired. Fig. 1 is a sketch-map of California, showing gold-dredging areas. It is not my intention to narrate in detail the history of the early failures in gold-dredging, and the various steps in the development of the modern boat, but merely to touch upon this in a general way, and to call attention to the wide difference in capacity and operating-cost between the first successful dredge, with an actual capacity of 600 cu. yd. per day-though its rated capacity was in excess of this-and the present modern dredge with 15-cu. ft. buckets, and an average capacity of 250,000 cu. .yd. per month. Even this enormous capacity has several times been exceeded on monthly runs. The first successful dredges

Mar 1, 1912

By Jerry Tien

Mine regulators are normally used for proper air distribution in underground mines. They are deliberately introduced resistance in the regulated airway, and by altering sizes, they can distribute specific air quantities to regulated splits and free splits (4, 5). The enactment of the Federal Coal Mine Health and Safety Act of 1969, the Federal Mine Safety and Health Amendments Act of 1977, and the regulations adopted by the Mining Enforcement and Safety Administration (now called the Mining Safety and Health ministration) prompted greater discussions of optimal mine regulator locations because of the Act's stringent ventilation requirements (2, 3). For example, by requiring the separation of the air used in the belt haulage entries from the intake and return airways, the regulations required the creation of a third type of airway---the neutral airway, as opposed to the intake and return airways, adding to the complexity of a mine's ventilation network. It is the intent of this report to show that panel regulators should be located in intake airways at the neck of a panel for a blowing fan system and in return airways at the neck of a panel for an exhausting fan system in order to achieve optimal air control. A computer simulation model is used to determine optimal mine regulator location.

Jan 1, 1983

By F. Keller, J. D. Edwards

THE anodic treatment of aluminum presents problems of scientific as well as of commercial interest.1-3 Of particular interest is the fact that, during the anodic oxidation process, the oxide continues to form at the metal-oxide interface under any oxide previously formed. This has led to speculation as to the mechanism involved in the formation of the relatively thick oxide coatings that are used commercially for decorative or protective purposes. Furthermore, the ability of certain types of oxide coatings to adsorb dyes and other substances has stimulated research to determine the actual structure of these adsorptive coatings. It has been found that anodic oxide coatings on aluminum are composed essentially of aluminum oxide. They are formed by the action of oxygen ions penetrating to the metal surface during the electrolytic oxidation treatment. These coatings can be formed in a number of different electrolytes, as for example, those which contain sulphuric acid, chromic acid, oxalic acid, or boric acid. These are the commonest and most useful electrolytes employed commercially. Except for certain specific conditions of formation, the coatings in general have been found to be amorphous alumina, as far as can be determined by X-ray or electron-diffraction methods. Anodic oxidation processes can be arranged in three rather general classes if they are grouped in relation to the solvent action of the electrolyte on the coating.4 In the first class, the electrolyte has little or no solvent action on the coating that is formed. In general, coatings produced under such circumstances are nonporous and non- adsorptive. In the second class, the electrolyte exerts an appreciable solvent action on the coating. These coatings are porous and adsorptive. Finally, for the third class, the electrolyte tends to dissolve the coating about as rapidly as it is formed. This action produces electrolytic brightening or anodic polishing of the aluminum surface and at most leaves only a very thin film of oxide. The nonporous and nonadsorptive type of oxide film is represented by the coatings that are formed when solutions of boric acid are employed as the electrolyte. It is especially significant that these impervious films are formed in electrolytes that exert little or no solvent action on the coating. Where a boric acid electrolyte is used, the coating tends to form rapidly, with the result that the flow of current is soon reduced to substantially zero. This indicates that the growth of the coating has stopped. As a rule, the thickness of the coating is roughly proportional to the voltage employed for formation and the coatings of this type are exceedingly thin. In an electrolyte of this type, the coating has a high resistance when the aluminum is made anode; consequently, any current that may flow (leakage current) is very

Jan 1, 1944

By Thunaes, Arvid

Pilot plant test work in 1942 and 1943 showed that by a combination of desliming, fine-size classification, and Sullivan deck concentration it is possible to recover heavy minerals such as cassiterite at least as fine as 10 microns in size. This appreciable improvement in gravity concentration practice has been substantiated by several full-sized plants.

Jan 1, 1950

By H. H. Rachford, and J. D. Rice

The effectiveness of digital computing machines in making technical calculations depends on how well the work is arranged to utilize the capability of the machines. This note presents a particularly useful way of calculating hydrocarbon vapor-li.quid equilibrium in the flash vaporization (or condensation) system. The method is well suited to sequence-controlled computing equipment. It is not limited to equilibrium calculations and may be used for solution of most implicit equations in one variable. INTRODUCTION There is increasing interest in the use of electronic digital computers in research and engineering calculations. This is a fortunate and inevitable trend in view of both the increasingly extensive numerical work which is becoming a routine part of many daily production operations and growing demand for the overwhelming amounts of calculations required by newly developed numerical methods for solving heretofore unsolved problems. Machines are in many ways ideally suited to the task but of necessity present certain difficulties. for a particular poblem to be solved must often be formulated quite differently from the way it would be arranged for manual solution. This is done in order to take advantage of the inherent speed and precision of electronic computers and at the same time to limit the need for number storage to the capacity of the machine. Therefore, this note is submitted to present a general and quite powerful method of finding solutions of the frequently encountered implicit equation: F(x,y1,y2,...ya)=0.......(1) where the root, x, is to be found for a given set of y1, ... yn.. The procedure is well suited for use with computing machines, for it usually requires but little storage or programming beyond that necessary to evaluate F. HYDROCARBON EQUILIBRIUM The method is described in terms of the problem it was designed to solve, i.e., the calculation of hydrocarbon vapor-liquid equilibrium in flash vaporization. Given the composition of a hydrocarbon mixture and appropriate values of the equilibrium ratios K, to find the phase ratio and compositions in a closed system: let z, be the mol fraction of the i-th component in the mixture. If K, is the ratio yl/xl, where y, and x,

Jan 1, 1952

By A. H. Larson, R. J. McClincy

Laboratory-scale decopperizing experiments with multiple sulfur addifions were conducted at 330°C on ternary Pb-Cu alloys containing, as the third elenlent, Sn, Ag, As, Sb, Bi, Zn, and Au, common impurities in lead blast-furnace bullion. For silver and tin, an increased rate and extent of 'cofifier removal was obsert3ed. The elements As, Sb, Zn, Au, and Bi had no effect or less effect as compared to sulfur additions with no i)npurily additions. THE production of primary lead in the blast furnace yields an impure lead frequently containing such impurities as copper. antimony. arsenic. tin, gold, silver iron, oxygen. and sulfur. By cooling this lead to a temperature near its melting point. most of the iron, sulfur, and oxygen and part of the other impurities are removed in the form of a dross. With incipient solidification of the lead, the copper concentration wil have been reduced to 0.02 to 0.05 pct. depending upon the concentration of the other impurities. according to Davey.' Since copper interferes with the treatment of silver after the desilverizing process, it is desirable to decrease the copper content of the lead still fur-ther before the lead is desilvered. The decopperizing of the lead is accomplished by stirring a small quantity. approximately 0.1 pct. of elemental sulfur into the lead at a temperature near its melting point, 330" to 360°C. The copper is removed as a copper sulfide which constitutes a small fraction of a voluminous dross consisting mostly of lead sulfide and entrained metallic lead. The residual copper concentration following the decopperizing operation is frequently as low as 0.001 to 0.005 pct. Thi fact has aroused considerable interest because the equilibrium copper concentration of lead in contact with solid PbS and solid Cu2S is at least an order of magnitude greater, 0.05 pct Cu at 330C. 1, 2 Most investigators have suggested that various impurities in the lead bullion are responsible for the very low copper concentrations frequently encountered in practice. There is little agreement, however? as to which of the impurities are helpful and which are not.3"11 Also. few investigators have sought to explain the mechanisms responsible for the removal of copper to very low concentrations. Willis and Blanks9 have proposed that a nonstoichiometric copper-deficient cuprous sulfide forms in place of the supposed Cu2S. Being copper-deficient, this sulfide phase would possess a low copper activity, and the diffusion of copper dissolved in the liquid lead into this phase would be greatly facilitated. Pin and wagner2 have investigated the removal of copper from liquid lead by studying the effect of impurity-doped lead sulfide on the decopperizing of pure Pb-Cu alloys. Samples of the doped PbS were held in contact with copper-saturated lead for 1 week at 33'7°C. They reported a beneficial effect on decopperizing with bismuth and antimony and no effect with tin or silver. which is directly opposite to the results observed in practice and those reported by Davey 3 and this studv. The purpose of this paper is to describe the effects of certain additive elements on the extent to which copper can be removed fro111 liquid lead by successive additions of sulfur. The impurity elements were added individually to prepared Pb-Cu alloys. The resulting ternary alloys as well as a binary Pb-Cu alloy were then decopperized with repeated additions of sulfur. EXPERIMENTAL Materials. Granulated test lead with a purity of 99.999 pct and the additive elements Cu. Ag. Sb. Bi. Zn. Sn. and Au with purities of 99.99 pct were American Smelting and Refining Co. research-grade materials. The major impurities in the lead were 1 ppm each of iron and copper. all others being less than 1 ppm. The arsenic used was a technical-grade arsenic of 98+ pct purity. Reagent-grade flowers of sulfur were melted under argon to provide small pieces free of fines. Apparatus. The decopperizing experiments were carried out in a 25-mm-OD by 375-mm-long Pyrex tube sealed at one end. The tube was mounted vertically in a resistance-heated. hinge-type tube furnace controlled to within ±lcC. Temperature measurement was accomplished by means of a standardized chromel-alumel thermocouple sealed into the base of a silica. paddle-type stirring rod. All decopperizing experiments were carried out under an argon atmosphere. Procedure. A Pb-Cu starting alloy containing 0.05 pet Cu was prepared under carbon and poured into cold tap water to produce shot. The ternary alloys were prepared by melting together 100 g of the starting alloy and a sufficient amount of the impurity element to yield the desired concentration. The resulting alloy was then homogenized in a Pyrex tube at 450C with continuous stirring. The furnace temperature was then lowered to the operating temperature of 330°C. When thermal equilibrium had been obtained at the operating temperature, individual additions of 0.2 pct (0.2 g) of solid sulfur were added to the melt and stirred in. Stirring was continued for a period of 3 min. discontinued for 5 min. and resumed for the remaining 2 min of a 10-min cycle. This cycle was repeated for as many sulfur additions as desired. When the decopperizing experiment had been completed the lead bullion was quenched and samples of the bullion and dross phases were taken for analysis. Results. The results obtained in the decopperizing

Jan 1, 1970