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By Helen L. Cannon

BOTANICAL methods of prospecting for metalliferous ores are based on the premise that deposits at depth may be reflected chemically in surface vegetation. For the past several years, on behalf of the Atomic Energy Commission, the U. S. Geological Survey has investigated on the Colorado Plateau the application of botanical methods to uranium prospecting. Results suggest that orebodies may be found under a considerable cover of barren sandstone through the absorption of uranium and associated trace elements by plants growing at the ground surface. Plant physiologists have demonstrated that uranium is a necessary nutrient for plant growth and therefore is present in all plants.' The amount present is small but measurable. The absorption of uranium by plants growing over ore deposits forms

Jan 1, 1955

By J. E. Stukel, J. Cocubinsky

A CONSIDERABLE amount of information is available on the equilibrium distribution of manganese between slag and metal under oxidizing conditions. These data have increased our knowledge of the manganese reactions in the open hearth, ladle, and ingot mold. In contrast, there is a paucity of data on the slag-metal distribution of manganese under reducing conditions. The purpose of the present investigation was to study the equilibrium distribution of manganese between blast-furnace type slags and iron saturated with carbon. Experimental Method Furnace: The induction furnace used for the experiments is shown in Fig. 1. A 1 in. pipe, attached to the transite cover, was fitted with a window through which the charge could be observed. Material could be introduced into the furnace through a tee and plug without removing the cover. A graph-it cylinder (3 in. ID and 10'/2 in. long), centered within the induction coil, was used as a heating element. During a test, a zircon plug kept the top of the furnace from becoming too hot from heat radiation. At the bottom, a graphite block on the vertical center line of the furnace and extending 1 1/2 in. into the coil, was used as a support for the graphite crucibles containing the melt. The graphite crucibles, machined from regular carbon electrode stock, had a 2% in. OD with 3/16 in. walls and were 5% in. long. The fumes present in the furnace during the early part of a run made optical readings uncertain. A noble metal thermocouple was, therefore, adopted to measure the temperatures. The arrangement used, shown in Fig. 1, allowed the silmanite protection tube to be replaced with a minimum effort. The thermocouple was calibrated against a standard Pt-Pt-Rh thermocouple in a fused quartz protection tube. The latter was inserted in the molten iron by removing the glass window on the cover. The lower couple was found to be very sensitive to temperature changes. To insure accurate temperature readings, the graphite crucibles were made to fit tightly against the silmanite protection tube. Further, to avoid contamination of the thermocouple by carbon, the silmanite tube was changed and the calibration procedure was repeated at frequent intervals. By using this temperature measuring technique, the furnace was easily held within *1O°C of the desired temperature. Because of the small free space in the furnace, no attempt was made to control the atmosphere. It

Jan 1, 1955

By C. S. Barrett

Measurements of impact hardness of ß-brass are reported for a wide range of temperatures. Abrupt softening is observed when temperatures are raised above 425ºC, accompanied by abrupt widening of deformation bands in the deformed samples. Current theories of these effects, and of the lack of twinning, are discussed. HARDNESS1 and flow stress2 of a sample of ß-brass at room temperature depend upon the temperature from which the sample is quenched. It is believed that the state of order in the superlattice is responsible for this dependence—not the order within individual domains, which reaches near-perfection during the quench from any temperature, but the size of the domains which is presumed to be a minimum in the hardest samples, those quenched from temperatures near the critical disordering temperature of 468°C. Measurements of impact hardness made over a range of temperatures and microstructural studies of samples deformed both rapidly and slowly over a range of temperatures, reported herein, should be of aid in reaching a more complete understanding of the underlying factors controlling the properties of the disordered body-centered-cubic material and the ordered material. It appears that such data have not

Jan 1, 1955

By D. L. Harris, A. M. Gaudin

Observations were made of the distribution of mercaptan containing S35 between aqueous solution and mineral and between aqueous solution and the gaseous phase. Although equilibrium may not have been attained, adsorption of the reagent was shown to occur reasily from air or aqueous solution on sphalerite, zincite, and willem-ite and to correspond to flotation. Adsorption on quartz did not similarly occur. THE following results, presented here in condensed form,' were obtained in a preliminary study of the adsorption of n-hexane thiol, hexyl mercaptan, on sphalerite, zincite, willemite, and quartz, from aqueous solution and from a gas. Interest in this subject was aroused by a Belgian report' of effective use of hexyl mercaptan for flotation collection of oxidized zinc minerals. The relatively low boiling point, 149°C, of the mercaptan3 suggested the desirability of extending the usual measurements of partition of collector between aqueous solution and gas and between gas and mineral. It is believed that this paper presents the first measurements of this type on a flotation system. Attempts were made to carry out the measurements at equilibrium, but as the work progressed it became increasingly doubtful that this desirable condition had been achieved. To control composition and extent of the gas phase, the apparatus was a wholly-enclosed thermally-controlled glass system. Because of these constraints and the desirability of dealing with pure minerals, a scale of operations was chosen in which a few grams of deslimed mineral were used in each test. It was also necessary to choose a particularly sensitive method for mercaptan analysis, and in fact a method that would permit the experimenters to follow the approach to equilibrium. For these reasons mercaptan marked by radiosulphur 35 was used. An analysis was made for the radiosulphur by a modification of the method of Gaudin and Carr. Coarsely-crystallized sphalerite was handpicked, stage-crushed in the dry state, wet-screened on a 200-mesh sieve, and deslimed in water at about 5 microns. Further treatment consisted of a wash in dilute aqueous hydrogen peroxide, drying, removal of the dark-colored fraction in a Frantz magnetic separator, washing in very dilute hydrochloric acid, repeated washing in distilled and conductivity water, and drying. The last washings showed a conductivity equivalent to a few ppm NaC1, that is, much more than would be provided, theoretically, by a saturated ZnS solution. The material was stored dry in sealed bottles. Analyses were as follows: Zn, 62.3 pct; Fe, 0.43 pct; Cd, 0.44 pct; S, 31.2 pct; Mn, 0.001 pct. The specific surface (BET method) was 2000 cm2/g. Zincite from Franklin furnace of the New Jersey Zinc Co. was hand-picked, dry-crushed, wet-screened at 100 mesh, and deslimed at about 10 microns. After drying, the associated zinc, manganese, calcium, and silicate minerals were removed in a Frantz magnetic separator. The purified zincite was washed in distilled water and conductivity water to a conductance of less than 2 ppm equivalent NaC1, dried, and stored. Analyses were as follows: Zn, 75.1 pct; Fe, 0.9 pct; Mn, 2.78 pct. The specific surface (BET method) was 1740 cm 2/g. Willemite, also from Franklin furnace, was purified similarly. Analyses were as follows: Zn, 52.5 pct; Fe, 0.12 pct; SiO², 27.3 pct; loss on ignition, 0.13 pct. The specific surface was 1760 cm 2/g. Conductivity water (double-distilled) and demin-eralized-distilled water were used in most of the tests. The specific resistance was not less than 600, 000 ohms, and usually above 1,000,000. Radiosulphur-marked hexyl mercaptan (1-hexane thiol) was synthesized by Tracerlab, Inc., Boston. Two lots were secured several months apart. The last lot, consisting of about 0.5 g of the mercaptan, had a total activity of about 10 millicuries. Tracerlab Co. guaranteed only the activity; hence a quasi -vapor pressure determination (based upon an S analysis) of the mercaptan was made. The calculated value, 4.2 mm of mercury at 25.5' C, has been compared with that of a sample of Highest Purity 1-hexane thiol from Fisher Scientific Co. The latter had a vapor pressure of 4.5 mm of mercury at 2.5 C. Analytical Procedures The sample containing radiosulphur-marked mercaptan was oxidized to convert the mercaptan sulphur to sulphate, carrier barium sulphate being added to provide a suitable quantity of total barium sulphate in a filter cake. The precipitate was filtered and dried, and counting was carried out either in a streaming-gas (Q-gas) counter for high sensitivity or with an end-window G-M counter for convenience. The oxidized and precipitated mercaptan gave a radioactive count of 65 counts per minute per microgram in the end-window Geiger-Mueller counter and 1100 counts per minute per microgram in a Q-gas counter. For standardization of the mercaptan solution, 15 replicate analyses were made. The average deviation per measurement was about 1600 cpm in 65,000 cpm, the probable error in the mean being 275 cpm. It

Jan 1, 1955

By W. A. Boyer

If the safety factor of a mine hoisting rope is checked for the lowest depth, is the rope then safe for all levels? The answer here is no. A new set of volues is proposed. HOISTS for metal mines are seldom designed for one particular depth. They are intended for an ultimate load and depth with a given speed but are first used to hoist from a shallower depth, gradually working to the ultimate as development progresses. Sometimes the mine is not worked on the upper levels because of the kind and grade of ore, the mining of which depends on market conditions. In this case the hoist may be used in the same working shift to lift ore, for example, from the 1200 and the 4400-ft level. This means that the safety factor of the rope should be considered not only when it hoists from the greatest depth, but also when it hoists from the upper levels. According to present safety factor standards, a hoisting rope can have ample safety margin when hoisting from the lower or lowest level and still be shy of sufficient safety margin when hoisting from the upper levels. This will be shown by curves presented in this paper. The safety factor of a hoisting rope as defined by the U. S. Bureau of Mines' is the ratio of the static load to the tensile strength of the rope. It is calculated by dividing the breaking strength of the rope* In Fig. 1 curves A and B are plotted against the vertical suspended distance, which is the abscissa, and the factor of safety, the ordinates. Curve C is a smooth curve drawn through the midpoints of the steps of curve A and would more closely represent the minimum factor of safety for new rope for any particular depth. Curve D is a smooth curve drawn through the midpoints of the steps of Curve B and would more closely represent the minimum factor of safety when ropes should be discarded for any particular depth. If a new rope were applied with a minimum factor of safety, then the vertical distance or ordinate under curve D for any particular depth, divided by the vertical distance or ordinate under curve C, would represent the minimum percent of remaining area intact that could be allowed before the rope would be discarded. Also, that section of the ordinate between curve C and curve D is proportional to the section of the area of the new rope that could be allowed for wear and broken wires. Considering that point at 2500 ft on the chart, the ratio do to co would be the minimum percent of rope area remaining at the point of discard. The ratio of that portion of the ordinate cd to co would represent maximum percent of area of a new rope available for wear and broken wires.

Jan 1, 1955

By W. Rostoker, R. P. Elliott, B. W. Levinger

Phase equilibria in the Ti-Mn-Mo system have been investigated in the composition range 100 to 60 pct Ti and in the temperature range 550 to 1150°C. Three out of ten isothermal sections are presented as well as seven vertical sections, projections of the beta space and the surface of incipient melting. A STUDY of the system Ti-Mn-Mo was undertaken as part of a program to aid in the development of titanium-base phase equilibrium diagrams of potential technical importance to alloy development. The scope of the investigation included the composition range 100 to 60 wt pct Ti (all compositions refer to weight percentages) and the temperature range 550" to 1150°C. A surface of incipient melting was constructed from measurements of a large number of alloys. In the binary system Ti-Mo,' the high temperature modification of titanium generally spoken of as the p phase is stabilized to successively lower temperatures with increasing alloy content. There are no known intermediate phases, and complete miscibility exists between body-centered cubic titanium and molybdenum. The u solid solution is limited to less than 0.8 pct Mo at temperatures between 885" and 600°C. An equilibrium diagram for the binary system Ti-Mn has been published.' Manganese behaves as a p stabilizer but undergoes a eutectoid transformation at about 20 pct Mn and 550°C to a plus an intermediate phase. The structure of this phase has been found to be isomorphous with the a phase FeCr." Accordingly, the phase is assigned the formula TiMn, although its actual location on the composition scale has not been determined and may well be not exactly at the equiatomic composition. In disagreement with ref. 2, the origin of the TiMn phase has been shown' to be a peritectoid transformation at a temperature between 900" and 1000°C. A second intermediate phase occurs at the atomic proportions TiMn,. The structure of this phase was originally established by Wallbaum" as having a hexagonal lattice (C 14 type, 12 atoms per unit cell) isomorphous with MgZn,. In this work, the structure determination was confirmed and lattice parameters determined to be: a = 4.815 kX, c - 7.901 kX. Because of the extensive range of the P phase, the ternary system was suited to the determination of the phase boundaries by the parametric method of Andersen and Jette." During the course of the investigation, this method was found applicable only to the P/a+P boundaries but not to P/P+ compound boundaries. Metallographic methods were used alternatively for delineating these phase boundaries. Preparation and Treatment of Alloys Over 70 alloys were prepared for the study of this system. Ten gram alloy buttons were arc melted in a nonconsumable electrode furnace using inert atmosphere protection, and a water cooled copper crucible. The construction and operation of this type of melting unit has been described.' To insure complete solution of alloy additions, especially molybdenum, the buttons were remelted alternately on top or bottom as many as five times. This was accomplished by a suitable mechanism for "flipping" the ingots over. It was very difficult to obtain homogeneous melts in the region of less than 75 pct Ti because of the very high melting point of molybdenum and Ti-Mo master alloys and the comparatively low boiling point of manganese. Thus, the arc conditions for insuring complete solution of molybdenum were incompatible with the prevention of heavy losses of

Jan 1, 1955

By R. J. Hopkins, L. B. Haney

On the basis of limited experimental work conducted at the Port Pirie smelter, it would appear that, by increasing the specific surface of sinter, and possibly that of coke as well, a marked increase in the rate and degree of sinter reduction in the furnace shaft can be achieved. Fusion-point tests have shown that this increased reduction means a much higher sinter fusion point and narrower plastic zone, while the more efficient utilization of coke in the furnace is inherent in the intensification of reduction by the provision of a more reactive sinter surface. Investigations aimed at increasing the ability to operate the blast furnace with a higher lead tenor of sinter reducing fuel cost proportionately, and at eliminating the loss in reduction potential in coke entering the furnace, as shown by the presence of appreciable proportions of CO in the top gases, are reported. Several lines for future investigations that could result in improved smelting methods are proposed. A SOMEWHAT informal presentation of ideas on lead blast-furnace smelting will be given in this paper. These ideas have been developed during observations of furnace behavior at Port Pirie and earlier at Mt. Isa, and have been guided by the results of laboratory experiments at Port Pirie. The authors do not intend to propound any particularly new theories, but present their ideas as a basis for discussion which may help toward a better understanding and improved control of blast-furnace operation. Performance variations of considerable magnitude occur from time to time at most lead blast-furnace plants. While Port Pirie is fortunate in having a very regular supply of high grade concentrates, it is no exception in this respect. Such irregularities are of considerable economic importance and they constitute a challenge to present-day metallurgists in their efforts to obtain an ever greater degree of control over furnace operation. In operating as Port Pirie does with a relatively high lead charge, it has been recognized for a long time that shaft conditions are ,of the greatest importance. A practical, or engineering, attack on the problem of accretions consisted of changes in furnace design, e.g., by widening the shaft to 10 ft above the bottom row of tuyeres, and by the provision of curved ends and vertical walls.' That this attack has had a great measure of success is shown by the fact that barring down of these wide furnaces is rarely necessary, shaft conditions have greatly improved, and sensitivity to charge variations has been markedly reduced. These modifications, followed by some metallurgical changes (chiefly the incorporation of pig iron into the furnace charge in 1948), have brought furnace operation to a point where some variables which were previously masked can now be studied. Accordingly, over different periods of time during the last five years, such variables as could be given numerical values have been recorded and subjected to statistical examination. The objectives of this work were: 1—to reveal the true importance of the different variables and 2—to show the proportion of total furnace variation which is unexplained and therefore referable to causes not measured at present? e.g., shaft accretions, sinter structure, coke structure, and others. Statistical Study of Variables In this work factors relating to furnace speed and lead reduction have been examined: 1—slag com-

Jan 1, 1955

By N. Brown

From the theories of flow and fracture it is shown that the difference in reciprocals of the transition temperatures (OK) is a quantitative measure of temper ernbrittlement. Experimental data are given which support this conclusion. STUDIES of temper embrittlement have been made with various viewpoints; some involved a study of the kinetics of the reaction,',2'" others were concerned with changes in the mechanical properties," . and still others investigated the structural differences between the embrittled and unembrittled states by means of the microscope," -ray ,' measurements of electrode potential," and electrical resistivity." In all these studies, the difference in impact properties was the criterion for distinguishing between the embrittled and unembrittled states. By common agreement the difference in transition temperatures is now taken as a measure of the degree of embrittlement, and this measure is used as the quantitative measure upon which studies of the phenomenon are based. Vidal and Jolivet"' suggested that the degree of embrittlement was the same whether measured by impact or by a slow bend test. Their conclusion was based on tests at constant temperature. Jaffe and Buffum" using the impact and slow bend test showed that, for a given degree of embrittlement, the difference in transition temperatures varied with the method of testing. Hultgren and Chang" showed that the difference in transition temperature produced by the V-notched Charpy impact test was not the same as the value produced by the keyhole-notched impact test. This is a very fundamental point because there can be no true measure of temper embrittlement unless it is invariant with respect to the test method. Theory The purpose of this analysis is to show how the transition temperature depends on the stress distribution and the state of the material. The criterion for fracture may be stated as follws: where iF is some function of the principle stresses and F is a critical condition depending on the state of the metal. Similarly yielding occurs when Where is another function of the prin-ciple stresses and Y is a critical value depending on the state of the material. There is some controversy as to the exact form of the function f,.(u,, u,, us) but most experimental data give the following criterion:= where 8, and 6, = 21 or 0. Combinations of 6, and 8, give the various criteria such as the normal stress, the hydrostatic tension, and the maximum shear stress laws. Agreement is general that the octahedral shear stress law adequately describes the yield condition. where the bracketed factor will be called the design factor and depends on the stress distribution. Whether the metal decides to yield or fracture is given by the condition that The effect of temperature and strain rate upon Y has been studied by various investigators, It has been shown by MacGregor and Fisher" that

Jan 1, 1955

By W. J. West, W. W. Garvin, J. W. Sheldon

One of the most important problems of reservoir mechanics is the prediction of the behavior of a gas and oil producing reservoir for a variety of production programs. In the absence of a knowledge of the behavior of even idealized systems, it has been difficult, if not impossible, to determine which production program would yield maximum economic recovery. The problem was formulated mathematically many years ago, hilt a solution of the equations had never been obtained because of their extreme complexity. The solution of the problem became possible, however, with the advent of modern computing machines. This paper describes a digital method of solving the problem and discusses some of the results which have been obtained to date. The IBM Type 701 Electronic Data Processing Machines located at IBM's New York Scientific Computing Service were used successfully to perform the computations. The flow of gas and oil through a reservoir can be described mathematically by two second-order, nonlinear partial differential equations which must be solved simultaneously. All derivatives were replaced by finite differences to bring the equations into a form suitable for digital calculations. A number of finite ditference formulations were investigated and one form was found which resulted in stable, convergent solutions. This form was used to obtain .solutions for both radial and linear systems producing by solution gas drive. The results presented in this paper are: (a) saturation profile within the hypothetical reservoir vs. time, (b) pres.strre profile within the hypothetical reservoir vs. time. (c) gas-oil ratio vs. cumulative recovery, and (d) ultimate recovery. The saturation profile clearly shows the effect of critical gas saturation. The saturation near the well-bore drops quickly to the critical gas saturation and remains essentially at that value until the remainder of the reservoir also has dropped to the critical gas saturation. The pressure profile shows a smooth variation of pressure across the reservoir. The gas-oil ratio drops slightly during the early stage of production until the critical gas saturation is reached, rises rapidly from then on and eventually passes through a sharp maximum just before the economic limit of production is reached. For the radial example presented in this paper, the average oil .saturation of the reservoir at a time corresponding to the limit of economic production was 56.5 per cent and the ultimate recovery was 6.86 per cent. The difference between change in saturation and ultimate recovery is caused by .shrinkage of the oil phase. The solution time with the 701 Computer is sufficiently short to permit an economically feasible investigation of the effects of variation of the many parameters which describe an oil reservoir. In particular, the ultimate recovery for various systems can he determined as a function of rock and fluid properties, of well spacing. and of production rate. INTRODUCTION The effective planning for maximum economic depletion of oil reservoirs is one of the major problems confronting oil producers. The most important part of the planning is prediction of the response of the oil reservoir to a particular production program. The production program can be selected by imposing certain controls available to the operator. Some of these controls are: (a) well spacing, (b) production rate, (c) time

Jan 1, 1955

OFFICERS AND DIRECTORS (The Officers are the President, 6 Vice-Presidents, the Treasurer, and the Secretary) President and Director HENRY DEWITT SMITH' Past President and Director LEO F. REINARTZ President-elect and Director C. E REISTLE, JR

Jan 1, 1955

By R. E. Carter, F. D. Richardson

Self-diffusion coefficients have been measured for iron in wustite (700° to 1000°C) and for cobalt in cobaltous oxide (800&apos; to 1350°C) by means of radio-isotopes. Both sectioning and decrease of surface-activity methods have been used and a particular shortcoming of the latter method has been disclosed for wustite. The effects of oxygen pressure on the composition of cobaltous oxide and on the diffusion coefficient of cobalt in the oxide have been established. The effect of the preparation conditions of the cobalt-oxide specimens on the diffusion measurements has been determined. It has been concluded that diffusion of cobalt occurs via vacant cation sites and that a cobaltous-oxide disk reaches equilibrium with its environment in a time which is very short compared with that needed for diffusion of the radio-isotope. THE availability of radioactive isotopes in recent years has permitted the measurement of many self-diffusion coefficients which were hitherto impossible to determine. With the advent of radioactivity, the method of measuring diffusion coefficients has also changed. The earlier sectioning method by which the concentration profile of the diffusing species was determined in the diffusion specimen has often been rejected in favor of the decrease of surface-activity method first developed by Von Hevesy,&apos; and extended by Steigman, Shockley, and Nix,&apos; and Raynor, Thomassen, and Rouse." With the experimental arrangement where an infinitely thin deposit of tracer is diffused into a semi-infinite cylinder, the decrease in activity of the active face due to diffusion of the tracer into the specimen is measured by counting the active face before and after diffusion. Under these conditions, the appropriate solution of the diffusion equation is R = e*(l-<K/Z) [1] where R is the ratio of the counting rates after-to-before diffusion, $& is the Gaussian error integral of \/Z, and Z is defined as Z = p2Dt, p being the linear-absorption coefficient of the detected radiation in the diffusion specimen, D the self-diffusion coefficient, and t the diffusion time. In the older sectioning method the concentration distribution of the tracer is found after diffusion by analysing thin parallel sections cut from the active face of the diffusion specimen. As seen from the solution of Fick&apos;s second law for the distribution of an infinitely thin source after diffusion into a semi-infinite cylinder the log of the concentration plotted against x&apos; will be a straight line of slope log e/4 Dt. The diffusion coefficient thus can be calculated directly. The units of the tracer concentration are completely arbitrary, since any change in units does not change the slope of the log c vs x2 lot. Although both of the above methods have been widely used, a thorough experimental comparison does not appear to have been made. Birchenall and Mehl,&apos; during an investigation of the self-diffusion rate of a and r iron by the surface method using Fe" tracer, diffused and sectioned one welded couple. The diffusion coefficient from this run agreed with those by the surface method. Buffington, Bakalar, and Cohen," during an investigation on a and y iron

Jan 1, 1955

By C. A. Siebert, S. H. Bush

Isothermal temper-embrittlement studies were conducted on a 5140 steel at various temperatures for times as long as 3000 hr. Specimens from the embrittled steel were subjected to impact tests, metallographic examination, microhardness, and lattice-parameter measurements. SEVERAL of the steels in the low alloy group are subject to a pronounced decrease in impact energy if held within, or cooled slowly through, a range of temperatures below the lower critical. This phenomenon, known as temper embrittlement, is quite pronounced in the chromium steels of which AISI 5140 is typical. This study considered the response of one heat of 5140 steel when embrittled isothermally at various temperatures for times as long as 3000 hr. Excellent reviews of the work done in the field of temper embrittlement have been written by Hollomonl and Woodfine.&apos; Both authors list the various theories which have been advanced to explain temper embrittlement. Some of the mechanisms considered were: 1—a transformation below 700°C; 2—an allotropic modification of iron; 3—precipitation from the ferrite of such compounds as carbides, nitrides, phosphides, or chromium oxides; 4—decomposition of retained austenite; 5—modification of special carbides; 6—grain-boundary segregation; and 7—selective distribution of carbides. The present study investigated the changes in hardness, Meyer&apos;s number, impact properties, micro-structure, and lattice parameter which occurred on embrittlement. Previous studies considered the influence of microstructure and of prior austenitic grain size3 on the response of 5140 steel to temper embrittlement. Equipment and Procedure All samples were taken from one heat of 5140 steel; the chemical composition of this steel was: 0.43 pct C, 0.86 pct Mn, 0.020 pct P, 0.019 pct S, 0.27 pct Si, 0.84 pct Cr, 0.10 pct Ni, 0.06 pct Mo, 0.10 pct Cu, and the remainder Fe. The material was received as % in. rounds. This stock was cut down to blanks measuring approximately 0.425~0.425~2.196 in. Heat Treatment: The rough blanks were normalized at 1600°F (870°C) for 1 hr, then austenitized at 1600°F (870°C) for 1 1/2 hr, and quenched into an agitated oil bath. The specimens were tempered at 1275°F (690°C) for 5 hr and water quenched. These tempered specimens were designated as the toughened state. Embrittling Treatments: The tempered bars were divided into sets and subjected to the various embrittling treatments listed in Table I. Temperatures from 750" to 1050°F were investigated for times of 1 to 3000 hr. Special tests to determine the effect of heating a short time at a higher temperature after long-time embrittlement at some lower temperature were also conducted. All specimens were water quenched at the end of the embrittling cycle, then ground and notched to obtain standard Charpy V-notch specimens. Impact Tests: The bars were fractured in a 260 ft-lb Charpy impact unit; specimens were fractured at temperatures ranging from —315°F to room temperature. Fixed temperatures used consisted of —315°F with liquid nitrogen, —115°F with dry ice and acetone, and 32°F with ice and water. Intermediate temperatures were obtained by suspending the bars in a jig over the liquid nitrogen, dry ice and acetone, or ice and water.

Jan 1, 1955

By R. I. Jaffee, F. C. Holden, H. R. Ogden

Ti-Mn alloys were studied in order to determine the factors affecting the mechanical properties of &stabilized titanium alloys. The principal compositional factors have been found to be solid-solution strengthening, the martensitic transformation, and instability of the P phase. Structural factors, such as grain size and shape, were found to have more influence on ductility and toughness than on strength. THE alloys of titanium with the &stabilizing elements offer the chief hope for developing useful heat treatments. Conversely, the heat-treatment response possible with the p-stabilizing elements causes difficulties such as weld embrittlement and thermal instability during service at elevated temperature. Therefore, it is of considerable technical importance to understand the factors that govern the heat-treatment responses in these alloys, so as to be able to soften the alloys if they are embrittled by an adventitious heat treatment, to render them stable in service, or to harden them while maintaining adequate ductility and toughness. The Ti-Mn system is a good example with which to demonstrate the factors that govern strength and heat-treatment response in. a P-stabilized system. The region of the a-j3 transformation, after the work of Maykuth, Ogden, and Jaffee,&apos; is shown in Fig. 1. The a solubilities are low. This means that, in the two-phase a-p field, partition of manganese between the two phases occurs practically only to the P phase. The solid-solution effects are therefore chiefly the result of solution in the ,8 phase. The eutectoid occurs at 20 pct Mn and 550°C, and proceeds very sluggishly. It can be ignored in heat treatments in hypo-eutectoid alloys, except for long-time storage at low temperatures below the eutectoid temperature. Even here, there is some question that diffusion proceeds far enough to involve eutectoid decomposition. Three compositional factors bear on the mechanical properties and structure of titanium a-P alloys. These are: 1—solid-solution strengthening, 2—mar-tensite transformation, and 3—P instability. Combined with the purely structural factors of grain size and shape, these govern the properties of the alloys. Perhaps the most important factor is solid-solution strengthening. The facts that manganese dissolves in a titanium to a maximum of only 0.5 pct and most of the manganese partitions to the p phase dominate the structure and properties of the a-/3 alloys. Because of the overwhelming preference of manganese for the ,3 phase, the P phase is harder and the a phase is softer. The relative amounts of both phases may be modified by heat treatment in the a-P field as application of the lever rule in the two-phase field clearly shows. A critical temperature in the Ti-Mn diagram is 800°C. This is the P transus temperature of the 6.4 pct Mn alloy, which has the lowest manganese content which will form all retained-P phase on quenching to room temperature. Any quench performed from below 800°C will produce a structure consisting of only a, a plus retained P, or retained p, for alloys of the compositions used in this work. For alloys containing less than 6.4 pct Mn, any quench from above 800°C will always result in structures

Jan 1, 1955

By Strathmore R. B. Cooke, Iwao Iwasaki, C. S. Chang

The effects of aeration on an aqueous suspension of pyrrhotite were studied and their results correlated with flotation tests using xanthates as collectors. The effects of copper activation and of pH variation were determined and possible mechanisms postulated. PYRRHOTITE has long been considered a gangue mineral to be eliminated as tailing in the treatment of various sulphide ores. However, in recent years the world-wide lack of sulphur resources has called attention to this mineral as a potential source of both sulphur and iron. Its importance as an economic mineral, however, has not been particularly emphasized. For this reason very little is known about its response to flotation, except that it can be depressed easily in alkaline circuit, by long aeration,1,2 addition of oxidizing agents,3 or by starch.&apos; The object of this work was to study the floatabil-ity of pyrrhotite. This includes the effect of oxidation by aeration, of copper activation, and of change in pH. Preparation of the Pyrrhotite Sample: It was desirable that the highest grade of pyrrhotite obtainable be used for this experiment, since the presence of other minerals could affect the surface properties.5 However, no pyrrhotite was available as crystals, and massive deposits of hydrothermal origin commonly contain considerable amounts of chalcopyrite. Pyrrhotite concentrate was, therefore, prepared from a sulphide deposit occurring near Aitkin, Minn. The deposit is of pyrometamorphic nature consistirlg mainly of pyrrhotite and pyrite with graphite, silicates, and carbonates as gangue. The ore, already crushed through 3 mesh when received, was screened at 65 mesh and the undersize discarded. The oversize was crushed through rolls, and then stage-ground dry in an Abbe porcelain mill, the —65 mesh portion being screened out after every 15 min of grinding until all the material passed through this size. The ground product was then concentrated with a drum-type dry magnetic separator. The rougher concentrate was cleaned twice and then demagnetized. The final product was split in a Jones splitter and stored in air-tight bottles. Microscopic examination of the concentrate showed that it was relatively clean and free of pyrite, locked particles, and gangue. By means of the krypton gas adsorption method," the specific surface was determined to be 3000 cm2 per g. The chemical and screen analyses of the final concentrate are given in Tables I and II respectively. It is a well-recognized fact that the oxidation of some sulphide ores during stockpiling, grinding, and conditioning affects their flotation behavior. The problem of oxidation may become serious in the case of pyrrhotite, since this is known to be more easily oxidized than many other sulphides. To ascertain the extent of oxidation, an experiment was carried out by aerating an aqueous suspension of pyrrhotite with air, oxygen, and nitrogen as follows. A 300-g sample of pyrrhotite in 2700 ml of water was agitated and simultaneously aerated in a Fager-gren-type laboratory flotation machine. A Precision wet test meter was connected to the air inlet valve, the flow rate of the gas being kept constant at 0.3 cu ft per min throughout the experiment. Samples of approximately 30 ml each were taken from the cell at 0, 4, 10, 20, 35, 60, and 90 min. After the pH was taken, each sample was filtered and the filtrate was analyzed for total iron and sulphur. The iron was determined colorimetrically by the thioglycolate method using a green filter.&apos; The filtrate was oxidized with bromine to convert all of the soluble sulphur compounds into sulphate and this was determined with a Parr turbidimeter." When aeration tests were made in alkaline circuit, calcium hydroxide or sodium hydroxide was added at regular intervals to maintain a constant pH. A similar procedure was followed in an experiment to determine the abstraction of copper. ion by pyrrhotite. In this case various quantities of cupric chloride were added. The filtrate from each sample taken was analyzed for copper, total iron, and sulphur. The carbamate method with a green filter was used for the copper analysis,&apos; since this method could tolerate a considerable amount of iron in the solution. A pneumatic cell, made from a 350-ml fritted glass Buechner funnel, was used for this experiment. The detail of the assemblage has been described elsewhere." In the present work a stainless steel baffle was inserted in the cell. This baffle overcame the tendency for the coarse pyrrhotite particles to be swirled around the wall of the cell and thus fail to collect in the froth. A 50-g sample of pyrrhotite was added to the cell which contained 260 ml of water. When pretreat-ment of the sample was desired, reagents, such as activator and pH regulator, were then added and the pulp was conditioned for a specified conditioning time. Prior to the addition of the collector approximately 15 ml of the solution were removed for pH measurement and for iron and sulphur analyses. Copper when used as activator was also determined. Collector and frother were then added and the pulp was conditioned for an additional 2 min. Air was admitted to the cell and the froth removed. The separation required from 4 to 6 min, depending on the characteristics of the froth. The float and non-float products were filtered, dried, weighed, and assayed for iron.

Jan 1, 1955

Safety Factor Characteristic Curves. Their Application to Mine Hoisting Ropes. (Paper by W. A. Boyer, Transactions AIME, 199, 989; Mining Engineering, October 1954. Discussion by B. E. Grant.) ............................................................................................................................. 1101 The Use of Wooden Rock Bolts in the Day Mines. (Paper by Rollin Farmin and Carville E. Sparks, Transactions AIME, 196, 922; Mining Engineering, September 1953. Discussion by Edward Thomas.) ................................................................................................................................. 1101 An Analysis of Mine Opening Failure by Means of Models. (Paper by Bernard York and John J. Reed, Transactions AIME, 196, 705; Mining Engineering, July 1953. Discussion by J. P. Zannaras.) ... 1102 B — Minerals Beneficiation Flotation and the Gibbs Adsorption Equation. (Paper by P. L. de Bruyn, J. Th. Overbeek, and R. Schuhmann, Jr., Transactions AIME, 199, 519; Mining Engineering, May 1954. Discussions by W. E. Ewers and Masayoshi Wada.)........................................................................................... 1103 Manganese Upgrading at Three Kids Mine, Nevada. (Paper by S. J. McCarroll, Transactions AIME, 199, 289; Mining Engineering, March 1954. Discussion by J. Bruce Clemmer, J. B. Rosenbaum, and C. H. Schack.)............................................................................................................. 1105 A Physical Explanation of the Empirical Laws of Comminution. (Paper by D. R. Walker and M. C. Shaw, Transactions AIME, 199, 313; Mining Engineering, March 1954. Discussions by Dimitri Kececioglu, George B. Clark, and Fred C. Bond.) ......................................................... 1106 F — Coal Underground Electrocarbonization of Coal and Related Hydrocarbons. (Paper by T. C. Cheasley, J. D. Forrester, and Erich Sarapuu, Transactions AIME, 199, 908; Mining Engineering, September 1954. Discussions by John G. Tripp and James L. Elder.)....................................................... 1108 Longwall Mining and Mechanization, with Special Reference to Nova Scotia. (Paper by Frank Doxey, Transactions AIME, 199, 701; Mining Engineering, July 1954. Discussion by Louis A. Turnbull.) ........................................................................................................................................ 1109 Cleaning Various Coals in a Drum-Type Dense-Medium Pilot Plant. (Paper by M. R. Geer, W. A. Olds, and H. F. Yancey, Transactions AIME, 196, 696; Mining Engineering, July 1953. Discussion by John Griff en.)................................................................................................................................. 1110 Frontiers in Heat Extraction from the Combustion Gases of Coal. (Paper by Elmer R. Kaiser, Transactions AIME, 199, 304; Mining Engineering, March 1954. Discussion by G. A. Vissac.) ............ 1112 Exploration of the Oaxaca Coal Fields in Southern Mexico. (Paper by Luis Toron and Salvador Cortes-Obregon, Transactions AIME, 199, 505; Mining Engineering, May 1954. Discussion by John D. Price.).................................................................................................................. 1113 H — Industrial Minerals Alkali Reactivity of Natural Aggregates in Western United States. (Paper by William Y. Holland and Roger H. Cook, Transactions AIME, 196, 991; Mining Engineering, October 1953. Discussions by Dexter H. Reynolds and W. L. Merritt.) ......................................................... 1114 Characteristics of Titaniferous Concentrates. (Paper by L. E. Lynd, H. Sigurdson, C. H. North, and W. W. Anderson, Transactions AIME, 199, 818; Mining Engineering, August 1954. Discussion by D. R. Grantham.)........................................................................................................................ 1116

Jan 1, 1955

By Shiou-Chuan Sun

THE effects of oxidation on the flotation behavior of sulphide minerals have been extensively studied 1-3 but no similar study has been made of coals. Coals of bituminous and lower rank undergo atmospheric oxidation during mining and storage, and their degree of oxidizing increases with temperature, 4,5 and time of exposure." The problem of recovering fine oxidized coal from culm piles, rivers, and streams by froth flotation has become increasingly important to the coal industry as well as to those concerned with air and stream pollution. This paper describes the flotation behavior of oxidized and unoxidized coals and carbons in the presence of oily collectors and presents the reagents found effective in the flotation of oxidized coals and carbons. Except where otherwise stated, flotation tests were performed in a 50-g Denver flotation cell. Solid feed for each test was 30 g, and the pulp dilution was kept at 8.5. The —65 mesh coal sample was wetted by agitation with water in the flotation cell for 6 min, then conditioned with a predetermined amount of collector for 2 min, and finally floated with pine oil as frother for 3 min. The oxidation of coals and carbons was performed in a vertical, electrically heated glass tube, shown in Fig. 1. One hundred grams of —65 mesh coal were fed into the glass tube and heated to 10° to 20 °C below the predetermined temperature of oxidation. Compressed air was admitted to the tube at a rate of 0.05 cu ft per min and the temperature was controlled by a variable voltage regulator. The oxi-

Jan 1, 1955

Jan 1, 1955

By R. I. Jaffee, C. M. Craighead, G. A. Lenning

Hydrogen forms a beta-stabilized system with titanium, with a beta eutectoid at about 300°C and 44 atomic pct H2. &apos;The solid solubility of hydrogen in alpha decreases from about 8 to about 0.1 atomic pct from 300°C to room temperature. Hydrogen has little effect on tensile properties, but decreases notch-bar toughness to a large degree. This latter effect appears to be the result of increased notch sensitivity. PRIOR to this investigation, only a small amount of information was available on the effect of hydrogen on the mechanical properties of titanium. The effects of the other interstitially soluble elements, carbon, oxygen, and nitrogen, had received detailed study. Jaffee and Campbell1 indicated that hydrogen up to 1 atomic pct did not affect tensile properties deleteriously. Pitler&apos; indicated that 1 atomic pct H, in titanium reduced the impact strength appreciably, but his alloys contained appreciable amounts of oxygen, and it was difficult to attribute the embrittlement entirely to hydrogen. The high temperature portion of the equilibrium diagram for the Ti-H system was established by McQuillan," and his data generally corresponded with the results of Kirschfeld and Sieverts," Gibb and Kruschwitz," Bevington, Martin, and Mathews," and other investigators. The lower concentration limit of the hydride phase varied considerably among investigators, and Gibb and Kruschwitz9 ad shown that small amounts of contaminants in either titanium or hydrogen caused considerable variation in this lower limit. In view of this pronounced effect of contaminants, the extrapolated value of McQuillan&apos;s, about 48 atomic pct at the 325°C eutectoid, appeared the most reasonable. McQuillan&apos;s lowest experimental value was 54 atomic pct at a temperature of 450 °C. The density of titanium had been shown to decrease with increasing hydrogen content, but discrepancies were noted among the various investigations. The best values indicated that the density was decreased from 4.56 grams per cc at 0.27 atomic pctl to 3.84 grams per cc at 61.3 atomic pct? This investigation was conducted to determine the effects of hydrogen on a titanium, both in high purity and commercially pure metals, and on high purity a titanium alloys. Material and Fabrication The literature indicated that impurities in either the hydrogen or the titanium must be kept to a minimum. For this reason, the initial studies were made with high purity iodide-refined titanium. The vendor&apos;s analysis of the iodide titanium and the hydrogen content of the as-fabricated Y4 in. diameter rods are shown in Table I. Two 1 lb ingots were prepared by arc melting under argon in a water-cooled crucible, using a water,cooled tungsten electrode. This equipment has been described.&apos; As-cast Brine11 hardness numbers of 88 and 58 for these ingots were low enough to insure that the high purity of the metal was maintained during arc melting. The ingots were hot forged to % in. diameter rods at 800°C, cleaned by grit blasting, and then cold swaged to Yz in. diameter rods. The rod was then air annealed at 725 "C, ground to remove scale, and cold swaged to Y4 in. diameter (75 pct reduction in area). The material was then annealed for 1 hr in argon at 800°C to develop an equiaxed a grain size of about 0.05 mm. Micro tensile specimens and microimpact specimens were machined from this rod prior to treatment in the Sieverts-type absorption apparatus. Two lots of commercially pure RC-55 titanium were also used in this investigation to determine the effects of hydrogen and the normal impurities on mechanical properties. The commercially pure RC-55 alloy was obtained in the form of % in. diameter rod. The analysis of this material is also given in Table I. The % in. diameter rods were hot swaged

Jan 1, 1955

By C. K. Ferguson, J. A. Klotz

This paper describes experimental investigations conducted at the California Research Corporation&apos;s model oil well. The first part describes filter loss from several drilling muds through bore hole walls during mud circulation and drill string rotation. The effect of mud properties and drill string rotation with mud circulation is described. Filtration from a bore hole full of drilling mud, not circulating, but under pressure for extended time periods, is also discussed. The second part describes filter loss to permeable formations from beneath a drilling bit where filter cuke has no opportunity to develop appreciable thickness. If potential flow theory is applied to predict filtrate invasion from this hole bottom, targe invasions arc calculated. But model well experimentation shows that filtrate invasion from the hole bottom is controlled by mud particles that penetrate the formation ahead of the bit. This experimentation provides data to estimate the effect of mud particle penetration on fluid loss to formation. The third part presents an estimate of mud filtration during drilling of a well. INTRODUCTION As oil wells are drilled by the rotary method, drilling mud circulates up the annulus between drill pine and well wall. Drillers adjust mud density so that the pressure at the bottom of the mud column is several hundred psi greater than the pressure of reservoir fluid. As a result of this pressure difference, the liquid part of the mud filters into the rock around the bore and mud solids deposit as a filter cake on the well wall. For many reasons the petrogleum industry, within the past 20 years, has spent much money and energy to determine the volume of mud filtrate that enters rock around the well bore and dedicated much research effort to reduce this volume. Among the reasons for attempts to determine the volume of mud filtrate and to reduce this volume are the following: 1. If filtrate damages the permeability of oil sand, the resultant damage to oil well productivity will depend on the distance that the filtrate invades the oil sand; reduction of filtrate volume may, therefore, increase well productivity. 2. Filtrate that penetrates shale sections may cause the shale to swell and to slough into the well bore. Uncontrolled sloughing may stick drill pipe. Reduction in filtrate volume may reduce drilling trouble. 3. Electric log resistivity curves are changed by invasion of a mud filtrate; the change depends on the depth to which filtrate invades. Knowledge of this depth is necessary before resistivity logs can be interpreted accurately. For these reasons, specifications the place an upper limit to drilling mud filter loss are now written into almost all drilling programs. These specifications are based on APT Recommended practice 29, Standard Field Procedure for Testing Drilling Fluids,&apos; which describes a static filtration test operated at 100 psi filtration pressure and at ambient temperature. Although this test is adequate for mud control, it cannot be used to compare filtration properties of different muds. Schremp and Johnson&apos; showed, for example, that mud with a low API filter loss does not necessarily have low filter loss at bottom hole temperature and pressure. Also, no information has been available about the effect of bottom hole mechanics (mild circulation, drill string rotation, and bit action) on mud filtration. This paper discusses filtration data measured in the California Research Corporation&apos;s model oil well, which models closely oil well bottom hole geometry and hydrodynamic conditions. The filtration processes that

Jan 1, 1955

By J. D. Price, W. M. Bertholf

Making maximum possible use of available equipment and material, CF&I placed a high-efficiency, high-capacity washery unit in the existing buildings to gain simplified operation, reduced manpower requirements, raised efficiency, and boosted production. THE central washing plant of the Colorado Fuel & Iron Corp. was first operated in 1918 to furnish coal for two 60-oven batteries of Koppers design. Prior to that time the coke for the blast furnaces had been secured from a number of beehive operations, some with their own washeries. The original washery had four Elmore jigs, which did not do as well as had been expected. In 1923 the jigs were taken out and replaced by Deister Plat-O tables, with various changes in auxiliary equipment. In 1936 the throughput of the plant was considerably increased by the installation of vibrating filters for recovery and drying of fine coal, thereby reducing a large recirculating load of fine coal which passed through the screens of the Carpenter driers. In the late 1940&apos;s it became evident that something would have to be done to keep the washery abreast of progress at Pueblo and other washeries. Coal requirements were nearly two and one-half times the original requirements of the 120 small ovens, as additional ovens had been built in 1930, 1938, and 1945, whereas no additional coal washing capacity had been added since the 1936 modifications. Much of the equipment, moreover, had seen better days. One answer to the problem was to build a new and completely up-to-the-minute plant, with sep- arate sections for coarse, medium fine, fine, and very fine coal. On the other hand, it might be financially more profitable to place a high-efficiency, high-capacity unit in the existing buildings. The washing problem at Pueblo is not unique, but it is approached differently. There are no established specifications for coke ash and sulphur. The plant is operated on the principle that if it is more economical to wash it out than to slag it out, wash it out; otherwise, send it on to the blast furnaces. With coals at the Pueblo plant costing what they do, the benefits of washing at a low gravity are questionable. Hence the primary problem is to eliminate the high-ash components and retain all the low and medium-ash components. Sulphur is no problem at all, averaging 0.6 pct in the coke. Since a good proportion of the free impurity in the coals is as large as the coal or bone or larger, it appeared that it would be safe to go to jig washing and discontinue crushing the coal before washing, as had been the practice with the tables. This would boost the throughput. It might also decrease manpower requirements and washing costs considerably. It was assumed at the start and has been demonstrated in the first year of operation that a jig will do as well on the fines as the tables had been doing. It would not be necessary to discount any gains due to increased efficiency in washing the coarse material because of incapacity to wash the fines. By washing at —2+0 mesh it would be possible to dewater, by screening, a considerable tonnage satisfactorily, for example, at —2 + % or —2 + l/4, and then crush it in a hammer mill. The —?+20 could be dewatered in centrifugal driers and the remain-

Jan 1, 1955