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By Fazakerley VW

The Murrin Murrin deposit is located about 210 km NNE of Kalgoorlie and 50 km E of Leonora in the North Eastern Goldfields region of Western Australia at latitude 28¦ 50'S. longitude 121¦ 54'E on the Laverton (SH 51-2) 1:250 000 map sheet. The tenements are held by Anaconda Nickel NL. Geological investigations between 1994 and 1996 resulted in resource calculations being completed for the ten lateritic nickel cobalt deposits shown in Figure 1. At a 0.8 per cent nickel cut-off the resources at May 1996 for the nine deposits are 116.8 Mt at 1.10 per cent nickel and 0.082 per cent cobalt. The nickel-cobalt mineralisation is contained in a laterite profile developed over Archaean serpentinised peridotites. A bankable feasibility study has been completed and the project is scheduled to be in production by the beginning of 1998.

Jan 1, 1996

Pyrite is one of the principal Au-bearing minerals in refractory gold ores. Significantly high Au concentrations of up to 5200 ppm are present in pyrite. Pyrite hosting high levels of Au is also enriched in As. Pyrite as an unwanted mineral ends up in wastes and constitutes one of the primary sources of As in the mining and metallurgical wastes. Arsenic can be readily released to the environment due to rapid oxidative dissolution of the host pyrite under atmospheric conditions. In order to determine the form and occurrence of arsenic in pyrite, micro-X-ray absorption fine-structure spectroscopy (XAFS) spectra were collected from a range of arsenical pyrite grains having different morphologies and a range of arsenic and gold concentrations. All the pyrite grains are characterised by the dominant edge aligned with As-1 valence state. In pyrite, arsenic atoms substitute for S atoms that are in six-fold coordination about each Fe atom. XAFS data suggest that As atoms occur in clusters within the pyrite structure. In addition to As-1, fine-grained, inclusion-rich and framboidal-type pyrite grains have a second As species at ~11 875 eV corresponding to As5+. This As5+ species in pyrite is highly variable and attributed to the oxidation of arsenic exposed on the surfaces of pyrite.

Jan 1, 2008

By Abhilash, S. Sarkar, T. Venugopalan, P. Meshram

"To explore blast furnace slag as a secondary resource for rare earth elements (REEs), blast furnace slag containing lanthanum (La), cerium (Ce), erbium (Er) and neodymium (Nd) in concentrations of 17, 16, 4 and 44 ppm, respectively, was processed with sulfuric acid while optimizing the parameters of acid concentration, temperature and pulp density. The experiments showed that recovery rates of 92, 36, 35 and 52 percent for La, Ce, Nd and Er, respectively, were achieved at 1 to 5 weight/volume (w/v) percent pulp density using particles smaller than 250 µm and treating with 1 M sulfuric acid for one hour at room temperature. Raising the temperature to 95 °C promoted the dissolutions of Ce and Nd to 89 and 84 percent, respectively, for the same 1 M acid concentration and one-hour duration at 5 w/v percent pulp density. Cyanex 923 was preferred over Cyanex 301 for the purification of REEs from leach liquor. In another route, the leach liquor was subjected to precipitation with 0.5 to 1 M oxalic acid, resulting in a product with 4 to 5 percent concentration of REEs.IntroductionRare earth elements (REEs) are important materials in numerous high-technology applications, but they have high supply risk, giving rise to the study of new sources. The recycling of REEs has been well researched, especially on a small scale, but has not been widely implemented. Less than 1 percent of REEs were recycled in 2011 (Binnemans et al., 2013). REEs occur in a large number of minerals in oxidic compounds, such as oxides, carbonates, phosphates and silicates, and are present as mixtures at 10 to 300 mg/kg concentrations in many rock formations, such as basalts, granites, gneisses, shales and silicate rocks. The most abundant REE in the Earth’s crust is cerium (Ce), at a concentration of 20 to 70 mg/kg, followed by neodymium (Nd) and lanthanum (La), with heavier REEs being less abundant (Binnemans et al., 2013). REEs occur in nature in their oxidized forms in salts and minerals due to their electropositive nature and high affinity for oxygen. The possibility of recovering REEs"

Jan 1, 2017

By John P. Borovsky

A 3-year study was conducted to evaluate the problems and benefits of using vegetation to stabilize tailing from a potential Minnesota copper-nickel milling operation. The project consisted of three separate investigations: a waste characterization study, a greenhouse study and a field study. With few exceptions, the physical and chemical characteristics of the tai ling were found to lie within the range of properties of Minnesota soils. The tailing lacks organic matter; is deficient in nitrogen, phosphorus and potassium; and may contain elevated levels of soluble salts and heavy metals, particularly copper and nickel. Numerous grasses, forbs and woody plants will tolerate the tailing as a rooting medium. Peat incorporation and topsoil dressing provided few benefits to the revegetation process which were not provided by a fertilizer application. With fertilization, grass/legume production in the tailing was comparable to local agricultural yields. Concentration of heavy metals in grasses grown in the tailing were generally below suggested tolerance limits for plants and animal forage. Legumes tended to accumulate higher concentrations of copper and nickel, and metal uptake of most plants was positively correlated with rate of fertilization. Tailing drainage water contained elevated levels of heavy metals, and establishment of vegetation had little effect on the quantity and quality of tailing drainage water. However, topsoil dressing significantly increased drainage water volume when compared to unvegetated control plots. Copper-nickel tailing revegetation recommendations were developed.

Jan 1, 1983

By Albert E. Ketler

Introduction – The introduction of computerized monitoring and control (M/c) equipment into the U.S. coal mining industry may prove to be of truly revolutionary proportions in the 801s.Many of you are aware that the British have developed and have been using such sophisticated M/C equipment for performing production and safety related tasks in their coal mines for nearly a decade. The benefits of M/C systems in the mining industry are usually separated into those which improve productivity, and hence make money for the company, and those which improve safety, and hence cost money. The economic benefits of M/C are startling for the production related functions such as for monitoring and controlling conveyor belts, de-watering pumps, electrical power distribution, and the like. It doesn't take much analysis to show that hundreds and even thousands of tons of coal don't get mined every time a belt shuts down or when power is out due to circuit breakers tripping for any number of reasons. A flood, caused by a malfunctioning pump which goes undetected for lack of feedback monitoring of pumping parameters, can destroy literally millions of dollars worth of mining equipment. The M/C system would be justified or not based on whether or not the productivity benefits balanced the cost within a timespan commensurate with the return on capital philosophy of the company. The safety related benefits are easily underestimated or ignored completely and the purpose of this paper is to under-score some of these benefits, as well as to review the application of M/C to the coal mining industry. The companies involved are Transmitton Ltd of England and Minetics Corp of Pittsburgh, Pennsylvania. Transmitton is probably the most experienced manufacturer of M/C equipment in the world having some 200 installations to its credit. Minetics is the marketing and manufacturing arm for Transmitton in the U.S.A. and is responsible for all aspects of distribution and service. Plans are underway for manufacturing of the Transmitton hardware for U.S. sales to be transplanted into U.S. subcontractors by 1981. Thus our coal mining industry will benefit from British technology, but without the delays and additional costs usually involved in international shipments.

Jan 1, 1981

By Chapman Young, William L. Fourney, Richard D. Dick

During 1981 and 1982, an extensive oil shale fragmentation research program was conducted at the Anvil Points Mine near Rifle, Colorado. The primary goals were to investigate factors involved for adequate fragmentation of oil shale and to evaluate the feasibility of using the modified in situ retort (MIS) method for recovery of oil from oil shale.

Jan 1, 1985

By G. Andrews

This case study details the process that was used for project planning and permitting for the Greens Creek Mine, located near Juneau Alaska, as seen through the eyes of one of the primary environmental consultants. This case shows how a Company could involve the public and the agencies in the early 1980's and develop a project sensitive to concerns expressed with a high level of environmental protection. Comparisons are made to the current environmental permitting situation. Initial baseline studies performed during the exploration phase provided helpful information for more detailed environmental work in 1980-1981 as planning and permitting formally got underway. Since the mine was in a National Monument and abuts up to a designated wilderness, the Monument Manager administered the project for the lead agency, the USDA Forest Service. Planning and permitting progressed smoothly to a Final Environmental Impact Statement (FEIS) in 1983. Metal prices were depressed when the FEIS was completed and the project permitting proceeded slowly. Ownership changed several times in the mid-1980's. New owners re-evaluated the project and suggested five changes that required a supplemental EA prior to development. The project was fully permitted and started construction in 1988. Operation began in 1989. Today the environmental process in southeast Alaska is now much more complex, detailed, expensive, and time consuming than in the early 1980's. Significant issues discussed that may impede development and operation include overlapping agency jurisdictions, personal agendas of agency staff, conflicts between agencies that impede project progress, changing regulations, and a well organized environmental opposition.

Jan 1, 1993

By E. B. Viljoen

I. R. M. Chaston* As a gravity concentration man in the midst of so many eminent flotation experts I feel like Daniel. However, I would respectifully disagree with the opening remarks by Mr Viljoen. First, he suggested that gravity concentration of cassiterite was not effective in sizes below 30 microns. In a paper to the Institution of Mining and Metallurgy in 19621, I gave some figures for gravity concentration of deslimed material both for cassiterite and for wolfram which indicated that careful shaking table concentration of fine deslimed material could give recoveries of 75 to 90 percent in the size ranges above 13 micron. These were figures obtained from normal plant operation. It would be interesting to know if any tests were carried out on gravity concentration of the efficiently deslimed feed to this flotation plant to see what the recovery would be. Secondly, Mr Viljoen suggested that gravity concentration plants were expensive. He gives the cost of a flotation plant at R300 000 to treat a feed of 400 t.p.d. to the desliming section or 160 t.p.d. to the flotation cells. From his operating cost figures it would appear that the flotation cost is approximately R2 to R4 per ton of feed to flotation and the total operating cost about R2 per ton of feed. A table plant to treat this tonnage of deslimed feed would consist of about 30 tables and should cost considerably less to install and very much less to operate than the flotation plant. Third, Mr. Viljoen suggests that the concentrate grade from a gravity concentration operation would be unacceptably low. The paper quoted abovel showed that once a primary fine concentrate had been made, giving a suitably deslimed material, further gravity concentration could give concentrates of over 40 per cent Sn with high recoveries. Tailing from this dressing stage was naturally returned to the feed. To give these high grades, sulphides had been removed by flotation but this necessary flotation step is simple and cheap to operate and could be restricted to the final stage when the quantities involved are small. I would agree that flotation has a part to play in fine tin recovery but this role would only seem to become fully effective at sizes below 10 micron and would seem to require, as Mr. Viljoen has suggested, a mechanism for sizing which is effective down to, say, 1 micron. In the meantime it would be interesting to try tabling the flotation tailing to see if it was possible to recover the plus 20 micron cassiterite which is not recovered well by flotation. One point which has been made during discussion is the suggestion that cassiterite particles have a fully hydrated surface at normal pH. I wonder if this layer could materially affect the overall specific gravity of a very small cassiterite particle and, if so, whether gravity concentration of the very fine cassiterite would be improved if carried out in acid conditions, which would inhibit the formation of this hydrated surface. REFERENCES 1. CHASTON, I. R. M. 'Gravity concentration of fine cassiterite'. Trans. Inst. Min. and Met. Vol. 71, p. 4, 1961 and 1962, and discussion of this paper. Dr. R. P. King Mr Viljoen has drawn attention to the difficulties associated with the presence of very fine particles in the flotation pulp and he has indicated that, on the Union Tin plant, they must sacrifice 30 percent of the cassiterite in the minus 7 /Lm material which they separate and lose. He has also indicated that the rate of flotation of cassiterite remained high at these small sizes. The problem arises because the very small particles stabilize the froth making it impossible to handle. These stable froths cannot be easily broken and therefore cannot be pumped and processed. It seems that further fundamental research work on the properties of stabilized froths is urgently required. We have found another difficulty associated with the presence of very fine particles in phoscorite slurries; these particles can be easily floated but with very poor selectivity. We believe that it is possible that a purely physical mechanism such as entrainment is responsible for the collection of fine particles in the froth. We have also demonstrated that the presence of fine particles in the pulp adversely affects the rate of flotation of the larger particles. For esample, we have found an increase in recovery of + 100 um material from 2 percent to 17 percent in a standard laboratory batch flotation test on phoscorite when the - 37 um was removed from the feed. Such interactions between particles are not universally recognised as an important aspect of the complex flotation mechanism. They should appear in any quantitative formulation of the flotation rate process.

By R. Wiesenthal

A method is developed for improving the low recovery efficiency which results when viscous oils are flooded by water. Viscous oil has been diluted with a lighter liquid miscible in it in any ratio which produces a mixture possessing a reduced viscosity and which is then displaced by water. Light gasoline was used in these tests to reduce the viscosity of the oil in place. Oils possessing viscosities in the range of 1.28 to 324 cp at the test temperature of 30C were displaced from a cylindrical unconsolidated sand core, with a length of 2 m (6.6 ft) and a diameter of 10 cm (3.9 in.) at a flood of 6.27 cc/sq cm/hr. In two test series up to I PV of light gasoline was injected into the core before water flooding. In the first series the recovery of a low-viscosity oil (1.28 cp) increased as the volume of light gasoline was increased. However, only the oil which could not be recovered by water flooding alone could be replaced by the light gasoline. In the other series, the recovery of a more viscous oil (13.5 cp) was not increased even if large quantities of light gasoline were injected. An oil bank built up ahead of the water front so that the flood water met with equivalent saturation conditions, as would be the case in flooding solely with water. However, the recovery of more viscous oils could be increased substantially when the core was first flooded with water, followed by a slug of light gasoline, and then flooded with water again. Furthermore, an oil bank ,built up ahead of the second water front. The formation of this oil bank is particularly favorable for the displacement process; the greater part of the light gasoline injected was pushed out of the core ahead of the oil and recovered. Using a light oil of low viscosity, it was possible to replace only the residual oil that could not be recovered by water flooding by the light gasoline. As the basic study had shown that highly viscous oils could be recovered by flooding first with water, then with light gasoline, followed by a second injection of water, the study was extended by tests made with reservoir fluids and cores taken from the low-gravity oil reservoir of the Wietze field, Germany. A great increase in recovery over flooding with water alone was obtained in these tests. The results may show a way to recover high-viscosity oils by a comparatively simple flooding procedure. INTRODUCTION In fields where oil recovery has not benefited from natural water drive, increased recovery may be obtained by the injection of water into the reservoir, especially in the case of fields which produce high-gravity, low-viscosity oil. There is a rather close relation between the viscosity of the reservoir fluid and the recovery that can be obtained by water flooding. As the viscosity increases the oil recovery decreases proportionately, so that an oil viscosity about 30 times that of water is generally considered to be the upper limit for an economically successful water flood.' This limitation has been recognized theoretically by Buckley and Leverett,' and has been verified by numerous laboratory flooding tests, such as by Croes and Schwarz,V n the viscosity ratio range of oil to water from 1 to 500. The reason for the inferior recovery of viscous oils by water flooding can best be understood by considering the mechanism of flood tests. In such tests water is introduced into one end of a sand-packed tube which is saturated with oil of the viscosity to be tested, and oil is produced from, the other end. Oil, with a viscosity lower than that of water, is pushed ahead of the advancing water with considerable uniformity, and irregularities in the displacement process tend to be eliminated as the oil saturation decreases and the water saturation increases. However, oil recovery is not complete, for the water forms interfaces with the oil and traps residual oil droplets in certain of the pore spaces. These residual oil droplets are distributed rather uniformly through the sand, and they are not susceptible to recovery regardless of the amount of water passed through the test cylinder. In the case of an oil possessing a viscosity greater than that of water, the injected water tends to move irregularly through the sand in the test cylinder. At the place in the sand where initial water movement takes place, resistance to the movement of water is lowered and the water finger so formed will grow perceptibly; it will extend to the outlet end of the test cylinder so that a breakthrough of water takes place long before much of the oil-saturated volume of the sand has come in contact with water. Once the breakthrough of water takes place, the water-oil ratio is gradually approaching the economic limit, even though much of the oil in the test cylinder remains unaffected by water. Disconnected drops of oil are trapped in the portion of the sand that has been invaded by water, just as when an oil of low viscosity is flooded. The poor recovery of the more viscous oils, therefore, is due to the irregularity of water movement through the test cylinder, and the rate of water movement through restricted sections of the oil-saturated sand increases with the more viscous oils. There are three ways whereby the recovery of viscous oils by water flooding can be improved:' (1) adding materials which will increase the vis-

Jan 1, 1965

Jan 1, 1927

By Michael Hoch, Michel Desjardins

The isothermal section of the Mo-Ti-Zr-0 system at 1500°C was investigated using X- ray diffraction and mefallographic techniques. Up to 66.7 at. pct 0, the system contains ten four -phase regions. Isopleths at 10, 30, 45, 55, and 60 at. pct 0 were constructed. THE purpose of this investigation was to determine the general shape of the quaternary equilibrium phase diagram of molybdenum, titanium, zirconium, and oxygen at 1500°C. The system was truncated at 66.7 at. pct o. PREVIOUS INVESTIGATIONS The Ti-Zr-0 system was investigated in this laboratory.' The binary systems of interest have been compiled and discussed by Hansen' and Levin, McMurdie, and Hall.3 Farrar, Stone, and Margolin studied the titanium-rich corner of the Ti-Mo-0 ternary. MATERIALS The titanium powder, 99.6 pct pure, the zirconium dioxide, and the molybdenum powder were supplied by the Fairmont Chemical Co. The zirconium powder,

Jan 1, 1962

By W. L. Jiang

Reverse-flotation technology is often applied in iron ore dressing plant, in order to enhance the quality of iron concentrate from magnetic separation. However, this technology has disadvantages in operating cost, energy consumption, and environmental protection. Developing innovative equipment to process magnetite ore more-effectively is a way to get rid of these disadvantages of reverse flotation and improve the quality of iron concentrate. This paper describes the development of Complex Flashing-Field Magnetic Cleaner, a new kind of equipment based on the principle of combination of separation in magnetic field and separation in gravity field. This innovative equipment possesses a tailor-made magnetic system and has the characteristics of a magnetic field, which can strengthen the formation of magnetic agglomerations and the dispersion of gangue minerals, improving the quality of separation. The automatic control system developed specifically for this equipment can further increase the accuracy of separation and stabilize the process. Test results showed that this equipment is reliable in operation, economically beneficial, and has large potential of application.

Jan 1, 2014

By R. P. Fischer

Traditionally, molybdenum and vanadium have been used chiefly as alloy metals in steel. They impart similar characteristics to most steels, and to some extent one can be substituted for the other. In the United States during the 1950's the production of steel increased about 5 percent, and the reported consumption of both of these alloy metals in steel increased some 40 percent. In Europe during the 1950's the production of steel in¬creased nearly 100 percent. Data on the actual consumption of these alloy metals in European steels are not available, but production and trade records show that the European supplies of molybdenum increased about 150 percent and those of vanadium about 350 percent during the 1950's. If most of the molybdenum supplies in Europe are being added to steel, as seems likely, then the European steel industry has nearly caught up with the United State in the rate of consumption of molybdenum in steel. The vanadium supplies, on the other hand, are puzzling--unless Europe is adding mach more vanadium to steel than is done in the United States, it seems reasonable to assume that other uses are consuming moderately large quantities of this metal or that appreciable amounts of it are being transshipped from Europe. To the extent that a changing volume of supply signifies a changing pattern of use, the increased demand for molybdenum and vanadium in Europe should be of interest to domestic producers and consumers of these metals.

Jan 1, 1964

By M. A. Reyes, L. Yan

Heat and humidity buildup within refuge alternatives (RAs) may expose occupants to physiological hazards such as heat stress. The Mine Safety and Health Administration (MSHA) regulations require RAs in underground coal mines to provide a life-sustaining environment for miners trapped underground when escape is impossible. RAs are required to sustain life for 96 h while maintaining an apparent temperature (AT) below 95 °F (35 °C). The National Institute for Occupational Safety and Health (NIOSH) tested a 10-person tent-type RA, a 23-person tent-type RA, and a 6-person metal-type RA in its underground coal mine facilities to investigate the thermal environment over a 96-h period. The test results showed that mine air and mine strata temperatures surrounding an RA occupied by simulated miners (SMs) increased over the 96-h test period. The test results suggest that RA manufacturers should consider this increase in temperatures when calculating and evaluating RA components during surface and laboratory tests. The findings can equip stakeholders with additional considerations for calculating the interior heat and humidity temperature profiles for occupied RAs not tested in situ

Nov 22, 2019

By J. E. Willson, N. K. Bohidar

An evaluation of internal stress distribution based on photoelastic studies and destructive testing of simulation models shows that pillar failure is a function of the internal stress distribution, and that stability can be changed by altering the internal stress pattern. Induced stresses in three-dimensional epoxy disks subjected to uniaxial forces were evaluated by photoelastic studies. Stress profiles across different sections perpendicular to the loading direction revealed two maxima for each profile. Based on the stress distribution for the entire column, an attempt was made to explain pillar spalling and the hour glass pattern of failure in a mine pillar. For maximum stability and optimum design of mine pillars, it is necessary to consider the external forces, the nature and distribution of induced stresses and the characteristics of the pillar material as determined in the laboratory. This paper summarizes the research done by N. K. Bohidarl and Ben L. seegrniller2 as partial fulfilment of the requirement for Master of Science degree in Mining Engineering, University of Utah. It is an evaluation of a study to determine the stress distribution in short columns in order that regions of high stress concentration in mine pillars may be found and their effect on pillar failure be ascertained. The ratios of the dimensions of the columns studied are representative of those found in mines located in flat-bedded deposits. The weight of the overburden generally constitutes the major external force. This force is calculated by taking into account specific weight and thickness of the cover. Determination of the distribution of this force on pillars may often require a complex analytical study. There have been many investigations of the strength

Jan 1, 1968

By Ward S. D

When using grinding time for a batch grinding operation as a measure of the energy usefully employed for comminution; the assumptions made are often not valid. A kinetic approach, based on a study of the rate constant, or k, value for the material is more acceptable. The Rosin-Rammler distribution equation has been theoretically derived from the general equation for first-order batch grinding. This relationship, incorporating a term for k, was used in a study of the rod milling of a binary mixture of quartz and limestone.The presence and degree of interaction between the components was considered by comparing the size distribution of the mill product with that predicted by assuming the overall distribution equal to the sum ofthe distributions given by the Rosin-Rammler equations for each component weighted according to its volume fraction in the mixture. The interaction was found to be complex and particularly sensitive to particle size.A simple graphical procedure was devised to predict the size distribution of the mill. Product components and this gave a fairly good approximation to experimental data.

Jan 1, 1976

[Consider a square block W in an ore body S2, to be valued from one centre sample w, and one corner sample w2 (Fig. 9.1). The sample set is ws = Iw,;w21. We can estimate the block average µw by the average of the sample values x, and x2: µw = 'z (x, + xz). (9.1) The error made is measured by the estimation variance: o' (ws to W) = 2 - (ws; W) - - (ws;ws) - - (W; W). (9.2) However, we know that the centre sample w, gives more information about the block value than the corner sample w2. In the example studied in § 8.4, where w, and w2 were considered to be points, we found that of (w, to W) was nearly one third smaller than o2E (w2 to W), therefore when estimating W one should give more weight to w, than to w2. In general, when evaluating a block W from a set of n samples ws, where WS = l w;w2; ... wn1, a better estimator of µw can be obtained if we give different weights to the sample values, depending on the size and the positions of the samples. Some desirable properties of such an estimator µw are: ? It should be a linear function of the sample values xi: n µw = bi xi (9.3) =t where bi = weight given to sample x . ? It should be unbiased, i.e. its expected value should be equal to the true block value: E [µw - µw] = 0. (9.4) ? The mean squared error of estimation of µw should be a minimum E [(µw - µw)2] = a minimum. (9.5) The estimator which satisfies these properties is a minimum variance, linear and unbiased estimator, and is known as the kriging estimator. The corresponding error of estimation is the kriging error. This estimator is also known as the BLUE (for Best Linear Unbiased Estimator) estimator. This was named by Matheron in acknowledgement of the early work of Krige's in the optimization of the evaluation of the South African gold mines. The following notations will be used: µK kriging estimator. o2k = o2K (w,, to W) kriging error.]

Jan 1, 1978

By Jonathon M. Hanson, John F. Schatz

A combined theoretical and laboratory test program is described with the purpose of providing a useful model of the multiple radial fracturing process. A non-quantitative conceptual model is developed as the basis for detailed mathematical modeling and test planning. The model includes borehole pressurization, flaw rupture, and gas- driven fracture propagation phases. The laboratory tests are carried out in blocks of scaled rock simulant loaded to a true three-dimension stress state and with miniature propellant/explosive charges in a wellbore as the fracturing energy source. The conceptual model, fracture initiation modeling, and laboratory test setup have been completed and are described. The remaining work is ongoing

Jan 1, 1986

By Robert D. Pehlke, Robert G. Blossey

The solubility of nitrogen in liquid binary and ternary Fe-Ni-Co alloys has been measured by the Sieverts' method between 1550°and 1700°C. Solubility data and standard free energzes and enthalpies of solution for nitrogen in the alloys are presented. Interaction parameters are discussed and presented for binary and ternary alloys. MOST of the studies of nitrogen solubility in liquid metals have been directed toward the dilute alloys of iron. Several of these investigations have included measurements of the nitrogen solubility in Fe-Ni al10s'- and in Fe-Co alloys.435 There has been some work, however, that has extended across the e-i-" and F-CO" binaries. This investigation was undertaken to determine the nitrogen solubility in both binary and ternary alloys of the Fe-Ni-Co system. It was also hoped that the differences between earlier studies might be resolved. EXPERIMENTAL METHOD This investigation was made using a Sieverts' apparatus described previously." The nickel (99.85 pct) and cobalt (99.9 pct) were obtained from Sherritt-Gordon Mines, Ltd., and the iron (99.95 pct) was Fer-rovac-E obtained from Crucible Steel Co. Recrystal-lized alumina crucibles were used throughout the entire investigation with no evidence of crucible-melt reaction. Melt temperatures were measured with an optical pyrometer and the temperature scale calibrated against the melting points of the three pure metals. The emissivity of the melt was assumed to be a linear function of composition for all alloys, as has been shown for Fe-Ni alloys.lZ The emissivity of the pure metals at 1600°C were taken as 0.43 for iron, 0.44 for cobalt, and 0.45 for nickel. Using these emissivities, the trans mis sivity of the system was found to be 0.51 i 0.01. The Sieverts' method was used for this study and followed the procedures outlined previously.l' The individual metals were weighed to give about 100 g of alloy. The alloys were melted in the crucible under a partial pressure of argon. The system was evacuated, and the "hot volume" was measured with argon. To avoid the errors caused by vaporization, the melt was held under vacuum only long enough to ensure that all of the gas in the system had been removed. The influence of any small amount of vaporization on the "hot volume" was shown to be negligible by measuring the "hot volume" after a run. This measurement agreed with that made at the start of the run within the implicit error, 0.2 cc, caused by the limitations in accurately reading the buret. The solubility-pressure relationship was measured in the pure metals and in several alloy compositions throughout the ternary system. These measurements were made by admitting measured amounts of nitrogen to the system, and then determining the equilibrium nitrogen pressure above the melt. This method has the distinct advantage of higher accuracy, particularly at lower pressures, than measurements made by withdrawing gas from the system to reduce the pressure after determining the solubility at 1 atm nitrogen pressure. This latter method has a practical lower limit of about 0.4 atm where an increased error is encountered because the buret must be emptied to permit further measurements at lower pressures. By determining the relation between apparent solubility and pressure, it was possible to make a good estimate of the initial nitrogen content of the metal from the intercept of the solubility curve extrapolated to zero pressure.11 DISCUSSION The solubility data corrected to 1 atm nitrogen pressure are summarized in Table I. The reported solubility has been corrected for the initial nitrogen content of the alloys. The initial nitrogen contents fell between 0.0002 and 0.0010 wt pct, and were lower in the iron and nickel than in the cobalt. Sieverts' law was obeyed in all alloys at pressures up to 1 atm. Examples of this behavior are shown in Fig. 1. The reaction for solution of nitrogen is Taking the standard state as 1 wt pct N in the alloy and the reference state as nitrogen at infinite dilution in the alloy, and noting the adherence to Sieverts' law, K becomes the solubility of nitrogen in the alloy at 1 atm pressure. Thus the solubility data of Table I were used directly to calculate the standard free energy for the solution reaction. These results are also presented in Table I. The enthalpy of solution is also summarized in Table I as calculated from a form of the van't Hoff relation: Iron-Nickel System. The data for the solubility of nitrogen in liquid Fe-Ni binary alloys is presented in Fig. 2 along the with data of aito, Schenck et al.,' and Humbert and 1liott.l' The data for studies of nitrogen solubility in Fe-Ni alloys containing less than 20 pc t i'- are not presented in Fig. 2, although they are in good agreement with the present work. The results of this study are in good agreement with Schenck

Jan 1, 1967