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By R. E. Mussler

As part of an overall goal to develop technology that can maintain an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines is evaluating a method for selectively extracting nickel and cobalt from low-grade domestic laterites. The method involves electrowinning to recover the metals in pure form; therefore, preliminary laboratory-scale electrowinning tests were conducted in both a nondiaphragm and a diaphragm cell to determine the effect of variables on energy efficiency under controlled conditions. Electrolytes were generally reagent-grade sulfate solutions that were prepared to simulate electrolyte that could be obtained by stripping nickel-and cobalt-rich solvent extraction reagents. Limited tests were conducted with electrolyte generated from laterite leach solutions. Electrical energy consumption in a nondiaphragm cell was 2.06 kwhr/lb Ni with the cell operated at 50° C, a cell feed of 90 g/l Ni, a pH of 3.5, an extraction of 3.2 g/l, and a cathode current density of 20 amp/ft2. The energy requirement decreased with increasing concentration and temperature, and increased with increasing. extraction and current density. At 50° C, energy consumption in the nondiaphragm cell was 21 pct greater than in the diaphragm cell, but it was only 5 pet greater at 65° C. For this reason and because of overall cost considerations, operation at 65° C with the nondiaphragm cell was preferred. Smooth sheets of cobalt were obtained by electrowinning in a nondiaphragm cell at selected temperatures from 50° to 85° C and with cobalt concentrations from 55 to 87 g/l. The energy consumption (1.48 kwhr/lb) was 22 pet lower with a cobalt concentration of 75 g/l and a cell temperature of 65° C than with a cobalt concentration of 55 g/l and a cell temperature of 50° C.

Jan 1, 1981

By R. Stratton-Crawley

Flotation-related processes utilizing an oil phase for processing fine mineral particles have been described and various applications discussed. The problems associated with the techniques are varied, but may be summarized by the following areas; (1) applicability to fine particle beneficiation, e.g. collector extender and emulsion flotation. (2) major 'mechanical' problems, e.g. emulsion breakage and oil recovery in oil flotation. (3) complex interfacial chemistry, e.g. empirical nature of pigment flushing .

Jan 1, 1979

By Mei-le He, Min Chen, Xiang Shen, Lei Xu, Lei Liu, Nan Wang, Xue-liang Yin

In the current study, Al2O3-MgO-CaO refractories were prepared at 1400-1600 by the addition of MnO micro-powders, and the effect of MnO addition on densification behavior of the refractory was discussed. The results showed that the doped MnO dissolved to MgAl2O4 phase, and promoted the growth of MgAl2O4 grains by the formation of MgAl2O4 solid solution. As a result, the dense microstructure was obtained, with the apparent porosity decreased from 19.2% to 5.4% and the bulk density increased from 2.78g/cm3 to 3.15g/cm3 after firing at 1600 for 2h by the addition of 4% MnO. In addition, a texture microstructure was observed, which is considered to be favorable to improve mechanical properties and the service life of Al2O3-MgO-CaO system refractories.

Jan 1, 2016

By S. K. Mohanty, T. M. Dittrich, M. J. Allen, M. Dardona, A. C. Strzelecki, J. Hovey, Boukhalfa. H.

Rare earth elements (REEs) have many critical uses in advanced technology and the lack of a reliable domestic supply has been identified by the US DOE as a vulnerability to US economic security. Our research focuses on developing an economical process for extracting REEs from coal fly ash and power plant wastewater sludge by coupling a hydrothermal extraction process with the engineering of a ligand-associated media for concentrating REEs from the extraction liquid. Ash samples have been collected from two Detroit-area Power plants that burn 100% low sulfur coal (Trenton Channel) or fuel blends of 75% low sulfur coal and 25% high sulfur coal or 70% low sulfur coal, 15% high sulfur coal, and 15% petcoek (Monroe Power Plant). Ash samples are then subjected to hydrothermal conditions from 100-350 °C for 1-24 h at Los Alamos National Laboratory and leachate concentrations are measured by inductively coupled plasma-mass spectroscopy (ICP-MS) and compared to hydrofluoric acid digestion results. Experiments designed to aid in ligand selection and loading optimization show that di-(2-ethylhexyl)methanediphosphonic acid (H2DEH or DIPEX™) can be successfully loaded to a commercially available swellable organically modified silica (SOMS) media. Preliminary results show that DIPEX-associated SOMS surface loading can exceed 4x on a mass/mass basis and in simplified sorption experiments with Nd solutions (~pH 2), the DIPEX-SOMS media can sorb >90 mg Nd per g of media. Recovery of the sorbed Nd with low pH solutions has had low efficiency with the high (4 g DIPEX/ g dry media); however, near complete recovery was achieved with lower surface loadings (0.05 g DIPEX/ g dry media). Column experiments are being conducted to evaluate the optimal ligand/media ratio for repeated use. Completive sorption with Fe and other major cations are also being evaluated.

Jan 1, 2019

PolyMet Mining is developing the NorthMet property near Duluth, Minnesota. Laboratory investigations had led to the development of the PLATSOL process to dissolve in one step the base metals (copper and nickel) as well as the gold and PGM’s. To complete the pre-feasibility study, a fully integrated ten-day pilot plant trial was undertaken, comprising of: high temperature (>220ºC) pressure oxidation in the presence of 5-10 g/L chloride (the PLATSOL process), followed by solid/liquid separation, gold plus PGM’s recovery from solution, conventional Cu SX/EW and recycling of the copper raffinate to the autoclave. The concentrate tested was a NorthMet bulk flotation concentrate assaying 14.7% Cu, 3.05% Ni, 0.14% Co, 26.7% S, 1.4 g/t Au, 2.2 g/t Pt and 9.9 g/t Pd. Laboratory results were fully confirmed and with minor adjustments of the laboratory PLATSOL® conditions, the following leach extractions were obtained during the pilot plant trial: Cu 99.6%, Ni 98.9%, Co 96%, Pd 94.6%, Pt 96% and Au 89.4%.

Jan 1, 2001

By Mowat B. A

I lamata is within the Morobe Goldfield (7¦ 25' S, 146¦ 39' E) on the Wau (SB 55-14),1:250,000 scale map sheet (Fig 1). The deposit is 13 km SW of Wau, within the headwaters of the Upper Watut River, at an average elevation of 2000 m. The steep mountainous terrain is covered by dense tropical rainforest and access is by helicopter or by foot track. The deposit has been described previously by Wells and Young (1991) and 1)enwer. Leach and Mowat (1995). Data collected to late 1996 have been used to estimate an Inferred Resource of 9.2 Mt at 3.1 g/t gold using a cutoff of 0.5 g/t. This contains a high grade portion for which an Inferred Resource of 1.2 Mt at 9.7 grt gold has been estimated using a 5.0 g/t cutoff.

Jan 1, 1997

By Kenneth P. V. Lei

The Bureau of Mines investigated a silver-catalyzed oxidative procedure for leaching an arsenical copper sulfide concentrate containing 10 pct As and 32 pct Cu_ Currently, there are no environmentally safe means to treat arsenical copper concentrates in the United States. Leaching was conducted in a 2-L autoclave reactor. The effects of catalyst concentration, O2 pressure, temperature, and H2S04, Cu, As, and Fe concentrations in the leaching solution on extractions of metals from the concentrate were determined. The best leaching conditions for extracting 95 pet eu and As and less than 21 pct Fe were 260 g/L concentrate, 0.007 mol/L (1.0 g/L) AgCI, 3.0 mol/L (294 gIL) H2S04, 1000 C, 60 psig 02, and 6 h. Copper as CuS04-5H20 was recovered by crystallization from the pregnant solution. Arsenic, as AS203, was recovered from the copper mother liquor by solvent extraction, with tributyl phosphate, S02 reduction of As5+ to As3+ in the strip solution, and crystallization of the As3+. The silver catalyst was recovered by contacting the leached residue with a brine solution. A conceptual scheme is proposed for treating arsenical copper sulfide concentrates.

Jan 1, 1987

By Robert G. Ditchburn

The Mariana arc is an ~1,400-km-long intraoceanic arc that marks the southern extension of the Izu-Bonin arc, and is host to 62 ?volcanic centers? of which at least 27 (21 submarine) are hydrothermally, or volcanically active. A surface ship cruise in early 2003 mapped the distribution of hydrothermal plumes emanating from these centers, followed by remotely operated vehicle (ROV) cruises with ROPOS in 2004 and Jason II in 2006. With the exception of one volcano (East Diamante), none of the vent sites visited by the ROVs were host to sulfide mineralization. Rather, they were characterized by high sulfidation mineral assemblages dominated by native sulfur. The sulfur was seen marking the vicinity of vent sites, or as sulfur ?chimneys? (e.g., NW Eifuku and Nikko), or more spectacularly as ?lakes? of molten sulfur, either occupying the summit crater of the volcano (e.g., Nikko), or perched on the flanks of the volcano, near the summit (e.g., Daikoku). Gas (H2S and CO2) was discharging through the molten sulfur. Evidence for these lakes to have either been substantially ?deeper? in their recent past (e.g., Nikko), or existing at other volcanoes (e.g., Seamount ?X?) is given by remnant ?pillars? of native sulfur that are reminiscent of rock pillars in lava lakes found along mid-ocean ridges.

Jan 1, 2008

By Ana E. Bohé, Georgina De Micco, Gastón G. Fouga

"In this work the reaction between several manganese oxides and chlorine is investigated in the range of temperatures between 650 and 950ºC. The reaction path for the chlorination of MnO is established, which involves recrystallization of high valence manganese oxides (Mn3O4 and Mn2O3) followed by its chlorination. For this reason, to understand the reaction of MnO, the chlorination of Mn3O4 and Mn2O3 has also been studied. The starting temperature for the reaction of these oxides is determined by non isothermal thermogravimetric measurements. The effect of temperature is analyzed, under our experimental conditions the rate of reaction is mass transfer controlled. The activation energy for the volatilization of manganese chloride is obtained which is in good agreement with volatilization enthalpy of MnCl2.IntroductionMany oxide ores which have manganese in their composition undergo chlorination processes during the extraction of refractory metals such as Ti, Hf and Nb. Although several works related with chlorination of manganese oxides were reported, there is no information about the kinetics or mechanism of the manganese oxide chlorination reactions. Okahara et al. studied the chlorination of manganese oxides and established that they react easily above 250ºC. Furthermore, they observed that chlorination of high order oxides is more difficult when there is not a reducing agent [1]. Ivashentsev studied the chlorination of manganese oxides using Cl2(g), CO(g) + Cl2(g) and COCl2(g). He established that the reaction of MnO started at 130ºC with formation of MnCl2(s), he also observed recrystallization of manganese sexquioxide [2]. Finally, the chlorination of manganese nodules from the ocean was studied by Murthy and Reddy [3] with the aim of obtaining valuable metals such as Mn, Co, Ni and Cu. They studied the influence of several parameters like temperature, carbon percentage, particle size and chlorine flow rate in the extraction process."

Jan 1, 2008

By W. L. Staker

Alternatives were developed to the conventional ammoniacal carbonate leaching-steam stripping procedure for recovering copper as an oxide from contaminated scrap metal. By entraining air bubbles in the leach solution, the copper dissolution rate was increased to 1.5 g/in2 of copper surface per hour, compared to 0.5 g/in2/hr produced by conventional agitation in stirred tanks. Using entrained nitrogen gas bubbles for agitation in conjunction with powdered sulfur not only resulted in rapid dissolution but also simultaneous precipitation of the copper from solution as a high-grade cuprous sulfide.

Jan 1, 1971

By I. S. Parrish

One of the most common errors uncovered while performing a reserve, or resource, audit is not in the geological modeling or grade problems due to poor sampling, prepartion or assaying. The error most commonly found is in tonnage or, more specifically, in the tonnage factor - that factor applied to volume to derive tonnage. Tonnage factors In the metric system, the tonnage factor is the density, or specific gravity. Specific gravity (Sp.g.) is defined by Dana (1947): • "The specific gravity of a mineral is the ratio of its density to that of water at 4° C (39.2° F). • "Density is the mass of the unit volume or weight of the body divided by the weight of an equal volume of water." When Sp.g. is multiplied by the metric volume it yields metric tonnes. In the English system, the tonnage factor is usually expressed in cubic feet per short ton (cu ft/st). When the volume in cubic feet is divided by cu ft/st, the resulting figure is in English short tons. Table 1 gives the cu ft/st factors equivalent to specific gravities from 1.6 Sp.g. to 5.8 Sp.g. The table is based on the following equation: cu ft/st = 0.9072 divided by Sp.g. times 0.02832 The blase attitude that most geologists have toward tonnage factors is echoed in the prevailing definitions of Reserves and Ore, as provided by the US Securities and Exchange Commission (S.C Form S-18), Canadian National Policy 2A and the SME Proposal for Reporting Terminology (SME February 1991). In each case, it is stated that "quantity" (SEC, SME), or "tonnage" (Can.2A), "is computed from dimensions revealed in...." etc. Unfortunately, "dimensions" do not directly yield tonnage. Dimensions must be factored by density to derive tonnage.

Jan 1, 1993

By Shenghui Guo, Jianbo Lan, Hongying Xia, Jinhui Peng, Lihua Zhang, Libo Zhang

Spent Hawaii nut shell was converted into a high-quality activated carbon via steam physical activation. Analysis of the experiment including activation temperature, activation duration, steam flow rate on the adsorption capability and yield of activated carbon were identified. Response surface methodology showed that the activation temperature was identified as 866 , an activation duration of 36 min and a steam flow rate of 2.5mL/min with the methylene blue adsorption number of 195 mg/g and yield of 77.75%. The key parameters that characterize quality of the activated carbon such as the BET surface area, total pore volume and average pore diameter were estimated to be 1125m2 /g, 0.94mL/g and 5.21 nm, respectively. Additionally, by the SEM analyses of char and activated carbon, the surface of activated carbon has large number of pores of irregular and heterogeneous morphology.

Jan 1, 2016

By D L. Decker, G C. Miller, C Papelis

Arsenic, often associated with precious metals ore deposits, is a major contaminant released during large-scale gold mining. Because of the complex oxidation/reduction and sorption behaviour of As, prediction of the long-term mobility of As in pit lakes is uncertain. The behaviour of As in pit lakes is investigated in this paper by conducting a series of laboratory experiments where As is allowed to adsorb onto pit lakes sediments. Experiments were conducted over a range of pH with both As(III) and As(V) allowed to adsorb onto sediments collected from existing pit lakes found in the three main orebody types in Nevada, USA; porphyry copper, quartz-adularia gold, and Carlin Trend type gold deposits. Results from adsorption experiments show that As(V) and As(III) adsorption is strongly pH dependent with higher uptake at pH 5 and lower uptake at pH 9 for As(V) and higher uptake at pH 9 and lower uptake at pH 5 for As(III). This behaviour, as expected for oxyanions, has been described previously for agricultural soils, iron oxides, and Carlin Trend heap materials. Maximum adsorption of As(V) for the Carlin Trend type gold sediment was 3.0 g/kg at pH 5, 2.0 g/kg for the quartz-adularia sediment, and 0.9 g/kg for the copper porphyry sediment. Maximum adsorption of As(III) for Carlin Trend type gold sediment was 2.5 g/kg at pH 9, 2.2 g/kg for the quartz-adularia sediment, and 2.1 for the copper porphyry sediment. Adsorption isotherms are non-linear and show Freundlich isotherm behaviour. Variations in sorption between the different pit lake sediments under similar conditions can be explained by differences in the elemental composition of the sediment. Most rock forming elements from XRF analysis are similar in quantity except for Fe. The Fe content is highest in the Carlin Trend type gold deposit sediments and lowest in porphyry copper deposit sediments and is the third most abundant element in all three sediments. The Fe content of the sediments correlates well with the amount of As sorption seen in the laboratory experiments.

Jan 1, 2003

By N. A. Gokcen, J. Chipman

Aluminum and oxygen dissolved in liquid iron were brought into equilibrium with pure alumina crucibles and atmospheres of known H2O and H2 contents to study the reactions: 1—Al2O3(s) = 2 Al + 3 0; 2—Al2o3(s) + 3H2(g) = 2Al+ 3H2o(g); and 3—H2(9) +O = H2O(g). Aluminum strongly reduces the activity coefficient of oxygen and similarly oxygen reduces that of aluminum. Values of the product [% All" • [% O]3 are much smaller than those found in previous experimental studies and are of the order of magnitude of the calculated values. ALUMINUM is the strongest deoxidizer commonly A used in steelmaking, but the extent to which it removes dissolved oxygen has been debatable. The relationship between aluminum and oxygen has not been determined reliably not only on account of the usual experimental difficulties at high temperatures but also because of uncertainties in the analyses of very small concentrations of oxygen and aluminum. The earliest experimental attempt of Herty and coworkers' was followed by a more systematic study of Wentrup and Hieber.' These authors added aluminum to liquid iron of high oxygen content in an induction furnace and considered that 10 min was sufficient to remove the deoxidation products from the melt. Parts of the melts thus obtained were poured into a copper mold and analyzed for total aluminum and oxygen (soluble plus insoluble forms), assuming that the insoluble parts were in solution at the temperatures from which samples were taken. It is conceivable that the furnace atmosphere in their experiments, consisting of mainly air at 20 mm Hg pressure, was a serious source of continuous oxidation and therefore that their oxygen concentrations were correspondingly high. Scattering of their data was explained to be well within the maximum inaccuracy of 10°C in the temperature measurements and errors of ±0.002 pct each in the oxygen and total aluminum analyses. Maximum and minimum deoxidation values, i.e., values of the product [% All' . [% O] differed by factors of 10 to 15; mean values of 9x10-11 and 7.5x10-9 ere reported at 1600" and 1700°C, respectively. Hilty and Craftsv determined the solubility of oxygen in liquid iron containing aluminum, using a rotating induction furnace. Pure alumina crucibles used in their experiments contained the liquid iron which in turn acted as a container for slags of varying compositions consisting mainly of Al2O3, Fe2O3, and FeO. The furnace was continuously flushed with argon, and additions of aluminum and Fe2O3 were made in the course of each experimental heat. The inner surfaces of their alumina crucibles were covered with a substance other than pure Al2O3, containing both iron oxide and alumina. Although frequent slag additions can change the composition of slag in the liquid iron cup formed by rotation, the inner surface of the crucible must depend upon the transfer of oxygen or aluminum through the liquid iron for any adjustment in composition. It is not clear that their metal was in equilibrium with the crucible wall, but it is clear that it was not in equilibrium with Al2O3. Their deoxidation product, [% A].]" • [% O]3, varied by a factor of more than 50; the average values of 2.8x10- and 1.0x10-7 were selected for temperatures of 1600" and 1700°C, respectively. Aside from the experimental determinations, attempts have been made to calculate the deoxidation constant for aluminum indirectly from thermody-namic data. Schenck4 combined the thermodynamic data for Al2O3 and dissolved oxygen in liquid iron by assuming an ideal solution. His calculated values are 2.0x10-15 and 3.2x10-13 at 1600" and 1700°C, respectively. Later, Chipman5 attempted to correct for the deviation from ideality and derived an expression which led to deoxidation values of 2.0x10-14 and 1.1x10-12 at 1600" and 1700°C, respectively. The errors in these treatments originate mainly from inaccuracies of thermal data and uncertainties regarding the activity coefficients of dissolved oxygen and aluminum. The purpose of this investigation was to study the equilibria represented in the following reactions in the presence of pure alumina: Al2O3(s) = 2Al + 3O K = aAl2.ao3 [1] Al2O3(s) + 3H2(g) = 2Al + 3H2O(g) H2O K2 = aAl2(H2O/H2 ) [2] H2(g) +O = H2O(g) K3 = 1/ao (H2) [3] The experimental method consisted of melting pure electrolytic iron, usually with an initial charge of aluminum, in pure dense alumina crucibles under a controlled atmosphere of H,O and H2 and holding

Jan 1, 1954

By C. D. Harrison

This paper presents the results of 18 high-G centrifuge tests performed at the Electric Power Research Institute's Coal Cleaning Test Facility in January 1985. These tests, using -28 mesh (0.6mm) froth flotation product, show that the high-G, solid-bowl centrifuge can produce clean-coal moistures of less than 12 percent at solids recovery rates exceeding 98 percent. The high-G centrifuge achieved these low moistures by applying centrifugal forces up to 2,000 times gravity. Because these forces are two to three times the forces used in a screen-bowl centrifuge, the high-G centrifuge can use a solid bowl and still produce a low-moisture product. The solid bowl captures ultrafines that would pass through a screen bowl, and thus obtains higher recovery rates than a screen-bowl centrifuge.

Jan 1, 1985

By Daniel E. Walsh

A pilot scale study was performed to evaluate the potential for gravity concentration of gold from -13 mm (-1/2"), crushed ore from Ester Dome, Alaska. 9.04 tonnes (9.94 tons) of crushed ore were sampled and processed through a Pan-American jig -Wifley table pilot plant. Plant products were sampled for assay and material balance calculations. Gold recovery through one stage of jigging and two stages of tabling was 17.4% at a concentration ratio of 615:1. Concentrate grade was 766.3 g/tonne (22.4 oz/ton). The feed grade to the plant was calculated at 1.71 g/tonne (0.050z/ton). Jig tailings, primary table tailings and secondary table tailings grades were 1.44 g/tonne (0.042), 1.30 g/tonne (0.038), and 5.47 g/tonne (0.16 oz/ton) respectively. Significant, coarse, free milling gold values were shown to remain in the jig tailings. Concentrate mineralogy is discussed.

Jan 1, 1991

By P. D. Rao, D. E. Walsh

A pilot-scale study was performed to evaluate the potential for gravity concentration of gold from -13 mm (-1/2 in.) crushed ore from Ester Dome, AK. 9.04 t (9.94 st) of crushed ore were sampled and processed through a Pan-American jig-Wilfley table pilot plant. Plant products were sampled for assay and material balance calculations. Gold recovery through one stage of jigging and two stages of tabling was 17.4% at a concentration ratio of 615:1. Concentrate grade was 766.3 g/t (22.4 oz/st). The feed grade to the plant was calculated at 1.71 g/t (0.05 oz/st). Jig tailings, primary table tailings and secondary table tailings grades were 1.44 g/t (0.042 oz/st), 1.30 g/t (0.038 oz/st), and 5.47 g/t (0.16 oz/st, respectively. Significant coarse, free-milling gold values were shown to remain in the, jig tailings. Concentrate mineralogy is discussed.

Jan 1, 1992

By Hiwa Salimi, Foley. Stephen R, Loghman Moradi

Common water-miscible organic solvents including DMSO, DMF, methanol, ethanol, acetone and THF in combination with HCl and low concentrations of H2O2 were investigated for dissolution of gold. THF showed the best result demonstrating that gold powder could be completely dissolved in 1.5 hours in 1.0 mol/L HCl and 0.2 mol/L H2O2. No complete gold dissolution was observed for the rest of solvents even after 24 hours. The rate of gold dissolution was measured by dissolving gold wire in THF/HCl/H2O2 mixture. The rate of gold dissolution in optimised condition was 75 g m-2 h-1 at room temperature and significantly increased to 590 g m-2 h-1 by raising the temperature up to 60 oC. Although a THF/HCl/H2O2 mixture showed a slower dissolution rate in comparison with aqua regia, however the applied conditions are considerably milder which is highly promising for gold leaching in an industrial scale.

Jan 1, 2015

By J. P. McGee

As part of a joint U.S. Atomic Energy Commission-Federal Bureau of Mines program for using nuclear energy to supply process heat, a simulated nuclear loop has been constructed to test components. This loop has been operated for more than 1,800 hours at 100 p.s.i.g. Of this period, 23 hours were at 2,500° F. and higher; 540 at 2,000° to 2,500° F.; 840 at 1,500° to 2,000° F.; 200 at 1,000° to 1,500° F.; and 260 below 1,000° F. Leakage at flanges and welds was not a serious problem. A helium-recycle system with gas temperatures of 2,300° to 2,500° F. and a static pressure of 250 p.s.i.g. appears feasible. Difficulties were encountered with the recycle compressor due to thermal distortion of the impeller and shaft. The use of sealed bearings limits compressor operation to the life of the bearings.

Jan 1, 1960

By S. S. Lisnyak, B. D. Lichter

An important question in the study of the "hot corrosion" phenomenon (i.e., accelerated oxidation of Ni-Cr-base and Co-Cr-base "superalloys" in the presence of sulfur) is the condition of formation and physico-chemical properties of different sulfides in the system Ni-Co-Cr-S. seyboltl has observed the presence of ((chromium-rich" sulfides of compositions M3S4, and M2S3 in the scales of superalloys after hot corrosion; however, as he points out, much confusion exists as to the identity of sulfides found on Ni-Cr and Co-Cr alloys. According to the literature,&apos; ternary sulfides, e.g., NiCr2S4, (monoclinic structure) and CoCr2S4 (spinel structure) exist in these systems. Therefore, it is likely that these compounds are found in the scale of alloys undergoing hot corrosion. At present this possibility has not been discussed in the literature. Accordingly, we have begun investigation on the properties of ternary sulfides and their mutual interaction. The magnetic and electrical properties of pure NiCr2S4 and pure CoCr2S2 have been previously determined."-&apos; In the present work we have studied the interaction between these sulfides at high temperatures by means of X-ray diffraction and magnetic susceptibility. The measurements were carried out at room temperature after appropriate thermai treatment of samples at high temperatures. For alloys containing the three elements nickel, chromium, and cobalt this interaction may be of importance in the study of the hot corrosion phenomenon. The compounds NiCr2S4 and CoCr2S4 were prepared from stoichiometric amounts of the elements and CoS in the case of CoCr2S4. Samples were mixed and sealed in evacuated silica tubes, slowly heated to 900&apos; to 100O°C, and held at temperature for a total of 120 hr (NiCr2S4) or 80 hr (CoCr2S4) with intermediate re-grinding~. X-ray diffraction showed a pure spinel structure for CoCr2S4 and a monoclinic structure for NiCr2S4. Samples of mixtures of the two ternary sulfides were prepared with different compositions, see Table I. Samples were heated for a total of 80 hr at 900&apos;C in evacuated silica tubes, with one intermediate regrind-ing. The capsules were slow-cooled to room temperature in the furnace. Samples for X-ray diffraction were prepared by placing powder on a glass slide with vaseline. Dif- fractometer traces were obtained on a G.E. XRD-5 diffractometer using a chromium tube and vanadium filter (40 kv and 31 ma). The size of the spinel unit cell was determined from the eight highest angle peaks (80 deg < 2b < 160 deg). Calculated lattice parameters were plotted vs cos B . ctn 0 and extrapolated to 6 = 90 deg. Measurements of the magnetic susceptibility were carried out at room temperature using the Faraday method in a magnetic field of 3000 G and using a Cahn RG automatic microbalance. The system was calibrated from the well-established susceptibilities of platinum and palladium: (Xpt = 0.968 x 10-6 g-1 and Xpd 7 5.04 x 10~6 g-1). The weight of samples were approximately 0.200 g. X-ray diffraction patterns for unsintered mixtures showed Bragg peaks from both the spinel (CoCr2S4) and monoclinic (NiCr2S4) structures. After sintering no monoclinic peaks were observed in samples containing up to 40 mol pct NiCr2S4. However, the spinel peaks were displaced to higher angles with increasing

Jan 1, 1970