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By David J. Kinneberg, Barbara E. Mangion, Arnold M. Savolainen

Analytical laboratories require a qualitative or semi-qualitative method of determining major and minor constituents in "unknown" samples to select optimal analytical techniques. This is exceedingly important in precious metal assay laboratories where the precision and accuracy requirements are exacting (routinely within 0.02%, absolute basis). This paper describes the use of an x-ray fluorescence spectrometer with a specially designed software package to select optimal analytical procedures and specify relevant analytical parameters. A wavelength dispersive XRF spectrometer is capable of quick and accurate analyses of properly prepared samples without extensive standardization. When coupled with a specially designed software package, this preliminary assay system is applicable to a wide variety of sample types including gold and silver bullion, karat gold and karat PGM alloys, high silver and high copper metallic samples as well as particulate samples of ores and sweeps. The system relieves the assayer of tedious calculations for silver inquartation and proofing, minimizes human error and standardizes selections over time. Most importantly, the system allows for independent verification of final assay results.

Jan 1, 1999

By Gong-yi Guo, Yu-li Chen

"A partially-stabilized zirconia powder was prepared by metalorganic precipitation process from technical-grade zirconium oxychloride and the effluent of an acrylic acid plant. The effluent contained low molecular weight carboxylic acids, i. e., acrylic acid and acetic acid. The· developed process is based on the selective precipitation of acrylic acid at suitable pH values by the addition of zirconium oxychloride to the effluent. The resulting precipitate is a precursor that can yield a pure, ultrafine, and partially-stabilized zirconia powder. The evolution of formation of the partially-stabilized zirconia in the present process was investigated using thermal analysis, infrared spectroscopy, and X-ray diffraction technique. Environmental, technological and cost advantages will make the present process feasible for manufacturing advanced zirconia ceramics.IntroductionIn recent years the superior mechanical, thermal, electrical and chemical properties of stabilized zirconia have become the focus of growing scientific and technological interest, and hence resulted in various structural and functional applications. The great potential of the material has given rise to numerous preparation approaches to obtain the material with the excellent properties; nevertheless, an extensive number of programmes are underway worldwide aimed at understanding and improving both the preparation and behavior of stabilized zirconia ultrafine powders. (1 – 8)."

Jan 1, 2000

By Garrett May

We present a periodic technique for measuring the thermal conductivity of thin, disk-shaped samples. In samples of this type, temperature measurements must be made across the sample faces and are therefore subject to large error due to the interface resistance between the temperature sensor and the sample. The technique uses measurements of the amplitude and phase of the periodic temperature across both a reference sample and the unknown material at several different frequencies. Modeling of the heat flow in the sample allows the simultaneous determination of the thermal parameters of the sample as well as the interface resistance. The technique is demonstrated on nanocomposite samples less than 1.0 mm thick.

Jan 1, 2008

By G. G. Richards

The zinc slag fuming process is used to recover zinc from molten iron-calcium silicate slags by treatment with pulverized coal and air. The rate of zinc fuming is controlled by the complex interaction of several kinetic factors including the rate of entrainment of coal in the slag, the extent of the coal-slag reaction and the rate of ferrous oxide oxidation to ferric oxide. This paper briefly outlines the mechanism of fuming and, on this basis, optimization of process parameters is discussed. Modelling analysis and recent industrial trials at Cominco show that coal entrainment in the slag, bath temperature, and bath depth are critical variables affecting process rate and efficiency. The first step in process optimization is to assess coal bypass of the bath. In general, changes which promote operation at a higher temperature, greater coal entrainment in the slag and extended residence time of the coal in the bath increase fuming performance. Coal entrainment is controlled by injection conditions whereas bath temperature is a function of coal combustion and ferrous oxide oxidation. Residence time of the coal is largely a function of bath depth. The implication of model predictions for continuous fuming is shown.

Jan 1, 1994

By Dajian Wang

To obtain the thermodynamic properties of a multicomponent liquid alloy system over the whole range of concentration at an arbitrary temperature, the free volume cell theory has been applied to derive the formula of activity coefficients of liquid solutions based on the infinitely dilute solutions at some temperature. The linear logarithmic relationship between activity coefficients of binary dilute solutions and reciprocal of absolute temperature have been verified, and are in good agreement with the experimental values from the literature. The Monte-Carlo algorithm was used to calculate the nonlinear end value equations of binary systems, then the free volume parameters obtained were correlated with the activity coefficients of liquid binary, ternary, and quaternary systems at an arbitrary temperature. Three dimensional a-X-T diagrams of some binary systems representing the temperature and concentration dependence of activities were plotted. The calculated results regarding non-ferrous alloy systems have been statistically examined with the experimental values from the literature. Hence, this simple approach could be useful for analyzing thermodynamic properties of liquid alloy systems.

Jan 1, 2000

By Michael I. Morris

The U.S. Department of Energy's (DOE's) Transuranic and Mixed Waste Focus Area (TMFA), funded from fiscal year (FY) 1996 though FY 2002, was tasked with finding solutions for the mixed waste treatment problems of the DOE complex. During TMFA's initial technical baseline development process, three of the top four technology deficiencies identified were the need for amalgamation, stabilization, and separation/removal technologies for the treatment of mercury-contaminated mixed waste. The Mercury Working Group (HgWG), a selected group of representatives from DOE sites with significant mercury waste inventories, assisted TMFA in soliciting, identifying, initiating, and managing efforts to address these areas. Solicitations and contract awards were made to the private sector to demonstrate both the amalgamation and stabilization processes using actual mixed wastes. The goal was to develop separation and removal processes that will address DOE's needs. This paper discusses the technology selection process, development activities, and the accomplishments of TMF A through these various activities.

Jan 1, 2003

By Fathi Habashi

During the recovery of copper, nickel, zinc, and lead from their sulfide ores, large amounts of sulfur dioxide are generated. A fraction of this gas is captured and transformed into sulfuric acid and liquid SOl and the remainder is emitted to the atmosphere. Numerous proposals were made to solve this problem. Hydrometallurgy offers the only valid solution by which elemental sulfur instead of sulfur dioxide can be produced. Sulfur can be easily stored, transported long distances, or transformed into S02 and H2S04 when desired.

Jan 1, 1996

By S. q. Honingh, G. Van Weert

Currently produced zinc-enriched blast furnace dust is stored on site at CORUS IJmuiden. To end this practise, a research program was started in 1996. Four technologies were studied: oxidative autoclave leaching in a chloride medium, fluid bed pyrohydrochloridisation (pyrohydrolysis) to yield lead-zinc-free (hematite) calcine, EAF (plasma) smelting/zinc fuming, and incorporation of the dust in 'iron foundry cupola charges. All aim to remove zinc and lead, recycle the iron residue internally, and produce a saleable zinc-lead product.

Jan 1, 2000

By J. Pesl, U. Kemey, F. Sauert

"The CONTOP® smelting cyclone is a water-cooled, upright, high-intensity smelting reactor. The technology for the reactor was initially developed and brought into industrial-scale operation in the area of non-ferrous metallurgy. The two largest smelting cyclones were built with a capacity of 32 tons per hour of copper concentrate mix.The newest industrial CONTOP® plant treats up to five tons per hour of zinc-bearing residues including EAF dust. The highly concentrated zinc-lead oxide produced is sold to the zinc industry. The slag fulfills the leaching criteria and is used in waterway construction. The heat transferred to the cyclone cooling system and the off-gas boiler produces steam from which power is generated in a turbine.V AI has erected a new CONTOP® demonstration plant at MEFOS, Lulea, Sweden. A zinc volatilization rate of 90% was achieved during hot commissioning with Swedish EAF dust.Treatment costs in the range of 85 to 100 EUR per ton were estimated in a feasibility study on the treatment of 73,000 and 57 ,000 tons EAF dust for a group of steelmaking mills in Southern Europe."

Jan 1, 2000

By Y. K. Rao

Relatively pure crystalline lead sulfate (PbSO4) can be produced by chemical vapor transport from an impure source such as the lead-acid battery paste or the roast-ore-leach-residue from a hy¬drometallurgical process-route. In a closed-reactor, transport of matter is induced by a tempera¬ture-gradient and the steady-state transfer rate can be calculated using the data on the standard free energies of formation for the species present and the pertinent binary diffusion coefficients. The present work focusses on chemical vapor transport in a tubular reactor (1.4-cm inner diameter x 10-cm long) with the source- and deposition-ends held at 850°C (T,) and 750°C (Td), respectively; PbC12(g) is the 'solvent' or 'transport agent' and NiSO4(s) placed in the source-zone -serves to maintain a sufficiently high S0,-potential such that the stability of the lead sulfate species is ensured. For the purposes of analysis, the gas-phase in the reactor is assumed to consist of eight species: H2O, PbC12, SO3, SO2. O2 HO, C12, and PbC14. The reaction between C12(g) and PbSO4(s) in the high-temperature source-zone produces PbCl2, SO2, and 02; four more reaction-equilibria in the same zone yield other species. In the low-temperature deposition-zone, reaction equilibrium involving PbC12, H2O, and SO, leads to the nucleation and growth of PbSO4 crystals; three other reaction-equilibria occur in this zone. By employing the virtual equilibrium state for the end-zones and coupling it to the Stefan-Maxwell diffusion equations for each of the gas species, the respective partial pressures for these, in the source- and deposition-zones, are computed at steady-state. From these data, the molar fluxes of PbCl2. PbCl4, and so forth, are determined. Allowing for the transport-enhancing effects of thermal convection, the net transport rate of lead (or PbSO4) is duly calculated for specified initial conditions. The predicted rates show very good agreement with measured rate data reported in the literature [ V. Plies, T. Kohlmann and R. Gruehn: Z. anorg. allg. Chem, 568, 62 (1989)

Jan 1, 1995

By V. V. Satya Prasad, A. Sambasiva Rao

Electroslag melting technologies have recently been developed for recycling light scrap of valuable metals and alloys such as superalloys and oxygen free high conductivity (OFHC) copper at Defence Metallurgical Research Laboratory (DMRL), Hyderabad. Conventionally, electroslag melting processes use consumable electrodes. Because of the difficulty in compaction of scrap into a consumable electrode of satisfactory quality, non-consumable electrodes such as graphite and water-cooled copper have been designed. Electroslag remelting using a water-cooled non-consumable electrode was developed to melt scrap of a nickel base superalloy. Sound ingots with smooth surface finish and properties comparable to vacuum melted superalloys could. be obtained from scrap using this process. A modified electroslag crucible melting process using graphite crucible and graphite electrode was developed for recycling OFHC copper scrap. Copper ingots with less than 10 ppm oxygen and electrical conductivity"" 100% IACS could be produced. The same process was also utilized to produce copper-based alloys such as copper-chromium and copper-titanium starting from copper scrap.

Jan 1, 2000

By Ernt. W. D.

A membrane based mixed extractant process was developed for selective removal of copper from waste acidic cupric chloride etchant solutions found in printed wire board manufacturing. The process uses a mixture of Adogen 381 (tri-isooctylamine), MOC®-45 (ketoxime) and MOC® 55TD (aldoxime) in a kerosene diluent. The mixed extractants recover the copper from a hydrochloric acid medium and transfers it to a sulfuric acid medium. The process also utilizes unique wetted membranes to separate the aqueous and organic phases. The driving force for these membranes is not pressure but the difference in surface tension between the two phases. By using these membranes, complete phase separation results. There is no physical entrainment contamination as found in conventional systems. The only cross contamination is the solubility concentration of one phase in the other. This however is less than 10 mg/l.

Jan 1, 1998

By Yimin Ruan

"An inverse design method is developed to obtain the optimal cooling conditions for the continuous quenching of precipitation hardenable sheet alloys to achieve the required yield strength. The yield strength of a precipitation hardenable alloy is obtained by allowing solute to enter into solid solution at a proper temperature and rapidly cooling the alloy to retain the solute in the solid solution. An aging process may be needed for the alloy to develop the final mechanical properties.The objective of the design is to optimize the quenching process so that the required yield strength can be achieved. With the inverse design method, the required yield strength is specified and the sheet thermal profile at the exit of the quenching chamber can also be specified. The conjugate gradient method is used to optimize the cooling boundary condition during quenching. The adjoint system is developed to compute the gradient of the objective functional. An aluminum sheet quenching problem is presented to demonstrate feasibility of the inverse design method.IntroductionQuenching is a critical step in metal production to achieve desired material properties, such as yield strength, hardness, etc., for precipitation hardenable alloys. In most cases, rapid quenching from the solution heat treatment temperature is necessary to obtain the required material properties, but rapid quenching may cause other problems such as excessive distortions of the quenched materials.In a solution heat treatment, the alloy is heated to a suitable temperature, held at that temperature to allow the soluble alloying elements to enter into the solid solution, and cooled rapidly (quenching) to retain the alloy elements in the solid solution. An aging process, which controls precipitation of fine particles at room (natural aging) or elevated temperatures (artificial aging), is generally followed after the quenching process to develop the final mechanical properties of the heat treated alloys."

Jan 1, 1998

By Adam Powell

A Cahn-Hilliard phase field model is formulated to describe transport-limited electrochemical reactions coupled with fluid flow in a metal reduction cell. When the reaction is limited by mass transfer of metal ions from the electrolyte to the cathode, the metal-electrolyte interface at the cathode exhibits a Mullins-Sekerka instability, leading to the growth of dendrite-like "streamers" of liquid metal into the electrolyte, which in turn significantly enhance the apparent mass transfer coefficient there. Model results for iron reduction from ferrous oxide in slag show formation of these streamers. Although the double-layer is not included in this model, the related phenomenon of electrocapillarity can be represented by a gradient penalty term which includes the electric potential gradient, such that interfacial energy is a function of the electric field normal to the interface.

Jan 1, 2003

By Harald Laux, Stein Tore Johansen

The plunging jet in tapping of steel from converters or electric arc furnaces entrains gas into the steel bath contained in a ladle. Gas entrainment rate and the effect of the gas on the flow pattern in the ladle are studied by means of Computational Fluid Dynamics CFD. The work focuses on the mathematical modeling. Two numerical methods, one for free-surface flows and one for dispersed multiphase flow are combined. A transport equation for the average bubble diameter that incorporates the effect of coalescence and breakup is presented. Results from computations for one ladle and tapping configuration are shown. Our findings indicate that the gas entrainment rate is affected by the material properties of the liquid in the sense that the material properties determine the shape of the jet. Moreover, bubble sizes in the range of two-orders of magnitude are predicted in the ladle. The dispersed diameter model seems to work well. It showed the expected response to material parameters and the turbulent field. However, the presented analysis is just a first step that was limited due to certain simplifications. In order to obtain better insight in the tapping process improvements of the analysis seem necessary.

Jan 1, 1999

By F. Shahbazian

attempt to systematize the knowledge on slag viscosities, the present work was carried out. The Among the physical properties of slags, viscosity is very important in understanding the mass out in the temperature range 1438-1762 Q The rotating cylinder method was used in the viscosity measurements. Crucibles and spindles made out of pure iron were employed. The transfer phenomena in metallurgical processes. The viscosities of fayalitic slags are of great interest in the non-ferrous metal industry, with special reference to copper production. In an slags were prefused before the measurements. In order to take into account the vaporization reactions involving CaF2, pre- and post measurement samples of the slags were chemically analysed and the compositions were ascertained. The results show that in the case of the CaO-SiO2 system, CaF2 additions tend to decrease the viscosity, in accordance with the expectations. In the case of the "FeO"-SiO2 system, at higher "FeO" / SiO2 ratios in the slags, a reverse trend was observed. The results are discussed on the basis of a viscosity model for silicate melts developed in the present laboratory as well as the structural considerations of silicates.

Jan 1, 2000

By P. Blazy

A hydrometallurgical procedure for the recovery of metal from ore, particularly of copper from sulphide materials is described. In the course of this procedure, the raw material is first of all submitted to the action of an appropriate reducing system and then treated with a ferric salt solution which brings about the selective solubilisation of the elements to be recovered with respect to those constituting the pyritic phase. This procedure is investigated using two ore samples proceeding from massive sulphide deposits, presenting different chemical and mine- ralogical characteristics. The results of this investigation are compared with those obtained by a classical process employing a ferric salt solution. It appears that one solubilisation of copper takes place under particularly advantageous conditions when our procedure is used. The principal parameters affecting leaching of zinc, lead and copper are examined. The selectivity of this treatment is evaluated by following the change during the treatment in the pyritic phase.

Jan 1, 1976

By Kenneth P. Michalek, James E. Kelly, Jonathan A. Dantzig

"Many investigations have been reported regarding the simulation of continuous casting with emphasis on in-mold heat transfer. These analyses have been limited, however, because they require either estimation or measurement of the characteristic heat transfer between the ingot and the mold. In this paper, a self-consistent model 'is presented for calculating the heat transfer between a solidifying continuous casting and the mold, in the context of the continuous casting of steel. Using both thermal and stress analyses, the air gap formed during continuous casting is calculated and used to compute the heat transfer coefficients. Iteration between the thermal and stress analyses is used to determine a self-consistent solution. IntroductionThe continuous casting process for steel is illustrated schematically in Fig. 1. Molten steel is tapped into a tundish from which it flows at a controlled rate into the continuous casting mold. The initial shell of the casting forms in the mold by transfer of heat from the metal through the mold wall to the cooling water. The remainder of the casting is solidified by application of water sprays, and/or radiation cooling below the mold.Heat transfer in the mold portion of the process is important because it controls the formation of various defects which are deleterious to subsequent processing. Examples of defects formed in this region are surface irregularities, such as cold folding and oscillation marks, and more serious defects, such as longitudinal or transverse cracks. A more catastrophic problem which may occur is a breakout, in which the shell ruptures and molten steel is discharged in an uncontrolled way."

Jan 1, 1986

By G. A. Irons, D. Colbert

Several electric arc furnace (EAF) shops have increased the zinc and lead grades of EAF dust by reinjecting it into their furnaces; however, the kinetics of this operation are poorly understood. To understand the kinetics, EAF dust was injected into 70 kg heats of iron or steel in an induction furnace. Supplemental additions of carbon and oxygen to overcome the heat load on the system were also investigated. In all cases, the dust was chemically transformed, and the zinc content increased from 16% Zn to 60 - 80% Zn. About 50% of the zinc in the EAF dust dissolved in the iron or steel. The zinc oxide in the dust is thought to be reduced by carbon and the zinc vapour subsequently dissolved in the iron. A kinetic model for the dissolution process is proposed, and the implications for EAF dust recycling are discussed.

Jan 1, 2000

By Dieter Wanner

Off-gas cleaning from metallurgical? plants, requires in many cases very low dust contents which are, difficult to achieve with conventional scrubbers, even with high energy input. Lurgi has developed a scrubber which improves the separation of the fine dust by electrical charge prior to the scrubbing zone,, An Electrostatic Scrubber has been successfully installed for the off-gas cleaning from slag granulation after a waelz kiln achieving less than l mg/m3 in the clean gas.

Jan 1, 1992