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By John Wallace, Chib Iheagwara

"Refinements in sensor design have produced low-cost rugged elements to act as loop coupled with stable detection hardware for eddy current measurement in difficult environments. This has allowed direct dimension gauging of nonferrous and ferrous products above the curie point for absolute dimensions and electrical conductivities independently. The software was developed for the analysis of electrical conductivity profiles in CZ silicon crystal growth, then refined for monitoring bar properties and tube properties. Since in most metal working operations, speeds at the minimum of a few hundred feet per minute are encountered the design of the gauge was optimized for a rapid measurement. Independently extracting electrical conductivity provides data in some metal systems for determining the temperature of the monitored product.IntroductionThe primary reason for the use of eddy currents in gauging is that in hostile environments of metal working techniques such as laser gauging and ultrasonics are not always robust enough for in process measurements. Our goal is to use the technique of eddy current measurement as a quantitative control element in various hot and cold processing operations. Inspection in the early stages of metal and semiconductor processing is usually too costly to introduce in a well developed process and these tools are usually only employed in process development. Until recently there has been no efficient general analysis to allow real time measurements in the cylindrical and the probe geometry that could separate dimensional changes from material property changes both which effect the eddy current response. The basis for these measurements is that forward electromagnetic problem for conductors can be solved exactly for the test geometry which allows an inverse analysis to be made by relaxing the dimensions and conductivity to values which reproduce the measured response[!]. This transformation is based on analysis developed in Robert Siegfried' s thesis and was explored both by modeling and by physical measurement. This analysis was extended over the last few years to allow a more compact data set to be used to exact physical properties. The main result was that the technique would work on high ·quality physical data on as little as three test frequencies with the penalty being that the analysis is computational intensive. The main result of this work was that a quantitative inverse analysis of eddy current response would allow a general instrument to be used for a variety of measurements rather than being tailored for a specific measurement on a specific material test geometry. The development of these instruments has progressed over the last ten years for monitoring real time solidification, crystal growth[2] and hot seamless tube forming where the use of standards in traditional eddy current is limiting. The specific instrument design was dictated by the requirements of the algorithm for both frequency selection and levels of systematic noise that could be tolerated. Because the data is need for real time information this dictated that the system be a parallel multifrequency eddy current instrument feeding the same sensor. The sensor have to be simple and robust and usually a single loop or several loop of heat resistant wire or tube. This presentation is about using inversion of multifrequency eddy current data in real time to produce dimensional and property data on cylindrical conductors and planar conductors in real time. The object of the measurements is to produce dimensional outputs on measurements of conducting material without having to establish a detailed standard for each material or size tested. The dimensional measurements using eddy currents is complicated by material variations in conductivity due to temperature and composition. Those variations that are not geometric are often not of critical interest and complicate the measurement. The dimensional changes are often of more importance"

Jan 1, 1997

By R. G. Robins

Metal separations based on the selective precipitation of phosphates have a potential application in many hydrometallurgical processes. This paper reviews the literature on the solubility of a number of both divalent and trivalent metal phosphates and presents the result of some additional experimental measurements. The systems examined have been modelled to obtain free energy of formation data for the various species. Computer generated solubility diagrams which are described can be useful in predicting a variety of metal separations.

Jan 1, 1991

The merging of flash smelting with spray converting in one single furnace is proposed as a continuous copper making process. The proposed process is expected to produce blister copper, clean slag and gas with high sulfur dioxide concentration. Some high grade matte is an intermediate product recycled within the proposed furnace, spray-atomized and converted. The thermodynamic equilibria of the simultaneous oxidations which take place during copper smelting and converting are discussed in order to establish the gradient of oxygen potential along the furnace required for smooth operation. The proposed process is a dynamic system designed to reach equilibrium only close to the slag skimming end of the furnace. The process feasibility is based on the predesigned significant difference between the rates of converting reactions in a finely dispersed system and the rates of deconverting reactions between immiscible liquid phases of restricted interface area. The converting of small stationary droplets of matte, in a silica saturated system, was studied in the laboratory for extremely short oxidation times (10 to 120 seconds). These experiments led to some interesting observations on reaction mechanisms and kinetic trends. The droplet size and the matte grade affected very strongly the oxidation rate and the proportion of the different products obtained.

Jan 1, 1976

By J. Dille

Metallic cobalt exist in two allotropic forms : the hexagonal compact a which is stable at low temperature ( ( 420') and the cubic form 0 stable at higher temperature. This latest form is the only one which is ductile. During the electrode position of Co, in moderate acidic conditions, we noticed a code position of both a and B forms. The influence of several parameters on the B/a ratio in the deposit was investigated. High acidity and the presence of Fe increased its ratio; on the opposite, high temperature promote the a phase. No significant influence on the material were noticed. The differentiation of a and B forms of Co is rather difficult and the method of J. Scoyer was improved quite successfully.

Jan 1, 1988

By G. Bjorling

After complete dissolution of chalcopyrite concentrate in sulphuric acid in presence of nitric acid the excess of the latter is expelled by a surplus of concentrate and the last traces of nitrate removed in the mother liquor after crystallization of the copper and iron sulphates. Zinc accumulates in the mother liquor from which it can be removed by solvent extraction of zinc sulphate as a pair of ions. After dissolution of the sulphate crystals in water the neutral solution is oxidized in an autoclave at 140°C where iron sulphate is thermally hydrolyzed; the iron-free solution is taken to copper electrowinning and the cell acid after partial evaporation recirculated with the mother liquor to the leaching circuit. Total recovery of copper is about 96%; other metals like zinc and iron are concentrated in industrially usable products. At a copper price of about 70 c/lb, the method appears to be profitable also in a small unit.

Jan 1, 1976

By L. E. Murr

Preliminary studies of bacterial attachment to MoSp (molybdenite) have indicated a low correlation between dislocation density in the (0001) basal plane and the density of attached microbes. In the present investigation, poly- crystalline thin sections of CuFeSp (chalcopyrite) have been ion-etched or carefully comminuted to electron transparency and observed in the transmission electron microscope. The thinned test sections were then immersed in a culture solution in which bacterial attachment occurred. The attached bacteria were biologically stained in a uranyl acetate solution and the entire thin CuFeSp sections or tiny particles containing thin, electron transparent edges with bacteria attached were observed in the transmission electron microscope, allowing the coincidence of bacteria and their density to be directly observed in relation to lattice dislocations and crystallographic orientations of the exposed surfaces. This technique has the advantage of exposing crystallographic orientations where dislocation lines intersect the free mineral surface, and the emergence sites of dislocations could in principle be directly investigated as a possible preferential attachment site for bacteria. Bacteria morphologies were also extensively observed in the scanning electron microscope. The implications of the results are that although a strong correlation between dislocation density and distribution and bacterial attachment, density, and distribution has not been established, systematic multiplication of dislocation densities in crystalline mineral particles to be leached could enhance leaching rates by increasing the reaction rates as well as the density of attached bacteria at crystalline, metal-rich phases. Techniques for dislocation production in mineral and ore bodies and the particular implications in chalcopyrite leaching are discussed in relation to in-situ leaching where comminution is attained by explosives and the generation of strong shock waves in an ore body. The present study demonstrates the use of microanalytical and microscopic techniques in the investigation of fundamental microstructural phenomena in hydrometallurgical processes.

Jan 1, 1976

By Hang Goo Kim

A mathematical analysis based on equilibrium modeling has been developed to describe the distribution behavior of minor elements such as Pb, Zn, Bi, Sb, and As among gas, slag and recovered copper phases during the reduction of copper oxide in slag cleaning with CO gas. The results show that large fractions of the impurities transferred to slag during smelting or converting are recycled to the recovered copper metal. It is also shown that there is a limit to the recovery of copper from slag because iron oxides are also reduced to form a copper-iron alloy at low oxygen potentials. The effects of various operating parameters such as temperature, the activity of FeO, the initial amounts of the elements in the slag and CO content in process gas, on the behavior of these minor elements are discussed. The predicted results were compared with the results of a pilot plant operation in which pulverized coal was used as a reductant. Consistent trends between the two cases were obtained.

Jan 1, 1992

By B. Yawney

A copper-nickel sulfide concentrate was leached in water at about 2000C under oxygen pressures of about 0.35 MPa. Oxidation of sulfide to sulfate was virtually complete in about 30 minutes, resulting in greater than 95% copper and 98% nickel extractions. Leaching temperature was shown to be the most important factor affecting metal extractions. Measured rates of oxygen consumption were used to develop batch kinetic data. Mini-plant continuous pressure leaching tests agreed with batch leach results. A proposed overall flowsheet is briefly examined.

Jan 1, 1976

By Peter Willbrandt

The flash smelter at NA was commissioned in March 1972 with an initial throughput of 50 tons of dry copper concentrate per hour. As a result of various measures, for example, oxygen enriched process wind, extension of the radiation part of the waste heat boiler, etc., the throughput could be increased to the present 70 tons per hour of dry concentrate. NA's plant is located on the outskirts of the city of Hamburg. The flash smelter's location and the growing awareness of the German population as regards environmental issues necessitate again and again considerable capital expenditure being spent on environmental protection. Thanks to the numerous small and large measures taken to protect the environment the emissions of dust, heavy metals such as arsenic, copper, lead, etc., and as well SO, could be drastically reduced. This paper will be giving an overview on the present state of the flash smelting process and the impact of the increasing environmental awareness at NA.

Jan 1, 1993

By J. L. Sanchez

Using a special double-zone transpiration reactor, the vapor transport chemistry of vanadium pentoxide in the presence of water vapor has been investigated. Three possible volatile hydroxides above V,O,(s) are reported in the literature: VO,(OH),, V,O,(OH),, and VO(OH),. In the present study, it was established that VO(OH), is the principal gaseous hydroxide species formed. The predominant reaction was found to be: { } The vapor pressure of VO(OH), was measured as a function of temperature, water pressure, oxygen pressure and flowrate. The results have been used to determine the Gibbs free energy of the above reaction as a function of temperature: { } The results of the present work were combined with thermodynamic data reported in the literature to obtain expressions for the AGO for the reaction above V,0,(1) and the AGO of formation (units in cal/g-mole).

Jan 1, 1993

By Guo Gongyi

An extraction chromatography by which 99.99 % pure scandium oxide can be prepared from the starting materiel containing about 70% scandium oxide has been developed by taking advantage of some peculiar properties of the complex chemistry and extraction chemistry of scandium. The purification of scandium was performed at room temperature with relatively fast rates in two chromatographic columns. The preliminary separation of scandium from impurities was done by extraction chromatography using tri-butyl phosphate as the stationery phase in the presence of citric acid, and the nearly complete separation in the presence of perchloric acid. The scandium recovery was greater than 90 %.

Jan 1, 1989

By A. P. Paiva

Although the advantages of Solvent Extraction for separation/purification of relatively concentrated solutions are well known in Extractive Metallurgy, its use for the recovery of elements present in low levels only recently has been discussed, with particular attention devoted to precious metals. In this work, the extraction behaviour of Cyanex 471X towards silver, from an acidic chloride medium is reported, the extraction and stripping isotherms and related kinetic features analysed. Results on the selectivity of silver extraction against high contents of iron, copper and lead are discussed. Phosphine sulphide extractants are generally associated with solvation mechanisms: analysis of the extraction pathways along with the possibility of reaching a suitable loading in the organic phase are also presented.

Jan 1, 1993

By I. Gaballah

High and low grade concentrates of tantalum and niobium oxides were obtained by leaching a medium grade tin slag. Chlorination and carbochlorinalion of these concentrates were studied between 200 and 1000 "C. Chlorination or carbochlorination of the low grade concentrate led, at 1000 OC, to the extraction of about 95 % of the tantalum and niobium oxides. However, the tantalum and niobium chlorinated compounds were contaminated by iron and manganese chlorides. Complete extraction of the niobium and tantalum pentoxide was achieved during the carbochlorination of the high grade concentrate at 300 and 500 "C, respectively. While chlorination of this concentrate at 1000 "C, allowed to the volatilization of about 60 and 80 % of Ta205 and Nb205. In both cases, condensates were composed of almost pure tantalum and niobium chlorinated compounds. The results demonstrate the advantages of the lixivialion based on the "pseudo- structure" of the raw tin slag to obtain the high grade concentrate. The conclusions of this work suggest that the carbochlorination of the high grade concentrate is an efficient process for the extraction of refractory elements from tin slag.

Jan 1, 1993

By R. L. Miller

An industrial wastewater, including plating wastes, is treated with sodium sulfide and ferrous sulfate to form a sulfide-oxide precipitate containing chromium and other toxic metals. Hydrocarbons, in the water, coat the sulfide-oxide particles, impeding metal recovery. Froth flotation, without reagent addition, was found to recover 93.9% of the solids from the sludge with simultaneous rejection of 89% of the water. Methyl isobutyl carbinol (MIBC) improved recovery and potassium amyl xanthate improved both recovery and grade. The process design has wastewater feed (without MIBC) to the rougher circuit. The rougher concentrate is conditioned with MIBC and fed to a cleaner circuit to achieve a high grade concentrate. About 95% of the water is recirculated to the waste treatment plant.

Jan 1, 1992

By Brent W. Madsen

The acid-ferric sulfate leaching of low-grade sulfide copper mine waste provides more than 10 percent of the U.S. supply of new copper, but recoveries and leaching rates are very low. In Federal Bureau of Mines research to improve the leaching process, experiments on 5- to 10-ton lots of mine-run ore were more revealing than bench-scale tests on fine ore. This report discusses the results obtained by leaching run-of-mine and minus 6-inch plus 112-inch samples of low-grade chalcocite-bearing mine waste. The samples were leached for 461 days and 61.6 and 37.7 percent of the copper was extracted from the minus 6-inch plus -112-inch and run-of- mine samples, respectively. A mixed kinetics model was applied successfully to the leaching of the sample with the fines removed where bulk solution transport was not rate controlling. The model, when applied to the run-of- mine ore, gave somewhat higher predicted copper extractions than experimentally determined. Subsequently, oxygen was introduced into the run-of- mine ore, leaching continued for an additional 312 days, and an additional 53.0 percent of the copper was extracted. Before the leaching experiment was dismantled and the residue sampled, the ore was treated with sulfur dioxide and its permeability was improved markedly. The results of each of these procedures are interpreted in relation to the attendant condition of the test.

Jan 1, 1976

By R. A. Alock

The character, occurrence and genesis of the three types of nickel deposits, sulfide, laterite and deep-sea nodule are described, highlighting the differences in mineralogy and chemical composition that effect the extractive metallurgy of nickel and associated byproducts. World nickel production and current resources by deposit type and geographic location are also reviewed.

Jan 1, 1988

By A. Van den Steen

In the early fifties Professor Breckpot of the Louvain University in Belgium in collaboration with the Research Laboratory of Metallurgie Hoboken, discovered the possibility to separate nickel from cobalt sulfate solutions by a nickel sulfide depolarized cementation. This reaction, completed later with a zinc precipitation, was developed into purification processes for the Shituru and Luilu Gécamines cobalt plants in Zaíre. Due to increasing demand for higher quality products and the necessity of lowering the production costs, more laboratory and pilot plant investigations concerning the key parameters for the nickel and zinc sulfides precipitation were under- taken. Especially the relative stabilities of cobalt, nickel and zinc sulfides, precipitated with elemental sulfur or sodium hydrosulfide, were examined in relatlon with the pH and with the redox potential. These investigations have led to better plant practice and new development possibilities. The valorisation of the precipitated sulfides has also been considered.

Jan 1, 1988

By R. L. Miller

Oil -bearing metal sulfide sludges produced in treatment of an industrial wastewater, which includes plating wastes, have yielded to treatment by electrooxidation and hydrogen peroxide processes. The oxidation can be controlled to be mild enough to avoid decomposition of the organic phase while oxidizing the sulfides to sulfates. The pH is controlled to near neutral conditions where iron, aluminum and chromium(II1) precipitate as hydrous oxides. Other metals, such as lead and barium, may be present as sulfate precipitates with limited solubility, while metals such as nickel and cadmium would be present as complexed ions in a sulfate solution. The oxidations were found to proceed smoothly, without vigorous reaction; heat liberation was minimal.

Jan 1, 1992

By S. I. Sobol

The results of the study of the mechanism of a cathode process of cobalt electrolysis to explain disagreements in a form of kinetic equations of autoclave reduction of nickel and cobalt have been used.

Jan 1, 1993

By T. Inami

The chlorine leach of the anode slime was studied in order to improve the treatment process at the Niihama Nickel Refinery. The anode slime originates from the nickel matte electrorefining and, contains 3-5% of nickel as sulfides. A comparative study has been conducted on the filter cake resulting from the sulfur filtration of the molten anode slime. The kinetic factors of the chlorine leach such as temperature, grain size were defined. Under the optimized condition, 70-80% of the nickel is recovered from the slime or filter cake. On the basis of these results, the chlorine leach process for the treatment of anode slime has been established. The leaching plant has been installed and successfully operated since 1986.

Jan 1, 1988