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By Eiichi Kuzuno, Atsushi Shibayama, Toyohisa Fujita, Kazuo Koike, Toshio Miyazaki, Hitoshi Masuda

"A solid sulfur is more useful to recover and store than a sulfuric acid as a by-product in the zinc hydrometallurgy. In this experiment a zin concentrate (sphalerite) was leached with ferric sulfate at about 373 K for 3 to 6 hours. Zinc was leached more than 95%. After a solid-liquid separation, the leached residue contained solid sulfur was obtained. The particles in the residue were dispersed by lignin and the solid sulfur of approximately 85% was recovered as float product by a flotation with frother in the pH 4. The dried float product was heated at 413K for 2 hours. The pure solid sulfur was recovered. On the other hand in the leached liquid a zinc oxide was ·added and ferrous .iron was oxidized to ferric iron by blowing oxygen. This ferric iron was returned to the zinc leached process after solid-liquid separation.IntroductionZinc concentrate is usually roasted as pretreatment in zinc hydrometallurgy and the produced S02 is changed to sulfuric acid. However, recently in Japan the utilization of sulfuric acid has been limited and it is more costly to store. Instead of producing sulfutic acid the solid sulfur recovery has been examined by direct leaching of zinc_ concentrate in this experiment.In the direct leaching, several kinds of effects have been studied for leaching of sphalerite in ferric sulfate solution. The addition of lignine siilfonate1 • 2) and fine· grinding3) increases the · speed arid leaching fraction of sphalerite. The leaching ratio depends on impurities in sphalerite ores4 • 5). Here, the zinc concentrate is leached ferric sulfate solution under atmospheric pressure at 373K. The solid sulfur in leached residue is separated as float products from other solids by sink-float separation and flotation. The sulfur in float products is purified by evaporation at 413K and recovered."

Jan 1, 2000

By R. H. Hanewald

The INMETCO process has been modified so as to recover nickel. chromium and Iron from a wide variety of metal containing waste-streams. This now includes the recovery of metals from spent acid solutions such as chromic acid etching I1quids. nJcke1 and chromium plating solutions; stainless and superalloy pickling solutions. etc. In addition. hazardous electric furnace stainless steel and. superalloy baghouse bags can be processed so as to recover the valuable metall1cs. A detailed review of the above new recovery techniques w1ll be discussed as well as the current operating methods used at INMETCO.

Jan 1, 1992

By Mei Yang, Wei Gao, Jian Yang, Qingcai Liu, Wenchang Xi

"TiO2 has been loaded on cordierite porous ceramic to prepare the SCR catalyst carrier by using both APCVD and sol-gel technology. In APCVD method, TiC14 and O 2 were used as reaction precursor. TiC14 was gasified by using N2 as carrier gas which was controlled to 500sccm. Its reaction temperature and reaction time were limited to 773K and 30min respectively. The physical properties, SEM and SEM-EDX of the TiO2-cordierite carrier and the properties of SCR catalysts prepared by these carriers have been tested. The tests showed that TiO2 loaded by APCVD method were of graininess shape and even accumulation. The loading rate of TiO2 and the specific area of carrier sample were increased 114% and 21 % respectively comparing with sol-gel technology. In the result of sol-gel method, the maximal difference of Ti content was 66.92%, while the result of APCVD method was 18.89%. It demonstrated that TiO2 was uniformly attached with the cordierite ceramic by using APCVD method, which would ensure more active ingredients well loaded on the Ti02-cordierite carrier. This difference made the denitrification ratio of catalyst prepared by APCVD method was 8.1 % higher than that of catalyst prepared by sol-gel method.IntroductionIn recent years, the emission of NOx, which were caused by coal-fired power plants, has gotten more and more attention. SCR (selective catalytic reduction) is the most effective technology to DeNOx [ll. The core technology of it is the catalyst. The SCR catalyst usually uses Ti02 as the carrier, and V2O 5 as the active component [2, 3] . However, the thermal stability and mechanical properties of TiO2 carrier are unstable, which would influence the performances of the catalyst. The commercial catalyst generally uses WO3 or MoO3 to promote its heat stability at present [4-7] Besides, TiO2 is expensive. Compared with TiO2, the cordierite is of good thermal stability and lower price. So loading Ti02 on cordierite porous ceramic as carrier to produce SCR catalyst is of good prospects [S, 91 • Currently, TiO2 is usually loaded on cordierite by the sol-gel method. But some research has shown that the sol-gel method easily reduced the loading performances of TiO2, such as distribution, combination, etc. APCVD (atmospheric pressure chemical vapor deposition) has many advantages to preparing TiO2 films, such as high bonding strength, fast reaction rate and so on [l0-13l_ In this paper, TiO2 has been loaded on cordierite porous ceramic to prepare the SCR catalyst carrier by using both APCVD and sol-gel methods. The properties of the carriers prepared by the two processes have also been compared."

Jan 1, 2011

By A. Rawat

The removal of oxyanions of arsenic present in mine process water and drinking water to a regulatory level is a challenging problem. Recently a patented adsorbent lanthanum oxide has been developed which has shown strong specificity for the anions of arsenic. In this paper the kinetic and thermodynamic aspects of arsenic adsorption on to lanthanum oxide are discussed. Adsorption tests were performed at different temperatures using synthetic solutions of arsenic of varying concentrations. From the kinetic data and adsorption isotherms thermodynamic properties such as Gibb's free energy, standard enthalpy of adsorption, standard entropy, isosteric heat of adsorption and activation energy were determined. The results showed that temperature had a positive effect on the rate and degree of adsorption:The activation energy decreased with increase in the initial concentration thus indicating solute-solute interactions in the system. Also, the isosteric heat was found to decrease with increase in the adsorption density implying a heterogeneous adsorbent surface.

Jan 1, 1998

By Yongqi Sun, Zuotai Zhang

Hot slags, at the temperatures of 1450-1650 oC, carry a substantial amount of high quality thermal energy, which represents the largest undeveloped energy source in the steel industry. However, the waste heat recovery rate in China is less than 2%; thus there is a great potential of waste heat recovery. In this study, we investigated a chemical method to extract the waste heat from high temperature blast furnace slags, i.e., sludge gasification. Sewage sludge, another substantial waste produced in the municipal system, need to be timely disposed, the organics of which could be gasified using the waste heat in the slags for the purpose of syngas production. Both the kinetics and thermodynamics of the sludge gasification process were clarified here. Most importantly, an integrated system composed of multiple systems such as the steel industry, the cement industry, the municipal system and the chemical engineering industry, was analyzed in this study.

Jan 1, 2016

By Luciano E. Ramírez, Jesús L. Valenzuela, José R. Parga

"An innovative process for removing copper cyanide complexes including silver and zinc from cyanidation circuits has been developed. The technology was based on the inducing the nucleated precipitation of copper and silver in a tube serpentine reactor, using sodium sulfide as the precipitate and sulfuric acid as pH control. The results showed that pH had a great effect on copper cyanide removal efficiency and the optimum pH was about 3 to 3.5. At this pH value copper cyanide removal efficiency could be achieved above 97 and 99 % ,when influent copper concentration ions were 650 and 900 ppm respectively. In this process (sulphidizaton-acidification-recycle-thickening), the cyanide associated with the copper cyanide complexes is released as HCN gas under weakly acidic conditions, allowing it to be recycled back to the cyanidation process as free cyanide. This system was successfully commercial applied at Minera William in Mexico.IntroductionThe recovery of gold and silver from minerals and concentrates with cyanide is an important hydrometallurgical process, which has been studied for more than 124 years. Patented by MacArthur in 1888 [1], the process relies on the fact that gold dissolves in aerated cyanide solutions to produce the gold cyanide complex. The stoichiometry by wich this reaction occurs is known as the Elsner equation as shown here. Silver is accomplished in the same fashion."

Jan 1, 2012

By Lei Wang, Jianjun Wang, Lingen Luo, Zhengbang Li

Dearsenication in molten steel was studied by adding Ca-Fe Alloy-based arsenic removal agent. In order to improve the utilization rate of Calcium Iron Alloy and improve arsenic removal ratio, [O] is less than 0.0005% and [S] is less than 0.0035%, Al is added into the molten steel. In the processes of adding CaO-Al2O3 based alkalinity slag for arsenic removing in molten steel (initial arsenic content is 0.0080%), arsenic removal ratio reaches 50% when Ca-Fe Alloy addition amount is 18%. During the arsenic removal experiment, adding Rare Earth promotes the arsenic removal reaction and makes the arsenic removal more effectively.

Jan 1, 2015

By Jian Li, P. Liu, R. Zhang and J. Lo

In the past decades, focused ion beam (FIB) has evolved into a powerful microscope that provides capabilities that no other microscopes can offer. The combination of high-resolution imaging and stress-free ion beam cross sectioning provides valuable microstructure information both at the specimen surface and beneath. FIB techniques are also the preferred method to prepare site-specific transmission electron microscope (TEM) specimens. CanmetMATERIALS owns a world-class microscopy facility, where advanced microscopy work provides strong supports to research programs that cover a wide range of subject areas. This paper is aimed to provide a few practical examples of FIB applications in microstructure characterizations that include cross-sectioning and imaging, serial sectioning, and advanced TEM specimen preparation in materials research at CanmetMATERIALS.

Jan 1, 2015

By Takashi Miyamoto, Hideo Nakae, Hideki Yamaura, Takeshi Yanagihara

"For the production of partially composed metal matrix composites, namely discontinuous MMCs, using a casting· process, the interpenetrated phase composites with SiC particles were fabricated by pressureless iDfiltration using molten Al-Si alloys. This process is based on a wetting phenomenon, therefore, we discussed the technique based on the reactive wetting. The SiC particles coated by diluted water glass were sintered in a mullite Tammann tube and simultaneously infiltrated with molten Al-Si alloys in air at 1173~1573K. As for the improvement of the wettability between the SiC and the liquid aluminum alloy, Fe3O 4 powder was mixed with the water glass due to the thermit reaction between Fe3O4 and molten aluminum alloy. In some experiments, pure aluminum powder was placed on the sintered SiC to increase the interfacial area and the chemical reaction between the sintered Sic. and the melt. By combining these conditions, we succeeded in the complete infiltration without pressure at 1173K.IntroductionAs is well known, the mechanical properties of metal matrix composites (abbreviated MMCs) are superior than that of ordinary metals. However, their use has not been widely accepted because the production cost is very high due to their poor machinability. Therefore, the production of partially composed, namely discontinuous MMCs, by as the Lanxide process [l,2] has been investigated for many years. The Lanxide process, it takes a long time, sometimes up to 10h, in a nitrogen atmosphere for the infiltration. Therefore, the cost will be higher for common use. On the other hand, a high 'pressure process has been adopted for the production of discontinuous MMCs by the Toyota Motor Corp.[3]."

Jan 1, 2000

By Guolin Zheng, Jian Pan, Deqing Zhu, Xianlin Zhou

"In ferronickel production, nickel oxide and part of the iron oxide are reduced to metal by agglomeration and smelting in blast furnace. Due to the physical and chemical properties of the laterite ores, a large fraction of fines is generated during the pre-treatment stages and the strength of agglomeration is weakened, which results in low productivity and bad quality. In this paper, the process of pelletization of nickel laterite was developed, and some parameters to strengthen the pelletization of nickel laterite have been optimized. The results show that the compressive strength of fired nickel laterite pellet can reach over 2000 Newton per pellet while firing at the temperature of 1220 °C~1250 °C in 12 min. The product pellet can be used as high-quality burden for blast furnace to manufacture ferronickel.IntroductionIn recent years, the global stainless steel market was developed exuberantly, which greatly promoted the needs of the basic raw material of stainless steel smelting - metal nickel. Currently nickel sulfide ores are only 40% of global nickel reserves, but offer 60% of all the nickel production. However, with the deficit of resources, the nickel sulfide ore (high grade ore) is depleting, so there is an increasing focus on the utilization of low-grade nickel laterite. Recent research has focused on the wet treatment process to utilize nickel laterite, and less on the use of other technologies [1-8]. The economical and efficient technology relies on the reduction of nickel oxide and part of the iron oxide metal by agglomeration and smelting in blast furnace in China. Some domestic steel companies have adopted this process [9, 10]. Unfortunately a large fraction of fines is generated during the pre-treatment stages and the strength of agglomeration is weakened, which results in low productivity and bad quality of fired pellets. In this study, the process of pelletization of nickel laterite was developed firstly, and some parameters to strengthen the pelletization of nickel laterite have been optimized, and the product pellet can be used to produce stainless steel and ferronickel alloy by blast furnace."

Jan 1, 2011

By A. Martins, L. Goulart, E. Araujo, R. Batista, A. Costa e Silva

Steel cleanness is of great importance to the performance of almost all steel products. From very clean steel for bearings to long products used in civil construction, processing variables – in special those in steelmaking operations- must be properly balanced to achieve adequate cleanness for the desired performance. With the present complexity of steels as alloy systems, it is not efficient nor appropriate to develop these processes on empirical basis alone. Computational thermodynamics can greatly improve process development to achieve the desired cleanness level at reasonable costs. In this work, examples of these calculations and their applications to real steel processing are presented and discussed. The advantages, limitations and areas in which improvement in these calculations is desired are highlighted and discussed.

Jan 1, 2015

By Makoto Suzuki

After hot rolling, stainless steel strip is processed by the Hot Rolled Annealing and Pickling line (HAP) , where H2SO4 or mixed acid of HNO3 and HF is normally used. In the pickling bath, metal oxide accumulates in the form of sludge, which should be removed from the bath regularly. A new automatic continuous sludge disposal system has been introduced at Chiba Works of Kawasaki Steel Corporation to increase sludge removal efficiency and improve the working environment. The elements of the equipment are as follows. a. Ejectors in pickling bath: to carry the mixed acid into the circulation tank through the piping system. b. Sedimentation bath : to sediment sludge out of the bath. c. Skip conveyer : to convey a specified volume of sludge into a kneading for device for neutralizing. The sludge removal efficiency of this system is very high. and the volume of sludge accumulation in the pickling bath has substantially decreased.

Jan 1, 1996

By Zhen Zhang, Jiang Diao, Xuan Liu, Tao Zhang, Bing Xie, Hong-Yi Li

Extracting vanadium from vanadium containing hot metal by LD process has been proven an effective solution for the utilization of vanadium-titanium magnetite ore, but the systematic analyses of vanadium extraction rate and mechanism by basic slag are seldom reported. In this study, mathematical model of vanadium transfer from metal to slag was formulated and the rates of vanadium extraction of hot metal with basic slag were investigated. The results indicated that the apparent vanadium extraction rate constant, kp, were in the range of 1.33~9.07×10-4g/(cm3·s). And the rate constant was increased with the increase of final slag basicity, reaction temperature and stirring gas flow. The apparent of mass transfer parameter decreases significantly from 0.13 cm3/ s to 0 cm3/ s in 20min, and the data changed as negative due to the decrease of slag oxidation and recovery of vanadium from slag to metal.

Jan 1, 2015

By Eiki Ono, Atsushi Yamatodani, Shigeru Sunagawa, Yasushi Takasaki, Atsushi Shibayama, Yasunori Higuchi

"During metallurgical processing of non-ferrous metals, smelting residue (inc. smelter slag, flue gas and so on) is inevitably generated as secondary product.In this research, some experimental feasibilities were investigated to recover/remove Cu and As from the residue. Primarily, the removal of As and volatilized materials from the residue was examined by pyrometallurgical treatment (dry-process). In the second stage after treating the residue with a dry-process, leaching and solvent extraction as hydrometallurgical treatments (wet-process) were also investigated by using H2SO4 solution as a two stage leaching treatment, to dissolve various metals from the leach residue. Then, solvent extraction was examined by using LIX-84I as an extractant to recover and separate Cu from impurities from the final (2nd) leached solution. For the leaching stages, the removal of 90 % As and the leaching rate of 85 % Cu could be achieved by 0.25 mol/l and 1.0 mol/l H2SO4 solution, respectively. On the other hand, the extraction of over 90 % Cu and stripping was carried out by solvent extraction. 1. IntroductionIn metallurgical process for non-ferrous metals, smelting residue (inc. smelter slag, flue gas and so on) is inevitably generated as secondary product, i.e., flue dust, slug and so on. The smelting residue includes some useful metals and undesired toxic materials; Cu, Pb, Ca and As, etc.In Japan there is one undisclosed place stockpiled with 10,000 ton of smelting residue from abandoned smelters about 25 years ago. Therefore it is necessary to reduce the residual amount for space and environmental protection including water treatment by separating and removing toxic materials."

Jan 1, 2008

By Ibrahim Yusufoglu, Ahmet Orkun Kalpakli, Cem Kahruman, Sedat Ilhan

"The effects of oxalic acid concentration, temperature, stirring rate and particle size on the dissolution rate of synthetically prepared calcium molybdate were investigated. Dissolution of calcium molybdate in oxalic acid solutions takes place as a series - parallel type reaction. In the first reaction step, which proceeds according to the ""Langmuir - Hinshelwood Mechanism"", calcium aqua oxalato molybdate is formed as a complex chelate intermediate product. In the second reaction step, molybdic acid is formed during the slow hydrolysis of calcium aqua oxalato molybdate, and it reacts rapidly with oxalic acid to form the polymeric hydrogen oxalate dimolybdate chelate as an end product. Activation energies were calculated as 41.4 and 49.9 kJ mol-1 for the first and zero order reactions. The fractional conversion versus time relationship can be given by the following equation.IntroductionMolybdenum is used widely in electric-electronic, metal working, aerospace and aeronautic, nuclear, glass and petrochemical industries because of its high melting temperature and resistance against chemical effects. However, the largest molybdenum consumers are the iron-steel and super alloy industries where molybdenum is used as an alloying element. Industrially important molybdenum minerals are limited to molybdenite (M0S2), powellite (CaMo04) and wulfenite (PbMo04), which are considered as primary molybdenum resources. Secondary molybdenum resources are spent catalysts and scrap [1-4].Molybdenum has been produced by pyrometallurgical processes in the past. Since it is possible to process low grade molybdenum ores and industrial wastes by hydrometallurgical processes, which are more environmentally friendly than pyrometallurgical processes, the importance of the use of hydrometallurgical processes has increased in the molybdenum production industry."

Jan 1, 2012

By Toshiyuki Hashida, Victor M. Lopez-Hirata

"Small-punch tests and determination of fracture toughness JIC were conducted at 4 and 77 K on new cryogenic JN1, JJ1 and JK2 austenitic stainless steels, after isothermal aging. Equivalent fracture strain ?qf determined by measuring the reduction of thickness in the small-punch test specimen. A linear dependence of JIC on ?qf was found in these new materials. Regression analysis of experimental data produced the following linear relation JIC = 1304.1 ?qf + 8.09 [kJm-2]. An analysis of present work relation was pursued on the basis of material properties and evaluation method of he. Results showed that the slope value has a strong dependence on material yield strength and JIC evaluation method. This linear relation is useful for the evaluation of fracture toughness JIC, measuring the equivalent fracture strain ?qf by means of small-punch test. Thus it can be useful for assessing the degradation of fracture toughness in small areas such as, the heat-affected zone in welded components.IntroductionCryogenic structural materials for superconducting magnets of fusion nuclear reactor are required to possess a good combination of strength and toughness. The mechanical properties are required beyond the capability of conventional austenitic stainless steels [1]. New cryogenic JN1, JJ1 and JK2 austenitic stainless steels were developed by the Japan Atomic Energy Research Institute (JAERI) [1]. The structure of superconducting magnets is constructed by welding of 200 = thick plates of these steels, which are solution treated at high temperatures and then water-quenched to avoid intergranular precipitation. However, the welding process involves heating and cooling [2], which cause microstructural changes in both base metal and weld. In this heterogeneous microstructure, it is important to estimate the fracture toughness of these materials at cryogenic temperatures. Therefore, it is necessary to evaluate the effect of aging process on the fracture toughness behavior of these new steels. To determine the cryogenic fracture toughness, the elastic-plastic JIC value has been co=only used [2]; however, the specimen size is much larger than heat-affected zones in welded components. Small-punch (SP) testing method, employing miniature specimens, has permitted to evaluate the fracture toughness behavior at different temperatures in different nuclear reactor materials [3,4]. Mao et al. [5,6] and Misawa et al. [7] found a linear relation between JIC value and equivalent fracture strain ?qf, determined by SP method in non-ferrous alloys and ferritic steels at room temperature and austenitic stainless steels at 4 and 77 K, respectively. So that, this kind of correlation would be very useful to assess the fracture toughness JICe values by means of SP test in small zones of welded components."

Jan 1, 2012

By J. E. Dutrizac

The behaviour of the lanthanide elements during the precipitation of sodium and potassium jarosites at 98oC from sulphate media was systematically investigated. The lower atomic weight lanthanide elements (La to Gd) are characterized by the limited solubility of their alkali-lanthanide sulphates, such as NaNd(SO4)2?H2O, which commonly contaminate the jarosite precipitates. Hence, single phase jarosite-type compounds were precipitated only from solutions containing <0.4 g/L of the La to Sm lanthanides. The sulphates of the heavier atomic weight lanthanide elements (Tb to Lu) have significantly higher solubilities such that solutions containing up to 10 g/L of the individual lanthanides could be investigated without the precipitation of alkali-lanthanide sulphate species. Even at the highest lanthanide concentrations, however, none of the jarosite precipitates incorporated more than 0.3 wt% of any of the lanthanide elements. Comparable levels of lanthanide incorporation were noted in both Na-jarosite and K-jarosite. Although the mass of the jarosite precipitate increased with increasing ferric sulphate concentration or with increasing pH, the extent of lanthanide incorporation was not significantly affected. Clearly, the trivalent lanthanide elements do not substitute extensively for trivalent iron in the jarosite structure. This behaviour likely reflects the significantly lower hydrolyzability and larger size of the trivalent lanthanide ions relative to ferric ions.

Jan 1, 2003

By Richard D. Hagni

The United States is dependent upon foreign sources for more than 93% of its bauxite and alumina supply. Domestic production of bauxite, which comes from Alabama, Georgia and Arkansas, is limited to those bauxite ores containing less than about l ½ % iron. Bauxites with higher iron contents are generally not utilized because they cause problems in bauxite calcining and especially because they produce undesirable brick discoloration and cracking. In order to improve beneficiation and expand the utilization of high-iron or ferruginous bauxites, a mineralogical and textural study has been conducted on selected samples from the Eufaula, Alabama, bauxite district. Reflected light microscopic, petrographic, and X-ray techniques have shown that a variety of iron minerals are present, including hematite, goethite, lepidocrosite, siderite, pyrite, marcasite, and ilmenite. Although the iron minerals may be locally concentrated into concretions and pisolites, most occur as very fine grains that are disseminated and show a variety of intergrowths. Mineralogical and textural observations indicate that the fine-grained iron mineral grains may be amenable to high gradient magnetic separation.

Jan 1, 1981

By Pinakin C. Chaubal

Today?s steel industry is in a vibrant and resurgent mode. This transformation has been in the making for some time now. Over the last few decades, the industry was steadily transforming itself into becoming a high tech industry. New technology was adopted, efficiencies were enhanced, lean manufacturing concepts were brought in and a strong customer focus was developed. Today?s mills employ sophisticated instrumentation, computerized monitoring, on-line smart systems etc. driving processes that are producing at rates of many tons/minute. All this is not possible without judiciously using the latest available technologies in various fields and developing a more sophisticated work force. Prof. Sohn has been a pioneer in driving the concept of process engineering in process metallurgy. In this paper the focus is on some aspects of process engineering ? primarily process modeling - as applied to iron and steelmaking processes. Examples are shown to demonstrate how problems have been addressed. Some thoughts on future directions are presented.

Jan 1, 2006

By John A. Mavrogenes

The Texaco gasification system developed at the Monte Bello pilot plant efficiently bums petroleum-coke thereby producing syn-gas and electricity. This system produces more electricity than conventional burners, yet the only by-products are pharmaceutical grade sulfur and V -rich slag. Vanadium is known to exist in multiple valence states in compounds which possess a wide range of melting points and physical properties. Consequently, it becomes important to carefully regulate oxygen fugacity throughout the system in order to control vanadium valence state. Vanadium phase equilibria is presently poorly understood, in large part because of the multiple oxidation states of vanadium (-I, 0, +2, +3, +4, and +5) and the difficulty of unequivocally identifying the valence state(s) in many compounds. The operation of these gasifiers at approximately 1400°C is well above the melting point of V20S but considerably below the melting temperature of V02 and V 203. If J02 can be regulated to keep the burner within the V 205 field, slag material would more likely remain molten and more easily flow out of the bottom of the burner. In pure V oxides. the oxidation state is readily determined by microprobe analysis. where V20S (V+5) is 56% V, V02 (V+4) is 61.4% V, and V203 (V+3) is 68% V. However, V valence in multi-element phases (especially phases containing other elements of variable valence) cannot be resolved by microprobe analysis alone. Petroleum-coke gasification slags collected from within the gasifier under different oxidation conditions were studied by electron microprobe analysis (EMPA). X-ray diffraction (XRD). X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy. Raman spectrometry in conjunction with microprobe analysis was found to resolve the valence of vanadium in the phases of these slags. Raman spectra collected from homogeneous single phase V-oxide standards in vacuum at low temperatures (-150°C) yielded peaks characteristic to each valence state. Gasifier slag samples are, however, much more complicated. Oxidized samples contain: fine grained (Ca. Mg, Fe. V) oxide matrix of variable composition, (Fe. V, Ni) spinel. (Fe, AI, V, Ni, Mg) spinel, V205laths, AI-Si glass blebs and Ni sulfides. Reduced samples contain: crystalline Ca-siIicate matrix, subhedral to euhedral (V, Fe, Mg, AI) spinel, subhedral V02, Fe and Fe-Ni sulfides, Fe-Ni alloys, and complex Ca-oxide matrix. The different spinel assemblages, the characteristic V-oxides and the distinctly different character of the matrices makes the oxidized and reduced slags readily discernible.

Jan 1, 1995