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By Y. FUJII, E. CHANDA, J. KODAMA, D. FUKUDA, M. NISHIHARA, Y. NAKAYAMA, P. SINKALA

For over 40 years, Mufulira underground copper mine has been recording incidents of rockburst. Laboratory tests and numerical analyses were carried out to understand the rockburst mechanism at the Mufulira mine. Rockburst did not occur in the chain pillars or at the mining face, but mainly in the mining drives along diminishing pillars or ahead of the mining face. RQD suggested that the rock mass in the rockburst areas was relatively intact. Laboratory tests confirmed that the rock at Mufulira mine is very strong and brittle. Elastic stress analyses for the rockburst sites by 3D displacement discontinuity method (DDM) indicated very high stress in the chain pillars and low-stress concentration at the sites of rockburst during the initial mining stages. However, there was no apparent positive correlation between the elastically calculated normal stress values and the occurrences of rockbursts. The 2D elastic FEM analysis was conducted under the concentrated stress by DDM and indicated that some stress increase with face advance for the rockburst in the vicinity of the mining face. However, stress severity indicated almost no increase, and the rockbursts cannot be explained as an instantaneous rock mass failure due to stress increase by mining. Therefore, a creep damage model was proposed to clarify the mechanism of the rockbursts. Cumulative rock damage was evaluated for the edge elements of each sidewall of the mining drives, based on the normal stresses by 3D DDM. The rockburst occurrences were well hindcasted. A method to estimate the volume of the rockburst source was proposed, and a likely result was obtained.

Aug 12, 2022

By C. C. Li

The D bolt is a new type of energy-absorbing rock support element recently developed in Nor-way. The D bolt is not only able to accommodate large rock deformations, but can also provide a load-bearing capacity as high as that of rebar bolts. Furthermore, the anchoring quality of the D bolt is similar to rebar bolts because of its multi-point anchoring design.

May 1, 2009

By William R. Hardwick

Present information indicates that a copper deposit can be safely fractured with a nuclear explosive and the copper successfully recovered by the in-situ leaching method. The process is not yet at the stage where it can be presented t ) the mining industry as a technique proven in all its aspects, but it is a method with high success potential. Unknown factors must be evaluated by a full-scale test before the economics or the extent of the use of the method by the mining industry can be predicted. Preliminary calculations indicate that the cost of fracturing a copper deposit nuclear explosives may range from l.8 to 55.2 cents per ton or in some case: less than a cent per pound of recoverable copper. Copper may be recovered at less cost than by conventional methods. Deposits with 4 pounds of recoverable copper may be economic and production from a deposit may begin in less than half the time required for conventional methods.

Jan 1, 1967

By Alfredo Cámac Torres

El presente trabajo describe el proceso de planeamiento estratégico de la empresa minera, su entorno, la matriz, la visión, sus objetivos, el desarrollo de la estrategia, la fijación de acciones empresariales, presupuesto, control y evaluación del plan estratégico y la aplicacíón del software para un proceso de planeamiento estratégico. De acuerdo a la estructura de este proyecto, el Planeamiento Estratégico se constituye en un instrumento importante de la empresa, ya que es el proceso del pensamiento reflexivo aplicado a la misión de la organización y a las actuales condiciones del medio en que opera, en el cual se fija lineamientos, se elige alternativas y se establece una secuencia coherente de las acciones a realizarse. Asimismo, la herramienta SR permite a los ejecutivos ver representaciones textuales y gráficas de los planes desarrollados y representa los componentes de cada plan individual y su progreso hacia las metas y objetivos establecidos.

Sep 12, 2005

By F. Habashi

"The rare earths industry started in Austria in 1887 by Carl Auer von Welsbach (1858-1929) Professor of Chemistry at the University of Vienna. The process was based on monazite sand transported from Brazil as shipping ballast free of charge. This made possible producing thorium, cerium, and other rare earths at a low cost, thus permitting the growth of the industry. However, once the Brazilian authorities realized the strategic importance of the sand, shipping was stopped. Brazil then started its own processing of the sand in 1949. The background for Auer’s work, the role of Robert Bunsen in Heidelberg, and the invention of the spectroscope will be presented. INTRODUCTIONHeidelberg on the Neckar (Figure 1) was the meeting place for chemistry students from all over Europe in the nineteenth century. Her university founded in 1386 had already a famous professor of chemistry and medecine in the Faculty of Medicine by the name Leopold Gmelin whose three - volume Handbuch der theoretischen Chemie appeared in 1817-1819, that became later a multi-volume monumental work. As successor to Gmelin came Robert Bunsen (Figure 2) in 1852 who made this university town the Mecca of chemistry students. One of his students, the English Henry Roscoe (1833-1915) who became later a distinguished professor in Manchester, described him as follows: ""As an investigator he was great, as a teacher he was greater, as a man and a friend he was greatest""."

Jan 1, 2012

By V. S. Gupt, W. H. Somerton

Rock may undergo great changes in physical properties when heated to high temperatures and then cooled, The temperature and intensity of reactions causing rock alterntiorl.s can he controlled by introducing certain chemicals during heat treament. Three typical outcrop sandsone samples were saturuted with common salt solutions, then heated to several maximum temperatures. After cooling, it was found that per-rrreuhilities had increased much more for salt-saturated samples than for samples not saturated with salt but heated to the same temperatures. This was only true, however. for samples heated above the melting points of the particrrlar salts. Potassium chloritle was particularly effective with Bandera sandstone. Samples saturated with potassium chlorirlr. solution and heated to 900C showed an 11-fold increa.se in perrrieahility. Samples without potasrirdrn chloritle but heated to the .same temperature. showed only a 2.7-jold incresre in permecahility. In application, it seems possible that injecting chemicalc into the formations from a wellbore followed by applying intensive borehole heating might promote reactions which would greatly improve permeability of the formalions. INTRODUCTION Great changes in the physical properties of rocks which have been heated to temperatures in the range of 600 to 800C have been reported earlier. Permeability increases of 50 per cent, and equivalent decreases in sonic velocity and breaking strength have been observed. Although there might be some suppression of certain reactions responsiblc for these changes when rock samples are heated under simulated reservoir pressure conditions. recent work has shown that these are more than offset by the increased importance of other reactions at high pressures. The reactions considered responsible for alteration of rock properties by heating include differential thermal expansion. dehydration, phase changes and dissociation of mineral constituents. Ceramists have long known that temperatures at which reactions occur can be raised or lowered by the presence of certain impurities in the sys. tcnl. Thus the possibility exists that by saturating rocks with appropriate solutions. desired reactions might be accelerated and unwanted reactions might be suppressec! when the rock is heated. Purpose of the present work was to investigate the effects of several common salts on the thermal alteration of sandstones. Types of reactions which might occur are reviewed and the findings of a number of thernlochemical alteration tests are presented. THEKMOCHEMICAL ALTERATION OF SANDSTONE MINERALS The most abundant constituent of most sandstones is quartz. Quartz can exist in at least eight different forms, but in the temperature range of immediate interest (to 900C) only two forms are of importance—alpha quartz below 573C and beta quartz above this temperature. Although the alpha-beta inversion of quartz is very important in thermal alteration of rocks. it is not particularly important here because the inversion temperature cannot be changed significantly by the presence of impurities or by the application of pressure. The transition temperature of quartz to tridynlite is 867C. but the transition is very sluggish. Tridymite is considered to be a metastable transition phase between two stable phases: quartz?cristobalite. However. the transition temperature for tridymite to cristobalite is 1,470C.4 The quartz-tridymite-cristobalite transition can be accelerated substantially by the presence of fluxing agents. Finely divided calcium, magnesium and titanium oxides accelerate the conversion while A12O may retard it. A Mixture of NaCl and CsCl reduces the temperature for cristobalite formation by as much as 420°C. Feldspars constitute the second most important mineral in sandstones. The melting points of feldspars range between 1,000 and 1,700°C depending upon the variety. No information available indicated any important role of fluxing agents in the thermal alteration of this group of minerals. Carbonate minerals are subject to dissociation at temperatures within the range of the present investigation. The dissociation of magnesite can start at a temperature of 373°C, but the reaction is sluggish and might not occur untll a temperature of 500°C or ,higher is reached. Dolomite dissociates in two stages at 500°C and 890°C, whereas calcite dissociation temperature is about 885C. Because CO2 is released in the dissociation of carbonates, ail such reactions are somewhat dependent upon CO2 partial pressure. In the absence of CO: in the surrounding atmosphere, the dissociation of calcite starts at 500°C.However. when 1 atm of CO surrounds the sample, the dissociation does not start until 900C. The other carbonates are apparently much less sensitive to a change in partial pressure of CO2. The aragonite calcite transformation can occur an!. where within the temperature range of 357 to 488°C. depending upon the presence of impurities such as barium. strontium. lead and perhaps zinc. The differential thermal analysis (DTA) curves of both magnesitc and dolomite vary with the presence of 'impuritics. The presence of iron in particular seems to affect the magnesitc DTA curve

Jan 1, 1966

By G. M. Wilemon, Swanton. R. G.

The Bureau of Mines is investigating the leaching of phosphate values from Florida phosphatic clay wastes using sulfuric acid (H2SO4) as the leaching agent and methanol as the solvent. Acid-alcohol leaching studies were done using research-grade apatite to investigate potential causes of flow extractions. It was found that a barrier layer formed on the surface of the apatite. Initial discovery of the barrier layer was made by analyzing pure apatite samples before and after leaching using an optical microscope. Subsequent Fourier Transform Infrared (FT-IR) analyses proved the coating was calcium sulfate hemihydrate (CaSO4•1/2H2O) and that unreacted apatite existed beneath the coating. Scanning electron microscope (SEM) photographs depict the CaSO4• 1 /2H20 morphology as long slender crystals adhering to the apatite surface. It was also shown that grinding the leached tailings and leaching again in the H2SO4-methanol system resulted in additional phosphate extraction.

Jan 1, 1992

By W. J. O'CONNOR

THE production of lead in the United States for the period from 1720 to 1912 was 10,432,668 tons valued at $924,600,000. The average price during this period was 4.4c. a pound, although lead sold at times below 3 cents. We know that in the early days of lead smelting in Montana lead was deliberately lost in the slag and only enough reduced as bullion to collect the silver. This bullion was freighted by ox team to Corinne, Utah, the terminus of the railroad at that time, and shipped to Swansea or Omaha, Neb., for refining. The slag from some of the above mentioned operations contained as much as 15 per cent lead and has since been resmelted. Since 1921 the production of lead has increased each year and the price and tonnage have been as follows :

Jan 1, 1926

Although the 71 Minerals operation is now closed down and the operating data presented is almost five years old, it is well worth describing since it was the first heap leaching operation conducted on a primarily silver ore. Tombstone was discovered in 1877 by Ed Schieffelen; and it became one of the most famous mining towns in the West through the stories connected with Wyatt Earp, Doc Holliday, and the Clanton brothers. Like many silver deposits .in the western United States, the Tombstone ores were relatively shallow. Several million ounces of silver were recovered in the relatively few years the camp was active; but mining virtually ceased by the early 1900s and was only continued in a small way until the 19409, a history similar to that of Tuscarora. The 71 Minerals operation was started in May 1975 and continued until late 1978 within the city limits of Tombstone on waste dumps; one was the' Lucky Cuss, Schieffelen's discovery, which had accumulated from the old underground operations. This waste material was mostly less than 50 mm (2 in.) in size, although there was some larger lumps. The grade was about 34 g Ag and 0.5 g Au per mt (1.0 oz Ag and 0.015 oz Au per st). The Tombstone dumps contained approximately 1,000,000 tons. The dumps and patented claims were held by a single owner, Tombstone Development Company, thus sufficient leaching material could be acquired from one source rather than dealing with a number of individuals, as is usual in putting together leaching ventures in old mining camps. 71 Minerals Ltd. was formed and a lease of the properties obtained. A site was selected close to the major mine dumps not far from down- town Tombstone. Pads approximately 90 m (300 ft) wide and 180 m (600 ft) long with an 8-degree slope were prepared using compacted old mill tailings as a base sealant on the pads. Mining was done at a rate of about 2,000 tons per day with a dozer, two scrapers, a front-end loader, and 30 ton trucks. The ore was dumped by the scrapers as it came from the dumps with no screening or crushing in 460 mm (18 in. ) layers and trimmed with the loader. Based on bulk sampling and laboratory testing, the majority of thegold and silver values were recovered within 30 days of leaching.

Jan 1, 1981

By Charles LeMoyne

The Cable belt Company has been building single flight conveyors for a number of years. The simple design concepts of this type conveyor, introduced over thirty years ago, when distances of one to two miles were considered major advances in technology, remain relatively unchanged. Conveyors that are 6 to 20 miles (9.0 to 32 kilometers) long are being built and are presently in operation through- out the free world. The Cable Belt conveyor is not conventional in its construction. Cable welt differs from conventional troughed idler conveyors in that the driving medium and carrying medium are separated. Motion is provided by two endless steel cables running the length of the conveyor. The cables are driven by a single drive unit incorporating a differential gear which insures identical cable linear speeds and equal tension in both cables at all times. The belting is located and supported by "V" shaped shoeforms moulded to the belt which form a wedging action. The friction between the belting and rope is sufficient to prevent slippage (See figure 01).

Jan 1, 1983

By A. D. Garman

This paper presents one of a series of digests of foreign mining legislation and court decisions which is being prepared in advance of a general report relative to the right of American citizens to explore for minerals and to own and operate mines in various foreign countries. This interpretation of the laws of Colombia has been prepared from the best available information in Washington, but is released subject to correction and amplification; if necessary, by the proper American diplomatic and consular officers to whom it is being referred through the courtesy of the Department of State. SYNOPSIS OF LAW Minerals in Colombia belong to the owner of the soil unless otherwise provided in the law. The following lands and deposits, however, are described as fiscal property of the State: Class 1. The public lands, mines, and salines which belong to the individual States (now Departments) prier to the adoption of the present constitution (1886).

Jan 1, 1929

By Sean Dessureault

Las operaciones mineras a gran escala requieren de estrategias adecuadas para el control de la productividad y la calidad final del mineral. En ese sentido, el presente texto describe un mejor manejo de las actividades críticas de la mina a través del Sistema de soporte a las decisiones que utiliza la información histórica de un almacén de datos corporativos. Asimismo, las lecturas provenientes de los equipos y sensores distribuidos en la infraestructura son consolidadas para su análisis con herramientas de Inteligencia de Negocios. Los beneficios que presenta esta herramienta de investigación permite considerar la factibilidad de implementar prototipos similares al servicio de las minas peruanas y así contribuir con la optimización de los procesos productivos.

Sep 12, 2011

By Hongmin Zhu, Guihua Wang, Xiangsheng Wang

"The anode process of carbon electrode in fluoride melt was studied by voltammetry and chronoamperometry. Anode gases were analyzed by gas chromatography on-line during controlled-potential electrolysis. Two peaks were observed on the cyclic voltammograms. According to the results of gas chromatography, the first peak was corresponded to the discharge of residual oxide ions, with the formation of CO and CO2. Discharge of fluoride ions occurred at 4.1 V vs. Li+/Li, and leading to the anode effect. With the occurrence of anode effect, small amount of CF4 was detected. As the potential reached 4.5 V, CF4 and C2F6 gas evolution occurred, and the current increased to form the second peak.1.IntroductionIn the primary production of Aluminum and some rare earth metals like neodymium, a departure from normal cell operation known as anode effect results in the generation of perfluorocarbons (PFCs), which have high global warming potentials [1]. Owing to the pressure of environmental protection, considerable research has been carried out to clarify the mechanism of anode effect and PFC generation of industry and laboratory cells in the aluminum electrolysis system [2-9]. The common result on PFC generation is that the PFCs are emitted from Hall-Heroult cells only when they are on anode effect. In this article, we selected LiF, the main electrolyte for the neodymium electrolysis [10-11], to perform further investigation on the underlying kinetics of PFC generation and the nature of the reactions at the electrode.2. ExperimentalAll experiments were carried out in an alumina tube reactor, which was filled with high purity helium atmosphere. Spectrographic graphite crucibles were used, which played the dual role of molten fluoride container and the counter electrode. Lithium fluoride was analytical grade. The experiments were carried out at 900 °C."

Jan 1, 2011

By C. B. Jordan

LAVES and Wallbaum' have described TiRu and TiOs as having the same structure as TiFe; they had previously described the latter compound as having the CsCl structure. On the other hand, a careful investigation of the structure of TiFe by Duwez and Taylor- ailed to reveal the ordered CsCl structure, finding instead a random arrangement of titanium and iron atoms on the points of a body-centered-cubic space lattice. Consequently, it is not clear whether Laves and Wallbaum proposed the ordered or the disordered structure for TiRu and TiOs. In order to settle this question as to the structural type and to obtain values of the lattice para- meters (thereby completely determining the structures), the present investigation was undertaken. Samples having the compositions TiRu and TiOs were weighed out accurately from iodide titanium supplied by the New Jersey Zinc Co., ruthenium powder from Goldsmith Brothers Smelting & Refining Co., and osmium powder from Wildberg Brothers Smelting & Refining Co. No analysis was made of any of these metals. According to the respective analyses of the suppliers, total impurities amount to less than 0.03 pct in the titanium and to less than 0.5 pct in the osmium. The purity of the ruthenium is not known. The alloys were prepared by arc melting in a furnace of the type described by Schramm, Gordon, and Kaufmann.9 pecimens for X-ray diffraction were obtained by crushing the ingots and passing the resulting powders through a 200 mesh screen. Diffraction patterns were made with a powder

Jan 1, 1956

By McPherson M. J

An experimental investigation was carried out to determine the various gas flow characteristics of bituminous coal samples. Adsorption and desorption tests were first conducted to estimate the quantity of methane that is retained by coal, and the rate at which it is released. Experiments were then carried out to study the variation in coal permeability with changes in applied stress and gas pressure - factors that change continuously with time. To further understand the phenomena involved in retention, release, and flow of gas, electron microscopy was used to study the microstructure of coal and how it affects these characteristics of coal.

Jan 1, 1988

By Howard R. Hume, Terry R. West, William R. Judd

One of the outcomes of a sector slope design in a large open pit in the western United States has been the scrutiny of the structural domain concept. These domains essentially define the area of influence of particular structural characteristics. In the present instance these structural characteristics are joint discontinuities. One of the major drawbacks of defining a domain is that unless large quantities of discontinuity data are available this process of definition is largely qualitative in nature. Viewed from a discontinuity analysis aspect the orientations of all the major joint sets at a given point are a concise descriptor of the structural geologic regime at that location. This is important to domain boundary definition, this in turn is extremely important for assigning which joint sets to use as input for slope stability analysis in a given discontinuity domain. An attempt has been made to develop a quantitative method for defining these discontinuity domains based on limited amounts of orientation data thereby reducing the subjectivity normally involved in such operations. Subjectivity is not always a problem if large quantities of joint orientation data are available, since the mean and variance of joint clusters always can be compared and then grouped to define these domains. However, even this method suffers from the problem that only a single joint set orientation can be considered at a time during the grouping process. On the other hand a discontinuity domain requires that all joint sets at a point be considered simultaneously to truly define the structural discontinuity character of that point. This provides a far more complete

Jan 1, 1982

By Frederick Bloetscher

An improved parachute-type stopping for changing the course of mine ventilation air during mine emergencies has been developed by Goodyear Aerospace Corporation for The Bureau of Mines. The stopping can be quickly deployed by one man from a single attachment point and provides excellent stopping performance with the flow in the design direction. Adding pin and foam attachments between its skirt and the passage-way surfaces improves its performance with flow in the design direction and maintains the stopping with zero or reverse air flows. Stopping performance results for a range of airway sizes including 7.5 X 10 ft simulated airway with pressure differentials of up to 3.0 inches of water are presented. Predicted performance values for this stopping design for larger passageways are also presented.

Jan 1, 1977

By J. Cervik, P. C. Thakur, S. D. Lauer

Methane drainage by cross-measure boreholes on retreat longwall faces can be a viable alternative to the vertical gob degas boreholes under favorable circumstances. The research was done in a mine working Pittsburgh coal seam in northern West Virginia under USBM Cooperative Agreement No. 14-09-0050-3252. The study was the first application of this technique to Pittsburgh coal seam. A total of 14 small diameter, inclined boreholes were drilled over a retreat longwall panel from gate roads, to intersect the overlying coal seams. All boreholes were manifolded to a pipeline and the gob gas was extracted by a surface exhaust fan. The methane capture ratio was poor at 7% to 18% at various stages of the longwall panel. A vertical gob degas borehole captured an additional 20% gas. Poor results were due to premature failures of the cross-measure boreholes leading to air leakage. For better performance, the boreholes should be drilled from a point 30 to 45 m (98 to 148 ft) from longwall pillar over the largest chain pillar. The standpipe should be grouted for at least 6 m (20 ft), and the entry containing boreholes and the pipeline must be supported to ensure access for maintenance and optimization of methane capture. Coursing the ventilation air around longwall such that it forces methane migration toward cross-measure boreholes can further improve methane capture. The optimum vertical inclination is 45º ± 10º.

Jan 1, 1986

By Francesco Vegliò, Luigi Toro, Francesca Pagnanelli

Different hydro-metallurgical processes have been studied in order to recover manganese(II) from oxidised minerals such as MnO2. An innovative acid reductive leaching carried out in mild experimental conditions was here considered using agricultural and industrial wastes containing carbohydrates as reducing agents. The leaching process was investigated from a kinetic and equilibrium point of view in order to optimise the experimental conditions, develop a kinetic model and obtain high purity concentrated MnSO4 solutions. To study the leaching kinetic a Shrinking Core Model (SCM) was modified by a variable activation energy term to take into account both the variable reagent concentrations and the reaction rate change with respect to the manganese dioxide conversion. The influence of the particle size in the kinetic model is discussed with the support of SEM analysis before and after leaching. Manganese extraction yield was maximised (170-190 g/L) using appropriate carbohydrates and acid excesses, while impurity concentrations were kept low (Fe<10ppm and Ca<300ppm) pre-treating the ores, using hydro-alcoholic leaching medium and different combinations of down-stream processes. In particular precipitation, solvent extraction and adsorption onto active carbon were tested to eliminate Fe and Ca from MnSO4 solutions.

Jan 1, 2003

By A. D. Zunkel, A. H. Larson

Equilibrium arsenic contents of Pb-As alloys in contact with PbO-As2O3 slags containing less than 30 mol pct As2O3, were determined at 650°, 700: and 750 C in an inert at?rzosphere. In this temperature range, the arsenic content of the alloy increased with increasing temperature in the single-phase liquid slag region and decreased with increasing temperature in the two-phase slag region and the single-phase solid-solution slag region. The PbO-As2O3 phase diagram below 22 mol pct As2O3 was determined by thertrzal analysis and by application of a log ?As2O3/?PbO vS log XAs2o3 /x3pbO plot determined from the equilibrium actiuity data. The resulting phase diagram was not well-defined since the eutectic temperature was not detected in the thermal analysis experiments, although a region of terminal solid solubility of As2O3 was found. Results from the phase diagram determination are compared with an existing diagram in the literature. THIS experimental investigation is an extension of a study by the authors1 on the slag-metal equilibria in the systems concerned with commercial lead refining processes such as softening and dross fuming. The first part of this investigation was a study of the slag-metal equilibria in the Pb-PbO-Sb2O3 system. The only experimental work previously done on the Pb-PbO-As2O3 system was by Pelzel2,3 in which the phase diagram for the PbO-As2O3 system was determined below 50 wt pct As2O3 and the equilibrium constant for the reaction 3Pb + As2O3 + 3PbO + 2As was determined as a function of temperature. No slag-metal equilibrium data have been determined. It is due to the scarcity of information regarding the Pb-PbO-As203 system that this work was undertaken. This paper describes the determination of the slag-metal equilibria in the Pb-PbO-As203 system by equilibrating Pb-As alloys with PbO-As2O3 slags in an inert atmosphere, the effect of 1 wt pct additions of bismuth and copper on the slag-metal equilibria, and the PbO-As2O3 phase diagram both by thermal analysis and the use of the slag-metal equilibria data. EXPERIMENTAL Materials. The materials used in this investigation were analytical reagent-grade and assayed as follows: 1) 99.8 pct PbO (0.014 pct insoluble in CHJCOOH, 0.02 pct not precipitated by H2S, 0.1 pct CaO, and 0.08 pct SiO2); 2) 99.95 pct As2O3; 3) 99.99 pct Pb; 4) 99.0 pct As; 5) 99.99 pct Cu; and 6) 99.97 pct Bi. Room-temperature X-ray patterns revealed no detectable impurities in any of these materials. Apparatus for Equilibrium and Thermal-Analysis Determinations. The resistance-heated crucible furnace used in this investigation employed nichrome elements and was mounted so that it could be raised to surround the reaction tube during each experiment and, subsequently, lowered. A schematic diagram of the apparatus is shown in Fig. 1. Each charge was heated in a 3+-in.-OD by 31/2-in.-high 416 stainless-steel crucible placed in a 41/4-in.-1D by 18-in.-long fused-silica reaction tube which was closed at one end. On a shoulder around the crucible was placed a 3: -in.-OD by 12-in.-long open-end fused-silica condenser tube. The open end of the reaction tube was covered by a water-cooled brass cap with ports for 1) admitting an inert atmosphere to the system through a stopcock, 2) introducing a stainless-steel, motor-driven, paddle stirrer into the crucible, 3) evacuating the system with a mechanical vacuum pump, and 4) sampling the melt with Vycor sampling tubes. The brass cap was fitted to the open end of the reaction tube with a silicone gasket and collar clamp. The furnace temperature was controlled by a Barber-Coleman Capacitrol controller and a chromel-alumel thermocouple. Due to the corrosiveness of the melt, the controlling thermocouple also served as the measuring thermocouple. The temperature of the melt was calibrated against the controller temperature and was checked periodically during each test with a Vycor-enclosed calibrated chromel-alumel thermocouple. The temperature measurement and control can be considered accurate to ±3°C. Procedure. The charge placed in the crucible for each experiment consisted of 1000 g of Pb-As alloy and 300 g of PbO-As2O3 slag. The crucible was then placed in the reaction tube, the condenser tube was placed on the shoulder of the crucible, the silicone gasket and brass cap were fitted on the open end of the reaction tube, and the entire system was evacuated and filled with argon ten times. After the last flushing, a positive argon pressure of 1 psig was impressed on the system. The furnace was then raised to sur-

Jan 1, 1968