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By G. Gutzeit

METAL-ORGANIC INNER COMPLEXES AN inner complex is a cyclic chemical structure containing an inorganic cation that is bound simultaneously to several atoms in a single organic molecule; on the one hand by means of ordinary valence bonds (electron exchange), on the other hand through the action of the electric field thus created, which satisfies the so-called secondary valences. The relative positions of the salt-forming and complex-forming groups are such that most frequently a four, five, or six-membered ring results through this double attachment of the cation.1-6 The formation of inner-complex ring systems depends not only upon the nature and suitable position of the salt-forming and complex-forming groups for ring closure, but, to a great extent, also on the nature of the metallic cation entering the reaction. This selective character of chelate-forming organic compounds is one of their most interesting and most valuable properties. As a matter of fact, the largest number of their practical applications is based upon their specificity. 4,1-13 Once a chelate compound is formed, its character is definitely "organic" in nature. In other words, its properties are conditioned to a much larger degree by the carbon chains or rings than by the metallic atom. Many inner complexes are soluble in nonpolar solvents such as benzene, paraffin oil or carbon tetrachloride, while the chelate-forming reagent before closure of the metal-organic ring is water soluble. (Example: copper complex of salicyl-aldoxime.) It is obvious that such particular properties as those indicated above can be utilized whenever specificity and practically complete binding of inorganic ions into an undissociable complex are required. One of the well-known applications of chelate-forming compounds has been the development of specific reagents in analytical chemistry,, creation of the spot-test method,4,14-16 and the application of the same principles to the contact print method for determining minerals.17 CHELATE-FORMING COMPOUNDS AS COLLECTORS In the field of flotation, where selectivity is often a quality of paramount importance for the collector, various workers have lately attempted to apply their knowledge of specific organic analytical reagents to this purpose. A. C. Vivian18 has concentrated cassiterite by using ammonium nitrosophenylhydroxylamine (Cupferron) C6H5NO(=NONH4). Holman19 has tested dimethylglyoxime for the flotation of nickel oxide minerals, while deWitt has shown in a series of systematic experiments that alpha-dioximes were generally selective collectors for nickel ores. Taurin NH2(CH2)2SO3H has been proposed for the concentration of oxidized lead ores.19 Diphenylthiocarbazone

Jan 1, 1946

By Oswald J. Heinrich

The responsibility resting upon the owners and managers of mines where fire-damp is generated, renders it a matter of imperative duty that a frill and correct statement of any explosion that occurs should be given to the public. But such a statement must be based on the testimony of impartial eye-witnesses or trained experts. Then a sad experience may result in the adoption of effective preventive measures. In the absence of any official and professional body of mining experts in the State of Virginia, the writer desires to submit to his professional brethren of the American Institute of Mining Engineers an account of an explosion which recently took place in a colliery under his management, and earnestly desires a thorough and impartial discussion on the Fats submitted. Description and Plan of the Mine.—The "Grove" shaft is situated at the nearest point 825 feet from the last old workings upon the Midlothian property, south of the old Pump shaft works. (See Plate 111.) The shaft was sunk by the former company, some thirty years ago, to the depth of 622 feet. An incline over 230 feet long, starting in a northwest direction at a depth of 105 feet above the shaft bottom, had been driven to explore the coal on the dip. A return of very small dimensions had been driven round the shaft on the south side, entering the upcast chamber. With the information obtained from the former company that a seam of coal about four feet thick, at a depth of 490 feet, had been found, and with the information obtained by the present proprietor, R. T. Burrows, of Albion, N. Y., by means of two boreholes on the dip west of the old shaft, in both of which workable seams of coal at various depths had been ascertained, the clearing out and thorough retimbering of this shaft were commenced in March, 1873. Borehole No. 1, at a depth of 4773 feet from surface, revealed a seam of coal. This borehole was afterwards carried to a depth of 1140 feet to the granite, without finding any other seam of coal. Borehole No. 3, at a depth of 608 feet, revealed the first coal-seam, 14 1/2 feet thick; at 633 feet, the second, 12 feet thick; at 662 feet the third, 1 foot thick, and at 692 feet the fourth, 43 to 5 feet thick. The borehole was stopped at a depth of 715 1/2 feet.

By Gordon G. Bentle, W. P. Fishel

GREINER, Marsh, and Stoughton1 have reviewed the literature in a monograph on the iron-silicon system. The lack of agreement among the various studies may be due to the difference in the purity of materials in some cases. The results of the X-ray method indicate only a general rather than a specific limit of the y loop. The iron-titanium system was investigated by Roe and Fishel,' whose results are used in determining the iron-silicon-titanium y loop. The literature indicates that no study has been made thus far of the iron-silicon-titanium system in the y loop region. Experimental Procedure The alloys were made from Armco iron, 99.86 pct Si, and 98.5 pct Ti. The titanium contains 1.07 pct Fe. The Armco iron contains 0.01 pct C, 0.005 pct Si, 0.02 pct Mn, 0.006 pct P, 0.01 pct S, and 0.04 pct Cu. A dilatation sample of Armco iron was prepared in the same manner as were the other samples. Several dilatation runs indicated that Ac3 begins at 905°C and ends at 910°C, which compares favorably with the study of Wells, Ackley, and Mehl' employing specially purified iron. All alloys were melted in an induction furnace in Alundum crucibles and were top poured into baked core sand molds. The ingots weighed about 600 g as cast. Dilatation samples of 4 in. by % in. diam were taken from the bottom end of the ingot, from which turnings for analysis were taken. Turnings from each end of two of the samples indicated that the alloys possessed uniform silicon content. A hole was drilled halfway through each end of a 4 in, dilatation sample. A chromel-alumel thermocouple was inserted in each hole and the surrounding metal peened in to hold the thermocouple in place. Fig. 1 represents the dilatation apparatus. The heating unit is an Alundum tube wound with resistance wire; the dilatation tube is a McDanel combustion tube; the push rod is zircon; the dial gage is graduated in 0.0001 in. and was vibrated to prevent sticking. A blank run over the temperature range of interest gave no significant dilatation. The thermocouples were attached to a multiple recording micromax which indicated the temperature at each end of the sample at 35 sec intervals. A Lindberg control unit governed the rate of heating of the furnace, and lowering or raising the

Jan 1, 1957

Drainage and erosion control often become problems at mine reclamation projects. An example of this was an abandoned surface uranium mine on the south Texas plains. Engineers with the Texas Railroad Commission solved these and other problems with a three-dimensional geomatrix erosion-control matting at the 69-hm2 (170-acre) site, about 70 km (45 miles) southeast of San Antonio. Enkamat, manufactured by Akzo Nobel Geosynthetics, was installed to reinforce the grass waterways that handle runoff from the reclaimed mine. Reclamation was completed in the spring of 1992. Bill Walker is regional manager for Erosion Control Systems. He worked with the contractor to identify an erosion control product that complied with the project's design and installation parameters. "Use of erosion control matting enabled us to reduce erosion control costs," said Mark Rhodes, with the Texas Railroad Commission. "Also, the erosion control material was more aesthetically compatible with the reclaimed landscape." The commission's design called for a terrace ditch to be constructed midway up the reclaimed spoil slope to catch and collect water. Commission engineers selected spoil slopes, ranging from 5% to 8%, to build reinforced grassed waterways to drain the collected water from the terrace ditches. This was done instead of dropping the water at steeper slope location in rip rap- or concrete-lined channels. Enkamat's three-dimensional geomatrix of heavy nylon monofilaments is 95% open space that aids root growth. Its root-reinforcement system resists the hydraulic lift-and-shear forces created by high-volume discharges of water. In addition, fine eddy turbulences are prevented from isolating and uprooting individual roots and clumps of vegetation. Enkamat is flexible and lightweight. This makes it easy to install. And, because grass grows into it over time, it "disappears" after installation. Between 12,540 and 14,200 m2 (15,000 and 17,000 sq yds) were installed in the waterway using 150-mm (6-in.) staples to fasten the matting, said contractor Dale Blackstock. "It was easy to use; no problem at all to put down." Blackstock selected Enkamat from a list of eight different channel lining materials described as acceptable in the commission's design specifications. The design specifications were based on the results of channel-lining performance tests conducted by the Texas Department of Transportation. Rhodes said that the commission's Abandoned Mine Land Reclamation program had installed Enkamat on other abandoned uranium mines and on an abandoned surface lignite mine near Austin. "Pretty much all of our installations of Enkamat have worked out well," he said. "There have been no failures. The reinforced grass waterways have performed as designed."

Jan 1, 1998

By Akio Suzuki, P. G. Wahlbeck

AS a part of a study of the vaporization of transition metal-chalcogen systems, the vaporization reactions for the Ti-Se system have been studied. In order to establish vaporization reactions it is important to determine the identity of vapor species in equilibrium with the condensed phases. In some cases, it is possible to deduce the identity of vapor species through observations of composition change of the condensed phase with which the vapor is in equilibrium. Determination of vapor species in equilibrium with condensed phases should precede vapor-pressure measurements and is necessary for proper thermodynamic analysis of vapor-pressure data. Bear and McTag-gart' reported that vacuum heating ot TiSea at 950°C produced a residue with a composition of 1.7 Se/Ti atomic ratio units. Analyses of condensed phases existing for the Ti-Se system have been performed by Bernusset,2"4 Gron-vold and Langmyhr,5 Hahn and Ness,' and Ehrlich.~ Results and conclusions of two types of experiments are described herein: 1) experiments where samples of known composition were vaporized followed by chemical analysis of residues and 2) experiments where the vapor species were identified by means of a mass spectrometer. Experimental Section. Sarnple Preparation. Samples of TiSe2 were prepared in a sealed, evacuated quartz ampule by heating to 1000°C stoichiometric amounts of selenium of 99.999+ pct purity obtained from the American Smelting and Refining Co. and titanium of 99.2 pct purity obtained from A. D. Mackay, Inc. After heating, the sample was ground and reheated to insure homogeneity. Samples containing less selenium than TiSez were prepared by mixing amounts of titanium powder and TiSez appropriate for the desired composition; the titanium and TiSez mixture was heated in the same manner as described for TiSe2. Analyses of titanium selenide samples contained in quartz crucibles were performed by gravimetric oxidation in oxygen at 800°C; the products of the oxidation were solid TiOz and gaseous Se02. The mass of the original sample and the mass of TiOn determined the Se/Ti atomic ratio. The sample of TiSen used in these experiments had a composition of 2.04 Se/Ti atomic ratio units. The compositions for all samples reported were analyzed by this method. Va/!orization Experiments. Samples of titanium selenides were vaporized in tungsten Knudsen crucibles. Some vaporization experiments were carried out in glass vacuum lines followed by chemical analyses of residues, and some vaporization experiments were performed with a Bendjx mass spectrometer as described previously.8

Jan 1, 1967

By G. H. Tausch, J. R. Dublin, T. A. Huber

Simplified equipment and techniques have been developed to permit cementing a completion interval in a well and recompleting higher, lower, or at the same depth in such a manner as to: 1. Eliminate the need for a conventional drilling or workover rig. 2. Eliminate mud and other cement contaminants which have long interferred with ideal cementing. 3. Eliminate need for drilling out cement. 4. Provide a more satisfactory recompletion. 5. Provide a more economical recompletion. This technique involves the use of a small-diameter, lightweight, tubing extension which is run on a wireline and set in a landing nipple previously installed in the tubing string. Low squeeze pressure and small cement volumes, with their attendant cost reduction, are successfully used when wells are completed and reworked with salt water or other penetrating fluids. Relatively low-water-loss cement is an integral component of the technique which provides that excess cement be reverse-circulated from the well to leave the casing void of cement when recompleting lower or in the same interval. Substantial cost reductions are realized by using the simplified or low-pressure cementing technique, and the ratio of successful squeeze-cement operations has been increased. Squeeze-cementing or recementing is the act of filling a channel behind casing or filling holes purposely placed in the casing. To obtain a satisfactory squeeze-cement job, it is necessary only to fill the channel or the perforation holes with a cement filter cake and to allow it to harden in that position. In the past, the presence of mud in a well has been considered the chief deterrent to obtaining a good cement bond and satisfactory cement job; however, late developments in squeeze-cementing have made it possible to eliminate cement contamination or interference. Since it is possible to form a cement filter cake with a small pressure differential, squeeze-cementing with high pressures may not be necessary in most cases. The amount of cement needed to fill the annulus about the casing and even to fill part of the casing, if necessary, is generally small in quantity. Use of low squeeze-cementing pressures and small quantities of cement provides the following advantages: 1. Longer effective life of well tubing, casing, and other equipment; and less chance of costly equipment failure due to excessive pressure. 2. Monetary savings effected by elimination of retainers and specal squeeze-cementing tools. 3. Monetary savings effected by use of small quantities of cement and fewer squeeze-cementing operations. 4. Future surface squeeze-cementing equipment may be smaller and more economical to operate and maintain.

Jan 1, 1955

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.' Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By Gerhard Derge

Metallurgists have used borax as a fluxing agent traditionally, but until recently elemental boron has played an insignificant role as an alloying element. Neither the metal nor its compounds have been regarded as important metallurgical materials and there is a surprising lack of knowledge concerning their metallurgical behavior. The new applications to steel-making of both boron and borates, which arose in part from wartime incentives and restrictions, have been seriously handicapped by this lack of data. For example, rasorite, a naturally occurring sodium borate, has been shown to be an effective substitute for aluminum as a ladle deoxi-dizer in rimming steels.' Likewise, the effectiveness of boron as an alloying agent has been demonstrated,2,3 giving deep hardening when used in restricted amounts. The exploitation of both of these uses has been retarded by the difficulty of attaining suitable metallurgical control. Recognizing that the most important information required was a knowledge of the equilibrium between boron and oxygen dissolved in liquid iron. Gurry4 calculated this relation from the best thermal data available. However, estimates of the entropy of melting of boron, the activity coefficient of boron in liquid iron and the activity coefficient of B2O3 in slag were involved, and experimental work on this problem was obviously desirable. The experiments to be described were planned to establish the boron-oxygen relations in liquid iron and to demonstrate at the same time the ferroborate slag compositions in equilibrium with various amounts of oxygen in liquid iron. Accordingly, slags containing varying proportions of iron and boron oxides were held in contact with molten iron, and samples of both slag and metal were analyzed. The limitations upon the accuracy of the data will be considered, but in a practical sense the oxygen levels that can be attained in iron by iron borate slags, and the amounts of boron in iron at these oxygen levels were established. Experimental Procedure No entirely suitable refractory was found for the mixtures of iron oxide and boron oxide used as slags. Crucibles of silica, magnesia, Ramix, beryllia, and zirconia were all tried unsuccessfully. The must satisfactory method discovered for handling them was the rotating-crucible technique, which creates a parabolic crucible of liquid iron.5,6 Even this was not entirely successful, for at steelmaking temperatures (1600°C.) the slags had such a low surface tension that they crept up to the refractory and slowly dissolved it. These difficulties made it impossible to maintain a constant slag composition for an unlimited period Of time. However, by using the rotating technique, short runs could be made in

Jan 1, 1947

By M. Cohen, W. J. Harris

The recent application of lineal analysislt2 to the austenite-martensite reaction has made possible a quantitative study of the kinetics of this transformation during rapid cooling. Martensite range curves can thus be constructed to portray the onset of the reaction at Ma and its subsequent progress as a function of temperature down to and below the ambient. It now seems in order to investigate other aspects of the martensite transformation, using this quantitative method of approach. One of the least understood characteristics of the austenite-martensite reaction is that of stabilization which has been defined by Troiano and Greninger3 as 'la lowering of Ma, resulting from aging, without change in chemical composition of the parent solid solution." In other words, if the hardening quench is arrested at a predetermined subcritical temperature (TA) for a sufficient period of time, more austenite may be retained at a given lower Or reference temperature (Tr) than if the steel had been cooled directly and rapidly to Tr in the first place. For the purposes of the work at hand, the extent of stabilization produced by the isothermal treatment at Th is measured explicitly in terms of the excess austenite (6) that exists in the steel at T,, over and above the amount that is normally present after direct quenching to T,. T, is conveniently taken to be room temperature, but this choice is not essential and is sometimes undesirable. The holding temperature (TA) may be above or below M,, and still cause stabilization depending upon the themistry of the austenite. stabilization has been found to occur in the presence of bainite4 and of martensite6,6,7,8 as well as in the absence of either,g The phe-nomenon of stabilization is not concerned with (and may even be obscured by) ferrite formation or any other type of phase change occurring at T~ that alters the chemistry of the remaining austenite. Such a structural change would obviously influence the martensite transformation during subscquent cooling. Stabilization, however, is more subtle; it appears to manifest itself without detectable variation of the austenite composition, whether in the presence or absence of transformation products. There are relatively few direct references to stabilization in the literature. The stabilizing effect of room temperature aging and tempering on the subzero transformation of retained austenite has been clearly shown in plain carbon,6,8 low alloy6s7.8 and high alloy tool steels.10'5 ssa- with the as-hardened steel, the degree of stabilization increases with tempering time and temperature through

Jan 1, 1949

By Claude Froger

The compared advantages of digital and analogue computers for solving ventilation problems have for many years been a matter of discussion among the specialists whose respective arguments have prevailed in turn depending on the progress of technology. In the French coal mines however none of these two techniques has superseded the other so far. In France, between 1956 and 1962 only the digital computer and from 1962 to 1967 only the analogue computer was used. Since then they are both used concurrently and complementarily. Depending on the problems dealt with, the most advantageous method is chosen in each case. In the case of ventilation planning for projected workings, it is possible to test variant forms of the development plans and many parameters can be varied. In such a case the flexibility of the analogue computer is a great help. Wrong lines taken will be rapidly abandoned and little by little solutions will be found. By examining the results of a test, new ideas will generally come into the mind and they can be tested right away. Such an investigation is always-carried out in conjunction with the engineers of the mine concerned. In complex networks it often leads to solu¬tions which could not have been devised from the start. The same work could be done by using a numerical method and the digital computers operating in the different coal mine districts, but for the same tests, the time required would be much longer and the participants would not be encouraged to use their imagination so intensively. Or the other hand for calculations of ventilation networks in ventilation surveying, use is made of the digital computer which gives the possibility of storing the data corresponding to the different mines concerned. The questions to be solved concern problems for which the ventilation network is essentially known, and in which only a small number of parameters can be varied. The few possible alternatives to be calculated can therefore be handled by the digital computer in spite of the relative lack of flexibility of the method. To sum up our ventilation studies are conducted in France as follows: - For ventilation studies and modifications due to projected workings use is made of the ana¬logue computer. For a given mine the updating of such ventilation studies is carried out every 3 or 5 years according to the progression of the workings. - For ventilation surveying while normal working operations are in progress, use is made of the digital computer.

Jan 1, 1980

By Stephen C. Tadolini, Thomas M. Barczak

An underground investigation was designed and implemented by the National Institute for Occupational Safety and Health (NIOSH) to evaluate the effectiveness of pre-driven longwall recovery rooms supported with pumpable concrete roof supports. The pumpable roof supports were instrumented with hydraulic pressure cells to measure support loading. Displacement of the support was also measured to assess the support reaction to ground movements. Movement up to 12.5 m (40 ft) into the roof was measured with sonic probes and multipoint extensometers. Borehole pressure cells were installed in the panel fender and outby pillars to evaluate load transfer. Shield loading was also assessed to determine the impact of the panel fender yielding on face loading. The results show that the yielding of the panel fender produced uncontrollable convergence that caused yielding of the shields and stiff pumpable roof supports when the face was approximately 3.12 m (10 ft) from the recovery room. The shields continued to yield until the face advanced into the recovery room. Convergence in the pre-driven recovery room typically reached 15-20 cm (6-8 inches) once the pumpable supports yielded and shed load through a declining residual load capacity prior to being cut out by the longwall shearer. Roof deformations occurred beyond the 10 m (32 ft) horizon with total deformation ranging from five to 10 cm (2 to 4 inches), indicating that standing support was necessary to help control the span as the longwall face advanced into the pre-driven recovery room. Stability improved as the pumpable supports were cut out, thereby reducing the span between the shields and the outby pillars. In the end, the shields were successfully recovered under stable ground conditions. However, a disconcerting discovery was the load shedding of the outby pillars as the recovery room was mined into. This behavior was not expected with a relatively narrow room that is fully supported with standing support. If this mechanism is indeed occurring, the width of the room and performance of the standing support becomes even more critical. Premature failure of the support can lead to excessive convergence on the shield line that cannot be controlled even with modern shields, resulting in instabilities that can lead to catastrophic results. Understanding the load transfer mechanics associated with the advancement of the longwall face into the pre-driven recovery room and the widening of the room to recover the longwall shields is providing valuable information for the refinement of the NIOSH Ground Reaction Curve for standing and intrinsic roof support system design.

By W. H. Ashby, R. W. Cassingham, C. R. Blomberg, J. B. Justins

The Brookhaven field is one of several Basal Tuscaloosa reservoirs located in south-central Mississippi. It is a standstone reservoir, of erratic deposition and with several faults, having an approximate subsea depth of 9,800 ft. A large variation in permeability exists with a weighted average being 256 md. Estimated average interstitial water saturation is 45 per cent. The undersaturated reservoir fluid exhibits marked differences in physical properties with measured saturation pressures ranging from 733 to 2,255 psi. Early rapid decline in reservoir pressure caused the operating interests to unitize the field and initiate a program of pressure maintenance by gas injection. At the time gas injection was commenced, the reservoir pressure had fallen to nearly half of the original pressure with only 4.5 Per cent of the original oil in place produced. The reservoir pressure has since been maintained at approximately 2,750 psig, and cumulative production to date is 17 per cent of original oil in place. An analysis of field performance during gas injection is presented in detail. The program of pressure maintenance by gas injection is considered to be a success, since the expected ultimate recovery has been increased and the current production rate is in excess of 2 per cent of original oil in place per year. Performance has been better, anticipated ultimate recovery is larger, and total production costs are lower than for a similar Basal Tuscaloosa reservoir nearby, even though that field appears to have a more effective natural water drive. INTRODUCTION The history of the Brookhaven Unit is a testimonial for unitization and for the application of engineering techniques in the operation of an oil field. The operating and royalty interests in this field have mutually benefited from their early recognition of the need for unitization and pressure maintenance and from the forthright manner in which these were accomplished. The tangible benefits accruing to the participants in the Unit are: (1) income from gasoline plant products, (2) reduced lifting and operating costs from those of competitive operation, (3) maintenance of high levels of current income by mitigation of the inevitable decline in production rates inherent to natural depletion, (4) an increase in ultimate recovery of about 40 per cent over natural depletion operations. This paper should properly be considered a progress report; however, the performance of the field after five years of pressure maintenance clearly indicates that the ultimate success of the project is assured. LOCATION AND GEOLOGY The Brookhaven field is located in south-central Mississippi, about six miles from the town of Brookhaven. Production at Brookhaven

Jan 1, 1955

By T. Crivits, I. Bellemans, V. Cnockaert, K. Verbeken

It is well known that slag foaming can significantly complicate copper smelting processes. This is especially true for unpredictable events that generate large amounts of slag foam during a small period of time. These events are here referred to as eruptions and are typical for certain types of liquid bath furnaces such as modern top submerged lance (TSL) furnaces. A few authors already made the link between over- oxidation of the slag phase and slag foaming. In this work, the mechanism is studied in more detail and explained using the smelter chemistry and the behaviour of dynamic foam formation. Finally, the most influential parameters on the foaming behaviour of the process are presented. INTRODUCTION Copper remains one of the most important metals used in our modern society. In 2017, the annual amount of copper produced worldwide was about 23.5 million metric tons. This makes copper the third most produced metal in the world after steel and aluminium. The majority of this copper was produced by copper smelting, about 19 million metric tons, both from primary concentrate and secondary feed material as reported in ICSG’s World Copper Factbook 2018. In the past, copper smelting was mainly performed using Flash smelting, a technology developed before 1949 (Kojo, Jokilaakso & Hanniala, 2000). Nowadays, this type of smelter is being complemented by other smelter types such as ISASMELT and Ausmelt technologies. These are two types op smelter furnaces, based on the concept of a top submerged lance (TSL) furnace. These two technologies were both commercialized around 1990 (Arthur & Hunt, 2005). It is estimated by Wang et al. (2016) that at this time, both flash and TSL smelters contribute equally to the total amount of annually smelted copper. Flash smelting stays the most important technology for extracting copper from primary sources. TSL furnaces, on the other hand, are more suited than Flash smelters for the recovery of copper from secondary materials. This is because of the different ways that the feed material is inserted in both furnaces. In Flash smelters, the ore and fluxes needs to be fine and completely dry in order to be able to blow the mixture inside the burner area of the furnace. The feed material for TSL smelters show less constrains concerning humidity and particle size. The material is dropped from the top inside the molten bath. As a result, a more complex and flexible feed stream can be processed using TSL smelting (Wood, Hoang & Hughes, 2017). This feature will become more important in the future as primary copper sources gets more scarce and the need for a fully sustainable material cycle increases.

Jan 1, 2019

By M. Oliazadeh, A. Vazirizadeh

"The inclusion of small amounts of silicon, phosphorus and sulphur in iron ores or concentrates can have a profound effect on the steel making process and thus on the final iron and steel products. In nature however, it is inevitable that iron deposits contain unwanted elements. Each element has its own distinct effect on the final steel product. The effect of high silicon is the formation of gray iron. Phosphorus mainly increases hardness and strength, lowers solidus temperature and increases fluidity and cold shortness. Finally sulphur contamination causes cracks in the iron texture when smelting and forms white iron when casting. Overall, the acceptable level of phosphorus, sulphur and silica in the iron concentrate should be less than 0.04%, 0.15 % and 1.5 % respectively.Scarcity of high grade iron ores necessitates using lower grade ores with higher amounts of impurities. The purpose of iron concentrators is to increase iron grades to an appropriate level suitable for steel making as well as removing impurities. Although many impurities can be traced in the ore, the most predominant impurities are limited to one or two elements. In this paper the beneficiation methods for removing SiO2, P and S are presented, including flotation, and the parameters that need to be considered in the design of beneficiation plants are discussed. Finally industrial cases are discussed along with their metallurgical performance.INTRODUCTIONIn metal sector, value of iron ores and concentrates is determined by iron percentage as well ascontent of:• Useful elements (Mn, Ni, Cr, V, Ti): natural alloying elements in steel• Deleterious impurities (S, P, As, Zn, Pb, K, Na): impair metal properties or complicate operational process in blast furnace• Fluxing components (Si, Ca, Mg,, Al)Sulphur and copper result in red-short, phosphorus is the cause of cold brittleness and arsenic and copper decrease welding characteristics. Sulphur should not exceed 0.15 in commercial ore. Acceptable sulphur content in ores and concentrates for producing sinter and pellets is 0.6%max, as sintering and heat hardening of pellets remove sulphur 60-90%. Phosphorous content in ores, sinter and pellets is limited to 0.07%-0.15%. 0.00.1% As max, 0.1-0.2% Zn max and up to 0.2% Cu are allowed in iron-ore part of the blast furnace burden for the production of standard conversion pig iron. Slag-forming components are divided into basic oxides (Ca, Mg) and acidic (Si, Al). Higher ratios of basic to acidic oxides are preferred since this reduces raw fluxing material."

Jan 1, 2016

By V. F. Leferrer

A new process for the treatment of silver crusts from desilverization of lead has been developed by Societe de Penarroya. The zinc contained in the crusts is recuperated by vacuum distillation at low temperature. The use of special retort crucibles is avoided. AT Noyelles-Godault the Parkes process (zinc addition to a silver-bearing lead melt) is used to desilverize lead bullion from the blast furnace. The crust which rises to the surface of the bath is removed and pressed by a well-known process in a press of the Howard type. The pressed crust, called zinc crust or silver crust, contains 10 pct Ag, 30 pct Zn, and 60 pct Pb. It is melted under a salt bed in a small, narrow, and deep kettle heated only in its upper part. A liquid concentrated alloy is obtained which is called T.A.C. in France (triple alliage concentr6) analyzing approximately 25 pct Ag, 65 pct Zn, 8 to 10 pct Pb, and 1 to 1.5 pct Cu. This T.A.C. is a real metallic alloy, completely deoxidized, and can be stored indefinitely. The process used at Noyelles-Godault consists in distilling this alloy in a tight furnace, under low vacuum and at low temperature, so that only the zinc distills and is condensed into liquid form. The residual silver-bearing lead is almost entirely free from zinc and oxidized dross. The vacuum dezincing equipment, see Figs. 1 and 2, consists of: 1) A furnace, constituted of a casing of steel plate lined with refractory bricks, heated internally by means of graphite resistors. The temperature of the furnace is measured by a thermocouple device and controlled by an automatic temperature regulator which acts upon the flow of the current passing through the resistors. Two doors, numbered 1 and 2 in Fig. 2, are provided for, one for charging the T.A.C., the other for tapping the high silver-bearing lead. 2) A condenser, and an ordinary room lined with good heat conductor refractory material. This condenser is provided with a graphite resistor which serves to bring to temperature when starting the furnace. A thermocouple records the temperature of the zinc melt and controls the temperature in the furnace, that is, the flow of current through the resistors, by means of the above mentioned regulator, so that the distillation rate in the furnace does not exceed that of the condensation. The condenser is connected to the vacuum pump by a filter. The whole equipment should, of course, be fluid-tight. The operation is carried out under a vacuum of about 10 mm Hg.

Jan 1, 1958

By M. Tang, X. Tong

"SynopsisSlime coating is one of the most common ways for serpentines to contaminate metallic mineral concentrates during traditional flotation of coarse sulphide particles. This could pose quite a complicated and challenging problem in the case of some types of low-grade and finely disseminated Cu-Ni ores bearing high serpentine contents. This is the case for the copper and nickel sulphides from the Yunnan Mine, China. Previous batch flotation tests of this ore resulted in satisfactory recoveries of 86.92% Cu, 54.92% Ni, and 74.73% Pt+Pd, and concentrate grades of 4.02% Cu, 3.24% Ni, and 76.61 g/t Pt+Pd. However, the MgO content in these concentrates was more than 19%. In the current study, microflotation tests and settling rate tests were introduced to investigate the effects of a combination of strong collectors (a 2:1 weight ratio of butyl xanthate and butyl ammonium dithophosphate) on entrainment of serpentines in metallic mineral concentrate, as well as visual observations of the concentrates in suspension using still photography. All test results indicated the presence of serpentines entrapped in the hydrophobic flocs that resulted from these collectors, even with the use of effective gangue depressants. These strong collectors are used to flocculate the ultra-fine sulphides by forming loose and ‘fluffy’ hydrophobic flocs. However, these hydrophobic flocs may also be able to load or entrap some serpentine slimes into the concentrate, and this entrained serpentine could be harder to remove by using depressants or intensified conditioning than serpentine slime coating on the particle surfaces.IntroductionSerpentine minerals, which have the generalized composition (Mg,Fe)3Si2O5(OH)4, can be easy to crush and grind due to their convoluted and bent layered structures. These serpentines can hinder the enrichment of some metallic minerals and dilute their concentrates by entrainment during flotation. The resulting high pulp viscosities, slime coatings, and high content of dissolved ions adversely affect the flotation recoveries of copper and nickel sulphides, and high levels of MgO entrained in the concentrates lead to heavy penalties from smelters. Since the quality of nickel flotation concentrate depends heavily on its MgO content (generally less than 6–7% for No.1 or 2 grade nickel concentrate according to the standard requirement from National Nonferrous Industry), reducing the entrainment of serpentine during flotation is becoming more and more pressing. Previous research has focused on the collectors and depressants that are commonly used in copper-nickel flotation, as well as their interaction mechanisms."

Jan 1, 2015

By K R. Brentley

"Tshepong Mine, Harmony’s largest gold producing mine, is situated in the Free State portion of the Witwatersrand Basin, east of Odendaalsrus and north of Welkom, South Africa. The Basal reef is a narrow tabular conglomerate and is the main gold bearing ore body. The strata strikes mainly in a northsouth direction with an average dip of 22 degrees. Currently mining takes place at depths of between 1 690m and 2 150m below surface. The Basal reef unit consists of a conglomerate ranging between a few and 30cm in thickness. Some 80-90% of the gold occurs in the lower portion of the conglomerate. Directly above the conglomerate is a quartzite placer unit, the Basal quartzite, which is a clean, hard competent rock and varies in thickness between 50cm and 200cm. The Basal unit is overlain by the Khaki shale which can vary between 30cm and 500cm in width. It is weak and incompetent khaki coloured chloritic shale.A method of stoping, termed “undercut”, is practiced in order to remove the lower 15-20cm of the gold rich strata. The method entails removing this portion along with some 70-80cm of footwall host rock which is a strong competent quartzite. The hard competent quartzite overlying the conglomerate is left in-situ to form a competent hangingwall which can stabilize and prevent exposure of the weak Khakishale. This method of extraction was developed through trial and error and has been used reasonably successfully since its inception in the early 1960’s where the method was developed to extract the Basal reef at the Western Holdings Mines. Recently prospect drilling and a number of localised hangingwall failures indicated that the residual quartzite beam could be less than 60cm and in some instances as thin as 30cm in certain areas of the mine. The result of this is a less stable hangingwall which not only poses a safety risk to workers in these areas but also had the potential of locking up some 840 000 Tonnes of gold bearing ore. At the present gold price this amounts to revenue of approximately ZAR1.5 billion (U.S. $143 million).This paper discusses the method of “undercut stoping” and existing practices in place at Tshepong Mine. It also explores new initiatives such as the use of a simple freely-supported elastic beam solution to perform back analysis, on-site data capturing of beam thickness and support geometries in order to develop empirical design charts and numerical modelling to assist in the verification of the empirical design method."

Jan 1, 2015

By M. E. Wadsworth, I. B. Cutler, R. W. Bartlett

The oxidation kinetics of ZrC was studied between 450" and 580°C in oxygen pressures from 6.5 x 10-to 1 atm using a ther mogravimetric apparatus and sized powder samples. Two parallel rate controlling processes were observed. A surface reaction occurring at the ZrC-ZrO2 phase boundary accounted for most of the oxidation and had an activation enthalpy of 46 kcal per mole. The other process, believed to be diffusion of oxygen into the ZrC lattice partially replacing carbon, had an activation enthalpy of 53 kcal per mole. The enthalpy for chemisorption of O2 on ZrC was determined to be —13 kcal per mole. Water vapor in the presence of oxygen accelerated the surface reaction rate. THERE has been little reporting of formal rate studies or attempts to ascertain the mechanism of oxidation of carbides. MacDonald and Ransley1 studied the oxidation of titanium carbide which has the same structure as zirconium carbide, fcc. They observed an initial increase in rate with increasing temperature followed by a rapid decrease through a rate minimum and a subsequent second increase at higher temperatures. The discontinuity in the rate rise was attributed to a phase change in the oxide which changed the rate determining step from the surface reaction at the carbide-oxide interface to diffusion through the oxide layer. Samsonov and Golybera 2 studied titanium carbide and reported that during the initial period of oxidation a dense film of Tic-TiO was formed followed by the formation of less adhering layers of higher oxides. The purpose of this investigation was to study the kinetics of oxidation of zirconium carbide and to attempt to gain some knowledge of the mechanism by which oxidation occurs. EXPERIMENTAL PROCEDURE Measurement of the weight gain associated with the oxidation of ZrC was used to determine oxidation rates. The principal experimental parameters were surface area, temperature, and oxygen pressure. Although moderately sized crystals of ZrC can be grown by the Van Arkel method, the only commercially available ZrC is a powder. In using powders, the surface area must be controlled either by fabricating the powder into a sintered pellet with a measurable surface area, relatively fixed during oxidation, or by using sized unconsolidated powder and applying appropriate geometric considerations to the shape of the grains to correct for their diminishing surface areas as they oxidize. Both techniques involve some difficulties. pellets of binder-free zirconium carbide can be made by hot pressing, but it is difficult to obtain densities greater than 90 pct of

Jan 1, 1963

By Carl F. Floe, Michael B. Bever

TRE solubility of hydrogen in molten copper-tin alloys is of both practical and theoretical interest. From a practical standpoint, data on the equilibrium solubility as a function of temperature, pressure and alloy composition are valuable for a better understanding of porosity problems in bronze castings. From the theoretical point of view the determination of the hydrogen-copper-tin equilibrium is of interest since it extends the laws governing the solution of gases in metals. This paper presents the results of an investigation of the solubility of hydrogen in representative compositions of the copper-tin system at temperatures ranging from above the liquidus to 1300°C. and at pressures from less than 50 mm. of mercury to about atmospheric. REVIEW OF PREVIOUS WORK The solubility of hydrogen in copper was determined by Sieverts and Krumbhaarl in 1910 and by Roentgen and Moeller2 in 1934. Their values are in fair agreement. In 1926 Iwasé3 reported results that were very much higher. The published data on the solubility of hydrogen in tin do not agree. Smithells4 states that no reliable data are available. According to Sieverts and Krumbhaar,5 hydrogen is insoluble in tin. Bircumshaw,6 on the other hand, found a definite solubility at 800°C. The latter's experimental procedure did not provide for stirring of the metal and in his opinion he failed to reach equilibrium. Iwasé3 again reported large solubility values. For copper alloys, Sieverts and Krumbhaar6 distinguished between alloying elements that do not markedly affect the solubility of hydrogen, elements that increase the solubility, and elements that reduce it. They named gold, tin, and aluminum as examples of this last group and reported hydrogen solubility data at 1225°C. for the copper-rich side of these alloy systems at atmospheric pressure. Without giving experimental results, they stated that the amount of hydrogen dissolved by liquid copper alloys is proportional to the square root of the pressure as in pure metals. These authors suggested that in a limited way the effect of an alloying element on the solubility of a gas is related to the constitution diagram for the alloy system. Sieverts7 also called attention to the fact that the curve of hydrogen solubility versus composition of copper-tin alloys shows a sharp change of direction at the composition of Cu3Sn and suggested that this compound persists at least to some extent in the molten state. Iwas3é reported large hydrogen solubility values for several compositions of copper- tin alloys, which appear to be in error.

Jan 1, 1944

By D. B. Jugle, J. B. Darby, O. J. Kleppa

A systematic study has been made of the kinetics of solution under steady state, dynamic conditions of titanium, vanadium, chromium, iron, cobalt, and nickel in liquid aluminum. It was found that the temperature dependence of the solution rate obeyed an Arrhenius-type rate equation, and that at a given temperature the rate of solution of the various solutes correlates quantitatively with the equilibrium solubility of the solute in liquid aluminum. These results are consistent with a mechanism where the rate-controlling step is the diffusion of solute atoms through a liquid boundary layer. THE present study was initially started in order to explore the feasibility of liquid-metal solution calorimetry for transition metals and alloys. Previous work1 in this field employing liquid tin as a solvent at temperatures in the 500' to 600' range had indicated that the rates of solution of most transition metals in tin are very low. Under such conditions effective solution calorimetry is difficult. The objective of the present investigation was two-fold: a) To obtain, as far as possible, quantitative data on the rates of solution of a series of transition elements in liquid aluminum. b) To explore whether liquid aluminum might be a suitable solvent for liquid-metal calorimetry. In the course of this work a comprehensive set of data was obtained on the steady state rates of solution of transition metals in a common liquid-metal solvent. The results are consistent with the boundary layer model, which assumes that the rate-controlling step consists of diffusion of solute atoms through a viscous liquid layer. EXPERIMENTAL PROCEDURE A vacuum-tight stainless steel vessel was surrounded by a resistance furnace, as shown in Fig. 1. In all experiments the temperature of the liquid solvent was controlled to 2.5' by means of a Micromax controller. A high-vacuum manifold connected to the vessel maintained a vacuum of 1 x 105 mm of Hg or better. The vacuum vessel was equipped with a charging section isolated from the working chamber by a vacuum-tight gate valve. This arrangement allowed the specimen holder to be removed or inserted into the apparatus without removal of the liquid metal bath. The specimen holder was suspended from a closed end stainless steel tube, which also served as the thermocouple protection tube. The portion of the tube that was below the solvent level was surrounded by an alumina protection tube to isolate it from the liquid metal bath. The stainless steel tube was connected through a rotary vacuum seal and a gear train to a fractional horsepower motor. For most experiments the tube was rotated at a constant

Jan 1, 1963