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By T. Y. Yan

SUMMARY Laboratory high pressure column tests have shown that the presence of 1-20 ppm of aluminum ion effectively prevents permeability loss during uranium leaching with leachates containing sodium carbonate. If added after permeability loss has occurred, aluminum ion can restore the permeability to nearly its original value. No deleterious effect was observed on uranium leaching performance and the technique should be quite compatible with all field operations. INTRODUCTION The recovery of uranium values from underground deposits by in situ leaching or solution mining has become economically viable and competitive with conventional open pit or underground mining/milling systems (Merrit, 1971). In situ leaching processes are particularly suitable for small, low-grade deposits located in deep formations and dispersed in many thin layers. Many such ore bodies occur along a broad band of the Gulf Coastal Plain (Eargle et. al., 1971). The advantages of the in situ leaching processes have been reviewed (Anderson and Ritchi, 1968). In the in situ leaching process, a lixiviant containing the leaching chemicals is injected into the subterranean deposit and solubilizes uranium as it traverses the ore body. The pregnant lixiviant or leachate is produced from the production well and is then treated to recover the uranium. The resulting barren solution is made up with the leaching chemical to form lixiviant for re-injection. Upon completion of the leaching operation, the formation is contaminated with leaching chemicals and other species made soluble in the leaching operation and has to be treated to reduce the concentration of these contaminants in the ground water to levels acceptable to the regulatory agencies (Witlington and Taylor, 1978). Restoration is accomplished by injecting a restoration fluid, which could be the fresh water or water containing chemicals, into the formation. As it traverses the leached formation, the restoration fluid picks up the contaminants and is then produced at the production well. This produced water is either disposed or purified for recycle. In both phases of operation, formation permeability or well injectivity is one of the most important parameters which determines the viability of the in situ leaching process. Low formation permeability limits production rates, leading to uneconomical operations. The formation is said to be sensitive if there is a sharp loss of permeability on contact with water and other fluids. Many uranium bearing formations, for example, the Catahoula formation of the Texas Coastal Plain, contain significant amounts of clay minerals which are water sensitive. Serious permeability losses can occur when the pH and chemical composition of the lixiviant is significantly different from that of the formation water. Jones has investigated the influence of chemical composition of water on clay blocking of permeability (Jones, 1964) and Mungan studied permeability reduction through changes in pH and salinity of the water (Mungan, 1965). Various mechanisms of permeability damage have been proposed and reviewed (Jones, 1964; Mungan, 1965; Gray and Rex, 1966; and Veley, 1969). When large amounts of swelling clays are present, a significant fraction of the flow channels in the formation can be reduced due to swelling. However, in most cases, swelling need not be the main cause of permeability losses. Particle dispersion and migration or clay sliming can be more important causes for formation damage. Clay particles entrained in the moving fluids are carried downstream until they lodge in pore constrictions. As a result, microscopic filter cakes are formed by these obstructions, plugging the pores, effectively restricting fluid flow and reducing the formation permeability. Moore found that as little as 1-4 percent clays present in a fine grained sandstone could completely plug the formation if they are contacted by incompatible injected fluids (Moore, 1960). It has been found that injection of NaHC03/Na2CO3 lixiviant into formations with significant clay content often leads to loss of formation permeability and well injectivity. To alleviate this problem a change of the lixiviant composition to KHC03/K2CO3 has been proposed. At present, however, many in situ leaching operations employ NH4HC03/(NH4)2C03 mixtures as a source of carbonates. This approach has been successfully used in South Texas by Mobil, Intercontinental Energy, Wyoming Minerals and U.S. Steel, etc. The use of ammonium carbonates solutions, however, contaminates the formation and requires a time-consuming restoration operation. The other approach to reduce the permeability loss is to pretreat the sensitive formation with chemicals which prevent clay dispersion and migration. Such chemicals include hydroxy-aluminum (Reed, 1972 and Coppel et. al., 1973), hydrolyzable zirconium salts (Peters and Stout, 1977), hydrolyzable metal ions in general (Veley, 1969) and polyelectrolyte polymers (Anonymous). Still another approach, is to minimize the "shock" caused by sudden injection by gradually changing the chemical composition of the injected fluids from that of the formation water. THE APPROACH Since permeability loss can be an important factor limiting the efficiency and economic viability of the in situ leaching process, a study was initiated on

Jan 1, 1982

By W. H. Corbould

THE township of Cloncurry is situated in the northwestern part of Queensland, about latitude S. 20° 42' 53" and longitude E: 140° 30' 25". Townsville is the port through which all the trade passes and is about 470 miles east-northeast of Cloncurry township. The Cloncurry copper district covers an area about 200 miles long by 40 miles wide. Unfortunately the mines are very scattered over this area, there being no large groups of mines. Mount Elliott mine is situated about 70 miles south from the township of Cloncurry, and Mount Oxide mine about 150 miles north of Cloncurry. The district has been known for the last 35 years, and in the early stages a large amount of capital was expended with little to show for it; but within the last four years the railway has been extended from Townsville to Mount Elliott and about 40 miles north of Cloncurry, which has made possible the treatment of the ores of the mines on this extension. The Mount Elliott company within the last few years has smelted and converted on its mine 169,688 tons. of ore for 20,554 tons of blister copper, containing 20,377 tons of copper, 35,642 oz. of gold and 28,841 oz. of silver, at a cost of about £33 per ton of blister copper, f.o.b. Townsville. This cost included all ' development, wages, salaries, general management, office, agency, legal expenses, freight, etc. The gold and silver contents would practically pay for freight to Europe, refining, realization charges, etc. The costs of supplies are as follows: Firewood 15s., coke, 75s., mine timber, 54s., and coal, 60s. per long ton; explosives: dynamite and gelignite, 50s. and blasting gelatine, 65s. 6d. per case.

Jan 1, 1915

By F. E. Luborsky, K. T. Aust

RECENT interest has been shown in utilizing solid-state techniques for obtaining large oriented grains in the Alnico Alloys.1-4 Unfortunately, due to the inherent brittleness of these materials it is difficult to introduce sufficient imperfections by deformation to support the nucleation and growth of new, recrystallized grains. As a result, recrystal-lization methods for obtaining large grains, such as the strain-anneal technique, do not appear to be feasible. Steinort et a1.2 used a combination of a thermal gradient and internal strains to obtain large single crystals of Alnico 5 from a poly crystalline casting by annealing at temperatures above 1200°C. It was suggested that the strains were the result of the precipitation of the y phase which exists between -850° and 1200°C. The purpose of the present study was to determine if the grain size of the cast Alnico alloys can be markedly increased by solid state techniques involv-

Jan 1, 1963

By R. M. Hudson

The removal of nitrogen from a nitrogenized low-carbon sheet steel that contained 0.011 wt pct N was determined during heat treatment in Hz-N, mixtures. TIze process followed a first-order rate law; that is, plots of the logarithm of nitrogen content in steel were linear with the time of treatment at a given temperature. The rate of removal increased with an increase in temperature from 900" to 1300°F. By 1400°F the rate in dry hydrogen had decreased to a value intermediate between the rates at 1200" and at 1300°F; in wet (2.47 vol pct water vapor) hydrogen the rate at 1400°F was less than the rate at 1300°F and nearly the same as the rate at 1200OF. The rate at a given temperature increased as the 3/2 power of hydrogen concentration in the atmosphere. While wet atmosplzeres were generally more effective than the corresponding dry atmosplzeres, the effect of water vapor was much less pronounced than the influence of hydrogen content. NITROGEN is the principal agent in the strain aging of ferrite, the effect of carbon being secondary.' To eliminate the return of the yield point after straining and aging, it is claimed2 that the amount of nitrogen in solution in steel must be reduced to 0.0002 wt pct. Strong nitride-forming elements (titanium, vanadium, zirconium, and aluminum) can act to eliminate strain aging by combining with nitrogen. It is extremely difficult to decrease the nitrogen content in commercial steels to the low level required by conventional coil annealing because of the poor contact between the strip surface and the reactive atmosphere. However, a variety of gas-metal reactions can be effected by use of the open-coil annealing method,3 in which the metal surface is fully exposed to the atmosphere. With this possibility in mind, the Applied Research Laboratory has studied the influence of time, temperature, and atmosphere composition on the removal of nitrogen from low-carbon sheet steel. MATERIALS AND EXPERIMENTAL WORK Samples from a commercial nitrogenized low-carbon steel (0.010 in. thick) in the cold-reduced condition were used. The chemical composition of this steel is given in Table I. The gas mixtures used are listed in Table 11. The moisture content in the "wet" annealing atmospheres was controlled at a +70°F dew point (2.47 vol pct water vapor) by passing the gas mixture through a glass tube packed with a solid mixture of 10 pct anhydrous oxalic acid and 90 pct oxalic acid dihydrate held at 127°F; this technique has been described previously.4 For "dry" atmospheres, the gas mixtures were passed through a cold trap immersed in liquid nitrogen. A hinged-top Hevi-Duty electric furnace was used with a Vycor-glass furnace tube. When the furnace was at the desired temperature, the gas mixture was passed through the furnace at a flow rate between 1.1 and 1.2 cfh; coupons (size 3 by 3/4 in.) of the steel were pulled into the center of the Vycor-glass

Jan 1, 1964

By Kiyoshi Azuma, Hiroshi Kametani

The variation of the dissolution behavior of a ferric oxide with calcining temperature has been investigated. Samples were prepared by thermal decomposition of ferric hydroxide, nitrate, oxalate, and sulfate at low temperature, followed by the calcination in the temperature range between 600" and 1200°C. The samples of eight series and a fine crystalline sample of hematite were dissolved in 1 N hydrochloric acid at 55.2°C and the results are represented on double-log graphs for convenience. It is confirmed that all dissolution courses follouj either the accelerated process or the parabolic process except in the special case of the crystalline hematite which dissolced in accordance with the uniform dissolution of a particle. Examinations of the physical properties of the oxide powders revealed that the surface area measured by the permeability method is strikingly relevant to the dissolution behavior of the oxide. In the previous paper,' detailed data were presented on the effect of the kind of acid, the solution temperature, and the concentration of acid on the dissolution of two ferric oxides. It was also shown that these sam ples dissolved in strikingly different ways. The present investigation was carried out on the dissolution of various calcined samples prepared from various ferri salts by various methods to ascertain the course of dissolution. Pryor and Evans2 pointed out a change of the dissolution rate at around 700°C for a series of calcined ferric oxides prepared from the hydroxide. Several papers374 reported also the dissolution of ferric oxide samples. It seems, however, that a systematic account of the relationship between the dissolution behavior and physical properties of the oxide has not yet been given. This paper presents the variation of the dissolution of the oxide in relation to the calcining temperature and the change of physical properties of the calcines. EXPERIMENTAL Raw materials were prepared by precalcination of ferric hydroxide, thermal decomposition of ferric nitrate, oxalate, and sulfate, and aerial oxidation of ferric chloride vapor, at as low a temperature as possible. The products were crushed, ground, if necessary, and sieved with a 100-mesh Tylor screen prior to calcination, after which the specimens were dissolved in acid solution. The following is a detailed description of the preparation of the samples. Sample H. About 500 g of ferric chloride (guaranteed reagent) were dissolved in 5 liters of deionized water and filtered. Ferric hydroxide was precipitated by addition of the minimum amount of ammonium hydroxide solution, and the precipitate was washed continuously till chloride ion was not detected by silver nitrate solution, and then filtered. The filter cake was dried at 120°C for a week and ground, and the -100 mesh portion was used. Sample S. Ferric sulfate (guaranteed reagent) was pyrolytically decomposed in a crucible at 700°C for 24 hr and the product was sieved. In this case the following calcination was carried out at temperatures over 700°C. Sample B. Commercial ferric oxide (guaranteed reagent). About 15 kg of ferric nitrate were decomposed in a furnace maintained at 800°C for 2 hr. The actual temperature of the decomposition was not measured. The product was crushed and sieved, and the -100 mesh portion was used. Sample N. About 50 g of ferric nitrate (guaranteed reagent) were decomposed in a beaker in a sand bath until a red-brown dense solid was produced. This product was crushed and sieved, and subjected to complete decomposition at 500°C. The precalcined product was again sieved and used. Sample N2.5. Since the decomposition temperature was not controlled for sample AT, a different sample was prepared in a temperature-controlled furnace. The subscript represents the decomposition at 250°C. The product was treated in the same manner as sample N. Sample Nc. Under atmospheric pressure it is prac-tically inevitable that ferric nitrate hydrate melts to form a brown liquid at about 50°C before pyrolysis. For this reason, the salt was first slowly heated under reduced pressure (about 10-3 mm Hg measured in a trap refrigerated by dry ice-alcohol) to achieve dehydration without melting. About 5 hr were required for the dehydration and the partial decomposition. Then the temperature was elevated to 500° C in air for complete decomposition. The relatively porous product was sieved and used. Sample Ov. About 200 g of ferric oxalate hydrate (extra pure) were dehydrated under reduced pressure (as described above) followed by thermal decomposition at 500°C for 6 hr in air. The decomposition of this salt was accompanied by liberation of carbon monoxide, by which the ferric salt was initially reduced to a black powder. The powder changed in turn into brown ferric oxide as the gas liberation decreased and reoxidation predominated. The product consisted of sparkling fine particles passing through a 100-mesh screen. However it was ground and sieved as for the other samples. Sample D. Commercial fine powder for magnetic tape purposes. The preparation was as follows.5 Ferric chloride vapor and preheated excess air were mixed and passed into a reaction tube where oxidation took place at 450°C. The fine powder formed was collected in a cottrell chamber. The product was vacuum-degassed at 450°C for 1 hr and sieved.

Jan 1, 1969

By H. H. Waller, D. L. Monroe, D. P. R. Smyth

ORIGINALLY slusher drift development was conventional, advancing the drift full 10x13-ft size at 6 ft per round. This proved dangerous and costly because the weak fractured rock of the orebody cannot be left raw for any length of time without its reacting with air to cause spalling. With this method of drift development ground conditions were worsened by many blasts and the length of time it was necessary for the drift to remain open. The problem was practically solved by driving 5x7-ft pilot drifts, then enlarging to 10x13-ft raw size by slashing with 50 to 60-ft diamond drill holes. Calculated explosive charges are used to avoid wall and roof shattering. Still more recently jacklegs and sectional steel replaced the diamond drills, resulting in the same work for less than half the cost, see Figs. 1 and 2. Crosscuts at right angles to the main haulage drifts, which cross through the center of the ore-body, divide the ore into 200-ft blocks. Eight slusher drifts on 50-ft centers draw from one block. The slusher floor is 11 ft above the rail, inclined at 1 pct grade, and the top is 18 ft below the undercut. The finished slusher drift is 102.5 or 120 ft long, depending on whether it is north or south of the crosscut. Drawpoints are staggered on each side at 17.5-ft centers. The completed drift is concreted and has an inclined ramp and a vent at the back. When crosscuts and gangways have been excavated and concreted and slusher stations installed, slusher drift development is carried out in 10 clear-cut stages: 1—Pilot drift is driven full length, 5x7 ft. 2—Station is excavated at half-way point in pilot drift. 3—Pilot drift is enlarged to slusher drift size by drilling. 4—Lower part of slash is blasted and mucked for floor concrete. 5—Floor is poured. 6—Inside upper half of slusher drift is blasted, mucked, and concreted. 7—Outside upper half of slusher drift is blasted, mucked, and concreted. 8—Drawpoints are excavated. 9—Drawpoints are concreted. 10—Concrete ramp and sheave protection recess are constructed at back end of slusher drift. A 5x7-ft pilot drift is driven full length on the center line of the proposed slusher drift using a jackleg and detachable bits on 7/8-in. hexagon steel. A 10-hp air-driven slusher and 36-in. scraper pull muck directly into cars in the main haulage crosscut, see Fig. 2. Operations are on a three-shift basis. One man mucks the previous round, drills, and blasts his round in a shift. Average advance is 5 ft per shift. When the pilot drift is completed, 7 ft of drift in the center section is enlarged to full raw slusher drift size of 10x13 ft, for the set-up to drill long slash holes. The pilot drift is slashed to full raw size from this station with jacklegs and tungsten carbide chisel bits on 7/8-in. sectional steel. Crews line the holes without trouble, working from controls established by the engineers, and the pattern of holes for the slash is arranged to give the least shattering effect

Jan 1, 1955

By W. Hume-Rothery

RECENT interest has been shown in utilizing solid-state techniques for obtaining large oriented grains in the Alnico Alloys.1-4 Unfortunately, due to the inherent brittleness of these materials it is difficult to introduce sufficient imperfections by deformation to support the nucleation and growth of new, recrystallized grains. As a result, recrystal-lization methods for obtaining large grains, such as the strain-anneal technique, do not appear to be feasible. Steinort et a1.2 used a combination of a thermal gradient and internal strains to obtain large single crystals of Alnico 5 from a poly crystalline casting by annealing at temperatures above 1200°C. It was suggested that the strains were the result of the precipitation of the y phase which exists between -850° and 1200°C. The purpose of the present study was to determine if the grain size of the cast Alnico alloys can be markedly increased by solid state techniques involv-

Jan 1, 1963

By E. A. G. Colls

IN all branches of the chemical industry, corrosion plays a very costly part unless it is suitably com-batted, and as a result it is probably correct that chemical and design engineers are more corrosion conscious in the field of chemical industry than in others. Most metals occur in nature in combination with other elements. The refined or reduced state to which man converts them for his use, by removing the combining elements, leaves them in an unstable condition. Therefore in most of the media to which the metals are exposed they are constantly combining with the constituents of their environment, or in other words they are continually being corroded. Similarly, nonmetallic materials are corroded by undergoing chemical change. The rate at which corrosion takes place varies widely from metal to metal and medium to medium. In practically all cases the corrosion of metals in solutions (electrolytes) is electrolytic in nature and the rate of corrosion is dependent on many factors such as temperature, pressure, internal stresses, galvanic action, metal-ion concentration, and so on. In the chemical industry substances must be handled which are particularly corrosive to materials of construction. At the chemical plants of The Consolidated Mining and Smelting Co. of Canada, Ltd. (otherwise known as Cominco), situated at Trail, B. C., Canada, the following are some of the materials that have to be handled: Gases. Sulphur dioxide, sulphur trioxide, carbon dioxide, carbon monoxide, oxygen, hydrogen fluoride, ammonia, hydrogen sulphide, and oxides of nitrogen. Liquids. Solutions of ammonium sulphate, ammonium sulphite, ammonium nitrate, caustic soda and potash, sulphuric acid, nitric acid, hydrofluo-silicic acid, hydrofluoric acid, phosphoric acid, aqua ammonia, and formic acid. Solids. Gypsum (containing phosphoric acid), ammonium sulphate, ammonium nitrate, phosphate rock, caustic soda, potash, and phosphate fertilizers.

Jan 1, 1951

By E. A. G. Colls

IN all branches of the chemical industry, corrosion plays a very costly part unless it is suitably com-batted, and as a result it is probably correct that chemical and design engineers are more corrosion conscious in the field of chemical industry than in others. Most metals occur in nature in combination with other elements. The refined or reduced state to which man converts them for his use, by removing the combining elements, leaves them in an unstable condition. Therefore in most of the media to which the metals are exposed they are constantly combining with the constituents of their environment, or in other words they are continually being corroded. Similarly, nonmetallic materials are corroded by undergoing chemical change. The rate at which corrosion takes place varies widely from metal to metal and medium to medium. In practically all cases the corrosion of metals in solutions (electrolytes) is electrolytic in nature and the rate of corrosion is dependent on many factors such as temperature, pressure, internal stresses, galvanic action, metal-ion concentration, and so on. In the chemical industry substances must be handled which are particularly corrosive to materials of construction. At the chemical plants of The Consolidated Mining and Smelting Co. of Canada, Ltd. (otherwise known as Cominco), situated at Trail, B. C., Canada, the following are some of the materials that have to be handled: Gases. Sulphur dioxide, sulphur trioxide, carbon dioxide, carbon monoxide, oxygen, hydrogen fluoride, ammonia, hydrogen sulphide, and oxides of nitrogen. Liquids. Solutions of ammonium sulphate, ammonium sulphite, ammonium nitrate, caustic soda and potash, sulphuric acid, nitric acid, hydrofluo-silicic acid, hydrofluoric acid, phosphoric acid, aqua ammonia, and formic acid. Solids. Gypsum (containing phosphoric acid), ammonium sulphate, ammonium nitrate, phosphate rock, caustic soda, potash, and phosphate fertilizers.

Jan 1, 1951

By V. C. Rogers

ALTHOUGH surveying at mining properties is fundamentally the same regardless of the method of mining, at Climax, due to the nature of the ground, the policy of advance development work, and extremes in climatic conditions, surveying practice has had to be revised to meet the specialized conditions of this particular type of mining operation. The company's mine is one of the largest underground properties in the United States. It has proved ore reserves of 275,000,000 tons, 60,000,000 tons of which have been broken. To date, 109,000 ft. of development drifting have been driven, as well as 40,926 ft. of development raising, 10,000 ft. of ventilation drifting and raising, 16,000 ft. of exploration drifting, and 206,000 ft. of diamond drilling. Normal production varies between 1.2,000 and 15,000 tons daily. Development work proceeds at a rate of 11/2 tons developed for every ton milled and with a development of 18,000 to 20,000 tons per day, the following crew is required to take care of mine and surface engineering

Jan 1, 1946

By Luis Toron, Salvador Cortes-Obregon

THE Oaxaca coal fields, shown in Fig. 1, are located in the Alta Mixteca region in the states of Oaxaca, Puebla, and Guerrero. Known out crops are scattered over 3125 square miles. It is probable that further exploration will reveal a more extensive area of deposits. The region is of great importance to Mexico, as at present the only sources of coal are the fields near the U. S. border. Steel mills are also located in the North, and finished products must travel 600 to 800 miles to the area of consumption in central Mexico. The Oaxaca coal, only 120 miles south of Mexico, D.F., lies close to several iron ore deposits. If this coal can be used in steel production is will be possible for the Mexican steel industry to reach new dimensions, commensurate with the growing industry of the central region. Coal can be utilized in thermoelectric plants in this area, which lacks not only petroleum and natural gas but also electric power. It can be used as domestic fuel, replacing charcoal and firewood.

Jan 5, 1954

By George S. Rice

MECHANIZATION in coal mining is a phrase which has attracted world-wide attention, and those persons not engaged on the practical side of coal-mine operations seem to regard mechanization as a panacea for many difficulties of the industry. The term "mechanization" as now employed by experienced mining men is restricted to mean mechanical loading of coal at the face. In a broader sense mechanization in coal mining was begun nearly half a century ago with the introduction of compressed-air undercutting machines and locomotives and, later, of electrically operated locomotives, undercutting and shearing machines, and drills. The use of coal-cutting machines, which has increased until now about three- fourths of the bituminous coal produced is being mechanically cut, first displaced hand-picking except in a few long-wall mines, and later gradually displaced the dangerous and coal-smashing method of blasting-off- the-solid.

Jan 1, 1929

By J. Spreadborough, D. LaW. King, E. Anderson

Tmzsile tests were performed on Armco iron samples, at various ternpe.ralures and strain rates, ocer a wide range of grain sizes. Analysis of the data suggests that the plot of the lower yield stress, against d-1/2,where 2d is the acerage grain diameter, is not linear (as is often assumed) but is concave toward the d. axis over the range of d-from 7 to 53 . The different values of the parameters obtained by other workers can be explained, in part at least, by the observed curvature. This curvalure is shown to be consistent with a model of yielding based on dislocation pile-ups; however, the values of obtained by fitting our data to this model differ appreciably from the values generally reported. The equation proposed by Cottrell, viz.: is a plausible empirical fit to the experimental results. The purpose of this paper is to comment on the validity of the widely used linear relationship first proposed by all' and Petch and coworkers2"4 between ay, the lower yield stress, and 2d, the average grain diameter, for bcc metals, viz.: Many workers, see Refs. 2 to 7 and Table 11, have fitted this equation to their experimental results and have obtained acceptable fits over the relatively narrow range of grain sizes used by most of them. Indeed, in some cases, so few data points were available that any more sophisticated fit would have been irrational. In most of the interpretations,'-' oi is thought to be a measure of the friction stress accompanying dislocation movement, and ky was originally inter- preted as a measure of the dislocation locking but is now believed by Cottrell" to be a function of the dislocation creation rate. In the "unpinning" theories, k, is equated to where od is the unpinning stress and 1 is the average distance from the boundary of the grain where yielding is taking place to the nearest dislocation source in an unyielded grain. Other considerations (see, for example, Refs. 11 and 12) lead to equations with a similar form to [I] where different meanings may be attributed to the parameters. While there are doubts as to the physical significance of the parameters i and k, they continue to be used by many workers; interpretations of the variations in the behavior of ferrite materials following certain treatments, e.g., aging,'3 neutron irradiation,14 have been given frequently in terms of these parameters. Some theories of the mechanical behavior of bcc metals are based on this relationship. We have investigated experimentally the oy - d-'lZ relationship for Armco iron over a wider range of grain sizes and with more data points than those given in published results. The analysis of our data suggests that the oy—d-'" relationship is not linear but is in fact concave towards the d-'I2 axis. RESULTS AND DISCUSSION The experimental work was carried out on 3-mm-diam Armco iron rods which were prepared by wire drawing from 5-mm-diam rods. By annealing in vacuum at temperatures between 7000 and 1200°C for various times, grain sizes from 7 to 20,000 grains per sq mm were obtained, the grains in all cases being regularly shaped. Grain sizes were measured by lineal interceptand by area methods; only specimens with Amax/A values of 3 to 6 were used in the Petch-Hall plots (where A is the average area of a grain and Amax is the area of the largest grain observed). For all the specimens used, the number of grains in a cross section exceeded 50, which should be adequate to avoid grain size effects.'= Tensile tests were performed at 296", 219, and 17l°K, using

Jan 1, 1969

By Byron W. Cheever

While engaged in experimenting with the usual methods for estimating phosphorus in iron and steel, it occurred to me that potassium chlorate might be used to oxidize the carbon, and thus avoid the tedious and vexatious evaporations necessary for successfully carrying out the usual methods. After many trials, the following plan was adopted : Take, for analysis, of Bessemer or other low-carbon steels, from 3 to 5 grammes; of crucible steel, 10 grammes; of pig-iron, 1 to 5 grammes, according to the percentage of phosphorus supposed to be present. Of iron, high in phosphorus (1 per cent.), take 1 gramme. Place in a No. 4 evaporating dish the amount of iron or steel decided upon, cover with a funnel which will just fit inside the dish, and then add gradually HNO3, (1.20 specific gravity), using 12 C.C. of acid for each gramme of steel or iron taken. (A larger quantity of acid will be required for small samples.) When the full amount of acid has been added, and the violent action has ceased, place the evaporating dish on a sand-bath, add 10 C.C. HNO3, (1.40 specific gravity), and boil till the bulk of the solution is reduced about onehalf. Then add 10 C.C. HNO3, (1.40 specific gravity), continue the boiling, and add from time to time, during the next 15 minutes, small portions of pulverized KCIO3, till about 2 grammes have been added. (If the solution shows signs of going dry, more strong acid must be added.) This will precipitate the manganese, with some iron. Sometimes it happens that the manganese does not come down readily, and more KCIO3, or further concentration, or both, will be required. The process is not complete till the manganese is precipitated, which may be known by the appearance of a dark, mirror-like deposit on the dish, at the edge of the solution. Boil the solution 5 minutes after the last addition of KCIO3, and then add cautiously (to prevent sudden explosions) 5 C.C. strong HCl. This will dissolve the precipitated manganese and iron. Continue the boiling till the chlorine is all expelled, adding from

Jan 1, 1885

By Elmer Weber, W. M. Baldwin

Solid lead obeys a single parabolic weight increase vs. time law. In contrast, liquid lead undergoes three successive parabolic weight increases vs. time laws, the first of which has a low constant relative to the latter two. The conversion times for the change from one parabola to the next decrease with increasing temperature. IN recent reports on the subject,1,2 it was noted that zirconium and titanium scale in air by a complex mechanism. The scale first forming on the metal is protective to the extent that it gives a low constant, K, for Tammann's, and Pilling and Bedworth's parabolic equation: w² = Kt [1] relating weight increase, w, due to chemical reaction of the metal with the air, and time, t. After hundreds of hours of apparent stability in some cases the first scale yields to another that offers little protection to the metal. This transition from one scale to another, from a slow parabolic oxidation reaction to a fast one, was not due to impurities in the atmosphere or incidental effects (changing environment, etc.) but was a specific behavior of the metal itself, the transition occurring at definite times (dependent on temperature) and showing other reproducible traits. In view of this behavior how can long-time service behavior be predicted from short-time laboratory tests, not only in the case of these metals, but in any case? Certainly a systematic study of the type of scaling behavior described above—wherever it is found—would help to answer this question. The present paper is a report on the behavior as it is found in lead—the only metal to the authors' knowledge for which the behavior has been described at all, if inadequately, for our present purpose.* At least four oxides of lead are known, of which one occurs in two allotropic forms. They are ß (red) tetragonal PbO stable up to 486°C;8 a (yellow) orthorhombic PbO stable from 486°C up to its dissociation temperature in air at about 2300°C;9 minium or Pb3O4 which from the dissociation pressure data given in Fig. 1 decomposes to PbO at 540°C in air; lead sesquioxide or Pb2O3,; and lead dioxide or PbO2 which, according to Fig. 1, decomposes in air at 400°C to minium. In view of the high dissociation temperature of PbO, lead will scale up to at least its boiling point. Further, it is known that oxygen is almost insoluble in liquid lead.'V his implies a fair probability that an oxide scale would not dissolve in the molten metal and would afford the same protection to lead in the liquid state as in the solid. All of the oxides of lead for which specific gravity data are available are more voluminous than an equivalent weight of metal or a lower oxide from which they might form, hence the scales will be in compression. Lead oxides are known to be ductile, so it would be anticipated that they would form coherent nonporous scales. It is not surprising to learn, then, that both solid and liquid lead scale according to the Tammann, and Pilling and Bed-worth law.14,15 (Gruhl states that at 600°C and above lead oxidizes linearly with time because of "spitting" of the scale.) The parabolic constants K reported by various investigators3,14-16 are badly scattered, however, as shown in Fig. 2. The oxides formed on solid lead were described as being reddish-brown but were not chemically identified by Pilling and Bedworth.15 Gruhl's descripdin³ of the appearance of the scales On his liquid samples indicates that a (yellow orthorhombic) PbO is formed initially on the specimens but gives Way eventually—at least at temperatures below 486 °C— to .ß (red tetraunal) PbO, and that below 540°C minium—Pb3O4 :is firmed at an even later time as an overlay on either the red or yellow PbO. Fig. 3 is a graphical interpretation of Gruhl's description. Gruhl does not indicate any change in the parabolic scaling rate as yellow PbO converts to red. He does indicate that minium reduces the scaling rate, al-

Jan 1, 1953

By G. F. Loughlin

More than 20 years have passed since the publication of Lindgren and Ransome's report on the Cripple Creek District,1 which was made when the district was much more active and prosperous than in recent years. They concluded that the output of the district, which had reached its maximum of about $18,200,000 in 1900, would gradually decline, and their conclusion has been confirmed by records of subsequent production. Between 1905 and 1915 annual declines were partly compensated by encouraging increases, especially in 1908, 1914, and 1915; but a rapid continuous decline followed, due largely to the war and its after-effect's, until in 1922 the value of output was only slightly more than $4,000,000. It rose to nearly $5,000,000 in 1924, but declined again in 1925 and in 1926, when it was about $4,400,000, and represented ores mainly from deep levels in the Cresson and Portland mines. The profitable operations of these two mines were the principal factors leading to a study of ore at deep levels in the district by the U.S. Geological Survey in cooperation with the Colorado Metal Mining Fund. The principal reasons for Lindgren and Ransome's conclusion were three: (I) the greater cost and difficulty of deep exploration; (2) the decrease in the number of veins with increasing depth, and (3) the probability that the telluride ore, believed to have formed at comparatively low temperature, would not persist indefinitely in depth. Operations since they made these statements have verified the first two, but call for some modification of the third. Rich telluride ore is being mined at a profit in the Portland mine 3000 ft. below the present surface, 07. 5000 ft. below the original surface of the Cripple Creek volcano, as interpreted by Lindgren and Ransome. The question arises, therefore, as to the number and extent of such deep deposits, and the answer, so far as it can now be given, must be based mainly on structural data, supplemented by data on the processes of ore deposition. Presentation of these data based on a study of deep mines in the southeast quarter of the district, the only

Jan 1, 1927

By Foster J. Witthauer

First mining operations in the Tyrone District, located just north of the Burro Mountains in Grant County, New Mexico, commenced in the 1870's. A major operation was undertaken by Phelps Dodge Corporation in the early 1900's when a 2,000 ton per day underground mine was developed and a gravity concentrator was built east of the mine and across the Continental Divide. It was during this time that the picturesque Tyrone townsite was built and occupied. In 1921, however, the underground operation was closed because of high operating costs and low demand for copper. The area was drilled extensively during the 1950's and in October 1966 Phelps Dodge announced the pending development of the new Tyrone with a large open-pit mine, a modern concentrator, suitable support facilities, and a new townsite to be located between the mine and Silver City. Stripping for the pit and construction of shop and milling facilities began in 1967. By the spring of 1969, ore was being stockpiled near the primary crusher. Operation of the concentrator on a 3-shift per day basis commenced on July 17, 1969. The concentrator as initially built had one primary, two secondary, and five tertiary cone crushers, two grinding sections of six ball mills each, two flotation sections, four filters, and four tailing thickeners. The capacity was about 30,000 tons per day. In 1971 and 1972, the capacity was increased to 48,000 tons per day by the addition of one secondary and two tertiary crushers, one section of eight ball mills, one flotation section, two filters, and four more tailing thickeners. Centralized automatic control was built into the original and expanded facilities to the greatest extent possible, considering the state of the art at that time. Installation of additional control

Jan 1, 1976

By W. H. Bassett

ALTHOUGH brasses and bronzes have been made for ages, a systematic study of their physical properties has been carried out only during the years of the present century. Among these properties may be included those which are to be detected by means of microscopic examination; in other words by the science of metallography. The earlier workers in this field, both in this country and abroad, gave their attention to steel. When the senior author explored the situation in 1902, there was little encouragement to be found in undertaking the study of the non-ferrous alloys. A start was made, and the metallography of the brasses and bronzes, as well as of the copper-nickel- zinc alloys developed materially under his direction. Annealing experiments were begun in 1902, and in the succeeding years the effect of temperature, and the influence of previous working, on the grain size of brass were studied. The conclusions so well known and widely published today were largely reached during those earlier years. In 1905 the first complete annealing series were made. By this it is meant that brass and copper sheet, 5 B & S Nos. hard, was machined into tensile test specimens, then annealed under accurate control for 30 min. at temperatures up to the melting point of the material. Various determinations were made, including tensile strength and elongation in 2 in. There rapidly followed similar series on all of the copper-zinc alloys from 100 to 60 per cent. copper, on the bronzes, cupronickels, and on copper-zinc-nickel alloys. At this point there was published by Grard, in October, 1909,1 the very comprehensive and complete work on the tensile properties of cartridge brass, 90-10 copper-zinc, and electrolytic copper. The excellent photomicrographs in that paper illustrated the changes in structure produced by cold rolling as well as by annealing at different temperatures, but where Grard's work was confined to copper and to two alloys, the investigations in this laboratory have been over the entire fields of the commercial copper-zinc alloys, copper-tin alloys, representative copper-nickel and copper-nickel-zinc alloys as well as aluminum bronzes and others of a more special nature.

Jan 1, 1927

By B. C. Allen

Surface free energy and surface self-diffusion of solid molybdenum were studied in the temperature range 1600" to 2400°C using pressure-sintered bi-crystals. Comparison of groove angles formed in various surfaces perpendicular to the grain boundary indicate a maximum of 1 pct variation in surface free energy with crystallographic mientation. This anisotropy tends to decrease with increasing temperature. The surface diffusion of the bicrystals is equivalent to that of sheet with a mild (100) Preferred orientation. Anomalously low values found for bi-crystals with surface orientations of (OOl), (012), and (011) are rationalized in terms of anisotropy in surface free energy. THE effect of crystallographic orientation on surface free energy1,' and surface self-diffusion3,4 has been primarily studied in fcc metals. The object of this work was to study the effect of orientation on surface diffusion and surface free energy of bcc molybdenum using pressure-sintered bicrystals. EXPERIMENTAL WORK Materials and Crystal Preparation. Arc-melted molybdenum rod was obtained commercially and electron beam zone refined at 50 cm per hr at 10- 5 torr to form single crystals about 8 cm long and 0.65 cm diam. Three crystals were prepared with axial orientations about 1 deg from [001.], [011], and. [111]. To reduce the carbon content, the crystals were annealed 2 hr in 1.4 atm flowing wet hydrogen at 2050°C. Then the oxygen content was reduced by annealing for 2 hr in -30°C dewpoint hydrogen at 2020°C. The resulting impurity analysis is given in Table I. Bicrystal Preparation. The single crystal rods were cut into transverse slices with a thin silicon carbide abrasive wheel to produce specimens about 0.6 cm long. They were mounted in epoxy and surrounded by stainless steel washers. Cutting in half was done longitudinally at various angles to known crystallographic planes containing the cylinder axis according to Fig. 1. To reduce surface deformation resulting from the cutoff wheel and thus reduce parasitic grain boundary formation on subsequent annealing, about 0.003 cm was manually ground off each cut surface with 600 grit paper. Care was taken to keep the surface flat. After removal from the mounts, one half was generally ro-tated 180 deg with respect to the other to give a po- tential symmetrical tilt grain boundary between the two halves. In the other cases when low misorienta-tion angles were desired, the crystals were not rotated. On the basis of symmetry, sufficient bicrystals were prepared to cover the entire range of misorientations for symmetrical tilt boundaries. The misorientations, +, ranged from 0 to 45, 0 to 90, and 0 to 60 deg for [001], [011], and [111] bicrystals, respectively. One [Ill] twist bicrystal was prepared from 2 single crystal discs rotated 17 deg relative to each other. Each specimen consisted of two pieces which were placed in a cylindrical tantalum can. Sharp edges were rounded and the fit was made as snug as possible to reduce subsequent deformation during bonding. The assembly and crystals generally were vicuum outgassed at 900" or 1700°C and then electron beam welded in the can at l x 10-4 torr. After being leak checked, the samples were placed in an autoclave and hydrostatically gas-pressure bonded5 in four batches under helium at 10,000 to 18,000 psi at 1650°C for 3 hr. Satisfactory bonds were obtained in many cases, and most of the crystals bonded after two exposures. The results did not appear to be affected by the various pressures used, preannealing conditions, crystal orientation, or time-pressure-temperature route taken to the final bonding condition. After bonding, the tantalum cans were selectively removed in cold concentrated HF. Measurements indicated overall deformation was under 1 pct. The bicrystals were metallographically ground and polished flat and perpendicular to the axis. Examination showed the boundaries were straight and almost free of parasitic grains caused by extraneous local deformation. Annealing. In preparation for thermal grooving, the bicrystals were cleaned and annealed by outgassing at 10-5 torr at 1900°C and heating at 2300°C under 1 atm 99.996 Ar for 0.5 hr. The crystals were held in a closed 4-deck box made of molybdenum sheet, and were heated in a Ta-1OW resistance furnace. The ar-

Jan 1, 1970

Report of Secretary TO THE BOARD OF DIRECTORS OF AMERICAN INSTITUTE OF MINING AND METALLURGICAL ENGINEERS Gentlemen -I have the honor to present the following report for the calendar year 1920 The activities which-seem to call for special com¬ment are THE NEW FORM OF MAGAZINE MINING AND METALLURGY appeared every month during the calendar year and has been developed until it contains some ten departments It has brought forth more commendatory letters than have been received at headquarters on any other subject throughout the year Less than a dozen letters unfavorable to the change have been received, and the indications are that the magazine has met a want deeply felt, especially by members distant from headquarters The technical papers printed by the Institute are published in abstract in the magazine and opportunity is given to members who desire them to receive full copies of any or all papers published The Bound Volumes, as usual, contain all the papers in full and discussions thereof FINANCES The greatly increased cost of paper and printing has put a tremendous burden on the Institute's finances, since the dues of $12 per year are only 20 per cent greater than the members paid when the Institute was founded forty-nine years ago This has resulted in a temporary deficit, similar to that encountered by many of our sister engineering societies The fact that our Institute has lower dues and gives more in the way of publications to its members than any other of\the national engineering societies has rendered the situation more difficult for us MEETINGS The Annual Meeting in New York, the Field Meeting in the Lake Superior District, the meeting of the Petroleum and Gas members at St Lours, and of the Institute of Metals Division in Columbus, Ohio, have all been described in full in the magazine

Jan 1, 1923