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I. The Property. The Homestake Mining Co. has acquired through consolida tion the ground and equipment of the Father De Smet Con solidated Gold-Mining Co., the Deadwood-Terra Mining Go., the Caledonia Gold-Mining Co. and the Highland Mining Co., at and near Lead, Lawrence county, South Dakota, in the northern portion of the Black Hills. The company owns or controls 250 claims, comprising 2,616 acres and covering about 8,000 ft. along the strike of the lode. At the surface there are several veins, of which three have united in depth, where the main vein ranges from 300 to 500 ft. in width. The 1,100-ft. level is the lowest at present. The rock of both walls is, so far as known at present, carboniferous alate, and the country is penetrated by a system of porphyry dikes, and in some places capped with porphyry. The output of the company up to January, 1903, has been, approximately, $70,000,000. II. The Ore. The oxidized, open-cut ore is nearly all treated in the three mills on the northern part of the property, which are as follows : The Mineral Point (formerly the De Smet), of 100 stamps, the Monroe (formerly Caledonia), of 100 stamps, and the Pocahon tas (formerly the Deadwood-Terra), of 160 stamps. A cyanide plant, to treat the leachable portion of the tailings from these North End mills, has recently been installed and put into oper ation at Gayville, or Blacktail as it is now known. The Homestake lower-level ore, which comprises the greater part of that being milled at Lead, may be described as a horn blende, garnetiferous schist or slate, which has been crushed and infiltrated with free silica and pyrites, the latter being

Jan 1, 1904

By Frederick N. Rhines

Pure copper that has been allowed to oxidize at an elevated temperature in the air is found to be covered with two distinguishable layers of oxide scale. The outer of these, which is very thin, is composed of cuprie oxide, while the inner layer, comprising the bulk of the scale, is made up chiefly of cuprous oxide (Fig, la). If a small quantity of an alloying element, such as silicon, is present in the copper, silica particles are found disseminated through the cuprous oxide, deposited most abundantly near the metal surface, and, in addition, silica particles occur to a limited depth within the copper itself (Fig. 1b). It is this inner layer, composetl of oxide particles precipitated in a matrix of metallic copper, that is known as the "subscale" or the zone of internal oxidation. Under a low oxygen pressure it is possible to produce the subscale without the formation of external layers of copper oxides, thus leaving the metal surface bright and apparently clean while oxidation has occurred, in fact, to a considerable depth within the metal (Fig. 2). Although little is yet known in a detailed way of the mechanism of internal oxidation, the general nature of the process is evident. By virtue of the considerable solubility of oxygen in copper,' it is possible to bring the alloying element in contact with oxygen within the metallic solid solution. If the oxide of the alloying element is more stable than cuprous oxide, the foreign oxide may form and, since most oxides are relatively insoluble in copper, it will not long remain in solution, but mill separate as a precipitate. As the metallic solute is exhausted in the zone of precipitation, oxygen that is constantly being supplied at the surface diffuses farther into the alloy and thus produces an ever-thickening shell of subscale. The distribution of the reacting elements in the subscale and adjoining zones must be somewhat as indicated in Fig. 3. The conditions requisite to internal oxidation to be anticipated are thus: (I) a solubility of oxygen in the alloy, (2) the ability of oxygen to diffuse at an appreciable rate into the alloy, (3) the possibility of the

Jan 1, 1940

By Frederick N. Rhines

Pure copper that has been allowed to oxidize at an elevated temperature in the air is found to be covered with two distinguishable layers of oxide scale. The outer of these, which is very thin, is composed of cuprie oxide, while the inner layer, comprising the bulk of the scale, is made up chiefly of cuprous oxide (Fig, la). If a small quantity of an alloying element, such as silicon, is present in the copper, silica particles are found disseminated through the cuprous oxide, deposited most abundantly near the metal surface, and, in addition, silica particles occur to a limited depth within the copper itself (Fig. 1b). It is this inner layer, composetl of oxide particles precipitated in a matrix of metallic copper, that is known as the "subscale" or the zone of internal oxidation. Under a low oxygen pressure it is possible to produce the subscale without the formation of external layers of copper oxides, thus leaving the metal surface bright and apparently clean while oxidation has occurred, in fact, to a considerable depth within the metal (Fig. 2). Although little is yet known in a detailed way of the mechanism of internal oxidation, the general nature of the process is evident. By virtue of the considerable solubility of oxygen in copper,' it is possible to bring the alloying element in contact with oxygen within the metallic solid solution. If the oxide of the alloying element is more stable than cuprous oxide, the foreign oxide may form and, since most oxides are relatively insoluble in copper, it will not long remain in solution, but mill separate as a precipitate. As the metallic solute is exhausted in the zone of precipitation, oxygen that is constantly being supplied at the surface diffuses farther into the alloy and thus produces an ever-thickening shell of subscale. The distribution of the reacting elements in the subscale and adjoining zones must be somewhat as indicated in Fig. 3. The conditions requisite to internal oxidation to be anticipated are thus: (I) a solubility of oxygen in the alloy, (2) the ability of oxygen to diffuse at an appreciable rate into the alloy, (3) the possibility of the

Jan 1, 1940

C. W. GOODALE, * Butte, Mont.-In regard to the employment manager, the North Butte Mining Co. has undertaken that line of work and the rest of the companies are watching the experiment. If it is proved to be the proper thing, the system will be introduced into other mines. We have to combat the opposition to the use of the "rustling card. It is nothing more nor less than asking the nationality, where the plan formerly worked, and whether he is married or single. ROBERT RHEA GOODRICH, Anaconda, Mont. (written discussion?).¬Since the efficiency of the different phases of personnel work employed by industrial concerns, which are bringing about greater efficiency and lessening the labor turnover, the latter being intimately connected with "contentment of mind," depends on the individual workman, it is highly desirable, as far as industry is concerned, to keep the workman's mind and body in trim in order to lessen accidents and produce a higher grade of work. Prevention being better than cure, health supervision of the workmen during employment should be maintained by the employers in order that mental alertness and physical well-being may be obtained. I have long believed, from observation in many plants, that when any problem is dependent on the individual workman, what he believes and what he does is vitally dependent on his health. I will follow with much interest what is to be clone in the future in relation to the subject of health supervision during employment (as well as medical examinations at the time of employment), and I hope this idea will be generally instituted in personnel work. A workman with good health and a contented mind should be an ideal component of a progressive industrial concern. The contentment of the workman is fostered by a number of admirable phases of welfare work which are being still further developed. The mental and physical well-being of labor should be the issue in Labor vs. Capital in the new period of the industrial promotion of the United States into which we are now entering.

Jan 4, 1919

By T. G. Digges, C. L. Vold, M. R. Achter

A study was made of the effect of the growth conditions on the perfection of single crystals of niobium (columbium). Dislocation densities, determined by means of double-crystal diffractometer measurements , were not greatly affected by the method of crystal preparation but could be reduced by annealing treatments. However, the size, sharpness, and tilt angles of the substructures, observed with X-ray reflection macrograph, were sensitive to variations in growth procedures as well as to subsequent thermal treatments. Although the dislocation density was the same in both types, there were more low-angle bound-aries in crystals grown by zone melting than in those prepared by strain anneal. Mechanisms to account for these observations are discussed in terms of dislocation movements. A planned study of the structure-sensitive properties of refractory metals required the use of single crystals of a high degree of structural perfection and, for ease of handling, of large cross section. It appeared that the strain-anneal technique could satisfy both of these requirements. First, crystals grown in the solid state have been reported to be more perfect than those obtained from the melt.' Second, the diameters of rods which may be produced by zone melting should have a theoretical limit determined by specific gravity, thermal conductivity, and surface tension, while the diameter of strain-annealed rods is limited only by practical considerations. Previously it was shown that niobium (columbium) single crystals of 1 in. diam2 may be grown by strain anneal, compared to the 0.5 in. maximum diameter achieved by zone melting, as reported for molybdenum by Belk.3 The current research was undertaken to investigate and optimize the effect of various process variables on the perfection of 1/4 and 1/2-in.-diam niobium single crystals grown by strain annealing and to compare their perfection to those grown by zone melting. Characterization of these crystals was more conveniently accomplished by means of X-ray than by metallo-graphic techniques. EXPERIMENTAL PROCEDURE Specimen Preparation. Zone-melted crystals of 1/4 in. diam were produced by the standard electron-beam zone-melting technique. The swaged and cleaned rods were outgassed, in the solid state at a temperature near its melting point, at a rate of 12 in. per hr, and single crystals were grown by making two molten passes at 2 in. per hr. By maintaining a zone length of 4 to % in., very uniform single crystals several inches long were obtained. For the strain-annealed crystals, an induction heater was used, in preference to other types of heating, to take advantage of the good penetration of large sections. A five-turn coil, 1 in. long, operating at 10 kc and powered by a motor generator, was contained in a vacuum chamber. The rod, suspended from the upper end, was raised through the coil for both recrystallization and crystal growth. In preliminary work single crystals of the same material were also grown with single and multiturn coils powered by a 450-kc generator. A vacuum of 2 X 10-6 Torr was maintained at temperatures up to 2400°C. Starting with electron-beam-melted ingots of 21/2 in. diam, the analysis for which is given in Table I, the material was cold-swaged to the desired cross section of 1/4 and 1/2 in. diam and then recrystallized. The rods were then strained in a tensile machine and converted to single crystals by passing through the induction coil. As with zone melting, control of orientation is possible by the use of special procedures. Other investigators, see for example Williamson and smallman,4 have reported that orientation control may be achieved by a bending technique. In the present work the strained rod is partially lowered through the coil to start the growth of the crystal. Then it is removed and bent at a point in the poly crystalline portion. Finally, it is returned to the chamber and growth is continued "around the corner". This procedure has certain limitations. If the bending operation exceeds the critical strain, recrystallization may take place. Also, the amount of bending which can be imparted to the rod is limited by coil geometry, and up to now has been 10 deg. However, by repeating the bending and growing operations it should be possible to attain any desired orientation. In preparation for X-ray examination, single crystals were sectioned and planed by means of the spark-erosion technique. To obtain the maximum reflected intensity, the (110) plane was exposed for examination. They were then etched 3 to 5 min in a mixture of con-

Jan 1, 1967

By Frank Foote, Eric R. Jette

In a recent article,1 the authors reported the results of an X-ray investigation on the range of solid solutions that occurs in the iron-oxygen system in the vicinity of the compound FeO, which frequently is called "wüstite." The object of that investigation was primarily to study the unusual type of solid solution phenomena involved in this range. Briefly summarized the results were: 1. The NaCl type of lattice found by earlier workers was confirmed. 2. The lattice dimensions decrease rapidly with decrease in iron content. 3. No alloy that was a homogeneous single phase was ever found at compositions beyond 76.80 per cent Fe, while the theoretical iron content of FeO is 77.73 per cent Fe. 4. Measurements of the densities and lattice constants led to the conclusion that the form of substitution was complex, an FeO group being replaced by oxygen. Such a substitution, of course, is equivalent to removing an iron atom (or ion). The ideal unit cell of FeO can be considered as containing four groups of FeO and, thus, when this type of substitution takes place, there remain in the unit cell three FeO groups and an oxygen, or a total of seven atoms with a gross formula of Fe3O4 instead of the original Fe4O4. 5. This was the only interpretation that would fit the experimental results and at the same time be consistent with (a) the previously determined fact that the FeO lattice is ionic (i, e., consists of Fe++ and O? ions) and (b) the chemical fact that as the oxygen content of the substance increases, ferrous iron becomes oxidized to ferric iron. The experimental results of this investigation are included in Fig. 1. The purpose of the present investigation was to determine the limits of this homogeneity range by means of the X-ray structure analysis. This method has been applied frequently to the study of solid solutions by Westgren and his coworkers as well as by other investigators. The principle is simple: if the change in lattice constant with composition is

Jan 1, 1933

By J. C. Martin

A theoretical analysis of steam stimulation is presented for single sands. The analysis includes the effect of steam production and most of the effects of heat conduction. The results show the effects of a number of important variables on the performance of an idealized well under steam stimulation. Calculated responses are presented which indicate the effects of steam production, amount of steam injected, water production, formation thickness and formation damage. Results indicate that steam production can cause large reductions in the heat contained in the formation. This effect can be eliminated by drawdown control. Water production reduces the amount of oil produced during stimulation. The optimum amount of steam to inject depends on economic factors as well as the well response. In many cases, the increased temperature resulting from stimulation reduces oil viscosity near the well sufficiently to overcome the effects of formation damage even if the damage is not removed during steam injection. Calculated responses for thin sands are more favorable than anticipated. INTRODUCTION Little has been published on the theory of steam stimulation'-' despite the interest it has created and the wide variation in well responses. The results of the present analysis provide an insight into steam stimulation, and the methods employed provide a foundation for future work. Analyses presented in Refs. 1 and 2 are very limited and apply to gravity drainage conditions. Ref. 3 contains an analysis similar to the one presented here. The idealized models used and the assumptions made in Ref. 3 are different from those used in this paper. The analysis assumes that after steam injection has heated a small portion of the volume within the radius of drainage of a single uniform sand, a shut-in soaking period is allowed before returning the well to production. The effects of gravity, capillarity, transient pressure and water-sensitive sands are neglected. The injection and soaking times are assumed short compared to the stimulated production time. The initial temperature is assumed uniform; thus, the results apply primarily to first-cycle stimulation. The effects of gas production other than steam are neglected, and the water-oil ratio during production is assumed constant. Steam stimulation involves the simultaneous variation of the temperature, pressure and saturations. General mathematical equations for these variations are complicated and can be very difficult to solve. Simplified equations based on idealized models are used to reduce the mathematics sufficiently to allow approximate solutions to be obtained. DISCUSSION INJECTION An idealized model for which heat conduction is neglected is used to represent the behavior of a well during steam injection. The mathematics for this model is presented in Appendix A which also contains an approximate solution for the behavior of the no-conduction model. SOAKING During soaking, the well is shut in. Only the temperature, pressure and saturation distributions at the end of soaking are needed in the analysis. During soaking the heat is considered to be conducted in a uniform medium from an initially uniformly-heated circular cylinder confined to the producing interval. At the end of soaking the saturations and pressures are assumed to correspond to the cold zone. Analysis of the heat flow during soaking is included in the next section. The radius of the heated cylinder is calculated from the following heat balance (for constant quality steam injection). At the end of the soaking period it is assumed that little or no free gas is present near the well, and that the soaking period has been sufficiently long that the steam zone has had time to expand and the steam has condensed. The condition where there is no soaking is considered in the next section. PRODUCTION In this section, an approximate method is presented for solving the equations of heat and fluid flow associated with the production of oil and water during steam stimulation. Where initial pressure drawdowns are sufficient to cause steam to flow into the wellbore, steam production is assumed to occur within a short initial adjustment period (Appendix B). The production practices followed soon after the well is returned to production can have a large influence on the amount of oil produced during the stimulation cycle. Under most conditions, there is a period of time in which some or all of the water in the heated zone is converted into steam and produced. This flashing of hot water is caused by the pressure in the heated zone dropping below

By C. W. Vaupell

The Huitzuco mines lie in north central Guerrero, Mexico; production has been about 90,000 flasks of quicksilver since 1873. Near-surface ores fill extinct mud geysers and the deep deposits are chambered veins, stock-works in brecciated blocks, and replacements in limestone. The epigenetic minerals livingstonite, stibnite and sulphur occur in limestone, gypsum and dolomite through a developed vertical range of 260 meters. The deepest workings expose an increased amount of stibnite, which probably indicates that the lower limit of mercury mineralization is being approached. A resurgence of heat and water formed geysers over an extended area after the period of mercury mineralization. Mud geysers, which are situated, in the outcrops, contain the secondary mercury minerals, cinnabar and barccnite in the gravel and mud filling the vents. A 150-ton flotation plant is in operation concentrating stope fills that assay 3.0 kg. of mercury per ton. In one open stope, which is more than one hectare in area and 60 m. high, 150,000 tons are available. Introduction The Huitzuco mercury mines are of interest because of the unusual occurrence of ore in extinct geyser vents and the presence of several rare mercury minerals. Some of the deposits have typical characteristics of the telethermal zone and there is a gradation towards typical epithermal mineralization in depth. Halse,1 Villarel1o,2 Mactear3 and Merri114 have described the geology and the early operations in the district, and Bar-cena5 and Mallet6 have described the rare mercury minerals, livingstonite and barcenite, found at Huitzuco. Location The village of Huitzuco lies in the north central part of the State of (Guerrero, Mexico, 27 km. (16.7 miles) east of Iguala, which is the largest and most important town in the area. Iguala is served by the Mexican National Railways and also by the Mexico City-Acapulco highway. The highway is surfaced from Mexico City to Iguala, a distance of 200 km. (124 miles) by road, and there is a fairly good, level, dirt road from Iguala to Huitzuco. The elevation above sea level is about 1000 m. (3280 ft.). The climate is warm and very dry except during the rainy season, from June to

Jan 1, 1941

By C. W. Vaupell

The Huitzuco mines lie in north central Guerrero, Mexico; production has been about 90,000 flasks of quicksilver since 1873. Near-surface ores fill extinct mud geysers and the deep deposits are chambered veins, stock-works in brecciated blocks, and replacements in limestone. The epigenetic minerals livingstonite, stibnite and sulphur occur in limestone, gypsum and dolomite through a developed vertical range of 260 meters. The deepest workings expose an increased amount of stibnite, which probably indicates that the lower limit of mercury mineralization is being approached. A resurgence of heat and water formed geysers over an extended area after the period of mercury mineralization. Mud geysers, which are situated, in the outcrops, contain the secondary mercury minerals, cinnabar and barccnite in the gravel and mud filling the vents. A 150-ton flotation plant is in operation concentrating stope fills that assay 3.0 kg. of mercury per ton. In one open stope, which is more than one hectare in area and 60 m. high, 150,000 tons are available. Introduction The Huitzuco mercury mines are of interest because of the unusual occurrence of ore in extinct geyser vents and the presence of several rare mercury minerals. Some of the deposits have typical characteristics of the telethermal zone and there is a gradation towards typical epithermal mineralization in depth. Halse,1 Villarel1o,2 Mactear3 and Merri114 have described the geology and the early operations in the district, and Bar-cena5 and Mallet6 have described the rare mercury minerals, livingstonite and barcenite, found at Huitzuco. Location The village of Huitzuco lies in the north central part of the State of (Guerrero, Mexico, 27 km. (16.7 miles) east of Iguala, which is the largest and most important town in the area. Iguala is served by the Mexican National Railways and also by the Mexico City-Acapulco highway. The highway is surfaced from Mexico City to Iguala, a distance of 200 km. (124 miles) by road, and there is a fairly good, level, dirt road from Iguala to Huitzuco. The elevation above sea level is about 1000 m. (3280 ft.). The climate is warm and very dry except during the rainy season, from June to

Jan 1, 1941

By D. K. Crampton

The object of this work was to obtain and correlate information on effect of internal stress in variously drawn tubes on several properties. Also, a simple approximate method of comparing types of stress distribution in such variously drawn tubes was sought. There is also included some work on comparison of single and polycrystalline materials and effect of different types of operation and preferred orientation. Preparation of Material A series of tubes was drawn to study the effect of the type and degree of final reduction on various physical properties and the approximate distribution of stress intensity across the tube wall. The material used all came from a single heat of 70-30 brass melted in a regular production Ajax-Wyatt induction furnace. The analysis of the metal as cast was: copper, 70.36 per cent; lead, 0.04; iron, 0.02; zinc, balance. The material was cast in "shells" with 4 in. outside diameter and in. wall thickness. It was drawn part way down according to the usual standard mill schedule and then by suitable individual schedules to finish by a variety of types and degrees of drawing to the same final cases in every instance; namely, 0.750 in. outside diameter by 0.080 in. wall thickness. The exact final draws, together with the percentage area reductions, diameter reductions and gage reductions are given in Table 1. In fabricating these tubes, rather unusual precautions were observed to insure the elimination of ail variables not under immediate study. All intermediate anneals were carried out at about 1200" F. down to the so-called "cut-in size"; namely, 17/16 by 3/16 in. From this point on, all anneals were made at from 1050' to 1100" F. The greatest care was used all through to have the tubes as free from minor surface defects as possible. When such defects were visible on intermediate sizes they were carefully filed out. On the final draw to 3/4-in diameter the die was aligned with the greatest possible precision in order to insure as straight a tube as possible

Jan 1, 1933

By Y. Nakada, U. F. Kocks, B. Chalrners

THE orientation dependence of work hardening has previously been studied over the entire range, i.e., including special orientations of high symmetry, in aluminum1-3 and silver.* The differences between various orientations are substantial, and the trend is the same in all fcc crystals. However, there are quantitative differences in behavior between aluminum and silver at room temperature, particularly in the (100) orientation. While many experiments on gold have been reported,5'9 none included the special orientations. We therefore undertook tension tests on gold crystals of the axial orientations (100),(110), (Ill), (211), and, as a representative of single slip, one whose Schmid factor was 0.5 (hereafter referred to as m = 0.5). Single crystals of dimensions 1/4 by .1/4 by 6 in. were grown from the melt1' at a rate of 4 in. per hr, using gold of 99.99 pct purity obtained from Handy and Harman. A growth rate of 1/8 in. per hr, or a purity of 99.999 pct,ll produced no difference in results. The crystals were annealed at 1000°C in air for 24 hr and furnace-cooled down to room temperature, after which they were electro-polished in a solution of potassium cyanide (40 g), potassium ferrocyanide (10 g), soda (20 g), and enough distilled water to make 1 liter of solution, at a current density of 0.02 amp per sq mm. After 2 or 3 hr, a very smooth surface was obtained by this method. Nine m = 0.5, two (loo), one (110), three (Ill), and one (211; crystals were tested at room temperature in a floor-model Instron machine at a tensile strain rate of 0.5 pct per min. The accuracy of the stress measurement was k10 g per sq mm up to 500 g per sq mm, k2 pct for higher stresses. The strain measurement was accurate to t2 pct. The scatter of stress at a given strain among the crystals of the same orientation was small, *5 pct being the largest. The representative stress-strain curves for various orientations are shown in Fig. 1. Table I summarizes the work-hardening parameters as used by seeger.12 Results of other investigators are also included in this table for comparison. There are no previous data for the corner orientations. Values for m = 0.5 crystals agree fairly well with those of Berner. Tm is defined as the stress at which the stress-strain curve begins to deviate from linearity of Stage 11. However, in practice this is a very difficult value to estimate because each investigator has a different idea of linearity. Therefore, the comparison with the values of other investigators may not be valid. In the present experiment, (100) crystals had the highest 111, followed by (111) crystals. The work-hardening rate in Stage I1 was highest for the (111) crystal followed by the (100) crystals. Our value for 0x1 of m = 0.5 orientation agrees very well with those of other investigators. 1) Single-Slip orientation (m = 0.5). These crystals were oriented so that the primary-slip vector was contained in one side face. The dimension perpendicular to this side should then not change if single slip indeed takes place. Within the accuracy of measurement, this dimension did not change during the deformation. Since the accuracy is k0.2 pct, the amount of secondary slip is less than 0.7 pct of the slip on the primary-slip system at 30 pct tensile strain. This is in conformity with the results obtained by Kocks" for aluminum crystals. The tensile axis moved toward (211) during the deformation. Slip bands, Fig. 2(a), were very fine and closely spaced. Some deformation bands were observed. There were no clear-cut cross-slip traces such as the ones observed on aluminum m = 0.5 crystals. 2) (111) Crystals. The orientation of the tensile axis was stable during the deformation. From this observation, one can deduce that at least three slip systems must have operated, and probably all six because the remaining three all have cross-slip relation to one of the first three.' It was very difficult to observe the slip markings. Consequently, we could not confirm by this method that six systems were operative during the deformation. At high strains (above 50 pct shear strain), this orientation had the highest stress-strain curve. At 80

Jan 1, 1964

By Donald E. Cummings

Certain dusts are dangerous when inhaled, but most hazardous of all dusts are quartz or other forms of pure crystalline silica. The inhalation of dusts containing silica in combination with other elements gives rise to changes in the lung which differ from those produced by pure silica. As a generality, silicates are less dangerous than pure crystalline silica and vary greatly among themselves in harmfulness. Repeated analyses have shown that approximately 70 per cent of the total number of particles involved in any dust-producing operation are below 1 to 2 microns in diameter. (A micron is approximately 1/25,000 in.) Similar studies of dusts recovered from silicotic lungs post mortem have demonstrated essentially the same size frequency distribution, except that the upper limit of size retained in the air sacs is approximately 10 microns. Experiments carried on by Gardner and the author have further demonstrated that greater changes were produced by a fixed weight of very fine quartz particles (2 to 3 microns and smaller) than by the same weight of slightly larger particles (8 to 10 microns). Any attempt to control a dust hazard should therefore be directed toward the removal from the working atmosphere of particles less than 10 microns in size, and particularly those below 3 microns. All industrial hygienists agree on this matter, but there remains considerable dispute as to the lower limit of particle size capable of causing injury. It has been generally conceded, however, that particles of harmful dusts smaller than 1/4 to 1/2, micron are not essentially concerned in the development of pulmonary fibrosis. This opinion is partly substantiated by the existence of large numbers of these small particles in practically all atmospheres that are not associated with any known hazard. Such particles are so small that they have very little mass, fail to settle even in quiet air, and probably are not easily retained in the lung. Until further research proves that they are involved in the dangers provoked by the inhalation of certain dusts, engineers will generally agree that it is better to disregard them.

Jan 1, 1937

By Reginald S. Dean

Manganous oxide is readily soluble in concentrated ammonia solutions containing ammonium salts. Lixiviants of ammonia and ammonium carbamate permit ready extraction of manganese from reduced ores and the manganese in such solutions may be precipitated by heating to transform the carbamate to carbonate. THE widespread occurrence of manganese in low grade oxide and carbonate ores not amenable to mechanical concentration has led to extensive investigations of hydrometallurgical methods for producing a pure manganese compound suitable for further treatment. Manganese carbonate is the preferable compound. This product when fully crystalline and of not too fine crystal size is easily filtrable and stable in air. It can be converted to other compounds such as the oxides by heating in air or can be reacted with acids for producing salts. A useful hydrometallurgical process must produce relatively concentrated solutions that can be purified easily, reagents must be cyclically used, and heat requirements must be small. Neither the ammonium sulphate nor sulphur dioxide leaching processes that have been tested extensively fulfill these requirements. Other heretofore proposed processes have obvious limitations and have not been tried on a large scale. The present process is based on the discovery by the writer of a new group of aqueous manganese-ammonia complex solutions highly concentrated in ammonia, which permit rapid solution of manganous oxide to concentrations of 80 to 100 g Mn per liter and from which a fully crystalline, easily filtrable manganese carbonate is precipitated by the addition of carbon dioxide and partial ammonia removal. Although the process may be carried out with many ammonium salts, commercial advantages dictate the use of ammonium carbamate, which is obtained when CO2 is passed into concentrated aqueous solutions of ammonia. If the carbamate is used, the only reagents, ammonia and CO2, are volatile and may therefore be recovered from solutions and residues by heating, thus eliminating washing and extensive evaporation. Impurities are controlled easily as most metal oxides are either insoluble in the lixiviant or fail to precipitate with the manganese carbonate. Others are controlled by sulphide addition. The process has been tested extensively on a small scale on a wide variety of ores, including Three Kids, Artillery Peak, Cuyuna, and Chamberlain, as repre-

Jan 1, 1953

By Reginald S. Dean

Manganous oxide is readily soluble in concentrated ammonia solutions containing ammonium salts. Lixiviants of ammonia and ammonium carbamate permit ready extraction of manganese from reduced ores and the manganese in such solutions may be precipitated by heating to transform the carbamate to carbonate. THE widespread occurrence of manganese in low grade oxide and carbonate ores not amenable to mechanical concentration has led to extensive investigations of hydrometallurgical methods for producing a pure manganese compound suitable for further treatment. Manganese carbonate is the preferable compound. This product when fully crystalline and of not too fine crystal size is easily filtrable and stable in air. It can be converted to other compounds such as the oxides by heating in air or can be reacted with acids for producing salts. A useful hydrometallurgical process must produce relatively concentrated solutions that can be purified easily, reagents must be cyclically used, and heat requirements must be small. Neither the ammonium sulphate nor sulphur dioxide leaching processes that have been tested extensively fulfill these requirements. Other heretofore proposed processes have obvious limitations and have not been tried on a large scale. The present process is based on the discovery by the writer of a new group of aqueous manganese-ammonia complex solutions highly concentrated in ammonia, which permit rapid solution of manganous oxide to concentrations of 80 to 100 g Mn per liter and from which a fully crystalline, easily filtrable manganese carbonate is precipitated by the addition of carbon dioxide and partial ammonia removal. Although the process may be carried out with many ammonium salts, commercial advantages dictate the use of ammonium carbamate, which is obtained when CO2 is passed into concentrated aqueous solutions of ammonia. If the carbamate is used, the only reagents, ammonia and CO2, are volatile and may therefore be recovered from solutions and residues by heating, thus eliminating washing and extensive evaporation. Impurities are controlled easily as most metal oxides are either insoluble in the lixiviant or fail to precipitate with the manganese carbonate. Others are controlled by sulphide addition. The process has been tested extensively on a small scale on a wide variety of ores, including Three Kids, Artillery Peak, Cuyuna, and Chamberlain, as repre-

Jan 1, 1953

By B. V. P. Rao, H. L. Lovell, G. Simkovich

In the study described here, flotation tests were conducted on pure CaF2, on CaF2 doped at several concentration levels with either NaF or YF3, and on natural fluorite samples containing various amounts of impurities in an effort to extend previous knowledge of the influence of crystalline point imperfections on the flotation properties of solids. The results of these tests showed that although recoveries generally decreased as impurities increased, the differences in recovery were not nearly as striking as those detected in earlier experiments. A number of experimentalists have shown an interest in the way in which crystalline point imperfections affect the flotation properties of solids. As long ago as 1953, Welch hypothesized that it might be possible to control surface imperfections and thereby also control the flotation of solids.' A few years later, in some rather extensive work, Plaksin and his coworkers varied the surface imperfections of a number of compounds by oxidation or reduction processes and found that significant variations in flotation properties resulted.2-4 More recently, Simkovich showed that the recovery of both AgCl and PbS could be markedly varied by adding solid-solution impurities, which acted as doping agents, to these compounds.5 Then Mular studied the flotation of ZnO as a function of the doping agents Al2O3 and Li2O.6 Once again, it was found that these impurities, even in very low concentrations, had profound effects upon flotation recoveries. From an imperfection point of view, the defect structures of the compounds tested previously are as follows:7 PbS — amphoteric semiconductor with a Frenkel-type defect structure in the cation sub-lattice.8 AgCl - ionic conductor-Frenkel type defect structure? ZnO — n-type semiconductor, zinc ion interstitials and quasi-free electrons.10 All of these works undoubtedly bear some relation to the findings that the flotation properties of seemingly identical minerals from different ore deposits often exhibit extreme variation in flotation behavior, i.e., that small amounts of analytically undetectable impurities often have a great influence upon flotation

Jan 1, 1969

By B. B. Rath, Hsun Hu

In wedge-shaped bicrystals of zone-refined aluminum it is observed that (111) pure tilt boundaries migrate under the driving force of their own inter-facial free energy. The boundary velocity is a power function of the driving force. The driving force exponent decreases with decreasing angle of misorien-tation. For example, at 64O°C, the exponent decreased from 4.0 for a 40 deg to 3.2 for a 16 deg tilt boundary. An evaluation of the driving force acting on the boundaries during their motion indicates that for low driv-forces, up to about 2 x l03 ergs per cu cm, the velocity is relatively independent of misorientation, whereas at higher driving forces a 40 deg tilt boundary exhibits the highest velocity. The measured activation energy for boundary migration approaches that for bulk self-diffusion at low driving forces, decreasing from 33 to 27 kcal per mole as the driving force is increased from 1 x l0 to 5 x l03 ergs per cu cm. These results are compared with current theories of grain-boundary migration. In previous experimental studies of grain boundary migration the driving force has been limited to a difference in stored energy across the boundary. This stored energy has been introduced into the crystal either by prior deformation1-3 or by grown-in lineage structure. A part of the energy stored in the deformed crystal is released by recovery either prior to or concurrently with grain boundary migration, thus introducing an uncertainty as to the magnitude of the driving force responsible for grain boundary migration. The grown-in lineage structure, though thermally stable during annealing, neither provides conditions under which different levels of energy may be stored in the imperfect crystal nor provides a control of orientation difference across the migrating boundary of a growing grain. Furthermore, because of variation in the lineage structure, it is difficult to determine accurately the energy stored in the imperfect crystal. Several investigations of grain boundary migration during normal grain growth have also suffered from difficulties in estimating the driving force because of uncertainties in the principal radii of curvature.~ In the present investigation the velocity of pure tilt boundaries in zone-refined aluminum bicrystals of selected orientation (40, 30, and 16 deg around the [Ill] tilt axis) has been measured in the absence of a dislocation density difference across the moving boundary, thus eliminating the previous experimental difficulties. The driving force for boundary migration is derived from a gradient of the total interfacial free energy of the migrating boundary in wedge-shaped bicrystals. A similar method was attempted by Bron and Machlin in a study of grain boundary migration in silver. However, they found that one of the crystals was deformed and consequently the motion of the boundary was partly due to a difference of stored energy across the boundary. The observed behavior of boundary velocities as affected by the driving force is examined in the light of the predictions of the current theories of grain boundary migration.7"10 The effect of boundary misorientation on velocity is compared with the theory of " which is based on a dislocation core model for high-angle boundaries. EXPERIMENTAL METHOD Seed-oriented bicrystals of zone-refined aluminum, 2.5 cm wide, 0.5 cm thick, and 12 cm long, containing tilt boundaries with a common (111) axis, were grown from the melt in the direction of this axis. Spectro-graphic analysis, reported earlier,'' indicated the purity of the crystals to be 99.999+pct. Three such bicrystals containing 16, 30, and 40 deg tilt boundaries were used. Wedge-shaped specimens were prepared from these bicrystals by spark cutting followed by electrolytic polishing. The angle of the wedge was usually 40 deg and the specimens were usually 0.25 cm thick. The intercrystalline boundary was located within 0.2 to 0.5 cm from the tip of the wedge. Fig. 1 shows a section of an oriented bicrystal containing an outline of a wedge-shaped specimen. The crystallographic directions shown in Fig. 1 represent the orientation of one of the crystals (the larger section of the bicrys-tal); the orientation of the other crystal differs only by rotation around the common [lil] axis. The parallel faces of the wedge always corresponded to the common (171) planes in both crystals, whereas the orientation of the side faces varied, depending on the misorientation angle. The bicrystal orientations were determined

Jan 1, 1970

By F. H. Wilson, E. W. Palmer

Brass mills are familiar with a recurring problem which reveals itself during deformation of annealed metal as an opening up of cracks which are suggestive of a grain boundary pattern. A typical example is seen in Fig 1, which shows part of the convex surface of a cartridge brass disc which was slightly dished by the punching operation. Another illustration of the same type of defect was found in the surface of a finished cartridge case which split open on firing. These cracks, shown in Fig 2, were away from the split but indicate the presence of the type of weakness which permitted the splitting. Usually the weakness consists of separate cracks, the lengths of which are of the same order of magnitude as the grain size prior to the final anneal. Their typical appearance in a polished section is shown in Fig 3. This structure was found below the surface of a fractured tensile-specimen that had been cut from a large cartridge blank showing the defects on its convex surface. While the pattern formed by these cracks suggests a grain boundary origin, the cracks bear no relation to the currently existing grain structure. Thus Fig 3 shows that the grains have grown up to cracks already present. Since it is doubtful that the cracks were present in the metal before the anneal, they must have formed during the anneal but prior to recrystallization. The term "fire-cracking" has been generally applied to cracking that occurs during an anneal under the influence of internal stress, but refers more specifically to obvious macroscopic cracking attributable to the presence of a low melting phase, usually lead. Since the type of cracking described above may occur when the lead content is very low, we have considered it a somewhat different phenomenon, and have called it "inter-granular parting." While most examples involve cartridge brass, intergranular parting has also been observed in the fabrication of large seamless tubes from discs of both 85/15 red brass and 70/30 cupro-nickel. Similar cracking in nickel silver was investigated by Jones and Whitehead,1 who showed that it could occur during healing or cooling. That which occurred on heating they called "fire cracking," and they suggested that, a transformation at about 320°C might account for its occurrence. It was felt in this laboratory that the observed parting was probably one aspect of the general observation, first made by Rosenhain and Archbutt,2 that a tendency toward intergranular fracture under tensile stress increases with increasing temperature and decreasing rate of strain. In this case the stress involved would be internal. The rate of strain would be exceedingly slow, a localized internal creep. Reference to the literature uncovered no efforts to extend the observations of Rosenhain to conditions involving only internal stress. Accordingly, an exploratory research, sufficient in detail to satisfy us as to the probable truth of this explanation of the observed intergranular parting, was undertaken. The internal stresses present during the early stages of an anneal (prior to recrystallization) would be from two sources: residual stresses developed during deformation, and thermal stresses caused by uneven heating and expansion. Thermal stresses would vary widely according to shape, size and manner of heating, and can be considered as supplementary to residual stresses. It seemed necessary to determine the stress and temperature conditions under which parting would occur in a relatively short time, and then to establish whether or not in- ternal stresses may persist to an extent adequate to cause parting at such temperatures. (Jones and Whitehead1 and Moore and Beckinsale3 made tests which indicated that stress relief required an appreciable time.) During the course of the research the desirability of studying the effect of grain size became apparent, and this factor is one of the major variables of our investigation. Intergranular Parting under Tension at Elevated Temperatures In early experiments, hard 70/30 brass tensile specimens, with unknown residual stresses, held for 10 min. at applied stresses from 30,000 to 40,000 psi at temperatures from 300 to 350°C, showed no macroscopically visible cracks when unloaded and cooled, but cracks very similar in appearance to those observed in commercial practice were revealed in these specimens by pulling them to fracture. Annealed specimens, on the other hand, showed no cracks in such experiments, apparently because they deformed plastically at stresses below those necessary to cause parting in a reasonable time. Hence, the specimens used for this study were first strengthened by cold tensile elongation, giving them an unavoidable residual stress pattern (determined largely by grain size and orientation) which would, however, correspond in direction, at least, to the stress pattern obtained under stress at temperature. A variation in these residual stresses might be expected with variations in grain size, but following any given anneal the reproducibility of stress pattern should be as good as that of the grain size measurement. With no information as to the effect of the amount of prior deformation, tests were conducted on specimens given the same cold elongation, using a stress applied at temperature which was a constant proportion of the stress required to produce this elongation. In

Jan 1, 1950

By Robert W. Hendricks, John B. Newkirk

A simple method is described for determining the orientation of a single crystal by means of a cylindr cal X-ray camera. Orientation setting to within ±1 deg is attainable by a stereographic analysis of a single cylindrical Laue pattern produced by the originally randomly mounted crystal. Final precision adjustments which permit orientation of the crystal to within ±5 min of arc from the desired position can be made by the method of Weisz and Cole. A chart, originally Presented by Schiebold and schneider7 and which allows a direct reading of the two stereographic polar coordinates of the corresponding pole of a given Laue spot, has been recomputed to aid in the stereographic interpretation of the cylindrical Laue X-ray photograph. Detailed instructions for the use of the chart, a simple example, and a comparison with the conventional flat-film Laue Methods, are presented. 1 HE problem of determining the orientation of the unit cell of a single crystal relative to a set of fixed external reference coordinates is fundamental to most problems of X-ray crystallography and to many experimental studies of the structure-sensitive physical properties of crystalline materials. Several techniques for measuring these orientation relations have been developed which correlate optically observable, orientation-dependent physical properties to the unit cell. Examples of such procedures include the observation of cleavage faces or birefringence, as discussed by bunn,1 or the examination of preferentially formed etch-pits, as discussed by barrett.2 Each of these methods is limited, for various reasons, to an orientation accuracy of approximately ±1 deg—a serious limitation in some experimental studies. Several other limitations decrease the generality of these methods. Of these, perhaps most notable is the absence in many crystals of the physical property necessary for the orientation technique. The most widely used methods for determining crystal orientation are variations of the Laue X-ray diffraction method. Because of the indeterminacy of the X-ray wavelength diffracted to a given spot, the interpretation of Laue photographs is now limited almost exclusively to the procedure of using a chart to determine the angular coordinates of the corresponding pole for each spot. For the flat-film geometries, either a leonhardt3 or a Dunn-Martin4 chart is used in interpreting transmission patterns, whereas a greninger5 chart is used for interpreting back-reflection patterns. A less common method of interpreting flat-film transmission Laue photographs is by comparing the Laue pattern with the Majima and Togino standards,6 or with the revised standards prepared by Dunn and Martin.4 Although this last method is applicable only to crystals with cubic symmetry, it can be very rapid and just as accurate as the graphical methods. The primary limitation of all the X-ray methods mentioned is the relatively small number of Laue spots and zones which are recorded on the flat film. Often, few, if any, major poles appear, thus making interpretation tedious and sometimes uncertain. The use of a cylindrical film eliminates this problem. Schiebold and schneider7 prepared a chart by which the orientation of the specimen crystal could be determined from a cylindrical Laue photograph. However, it was only drawn in 5-deg intervals of each of the two angular variables used to identify the Laue spots, thus limiting the accuracy of orientation to about ±3 deg. An examination of this chart indicated that if it were drawn in 2-deg intervals, crystal orientations to ±1 deg would be attainable. Subsequent use of the replotted chart has confirmed this accuracy. It is the purpose of this paper to describe the redevelopment and use of this chart, and to point out its advantages and limitations. I) CAMERA GEOMETRY AND CHART CALCULATIONS The geometry of the cylindrical camera with a related reference sphere is shown in Fig. 1. The X-ray beam BB&apos; pierces the film at the back-reflection hole B, strikes the crystal at 0, and the transmitted beam leaves the camera at the transmission hole T. One of the diffracted X-rays intersects the film at a Laue spot L. The normal OP to the diffracting plane bisects the angle BOL between the incident and diffracted X-ray beams. The point P on the reference sphere can be located uniquely by the two orthogonal motions 6 and 8 on the two great circles ENWS and BPQT respectively. Because the Bragg angle 8 (= 90 - < BOP) is always less than 90 deg, P always remains in the hemisphere BENWS. Therefore, if every possible pole P is to be recorded on the same stereographic projection, it is necessary that the projection reference point be at T with the projection plane tangent to the sphere at B.* The great

Jan 1, 1963

HeRbert A. MeGRaw, San Luis de la Paz, Guanajuato, Mex. (communication to the Secretary*) :—Although Mr. Bordeaux prefaces his paper with the statement-that it is a general outline of practice in the Republic, many of his statements seem to be made from the view-point of a particular case, which does not always agree with general practice. For the purpose of calling attention to some of these variations, I respectfully offer the following comments: The operation of crushing and grinding is performed by so many different methods and systems that it is useless to select any one as the standard. However, primary crushing in rock-breakers followed by stamps is thus far so general that it might be so classified. Whether or not it is the best way, is open to question. Regrinding may be performed by any of the various types of Chilean mills, Huntington mills, or similar machines, or the material may be taken directly from the stamps and delivered to the tube-mills. Mr. Bordeaux&apos;s statement that " the slimes can be treated only by decantation; the new Butters slime-filter, as used in Nevada, does not seem to be successful with silver-ores," is surely an error. All over Mexico many of the purely silver-ores are being successfully handled by the Butters or similar filters, such as the Moore and the Burt filters, and a letter to the manufacturers of these filters will undoubtedly bring a list of the silver-ores now being successfully treated in this way. The statement that crushing silver-ores in solution is impossible is equally erroneous. Most modern mills crush the ore in solution, in some cases containing as much as 0.12 per cent, of KCN. I cannot for the moment recall any modern mill in Mexico which does not follow this practice. There may be some reason for it in particular instances, but, generally speaking, the practice is to crush in solution. Care in installation avoids any mechanical loss of cyanide, and the chemical loss is so small as to be negligible.

Jan 1, 1910

By L. G. Laureau

This paper is presented to call the attention of steel-manufacturers to the need of further reform in the manner of casting and handling ingots. The problem of making the work usually performed in and around the casting-pit less dangerous to the men and less costly to the management is one which has occupied the minds

Jan 1, 1885