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By W. A. Backofen

THE preferred orientations, or textures, resulting from many of the various methods for testing and forming metals have been the subject of numerous investigations.1,2* Despite this large amount of work, however, only a few limited studies have been made of the texture that is developed by torsional deformation. Ono3 found that in severely twisted wires of copper and aluminum a [Ill] direction lies parallel and a [1101 direction perpendicular to the longitudinal axis of the wire. Sachs and Schiebold4 have reported that a double-fiber texture exists in a twisted aluminum wire with both the [Ill] and [loo] directions parallel to the axis of the wire. Twisted iron wires have also been examined by Ono.8 Both the [1101 and [1121 directions were reported as parallel to the axis of the wire. Goss5 concluded from a study of twisted rods of a low-carbon steel that the preferred orientation existing at fracture is quite complex, but that many grains have a [1101 direction parallel to the axis of the wire. In addition to the earlier experimental work, some suggestions have been made about the possible nature of the torsion texture. These suggestions are based on the results of many experiments which indicate that the cold-working texture of a particular metal is largely determined by the geometrical change in shape that the metal undergoes during plastic deformation.1,6 Hibbard and Yen7 have considered the problem of deformation textures and have presented an analysis which is able to explain why equivalent changes in shape should yield similar textures. Therefore, a knowledge of the principal strains associated with torsional deformation would seem helpful in the interpretation of the torsion texture. The necessary analysis has been made of the state of strain in an element of metal lying in the surface of a cylindrical rod or tube that has been subjected to pure torsion.8,9 This analysis shows that the directions of the principal normal strains rotate continuously within a torsion specimen while it is being twisted. After the first infinitesimal amount of twisting, these directions make angles of 45" with the longitudinal axis of the bar. They rotate from this position as twisting proceeds, and after an infinite amount of twisting, the direction of the principal tensile strain is perpendicular, and the direction

Jan 1, 1951

VITRIOL is likewise a mineral substance from whose exhalation, according to the opinion of some, are generated and produced the elemental materials or substances which produce metals, particularly gold. It is not a fumosity from metal nor is it a thing from which metal is extracted in any manner, although it shows in certain ways that it is not entirely without metal since it produces a certain trace of it. It is a thing that has a great resemblance to alum; it has a biting substance, is sharp to the taste and pungent to the tongue, and has an astringent nature. It dissolves in water and every damp place in a short time. They say that the reason for this lies, as with every other mineral, in its poorly joined watery substances. Nor does this mean that it does not contain much earthiness; on the contrary it seems to me that there are in it five. [2.9v] different participating qualities, that is, the property of sulphur, the action of alum, the corrosion of niter or of salt, and from the metals, the properties of copper and of iron. Its ore is mined in the valleys of mountains in wild but not too rugged places. It is more a gray earth or soft dead rock than a hard stone. It always has in it some yellow and green spots or near it is some sulphur mineral, either large or small.. When it is beneath the earth it exhales a sharp and very strong foul odor of scorching similar to that of sulphur. And the waters that rise where it is are all foul, earthy, and thick, some boiling with great fumes and others without great fumes, so that they surely appear to be infernal products in many places where there is a large quantity of it. After you have excavated and sorted well the quantity you wish, the ore must be put in a heap in open airy places before the vitriol can be extracted from this soil or ore, however you wish to call it. And it is left thus exposed to the weathering of the rains, the cold, and the sun for five or six months. It must be turned several times in order to bring to the surface that which was underneath; and always when this is done it is broken small with the eye of a mattock so that it is better heated and baked throughout. When it has been brought to this point it is covered over by a shed built above it or it is carried under a hut that has already been made. Here it is left to stand for another six or eight months before it is worked.

Jan 1, 1942

By Thomas Clagett

THE Pocahontas coal field comprises the area in Tazewell County, Va., and Mercer and McDowell Counties, W. Va., in which Nos. 3 and 4 Pocahontas seams of bituminous coal are mined. It is a mountainous region with ridges rising 300 to 1000 ft. (91 to 305m.) above the very narrow valleys and, except for some poorly kept farms along the tops of the ridges and the area occupied by the mining and coking plants and villages, is wooded throughout. First shipments were made from Pocahontas in 1883. There are now, about 100 mines, 95 per cent. of which are drift mines. At the end of 1920, approximately 298,000,000 gross tons of coal had been produced and 35,000 acres of coal mined. No. 3 seam is from 4 to 10 ft. (1.2 to 3 m.) thick, but the change is gradual and the thickness fairly uniform in any particular locality. It has a streak of bone, about 2 in. (5 cm.) thick, io which the coal adheres on both sides. In parts of the field this bone is replaced by hard slate, usually from 2 to 4 in. thick. The seam has a slate or fireclay bottom and a draw-slate top. No. 4 seam is from 65 to 80 ft. (19.8 to 24 m.) above No. 3 seam, and of minable section only in the western part of the field. It is from 3 to 8 ft. thick and has two streaks off bone, each from 1 to 2 in. thick. It has a fireclay or slate bottom and is overlaid by from 4 to 24 in. of a laminated coal and slate, locally termed "black rash," which is separated from the coal seam by about 3 in. of slate. This "black rash" averages about 25 per cent. ash, but contains some clean coal. The coal in both seams is quite soft. Cleavage sufficiently well defined to exert an influence on the mining is rare. Overlying strata are slates, shales, and sandstones, the sandstones predominating, extending from .30 to 1000 ft. above No. 3 seam. The strata directly above the. draw slate of No. 3 seam, or "black rash" of No., 4 seam, and up to the first sandstone are usually slates or shales, about 10 ft. thick over the

Jan 5, 1922

Scraper and Slide Riddell Mucker Boskovich Device Hydro-mucker Inclined Shaft Mucking The Benching Method Performance Chart

Jan 3, 1950

By James Pollock

The possibility of colloidal deposition of cinnabar has been neglected. In opalite deposits cinnabar exists in particles within or near the colloidal size range. Colloidal processes have been admitted to be operative in hot springs and low-temperature deposits similar to most cinnabar deposits. Mercuric sulphide sols are stable to elevated temperature and pressure, and in nature probably are chiefly affected by the electrolytes in solution, dilution of colloid, and presence of protective colloids as silica. The stability of mercuric sulphide sols to electrolyte is measured, and shown to be greatly increased by dilution and by the protective action of silica. Mercuric sulphide sols follow the Schulze-Hardy valency rule, therefore the precipitating power of complex mixtures of electrolytes can be computed roughly. The stability of mercuric sulphide sols is shown to be greater than the equivalent precipitating power of the electrolytes in a hot spring depositing mercuric sulphide. It is concluded that finely divided or earthy types of cinnabar are colloidally deposited. Possibility of Collodial Deposition While colloidal solution has been suggested as a means of transport for a number of minerals, such as the sulphides of antimony, arsenic, and iron, it has been neglected in connection with mercury. This is surprising because there exists positive evidence that cinnabar is present in certain deposits in particles of colloidal or near colloidal size. Colloidal transport could result from either the rapid dilution or neutralization of alkaline sulphide solution bearing mercury coming in contact with deep ground waters, or from colloidal solution near the original source and subsequent flow to the point of deposition unchanged. That the dilution of a mercuric alkaline sulphide solution will precipitate mercury sulphide in colloidal form has been demonstrated a number of times and is easily confirmed. The dilution hydrolyzes the alkaline sulphide Na2S to the corresponding hydroxide and hydrosulphide NaOH and NaHS, and the diminution of the concentration of alkaline sulphide reduces the solubility. It is not the contention of this writer that colloidal deposition is the mode of transport of mercuric sulphide in all mercury deposits, but that the stability of a mercuric sulphide sol, as demonstrated below, in waters that are similar to those that have deposited mercuric sulphide necessitates consideration of this possibility in many deposits, especially those of the hot-spring and so-called opalite type. Evidence of Colloidal Deposition Ross1 has shown that most deposits of quicksilver are formed at low temperatures and pressures, and probably by solutions that have relatively simple chemical compositions. In most cases the solutions are probably similar to those observed in hot springs, and in two instances—at Steamboat Springs, Nevada, and Sulphur Bank, California—hot springs have been reported by Becker as actually depositing cinnabar.2 Opalite deposits were believed by early investigators to be surface phenomena

Jan 1, 1949

By James Pollock

The possibility of colloidal deposition of cinnabar has been neglected. In opalite deposits cinnabar exists in particles within or near the colloidal size range. Colloidal processes have been admitted to be operative in hot springs and low-temperature deposits similar to most cinnabar deposits. Mercuric sulphide sols are stable to elevated temperature and pressure, and in nature probably are chiefly affected by the electrolytes in solution, dilution of colloid, and presence of protective colloids as silica. The stability of mercuric sulphide sols to electrolyte is measured, and shown to be greatly increased by dilution and by the protective action of silica. Mercuric sulphide sols follow the Schulze-Hardy valency rule, therefore the precipitating power of complex mixtures of electrolytes can be computed roughly. The stability of mercuric sulphide sols is shown to be greater than the equivalent precipitating power of the electrolytes in a hot spring depositing mercuric sulphide. It is concluded that finely divided or earthy types of cinnabar are colloidally deposited. Possibility of Collodial Deposition While colloidal solution has been suggested as a means of transport for a number of minerals, such as the sulphides of antimony, arsenic, and iron, it has been neglected in connection with mercury. This is surprising because there exists positive evidence that cinnabar is present in certain deposits in particles of colloidal or near colloidal size. Colloidal transport could result from either the rapid dilution or neutralization of alkaline sulphide solution bearing mercury coming in contact with deep ground waters, or from colloidal solution near the original source and subsequent flow to the point of deposition unchanged. That the dilution of a mercuric alkaline sulphide solution will precipitate mercury sulphide in colloidal form has been demonstrated a number of times and is easily confirmed. The dilution hydrolyzes the alkaline sulphide Na2S to the corresponding hydroxide and hydrosulphide NaOH and NaHS, and the diminution of the concentration of alkaline sulphide reduces the solubility. It is not the contention of this writer that colloidal deposition is the mode of transport of mercuric sulphide in all mercury deposits, but that the stability of a mercuric sulphide sol, as demonstrated below, in waters that are similar to those that have deposited mercuric sulphide necessitates consideration of this possibility in many deposits, especially those of the hot-spring and so-called opalite type. Evidence of Colloidal Deposition Ross1 has shown that most deposits of quicksilver are formed at low temperatures and pressures, and probably by solutions that have relatively simple chemical compositions. In most cases the solutions are probably similar to those observed in hot springs, and in two instances—at Steamboat Springs, Nevada, and Sulphur Bank, California—hot springs have been reported by Becker as actually depositing cinnabar.2 Opalite deposits were believed by early investigators to be surface phenomena

Jan 1, 1949

By C. D. Hall, F. E. Dollarhide

Conventional static tests of fluid-loss agents do not realistically simulate conditions in a fracturing treatment. The dynamic tests reported here show that fluid-loss volume is better represented as proportional to time, rather than as the square root of time. This leads to a different equation for fracture area. The leak-off rate increases with increasing shear rate at the fracture wall, but appears to approach a limiting value. Pressure effects are minor. Spurt loss ordinarily is not affected by the flow velocity in the fracture and is inversely proportional to concentration of agent. The filter cake, once it is well established, is resistant to damage by the flow of plain fracturing liquid (without fluid-loss agent). The latter two findings indicate that a treatment employing a high-concentration spearhead followed by plain fluid can offer a more economical treatment under suitable conditions. INTRODUCTION The successful design of hydraulic fracturing treatments depends on accurate knowledge of the fluid-loss properties of the fracturing fluid. Howard and Fast,' in giving the basic equation relating fracture area to fluid and treating parameters, described three mechanisms which might control the rate of fluid leak-off from the fracture. One mechanism usually is dominant in a given well treatment. For each mechanism, the leak-off velocity is inversely proportional to the square root of time, and the proportionality constant is designated as the fracturing-fluid coefficient. For the wall-building type of fluid-loss agent, the coefficient is determined by a filtration test in a pressure cell, usually with a rock wafer or core as the filter medium. In these static tests, the cumulative volume generally is proportional to the square root of time, after an initial spurt volume. The static-fluid-loss test is not representative of the con,-&tions under which a fluid-loss agent performs in a fratturing treatment. The marked difference between the dynamic- and static-fluid-loss behavior of drilling fluids reported in the literature2,3 implies that dynamic testing is also needed with fracturing fluids. We have therefore undertaken a study of the dynamic-fluid-loss behavior of fracturing fluids. The testing apparatus has also afforded opportunity to evaluate the resistance of the filter cake to removal or damage by flowing fluid containing no fluid-loss agent, with and without sand. The results of these studies offer a means for more accurate evaluation of fluid-loss agent performance, and point the way to a "spearhead" fracturing technique which may offer more economical treatment for some wells. EXPERIMENTAL METHODS The dynamic-fluid-loss testing method is applicable to any type of wall-building fracturing fluid. The present study aimed first at finding what phenomena are involved, and therefore has been limited in the number of materials tested. All of the results specifically reported herein are for kerosene containing a commercial solid fluid-loss agent, which is commonly used at 50 lb/1,000 gal of oil. Another agent in liquid form, used usually at 20 ga1/1,000 gal oil, has shown all the same phenomena in dynamic tests, and generally the same level of fluid-loss control as the solid agent. The dynamic-fluid-loss core cell used in all tests is shown in Fig. 1. The fracture was simulated by the an-nulus between a 2.03 in. OD sandstone core and the surrounding pipe. Annulus widths of 0.234 and 0.117 in. were used, and the core was 3.5 in. long. The annular geometry provides a uniform fluid velocity and a well-defined shear rate over the entire filtering surface, and permits a large filter area (144 sq cm) in a reasonably compact cell. The leak-off fluid passed into a 0.5 in. diameter axial hole in the core. A hollow steel rod through this hole was threaded into a rounded "streamliner" upstream of the core, and into a mounting stud downstream. The streamliner and the stud had the same outside diameter as the core. In all tests except those where sand was circulated, the mounting stud had protruding rings which constricted the annulus, to minimize any tendency for channeling of the fluid to the side exit port. The ends of the core were sealed by Neoprene, steel and Teflon washers. The leak-off fluid was conducted from the hollow rod to an exit tube, through a metering valve (a fine-pitched needle valve) and a quick-opening toggle valve in series, and into graduated cylinders for volume measurement; Two separate circulating systems were used in the experimental program. The extensive initial testing was done at 50 to 150 Psi. The fluid was circulated by a variable speed Moyno pump, and the flow rate was read by a rota-meter flow meter. The filtration Pressure was supplied by holding a back-pressure with a throttling valve. The discharge streamcould be diverted into any of four sections

Jan 1, 1965

By F. L. Wolf

THERE is a tendency on the part of practical foundrymen to accept with reluctance the results of tests on sands, binders, and. such materials made in the chemical laboratory alone. They feel that such tests frequently emphasize and measure properties that are of minor importance and fail to take account of characteristics that are important in determining the value of the material in actual practice. Experience seems to indicate that the most thorough and conclusive, test for any new foundry material is an actual run in the foundry alongside of a standard material of known value. Such a test, however, involves certain difficulties and necessitates certain precautions. It is not always easy to obtain a fair trial for a new material. We all have certain prejudices, which unconsciously affect our judgment to a marked degree. A practical test frequently involves so many workmen, each of whom reacts in a different manner to the test, that; the personal equation becomes very, complex and the true results of the test are obscured. There are times, too, when a thorough experimental trial of a material would interfere too much with the rush of work in a department or would hazard the quality, of the product to such an extent as to make it inadvisable. Under such conditions a laboratory test is advisable before the material is sent into the foundry. These tests should be made as practical as possible and so closely related to foundry practice as to give a true index to the value of a, product for the purpose desired. Core sands and molding sands are as numerous "as the sands of the sea" and vary as much in quality. Old sources of supply are continually failing and new ones must be opened, so that we must continually search for new and better grades of sand. During the past year, the Ohio Brass Co. has developed tests for sands', cores, and binders which bear a close relation to the particular use to which these materials are put in

Jan 9, 1920

By R. J. Quigg, G. S. Doble

Commercial stress -relieved TD Nickel bar was shown to retain room- and elevated-temperature tensile strength after exposure up to 2501°F. Cold swaging increased both room -temperature and 2000°F tensile strength. After annealing at 2500°F the strengthening due to swaging was retained at 2000°F hilt eliminated at room temperature. Annealing produced changes in hardness and X-ray half peak width indicating the presence of recovery processes as 1071° as 1000°F but no recrystallization of swaged material was noted at any temperature. In contrast to swaging, rolling induced a recrystal-lized structure after annealing. The tensile strength of this recrystallized structure was comparable to the cold-worked condition. High-temperature tensile properties of as -received bar were highly anisotropic with the transverse tensile strength being one fifth the longitudinal value. The aniso-/ropy is affected by working direction and may he partially reversed by changing the direction of metal flow. The divergence in tensile strength, beginning above 550°F or- approximate one third the absolute melting point, is strain-rate dependent. T D Nickel is a commercial dispersion-hardened alloy containing 2 vol pct thoria. The dispersion, consisting of spherical particles 0.030 to 0.050 in diameter with an interparticle spacing of less than 1 is reported to maintain stable properties up to 2400°F.1 This stability of second phase results in maintenance of elevated-temperature strength at higher temperatures and longer times than normal nickel-base superalloys.2 The purpose of this paper is to describe the effect of various mechanical working operations on the strength and microstructural stability of TD Nickel bar. MATERIAL AND PROCEDURES All material used in this study was commercial TD Nickel bar. This material is produced by a chemical process which results in a nickel powder containing a dispersion of thoria particles. The powder is then pressed, sintered, extruded, and subsequently worked to bar stock. Three starting materials from three separate lots were used: as-extruded bar. 1-in.-diam stress-relieved bar, and 1/2-in.-diam stress-relieved bar. Since TD Nickel bar stock is cold-worked without a recrystalliza-tion anneal, the accumulated deformation or degree of cold work in these materials increases as the bar diameter decreases. Some of the 1/2-in.-diam bar was swaged to 1/4 in. diameter at room temperature in order to produce an as-worked condition for comparison with the stress-relieved stock. Tensile testing was performed on an Instron Tensile Tester at a constant crosshead speed of 0.020 in. per min. The 0.2 pct offset yield strength was measured from the load-crosshead movement plot. Specimen gage dimensions were 0.080 in. in diameter by 0.40 in. in length, producing a strain rate of approximately 0.050 min-1. Specimens were tested in air and heated within a resistance-wound furnace controlled to ±5°F. A 15-min soak at temperature was employed before testing. Samples were heat-treated in air and specimens machined after exposure with sufficient material removed to eliminate any surface contamination. X-ray line breadth was determined from a diffractometer scan of a transverse face of a bar using copper K, radiation. Metallographic preparation utilized standard mechanical polishing with Carapella's etch. Specimens for electron microscopy were electropolished in a 1:7 sulfuric/methaol solution and chromium-shadowed collodion replicas prepared. RESULTS AND DISCUSSION I) Effect of Elevated-Temperature Exposure on the properties of TD Nickel. The effect of various elevated-temperature exposures on the room-temperature tensile strength of TD Nickel is shown in Table I. In the unexposed condition the tensile strength, reduction in area, and hardness all increase with increasing accumulated deformation while the elongation decreases. After exposure at 2500°F the strength of all three materials decreases to about 65,000 psi and the elongations increase slightly. The apparent increase in strength of the 1-in. bar after a 2000°F treatment is probably experimental scatter. These results indicate that the room-temperature strengthening due to additional deformation is annealed out upon elevated-temperature exposure. In contrast to the room-temperature data, the 2000°F tensile strengths increase in order of increasing deformation even after exposure. Although some loss of strength occurs after exposure, much of the effect of working is still maintained at 2000°F. The room-temperature hardness after various

Jan 1, 1965

By C. R. Whitney, G. N. Maniar, D. R. Muzyka

Previous results have shown that Pyromet 860, an Fe-Ni-base heat-resistant alloy, is stable at temperatures as high as 1500°F for aging times as long as 100 hr. This Paper describes the results of long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Times as long as 37,660 hr were employed. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffraction, and microprobe techniques. phase, containing cobalt, nickel, and molybdenum, was detected after extended exposures from 1200" to 1400°F and careful study was performed to describe the kinetics of its formation in this alloy. µ phase formation apparently has little effect on the elevated-tem-perature properties of Pyromet 860. For times as long as 500 hr at 1300°F and below, with µ phase present, m significant effects on ambient temperature properties were noted. For longer times at 1300°F and after 1400°F exposure, the effects of u phase on ambient temperature tensile strength properties are not clear due to y' effects and grain boundary reactions. Electron-vacancy, N,, numbers were calculated using different methods described in literature and correlated with the present findings. In the selection of alloys for use in gas turbine applications, structural stability ranks as a primary criterion. High-temperature strength and cost are also of major concern. With these factors in mind, Pyromet 860 alloy, an Fe-Ni-base superalloy was designed. This alloy combines the cost advantages of Fe-Ni-base alloys such as A-286, 901, and V-57 with improved strength and structural stability'1,2 and no tendency to form the embrittling cellular 77 phase. A previous study3 reported on the stability of Pyro-met 860 at temperatures from 1375" to 157 5°F and times up to 100 hr. That study showed that the y' precipitates increased in size and separation and decreased in number with an increase in time or aging temperature. No deleterious phases were found to occur. In the present work, samples from four production heats were subjected to long-time creep-rupture testing at 1050" to 1400°F at various stress levels. Various heat treatments were used on the starting samples and tests were run up to 37,660 hr. The effects of time, temperature, and stress on the precipitates and their morphologies were studied by optical and electron microscopy, X-ray and electron diffrac- tion, and microprobe techniques. Electron vacancy numbers, Nv , calculations were made by TRW.4 Experimental results are correlated with the Nv data used to predict occurrence of intermetallic phases such as a phase. EXPERIMENTAL PROCEDURE Mechanical Tests. Material for the present study came from four production size heats of Pyromet 860 alloy, weighing from about 3000 to about 10,000 lb. All of these heats were made by vacuum induction melting plus consumable electrode vacuum remelting. The nominal analysis for this alloy is compared with the actual analysis of the four heats in Table I. Sections of these heats were forged to 9/16-in. round bar,3/4-in. square bar, 3-in. round bar, 4-in. square bar, and a gas turbine blade forging about 16 in, long, about 6 in. wide, and weighing about 20 lb. In general, all forging of this alloy is done from a 2050°F furnace temperature. Longitudinal test blanks were cut from the centers of the smaller bars, from mid-radius positions for the 3- and 4-in. bars, and from the air foil of the gas turbine blade and heat-treated according to the procedures outlined in Table 11. Heat treatment A is the "standard treatment" recommended for this alloy for best all-around strength and ductility. Heat treatment B is a modification of treatment A for improved tensile strength at moderate temperatures. The treatment coded C was designed for treating large sections according to a procedure previously described.' Heat treatment D was developed to yield optimum stress relaxation characteristics at 1050°F for a steam turbine bolting application. After heat treatment, the test blanks were machined either to plain bar creep specimens with a gage diameter of 0.252 in., to combination smooth-notched stress-rupture bars with a plain bar diameter of 0.178 in. and a concentration factor of Kt 3.8' at the notched section, or to notch-only specimens. All specimens conformed to ASTM requirements. Metallography. Most of the creep-rupture tests were continued to failure. A few bars were fractured as smooth or notch tensiles after creep-rupture exposures. After fracturing, ordinary metallographic sections were made primarily in gage areas adjacent to fractures to represent a "high-stress" region and through specimen threads to represent a "low-stress" region. All metallographic sections were made in a longitudinal direction with respect to the test specimen axes. For optical microscopy, the samples were etched in glyceregia (15 ml HC1, 5 ml HNO,, 10 ml glycerol). For XRD analysis, the phases were extracted electrolytically in two media: 20 pct &Po4 in H20 for selective extraction of y' and 10 pct HC1 in methanol for carbides and other phases.

Jan 1, 1970

By W. T. Bishop

For many years pine oil has been used extensively as a frother for the flotation of minerals, particularly sulphides, yet the published information available to the average user on its composition, chemical and physical properties, has been rather meager. It is the purpose of this paper to discuss these points and their relationship to the frothing properties of pine oil used in flotation processes. Pine oil, as the name implies, is a liquid obtained from the processing of wood of the longleaf and other southern pines. It is a complex mixture of naturally occurring terpene derivatives, primarily alcohols, and a smaller amount of terpenes, which has found many uses in various industries. Its use as a frother in flotation processes was the first large-scale application in industry and today the mining industry still consumes large quantities of pine oil but the textile and disinfectant industries consume comparable volumes. Much is used in soap manufacture and laundry operations. The surface-active properties of pine oil are in a large degree responsible for this versatility. History The name "Naval Stores" goes back to the days when pine tar and pitch were used to caulk leaky ships and 'Oat their ropes and rigging. Today this term is still used to include not only the oleoresinous products of the pine tree—rosin and turpentine— but other products such as pine oil, pine tar, and the many terpene and resinous compounds obtained by extracting the pine wood or tapping the tree. That part of the industry known as "wood naval stores" dates from about the beginning of this century and today produces a large part of the country's rosin and turpentine by processing pine wood. In addition, all of our natural pine oil is supplied by the wood naval stores industry, as tapping of the live tree gives only rosin and turpentine. This latter phase is known as the "gum naval stores " industry. The first successful commercial operation of the steam and solvent process of the wood naval stores in industry was carried out by Yaryan at Cadillac, Mich., in 1909.1 This operation did not prove profitable, so Yaryan went south to utilize the longleaf pine, and built a plant at Gulfport, Miss.2 Soon after, another plant was built at Brunswick, Ga., which is still in operation, and in 1914 was reported to have processed about 500 tons of wood per day.' In 1921 Hercules Powder Co. acquired the Yaryan interests, at which time the production of pine oil was only 3 to 5 million pounds per year and flotation was the largest customer. As time went on, technological advances were made, other companies entered the field, and the production of pine oil increased many fold. The growth of the industry was especially marked during the past 10 years, and in

Jan 1, 1947

By W. T. Bishop

For many years pine oil has been used extensively as a frother for the flotation of minerals, particularly sulphides, yet the published information available to the average user on its composition, chemical and physical properties, has been rather meager. It is the purpose of this paper to discuss these points and their relationship to the frothing properties of pine oil used in flotation processes. Pine oil, as the name implies, is a liquid obtained from the processing of wood of the longleaf and other southern pines. It is a complex mixture of naturally occurring terpene derivatives, primarily alcohols, and a smaller amount of terpenes, which has found many uses in various industries. Its use as a frother in flotation processes was the first large-scale application in industry and today the mining industry still consumes large quantities of pine oil but the textile and disinfectant industries consume comparable volumes. Much is used in soap manufacture and laundry operations. The surface-active properties of pine oil are in a large degree responsible for this versatility. History The name "Naval Stores" goes back to the days when pine tar and pitch were used to caulk leaky ships and 'Oat their ropes and rigging. Today this term is still used to include not only the oleoresinous products of the pine tree—rosin and turpentine— but other products such as pine oil, pine tar, and the many terpene and resinous compounds obtained by extracting the pine wood or tapping the tree. That part of the industry known as "wood naval stores" dates from about the beginning of this century and today produces a large part of the country's rosin and turpentine by processing pine wood. In addition, all of our natural pine oil is supplied by the wood naval stores industry, as tapping of the live tree gives only rosin and turpentine. This latter phase is known as the "gum naval stores " industry. The first successful commercial operation of the steam and solvent process of the wood naval stores in industry was carried out by Yaryan at Cadillac, Mich., in 1909.1 This operation did not prove profitable, so Yaryan went south to utilize the longleaf pine, and built a plant at Gulfport, Miss.2 Soon after, another plant was built at Brunswick, Ga., which is still in operation, and in 1914 was reported to have processed about 500 tons of wood per day.' In 1921 Hercules Powder Co. acquired the Yaryan interests, at which time the production of pine oil was only 3 to 5 million pounds per year and flotation was the largest customer. As time went on, technological advances were made, other companies entered the field, and the production of pine oil increased many fold. The growth of the industry was especially marked during the past 10 years, and in

Jan 1, 1947

By R. W. Jenkins

RACKLESS equipment is being used by the T Coplay Cement Manufacturing Co. to develop a folded limestone deposit economically and safely with inexperienced men. Cost and quality of development stone results in a saving when it is used instead of outside sources of limestone. This favorable cost has been attained by following a methods development and training program described in this paper. It is expected that further savings in favor of the mined stone will be made when stopes now being prepared are in production. The present equipment will be used for loading from stope draw points. The limestone is blended with quarried cement rock to serve as raw material for Portland cement, first produced in this country by Coplay Cement Manufacturing Co. from a process developed by its president, David 0. Saylor, in 1873. For many years the cement rock alone or with a small amount of added limestone was used for raw materials. Later as specifications were raised and the richer portions of quarries were depleted, limestone from outside sources was required in increasing amounts. In 1925 D. J. Uhle, the general manager, began to prospect company property for limestone. It was known that the argillaceous cement rock was underlain by crystalline high calcium limestone. After an extensive drilling program it was found that there were large reserves of limestone underlying a recumbent syncline exposed in the south wall of the company's No. 3 cement rock quarry. A quarry was started on the vertical limb of this fold in 1927, and by 1930 the full requirement of the plant was met. After 1945 production diminished because of the occurrence of dolomite beds in the south wall. The quarry floor was then 135 ft below the cement rock level and 285 ft below surface. In 1949 Gerald I?.

Jan 1, 1955

By M. C. Smith, W. V. Green, D. M. Olsen

The creep-rupture behavior of commercial powder-metallurgy molybdenum rod is reported in the temperature range 1600" to 250O°C, at stresses up to 9000 psi and times up to 1 month. The effects of temperature, stress, and grain growth are discussed. Rupture time is fitted to the Larson-Miller parameter and compared to lower-temperature and higher-stress results reported by pugh.1 BECAUSE of its high melting point, molybdenum should retain useful strength to relatively high temperatures. Combined with its ready availability in the United States, this makes it attractive for many applications in missiles, rockets, and so forth—wherever its susceptibility to oxidation can be tolerated or overcome. The mechanical properties of molybdenum rod in the temperature range —200" to 1540°C have been reported by pugh,' Bechtold,' Parke,3 and Carriker and Guard.4 Madden and chen5 have measured the tensile properties of molybdenum single crystals in vacuum up to about 2500°C. As one further step in evaluating its mechanical usefulness, the constant-load creep-rupture properties of commercial powder-metallurgy molybdenum rod have been investigated in the range 1600" to 2500°C. MATERIAL TESTED Creep specimens were machined from 1/2-in. round commercial molybdenum rod, manufactured from powder by pressing, sintering, and swaging. Spectrochemical analysis of the rod showed "traces" (less than 0.01 pct) of silicon, aluminum, chromium, iron, and zirconium, and "faint traces" (less than 0.001 pct) of manganese, magnesium, cobalt, and nickel. Carbon content was 130 to 200 ppm, nitrogen was 110 to 180 ppm, and oxygen 30 to 35 ppm. A typical microstructure of the as-received rod is shown in Fig. 1. Room temperature tensile properties for five specimens strained at about 0.015 in. per in. per min are shown in Table I. CREEP SPECIMENS USED The specimens used for creep-rupture testing are illustrated in Fig. 2. The 1/4-in.-diam gage section was 3/4 in. long, and terminated at shoulders 5 mils high. These shoulders served as fiducial marks for optical strain measurements. Surface finish on the gage section was 16pin. r.m.s. One specimen, for a "long-time" test described below, was modified by dividing the 3/4-in. gage length into three 1/4-in. long sections with individual diameters of 0.250, 0.230, and 0.210 in., each terminating in a pair of fiducial shoulders. TESTING PROCEDURE The constant-load creep-testing machine used has been described by Smith, Olson, and Brown.6 In it the specimen is held vertically on the axis of a cylindrical tantalum or tungsten heater tube by threaded molybdenum or tungsten grips. Both specimen and grips are heated by radiation from the heater-tube, which is heated by its own electrical resistance. The bottom specimen grip is held at its lower end by a clevis pin. The testing load is applied to the specimen through the upper grip by means of hanging weights, a constant force-multiplication lever system, and a pull rod sealed to the chamber lid by a bellows. The incandescent specimen is viewed by an external optical system through slots in the heater-tube and radiation shielding, and an enlarged image of it is projected on a ground-glass screen. Gage-length measurements are made on this image with a pair of cathetometers. Thorium oxide coatings were applied to the threaded ends of most specimens, to prevent diffusion-welding of specimens to grips during testing. Without such a coating welding usually occurred, and grips were often broken by subsequent efforts to remove the tested specimens.

Jan 1, 1960

By A. Gatti

Studies were made on the system iron plus alumina. Various methods of dispersing and various amounts of alumina were used. Powder metallurgy techniques were used to produce the final product. Microstructures and some mechanical properties are presented. Alloys containing up to 16 pct alumina by weight are ductile at all temperatures tested. The ivon-alumina materials have a higher yield stress and improved creep resistance over that of pure iron. SINCE the development of SAP' an A1- Al2O3 powder metallurgy product, great interest has been shown in the development of a SAP-like structure in metals and alloys other than aluminum. The outstanding properties of this class of materials are: 1) Good creep resistance at high temperature. 2) High yield strengths and high hardness at high temperatures. 3) High recrystallization temperature. However, the lack of ductility and formability has thus far limited the applications of SAP-like materials. The following report deals with methods of dispersing A12O3 in Fe, processing of powders into rod, structures produced after processing, and mechanical properties of the iron-alumina material produced. Methods of dispersing the alumina and also the volume fraction of alumina added were varied. MATERIAL Powder Processing— Four methods of obtaining dispersions of alumina in iron were studied. 1) Oxidation-reduction of a Fe + 8 pct Al alloy. .2) Coprecipitation of Fe(OH)3 + Al(OH)3 from aqueous solution. 3) Colloidal mixing of Fe,O3 and Al2O3. 4) Colloidal mixing of Fe powder and A1,O3. Fig. 1 is a processing flowsheet which outlines the processing steps taken to produce a final extruded bar 1/4 in. in diameter and about 30 in. long. The - 100 mesh iron-aluminum alloy was oxidized by placing a thin layer of powder on an alumina plaque. The reduction step was modified to include 1/2 hr at 1000°C since the powders tended to become pyro-phoric unless sintered slightly after low-temperature reduction. Compacting was done in a 1-1/8-in.-diam pressing die. The slugs produced averaged 1 in. in length. The billets were encased in low-carbon steel cans shown schematically in Fig. 2. The blank is included for structure and property comparison purposes. TESTING PROCEDURE All tests were made on as-extruded material.

Jan 1, 1960

By Luther Lennox

DURING the last few years, one of the great problems in the milling of all ores has been that of crushing. This subject involves not merely the cost of the operation, but also the selection of the proper degree and character of crushing to yield the best metallurgical results on the given ore. Considering the diversity of machinery, one is led to wonder at the variety of crushing methods employed, even when realizing that metallurgy demands varying products. In an attempt to investigate the relative crushing resistances of a number of ores now being milled in this country and Alaska, the management of the Portland mills requested samples of average mill-run of ore from various companies. The request met with a ready response, indicating the desire of all operators to gain information on the subject. The difficulties involved in this investigation were numerous, lack of time for outside problems during this strenuous period being a serious one. Also, we were unable, in the time, to obtain a correct 150-mesh . screen; in the screen analyses tabulated and plotted herewith, the 150 mesh screen was used merely to protect the 200-mesh screen, not to ascertain points on the curves.

Jan 8, 1918

By E. R. Buchanan, R. E. Reed-Hill

A transmission electron microscope study was made of magnesium single crystals deformed in torsion using the basal pole as the forsional axis. While this type of deformation is predicted to result in the formation of hexagonal networks of screw dislocations, these networks were not observed. The basic dislocation arrangement consisted of arrays of nearly parallel and approximately equally spaced dislocations. The average dislocation density was over an order of magnitude higher than that required to account for the torsional deformation. The observed high rate of work hardening in these crystals is consistent with both their high dislocation densities and the arrangement of dislocations in pile-ups. The experimental observations are also in agreement with the assumption that dislocation sources are activated not only at the surface but at interior locations as well. In considering torsional deformation, Amelinckx and Dekeyser1 postulated that when a torque is applied to a crystal oriented with a glide plane normal to the specimen axis, deformation occurs by the following steps: 1) Nucleation of dislocation sources at or near the specimen surface in areas where the shear stress, resolved along a slip Burgers vector, is a maximum; 2) the screw orientations of the dislocations accommodating the twist move inwards towards the specimen center. If two glide directions lie on the glide plane, the geometry shown in Fig. 1 should result; 3) the screw dislocations that pile up in the central part of the specimen cross-slip to form a grid. At the same time, screws of opposite sign and most edges leave the specimen. Tinder,2 using zinc crystals twisted about the basal pole, independently reached essentially the same conclusions. He suggested a mechanism involving nucleation of ?(1120) screw dislocations at the six points of highest resolved shear stress that lie on the cross-section near the surface. Under the applied shear stress these dislocations were assumed to move inward and interact so as to form a hexagonal network of screw dislocations. Today it is often accepted that rotational slip occurs by a mechanism of the above type, but to our understanding this has never been experimentally proved. This paper reports an experimental study of rotational slip, using magnesium single crystals, that indicates that in this metal rotational slip does not conform well to this mechanism. EXPERIMENTAL PROCEDURES Mechanical Testing. Specimens with a (0002) axis were prepared from magnesium crystals of 99.95 pct purity grown by Jillson's3 modified Bridgman technique. The crystals were acid machined into cylindri-

Jan 1, 1970

By H. Van F. Furman

TO those engaged in the purchase and sale of gold- and silverores, mattes and bullion, the frequent differences in the gold- and silver-contents, as reported by different assayers, is a source of much annoyance and expense. The desirability of uniform methods of assay has long been recognized by certain refiners who specify in their bullion-contracts the method to be adopted in assaying the bullion. One large producer of base bullion employs at each refining-works with whom it has a bullion contract an assayer whose duty it is to see that the bullion is sampled and assayed according to contract-specifications. For the assay of gold- and silver-bullion, standard methods are now generally adopted; the reeult being that differences seldom occur. While we cannot hope for anything near perfection from fireassay methods for ores, mattes and base bullion, as carried out cornmercially, such methods may be made to yield results which answer all commercial requirements, and they will probably be retained for obvious reasons. The object of the present paper is to point out some of the sources of error and to show the importance of more uniform methods of assay and close attention to the details of the work. The sources of error in the assay of ores and mattes are: improper sampling; losses of the precious metals during fusion, scorification and cupellation; imperfect elimination of the base metals on the cupel and imperfect extraction of the silver during the parting in nitric acid. It is not the object of the present paper to enter upon the subject of sampling; but a few remarks may be of value. There has been considerable discussion recently in Colorado upon the frequent differences which occur in the assays of Cripple Creek gold-ores, and these differences have been attributed to various causes. The writer is informed by two of our most prominent smelters that since they have adopted 100-mesh screens (the general practice is 80-mesh) the

Jan 1, 1895

By W. E. Quist, R. Taggart, D. H. Polonis, C. J. van der Wekken

An intermediate compound that has been identified as Niab is observed to form as a decomposition product from supersaturaled Ni-Nb solid solutions during aging at temperatures between approximately 300" and 500°C. On the basis of data from electron microscopy and selected-area diffraction, the structure of this compound has been determined as fct with a = b - 3a0 and c = a, wlzere a,, is the lattice parameter of the parent solid solution. The compound consists of close-packed layers with triangular ordering, where the niobiutrl atoms are separated by two nickel atoms ([long- close?-packed directions. A nine layer stacking sequence is required to describe the proposed structure. STUDIES of the Ni-Nb binary system have been limited primarily to phase diagram determinations,'-4 investigations of high-temperature equilibrium phases,5"1 and the determination of the influence of deformation on the structure of the equilibrium compound.8 The nickel-rich portion of the binary system is reported to be of the simple eutectic type in which the maximum solubility of 12.7 at. pct Nb occurs at 1282"c.' The two-phase field below the eutectic temperature is bounded by the a fcc solid solution and an orthorhombic Ni3Nb compound. No metastable phases have been reported in previous investigations. In transformation studies of certain nickel-base commercial alloys that contain niobium, two ordered metastable compounds containing niobium have been shown to precipitate from the solid solution, both of which have been identified as y' and have the composition NisNb or Ni,Nb. One compound has been reported to have the bct DOz2 type Al3Ti structure" and the other the cubic LI2 type Cu3Au structure.9,11 In the present work on Ni-Nb binary alloys a metastable y' compound has not been detected after conventional quenching and aging treatments. An anomalous behavior was noted in electrical resistivity measurements. in alloys containing between 7 to 12 at. pct Nb when aging treatments were performed below 500°C after fast quenching from 1250°C. Transmission electron microscopy has shown that this behavior is caused by the formation of a low-temperature precipitate of unreported structure type and composition. EXPERIMENTAL METHODS Several Ni-Nb alloys, containing up to 11.5 at. pct Nb. were prepared by either levitation melting and casting in copper molds or by induction melting in alumina crucibles; both techniques employed purified helium gas as a protective atmosphere. The purity of the nickel and niobium used to make the alloys was 99.98 wt pct Ni and 99.9 wt pct Nb. The composition and homogeneity of the alloys were checked by weight measurements and by electron microprobe analysis. The induction-melted alloys were homogenized for 100 hr at 1100°C. The resistivity specimens were prepared from rods swaged to 2.5 mm and the electron microscopy specimens were cut from sheet that was rolled to 0.4 mm and thinned using a modified Bollmann technique." The elevated-temperature solution treatments were carried out in a purified helium atmosphere followed by direct quenching into a 10 pct NaCl solution at 23°C. Additional protection against oxidation of the samples during solution treatment was accomplished by using tantalum foil as a "getter" in the furnace. The specimens were aged at various temperatures in salt baths controlled to +2oC. A Leeds and Northrup K5 potentiometer was used to make electrical resistivity measurements on specimens immersed in liquid nitrogen. Electron microscopy and diffraction studies were carried out with JEM-7 and Philips EM-200 microscopes operating at 100 kv. RESULTS AND DISCUSSION Ni-Nb alloys containing between 7 and 11.5 at. pct Nb that have been solution-treated in the range 1220" to 1280°C and quenched to 23°C undergo a precipitation reaction when aged in the temperature range 300" to 500°C. Precipitation was detected by selected-area electron diffraction after aging a specimen for as little as 30 sec at 350°C) whereas the reaction was well-advanced after aging for 150 hr at 475°C. Electrical resistivity measurements were used to monitor the progress of the precipitation reaction. In the present experiments the nucleation process for precipitation required a high solution temperature and a rapid quench into brine. The presence of aluminum, iron? and carbon in amounts totaling less than 1 wt pct was found by electron diffraction to completely suppress the formation of the low-temperature precipitate that has been detected in the binary alloy. Electron diffraction techniques were used to determine the structure of the precipitates that formed during the decomposition of the Ni-Nb supersaturated solid solutions. Figs. l(a) through l(d) show electron diffraction patterns oriented to the [loo], [110], [lll], and [I031 zone axes of the matrix. Areas of reciprocal space between these sections were investigated by slowly varying the orientations of the crystal under study; this procedure revealed no reflections other than those depicted in Fig. 1. The presence of super-lattice reflections at points coincident with the matrix reflections was confirmed by the examination of an almost completely transformed structure. On the basis of the accumulated diffraction data, the reciprocal lat-

Jan 1, 1970

By Marius S. Darrow, William B. White, Rustum Roy

The PbS-PbTe systen has been studied by quench-ing and D.T.A. techniques f?om 400' to 1150°C. Runs were made in evacuated silica tubes so that all equilibria are at the vapor pressure of the system. Lattice parameters of the quenched salnples , measured by X-ray diffraction, show a complete crystalline-solution series existing over a narrow temperature range between approximately 805" and 871°C. An exsolution dome extends from a maximum of about 805"C (approximately 30 mole pct PbTe) to 1 and 96.5 pet PbTe at 400°C. A narrow melting region, deternined by D.T.A., extends form 918c (mp PbTe), The shapes of the liquides and solidus curves imply the existence of a minimum at 871°C at approximately 65 pct PbTe. THe exact composition of the minimum could not be established due to the very narrow two-phase region. At compositions containing less than 50 pet PbTe, liquidus temperatures begin to increase, while the solidus remains almost flat to about 15 mole pet PbTe before beginning to vise toward the mp of PbS (1075 C). LEAD sulfide and lead telluride are isostructural (NaC1 type) semiconductors whose electrical and optical properties have been extensively studied and used in recent years. If appreciable crystalline solution exists between these compounds, the variation of physical properties with composition could be of interest. The purpose of this investigation was to determine the extent, if any. of crystalline solution, and to obtain the phase diagram for the system. To the knowledge of the authors, only three studies of the system PbS-PbTe have been reported, and, in chronological order, each investigation found an increasing amount of crystalline solution. In 1956, Yamamoto reported finding no evidence of crystalline solution between the compounds. Sindeyeva and Godov-ikov,' in 1959, found very limited crystalline solution. but only under conditions of excess tellurium concentration. Finally Melevski s3 investigation in 1963 indicated that one solid phase exists in the region from PbS to 7 pct PbTe and from 82 pct PbTe to PbTe at 886'C, with an eutectic at 55 pct PbTe at that temperature. Detailed data on the solvus boundary were not given. EXPERIMENTAL EQUIPMENT AND MATERIALS Commercially produced PbTe and PbS powders were used as starting materials. Batches of specific mole percent composition were accurately weighed and mixed in a plastic bottle, in a shaker mill. An analy- sis of impurity content is given in Table I for pure PbS and PbTe and for two randomly selected batches after the powders were mixed. Individual samples, ranging in weight from 0.2 to 0.5 g, were sealed in evacuated silica tubes which had been thoroughly washed and rinsed with acetone and distilled water. Thus all data taken were at the pressure of the system. Subsolidus relations were studied down to 400°C by heating the samples in a vertical tube furnace for 24 hr. The sealed tubes were quenched in water with quench time from the hot zone not exceeding 1 sec. Temperatures were measured by a chromel-alumel thermocouple and controlled to 53°C for most runs. The number and composition of phases present were determined from powder X-ray diffraction patterns taken at room temperature on a Norelco diffractome-ter, using silicon as an external standard. Above 850°C quenching techniques were, in general, found to be unsatisfactory, and differential thermal analysis (D.T.A.) was used to determine melting relations. The evacuated tubes were recessed about 1 cm at one end to accommodate the differential thermocouple. Al203 was used as the reference material in a similar tube containing the other side of the differential couple. For temperature measurements, a separate thermocouple was placed in the recess of the tube containing the sample to be measured, thus providing an opportunity to obtain thermal, as well as differential, analysis. All thermocouples for these measurements were Pt-Pt 10 pct Rh. Temperature and differential curves were recorded separately on synchronized strip-chart recorders. Thermocouples and recording equipment were calibrated using NaCl and gold standards, using the melting points 801" and 1063 C, respectively, which span most of the temperature range of interest. Heating and cooling rates generally were from 4 to 7°C per min. It was found, in fact. that rates ranging from 1.5 to 25°C per min did not significantly change the data obtained.

Jan 1, 1967