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By Raymond L. Jones

With the inauguration of open-pit copper mining in Bagdad, Ariz., plans were formulated for a large scale leaching operation. Dump stockpiling was started almost immediately, but actual production was not initiated until spring 1961.

Jan 9, 1977

By C. O. Dale, W. J. Rundle

THE upper Mississippi Valley zinc-lead area was the first major lead-producing section in the United States. The lead ore, found near the surface in crevices, was relatively pure galena that could be smelted directly into lead, at first in log hearth furnaces and later in more efficient blast type furnaces. French Canadian fur traders encouraged the Indians to mine the lead ore and showed them how to smelt it into lead that had a high value for bullets1 Nicholas Perrot found lead ore on the Mississippi River bluffs near the junction of Wisconsin and Illinois and in 1690 established a trading post on the Wisconsin side of the river opposite the present site of Dubuque, Iowa.2 Shortly after 1720 discovery of Mine La Mott in Missouri diverted considerable attention from the Upper Mississippi area. Mining continued on a desultory basis with operations concentrated in the Galena, Illinois-Dubuque, area. In 1740 at least 20 miners were at work in the Fever River area around Galena and are reported to have shipped 2500 70-lb pigs of lead to Kaskaskia in 1741." Julien Dubuque established a mining and smelting operation in 1790 near the city that bears his name and was granted sole right to exploit the mining operations on the lands of the Sauk and the Fox Indians. He is reported to have produced 30,000 70-lb pigs of lead in 1805. Following the death of Dubuque in 1810 the Indians refused to let the white miners enter their lands, and little was done on the Iowa side of the river until the Indians were removed by treaty with the United States government in 1832." Early mining was entirely for lead but as the crevices were followed down, increasing percentages of zinc sulphide and zinc carbonate were encountered and at first discarded. Later a market became available for the zinc ores, and hand jigging devices were made to separate the lead, the zinc, and the rock or waste materials. The first record of zinc production from the area is for 1860. Production of zinc passed that of lead before 1900, reached a peak of 64,000 short tons in 1917, fell off rapidly and continually to about 2000 short tons in 1938, and since 1940 has ranged from 11,000 to 19,000 short tons. Lead has been of considerably less importance since 1900, and at present only about 10 pct as much lead as zinc is produced. Practically all of the zinc ore has come from orebodies that are rather flat and wide with considerable length as compared to width. Most of the early lead came from the crevice type deposit, but present production is from the predominately flat zinc orebodies. The Graham-Snyder orebody, scene of Eagle Picher operations, is practically all zinc with little or no lead being recovered. Marcasite, present in varying amounts, makes production of finished concentrates by gravity separation impractical. Satisfactory lead and zinc concentrates have been produced since flotation was introduced in the area in 1927. An acid recovery plant was operated for about 20 years after World War I, but it has been dismantled, and no recovery of the iron sulphides in the ores of the district is being made at the present time. In June 1950 there were three companies operating mines and mills, Tri-State Zinc Co., Calumet & Hecla Consolidated Copper Co., and Eagle Picher Mining and Smelting Co. The Vinegar Hill Zinc Co. had completed a shaft at a new orebody and had started to develop the mine which will supply the Cuba City mill. The Cuba Mining Co. was holding the Andrews Mine inactive. The Dodgeville Mining Co. was not operating but was exploring for additional reserves. Several small mines were selling ore to the Eagle Picher mill. A general area map is given in Fig. 1. The Eagle Picher Mining and Smelting Co. entered the area in 1946 with an active exploration campaign. Leases on a block basis were secured for the area south from the Wisconsin-Illinois line near

Jan 1, 1953

By C. O. Dale, W. J. Rundle

THE upper Mississippi Valley zinc-lead area was the first major lead-producing section in the United States. The lead ore, found near the surface in crevices, was relatively pure galena that could be smelted directly into lead, at first in log hearth furnaces and later in more efficient blast type furnaces. French Canadian fur traders encouraged the Indians to mine the lead ore and showed them how to smelt it into lead that had a high value for bullets1 Nicholas Perrot found lead ore on the Mississippi River bluffs near the junction of Wisconsin and Illinois and in 1690 established a trading post on the Wisconsin side of the river opposite the present site of Dubuque, Iowa.2 Shortly after 1720 discovery of Mine La Mott in Missouri diverted considerable attention from the Upper Mississippi area. Mining continued on a desultory basis with operations concentrated in the Galena, Illinois-Dubuque, area. In 1740 at least 20 miners were at work in the Fever River area around Galena and are reported to have shipped 2500 70-lb pigs of lead to Kaskaskia in 1741." Julien Dubuque established a mining and smelting operation in 1790 near the city that bears his name and was granted sole right to exploit the mining operations on the lands of the Sauk and the Fox Indians. He is reported to have produced 30,000 70-lb pigs of lead in 1805. Following the death of Dubuque in 1810 the Indians refused to let the white miners enter their lands, and little was done on the Iowa side of the river until the Indians were removed by treaty with the United States government in 1832." Early mining was entirely for lead but as the crevices were followed down, increasing percentages of zinc sulphide and zinc carbonate were encountered and at first discarded. Later a market became available for the zinc ores, and hand jigging devices were made to separate the lead, the zinc, and the rock or waste materials. The first record of zinc production from the area is for 1860. Production of zinc passed that of lead before 1900, reached a peak of 64,000 short tons in 1917, fell off rapidly and continually to about 2000 short tons in 1938, and since 1940 has ranged from 11,000 to 19,000 short tons. Lead has been of considerably less importance since 1900, and at present only about 10 pct as much lead as zinc is produced. Practically all of the zinc ore has come from orebodies that are rather flat and wide with considerable length as compared to width. Most of the early lead came from the crevice type deposit, but present production is from the predominately flat zinc orebodies. The Graham-Snyder orebody, scene of Eagle Picher operations, is practically all zinc with little or no lead being recovered. Marcasite, present in varying amounts, makes production of finished concentrates by gravity separation impractical. Satisfactory lead and zinc concentrates have been produced since flotation was introduced in the area in 1927. An acid recovery plant was operated for about 20 years after World War I, but it has been dismantled, and no recovery of the iron sulphides in the ores of the district is being made at the present time. In June 1950 there were three companies operating mines and mills, Tri-State Zinc Co., Calumet & Hecla Consolidated Copper Co., and Eagle Picher Mining and Smelting Co. The Vinegar Hill Zinc Co. had completed a shaft at a new orebody and had started to develop the mine which will supply the Cuba City mill. The Cuba Mining Co. was holding the Andrews Mine inactive. The Dodgeville Mining Co. was not operating but was exploring for additional reserves. Several small mines were selling ore to the Eagle Picher mill. A general area map is given in Fig. 1. The Eagle Picher Mining and Smelting Co. entered the area in 1946 with an active exploration campaign. Leases on a block basis were secured for the area south from the Wisconsin-Illinois line near

Jan 1, 1953

EDITORIAL comments on the anthracite report of the Federal Fact-finding Coal Commission, which became public on July 5, together with an analysis of its more important conclusions, will be found on another page of this issue. In this place, only a few extracts from the report, bearing more directly on technical matters, can be quoted, for lack of space. COST OF MINING Mining cost, as it stands on the books of each mining company, represents the average cost of the total output, all sizes, of anthracite. Egg coal has at least five times the market value of barley, but these' sizes are mined together and their costs can not be separated. Mine costs directly reflect the conditions under which these deposits of coal are recovered. Even within the few counties in which anthracite is found there is a conspicuous range of natural conditions. The distinc-tion between the Northern, Middle, and Southern field, or, as they are also termed, the Wyoming, Lehigh, and Schuykill regions, is primarily geologic and topo-graphic, but the effects of the natural conditions largely control costs. The contrast is great between Some of the level-lying beds of moderate but fairly constant thickness under the broad Wyoming Valley, where mining and underground haulage present relatively simple problems to the engineer, and the steeply pitching or overturned and faulted beds of variable thickness in the Schuykill field, where crushed coal' and treacherous roof multiply the difficulties of mining; and increase the unavoidable waste. Even more direct is the connection between geologic processes and the, differences in the character of the coal as mined, the varying proportions of large and small sizes demanding differences in preparation and resulting in different average prices realized for the product of the mines.

Jan 8, 1923

By F. C. Newton

RefineRs of lead by the Parkes process have always been solicitous of recovering the zinc used in the desilverization, and justly so, as the loss in zinc constitutes one of the heavy costs in this method of refining. Part of this loss is due to the absorption of zinc by lead, and in the present state of knowledge is not recoverable as metallic zinc. The remainder of the zinc, which finds its way into the precious-metal-bearing crust, is recoverable and naturally engages the operators' most exacting attention. Careful elimination of the impurities in base bullion has enabled the refiner to produce a zinc crust better adapted to retorting, which reflects favorably in the zinc recovery;- and to produce a richer crust, thereby lowering the zineking cost, as the increased efficiency of the zinc results in less of it being in circulation. It is obvious that if the ratio of concentration be increased, a lessening of the amount of crust formed will ensue, throwing less work on the retorts and diminishing the amount of retort metal sent to the cupels, thus making an actual money saving in all these operations. In the effort to obtain a rich crust, the metallurgist has increased the heat to a considerable degree, upon the assumption that at the higher temperature the zinc-dver alloy could be squeezed free from the adhering lead. A further possibility for improvement suggested itself in the freezing-point curve of Prof. H. C. Carpenter, upon zinc and silver. Study of this curve disclosed the existence of a definite chemical compound, Zn3Ag2, with a freezing point of 665" C., a promising compound for practical application. In the experiment undertaken it was endeavored to force this compound into the crust, hoping thereby to obtain a higher concentration than formerly. It was recognized that in bringing a large kettle of lead to such a heat, more fuel would be used, the life of the kettle would perhaps be shorter, and other disadvantages would be experienced. AS a commercial operation, the project would have to stand on its own feet,

Jan 1, 1915

By Albert Stazicker

AT Climax the warehouse department operates as an independent unit similar to the mine and mill departments. It has the responsibility of receiving, checking, unloading, and storing all material and supplies delivered to the plant. In addition, the transportation of all supplies comes under the direction of the warehouse so that prompt delivery of supplies to all departments is one of its major functions. The transportation division operates heavy and light trucks, trailers, two large tractors, and two snowplows. In addition to delivering supplies it is also responsible for snow removal from the roads, hauling of sand and gravel for concrete and domestic coal to employees. and all miscellaneous work involving the use of tractors or trucks.

Jan 1, 1946

By R. Havens, K. C. Dean, H. Dolezal

Mine, mill, and smelter wastes aggregating billions of tons are scattered across the country as unattractive barren piles that mar the natural beauty of the land. As the population of the United States increases and the demand for land intensifies, populous centers are slowly encroaching on these formerly isolated wastes. Encroachment sharply intensifies the importance of controlling the air and water pollution derived from natural weathering of such wastes. Use or stabilization of these wastes comprises the only viable means for minimizing pollution. Utilization is preferable to stabilization, because full use would both eliminate the waste and broaden the mineral resource base. However, the wastes typically comprise immense tonnages of materials discarded by selective mining or after recovering the significant mineral values by milling and/or smelting. Only rarely can such low-grade material be reprocessed to extract additional minerals at a profit. Some mineral wastes are suitable for disposal as mine fill, railroad and highway road ballast, and land fill. Similarly, some mineral wastes can be utilized as raw materials for making brick, rock wool, concrete, and ceramic products. Several means exist for stabilization of relatively fine-sized wastes, which constitute the chief sources of air and water pollution. These include physical, chemical, and vegetative stabilization, and combinations thereof. Massive coverings of coarse slag, concrete, and soil may be used to prevent erosion of waste piles. A variety of chemicals can be used to bond the particles of fine-size waste into a relatively inert mass. However, the most promising method of producing an esthetically appealing storage site is vegetative stabilization. Numerous species of plants can germinate, grow, and reseed in waste materials which have been adequately prepared to support plant life.

Jan 3, 1969

By G. L. Tufford, R. L. Bleifuss

Low-grade manganiferous iron ores of Minnesota's Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite with subsequent magnetic separation and flotation have not given satisfactory results because, in many instances, concentrate grade and manganese recovery are low. Metallization of iron and concurrent reduction of higher manganese oxides to MnO, as in the R-N process, followed by recovery of iron by magnetic separation and manganese by leaching, seems to be a technically feasible process. High-temperature x-ray diffraction studies show that solid-state reactions between iron and manganese, with the formation of intermediate iron-manganese oxides, occur during reduction and affect recovery of both iron and manganese from the final product. Solid state reactions also occur between FeO, MnO, and SiO, at temperatures as low as 900°C. The kinetics of these reactions are such that they become an important factor in the treatment of ores by the R-N process. These investigations suggest a temperature and gas composition cycle that would maximize both iron and manganese recovery. During the past ten years, iron ore shipments from the Cuyuna Range of Minnesota have decreased sharp1y. Because of adverse grade, structure, and cost, many Cuyuna ores are no longer competitive with high-grade foreign ores and domestic pellets. The low-grade manganiferous iron ores from the Cuyuna Range, in general, do not respond to conventional mineral dressing techniques because of their fine-grained texture. Reducing these ores to magnetite for subsequent magnetic separation and flotation has not given satisfactory results because concentrate grade and manganese recovery are often low. However, a technically feasible process appears to be metallization of the iron and concurrent reduction of manganese oxides to MnO with recovery of metallic iron by magnetic separation and extraction of manganese from the tailings by leaching. In 1962 the R-N Corp., with a grant from the Area Redevelopment Administration, conducted an amenability study of the metallization of manganiferous iron ore from the Cuyuna Range. The results of this preliminary investigation were sufficient to interest the Economic Development Administration in sponsoring further studies of the process with emphasis on secondary recovery of manganese from the nonmagnetic tailings. Inasmuch as the metallization process has considerable influence on the final form of the manganese - its texture and distribution between the magnetic concentrate and nonmagnetic tailings-the investigation included a study of metallization of the ore as well. Therefore, the investigation conducted at the Mines Experiment Station covered three interrelated phases: (1) laboratory R-N roasting studies and magnetic separation tests, (2) laboratory chemical extraction experiments of the nonmagnetic tailings, and (3) a mineralogical study of the crude ores and their various roast products. High-temperature x-ray diffraction investigation of the Fe-Mn-Si0,-0, system is the main topic of this paper and an extension of the mineralogical work. GENERAL GEOLOGY The Cuyuna Range is known for its complicated geologic structure, complex orebodies, and generally indifferent response to attempts at conventional beneficiation. Several geologists have made intensive studies of the Cuyuna Range, including Leithl (1907), ~darns' (1910), Zapffe3 (1925), Grout and Wolff4 (1955), and schmidt5 (1963), whose study was the most comprehensive of all. The Range is covered with glacial deposits - till, out-wash, and lake sediments -up to 250 ft thick. Bedrock stratigraphic units of the Cuyuna Range consist of three tightly folded Precambrian sedimentary formations. The lower unit is the Mahnomen formation, composed of 2000 or more feet of argillite, slate, siltstone, and quartzite. The middle unit is the Trommald formation, which varies from 45 to 500 ft in thickness and comprises the major iron-bearing formation. The upper unit is the Rabbit Lake formation, consisting of over 2000 it of argillite, slate, and interbedded lenses of lean iron formation. In the central part of the Cuyuna Range, the units have been folded into a series of

Jan 1, 1969

By George T. Hansen

WHY try to find oil in Utah? Why try to find oil anywhere? Isn't there too much oil already? Answers to these questions involve general oil conditions but are pertinent to my subject. In the first place oil produced in Utah up to the total amount of local consumption would not be subject to nor concerned with the national oil situation. An oil field in this State capable of producing up to 15,000 bbl. per day would have a large value and prompt realization. In the sec¬ond place, there is not too much oil nationally although the markets have been upset temporarily from time to time. Petroleum is so necessary and is in such general demand that an oil field anywhere, anytime, is a valuable and live asset. The oil business in general shows the best condition of any major industry. It has never been hit as hard as most industries and 1932 was a large improvement over its low spot of 1931. It can be and probably will be the one to lead the country back into business stability. Consumption of its products has been reduced less than that of any other important commodity. There are good and valid reasons why it should have been making a normal profit continuously. It has the oil and the processes and the facilities and the policies and the consumption of its products. There is only one reason why it has not been profitable recently and that is the lack of intelligence of from five to ten per cent of the producers. An op¬erator lacks intelligence when he cannot see that it is better for him to sell one barrel of oil at $1 than two or three barrels at 25 or 35c. per bbl.

Jan 1, 1933

By W. R. Hibbard Jr., R. W. Guard, N. G. Ainslie

Evidence is presented that copper-base solid solutions of different solutes having equal grain sizes, no preferred crystal-lographic orientation, equal electron-atom ratios, and, within experimental scatter, identical initial yield strengths, need not have identical stress-strain curves at strains larger than about 0.04. The stress-strain behavior is rationalized in terms of the proposed Suzuki chemical interaction between solute atoms and extended dislocations using what is thought to be a somewhat different means of representing stress-strain data. ALTHOUGH the effect: of alloying element upon the strength characteristics of sold solutions is a subject which has received considerable attention in the past, the exact relationships between the common deformation parameters and certain common variables are not really known in some cases. As a result some of the experiments reported in the literature in which these variables are inadequately controlled lose some of their persuasion regarding underlying principles. Nonetheless, facts are known which bear pointing up: When the true stress, a, and true plastic strain, E, of tensile deformatic~n are plotted on a double logarithmic coordinate system, one may observe a straight-line relationship at strains greater than 0.02. The form of the curve in the linear region is given by a = Ken! where a represents true stress, E, true strain, and K and tn, constants. If the relationship holds, K and m define the flow characteristics of the material being tested. m and K, however, may vary with other parameters. Hollomon found that in a-brass, m is influenced by grain size. French and HibbardZ found in alloys of copper that inverse relationships existed between m and 1) the solute concentration for a given solute, 2) the 0.01 yield strength, and 3) the constantK. Lacy and Gensamer3 observed (du/d~) (= U/Em) to increase with increasing values of K in systems of alloyed ferrites (although with considerable scatter of data which may be attributed to uncontrolled grain size). Brick, Martin, and Angier* deduced in copper-base alloys a straight-line relationship (with some scatter) between the change in the Dph number due to solid-solution strengthening and the change in the Dph number due to work hardening which suggested that copper-base alloys having equal yield strengths might have identical stress-strain curves in the plastic flow regions. French and HibbardZ concluded that the yield strength of copper-base solid solutions is the proper basis for comparing the effects of solute elements. Also, Allen, Schofield, and ate' showed that, within their experimental variation, copper-base alloys of zinc, gallium, germanium, and arsenic having the same electron-atom ratios have the same true-stress true-plastic strain curves. Dorn, Pietrokowsky, and ~ietz' also found that with aluminum-base alloys the stress-strain curves in the flow regions are approximately the same if "equivalent" concentrations of alloying elements are used. Solute valence and lattice parameter distortion were the parameters used to determine equivalency. The present report describes an investigation in which an attempt was made to obtain copper-base solid-solution alloys of four solute elements having within close tolerances equal grain sizes and yield strengths, and to see if the level of yield strength does indeed define the flow curve regardless of solute type. During analysis of the data certain unexpected features of the stress-strain curves became apparent which gave rise to some speculation and are discussed at length in the paragraphs that follow. EXPERIMENTAL PROCEDURES Alloy Preparation—Using the data of French and HibbardZ as a first approximation, four different binary copper-base alioys were designed so as to have the same yield strength. In addition, other alloys were prepared in which the solute aoncentrations varied slightly from those calculated above so as to span a range of yield strengths, see Table L The yield strengths of all alloys prepared except the copper-tin alloys were subsequently found to Lie fairly close to one another. The copper used in the alloys was produced by the American Smelting and Refining Co. and was of very high purity (99.999 pct). The alloy additions and their initial purities are as follows:

Jan 1, 1960

By D. A. Elgillani, S. Atak, D. A. Rice, M. C. Fuerstenau, R. B. Bhappu

Quartz and feldspar cannot be floated with sulfonate at any pH; spodumene floats over a narrow acid pH range, while beryl responds moderately over a broad pH range. After wet-grinding in a steel mill, beryl, quartz, and spodumene float well with sulfonate below about pH 7, whereas the improvement in the response of feldspar is not so marked. A mechanism by which iron can be adsorbed on these minerals is presented. Also, the responses of leached, natural, and wet-ground beryl to amine, sulfonate, and oleate flotation are shown and related to the measured zero-points-of-charge of these materials. Earlier work with leached beryl showed that good flotation could be obtained with alkyl aryl sulfonate over a rather wide pH range using a Fagergren flotation cell.' When a similar response was observed with leached quartz, it was decided that unintentional activation was being obtained from the metallic components of the Fagergren cell. To obviate this difficulty, a microflotation cell was designed, and an experimental technique was devised. These have been described elsewhere. Experiments conducted with the small cell showed that leached quartz could not be floated at any pH with any sulfonate addition,3 which is in agreement with the observations of Kraeber and Boppel.4 Similarly, it was also found that leached beryl responded to sulfonate flotation only over a narrow pH range rather than the broad range reported earlier.1 This early work,1 however, revealed the important effect that wet-grinding in a steel mill has on the flotation response of certain silicates. That is, it was found that quartz and especially beryl floated well over an unusually wide pH range after wet-grinding in a steel mill. Microcline, however, floated poorly below pH 4, even though wet-ground under the same conditions. The work of Eigeles6 on adsorption of oleic acid on leached quartz and iron-contaminated quartz at constant pH is in agreement with these flotation data. Other research has shown that ferric iron, added as a salt to the system, functions as an activator in the narrow pH range in which Fe +++ iron hydrolyzes to its hydroxy complexes.3,5 These phenomena indicate that iron functions differently in flotation systems depending on its method of introduction. The object of this paper is to determine the mechanism by which iron is adsorbed on certain minerals, the mechanism of collector adsorption after iron abstraction, and the role that Fe++ and Fe+++ assume in the selective separation of these minerals. EXPERIMENTAL MATERIALS AND METHODS Sodium alkyl aryl sulfonate, mol wt 450,7 pure potassium oleate, and pure dodecylamine were used as collectors. All other chemicals were reagent grade in quality, i.e., n-amyl alcohol as frother; HC1, H2SO4, and KOH for pH adjustment; and ferric chloride as activator. Conductivity water, made by passing distilled water through an ion exchange column, was used in the experimental work. All minerals used in the investigation were hand-picked specimens. Sample Preparation: Each of the minerals was crushed through 8 mesh, and the product was divided into two groups, one to be ground dry and the other wet. Dry grinding was accomplished with an alumina mortar and pestle. The product was dry-screened to 48 x 150 mesh, cleaned magnetically, deslimed in conductivity water, and dried. Preparation of the samples by wet-grinding involved grinding a 200-g charge of the mineral (-8 mesh) at 60% solids with natural water in a mild steel rod mill for four minutes. This charge was then wet-screened immediately with natural water to 48 x 150 mesh, dried, and cleaned magnetically. Some experiments were also conducted with leached beryl and quartz. These products were prepared by leaching the sized sample (48 x 150 mesh) with concentrated HC1 with a percolation technique until no iron could be detected in the leach liquor. Following this step, the sample was rinsed with conductivity

Jan 1, 1967

By AIME AIME

YOU can place an exclamation point after the "and How" if you want to, but the way it stands it sum¬marizes the Mining Geology sessions quite nicely; "Why" in the morning, "How" in the afternoon. It is altogether fitting that Prof. McLaughlin and Reno Sales, who have themselves achieved enviable reputations in company work, should have led the program by presenting informally a chapter from the volume dedicated to the beloved dean of all economic geologists, Waldemar Lindgren. In opening the morning session, over which Sydney Ball presided, Donald McLaughlin emphasized the continuous role mining geology should play in operating technique. He pointed out the importance of structural relations in a broad sense, and the preponderant role they play in developing the manner of ore occurrences. He illustrated this by an account of the work at Homestake, using slides to show the stratigraphic sequence, the folding, and the orebodies of that camp. An interesting piece of detail was the distinction they found could be made be¬tween the chlorite near the ore masses, and that in the country rocks. Whether the cummingtonite, characteristic of the rock in which the ore is found, is of regional or of contact metamorphic origin caused some discussion. Dr. Lindgren inclined to the belief that it was contact, but L. C. Graton replied that they had found the weight of evidence was for a hydrothermal origin. D. F. Hewett raised the question as to whether, in the advancing development of the mining industry, there was still a place for the U. S. Survey geologist, and the consensus seemed to be that there should be. His role is changing from that of mapping mining districts in detail, now the task of the companies, towards a more general serving of the industry through the wider perspective his work gives him in contradistinction to the greater detail of knowledge accumulated by the resident geologist.

Jan 1, 1933

By Linda Lee, R. E. Reed-Hill, C. R. Smeal

Four fcc metal surfaces, etched to make them responsive to polarized light, have been studied with an electron microscope. Jones'prediction that these surfaces are grooved has been verified. Optical-goniometer measurements made on commercially pure nickel indicate that the groove walls are poorly defined (100) facets. Surface mientations close to either 4001 or {ill).- show no extinctions on the polam'zid-light microscope. An explanation is offered for this orientation dependence. It has also been deduced that polarized-light extinctions on a grooved cubic-metal surface should not be used directly in crystallographic-orientation determinations. The nature of the etching solutions that produce these surfaces is considered. A cubic-metal surface may be made responsive to polarized light in two basic ways."' In one, an anodic film, believed anisotropic, is formed on the surface. A plane-polarized-light beam, at normal incidence, should be reflected from this type of film with an ellipticity that varies with grain orientation. Under crossed polarizers of a polarized-light microscope, each grain may be distinguished from its neighbors by a difference in reflected-light intensity. An alternate treatment,' more generally applicable to cubic metals and of principal concern here, involves etching of grain surfaces. The characteristic features of this surface were first deduced by Jones3 from light-microscope observations. She concluded that, in general, grain surfaces were furrowed so that light was reflected from two parallel sets of etched facets. A grooved surface produces elliptical polarization of a plane-polarized beam because the beam does not strike groove walls at normal incidence. Jones also observed that the furrows must have faces inclined to each other by approximately 90 deg, since the light returns along the incident path, and that a grooved surface should show four maxima and minima of reflected-light intensity during a 360-deg stage rotation of the polarizing microscope. Positions of maximum extinction were predicted to occur when groove axes were parallel to either polarizer or analyzer vibration directions. Because of the limited resolving power of Jones' optical microscope, her deductions were primarily indirect. Proof of the correctness of her conclu-sions, as demonstrated by the electron microscope, will be given as well as evidence concerning the crystallographic nature of the etch furrows and the types of etching solutions that produce them. EXPERIMENTAL PROCEDURE During a comprehensive study of hot plastic deformation in nickel and nickel alloys, an etch was evolved that produced a surface with an excellent polarized-light response on Nickel 200 ("A" Nickel). The etching solution and associated metal-lographic procedures are given in Table I. In evaluating this etch, a study was made of the topological features of the etched surface and their relation to the underlying crystalline structure. As part of this investigation, large crystals (2 mm average diameter) were grown in a 1-cm-sq Nickel 200 specimen. After the surface was etched, the crystallographic orientations of ten grains were determined by the standard back-reflection Laue technique of Gren-inger.4 Maximum extinction positions during a microscope stage rotation were also measured for the ten grains. Groove-wall positions on the surfaces of the ten grains were measured with a two-circle optical goniometer. The technique was essentially that of Barrett and Levenson.5 Several grain surfaces were photographed with a Philips Model 100A electron microscope. All specimens were replicated with collodion, or collodion backed with formvar and chromium shadowed at 18 to 20 deg. The basic material was Nickel 200. However, an electron-micrographic study was also made of surfaces developed by polarized-light etches on other fcc metals (90-10 a brass, Monel 400, and lead). All etching procedures are given in Tables I and 11. EXPERIMENTAL RESULTS Fig. 1 shows typical electron micrographs of three different fcc metal specimens and an optical micrograph of a fourth. All photographs show a grooved structure corresponding closely to Jones'3 predictions. Also, as noted by Jones, extinctions were always observed when groove axes were either parallel or perpendicular to the microscopes' vertical cross hair. The symmetry of the grooves, with respect to the twin boundaries in Fig. 1, implies that furrows have a crystallographic basis. The coarse-grained Nickel 200 specimen was used to study this basis. Facet Orientation. The poles of the ten Nickel 200

Jan 1, 1964

By James H. Hance

Discussion of the paper of JAMES H. HANCE, presented at the New York meeting, .February, 1916, and printed in Bulletin No. 110, February, 1916, pp. 299 to 326. FREDERIC P. DEWEY, Washington, D. C. (communication to the Secretary*).-I wish to congratulate Professor Hance and to thank him for his extremely valuable addition to the fund of data upon this subject. It presents clearly conclusive and incontrovertible proof of the unreliability of drill samples of this class of metal for determining the value of such bullion. I am afraid, however, that his hope that some one in the mint service might continue such an investigation upon a more elaborate and exhaustive scale is, for the present at least, doomed to disappointment. As a practical matter, the mint service is not now particularly interested in segregation in crude bullion. So much trouble and friction arose, -both in the original purchase and in the transfer from one institution to another, in handling segregated bullion, that it became necessary to adopt drastic measures and now it is seldom attempted to determine the value of such bullion in the service. When bullion known or even suspected of being segregated is presented for purchase, it is at once strongly refined in the pot and the disturbing elements so far removed that concordant assays may certainly be obtained from the dip samples and a reasonably fair agreement obtained from drill samples. The mint service prefers that the owner should refine his bullion himself, but if he does not we will do it at his expense and return the slag to him when desired. Much work has been done in the mint service trying to arrive at the value of deposits of segregated bullion without strong refining. It was no unusual thing for such deposits to be melted three times at the purchasing office and to have 30 to 40 assays on the metal made before buying it. Yet when shipped to a mint it was found necessary to melt two or three times more and to make 15 to 25 assays before the mint would accept the bar, and there were considerable differences between the valuations of the two offices. In what was undoubtedly the worst case ever investigated, the purchasing office melted the deposit, 953 oz., three times, with a loss of 105.5 oz., and made 46 assays; the mint melted three times, with a loss of 6.6 oz., and made 28 assays. The mint allowed the purchasing office 1.178 oz. of fine gold more than the purchasing office claimed, while an extensive investigation of the mint samples by the Bureau, in which over 100 independent assays were made in various service laboratories, indicated that the metal carried 0.7 to 0.9 oz. more of fine gold than the mint allowed. Preliminary assays on the original metal

Jan 5, 1916

Jan 1, 1977

By J. E. Hanlon, S. R. Butler, R. J. Wasilewski

The temperature, orientation, and strain-rate dependence of tensile flow in single-crystal NiA1 of equiatomic composition have been investigated up to 800°C. Compression tests at room temperature have also been carried out. Optical and replica electron microscopy and X-ray diffraction methods were used to investigate the slip mechanisms. NiAl exhibits {110)(001) slip and cube slip {l00)(010) was also observed. This results in very high strength of single crystals in cube orientation. The implications of this slip mode, with the resultant small number of possible slip systems and three mutually perpendicular slip vectors, are discussed. ThE CsCl structure compounds represent a class related to the bcc elements, but their behavior is affected by three additional variables: composition (within the stability range of the compound), extent of long-range order perfection, and bonding energy. Very little data are available on the effects of these variables on mechanical properties. Rachinger and ~ottrell' suggested slip to occur along (111) in compounds of low ordering energy; in compounds of higher bond strength (>0.06 ev), they observed (110) (001) slip. As pointed out by copley,' only three in- dependent slip systems are available in the latter case; hence general deformation is impossible. Brown3 carried out a theoretical calculation of the yield-point variation with the degree of long-range order in the CsCl structure, based on the assumption of superdislocations. More general approaches, based on considerations of superlattice dislocations and antiphase domain boundaries in ordered structures, were carried out by Flinn~ and by Vidoz and Brown.' These, however, give no information on changes in the slip structure—if any—between the ordered and the disordered compounds. This aspect was investigated experimentally and theoretically by Stoloff and Davies' and by Marcinkowski and chessin7 in FeCo. The latter workers proposed the deformation behavior of the ordered FeCo to be essentially the same as that in many other bcc metals. Investigations of polycrystalline A~M~'-'O indicate considerable variation in mechanical properties with composition and test temperature. The existence of {123)(111) slip was reported in AgMg.'9'9'0 (The formation energy of this compound, presumed to be ordered at all temperatures below melting, is 4.38 cal per g-atom," i.e., 0.024 ev per bond.) The yield strength has been reported as relatively independent of temperature below 0.45 T, (where T, is the absolute melting temperature). Tensile deformation of single-crystal AgMg was also investigated by Kurf-man," who observed marked tendency to single glide on{112}(111) and {110)(111). From observations of slip lines in deformed poly-crystalline NiA1, Westbrook et a1.I3 suggested the

Jan 1, 1968

By Paul F. Fulton, Robert K. Estes

INTRODUCTION Relative permeabilities are factual data necessary to any prediction of reservoir production behavior. One important problem in determining relative permeabilities of porous media to gas is the effect of gas slippage on these determinations. Since certain aspects of the slippage phenomenon still remain unknown, this study is particularly concerned with that problem. The validity of the theory of gas slippage as it is applied to the flow of gas through porous media has been well established. 1,2,3 Therefore, in determining the permeabilities of porous media to gas by ordinary laboratory procedure, i.e., at atmospheric pressure, the slippage correction should be considered. Rose3 performed experiments on gas relative permeabilities which indicated that the effect of gas slippage on the measured effective gas permeabilities at various liquid saturations decreased with an increase in liquid saturation. Following Rose, it was substantiated experimentally' that the effective gas permeabilities at the various liquid saturations extrapolated to infinite mean pressure were the same as the non-wetting liquid permeabilities at the same saturations. This same paper also presented data which showed that the magnitude of the slippage between those values of gas effective permeability determined at atmospheric pressure and those found by extrapolation to infinite mean pressure decreased with an increase in liquid saturation. However, these experiments were not performed at liquid saturations above 30 per cent. Therefore, the purpose of this experimental work was to determine the effect of gas slippage on permeability measurements at liquid saturations in excesh of 30 per cent. APPARATUS Five core samples were used In this work: two synthetic Alundum samples (A-1, and A-2). a Nichols Buff sandstone sample (NB-13), and two samples from producing formations, a Soso sandstone (S-1), and a vugu-lar dolomitic limestone (R-7). The core samples ranged in permeability from 32 to 663 md. These cores were chosen because they represented a fairly wide range of permeabilities and probably a considerable difference in pore size and pore size distribution. Fig. 1 is a schematic diagram of the apparatus which consists of an air dehydration filter A, two Moore null-matic sub-pressure regulators B and C, the differential oil manometer D, the core holder E, the flowmeter F, the soap reservoir G, and a mercury manometer H measuring the downstream pressure. The interesting features of the apparatus are the two Moore vacuum-pressure regulators. The regulators permit the rapid establishment and easy control during flow at sub-atmospheric pressures of both the differential and downstream pressures, and prevent the surging action of the vacuum pump from disturbing the system during flow. Provided there are no leaks in the system, these regulators will maintain without measurable change selected downstream and differential pressure. Specifically, regulator B controls the downstream pressure and regulator C controls the differential pressure. In opera-

Jan 1, 1957

By L. H. Levenson, Charles S. Barrett

Numerous determinations1-' of the texture of cold-rolled polycrystalline iron, steel, and ferritic alloys have been made with good agreement among the various observers as to the principal features of the texture common to all, but there has been no adequate explanation of the texture in terms of, the behavior of individual grains. This study presents an explanation of the texture based on the observed rotation of single crystals when deformed in a manner similar to a grain in the aggregate, a method we have found useful in leading to a better understanding of compression and tension textures;8,9,10 in particular, the aim has been to determine experimentally the end orientations of rolled single crystals of iron. These are discussed in connection with the point of view of Weverl and of Boas and Schmid2 that the rolling texture is a simple compression texture (compression normal to the rolling plane) superimposed on a simple tension texture (tension in the rolling direction), and the point of view of Kurdjumow and Sachs3 that three ideal end orientations exist. Experimental Method The single crystals used were in the form of disks cut from a stock of crystalst pre- pared in this laboratory by a strain-anneal method from mild steel decarburized and purified in hydrogen, the details of which have been described elsewhere.11 To ensure maximum elongation in the rolling direction and to simulate approximately the rolling of a grain in an aggregate, lateral flow was constrained by placing each crystal in a close-fitting hole in a plate of copper or iron of equal thickness and rolling the plate and crystal together. About one-third of the crystals were rolled in a "sandwich" pack by adding top and bottom cover plates. The two-high mill used had 8-in. diameter rolls and was operated at 15 r.p.m. The initial diameter of the crystals was between 1/4 and 1/2 in., while the starting thickness varied from 0.031 to 0.376 in. With a single exception, which was rolled 63 per cent, the crystals were rolled to a final reduction in thickness of 82 to 97 per cent in 20 to 40 passes, alternately changing the sense of the rolling direction. The initial orientations of the crystals were determined either by X-ray back reflection12 or by optical reflectionl3 from etch pits; the mean final orientations were determined by X-ray Laue photograms using molybdenum, silver, or tungsten radiations, by optical reflection, and in many cases by both methods. Results Twenty-six crystals were studied. It was found that there were three typical be-

Jan 1, 1941

By Charles S. Barrett, L. H. Levenson

Numerous determinations1-' of the texture of cold-rolled polycrystalline iron, steel, and ferritic alloys have been made with good agreement among the various observers as to the principal features of the texture common to all, but there has been no adequate explanation of the texture in terms of, the behavior of individual grains. This study presents an explanation of the texture based on the observed rotation of single crystals when deformed in a manner similar to a grain in the aggregate, a method we have found useful in leading to a better understanding of compression and tension textures;8,9,10 in particular, the aim has been to determine experimentally the end orientations of rolled single crystals of iron. These are discussed in connection with the point of view of Weverl and of Boas and Schmid2 that the rolling texture is a simple compression texture (compression normal to the rolling plane) superimposed on a simple tension texture (tension in the rolling direction), and the point of view of Kurdjumow and Sachs3 that three ideal end orientations exist. Experimental Method The single crystals used were in the form of disks cut from a stock of crystalst pre- pared in this laboratory by a strain-anneal method from mild steel decarburized and purified in hydrogen, the details of which have been described elsewhere.11 To ensure maximum elongation in the rolling direction and to simulate approximately the rolling of a grain in an aggregate, lateral flow was constrained by placing each crystal in a close-fitting hole in a plate of copper or iron of equal thickness and rolling the plate and crystal together. About one-third of the crystals were rolled in a "sandwich" pack by adding top and bottom cover plates. The two-high mill used had 8-in. diameter rolls and was operated at 15 r.p.m. The initial diameter of the crystals was between 1/4 and 1/2 in., while the starting thickness varied from 0.031 to 0.376 in. With a single exception, which was rolled 63 per cent, the crystals were rolled to a final reduction in thickness of 82 to 97 per cent in 20 to 40 passes, alternately changing the sense of the rolling direction. The initial orientations of the crystals were determined either by X-ray back reflection12 or by optical reflectionl3 from etch pits; the mean final orientations were determined by X-ray Laue photograms using molybdenum, silver, or tungsten radiations, by optical reflection, and in many cases by both methods. Results Twenty-six crystals were studied. It was found that there were three typical be-

Jan 1, 1941

By J. J. Arps, T. G. Roberts

Since the introduction of the relative permeability concept in the middle thirties1,2 various investigators have shown3,10,11,12,15 how the basic equations for the flow of oil and gas through porous media can he utilized to compute the recovery from depletion type or solution gas drive type reservoirs under certain conditions, when the necessary physical data pertaining to the reservoir rock and its reservoir fluids are known. In the study by Muskat and Taylor" in 1945, the effects of viscosity, gas solubility, shrinkage, and the permeability-saturation characteristics of the producing formation on the production histories and the recovery of gas drive reservoirs were analyzed. Each parameter was varied a limited number of times, while keeping the others constant. The work was not carried to the point where the data could be used directly to estimate the primary recovery in those cases where certain rock and fluid characteristics were known or could be assumed. Since the publication of this classic study, the work by Beal in 194616 and Standing in 1952'" has established general correlations of oil viscosity and shrinkage with gas solubility and oil gravity. In addition. a considerable number of relative permeability relationships for different types of reservoir rocks has been published2,5,13,17,19,20. Also, the burden of the numerical work required in the solutions of the differential equation has. during the last few years, been greatly reduced with the availability of modern electronic computing facilities. The purpose of this paper is therefore to present the results of a large number of such recovery computations covering the normal range of variation of the main parameters such as the type of rock, the API gravity of the oil, and the amount of gas in solution. As is to be expected, the ultimate recovery is found to increase with the oil gravity. except for the higher solution gas-oil ratios. Within the normal range of solubilities, the ultimate recovery generally appears to decrease with the amount of gas in solution for the higher oil gravities, and to show a slight increase for the lower oil gravities. Intermediate oil gravities seem to fall between the two trends. The type of reservoir rock, as identified by its relative permeability relationship, appears to have a very pronounced effect on the ultimate recovery. In general, sands and sandstones show higher recoveries than limestones and dolomites, although certain intergranular limestones seem to show a higher theoretical recovery than unconsolidated sand. The recovery from sands and sandstones generally decreases with increasing cementation and consolidation, while the recoveries from limestones and dolomites are highest for the intergranular type and lowest for the fracture type porosity.

Jan 1, 1956