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Apparatus and a method for determining the volumetric behavior of hydrocarbons at pressures up to 10,000 psia and at temperatures between 0° and 460°F are described. The equipment is suitable for measuring the total volume of the system and the volume of a liquid phase as functions of state within these ranges of temperature and pressure. Introduction During the past two decades there has been a marked increase in the ranges of temperature and pressure encountered in underground hydrocarbon reservoirs of commercial interest. In addition, greater interest in the intensive characteristics of the fluids found in these reservoirs has developed. Apparatus Several types of apparatus have been developed in the authors' laboratory for volumetric measurements of hydrocarbon systems. The earliest equipment described1 was characterized by constant volume, and the weight of material present was varied systematically in order to attain the different pressures desired in the study. Later another apparatus2 was built in which the effective volume of the cylindrical cell, which confined a hydrocarbon sample of constant weight was varied by injection or withdrawal of mercury. The effective total volume of the equilibrium cell was measured by ascertaining the position of the mercury surface but no measurement could be made which gave knowledge of the volumes of individual phases existing within the hydrocarbon system. A third apparatus3 was designed for use at higher pressures and temperatures than the earlier equipment would tolerate. This apparatus was of the variable volume type but was built in the general form of a U-tube, the mercury level being measured at the surface which was not exposed to the hydrocarbon system. This arrangement avoided the need of subjecting measuring equipment to the extremes of temperature at which studies were made, but it gave no provision for measurement of the volumes of individual phases. Although this last apparatus was satisfactory as to accuracy and convenience for many purposes, need was felt for measurements of the volume of the liquid phase of the hydrocarbon system. For this reason a fourth equilibrium apparatus was designed and constructed, and it is the purpose of the present paper to describe it. The equilibrium cell has a working range of temperature from 0° to 460°F at pressures up to 10,000 psi. Provision for measurement of both total volume and liquid-phase volume makes it particularly suitable for the equilibrium study of heterogeneous systems consisting either of simple mixtures or of complex field samples of hydrocarbons. The general arrangement of the ap-

Jan 1, 1948

Apparatus and a method for determining the volumetric behavior of hydrocarbons at pressures up to 10,000 psia and at temperatures between 0° and 460°F are described. The equipment is suitable for measuring the total volume of the system and the volume of a liquid phase as functions of state within these ranges of temperature and pressure. Introduction During the past two decades there has been a marked increase in the ranges of temperature and pressure encountered in underground hydrocarbon reservoirs of commercial interest. In addition, greater interest in the intensive characteristics of the fluids found in these reservoirs has developed. Apparatus Several types of apparatus have been developed in the authors' laboratory for volumetric measurements of hydrocarbon systems. The earliest equipment described1 was characterized by constant volume, and the weight of material present was varied systematically in order to attain the different pressures desired in the study. Later another apparatus2 was built in which the effective volume of the cylindrical cell, which confined a hydrocarbon sample of constant weight was varied by injection or withdrawal of mercury. The effective total volume of the equilibrium cell was measured by ascertaining the position of the mercury surface but no measurement could be made which gave knowledge of the volumes of individual phases existing within the hydrocarbon system. A third apparatus3 was designed for use at higher pressures and temperatures than the earlier equipment would tolerate. This apparatus was of the variable volume type but was built in the general form of a U-tube, the mercury level being measured at the surface which was not exposed to the hydrocarbon system. This arrangement avoided the need of subjecting measuring equipment to the extremes of temperature at which studies were made, but it gave no provision for measurement of the volumes of individual phases. Although this last apparatus was satisfactory as to accuracy and convenience for many purposes, need was felt for measurements of the volume of the liquid phase of the hydrocarbon system. For this reason a fourth equilibrium apparatus was designed and constructed, and it is the purpose of the present paper to describe it. The equilibrium cell has a working range of temperature from 0° to 460°F at pressures up to 10,000 psi. Provision for measurement of both total volume and liquid-phase volume makes it particularly suitable for the equilibrium study of heterogeneous systems consisting either of simple mixtures or of complex field samples of hydrocarbons. The general arrangement of the ap-

Jan 1, 1948

By Robert W. Fullerton, Donald T. King

INTRODUCTION AND THEORY by Robert W. Fullerton In coal preparation plants, as in any industrial operation where raw materials are handled, nuisance problems arising from the generation of dust are inevitable. Devices for the control or collection of dust are there- fore essential components of the plant process equipment. The general term "aerosol" is applied to small particles suspended in a gaseous medium, usually air, whose velocity under the force of gravity is small enough that the particles remain suspended for a reasonable length of time. Aerosols can be classified as dust, smokes, fumes, mists or fogs. Dust includes particles originally formed by pulverization of materials by such processes as crushing, grinding, drilling, blasting and abrasion. Smoke includes particles formed from the burning of organic materials. Fumes are particles formed by processes such as condensation and sublimation, usually at high temperatures. Mists or fogs are particles formed by the condensation of water or other vapors on some nuclei. The size of aerosol particles is generally designated in units of microns, there being 1000 microns to a millimeter and 25,400 microns to an inch. Particles of about 10 microns or above are visible to the naked eye. Table 14-1 shows size characteristics of the general classifications of particles discussed above and includes typical examples of particles commonly en- countered. Table 14-1 also shows the relationship between micron size and standard screen mesh sizes. Smoke and fume are usually in the range of 0.01 to one micron, dusts are in the range of one to 400 microns, mists are in the range of 0.1 to 100 microns, and fogs are in the range of one to 100 microns. For purposes of dust control, particles greater than 10 or 20 microns in size are considered large, particles one to 10 microns are considered fine and particles below one micron are ultrafine. Sources of Dust Because coal is relatively friable, the mining and subsequent handling operations break part of the coal into dust that can be readily carried by currents of air. In a coal preparation plant mechanical handling operations such as unloading, transferring from one belt to another, screening, cleaning, and crushing in a dry state result in the generation and release of varying amounts of additional dust. The dust problem, of course, is much less serious in plants employing entirely wet processing. In addition to dust from handling operations, thermal drying of the fine coal product frequently presents another dust collection problem. Most coal driers are

Jan 1, 1968

By F. W. Steadman, Charles S. Barrett

Deformation bands of surprising regularity are found in large-grained poly-crystalline copper after cold-rolling (Fig. I). Individual bands frequently are large enough to permit a determination of their orientation by means of etch pits and an optical goniometer. Measurements have been made on 21 areas in seven different grains, and these, combined with X-ray studies of nine single crystals that had been cold-rolled after mounting in a polycrystal-line block, have contributed to a better understanding of the preferred orientations in rolled copper just as similar studies have for rolled iron1 and brass.2,3 Particular attention was given to determining orientations that are stable during rolling and to the manner of fragmentation and rotation of unstable grains. The possible role of twinning was also carefully investigated. The texture of polycrystalline copper after cold-rolling is well established by the pole figures that have been plotted by Schmid and Staffelbach,4 Iweronowa and Schdanow,6 and Brick and Williamson,8 all of which are in substantial agreement. There has been some divergence in the list of individual "ideal" orientations that have been used to describe the texture by these observers and others," although the orientation (110) [II2]—that is, (110) parallel to the rolling plane and [TIP] parallel to the rolling direction—is generally recognized as the most prominent orientation and (112) [III] one of the lesser orientations. Other orientations have been given by some observers as (236) [535], (100) [00I], and (110) [00I]. The texture of copper has also been described as (I35) [533].6,7 The sum of these orientations provides a reasonable approximation to the complete pole figure, but it does not follow that these specific orientations are necessarily of fundamental significance, for the choice of indices is arbitrary, within limits. Furthermore, a detailed investigation of the ideal orientations in cold-rolled iron discloses continuous ranges of equally favored positions rather than definite positions of high stability,' and similarly Brick's observations in a single crystal of a brass2 suggest that all orientations in the range between (110) [II3] and (110) [II7] are about equally stable. Materials and Methods The material used was vacuum-cast electrolytic copper kindly supplied by L. L. Wyman, of the General Electric Co.* Slicec 1/2 in. thick and 21/2 in. square, cut from the ingot, were rolled with 50 per cent reduction per pass to final thicknesses between 0.02 and 0.04 in., and etched to develop cube-face etch pits suitable for goniometric work.8 The etch was light on some strips and deep in others.

Jan 1, 1942

By Charles S. Barrett, F. W. Steadman

Deformation bands of surprising regularity are found in large-grained poly-crystalline copper after cold-rolling (Fig. I). Individual bands frequently are large enough to permit a determination of their orientation by means of etch pits and an optical goniometer. Measurements have been made on 21 areas in seven different grains, and these, combined with X-ray studies of nine single crystals that had been cold-rolled after mounting in a polycrystal-line block, have contributed to a better understanding of the preferred orientations in rolled copper just as similar studies have for rolled iron1 and brass.2,3 Particular attention was given to determining orientations that are stable during rolling and to the manner of fragmentation and rotation of unstable grains. The possible role of twinning was also carefully investigated. The texture of polycrystalline copper after cold-rolling is well established by the pole figures that have been plotted by Schmid and Staffelbach,4 Iweronowa and Schdanow,6 and Brick and Williamson,8 all of which are in substantial agreement. There has been some divergence in the list of individual "ideal" orientations that have been used to describe the texture by these observers and others," although the orientation (110) [II2]—that is, (110) parallel to the rolling plane and [TIP] parallel to the rolling direction—is generally recognized as the most prominent orientation and (112) [III] one of the lesser orientations. Other orientations have been given by some observers as (236) [535], (100) [00I], and (110) [00I]. The texture of copper has also been described as (I35) [533].6,7 The sum of these orientations provides a reasonable approximation to the complete pole figure, but it does not follow that these specific orientations are necessarily of fundamental significance, for the choice of indices is arbitrary, within limits. Furthermore, a detailed investigation of the ideal orientations in cold-rolled iron discloses continuous ranges of equally favored positions rather than definite positions of high stability,' and similarly Brick's observations in a single crystal of a brass2 suggest that all orientations in the range between (110) [II3] and (110) [II7] are about equally stable. Materials and Methods The material used was vacuum-cast electrolytic copper kindly supplied by L. L. Wyman, of the General Electric Co.* Slicec 1/2 in. thick and 21/2 in. square, cut from the ingot, were rolled with 50 per cent reduction per pass to final thicknesses between 0.02 and 0.04 in., and etched to develop cube-face etch pits suitable for goniometric work.8 The etch was light on some strips and deep in others.

Jan 1, 1942

By J. M. Hodge, M. A. Orehoski

THE relationship between hardenability based on a 50 per cent martensite criterion, and that based on higher percentages of martensite in a number of low-alloy steels was discussed in a previous paper by the authors.1 It was found that the differences between the hardenability values based on the 50 per cent martensite and full martensite criterions increased as the hardenability increased and that, in the steels of higher hardenability, these differences were fairly large. Furthermore, it was found that these relationships could be expressed with reasonable accuracy as a function of the hardenability. The importance of the full martensite criterion of hardenability in relation to the attainment of the optimum mechanical properties of tempered martensite was emphasized in the earlier paper. The purpose of the present work is to study the effects of some of the individual alloying elements on hardenability, using three different percentages of martensite as criteria, and thereby to evaluate the role of these individual elements in the general hardenability relationships previously reported. EXPERIMENTAL PROCEDURE Induction-furnace heats weighing 17-lb., of the compositions given in Table I, were cast and forged into 1 ¼ in. round bars. All heats were killed with aluminum additions corresponding to 1 lb. per ton. The compositions were chosen to represent several series of steels, in which only one alloying element would vary and in which the nonmartensitic constituents on quenching would be predominantly bainitic. All bars were normalized from 1650°F. and tempered one hour at I 150°F. prior to the hardenability determinations. Hardenability values are based on metallographic examination of standard Jominy bars, quenched from 1600°F. (I hr. and 20 min. heating time). The general procedure was the same as outlined in detail in the previous paper; (I) that is, the distance from the quenched end of the bar to the point of 0.1 per cent transformation was first measured on the microscope and then the percentage of martensite was estimated at every 0.05 in. from the quenched end, and these percentage values plotted against the distance along the bar. In this case, samples 2 in. long were cut from the quenched end of the Jominy bars and 10 fields were examined and averaged at each distance. The conversion of Jominy distance to ideal diameter is based on a revised correlation curve (Fig. I). This curve is based on work carried out at the Research Department of the South Chicago Works, Carnegie-Illinois Steel Corporation, and represents a direct correlation between hardenability values as deter-

Jan 1, 1946

By Waldemar Dyrssen

I CANNOT agree with the results obtained by the committee. The gas obtained per pound of coal is too high in calorific value and the amount of gas is too large. It should require about 190 cu. ft. of oxygen per 1000 cu. ft. of gas and not 75.14 cu. ft. as is given on page 35 of the report, or about 2.5 as much. Calculating the calorific value per pound of coal from the coal analysis given on page 34, according to Dulong's formula, the gross and net calorific heat are about 12,890 and 12,430 B.t.u., respectively, which is about 18,600 and 17,900 B.t.u., respectively, per pound of carbon in the coal. This is an unusually high figure, as ordinary bituminous coal has less than 18,000 gross B.t.u. per pound of carbon. Assuming, however, that the calorific values calculated are correct, the following results are obtained. On page 35, the net calorific heat in the gas per pound of coal is given as 12,856 B.t.u. and calculation for the gross value shows it to be about 13,950; in other words, the gas contains (13,950 - 12,890) ÷ 12,890 = 8.2 per cent. more heat than the coal on a gross basis and (12,856 - 12,430) ÷ 12,430 = 3.4 per cent. more on a net basis. The calculated amount of carbon in this gas per pound of coal gasified is about 0.688 lb., or nearly the same as in the coal (0.6972) and the gross and net calorific heat per pound of carbon in the gas are 20,300 and 18,710 B.t.u. which are 9.1 and 4.5 per cent. more than for the carbon in the coal. These calculations show that the results given in the report cannot be correct. There must always be some heat losses in the gasification of coal, in radiation from the producer, and in sensible heat in the gas; there must be some loss of carbon in ashes and in soot, and there are always tarry vapors in the gases that are condensed and do not appear in the fixed gases. From the excessive heat in gas per pound of carbon contained therein, it can also be concluded that the percentage of hydrogen in the gas is too high, from which it follows that the moisture decomposed is too high and that more free oxygen must be used.

Jan 11, 1924

By E. I. Larsen, E. F. Swazy, F. R. Hensel

EXPERIENCE has indicated that hard bronzes are not suitable for bearing applications where high bearing loads and speeds are involved. It is the general practice to utilize softer materials for these purposes, such as copper, lead, silver, babbitt, lead-base alloys, and more recently aluminum-base alloys, preferably supported by a steel backing. It was the objective of the present investigation to study a new material produced by powder metallurgical methods susceptible to precipitation-hardening. TEST MATERIALS Preliminary tests were made with compacts containing copper, nickel and silicon in quantities sufficient to form 3 to 5 per cent nickel silicide. It was found that this type of alloy was susceptible to the formation of a soft surface shell when sintered in tank hydrogen. The depth of the shell depended on the length of sintering time and sintering temperature, and varied in thickness from a few thousandths to as much as one eighth inch. This soft shell resulted from the preferential oxidation of silicon, thereby reducing the efficiency of age-hardening by the nickel silicide compound. The body of the sintered compacts below the soft shell could be precipitation-hardened to a hardness of 70 to 85 Rockwell B, by quenching from. 900°C. and age-hardening at 450°C. A series of tests was made with various addition agents, in order to decrease the rate of preferential oxidation, and it was found that phosphorus was most beneficial in this respect. After considerable experimentation, the following nominal composition was accepted as standard: 2.4 per cent nickel; 0.8 silicon; 0.3 phosphorus; balance copper. The physical properties and certain bearing properties of this alloy are described in the present paper. PREPARATION OF COMPACTS Several methods of incorporating the hardening ingredient (nickel silicide) were studied. Compacts formed from copper, nickel and silicon powders were found to be inferior to those fabricated from prealloyed nickel silicide master alloys, because of the rapid oxidation of pure silicon during sintering. The use of a prealloyed nickel silicide hardener containing 25 per cent silicon and 75 per cent nickel could be further improved by preparing a master alloy, incorporating nickel, silicon, phosphorus and copper, having the following nominal composition: 25 per cent nickel; 7 silicon; 3 phosphorus; 64 copper. This alloy is brittle in. the cast condition and can be readily powdered. SINTERING PROCEDURE The blended powders were pressed at 25 to 40 tons per sq. in., the pressure depending on the size and shape of the compacts. Sintering was carried out in hydrogen or cracked ammonia atmospheres at

Jan 1, 1946

By Frank R. Milliken, Robert Goodwin

In September 1937, the Ohio Copper Co. inaugurated the treatment of its copper-bearing mill tailings at Lark, Utah. These tailings had been accumulated during the regular operation of the Ohio Copper mine and mill over the period 1907 to 1919. Gravity concentration had been employed except for a comparatively short period in 1919, when flotation was used. The ore milled during that period assayed about I per cent Cu. The chief copper mineral, chalcocite, was disseminated in a shattered quartzite, mainly along fracture or cleavage planes. The quartzite gangue was extremely hard and grinding to liberation resulted in excessive sliming of the "sooty" chalcocite, with consequent high tailings losses. Recovery on the seven million tons treated was probably less than 60 per cent of the total copper content. As early as 1918, attempts had been made to sample the dump. In 1928, a complete sampling program was undertaken. The sampling consisted of seventy-four 5-in. post auger holes drilled to the full depth of the dump at regular intervals of 250 ft. Each 10-ft. portion thereof comprised a sample for analysis. Each sample was screened, rolled, divided into three parts, dried and assayed. The reject was retained for testing purposes. From the depth of the auger holes a contour map of the dump was plotted, Fig. I, which gives percentages of tonnage and copper content. The tonnage within the limit of the drill holes was estimated at about five million tons with an average content of 0.42 per cent Cu, 31 per cent of which (0.13 per cent) was acid-soluble. A screen analysis of the composite dump sample is shown in Table I. Flotation tests by several companies and individuals were then made, the results of which ranged from 62 to 74 per cent recovery. On the basis of these, a 200-ton pilot plant employing straight flotation was built and operated for a few months. Operation of this plant was unsuccessful, as no provision had been made to handle the copper-bearing solutions resulting from the water-soluble copper, a point that was overlooked in the laboratory test work. Attempts to decant the copper-bearing solution for precipitation in the usual manner ahead of flotation were not satisfactory because of low water recovery (owing to poor settling characteristics of the pulp) and contamination of the copper precipitate with unsettled slime. Low copper prices in 1931 necessitated the termination of testing. With the stimulus of higher copper prices in 1937, a review was made of metallurgical

Jan 1, 1943

By Robert Goodwin, Frank R. Milliken

In September 1937, the Ohio Copper Co. inaugurated the treatment of its copper-bearing mill tailings at Lark, Utah. These tailings had been accumulated during the regular operation of the Ohio Copper mine and mill over the period 1907 to 1919. Gravity concentration had been employed except for a comparatively short period in 1919, when flotation was used. The ore milled during that period assayed about I per cent Cu. The chief copper mineral, chalcocite, was disseminated in a shattered quartzite, mainly along fracture or cleavage planes. The quartzite gangue was extremely hard and grinding to liberation resulted in excessive sliming of the "sooty" chalcocite, with consequent high tailings losses. Recovery on the seven million tons treated was probably less than 60 per cent of the total copper content. As early as 1918, attempts had been made to sample the dump. In 1928, a complete sampling program was undertaken. The sampling consisted of seventy-four 5-in. post auger holes drilled to the full depth of the dump at regular intervals of 250 ft. Each 10-ft. portion thereof comprised a sample for analysis. Each sample was screened, rolled, divided into three parts, dried and assayed. The reject was retained for testing purposes. From the depth of the auger holes a contour map of the dump was plotted, Fig. I, which gives percentages of tonnage and copper content. The tonnage within the limit of the drill holes was estimated at about five million tons with an average content of 0.42 per cent Cu, 31 per cent of which (0.13 per cent) was acid-soluble. A screen analysis of the composite dump sample is shown in Table I. Flotation tests by several companies and individuals were then made, the results of which ranged from 62 to 74 per cent recovery. On the basis of these, a 200-ton pilot plant employing straight flotation was built and operated for a few months. Operation of this plant was unsuccessful, as no provision had been made to handle the copper-bearing solutions resulting from the water-soluble copper, a point that was overlooked in the laboratory test work. Attempts to decant the copper-bearing solution for precipitation in the usual manner ahead of flotation were not satisfactory because of low water recovery (owing to poor settling characteristics of the pulp) and contamination of the copper precipitate with unsettled slime. Low copper prices in 1931 necessitated the termination of testing. With the stimulus of higher copper prices in 1937, a review was made of metallurgical

Jan 1, 1943

By Gerald Edmunds

In a paper1 before this Institute in 1940, the writer reported that the surface orientation texture of zinc and cadmium differed from the texture existing within the casting, in that basal planes were parallel to the surface. He was unable to rationalize the , origin of this surface texture. It is conceivable that the surface orientation texture is influenced by the atomic force fields, which are different at the surface and within the body of metal. It was considered that a radical changc in the surface against which the metal is cast might alter the surface texture. In trial of this, zinc has been cast against a surface of molten lead, but the same result has been obtained—i.e., (001) parallel, ± 2oo, to the surface—as was obtained when it was cast against air, Transite or iron.' Into the bottom of an open cast-iron tray, 7 by 14 in. by 2 in. deep, preheated to about 275°C., about 1/4 in. of lead, then 1/2 in. of zinc was poured, and the whole was covered with an electric heater to enforce freezing from the bottom upward. After a lapse of time sufficient for the zinc but not the lead to solidify, the zinc slab was raised free of the molten lead. The bottom surface of the zinc casting was coated with a thin layer of lead. A specimen of the slab 136 in. square was metallographically polished to flatten it and remove the slight film of lead, and the orientation was determined by the method used before,' with the result stated above. Some determinations have also been made on other metals, as follows: Surface orientation determinations were made on the 3/8-in. diameter grip section of two 1/4-in. diameter aluminum-alloy die-cast tensile bars and on a 1/8 by 1/2-in. flat aluminum-alloy die-cast tensile bar. None of these three aluminum die castings exhibited any preferred orientation at the surface. A brass die casting (nominal composition: 60 Cu, 37.75 Zn, 1.00 Sn, 1.00 Pb, 0.10 Al, 0.15 Si) furnished by C. S. Smith was also examined. The surface showed a random orientation of alpha and beta. Summary A zinc casting solidified against a molten lead surface was found to have the same surface orientation texture, (001) parallel to the surface, as other zinc and cadmium castings. Aluminum and alpha-beta brass die castings were found to have random grain orientation textures at the surface. Acknowledgment The X-ray determinations were conducted by M. L. Fuller.

Jan 1, 1945

By R. M. Waterstrat

The phase VPt has been reported to have a crystal structure of the B19 (AuCd) type at low temperatures.''' A recent investigation3 has indicated that this phase forms by an ordering reaction from the disordered fcc Pt(V) solid solution which is stable at high temperatures. olander4 has shown that there exists a close structural relationship between the orthorhombic B19 structure and a fcc structure possessing the L1 , (CuAu) type of atomic ordering. One may derive the B19 structure by a shear-like displacement of the atoms in the (002) plane of the ordered fcc lattice along the (010) direction through a distance equal to one eighth of the unit cell dimension, see Fig. 1, followed by an orthorhombic distor; tion of the cube axes such that a = 2.693A. h = 4.413A. and c =4.767A (estimated uncertainty 0.005A). Filings of this phase were produced by grinding a VPt alloy having the B19 structure with a diamond dental grinding disc. When these filings were subjected to X-ray diffraction examination, a pattern of a severely cold-worked fcc structure was obtained. higher solution temperature used (1200 C) or to a much lower oxygen pressure than he reported, due to transfer through many bends and tubes in his complicated apparatus. An interesting observation was made when an oxygen addition was attempted in a cylindrical sample of columbium in the cold worked condition rather than in the annealed condition. The interior of the sample re-crystallized during the oxygen addition at 900°C. The periphery, however. (1 mm) did not recrystallize. A similar sample without oxygen recrystallized throughout the entire cross section. It appears that the re-crystallization is hindered by interstitial oxygen. Presumably, the interior recrystallized before appreciable oxygen could diffuse into the core. This work was supported by the United States Atomic Energy Commission. When the filings were annealed in a high vacuum furnace for 15 min at 110O0C, however. they returned to the B19 structure perhaps as a result of reordering. Subsequent less-severe cold-working of these filings by grinding in a hardened steel mortar and pestle at room temperature produced a transformation into a cold-worked L1, structure which was slightly tetragonal. Thus it appears that the degree of deformation may influence the final structure. Considerable line-broadening was observed in X-ray diffraction patterns obtained from the cold-worked filings and therefore no attempt was made to obtain accurate lattice parameters. Vacuum annealing treatments at 1100'C intended

Jan 1, 1970

By C. S. Barrett, P. Coheur

ANNEALING twins are common in the microstructure of copper that has been rolled and recrystallized. In such samples it follows that a twin relationship should exist between components of the recrystallization texture,1 and several examples of this have been reported. For example, twin relationships have been found in recrystallized electrolytic copper sheet, as indicated in Fig. I, from a paper by Coheur and Lejeune.2 In this pole figure the cube texture (100) [001] is indicated by the hollow squares in the lower half of the figure (the pole figure for 200 reflections) and in the upper, (111), part of the figure. The texture contains, in addition to this orientation, the first-order twins of it, shown in the figure by the filled triangles. This orientation relation has been suggested by others also, under certain annealing conditions,3,4 although pole figures have not been published to confirm it. Some orientations in recrystallized sheets are identical with their twins, because of the symmetry elements of the texture this is true, for example, with the (113) [211] texture so commonly reported for brass-hence it appears impossible in such samples to decide whether the twin relationships result from twinning or merely from the symmetry of the deformation process. The present investigation of a commercial copper strip seems to yield an example in which annealing twins account unambiguously for the principal orientations present. It proves to be a case, also, for which the recrystallization texture cannot be viewed as derived from the deformation texture by a first or second-order twinning mechanism . MATERIALS AND METHODS The samples investigated were of secondary copper (melted in Belgium) to which 0.19 per cent iron had been added to raise the recrystallization temperature. How much the orientation characteristics of this metal can be ascribed to the iron content and how much to other impurities or to melting and pouring practice has not been investigated.* The rolling was done in one direction only, on a mill with rolls of about 20-cm diameter. A strip 10 cm wide was reduced from 5 mm thickness to 0.05 mm by several cold passes at commercial speeds. The samples cut from this 99 per cent reduced strip were X-rayed throughout their entire thickness. A pole figure made soon after rolling and annealing was identical, within experimental error, with one that was made when a two-year interval occurred between rolling and annealing. X-ray patterns were made on a cameral that traversed

Jan 1, 1946

The Alligator Ridge Project is owned jointly by Amselco Minerals Inc. and Occidental Minerals, with Amselco being the operator. It is the latest of Nevada' s gold heap leaching operations , having gone into operation in October of 1980 after a design and construction period of only seven and one-half months. Alligator Ridge is located about 77 km (48 miles) northwest of Ely, Nevada. Three separate but adjacent ore bodies will be mined: Vantage I, II and III. The first lies virtually at the surface and is totally oxidized; the second is somewhat deeper and contains some carbonaceous material; and the third is at the lowest horizon and contains substantial carbonaceous ore. The ore is a Carlin- type siltstone which has been silicified, especially at depth, and contains finely disseminated free gold. Exploration drilling on Alligator Ridge resulted in the defining of an ore reserve of about 4.54 million mt (5 million st) averaging 4. 12 g Au per mt (0. 12 oz Au per st). A pilot heap leaching program was run during 1979. Because of the high content of fine material in portions of the ore body, one test heap of 5,000 tons was leached, after being crushed to 19 mm (314 in.), in the conventional manner using cyanide and caustic while a second heap of 2,500 tons of ore was agglomerated with cement before leaching. Results of this work were reported at the 1980 American Mining Congress meeting by Paul Chamberlin (see Bibliography). The test work clearly indicated the superior leaching qualities of the agglomerated ore, and the plant was designed on this basis. Run-of-mine ore is crushed in an open-air crushing plant using a jaw crusher followed by two cone crushers, one standard and one shorthead. Provision was made to bypass the shorthead when the ore is wet from rain or snow. Crushed ore at 19 mm (314 in.) size is mixed with cyanide solution and cement, with the ratio of the latter to the ore being 2 to 5 kg per mt (4 to 10 lb per st). The resulting moisture content is about 870, and the fines are effectively bound to the coarse particles so that migration of the fines in the heap does not take place during leaching. For agglomeration, Amselco uses a rotating drum 2. 75 m 0 by 6 m long (9 ft 6 by 20 ft). For the same agglomeration, Candelaria uses three "grasshopper" conveyors, with introduction of caustic- cyanide solution at the conveyor transfer points. Provision was made for future addition of cement slurry at these same points.

Jan 1, 1981

By Arthur F. Taggart, T. C. Fitt, A. W. Thomas

IT was noticed early by operators that high recoveries and flocculation of the sulphide minerals were closely correlated in agitation-froth flotation. Later, this readily visible flocculation was found almost invariably to be due to the binding together of the oiled sulphides by minute air bubbles, and is now known to be characteristic of pulps in which at least one of the mineral species is coated with an insoluble collecting oil. In 1930 it was reported1 that in differential flotation a correlation exists between Brownian movement of particles in the pulp and their nonfloatability, and that Brownian movement and dispersion are likewise correlated, whence it would appear to follow that dispersion of a mineral particle in a flotation pulp denotes a particle condition unfavorable to flotation. In 1934 it was postulated2 that Brownian movement, dispersion and nonfloatability all flow from the condition of the surface of the dispersed particles. It was also postulated at that time that the surfaces of dispersed particles are ionized, the ionized compound being a product of reaction between a component of the particle and a. component of the pulp, of a mass solubility of the general order of a fraction of a milligram to 15 to 20 mg. per liter. It was then further asserted, and has since been confirmed by Bankoff,3 that sulphides so conditioned with soluble collectors as to be floatable flocculate without the intervention of air bubbles as binding media. The present paper comprises an inquiry into the nature of the bound and counter ions in zinc sulphide dispersed by sodium arsenate. A part of its findings was mentioned in the 1934 paper above cited.2 The tests show that: I. When powdered granular zinc sulphide is immersed in aqueous solutions of sodium arsenate, arsenate ion is abstracted from solution and anchored to the solid surface, while sulphate and lower sulphoxy ions are concurrently displaced therefrom in substantially stoichiometric quantities. 2. The ion counterbalancing the anchored arsenate ion is zinc. 3. Dispersion and Brownian movement of zinc sulphide are concurrently maxima at an arsenate-ion concentration lying between 0.01 and 0.001-molar sodium arsenate. 4. Any condition or reaction that tends to remove the zinc arsenate coating from the zinc sulphide particles decreases dispersion and Brownian movement concurrently. EXPERIMENTAL Three samples of zinc sulphide were used. Lot I was C.P. zinc sulphide, washed well beyond absence of chloride, as shown by test with silver ion. Lot 2 was prepared by precipita-

Jan 1, 1943

By R. S. Shoemaker, F. W. McQuiston

RECOVERY METHODS AS RELATED TO PROPERTIES OF SILVER ORES The earliest metallurgical process for treating silver ores was amalgamation with mercury which was in use in the early 1500's. Closely following was the development of the Patio process for treating ores at Pachuca, Mexico. Silver often occurs as the native metal and in deposits associated with other metals such as gold, copper, lead and zinc. Principal silver minerals include compounds of sulfur, antimony, arsenic, and copper. Silver chloride, and argentiferous galena are also prime sources. Native silver and the chloride characterize the oxide zone of most deposits. Native silver can be concentrated, amalgamated, or cyanided. Silver chloride rapidly dissolves in cyanide without oxygen. Oxidized silver ores containing the higher oxides of manganese are generally refractory to metallurgical treatment. A refractory compound of manganese and silver is formed, probably a manganite , which is insoluble in cyanide solutions. Argentite is the predominant silver mineral. Other important economic minerals are native silver, argentiferous galena, cerargyrite, pyrargyrite and tetrahedrite. Argentite dissolves slowly, the reaction being reversible requires an excess of cyanide. Argentite with disseminated fine grained gold occurring in quartz veins with minor amounts of chalcopyrite and galena may be cyanided directly after grinding, with high silver and gold recoveries. The flowsheet adapted to this type of ore is the Minas de San Luis, Tayoltita cyanide plant, which treats a high grade argentite silver ore containing gold. It is a standard cyanidation circuit but employs long periods of agitation contact for the high silver sulfide content ore. Lead-zinc base metal semi-oxidized- complex ores in pipes and chimneys are replacement deposits in limestone at El Mochito Mine, Honduras. Mineralization comprises galena, cerussite, anglesite, sphalerite, calamine, and smithsonite. The silver content of about 16 ounces occurs as native silver globs, wire and the mineral argentite. After flotation of lead and zinc concentrates, the tailings are cyanided for gold and silver recovery. The great Huelva pyritic copper deposits of Spain carry a little gold and silver. At Cerro Colorado, these metals were concentrated above the chalcocite zone into the so-labeled Mgossanu. This material with a content of 0.08-0.09 oz Au and 1.50 oz Ag per ton is amenable to cyanidation. See Cerro Colorado flowsheet. In southern Hidalgo, about 60 miles north of Mexico City, are the great silver--gold veins of one of the foremost silver mining districts of the world. Real del Monte, Pachuca. The mineralized area consists of flow rocks and intrusives. The oxidized ores carry pyrites with oxides of iron and manganese and other minerals, silver and gold. The first zone contains

Jan 1, 1975

By G. M. Ritcey, A. W. Ashbrook, E. G. Joe

Solvent-in-pulp extraction of uranium from acid leach slurries of flotation concentrates is described. Solvent extraction was carried out in a 10 in. diam pulsed-plate column. The extractant was a 0.1 M tertiary amine (General Mills Alamine 336) in a kerosene diluent containing isodecanol as an emulsion suppressor and third phase inhibitor. In pilot plant operation at the Beaverlodge mill of Eldorado Mining and Refining, Ltd., slurry feeds containing up to 35% solids were processed at a throughput rate of 13.5 tpd of dry feed. Uranium extraction obtained was as high as 98%. Amine losses to the raffinate were approximately 0.07 lb amine per ton of original dry feed. The Beaverlodge Mill of Eldorado Mining and Refining employs a carbonate leach for the extraction of uranium from the ore.',' Prior to carbonate leaching sulphides are removed by flotation to reduce reagent consumption. This flotation concentrate containing some uranium is then leached with sulfuric acid, filtered, and the uranium precipitated with magnesium hydroxide. The precipitate is then returned to the carbonate leach circuit. Although the tonnage of flotation concentrate treated by acid leaching is low, reagent costs are relatively high. Also maintenance costs on the acid leach filtration circuit were beginning to show significant increases. The choice of solvent extraction-in-pulp as an alternative to the present circuit was influenced by the following factors: 1) elimination of acid pulp filtration, 2) increase in overall recovery because of soluble loss elimination, 3) reduction of reagent cost (mill sodium carbonate solutions are used as strip), and 4) production of higher purity precipitate at the mill site. Because a solvent-in-pulp process would be difficult to test on a bench-scale, the Eldorado experience in the use of pulse columns,3-5 mixer-settlers,6 and solvent-in-pulp operations in particular7 was applied directly to the initial pilot plant carried out during the summer of 1965 and followed by the second pilot plant in 1966. The latter work, which is presented in this paper, determined the following factors for anticipated scale-up to plant production: 1) overall uranium recovery by this process, 2) tonnage throughput expected, and 3) solvent losses anticipated for the full-scale plant. The equipment used consisted of a 10 in. diam extraction pulse column and three mixer-settlers for scrubbing, stripping, and acid equilibration. All equipment was designed by Eldorado and much of the pilot plant was built at the mill site. PROCESS CHEMISTRY Feed to the acid leach plant consists of a sulphide flotation1,2 concentrate containing mainly pyrite, uranium and graphite, with a particle size of 90%

Jan 1, 1968

By H. L. Riley, B. W. Gandrud

A froth flotation unit was added to the DeBardeleben Coal Corporation's Empire washer at Empire, Alabama, in the fall Of I94O following an investigation of possible ways and means of recovering coal values from settling-tank overflow or slurry. Officials of the DeBardeleben corporation hoped that some practical and reasonably economical way could be found for recovering fine coal from overflow water, although there had as yet been very little progress along this line in the Alabama coal fields. The Bureau of Mines was asked to cooperate in the project through its Southern Experiment Station, at University, Alabama. This paper presents a brief description of the process and the installation that resulted from the investigation of the overflow water or slurry problem at the Empire mine. The experimental data include' as a Part of this Paper were obtained during the course of the investigation in 1940 Since that time, however, the flotation unit has been running more or less continuously without significant operational changes and is still Performing pretty much in accordance with the data obtained in 1940. Flowsheet at Empire and Type of Coal Treated The Empire mine is developed on the Black Creek bed near the the border of the Warrior field. The coal in this bed is extremely low-ash and although there is an almost complete absence of bone coal and partings, the bed is so thin that, with mechanized mining, a high percentage of rock from roof and floor inevitably gets into the run-of-mine coal. The thickness of the Black Creek bed throughout the part of the Warrior field in which it is mined extensively is rarely over 30 in. and probably would average about 25 in, the coal is of the high-volatile A rank and of excellent quality, but as a result of admixture of roof and floor material, the run-of-mine product usually contains I ; to 20 pct rock by weight. he following is a proximate analysis on an "as-received " basis of a typical seam sample from the Empire mine:' moisture, 3.0 pet; volatile, 34.6 fixed carbon 58.3; ash, 4.1 This sample shelved 15,070 Btu per pound and 0.9 pct sulphur on a moisture-and-ash-free basis. In the Empire preparation plant the lump sizes above 3 in. are removed and hand-picked on a Marcus conveying Screen, the 3 to ? -in. size is removed by vibrating screens and washed in two Montgomery single-cell jigs, and the ?-in. to o slack is cleaned on four diagonal

Jan 1, 1949

Silver ore was first discovered in 1866 at Manhattan, and a few ore shipments were treated in a mill at nearby Belmont. The district was abandoned from 1869 to April 1, 1905, when rich gold float was discovered on what was to be called the April Fool claim. By early 1906, 4, 000 people lived in Manhattan. The San Francisco earthquake, in April of 1906, caused the withdrawal of capital from Manhattan and most of the mines were shut down. Later that year and in 1907, however, more strikes were made. The camp prospered until the mid-1920s, but a steady production of several hundred thousand dollars per year was sustained even during the great depression. Then, in 1939, Nevada's first bucket-line dredge was installed below the town and operated until 1947, producing $4.6 million in gold. The Houston International Minerals operation at Manhattan was started in July of 1980 at a throughput of about 545 mt per day (600 st per day). In contrast to the early day underground operations, Houston's mine is open-pit and processes low-grade disseminated ores. The ore is a metamorphic schist containing 2. 7 g Au and 1. 03 g Ag per mt (0. 08 oz Au and 0. 03 oz Ag per st). Some coarse gold, up to 1 mm in size, is present. Mining and haulage is done by a contractor. Stockpiled mine-run ore is crushed in three stages comprising a jaw crusher and two cone crushers, with screens ahead of the cone crushers. Crushed product, at about 19 mm (3/4 in.) size, is stored in a silo. Grinding is by single stage ball mill with the discharge passing over two hydraulic traps for coarse gold removal. These traps will be replaced in late 1980 by a two-cell Pan American jig treating the cyclone underflow. The jig hutch product, along with the hydraulic trap product that has been stored, will be treated further for gold recovery. The gravity tails will then be cycloned with the underflow being recirculated in the ball mill and the overflow being treated by flotation. A rougher concentrate is made in twelve No. 48 Galigher cells with the float tails being cycloned. Cyclone underflow is refloated in another four No. 48 cells; the overflow is treated in sluice boxes for further gold recovery before being sent by gravity to the tailings pond. Bulk flotation concentrates are cleaned three times with the final concentrate being thickened. The thickener underflow is then batch cyanided in mechanically agitated tanks and washed with barren liquor

Jan 1, 1981

By Henry P. Ehrlinger, James C. Bradbury

Tripoli is a naturally occurring, very finely divided form of silica found chiefly in some midwestern and southeastern states and used commercially as fillers and abrasives. Definitions Tripoli is a microcrystalline, finely particulate, more or less friable form of silica that appears to be the product of leaching of siliceous limestone or calcareous chert. The term was originally applied to a deposit near Seneca, Mo., that resembled material of that name found near Tripoli in North Africa (Hovey, 1894). The two deposits were subsequently found to have different physical characteristics -the North African tripoli, now called tripolite, is a diatomite, composed of the siliceous skeletons of microscopic marine plants called diatoms, and the Missouri tripoli contains no diatom remains; the term tripoli, however, continued to be used for the Missouri material and is now applied in a general way to most silica deposits similar to it in characteristics and geologic origin. In commercial trade tripoli is commonly understood to designate material from the Missouri-Oklahoma field; silica from southern Illinois, the other major producing area, is referred to commercially as amorphous silica. Each term, however, may be used commercially for material, regardless of place of origin, that has the characteristics or uses commonly ascribed to the material from one or the other major producing area. For example, in the commodity price listings, Engineering and Mining Journal routinely lists under Tripoli, prices "f.0.b. Elco, III." and "f.0.b. Seneca, Mo., and Rogers, Ark.," and under Silica, amorphous, prices "f .o.b. Ill.," and "f .o.b. Dierks, Ark." Amorphous silica, the commercial designation given to southern Illinois tripoli, is, like the term tripoli, a misnomer. Mineralogically, the southern Illinois deposits are composed of microcrystalline quartz, and no amorphous material has been detected during X-ray and scanning electron microscope investigations (Leamnson, Thomas, and Ehrlinger, 1969; Thomas et al., 1970). Soft silica is another term that has been applied to Illinois and Tennessee tripoli, presumably to distinguish it from the more compact Missouri material. It has also been used in the ceramic trade to distinguish tripoli from "hard" silica, or silica flour, produced by pulverizing silica sand (Heinz, 1937). Rottenstone, produced commercially in Pennsylvania, is similar to tripoli in that a major constituent is finely particulate silica, and its uses are much the same as those of tripoli- as abrasives and fillers. The origin of rottenstone also is similar to that of tripoli-decomposition of a siliceous sedimentary rock. The parent rock is defined as a siliceous limestone (Gary, McAfee, and Wolf, 1972; Thrush, 1968) or as shale (personal communication). Heinz (1937) quotes a brief statement describ-

Jan 1, 1975