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By Alvaro Abreu, Thomas Fraser

The work described in this paper was carried out under the sponsorship of the Foreign Economics Administration and in cooperation with the Departamento Nacional da Produggo Mineral, Rio de Janeiro. The project was undertaken to obtain complete data on the variations in washability of coal to be used for coke manufacture in the steel industry and to determine the economy of preliminary hand-sorting operations. The coal-producing industry of Brazil is in that pioneering stage in which operating practices and methods are just being developed. Increased wartime demand for fuel, coincident with a drastic curtailment of foreign supplies due to lack of shipping facilities, has put a tremendous pressure on the national industry to furnish more coal. Under this incentive, production facilities are being -expanded- and new methods of operation are being tested. Such changes are being developed both by improvement of existing methods that originated in the field and by adaptation and modification of methods introduced from the United States and Europe. These mining conditions and mining practices in Brazil are typical of what the American mining engineer will find in many instances when he goes pioneering into the developing coal fields of the Southern Hemisphere. The producing coal fields of Brazil are all in the southern states of that country. The coal measures are in a band roughly paralleling the coast and extending in a generally southwesterly direction from northern Sao Paulo through the states of Paraná, Santa Catarina and Rio Grande do Sul to near the Uruguayan border in the vicinity of Bajé. The accompanying map1 (Fig. I) shows the general location of these fields and also the principal routes of movement of both national and imported coal in a late pre-war year (1940). Statistical data on production by states up to that year are given in Table I. Rio Grande do Sul is still the largest producer among the coal states; but wartime

Jan 1, 1947

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Jan 1, 1938

By James E. Harding

The usual method of sampling mineral deposits is to drill holes and assay the sludge or core. Though the results thus obtained may not represent the true average value of the deposit, it is on these results that estimates of practically all large orebodies are made. In a large number of cases, the results of exploitation fall far short of the estimated value of the orebody. The standard method of making these estimates is to find the cubic contents of triangular prisms, in the apexes of which the drill holes are placed, by. multiplying the surface area by the average depth of the ore in the three drill holes and then multiplying the cubic contents by the specific gravity of the ore or rock to find the tonnage. The assay value is found by dividing the sum of the products of the depth of ore in each hole and the corresponding assay value by the sum of the depths of the ore in the three holes. As the latter part of this method is subject to many mathematical errors, it should not be depended on. Some engineers, therefore, use a discount factor, but as this factor is either arbitrarily selected or is obtained by obscure methods, the results are no better than guesswork. The standard method is correct when the drill holes are so laid out that the triangular prisms are equilateral in cross-section. But as ore deposits cannot always be drilled into at regular intervals and because of the human factor, if many holes are drilled, triangular prisms of all degrees of angularity are produced. In such cases it is necessary to assume that the influence of the different holes is not the same in all directions, which assumption of course is absurd. The area of the triangular prism is usually found by scaling; an ore-body of sufficient size to justify churn drilling is too large to be handled conveniently on maps having a scale larger than from 1000 to 1 to 1,500 to 1 and maps of such scales cannot be accurately measured. A variable is thus introduced in the first operation. In addition, the scaling is frequently done from blueprints, which sometimes shrink as much as 4 per cent. between printing, washing, and drying. The error due to scaling may be eliminated by surveying the location of each hole and

Jan 1, 1922

By I. Milton LeBaron

OPERATION of the phosphate flotation plant at the Peace Valley mine of the International Minerals and Chemical Corporation, Florida, began in the summer of [ ] 1942. Since that time several changes have been made in the flowsheet, with resultant increases in metallurgical results. Three flowsheets, together with the comparative plant results, are given in this paper, together with a discussion of the desliming circuit used for preliminary washing of the flotation feed. FIRST FLOWSHEET CHANGES Fig. I lists the essential units in the original flowsheet at the Peace Valley plant. The figures for tonnage and grade are average for a period of two months. Mineral Separation Airflow cells are used for both the fatty acid and the amine float. Three immediate difficulties presented themselves in the use of this flow sheet: I. Floating a maximum amount of phosphate in the rougher section to give good recovery sent a low-grade concentrate to the silica float, resulting in high costs for amine reagent in that section.

Jan 1, 1946

By E. S. Machlin

RECENTLY, there has been much activity in the field of nucleation of martensitic transformations.'- One of the problems in this field is the calculation of the rate of nucleation (number of plates nucleated per unit untransformed volume per unit time) in terms of observable parameters. Two such observable parameters are the fraction of the length of a straight line which corresponds to the portion of the total length of the line that lies in the martensitic phase and the number of plates intersected by this straight line per unit length of line. Because of the necessity of a valid answer to this problem, the following investigation was undertaken. Although this problem has been treated in the past, a derivation of the relation between the volume and linear fractions of martensite will be described to illustrate the method used in the succeeding analyses. It is assumed that the martensitic plates are in the form of a right circular cylinder having a small height relative to the radius of the base. The volume fraction of martensite is then: fr = lXNl,hjAl [1] where f, is the volume fraction of martensite, and Nij is the number of plates per unit total volume having the area Ai and the height hi. The linear fraction of martensite is obtained as follows. For the plates having the particular area A, and height h,, the fraction sin 0 dB* will have their cylinder axes between the angles 0 and 0 + d0 to the straight line along which the linear fraction of mar-

Jan 1, 1953

By J. Nutting, D. H. Kirkwood

The oxidation of lead sulfide in air between 200° and 350°C has been investigated by electron diffraction from thick sulfide films and from galena surfnces. It has been demonstrated that sulfate is the stable reaction product up to 570°C. Sulfate is HAGIHARA has investigated' single crystals of galena roasted in air by the reflection electron-diffraction technique, which owing to the very limited penetration of the beam into the crystal gives information of the nature of the surface only. He has shown that up to 280°C the first oxidation product is lead sulfate, followed by lead mono-oxysulfate (PbO . PbS04). At longer times and higher temperatures more complex patterns appeared which could not be analyzed. All of these patterns were of streaks or spots arising from crystals oriented on the galena surface, and it is probable that these crystals are lead compounds whose structures have not been determined, such as the other oxysulfates (2Pb0 • PbS04 and 4Pb0 . PbS04) or a number of oxides. Certain lead sulfide films, formed chemically, give ring patterns in transmission electron diffraction2 because they are polycrystalline, and should also give ring patterns of the products after oxidation. It was thought that a diffraction study would reveal the sequence of phases produced in the reactions at different temperatures, since X-ray powder patterns are available for many lead compounds. PREPARATION OF FILMS The films were prepared by passing H2S over a saturated solution of lead nitrate in water. Once a silvery film had formed on the solution surface, no further thickening was apparent. The films were transferred by a gauze to a bath of distilled water for washing and pieces of film were caught on small discs on which they were dried. The discs were formed initially on galena up to temperatures of 300°C, followed by oxide and oxysulfates in turn at longer times. The appearance of- these phases is believed to result from an inadequate rate of supply of sulfur to the top surface 01. the crystal. standard Siemens mounts, made of platinum alloy, and had seven 20-p apertures drilled through them. The parts of the film which had dried onto the disc surface were light blue in color, which is the interference color of a film about 600A in thickness. A strong pattern of lead sulfide was obtained in transmission electron diffraction through the apertures but slight broadening indicated a crystallite size of around 200A. Tilting a sulfide film in the beam produced arcing of the rings, increasing the intensities of the (Ill), (3111, and (222) rings and reducing (200) and (220). This arises from preferred orientation in the film, a [loo] direction of the crystallites being normal to the plane of the film. These specimens were oxidized in an oven maintained at the required temperature. The reported times include that taken to heat the film to the reaction temperature. STABLE PHASES FORMED IN OXIDATION The conditions in which various oxidation products of lead sulfide are stable have been considered by the authors in a previous paper.3 It was shown that in a normal atmosphere, taken as containing lo-' atm of SOs, lead sulfate would be stable up lo about 570°C. This was confirmed by oxidizing thin films of sulfide for several days, and the analysis of the transmission-diffraction pattern is given in Table 1. The fit with the patt$rn from X-rays is good, except for the missing 3.62A ring. Some disagreement in intensities of reflections given by X-rays and electrons is to be expected. Up to 570°C a spotty pattern of sulfate was still obtained, indicating grain growth, but above this temperature the film disintegrated. Probably this is associated with the decomposition to PbO . PbS04. It needs to be emphasized that the atmosphere

Jan 1, 1965

By J. T. Ryan

SiR Humphry Davy's epoch-making treatise delivered on Nov. 9, 1815, before the Philosophical Society of London, first announced and demonstrated a flame safety lamp for detecting methane in mine air. Coal mining was known in England as early as 1180, more than 600 years before the advent of a safe lighting and gas-detecting appliance. Mining, no doubt, took place first in outcrop coal, and danger from gas did not become apparent until the workings became deeper and more extensive. Davy's lamp did much to increase the safety of miners, and a modified Davy lamp is still widely used for detecting the presence and approximate amount of combustible gas in mine air. No factor in coal mining has improved more rapidly during the past 15 years than safety measures. This progress came about not only as a result of the workmen's compensation laws now in force in most of the states of the Union, but because the research work of the U. S. Bureau of Mines had demonstrated some dangers incident to coal mining which were not considered to be serious matters prior to that time. Electric power and explosives are necessary but potential hazards in American coal mines. A general mechanization program is now under way, while the mines are growing deeper and more extensive. Consequently ventilation problems are more complex and a demand has been created for positive detecting devices for carbon monoxide as well as methane. Scientists and manufacturers, working hand in hand during the past 10 years, have invented and developed appliances which make systematic and effective examination of mine air possible. The object of this paper is to describe briefly the approved testing devices in use today, with the hope that they may lead to the saving of life. Two Groups of Dangerous Coal Mine Gases Dangerous coal mine gases may be placed in two groups: (I) those that are dangerous because of their explosive properties, and (2) those that are dangerous because of their toxic properties. Methane (CH4) is the important gas of the first group, and in so-called gaseous mines constantly exudes from the coal and rock; it may accumulate and form an explosive mixture. The explosive range of methane-air mixtures is well defined. The low limit is 5 per cent., the high limit 15 per cent., and the most explosive

Jan 1, 1927

By H. W. Miller, V. H. Wilhem

Although the year 1933 was a period of uncertainty, considerable new development was initiated, with a high percentage of favorable results, for owing to financial conditions only projects of merit were proposed and developed. Unfavorable marketing conditions caused severe financial losses to refinery and sales departments of nearly all companies during the first half of the year. In anticipation of stabilized Government control, earnings were generally favorable during the third quarter but failure of the Government to take legal action against violators of the proration orders, and lack of agreement on a definite plan of curtailment, resulted in considerable overproduction and demoralization of the market structure during most of the final quarter. However, toward the close of the year Government action against violators of the Oil Code had a tendency to decrease overproduction materially and give the market a firmer tone. As a whole, the price structure of crude oil was maintained at a high level during the year; in fact, at a much higher level than the price of refinery products warranted. At no time during the year was production within 10,000 bbl. daily of the state allotment, overproduction of crude reaching a peak of 70,000 bbl. on Sept. 7, average daily average for the year being about 27,000 barrels. Numerous plans for equitable curtailment were prepared and tested during the year, none of which fully solved the many and intricate problems faced by operators who were in most cases willing to curtail if they could feel that cooperation was being practiced by their neighbors. Outstanding events in California oildom during the period under discussion may be classified under the following headings: 1. New discoveries. (a) New development in proven areas. (b) Deeper zones in settled pools. 2. Unproductive wildcat operations. 3. Whipstocking practice and procedure. 4. Progress of unit and orderly plans of development.

Jan 1, 1934

By C. R. Kyle, R. L. Perrine

A transparent model of a reservoir has been used to study some characteristics of instability in miscible displacement. The linear model dimensions are 1/4 in. x 91/2 in. x 10 ft. The model is packed with spherical glass beads. Thee groups of experiments have been performed. The objectives were to measure, respectively, the rate of growth of the transition zone, flow velocity variations in the transition zone, and the effect of a graded viscosity zone on stability. All experiments were compared, where possible, with theory. The transition zone grew almost linearly with distance traveled, regardless of flow rate, where adverse viscosity ratios were used. At very adverse viscosity ratios and large distances traveled, some reduction below linear growth was noted. This could be attributed to the effects of mixing. General similarity in flow pattern was commonly shown in different tests, although exceptions occurred at the higher viscosity ratios. Injection of tracer spots permitted direct experimental measurement of velocity variations. Statistical methods were used to compare observed velocity variations with recently published theories. Surprisingly good agreement with some theoretical predictions was obtained. In the experiments using an initially graded viscosity zone, macroscopic stability was reached before predicted by theory. Under conditions theoretically considered to be slightly unstable, any fingering tendency was too slight to become observable within a 10-ft long system. The general correlation of all experiments with published theory was good, and suggests that theoretical predictions can be extended to reservoir problems. INTRODUCTION Early laboratory studies of miscible displacement demonstrated the high recovery efficiency possible with this method. Linear laboratory models showed that, under some circumstances, all in-place hydrocarbons could be recovered using as little solvent as 5 per cent of the pore volume. These results led to a series of pilot field projects. Under realistic conditions, however, other laboratory studies showed that a small solvent bank may not recover much more oil than a conventional gas drive. The cause of this lack of efficiency is unstable viscous fingering. The size of the solvent bank required to give optimum recovery is, therefore, a question of great economic significance. The object of the experiments described in this paper was the quantitative measurement of unstable flow parameters, the verification of present theories on the miscible displacement process, and correlation of these theories with ex peri mental observation. Of the theories which have been advanced, those by Dougherty, Koval and Perrine show promise of predicting reservoir performance with reasonable accuracy.l-7 The present experiments were correlated, where possible, with the theories of Koval and Perrine. Dougherty's theory was not used because of the additional computational difficulty it presented and the belief that no further information would result. EXPERIMENTAL EQUIPMENT A transparent reservoir model, consisting of a vertical reinforced plexiglass column, was used for the experiments. The column was packed with glass beads, which served as the porous medium. To induce a known velocity disturbance in the flow, a double cosine wave restriction in the transverse cross-section was placed at the top of the column. To mark the flow field and provide a means of measuring the local fluid velocity, a dye-spot injection system was provided. The column was 10 ft high by 1/2 in. wide by 1/4 in. deep. The cosine restriction was placed 16 in. from the top of the column. The glass beads were smooth and spherical and had a mean diameter of 0.0102 cm. Liquids entered the top of the column through a manifold allowing three points of entry (left, center, and right, or any combination of these). A positive-displacement pump with variable-speed drive was used to control liquid flow rates. The pump transferred viscous oil from a reservoir to an accumulator, which displaced the test liquid into

Jan 1, 1966

By Noel Jarrett, Allen S. Russell, Bernard M. Starner, Stanley C. Jacobs

A process has been developed to refine high-grade commercial aluminum to 99.99 pct purity. This enzploys precipitating titanium, vanadium, and zirconiu~ as borides. The upgraded liquid is partially crystallized under conditions that prevent massive freezing. The resulting crystals are compacted and washed free of adhernig impure liquid aluminum by melting the top crystals while draining off the liquid. Finally, the bottorn portion of the crystal bed is melted and removed as the pure product. Leakage from the crystallizat~on vessel is prevented by a layer of alumina granules that are not wetted by the aluminum. ALUMINUM of 99.99 pct purity is desired in a variety of applications. These include electrolytic capacitors, catalyst carriers, decorative trim for automobiles, aluminum powder, and high-strength alloys. This market was for many years filled by refining commercial-purity aluminum in a three-liquid-layer electrolytic cell of the type originally proposed by Hoopes. To meet the expanding need for lower-cost high-purity aluminum, a refining process based on chemical precipitation and fractional crystallization was developed. The availability of this super-purity metal was announced in November 1961, and three patents1-3 relating to the process were issued in 1965. An alternate process, comprising continuous fractional crystallization of a portion of a liquid-aluminum feed stream under conditions of strong agitation at the surface of the growing crystals, was published by Dewey4 in 1965. Earlier proposals by Larsen 5 and by Regner6 also emphasized the advantage of rapid agitation of the melt in the region of the crystallization zone. johnson 7 more recently proposed extracting purified aluminum from an alloy by mixing crystals of pure aluminum into the molten alloy, allowing them to grow, and removing the pure aluminum as by casting. Aamot's 8 recent patent describes a freeze refining process that involves controlled partial freezing against cooled moving retort walls. The Alcoa process to produce high-purity aluminum is schematically described in Fig. 1. Relatively pure aluminum is treated with boron in a furnace (a) to precipitate high melting point impurities, the supernatant liquid is transferred to a crystallization vessel (b), the liquid is partially crystallized with mechanized "tamping" (c), the remaining impure liquid is tapped out and the crystal bed partially and directionally re-melted to wash the underlying crystals (d), and the balance of the crystals is melted and withdrawn as high-purity aluminum (e). PRINCIPLES OF FRACTIONAL CRYSTALLIZATION Commonly encountered impurity elements form two types of systems with aluminum. Titanium, vanadium, and some other transition elements in periodic groups IV, V, and VI are the high melting point impurities. Initial solidification of aluminum containing small percentages of these elements will produce solid markedly enriched in them at temperatures slightly above the freezing point of high-purity aluminum. Most other elements, such as silicon and iron, produce eutectic type reactions with aluminum. In this case the first solid formed on initial solidification at temperatures slightly below the freezing point for high-purity aluminum is markedly depleted while the remaining liquid is enriched in these elements. The equilibrium change in composition during solidification of aluminum contaminated with silicon, iron, or titanium is illustrated in Fig. 2. Here, for clarity, the temperature scale is expanded beyond the

Jan 1, 1968

By R. A. Vik, C. B. Daellenbach, W. M. Mahan

The influence of reduction roasting and thermal shock on the grindability of a refractory low-grade Michigan iron ore was examined in bench-scale tests. The quantitative effects of the various treatments were evaluated at three sieve levels, 48, 100, and 400 mesh, with ball-mill-grindability and work-index parameters as response indicators. Data from the testing program were statistically analyzed to isolate the effects of cooling rate, roasting temperature, mesh level, and ore chemical condition. All four variables were found to have an important influence on the grindability of the treated ore. Ore chemical condition and roasting temperature had the most pronounced effects.

Jan 1, 1972

By Damon H. McFadden

5.1-1. Geographic and Geologic Factors. Surface mines are located where the coal seam can be economically uncovered and where the product can be utilized competitively with other fuels. The planning and designing of a pit may follow various procedures. The sequence for consideration of the influential factors as considered here may not be complete for every pit, nor will it be necessary to be completely used in each design. It is suggested as a check and outline for the engineering approach. Controlling conditions for the layout should be listed and considered with the facilities and equipment for the exploitation. After these items, as listed below, have been discussed and the feasibility agreed upon, then the actual planning and design of the pit can be done. GEOGRAPHIC FEATURES. The location of the coal area sets the climatic stage. The rainfall, the temperature extremes, and the general weather conditions all affect the design of the pit. Overburden soil when wet may not be stackable and may be impossible to move by standard procedures. The coal seam itself may be so soft that it must not be traveled on when wet, as the losses may be the difference between a profitable venture and an unsuccessful one. Some equipment will work well on dry soil only, just as a dredge works only in the wet. The conditions must be checked and analyzed. Some equipment cannot handle frozen soil (wheel excavators), so temperature extremes must be noted. The extreme weather conditions may also govern the expected working days and therefore the ultimate production. The altitude (atmospheric pressure) may affect the equipment, and this should be checked. All of these conditions should be noted on the preliminary map of the area. GEOLOGIC FACTORS. The geologic and surface conditions of the coal field dictate the type of pit generally feasible. Rough terrain, rolling terrain,

Jan 1, 1968

By R. C. Earlougher

Based on laboratory tests conducted with the use of fresh core samples as well as a considerable amount of field data obtained from numerous water floods in northeastern Oklahoma, it appears that for any given oil saturation there is a critical maximum velocity above which the oil-recovery efficiency falls off very rapidly. In effect, when a water flood is operated above this critical velocity, the injected water-oil ratio rises extremely fast, thus shortening the economic life of the flood and reducing the ultimate oil recovery. This critical velocity apparently varies considerably with the percentage of oil saturation of the sand, so that in effect the higher the oil saturation at the beginning of a flood the higher the velocity that can be used successfully. In reviewing several of the earlier floods in the Mid-Continent area, it is concluded that most of the failures were due to two things: (I) too low an oil saturation, such as 30 per cent, and (2) too high water-injection rates, Although considerably more field data are necessary to establish definite limits, it would seem that the proper field injection rate for a 330 by 330 or 440 by 440-ft. spacing varies from approximately I bbl. per foot of sand per day where the oil saturation is as low as 30 per cent up to 5 bbl per foot of sand per day when the oil saturation is as high as 45 to 50 per cent, Introduction With secondary recovery by water-flooding receiving more and more attention throughout the industry, a greater working knowledge of multiphase flow under field conditions becomes more and more necessary A great deal of research has been carried on in highly idealized laboratory conditions, from which certain trends have been indicated, but with few exceptions no direct application to field use has been reported. widely varying conclusions have been drawn from the mass of idealized laboratory experiments and often this divergence apparently was due to the neglect of connate or interstitial water. Since interstitial water is such an important factor in water-flooding operations, it then follows that any laboratory flooding experiment must necessarily take it into account; and since it is difficult to set up laboratory models to allow for interstitial water, the next best procedure is to use fresh core samples for such tests. Even this procedure has its difficulties, inasmuch as it is possible to run only one flooding test on each sample, as each sample differs somewhat in character from all other samples. However, this disadvantage can be overcome to a large degree by the use of an extremely large number of samples. The next question that arises is: "IS it possible to get uncontaminated core samples having a true oil and water saturation like that existing in the reservoir?" If the sand under consideration is still in the primary stage of production, with a normal or relatively high amount of gas still in solution in the oil, probably it is not possible to get a nonflushed core. On the other

Jan 1, 1943

By R. C. Earlougher

Based on laboratory tests conducted with the use of fresh core samples as well as a considerable amount of field data obtained from numerous water floods in northeastern Oklahoma, it appears that for any given oil saturation there is a critical maximum velocity above which the oil-recovery efficiency falls off very rapidly. In effect, when a water flood is operated above this critical velocity, the injected water-oil ratio rises extremely fast, thus shortening the economic life of the flood and reducing the ultimate oil recovery. This critical velocity apparently varies considerably with the percentage of oil saturation of the sand, so that in effect the higher the oil saturation at the beginning of a flood the higher the velocity that can be used successfully. In reviewing several of the earlier floods in the Mid-Continent area, it is concluded that most of the failures were due to two things: (I) too low an oil saturation, such as 30 per cent, and (2) too high water-injection rates, Although considerably more field data are necessary to establish definite limits, it would seem that the proper field injection rate for a 330 by 330 or 440 by 440-ft. spacing varies from approximately I bbl. per foot of sand per day where the oil saturation is as low as 30 per cent up to 5 bbl per foot of sand per day when the oil saturation is as high as 45 to 50 per cent, Introduction With secondary recovery by water-flooding receiving more and more attention throughout the industry, a greater working knowledge of multiphase flow under field conditions becomes more and more necessary A great deal of research has been carried on in highly idealized laboratory conditions, from which certain trends have been indicated, but with few exceptions no direct application to field use has been reported. widely varying conclusions have been drawn from the mass of idealized laboratory experiments and often this divergence apparently was due to the neglect of connate or interstitial water. Since interstitial water is such an important factor in water-flooding operations, it then follows that any laboratory flooding experiment must necessarily take it into account; and since it is difficult to set up laboratory models to allow for interstitial water, the next best procedure is to use fresh core samples for such tests. Even this procedure has its difficulties, inasmuch as it is possible to run only one flooding test on each sample, as each sample differs somewhat in character from all other samples. However, this disadvantage can be overcome to a large degree by the use of an extremely large number of samples. The next question that arises is: "IS it possible to get uncontaminated core samples having a true oil and water saturation like that existing in the reservoir?" If the sand under consideration is still in the primary stage of production, with a normal or relatively high amount of gas still in solution in the oil, probably it is not possible to get a nonflushed core. On the other

Jan 1, 1943

By L. H Levenson, Charles S. Barrett

The orientation of metal crystals and grains, both large and small, can be detcrmined conveniently and accurately without the use of X-ray apparatus. This seems to be appreciated by so few metallurgists that it may be useful to explain in detail the method we have found most satisfactory in the laboratory—the reflection of light from crystallographie etch pits. This note includes a description of a suitable inexpensive instrument and instructions for etching various metals and for plotting the data. As the stereographie projection is used to facilitate handling the data, this note may he considered as an appendix to an earlier review of the metallurgical uses of the stercographie projection.' Various methods involving etch pits have been used by other investigators. Bridgman's method2 consists of attaching the specimen to a sphere (a transparent sphere is convenient4 , holding it at arm's length, and marking a spot on it when it has been turned so that the eteh pits reflect light into the eye of the observer from a lamp standing behind him. It has an accuracy of about 2" and is extrernely rapid. A greater accuracy can be obtained by having the reflected light fall on a screen, as has been done by Czochralski,5 Chalmers,6 and Schubnikov.7 All of these methods have been intended for undeformed single crystals. Tammann and his coworkers3,8 developed a method for estimating the number of grains in a polyerystalline aggregate having orientations in a given region of the stereographic triangle and thus obtained statistical information about deformation and reerystallization textures. While the method has had some use in recent years,9 it is not applicable to the majority of problems in physical metallurgy. Smith and Mehl10 determined orientations by plotting the directions of the sides of individual etch pits on a stereographic projection. The accuracy is limited to about 3" and the method requires careful polishing and high magnification.

Jan 1, 1940

By Charles S. Barrett, L. H. Levenson

The orientation of metal crystals and grains, both large and small, can be detcrmined conveniently and accurately without the use of X-ray apparatus. This seems to be appreciated by so few metallurgists that it may be useful to explain in detail the method we have found most satisfactory in the laboratory—the reflection of light from crystallographie etch pits. This note includes a description of a suitable inexpensive instrument and instructions for etching various metals and for plotting the data. As the stereographie projection is used to facilitate handling the data, this note may he considered as an appendix to an earlier review of the metallurgical uses of the stercographie projection.' Various methods involving etch pits have been used by other investigators. Bridgman's method2 consists of attaching the specimen to a sphere (a transparent sphere is convenient4 , holding it at arm's length, and marking a spot on it when it has been turned so that the eteh pits reflect light into the eye of the observer from a lamp standing behind him. It has an accuracy of about 2" and is extrernely rapid. A greater accuracy can be obtained by having the reflected light fall on a screen, as has been done by Czochralski,5 Chalmers,6 and Schubnikov.7 All of these methods have been intended for undeformed single crystals. Tammann and his coworkers3,8 developed a method for estimating the number of grains in a polyerystalline aggregate having orientations in a given region of the stereographic triangle and thus obtained statistical information about deformation and reerystallization textures. While the method has had some use in recent years,9 it is not applicable to the majority of problems in physical metallurgy. Smith and Mehl10 determined orientations by plotting the directions of the sides of individual etch pits on a stereographic projection. The accuracy is limited to about 3" and the method requires careful polishing and high magnification.

Jan 1, 1940

Jan 1, 1931

By L. G. Graper, E. L. Ramsey

THE present program of increased production of armament and lend-lease material for mechanized war has created a problem for the shops that must do the machining. They have naturally turned to the steel producers to provide them with a steel that can be accurately machined with the greatest possible speed. The adding of sulphur to steel as an aid to machinability has long been practiced; however, it may cause red shortness in rolling and may result in billets with seams and cracks, which must be removed before rolling can be continued. This conditioning of billets slows down production and' adds to the cost of making steel. Experience with various grades of sulphur steel made to different specifications has shown that Bessemer sulphur steels roll better than similar grades made in the open hearth, and also that low-carbon steels that are open or semikilled .as tapped roll better than completely deoxidized or killed steels. This has led to the belief that oxygen plays an important part in the rolling qualities of sulphur-bearing steels. It is generally held that the red shortness of sulphur steels is due to the low melting point of the sulphide compounds that separate out at the grain boundaries when the steel solidifies. At the rolling temperature of steel these sulphide compounds melt and cause cracking. ADDING SULPHUR AS A SULPHITE These difficulties can be avoided if sulphur is introduced into the steel by means of an anhydrous sulphite, such as sodium sulphite or sodium bisulphite, which-upon decomposition-forms sulphur dioxide. It is assumed that, in this case, the oxygen of the sulphur dioxide forms part of the sulphide inclusions in the steel, and raises their solidification temperature enough so that the formation in the steel of a low-melting eutectic is prevented. The result is the prevention of hot shortness and a more uniform distribution of inclusions. Fig. I shows photomicrographs of steels made with sulphur, while Fig. 2 illustrates the structure of steels made with sodium . bisulphite. These samples were cut from the steels as cast-that is, before rollingand were polished and lightly etched to bring out the grain boundaries. Fig. I shows that sulphide -inclusions segregate more or less at the grain boundaries, and it can be seen how the continuity of these low-melting inclusions would cause red shortness. Fig. z shows that the sulphide inclusions are more or less uniformly distributed throughout the matrix. This arrangement of inclusions has no apparent effect on the rolling qualities of a steel. This statement has been substantiated by the observation of the rolling of over 6000 tons of steel made with a sulphite addition. RESULTS As stated before, the sulphur dioxide-is added to steel by means of the decomposi-

Jan 1, 1942

By E. Miller, K. Komarek, W. Johnson

The activity of aluminum in solid Cr-A1 alloys has been measured by an isopiestic technique between Cr-A1890' and 1126" and 13 and 80 at. pct Al. The integral free energy of mixing has a minimum value of —5600 cal per g-atom at 59 at. pct Al. The maximum solid solubility of aluminum in chromium was determined to be 43 at. pct Al, and the composition limits of the compounds CrA14, Cr4A19, and Cr5Al, at 1000"~ were found to be 79 to 80, 66 to 70, and 59 to 63 at. pct Al, respectively. The thermodynamic properties of the Cr-A1 system have been investigated as part of a thermodynamic study of aluminum-transition metal systems.172 Little information is available on the equilibrium properties of the Cr-A1 system. The heats of formation of solid Cr-A1 alloys have been determined by Kubaschewski and Haymer at 600" and low-temperature specific heat data have also been obtained.~ More extensive work has been performed on the phase diagram, and a compilation has been provided by Hansen and Anderko,~ their phase diagram at elevated temperatures being essentially based on the work of Bradley and LU.~ The high-temperature portion of the phase diagram shows an intermediate phase CrA14 decomposing peritectically at 1018°C and existing at 82 at. pct A1 at 1000°C. They also identified the compounds with solubility limits of 72 to 75 at. pct A1 at 1000°C, and Cr5A1,, existing at 61 at. pct A1 at 1000°C. The maximum solid solubility of aluminum in chromium at 1000°C was found to be 46 at. pct Al. These elevated-temperature data were obtained by examination of quenched samples and were considered as less precise than the lower-temperature data. Koester, Wachtel, and Grube7 have revised the phase diagram as a result of their magnetic susceptibility and X-ray study. The results of this work differ appreciably from those of Bradley and Lu at temperatures above 800°C. The CrA1, compound is given as existing between 79 and 81 at. pct A1 at 1000°C, and they do not indicate the presence of a CrA13 phase reported by Bradley and Lu. They also report the compound Cr4Alg as having solubility limits of 66 to 70 at. pct A1 at 1000°C, while Bradley and Lu show this compound stable only up to 870°C. Koester et al. state that the high-temperature modification of the compound Cr5A18 is stable down to 1125"C, and not 980°C as stated by Bradley and Lu, and that the low-temperature modification of Cr5Al, has a range of homogeneity of 58 to 63 at. pct A1 at 1000°C. They also report that the maximum solid solubility of aluminum in chromium is 43 at. pct A1 at 1000°C. APPARATUS AND EXPERIMENTAL PROCEDURE An isopiestic method was employed which has been successfully applied to the determination of aluminum activities in solid ~e-All and Ni-Al alloys. Alloy specimens were held at different positions in a temperature gradient and were equilibrated with aluminum vapor from an aluminum reservoir kept at the temperature minimum of an impressed thermal gradient in a closed alumina system. Diffusion of aluminum into the specimens occurred until equilibrium was reached, at which the partial pressure of aluminum in each of the specimens was given by the vapor pressure of the pure aluminum reservoir. The activity of aluminum referred to liquid aluminum as the standard state in a given equilibrated sample at temperature T could therefore be expressed by: vapor pressure of pure aluminum at _ the temperature of the reservoir Vapor pressure of pure liquid aluminum, at specimen temperature T Since both the temperature of the aluminum reservoir and the specimen temperatures were determined experimentally, and the vapor pressure of pure aluminum is known as a function of temperature,' the activity of aluminum in a given aluminum alloy of known composition could be calculated. Initial runs were made with samples consisting of pure chromium chips placed in alumina crucibles. These runs exhibited large inconsistencies, indicating that equilibrium was not attained. High aluminum content Cr-A1 alloy powders were therefore substituted for the pure chromium specimens. The starting composition of the alloys was adjusted through experimentation until the concentration change necessary to attain equilibrium was small. In this manner, consistent results were obtained in reasonable times. SPECIMEN PREPARATION Alloy specimens were prepared from chromium of 99.997 pct minimum metallic purity: with 0.028 to 0.038 pct H, 0.0002 pct N, and 0.27 to 0.46 pct 0 (Aviquipo, Inc.). The aluminum had a purity of 99.99+ pct and the following impurities: 0.003 pct Cu; 0.002 pct S; 0.002 pct Fe; 0.001 pct Pb; 0.001 pct Ga (Aluminum Corp. of America). Alloy powders were prepared from weighed mixtures of chromium and aluminum by double-arc melt-

Jan 1, 1969

By Herbert H. Kellogg, Hugo Vasquez- Rosas

Recently the long-chain primary amines have been used extensively for the flotation of silicate minerals. The use of amines to float sulphide minerals has been investigated by several authorsl-5-l8 but most of this work has been done with the short-chain (less than six carbon atoms) primary amine compounds or the more expensive secondary, tertiary and quaternary amines. Perhaps the fact that the long-chain amines are good collectors for the common gangue minerals has led investigators to omit them from consideration as collectors for the selective flotation of metallic sulphides. The work reported in this paper was designed to investigate the use of a typical long-chain amine salt, laurylamine hydro-chloride, as a collector for the flotation of galena-sphalerite ores. The results show that laurylamine hydrochloride (LAmHCl), when used in small amounts, is a good collector for the selective flotation of sphalerite and galena from the common gangue minerals. The differential flotation of sphalerite from galena was not accomplished but the amine flotation of sphalerite after the standard xanthate flotation of galena is possible. The experimental work reported herein is not complete enough to be able to say whether amine flotation of lead-zinc ores would prove superior to xanthate flotation, or whether the method is even applicable to a more complex ore than the one used for this work. However, the apparent reagent costs for the flotation operations described in this paper seem to be less than for xanthate flotation. This fact alone should be sufficient to encourage the millman to investigate the use of these amine reagents, especially as these reagents are available on a commercial scale at a reasonable price. This paper has as its secondary purposes to illustrate how contact-angle measurements have aided in this investigation, and to bring forward some evidence concerning the mechanism of the collecting action of primary amines. Contact-angle Tests The contact-angle measurements were made by the method described by del Giudice6 and used in recent work by Taggart and his collaborators.7-9 The mineral specimens for the contact-angle tests were carefully chosen, to avoid cracks and inclusions of other minerals. All specimens were mounted in "transoptic" plastic mounts and the surfaces were cleaned by polishing with levigated alumina on a cloth-coverkd glass polishing wheel. Distilled water was used on the lap during the polishing and at all subsequent steps in the contact-angle tests. The mounted mineral specimens were handled with glass forceps and special care was exercised to prevent exposure of the clean surface to air or any other source of contamination.

Jan 1, 1947