Search Documents

By J. A. Fellows, Earnshaw Cook, H. S. Avery

THE increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloy presented in a companion paper.? The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. THE CREEP TEST Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test laboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit 1000-hr. tests in the temperature range of 1200° to 2200°F. with a choice of applied stress extending from 50 to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10.1 ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a 1-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, 20 per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with alundum cement; the distribution of turns is adjusted to give a maximum temperature gradient of ± 1°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used to reduce the temperature of the threaded

Jan 1, 1942

By H Pray, H. W. Russell, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By H. W. Russell, H Pray, Paul D. MILLER

It is known that austenitic chromium-nickel steels that have free carbide in the grain boundaries are subject to intergranu-lar corrosion. It is difficult to detect such a susceptible condition in a fabricated article because present test methods require a sample section for examination and in most cases this is difficult to obtain. The question of the nature and prevention of intergranular corrosion in austenitic stainless steels has been ably discussed by Bain and co-workers1-3 and by other investigator4-10 The present methods of study subject samples to corrosive conditions in such reagents as the Strauss solution, a mixture of copper sulphate and sulphuric acid. Such tests usually require at least 72 hr. to run. Various methods of measuring the degree of sensitization have been employed, such as the measurement of electrical resistivity, magnetic measuremerits, measurement of the degree of cracking produced on bending over a malldrel, and microscopic studies. The detection of carbides at the grain boundaries by metallographic polishing and etching methods is tedious and requires a skilled operator. A recent report on such methods of carbide detection is given by the American Society for Testing Materials Subcommittee VI of Committee A.-1011 and by Arness.12 The present investigation was undertaken to develop a simple test procedure for detecting carbide precipitation or susceptibility to intergranular corrosion. The test is designed for use in the plant and for the testing of fabricated structures. Carbide precipitation, the factor leading to susceptibility to corrosion, is produced by heating the alloy in the temperature range 800° to 1600°F., as in welding, in improper annealing or in service where such temperatures are met. The connection between such precipitation and susceptibility to corrosion has been thoroughly discussed, as has been the use of stabilizing addition elements to prevent precipitation. Experimental Method A small area of the steel under test is subjected to an anodic treatment in a cell that can be 'lamped Onto a a Or an actual structure. The cell and electrical circuit used are illustrated in Fig. I. The cell C is lead, joined to the steel plate D and insulated from it by a short piece of rubber tubing E. The cell is forced tightly against the steel plate by a spring Or clamping device. The seal formed by the rubber against the steel plate is sufficient to retain the liquid bath inside the cell. The spot treated can be made any shape desired, depending on the shape of the rubber gasket. The cell illustrated polishes a circular spot about 3/8- diameter' The bath consists of 60 per cent (by weight) sulphuric acid to which is added 5 ml. per liter of Glycyrrhiza extract (U.S.P.). The cell requires about 2 to 2.5

Jan 1, 1941

By C. R. Dodson, D. Goodwill, E. H. Mayer

The paper summarizes the historical background of the pressure-volume-temperature analyses of reservoir fluids, the errors involved in both the sampling and testing of reservoir fluids, the type of information required of a PVT determination, and the field conditions that limit the application of any one analysis. Particular emphasis is placed on the necessity for approximating as closely as possible the liberation sequence occurring in the producing formation, flow string, and surface separators. A combined differential and flash or "composite" liberation is suggested as the best means of approximating this liberation sequence. HISTORICAL BACKGROUND Petroleum reservoir engineering commonly is considered to be one of the newest fields of petroleum science, yet much work of a theoretical and intuitive nature was done many years before the modern techniques of reservoir analyses were developed. The period 1910-1924 saw considerable work in the field of reservoir behavior done by the U. S. Bureau of Mines. This work:.' although entirely theoretical, pointed out the importance of gas in the recovery of oil from the reservoir. The statement by J. 0. Lewis that 20 per cent or less of the oil originally in place in a pool was recovered from the ground under uncurtailed production conditions caused some operators to re-examine and modify their production methods. However, though these works showed methods of production that have subsequently resulted in greater oil recoveries, they in general went unnoticed, even though there was a fear that the nation's petroleum resources were being exhausted. The period 1924-1933 saw the industry take considerably more interest in reservoir behavior because of an unfounded fear of its inability to replace oil reserves, the possibility of government regulation, and the energy of one man, Henry L. Doherty. Doherty aroused heated discussions in the industry concerning conservation. To prove or disprove his theories the first experimental work on the reservoir behavior of petroleum was undertaken. The papers of Dow and Calkin,' Beecher and Parkhurst," and Mills and Heitheckere are classics although their experimental procedures were crude. These papers proved that the properties of petroleum in the reservoir are quite dissimilar to the properties measured at the well head. Gas dissolved in the oil phase was recognized as having considerable importance as had been predicted by the earlier theorists. Slightly later Miller and his co-workers assembled the first text correlating all the known data on the reservoir behavior of petroleum and used, these data to show the economic value of conservation. Quantitative application of pressure-volume-temperature analyses of reservoir fluids was given in the paper of Coleman, Wilde, and Moore"; this work showed that with sufficient laboratory and production data prediction of reservoir behavior was possible. The refined sampling and labora-

Jan 1, 1953

By W. Bradley, R. G. Hall

This paper will attempt to show how a metallurgical problem at one California quicksilver mine was solved, and how the solution was applied successfully at another mine. The pronouns "we" and "our," as used below, refer '0 the Bradley 'lining Co. of San Francisco. The term "concurrent firing" for the purpose of this paper can be defined as feeding and firing a a kiln at the same end—that is, of course, the upper end' This is as opposed to "countercurrent firing," the orthodox method, in which a kiln is fed at the upper and fired at the lower end. The terms "quicksilver" and "mercury" are used interchangeably. Early References The earliest work on nonferrous metallurgy, we believe, was The Pirotechnia of Vannocio Biringuccio,l its first edition having been printed in Italy in 1540. Quoting from its chapter entitled "Concerning Quicksilver and Its Ore": Quicksilver ... is one of the gods and has divine strength in itself, and also, to the annoyance of the alchemists, it is winged. Hence, when it sees that it is in gravest danger, it loosens itself from . . . every bond . . . and fies away into the heavens, escaping from the hands of those who crucify it. Almost laughing, it leaves all its adversaries mocked and scorned, with their phials and filters empty . . . How thorough a job, under certain conditions, it can do of mocking its adversaries and leaving their phials and filters empty, was found out four centuries later at the Sulphur Bank mine, on the east shore of Clear Lake, in Lake county, California, The other mine mentioned in the title is the Reed, in Yolo County, California, 35 miles by road southeast of Sulphur Bank, Reed and Sulphur Bank ranked respectively Nth and seventh in U. S. production in 1943. The earliest direct reference we can find to furnacing troubles at these mines was by Thomas Egleston in 1890.2 Speaking of Sulphur Bank, Egleston says: of there is more sulphur than cinnabar in the ore, which is a detriment to both . . . making the sulphur impure, and rendering the cinnabar difficult to work on account of the soot. In some of the early . . . furnaces the accumulation of soot from the excess of sulphur has been known to penetrate as far as the fan blower at the end of the . . . condensers, and completely prevent its revolution. In order to get rid of the inconvenience of this accumulation . . . , as well as to get a commercial value from the sulphur, it (the sulphur) is now separated by steam and sold. It is claimed that the sulphur alone pays all the expenses of ... the mine. The mine was first worked for sulphur, and the cinnabar it contained was considered to be an inconvenience, and was carefully picked out and thrown away, as its richness and value were not

Jan 1, 1949

By L. C. Brown, E. B. Hawbolt

The formation of grain boundary precipitates has been studied in Ag-5.64 wt pcl Al alloys at 688°C. Large-grain specinzerzs were used and the boundary misorientation measured by X-ray diffraction. At low-angle grain boundrrries Primary sideplates form. u)hile abore a 17-deg misorientation lenticular precipitates predominate. Growth of the lenticular precipitates was studied on individual grain boundaries using a statistical technique. The thickening and lengthening rates appeared to be independent of &apos;pain boundary misorientation, indicating that grain boundary diffusion was not significant in this system. The precipitates grew urith constant shape, with both the length and thickness increasing parabolically with time. The parabolic lengthening rates were unexpected since previous theory and experimerztal results had indicated linear growth. By approximating the shape of the precipitate to that of an oblate spheroid grouling with constant shape an equivalent diffusion coefficienl was calculated. The zlalue obtained was in good agreement with nleasurements obtained fron, diffusiorz couples. IF a single-phase alloy is heated or cooled to a temperature such that the phase becomes supersaturated, there is a tendency for a second phase to precipitate from it in order to remove the supersaturation. Precipitation takes place initially on grain boundaries due to preferred heterogeneous nucleation, but subsequently Widmans kitten plates may form in the grain interiors if the grain size and supersaturation are sufficient. The type of grain boundary precipitate formed depends on the nature of the boundary. Aaronson1 and clark2 have shown that grain boundary misorientation can be characterized by the simple parameter R, where and X, Y, and Z represent the minimum rotations about three orthogonal axes required to bring the two lattices forming the grain boundary into coincidence. The maximum value for R is 60 deg. In using this parameter the orientation of the grain boundary itself is, of course, neglected. However it was found in both Fe-si3 and A1-Ag2 that the precipitate shape depended only on the parameter R. Clark found that the vast majority of precipitates formed were allo-triomorphs— lens-shaped precipitates that grew along the grain boundaries. At low-angle boundaries, however, (R < 15 deg) Widmanstatten sideplates nucleated at the grain boundaries and grew into the adjacent grains. It has been reported that the rate of growth of grain boundary precipitates is controlled by diffusion within the supersaturated phase.&apos; The theories which have been developed for growth rates have assumed the diffusion coefficient constant over the composition range of the supersaturated phase. This is a fairly good approximation if the composition range involved is not large. Thickening rates have been calculated using the theory developed by Zener4 and by Frank5 for the growth of planar precipitates. A parabolic growth law

Jan 1, 1968

By K. E. Merklin, F. D. DeVaney

In the past most of the research in pelletizing has as its aim the production of a physically strong pellet. Now that this problem is solved, more attention is being paid to uniformity in grade and chemical composition. Consideration has been given in recent years to a study of additives which will make pellets partially or fully fluxed. Blast furnace tests show fluxed pellets to have advantages over both fluxed sinter and acid pellets. Lower slag volumes are used more frequently in the blast furnace and the uniformity of the charge, both physically and chemically, is becoming increasingly important. A considerable improvement can be secured by having all of the flux uniformly distributed through the pellets in a calcined state. A fluxed pellet, therefore, should be a superior product. The use of an ore burden that contains an appropriate quantity of fluxing materials is not new to the blast furnace industry. For years the Minette ores of France and Germany, the Clinton ores of the Birmingham, Ala., areas, as well as others, which are low in iron but contain calcium carbonate in sufficient quantities to give them self-fluxing properties, have proven economical. The adaption of the sintering process to the preparation of ore burdens provided a means for artifically associating the fluxstone with the iron ore prior to charging to the blast furnace. In 1944 Torpl discussed the effects of using lime in sinter made in Sweden on the sinter&apos;s metallurgical performance in a blast furnace. Hessle2 reported in 1945 on the advantages of using lime in sinter to increase the sintering plants&apos; capacity and reduce fuel requirements. Robinson3 discussed the use of lime in Swedish sintering practice at the 1950 Blast Furnace, Coke Oven, and Raw Materials meeting. One of the suggested advantages was the combining of lime with silica to prevent the formation of a fayalite slag, which is difficult to reduce in the blast furnace. Nilson4 at the same meeting commented briefly on experimental work that had just started in the U. S. on the use of lime in sinter. The literature tends to indicate that most of this early work was directed towards improvement in sinter physical quality, and the fact that the feed to the blast furnace was partially fluxed was incidental. It was not long, however, before blast furnace advantages were being claimed. The matter was forcibly called to the attention of North American operators by reports of remarkable production records established by the Russians using fluxed sinter. The leading step was taken on this continent by the Steel Company of Canada in 1957; McMahon5 reported on the marked improvement in performance of an 18-ft blast furnace using fluxed sinter at its Hamilton works. Other North American operators quickly followed theStelco lead.

Jan 1, 1963

By P. K. Koh

Chi phase (body-centered cubic, a = 8.89A) was found in as-cast 23 pct Cr-10 pct Mo-Fe alloy as well as in heat-treated 316, 316L, 317, and modified 446 stainless steels. Chi phase resembles sigma phase in its metastability, chemical composition, and brittleness. Microstructure and some of physical properties of chi phase were developed. MOLYBDENUM has been established as a desirable alloying element for the enhancement of corrosion resistance in Cr-Ni steels and creep and rupture strength in high temperature alloys. On the debit side, however, the molybdenum addition has been known to stimulate u formation. When the molybdenum-bearing steels were subjected to prolonged heating at elevated temperatures, losses of corrosion resistance and/or ductility have been observed. Andrews1,2 first found the existence of a new phase among the anodic FeC13 extracts from type 316 stainless steel solution treated and then reheated from 800" to 1100°C. This phase was designated x and was identified by diffraction patterns as of body-centered cubic structure with a value equal to 8.89? and similar to that of a manganese. He found that the x phase in this steel always coexisted with s phase, but failed to distinguish one from the other by metallographic technique. No definite conclusion was drawn regarding the equilibrium temperature ranges of these two phases. The appearance of Andrew&apos;s work recalled an un- explained structure observed several years ago at the Allegheny Ludlum Research Laboratories during the investigation of an experimental alloy containing 25 pct Cr, 10 pct Mo, and balance Fe. X-ray diffraction patterns on the as-cast material revealed the presence of a body-centered cubic phase having a lattice parameter of 8.89?. The structure was sufficiently similar to that of y chromium that for a time it was thought that the structure might be caused by the presence of some undissolved electrolytic chromium particles. The alloy as-cast was so brittle that it shattered after the slightest hot reduction by hammer cogging. This paper gives the results of some metallographic and X-ray diffraction studies on x phase as found in several experimental alloys as well as a few molybdenum-bearing commercial stainless steels. The analyses of materials studied were as shown in Table I. Experimental Procedure Metallography: Solid specimens were polished mechanically and etched in boiling 50 pct HC1 solution in order to best delineate x and s phases in the alloys studied. X-Ray Diffraction: The difficulty of satisfactorily developing diffraction lines for s phase in solid specimens has been previously reported by Bindari, Koh, and Zmeskal.V or this reason all specimens used in this investigation were subjected to anodic

Jan 1, 1954

By G. R. Gardner, D. H. Davis

INCREASING realization of the importance of dust control, and the recommendations of various agencies, have led the mining industry to become actively concerned with this problem. The background and necessity for adequate dust-suppression measures have been discussed in a number of publications, including those of the U. S. Bureau of Mines, and the use of spray water to reduce dust at the face and on roadways has been recommended. The problem resolves itself into obtaining adequate dust reduction at a reasonable cost. Inasmuch as the term "adequate dust suppression" has never been clearly defined, nor have permissible limits of dustiness (in terms of dust count) been established, it is apparent that any method selected may be required to meet additional demands. Until the industry has been given some indication of permissible limits of dustiness, no permanent solution is possible. Progress will be somewhat handicapped until such information is available. In addition, dust reduction must be obtained without the addition of any excessive moisture to the coal, since consideration must often be given to: I. Quality standards, particularly reduction in heat value. 2. Handling characteristics, particularly in regard to unloading from railroad cars and bins. 3. Application of dry methods of coal cleaning. 4. Necessity for fine screening within specified limits of oversize and undersize. Little detailed information is available as to the advantages and disadvantages of the several methods of water distribution, the location and protection of sprays, operating data on pressure, quantity of water, and so forth, and results obtained. In 1940 an investigation was undertaken to determine and evaluate the principal factors involved. This paper constitutes a progress report on this work and cannot in any way be regarded as complete on any one of the several phases. CLASSIFICATION OF DUST SOURCES The various sources of underground dust may be classified as primary or secondary. A primary source is one associated with appreciable degradation of size, that is, where the greater part of the actual fines capable of becoming air-borne dust are produced. A secondary source may be considered as one in which the greater part of the fines have been produced at some previous operation and are in such condition that they can be dispersed as air-borne dust. These conceptions appear to be of practical significance, as experience indicates that when dust is controlled at the primary sources the importance of secondary sources is minimized. For these reasons, investigations to date have been concerned principally with the primary sources of dust, and this paper is concerned particularly with one of these-namely, undercutting. In accord with the foregoing definitions, the sources to which the following opera-

Jan 1, 1942

By Walter E. Duncan

The ores treated at the concentrating plant of the Mahoning Mining Co. at Rosiclare, Ill., come largely from the blanket replacement deposits of the northeastern part of Hardin County, Illinois, and consist of complex mixtures of galena, sphalerite and fluorspar in a gangue of quartz, limestone and sandstone. The several minerals are so intimately inter-grown that they are not liberated at the sizes usually treated by gravity concentration in the usual fluorspar plant. For this reason, an all-flotation method of concentration was developed in cooperation with the station of the U. S. Bureau of Mines at Rolla, Mo.1 This flotation separation made possible the commercial production of four coyentrates: (I) lead, (2) zinc, (3) acid-grade fluorspar and (4) metallurgical-grade Auorspar.2-3 Although fluorspar had been floated in Canada in 19214 and a plant at Rosiclare had been floating fluorspar since March 1929, fluorspar flotation was given considerable impetus by the Mahoning developments, since some features of the separation were quickly adopted by other fluorspar companies. The Bureau of Alines5 reports that in the 10 years preceding 1938 only 50,552 tons of fluorspar flotation concentrates were produced in the United States. The rise from this almost nominal figure to 153,750 tons (largely acid grade) in one year (1944)6 is indicative of the activity in fluorspar flotation occasioned by the war. The industry thus proved to be in a position to expand and keep up reasonably well with the requirements imposed upon it by such developments as occurred in high octane aviation gasoline alkylation, in the use of Freon as a refrigerant and as carrier in the Aerosol "bug bomb," and in the atomic bomb project as well as in the expansion of other activities requiring hydrofluoric acid; for example, the aluminum industry. Despite the fact that the greater portion of acid-grade fluorspar produced in the last few years went directly into war uses, the future of the acid-grade field still appears bright. As a result of the activity in fluorine chemistry during the war, it seems likely that in the relatively near future almost every phase of human endeavor will find some fluorine compound involved. The other three concentrates produced deserve some attention in these introductory remarks. The lead concentrates first produced contained both zinc and fluorspar but these did not interfere with their marketing. As will be pointed out later, the quality has steadily improved until today it is a relatively high-grade product. Although some zinc smelters accept concentrates containing limited quantities of fluorspar, it is a very objectionable impurity. Since flotation methods fail in the complete removal of the fluorspar, chemical methods were developed for

Jan 1, 1948

By Walter E. Duncan

The ores treated at the concentrating plant of the Mahoning Mining Co. at Rosiclare, Ill., come largely from the blanket replacement deposits of the northeastern part of Hardin County, Illinois, and consist of complex mixtures of galena, sphalerite and fluorspar in a gangue of quartz, limestone and sandstone. The several minerals are so intimately inter-grown that they are not liberated at the sizes usually treated by gravity concentration in the usual fluorspar plant. For this reason, an all-flotation method of concentration was developed in cooperation with the station of the U. S. Bureau of Mines at Rolla, Mo.1 This flotation separation made possible the commercial production of four coyentrates: (I) lead, (2) zinc, (3) acid-grade fluorspar and (4) metallurgical-grade Auorspar.2-3 Although fluorspar had been floated in Canada in 19214 and a plant at Rosiclare had been floating fluorspar since March 1929, fluorspar flotation was given considerable impetus by the Mahoning developments, since some features of the separation were quickly adopted by other fluorspar companies. The Bureau of Alines5 reports that in the 10 years preceding 1938 only 50,552 tons of fluorspar flotation concentrates were produced in the United States. The rise from this almost nominal figure to 153,750 tons (largely acid grade) in one year (1944)6 is indicative of the activity in fluorspar flotation occasioned by the war. The industry thus proved to be in a position to expand and keep up reasonably well with the requirements imposed upon it by such developments as occurred in high octane aviation gasoline alkylation, in the use of Freon as a refrigerant and as carrier in the Aerosol "bug bomb," and in the atomic bomb project as well as in the expansion of other activities requiring hydrofluoric acid; for example, the aluminum industry. Despite the fact that the greater portion of acid-grade fluorspar produced in the last few years went directly into war uses, the future of the acid-grade field still appears bright. As a result of the activity in fluorine chemistry during the war, it seems likely that in the relatively near future almost every phase of human endeavor will find some fluorine compound involved. The other three concentrates produced deserve some attention in these introductory remarks. The lead concentrates first produced contained both zinc and fluorspar but these did not interfere with their marketing. As will be pointed out later, the quality has steadily improved until today it is a relatively high-grade product. Although some zinc smelters accept concentrates containing limited quantities of fluorspar, it is a very objectionable impurity. Since flotation methods fail in the complete removal of the fluorspar, chemical methods were developed for

Jan 1, 1948

By C. S. Westerberg, C. P. Heiner

Observation of the clinkering action of coal from the Castle Gate D seam in underfeed stokers over a period of years has given rise to the present investigation of the effect of bony coal on clinkering. Some very costly examples of slagging clinkers in particular cases have been of especial interest to the authors. In such cases coal analyses and ash-softening and fluid temperatures have been found of little value. In general, it was noted that slagging mas accompanied by a somewhat higher ash content of the stoker slack, and the suspicion naturally arose that foreign matter was the troublemaker. One would naturally suspect bony coal and rock impurities because of their occurrence and prevalence within the seam and the relative absence of sulphur or other impurities in the coal mined. The test results given herein indicate that the concentration of the bony coal and rock impurities in the coal determines the clinkering tendencies of the ash during combustion. Castle Gate D Seam Extending from the Utah-Colorado line near Grand Junction, Colo., westward to Greenriver, Utah, and thence in semicircular form north and westward to Castle Gate, and from there southward to Mt. Hilgard in central Utah, is a line of nearly perpendicular cliffs, composed of interbedded massive sandstone and shales, making up the coal-bearing horizon of the Mesaverde formation of Upper Cretaceous age. The cliffs face roughly concentrically toward the south and southeast and the strata, with conformably enclosed coal beds, gently dip away from the face of the cliffs and at right angles to their front line. Back of these cliffs the mountain masses rise to an altitude of from 8000 to 10,ooo ft. above sea level. Stretching away from their foot is a great shale plain, on which the towns are situated and over which the railroad lines and highways run. The Castle Gate mines enter the coal beds at their outcrop; the workings extending within a particular coal bed away from the outcrop and under the mountain mass back from the cliff line (Fig. I). Throughout the Mesaverde formation in the Castle Gate general area, there are from two to five workable coal beds. Usually not all of these are coincidentally of workable size and merchantable quality throughout any given large tract. In the Castle Gate mine area, the base of the Mesaverde horizon and coal measures is marked by a massive, cliffmaking, gray sandstone bed 60 to 80 ft. thick. Locally this is referred to as the "Castle Gate sandstone floor." Frank R. Clark, in U. S. Geol. Survey Bull. 793, designates it as the "Aberdeen sandstone." At Castle Gate the various coal beds are designated by the letters A, B, C, etc., commencing with the lowest bed.

Jan 1, 1942

By C. P. Heiner, C. S. Westerberg

Observation of the clinkering action of coal from the Castle Gate D seam in underfeed stokers over a period of years has given rise to the present investigation of the effect of bony coal on clinkering. Some very costly examples of slagging clinkers in particular cases have been of especial interest to the authors. In such cases coal analyses and ash-softening and fluid temperatures have been found of little value. In general, it was noted that slagging mas accompanied by a somewhat higher ash content of the stoker slack, and the suspicion naturally arose that foreign matter was the troublemaker. One would naturally suspect bony coal and rock impurities because of their occurrence and prevalence within the seam and the relative absence of sulphur or other impurities in the coal mined. The test results given herein indicate that the concentration of the bony coal and rock impurities in the coal determines the clinkering tendencies of the ash during combustion. Castle Gate D Seam Extending from the Utah-Colorado line near Grand Junction, Colo., westward to Greenriver, Utah, and thence in semicircular form north and westward to Castle Gate, and from there southward to Mt. Hilgard in central Utah, is a line of nearly perpendicular cliffs, composed of interbedded massive sandstone and shales, making up the coal-bearing horizon of the Mesaverde formation of Upper Cretaceous age. The cliffs face roughly concentrically toward the south and southeast and the strata, with conformably enclosed coal beds, gently dip away from the face of the cliffs and at right angles to their front line. Back of these cliffs the mountain masses rise to an altitude of from 8000 to 10,ooo ft. above sea level. Stretching away from their foot is a great shale plain, on which the towns are situated and over which the railroad lines and highways run. The Castle Gate mines enter the coal beds at their outcrop; the workings extending within a particular coal bed away from the outcrop and under the mountain mass back from the cliff line (Fig. I). Throughout the Mesaverde formation in the Castle Gate general area, there are from two to five workable coal beds. Usually not all of these are coincidentally of workable size and merchantable quality throughout any given large tract. In the Castle Gate mine area, the base of the Mesaverde horizon and coal measures is marked by a massive, cliffmaking, gray sandstone bed 60 to 80 ft. thick. Locally this is referred to as the "Castle Gate sandstone floor." Frank R. Clark, in U. S. Geol. Survey Bull. 793, designates it as the "Aberdeen sandstone." At Castle Gate the various coal beds are designated by the letters A, B, C, etc., commencing with the lowest bed.

Jan 1, 1942

By W. R. Seyfried

THE problem of extracting alumina from clay and low-grade bauxites has been the subject of considerable interest for some time. The basic reason, of course, lies in the fact that known reserves of high-grade bauxite are not inexhaustible and that the present commercial process cannot successfully cope with low-grade bauxites or clay. Ultimately it may be necessary to use these poorer raw materials for all commercial operations. An unprecedented demand for aluminum during the war emergency and the constantly threatened shortage of imported bauxite caused the United States Government to take an active role in this problem. Through the National Academy of Sciences, the War Production Board and the Defense Plant Corporation, it investigated processes and finally selected four to be used in the construction and operation of four experimental plants. Each plant was to be designed in such a way as to facilitate its incorporation into a larger commercial plant should the need arise. The Chemical Construction Corporation process, or "Chemico" ammonium sulphate process as it is better known, was one of the four selected. The extensive literature and patents on record before the war generally follow one of two process-types depending upon the extracting reagent used. One group uses an acid reagent, the other an alkali. The Chemico process uses an acid reagent. For those interested in other processes described in literature, there is a short bibliography at the end of this paper. The basic steps of all acid extraction processes are: (I) to make the aluminum silicates acid soluble, (2) to separate the released alumina from impurities and insoluble gangue, and (3) to recover the reagent for re-use. THE PROCESS AS PLANNED In April 1941, a group of chemists and engineers of the Chemical Construction Corp. became interested in the problem of extracting alumina from clays and low-grade bauxites and, under the leadership of Mr. Blakeslee Barnes, Vice President and General Manager of the Company, first drafted a process in July of that year-five months prior to Pearl Harbor. The work continued in our research laboratories and with a small pilot plant. By June 1943, the work had progressed to a point where it was possible to apply for a patent on the process which was U.S. patent 2,405,426, granted August 6, 1946. Immediately prior to the development of the Salem plant, the process was envisaged to be as follows: I. The first step was to make the aluminum silicates acid soluble. It was planned: (a) Clay or low-grade bauxite would be roasted at 700 to 800°C (1292° to 1472°F), (b) The roasted ore would then be leached with hot aqueous ammonium bisulphate to form a slurry. In this way the

Jan 1, 1947

By A. G. Roach

THIS paper deals with a plant built under joint agreement between the Canadian and United States Governments to supply the strategic mineral, corundum, at a time when African production was dwindling and war demands still increasing. The operation began in September 1944, retreating the tailings from a former mill by gravity methods, and is still in production (Sept. 1946). In 1942, when it became apparent that South African production would be insufficient to meet mounting wartime requirements of corundum, a survey was made of Canadian sources of the mineral, at the request of the Foreign Economic Administration of the U. S. Government. The investigation1 indicated that the quickest and cheapest supply would be obtained by reworking the tailings deposit at Craigmont, Ontario. Sampling of the dump by Canadian Government engineers revealed that 125,000 tons of tailings, averaging 2.96 pct corundum, was available for retreatment. Ore-dressing tests on representative samples of the deposit were conducted by the writer in the laboratories of the Industrial Minerals Section of the Department of Mines and Resources at Ottawa; and gravity concentration on tables was indicated as the most suitable method of treatment. Decision to proceed with the project was deferred until May 9, construction was begun on May 18, and tune-up operation of the plant begun on Sept. 15, 1944. CORUNDUM-ITS PROPERTIES AND USES Corundum is an oxide of aluminum having the formula A1203. Its outstanding characteristic is its great hardness; 9 in the Mohs scale. In this respect it is second only to the diamond. It usually occurs in barrel-shaped crystals in nepheline syenites and other feldspathic rocks deficient in silica. It has a specific gravity of 3.95 to 4.1 and is insoluble and infusible. In color it ranges from white, through red and green, to black. Ruby and sapphire are gem varieties of corundum. Corundum is supplied to industry as closely graded grain.2 The coarser products (10 to 24-mesh) are used largely for snagging wheels in the steel-castings industry, while the finer grades (from 70-mesh down to flours) find a wide application in the polishing of lenses and for other uses in the optical trade. All sizes of corundum grain are in close competition with synthetic abrasives such as carborundum and alundum. In some fields of application the artificial product is superior to the natural grain but not in all. The shape of the particle and its behavior under conditions of actual use determine its sphere of employment. The United States is the largest consumer of corundum, annual consumption in peacetime approaching 3000 tons; during the war this figure was roughly doubled. During the years 1902 to 1913, the bulk

Jan 1, 1946

By A. Gatti

A dispersion of AI2O3 was produced within chromium by the hydrogen reduction of a solid solution of Cr2U3-A1203. The yesulting powder. was compacted, extruded, and the material tested in tension at various temperatures and in creep at 1800°F. The material is ductile above 1200°F and is at least twice as strong as electrolytic chvomium at all temperatures. Its creep resistance, rupture strength, and ductility at 1800°F warrant further work to improve its Low -temperatutre properties. BECAUSE of its high melting point and excellent corrosion resistance, chromium has long been considered as a base for high-temperature alloys. Most chromium base alloys, however, are extremely brittle at low temperatures. Elements such as nickel and iron lower the melting point of chromium and thereby limit its high-temperature usefulness. Chromium-alumina materials made by othersl, 2 have shown good high-temperature creep resistance but poor ductility and thermal shock resistance. Pure ductile chromium3 is weak at high temperatures and reverts to a brittle state if exposed to nitrogenous atmospheres. In sintered aluminum powder (SAP)4 and internally oxidized alloys of silver, copper, and nickel, fine dispersions of oxide phases can control hardness, recrystallization, and yield stress. The possibility of formation of a ductile, high-strength material by precipitating dispersions of alumina in a chromium matrix appears worthy of investigation. MATERIAL Powder Production—Chromium oxide and alumina in amounts to produce a final alloy of Cr + 16 pct AI2O3 by weight were colloid milled, filtered, dried and high fired for 16 hr at 1600°C in air. The resulting solid solution of oxides was ball-milled to a fine powder and the chromium oxide reduced to chromium by heating in pure dry hydrogen for 64 hr at 1400°C. Final Materials Produced by Powder Metallurgy Techniques—-Chromium powder, containing a disper-sion of alumina, was pressed into 1 1/8-in. diam slugs at 25 tons per sq in. and sintered 16 hr at 1400° C in pure dry hydrogen. The sintered slugs were encased in a stainless steel can, 2 in. in diam, and extruded at 1200° C through a 1/2-in. die. The 16 to 1 extrusion ratio produced a final chromium-alumina rod 1/4 in. in diam about 30 in. long. Samples of the rod were plunge-ground to small rupture bars of 0.82-in. gage length with a 0.01-sq-in. cross section. RESULTS Microstructure Studies—Fig. 1 is the microstruc-ture of the material in the as-sintered condition while Fig. 2 is the microstructure of the material as-extruded. Comparison of the as-sintered and as-extruded micrographs show the redistribution and realignment of the alumina inclusions by the extrusion

Jan 1, 1961

By W. R. Seyfried

The problem of extracting alumina from clay and low-grade bauxites has been the subject of considerable interest for some time. The basic reason, of course, lies in the fact that known reserves of high-grade bauxite are not inexhaustible and that the present commercial process cannot successfully cope with low-grade bauxites or clay. Ultimately it may be necessary to use these poorer raw materials for all commercial operations. An unprecedented demand for aluminum during the war emergency and the constantly threatened shortage of imported bauxite caused the United States Government to take an active role in this problem. Through the National Academy of Sciences, the War Production Board and the Defense Plant Corporation, it investigated processes and finally selected four to be used in the construction and operation of four experimental plants. Each plant was to be designed in such a way as to facilitate its incorporation into a larger commercial plant should the need arise. The Chemical Construction Corporation process, or "Chemico" ammonium sulphate process as it is better known, was one of the four selected. The extensive literature and patents on record before the war generally follow one of two process-types depending upon the extracting reagent used. One group uses an acid reagent, the other an alkali. The Chemico process uses an acid reagent. For those interested in other processes described in literature, there is a short bibliography at the end of this paper. The basic steps of all acid extraction processes are: (I) to make the aluminum silicates acid soluble, (2) to separate the released alumina from impurities and insoluble gangue, and (3) to recover the reagent for re-use. The Process as Planned In April 1941, a group of chemists and engineers of the Chemical Construction Corp. became interested in the problem of extracting alumina from clays and low-grade bauxites and, under the leadership of Mr. Blakeslee Barnes, Vice President and General Manager of the company, first drafted a process in July of that year—five months prior to Pearl Harbor. The work continued in our research laboratories and with a small pilot plant. By June 1943, the work had progressed to a point where it was possible to apply for a patent on the process which was U.S. patent 2,405,426, granted August 6, 1946. Immediately prior to the development of the Salem plant, the process was envisaged to be as follows: I. The first step was to make the aluminum silicates acid soluble. It was planned: (a) Clay or lour-grade bauxite would be roasted at 700 to 800°C (1292° to 1472°F). (b) The roasted ore would then be leached with hot aqueous ammonium bi-sulphate to form a slurry. In this way the

Jan 1, 1949

By Earnshaw Cook, H. S. Avery, J. A. Fellows

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By J. A. Fellows, Earnshaw Cook, H. S. Avery

TEe increased use of heat-resistant alloys (26 per cent Cr, 12 per cent Ni; 16 per cent Cr, 35 per cent Ni; 12 per cent Cr, 60 per cent Ni; etc.) in recent years has been accompanied by continued demands by the consumer for improvement in properties. The manufacturers of these materials, of necessity, have resorted to more critical studies of the basic causes of variations in fundamental properties. To keep pace with the need for augmented information, previous techniques of investigation have been refined and new test methods and instruments created. It is the purpose of this paper to describe the apparatus, experimental technique and precision of measurement that were employed in the exploration of properties of heat-resistant alloys presented in a companion paper. The detailed precautions in experimental procedure essential for attainment of accurate and comparable data at elevated temperatures cannot be too highly emphasized. The Creep Test Since the fundamental concepts of creep testing have been recognized for the past 20 years, present interest is restricted to refinements in equipment and experimental procedure. The creep-test iaboratory constructed for the American Brake Shoe and Foundry Co. is designed to permit I000-hr. tests in the temperature range of I200° to 2 200°F. with a choice of applied stress extending from jo to 50,000 lb. per sq. in. in increments of 50 lb. per sq. in. To simplify the calculation of weight combinations, the loading beams (Fig. I) are provided with counterweights to eliminate the tare. The precision of the knife-edges (10:I ratio) is such that a 10-gram weight placed on the upper specimen grip will be exactly balanced by a I-gram weight attached to the loading shackle. Check of the loading weights proved the maximum error to be 0.06 per cent. Axial alignment is provided by crossed knife-edges in the grip seats. The furnaces are similar in design to those of Crane and Company, Battelle Memorial Institute, and the U.S. Steel Corporation. An 80 per cent Pt, zo per cent Rh No. 19 B. and S. gauge wire is used as the heating element. The details of -construction are shown in the radiograph reproduced in Fig. 2. The windings are held in place on an alundum tube with aludum cement; the distribution of turns is adjusted to give a maximum temperature gradient of , I°F. over a 4-in. gauge length (Fig. 3). To avoid sharp temperature differentials at the ends of the test section, the length of the furnace is four times the gauge length. Sixteen-inch coupons are used „ to reduce the temperature of the threaded joints and thus to facilitate removal from the grips. Thermal losses are minimized by refractory insulators cut to shape and surrounded by diatomaceous ear,th. The taps

Jan 1, 1942

By Frank G. Norris, William C. Marshall

The term "total operation" is meant to include problems that cannot be answered from the standpoint of either the blast furnace or the open hearth separately but must be studied by considering the interrelations of these two processes. There are other ways of expressing this idea, such as reference to the blast furnace and the open hearth as an integrated process or by emphasizing the interrelation and interaction of the two processes. Much progress has been made in metallurgy and other fields by breaking complicated processes and reactions into simpler parts and studying each of these intensively. This intensive study frequently is done under the controlled conditions of the laboratory experiment. The entire process is understood better by this specialized study of each of its parts. This procedure is so satisfactory that an understanding of unit operations is a fundamental requirement of chemical engineering. Much discussion of the open-hearth process is in terms of one heat or one furnace. By this is meant that the conclusions apply to one furnace, wherever it may be. Furnaces seldom occur singly; they are located in groups and these groups are located in steel plants having characteristic blast-furnace equipment. Problems that are affected by the number of furnaces operating, by the number of blast furnaces in the plant and by the fact that the open- hearth shop is dependent on the bla furnace capacity rather than on its o needs for the amount of iron available among those which, in contrast to "u operations," we have chosen to call "to operations." Many of these problems, such as cha ing delays and the general mechani problem of material handling, are familiar that merely to define " total op ations" brings them to mind. These pr lems are of such importance that alrea they have received careful thought 2 study and probably will merit furt study. As will be shown later, these mechan problems are so intimately related metallurgical problems of total operati that the effect of certain changes cannot ascribed with certainty to either a mech ical or a metallurgical cause entirely. Although the problems coming under general term of "railroading" are inclu in the problems of total operations, &apos; others are selected for the discussion of paper, One of these is strictly a problem composition; the other is strictly a prob of tonnage production. The problem of phosphorus is pres whenever basic open-hearth slag is used the blast-furnace burden. This practice not secured universal acceptance chi because of difference in preference for h manganese or low-manganese pig iron hjgh-manganese (2.00 per cent) iron is to made, open-hearth slag as a source manganese is usually cheaper than m

Jan 1, 1943