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By Rossiter W. Raymond

The lead-mining industry of Missouri, as of other parts of the Mississippi basin, appears to have been paralyzed by the shock of competition with the mines of the States and Territories further west. It is difficult for establishments working galena ores, too poor in silver to pay for extracting it, to compete with the producers of the argentiferous carbonates of Utah and Colorado, who look upon their lead as a by-product of little value, and are satisfied if it pays the charges of transportation, or the loss in smelting for silver. But simultaneously with this depression in the lead-mining of the Mississippi States, the development of new zinc deposits has caused a notable revival in the mining of zinc ores. There has recently been a sndden and strong rise in the price of' spelter, which, though probably to a large extent temporary in character, has given important encouragement to prospectors and miners. Apart from the general recovery of business in the United States from the prostration of the past six years, the cause of the advance in spelter has been the falling off in production, resulting from the shutting clown of several leading Western works,—the Martindale and Carondelet works, at St. Louis, and the Consolidated Company in Kansas. At the same time, the principal works at La Salle, Ill., were undergoing repairs, and produced less than usual, while the sheet-mill of Matthieson & Hegeler, at that place, was running as usual; so that this concern, ordinarily a large producer, entered the already depleted market as a buyer. These causes are in their nature transitory, and it is quite likely that spelter will be superabundant in a few months. Having lately received from a well-informed Missouri correspondent some samples of the zinc ores and a general account of the ore deposits of Southwest Missouri, I have thought that it might interest the Institute to examine these specimens, and to hear such brief statements concerning the region as I am able, upon good authority, though without the aid of any personal investigation 011 the spot, to give. The zinc-bearing territory in Southwest Missouri appears to be very extensive; that is to sap, zinc ores have been mined during the last year at various points throughout a district extending from the eastern edge of Kansas, west of Joplin, to a line some 50 miles east

Jan 1, 1880

By Rossiter W. Raymond

THE lead-mining industry of Missouri, as of other parts of the Mississippi basin, appears to have been paralyzed by the shock of competition with the mines of the States and Territories further west. It is difficult for establishments working galena ores, too poor in silver to pay for extracting it, to compete with the producers of the argentiferous carbonates of Utah and Colorado, who look upon their lead as a byproduct of little value, and are satisfied if it pays the charges of transportation, or the loss in smelting for silver. But simultaneously with this depression in the lead-mining of the Mississippi States, the development of new zinc deposits has caused a notable revival in the mining of zinc ores. There has recently been a sudden and strong rise in the price of spelter, which, though probably to a large extent temporary in character, has given important encouragement to prospectors and miners. Apart from the general recovery of business in the United States from the prostration of the past six years, the cause of the advance in spelter has been the falling off in production, resulting from the shutting down of several leading Western works,-the Martindale and Carondelet works, at St. Louis, and the Consolidated Company in Kansas. At the same time, the principal works at La Salle, Ill., were undergoing repairs, and produced less than usual, while the sheet-mill of Matthieson & Hegeler, at that place, was running as usual; so that this concern, ordinarily a large producer, entered the already depleted market as a buyer. These causes are in their nature transitory, and it is quite likely that spelter will be superabundant in a few months. Having lately received from a well-informed Missouri corres¬pondent some samples of the zinc ores and a general account of the ore deposits of Southwest Missouri, I have thought that it might interest the Institute to examine these specimens, and to hear such brief statements concerning the region as I am able, upon good authority, though without the aid of any personal investigation on the spot, to give. The zinc-bearing territory in Southwest Missouri appears to be very extensive; that is to say, zinc ores have been mined during the last year at various points throughout a district extending from the eastern edge of Kansas, west of Joplin, to a line some 50 miles east

Jan 1, 1880

J. A. Mathews,* Syracuse, N. Y. (written discussion?).-It is interesting to note how frequently we hear of some process that is going to revolutionize the tool-steel business. I don't know why it is, but every one seems to have it in for us poor tool-steel men. About 15 years ago, a good-sized plant was built in Syracuse for the manufacture of cast tools of malleable iron. The promoter of the scheme claimed to have a secret, process that had been given to him by a tramp to whom he gave a lift along a dusty road. The widows and orphans invested liberally in the securities of the company without consulting the men established in the machine-tool business in Syracuse. About two years later, when the sheriff's sale occurred, the secret, which was carried on the books of the company as an asset valued at $2,000,000, brought $15 at auction. A little later another concern started on the theory of replacing scrap high-speed steel with new high-speed steel tools made therefrom. All the tool-steel companies have made a practice of purchasing high-speed

Jan 5, 1919

CONTENTS PAGE SOUTHWARD, GLENN B.-Coal Mining by the V System. Discussed by Glenn B. Southward, Howard N. Eavenson, Edward B. Raiguel, Thomas de Venny, J.. J. Rutledge, Graham Bright 1 ARMS, RAY W.-Dry Cleaning of Coal. Discussed by Ray W. Arms, S. A. Taylor, Howard N. Eavenson, W. R. Crane, F. F. Jorgenson, G. R. Delamater. 6 EAVENSON, HOWARD N.-Data About Labor Employed in Various Bituminous Coal Mines. Discussed by Howard N. Eavenson, George H. Ashley, E. A. Holbrook, S. A. Taylor, R. V. Norris 14 Coal Mining by the V System Discussion of the paper of GLENN B. SOUTHWARD presented at the New York Meeting, February, 1924, and issued as Paper No. 1300-C, with MINING AND METALLURGY, February, 1924. MEMBER.-How do you pay your men for loading? GLENN B. SOUTHWARD.-Everything is on time basis. MEMBER.-How many men do you have loading across one of the diagonal faces? GLENN B. SOUTHWARD.-From four to five, depending on the length of the face. Our loaders are so arranged that each will give about twenty-five tons per loader a day. MEMBER.-How much timber do you use? GLENN B. SOUTHWARD.-A little more than will be used in room-and-pillar work, but not a great deal more. We have not attempted to recover much of our timber. MEMBER.-IS the mine union or non-union? GLENN B. SOUTHWARD.-Non-union. HOWARD N. EAVENSON, Pittsburgh, Pa.-I went .through that mine some weeks ago, and think that the author has been very conservative in his statements about the amount of loadings, etc. EDWARD B. RAIGUEL, Huntington, W. Va. (written discussion).¬Page 7 shows 60 men employed in day and night shifts, inside the mine, producing 750 tons per day. Let us reduce these figures to a man-hour basis, for comparison with Mr. Eavenson's figures on West Virginia mines, as follows:

Jan 6, 1924

This brief resume of the events transpiring in Mexico, culled from the daily New York newspapers since the last Bulletin went to press, does not show any degree of improvement in the situation. MEXICO SEEKS TO AVOID BLAME FOR BANDIT RAIDS All foreign passengers leaving Nogales for Mexico on the Southern Pacific or Mexico Railroad. whose business would take them through territory occupied by the Yaqui Indians or Mexican bandits were requested by Mexican Consul Emilio Tamez to sign a statement that they relieve the Mexican government of responsi-bility for anything which might happen to them while in that part of Mexico. The Mexican consul stated, says the N. Y. Tribune, that this was by order of Mexican Ambassador Ignacio Bon ill as, at Washington. When the State Department was advised of this activity Secretary Phillips, in a message to the consulate at Tampico, according to the N. Y. Tribune, asserted that "compliance with the waiver requirement will not interfere with the relation existing between the United States and its citizens and that Americans so complying will in no way lose the protection of this government."

Jan 11, 1919

By R. P. King

The two-phase distributed-parameter kinetic model for flotation has been wed as the basis for a digital simulation of flotation plants of arbitrary configuration. Ores that contain any number of minerals can be handled. The effects of incomplete liberation and particle-size distribution are specifically allowed for. The simulator allows the investigation of variations in throughput and in the slurry density of the feed, and of variations in stage volumes and aeration rates. It can handle cell behavior even under conditions of hindered flotation. The requirements for data preparation are completely documented so that the computer program is suitable for general-purpose use. The program is written in Fortran. The output from the simulator consists of the complete material flows in the plant, as well as the grade, recovery, and particle-size distribution in each stream.

Jan 1, 1976

By C. S. Finney, John Mitchell

There is no field of human thought or endeavor which does not owe much to the past. Yet, surrounded by the prodigious scientific and technological achievements of our day, it is all too easy to forget the extent to which we have stood on the shoulders of giants. The coking industry of the United States is now a little more than one hundred years old. As with the American nation itself, the earliest beginnings of the industry owe a great deal to British influences, and its development owes much to those influences of continental Europe. No serious contribution to the history of coking in the United States can be written, therefore, which does not mention the work of the pioneers of the Old World. It is believed that the use of metallurgical coke dates back to antiquity. The fact that certain coals would soften under the influence of heat to yield a porous solid was known to the ancients of China and India, where a very crude coking operation was carried out by simply setting fire to piles of coal. After active combustion had started, turf or wet straw was used to seal off the pile. The coke obtained was used to forge iron and steel implements and weapons. Perhaps the earliest reference to the coking phenomenon is to be found in the writings of Theophrastus, pupil of Aristotle. In his History of Stones, which was written in or about the year 371 B.C., there appears the following observation. "But the Lipara stone empties itself, as it were, in burning and becomes like the pumice, changing at once both its colour and density; for before burning it is black, smooth and compact.... Certain stones there are about Tetras, in Sicily, which is over against Lipara, which empty themselves in the same manner in the fire." The first comparatively modern reference to coke is to be found in a recommendation for carbonization made in 1584 by Julius, Duke of Braunschweig-Luneberg, owner of the Hohenbuchen mine in the Harz district of Germany. In 1587, Sir Francis Willoughby of. Wollaton, England wrote: "There are twenty rooks broughte into charcoal and laid up in store." A rook of coal was equivalent to some 25 tons, and the coking would probably have been carried out in a manner similar, to that used for the production of charcoal. In 1589, Thomas Proctor attempted to carbonize coal, and in the year 1590 an English patent was granted to John Thornborough, Dean of York, in order that he might "purify pit coal and free it of its offensive smell". Sir Robert Cecil (1595), Robert Chantrell (1607), Simon Sturtevant (1611) and John Rovenzon (1613) were all granted patents for the use of coal or coke

Jan 1, 1961

By A. C. Fieldner, W. A. Selvig

For purposes of coal classification it is desirable to know the composition and calorific value of the pure coal substance; that is, of the coal free from its ash-forming minerals. Two methods suggest themselves: (1) To free the coal from most of the ash-forming material previous to the analysis; and (2) to analyze the coal as received and calculate the analysis, with certain more or less arbitrary corrections, to the pure-coal basis. Calculation methods are obviously more apt to give correct results with low-ash than high-ash coals. With coals of unusually high ash it would appear preferable to remove, previous to the analysis, as much of the inorganic matter as possible, by float-and-sink or acid-treating methods. Effect of Ignition on Inorganic Constituents of Coal The need of corrections in calculating analysis to the pure-coal basis is due to the fact that the ash, as determined by ignition, is not the same, in either weight or composition, as the inorganic mineral matter in the coal. On ignition a number of changes occur in the coal such as loss of water of hydration of the shaly material, conversion of pyrite (FeS2) to ferric oxide (Fe203) with evolution of the sulfur as sulfur dioxide or possible fixation of more or less of the sulfur in the ash as calcium sulfate (CaSO4), and decomposition of calcite (CaC03) to calcium oxide (CaO). The amount of sulfur from pyrite which remains in the ash as calcium sulfate depends on the amount of calcite and pyrite in the coal. Certain coals high in both calcite and pyrite show relatively large amounts of sulfate sulfur in the coal ash. The determination of total carbon and hydrogen in coal includes, besides the organic carbon and hydrogen, the carbon of inorganic carbonates such as calcite, and the hydrogen of the water of composition of some of the ash-forming minerals. For detailed discussion of corrections proposed for calculations of coal analyses to the " pure "

Jan 1, 1930

By J. M. Gaines, C. H. Herty

IRon oxide (FeO) plays an extremely important part in the manufacture of steel. In the open-hearth furnace and the Bessemer converter it is the chemically predominant compound and controls to a large extent both the operation of the furnaces and the composition and quality of their products. Almost all of the refining action is carried out through the medium of FeO, which oxidizes carbon, manganese, silicon and phosphorus. At the end of any open-hearth or Bessemer heat the steel contains dissolved iron oxide, which must be wholly or partly eliminated. The type of deoxidation product depends on the amount of dissolved iron oxide and on the deoxidizer used. After the heat has been deoxidized and while it is being teemed, iron oxide diffuses from the ladle slag into the metal, causing losses of deoxidizer and increase in iron oxide content of the steel. It is generally believed that non-metallic inclusions are responsible for a great many failures of steel in service and for decreased yield of steel during rolling. The basis of most non-metallic inclusions is dissolved iron oxide. This investigation was undertaken in order to determine the amount of iron oxide that will dissolve in iron under various conditions. Steel-making slags are complex and it has been thought best to determine solubility under simple slags as a first step. The study is being continued under slags whose compositions approach those of operating slags Previous Investigations The solubility of oxygen in iron has been determined by a number of investigators (see Table 1) but their effort's have been directed toward the

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By R. E. Delavault, H. V. Warren

In normal soils there are usually 10 to 50 parts of copper in every million parts of .soil. Only 0.2 to .5 pct of this copper can be found by any simple cold chemical attack. Now, with rubeanic mid reagent paper, a prospector or field geologist can detect as little us 4 ppm of readily available copper ill soil. This degree, of sensiticity is enough to determine the presence. of copper anamalous an as and, ecentually, to discouer copper mineralization. Circumstances determine whether it is better to make analyses in the field or in a permanent laboratory. The rubeanic acid test described in this article has been designed primarily for field use: it is simple and virtually foolproof, and it requires a minimum of field kit." It is sensitive, easily de- • Ed. Note: Persons Interested in purchasing kits suitable for rubeanic acid prospecting can obtain information by writing Eldrico Geophysical Sales Ltd., 633 Hornby Street. Vancouver 1, B.C. The University of British Columbia does not produce these kits for sale and has no financial interest in their production tecting 4 ppm of readily extractable copper in a soil. This is by no means a quantitative test, but it is accurate enough to provide a valuable indicator of copper anomalous areas for both prospectors and field geologists. The easiest method for detecting metal deposits that do not produce visible float or stains is to make a simple chemical test for the metal in overlying soil, or in the silt of a stream that may have picked up metal farther upstream. In Brief: Testing for copper may be done easily by shaking a soil sample with strong acetic solution in a small test tube and pouring the mud into a small filter, the tip of which rests upon a strip of reagent paper impregnated with rubeanic acid (di-thio-oxamide). When copper is present—and only when it is—a blue spot develops. The more copper, the darker the spot. If the copper content is merely the small amount present everywhere, there is a pale blue or hardly visible spot; if it is abnormally high, the spot will be dark. There are, of course, intermediate cases where the experienced geochemist cannot tell offhand whether a medium-strength spot represents rich agricultural soil, weak copper mineralization, or distant rich copper mineralization. Reagents and material are inexpensive; the test may be readily done on the spot with a simple kit easy to pack and handle. Anyone interested in general problems of soil sampling as applied to prospecting may refer to an article recently presented to the AIME. In exploration work it is the contrast between the metal content of anomalous and background areas that is important; absolute values become of greater interest when an anomalous area is being investigated in detail. With specific reference to copper, it has been the authors' experience that the amounts of metal extracted from anomalous and normal soils with buffer solutions of decreasing pH show better contrast if an acid reagent is used. This contrast tends to increase with increasing acidity until 3 to 4 pH is reached. Using a short cold attack on unheated soil, it has been found that further increases in acidity do not produce better results, and only increase the hazards involved in carrying strong acids. An acidity of about pH 4 is satisfactory for direct determination of copper by dithizone. But dithizone itself introduces some problems: it must be made up fresh at frequent intervals, and with some soils, notably those with much ferric iron, oxidation mag take place before all the copper has reacted with the dithizone. Rubeanic acid keeps its strength unimpaired for long periods, is unaffected by oxidation, and is practically specific for copper at pH 4. Consequently it seems an ideal reagent to use in prospecting for copper. History and Background: Rubeanic acid (systematic name: dithio-oxamide (SC-NH2) has long been known as a spot test reagent for some heavy metals with which it gives a number of compounds. Only copper and some metals of the platinum family are believed capable of providing any ru-beanate compounds under conditions of moderate

Jan 1, 1959

By C. A. Stickels

A heat of electrolytic iron, to whzch alunzinutn and nitrogen had been added, was hot-rolled, cold-rolled 90 pct, and recrystallized at temperatures from 500" to 700°C. Primary recrystallization textures appear to arise from competitive growth of two types of nuclei: 1) those having orientations belonging to the "usual" primary recrystallization texture found in riming steel, and 2) those with the {111} (110) ovientation. Development of a (111}(1 10) component in the primary recrystallization texture occurs only over a certain interval of isothermal recrystallizatzon temperatures when the material is supersaturated with respect to the precipitation of AlN. Lowering the degree of supersaturation depresses the temperature interval in which a (111)(110) component occurs. An elongated, 'pancake-shaped" recrystallized pain structure and a marked delay in the start of recrystallization were found in all specimens which were supersaturated with respect to A1N precipitation after cold work, regardless of their recrystallization texture. ONE of the consequences of killing low-carbon steel with aluminum is a significant change in recrystallization behavior. About 15 years ago, Solter and eatttiel showed that this behavior was largely controlled by aluminum and nitrogen in the steel. If complete precipitation of A1N was prevented before cold rolling, an increased "recrystallization temperature" was observed in subsequent. annealing, and the recrystal-lized grains were not equiaxed. Leslie et a1.2 studied this phenomenon in some detail and clearly demonstrated the relationship between A1N precipitation, recrystallization kinetics, and the development of "pancake-shaped" grains. It has also been known for some time that aluminum-killed steels, processed to produce elongated "pancake" grains, develop a (11 I}( 110) primary recrystallization texture. This texture has not been found in iron or low-carbon rimming steel as a primary texture4j5 but has been observed following grain growth in electrolytic iron.5 The present work was undertaken to study in more detail the effect of A1N supersaturation on recrystallization textures in iron. LITERATURE REVIEW The deformation texture in heavily rolled iron has been studied in detail by Bennewitz.~ The texture consists primarily of a partial fiber texture about a (110) axis in the rolling direction, designated here as fiber texture A. It includes the range of orienta- tions (111)[110] - (001)[ 110] - (11l)[110]. A weak secondary texture also is present.6 This is a duplex partial fiber texture about two (110) fiber axes located 60 deg from the rolling direction and 30 deg from the sheet normal. The range of this texture, designated here as fiber texture B, about the [101} fiber axis is (112)[110] - near (545)[252] - (211:1[011] *The range given here follows Bennewit~.~ A few pole figures from re-crystallized material indicate a broader range than this.' However, the components which are strongest in the recrystallization texture are in this range.'________________________________________________________ Primary recrystallization textures in unkilled steels can be accounted for by growth of members of fiber texture B present in the deformed metal.5 However, while members of fiber texture B dominate the primary texture, other orientations survive primary recrystallization as well. In particular, some {111}(110) members of fiber texture A must also grow during primary recrystallization, because a well-defined {1ll)( 110) texture develops during subsequent grain growth at 700°C.5 The unusual recrystallization behavior of deformed supersaturated solid solutions has been attributed to: 1) retention of the solute in solution,' 2) formation of coherent, preprecipitation solute clusters prior to and during re~r~stallization,~ and 3) formation of a precipitate prior to and concurrent with recrystallization.'~-'~ When aluminum is supersaturated with iron, the difference in grain boundary mobility between general high-angle boundaries and certain special coincidence site boundaries is apparently eliminated.' In aluminum-killed steels, precipitation of A1N can take place at ordinary subcritical recrystallization temperatures. The rate of precipitation increases with increasing aluminum or nitrogen contents.2'13 There is some doubt, however, as to whether true precipitates form during the time at temperature needed to complete recrystallization. Leslie ef a1.2 found that precipitation in one steel was complete after about 100 min at 700GC, or after about 1000 min at 650GC, as measured by chemical analysis for AlN. Aoki et a1.,13 using internal friction for dissolved nitrogen, showed that a large fraction of the dissolved nitrogen was removed from solution within a few minutes annealing time at temperatures from 400" to 800°C. However , the rate of formation of AlN, as detected bv chemical analvsis. was much slower than the apparent rate of nitrogen removal. Hasebe,'~~ using carbon extraction replicas, has identified A1N precipitates by electron diffraction in a 0.2 C steel, solution-treated at 1300°C and annealed 2 hr at 700°C. Borchers and kim,I6 also using a replication technique, observed precipitates after annealing treatments as short as 2 min at 640°C. However, Leslie et a1.' state that no A1N precipitate can be seen while recrystallization is being inhibited in aluminum-killed steel.

Jan 1, 1967

By J. P. Morris

PREVIOUS investigations1,2 have shown that alloying elements in liquid iron influence the thermodynamic activity of sulphur and thereby affect the partition of sulphur between metal and slag in the desulphurization process. For example, the greater efficiency of desulphurization in the blast furnace as compared to the open hearth can be attributed in part to a higher level of sulphur activity in blast-furnace metal due to the higher concentration of carbon and silicon. In the present investigation, a short study was made of the influence of manganese on the activity of sulphur in liquid iron and iron-carbon alloys. In contrast to carbon and silicon, manganese was found to decrease the activity coefficient of sulphur; and in iron-carbon alloys it counteracts to some extent the influence of carbon. However, at manganese concentrations normally present in the blast furnace or open hearth, the effect of manganese is small. Since manganese sulphide has a limited solubility in iron, manganese can act, under certain conditions as a desulphurizing agent. Considerable data on the manganese-sulphur product in carbon-saturated melts were obtained in the investigation and have been included in this report. The experimental procedure was the same as that used in the earlier investigations on the effect of silicon' and carbon' on sulphur activity. Briefly, the method was as follows: The molten alloy, contained in a graphite or sintered alumina crucible, was brought to equilibrium at a constant temperature with a mixture of hydrogen and hydrogen sulphide of constant composition by bubbling the gas through the metal. Samples of' the melt were taken for analysis at regular intervals by suction through a 2 to 3 mm bore silica tube dipped into the metal. The experiments were run in a graphite spiral resistance furnace with melts weighing 50 to 60 g. The gas bubbling tubes were made of sintered alumina and were 5/16 in. OD, 1/16 in. ID, and 24 in. long. Equilibrium was assumed to have been attained when the sulphur content of the liquid metal reached a constant value. During an experiment there was a rapid loss of manganese from the melt by volatilization. To offset this loss, small additions of manganese were made periodically. The rate of manganese addition needed to maintain a constant manganese concentration was determined in preliminary tests. In all of the experiments, deposits of manganese sulphide formed above the melts in a cooler region of the furnace. Apparently, these deposits resulted from a reaction between manganese vapor and hydrogen sulphide in the gas. To prove that manganese sulphide did not volatilize from the melts to a measurable extent, an experiment was run in which helium was bubbled through liquid iron containing both manganese and sulphur. Although manganese volatilized rapidly in this test, there was no appreciable loss of sulphur. Volatilization of manganese sulphide from a melt would have led to an apparent equilibrium condition in which the sulphur content of the metal was lower than the true equilibrium value. The experimental results are shown in the first seven columns of Table I. The data in the last two columns were obtained from the previous work on the effect of carbon' and show what the results would have been in the absence of manganese but with temperature, gas composition, and carbon content of the metal remaining the same. Comparison of the last four columns show that, in the presence of manganese, the sulphur content of the metal increased at equilibrium and the activity coefficient of sulphur decreased. However, the results show that, for manganese concentrations below 3 pct, the effect of manganese is small. The values for activity coefficient of sulphur given in Table I were calculated from the following relations: S (in liquid metal) + H2 (gas) = H2S (gas) [l] K ph2s/?s X %S X phg = 0.00251 [2] where K is the equilibrium constant for the reaction, PH2S and ph2 are the partial pressures of hydrogen sulphide and hydrogen, respectively, and ?s is the activity coefficient of sulphur. The standard state for sulphur was taken to be a 1 pct solution of sulphur in pure iron. The numerical value for K at 1600°C was determined in the earlier work. For the purpose of showing graphically the results of the tests run at 1600°C, the activity coefficients of sulphur were recalculated so as to correspond to a manganese concentration in the metal of 2 pct in each case. In the calculation it was assumed that the increase in sulphur content of the metal at equilibrium caused by the presence of manganese

Jan 1, 1953

By Allen D. Gorrison

EFFORT to develop fundamental quantitative information and improved technique in the production of petroleum has long been faced with difficulties of a particularly evasive nature, owing to a combination of circumstances. In the first place, petroleum comes from far below the ground, out of sight, so that information derived from indirect observations must be extrapolated to reservoir conditions. If one does not force the analogy too far, the petroleum engineer may be said to be somewhat in the position of the astronomer. The actual phenomena which he wishes to observe in detail appear at a place so deep in the earth?s crust that personal observations and direct experiments are impossible.

Jan 1, 1942

By James Douglas

American metallurgical inventions have not always been absolute metallurgical improvements, if accurate work be the standard of comparison; but when we review the new methods and machinery which have been generally accepted, we find that some have become essential to the metallurgist the world over, while all are so admirably adapted to the peculiar requirements of our local conditions that they have entirely supplanted foreign processes and appliances. The necessity of diminishing to the utmost the employment of labor (owing to its great cost), and the inexorable requirements of our modern joint-stock corporate system, which demands that large quantities be worked up in order to secure large returns, regardless betimes of waste, have been the impelling motives to invention, and indicate the special directions in which originality has been exercised. As might be anticipated, the West has been the most fertile field of inventions by miners and metallurgists, by reason of its great and varied mineral wealth, locked up in ores sometimes lean and often of intricate composition, which must be profitably handled, at a great distance from fuel and from building-materials, by workmen who are paid wages very much higher than those received by their fellow-workmen of like craft in Europe, and in some localities twice as high as those paid for like services even in the eastern States. Moreover, paradoxical as it may seem, the technical inexperience of many of those engaged in mining and metallurgy has helped rather than hindered the progress of invention; fop while there may have been ignorance, there has been radical freedom from

Jan 1, 1894

By John W. Weeton, Max Quatinetz, Robert J. Schafer

Nickel powders of 1-, 0.4-, and 0.2- average particle size were combined with 0.05- p MgO powder. Oxide was added in quantities of 4, 12, and 20 vol pct. The mixtures were vacuum hot pressed and extruded at 2100°F. In spite of a general tendency to growth of oxide particles during processing, dispersions of fineness comparable to those of Sintered Aluminum Powder, SAP, were achieved. A small amount of oxide considerably improved 1800°F stress-rupture strength, but further oxide addition resulted in a decrease of strength. RECENTLY there has been much speculation concerning the requisites for strong and stable dispersion-strengthened alloys. The nature of the dispersed phase, the stability of the alloys, and variables influencing the mechanical properties of alloys have been given consideration. Such topics have been reviewed by Bunshah and Goetzel. Of the many parameters related to the mechanical properties of dispersion alloys, mean free path between dispersed particles (a measure of the fineness of the dispersion), particle size, and vol pct of the dispersed phase have been shown to be very important. Generally, strength increases with decreasing mean free path, and there is an optimum vol pct of dispersed phase. Just how fine a dispersion ought to be is somewhat open to debate, but Irmann, Lenel, Backensto, and Rose, Gregory and Grant,4 and others have shown in the original SAP-type alloys, aluminum plus aluminum oxide alloys, that better strength is generally obtained with finer dispersions and the best strengths were obtained when the mean free path was less than . Further, Cremens, and rant' showed that in nickel plus aluminum oxide alloys, stress-rupture strength at 1500°F was definitely increasing with decreasing mean free path. In their investigation, however, the finest dispersions that were produced were about 2.0 mean free path. To determine the potential of the nickel plus oxide type of product, it would be neces- sary to obtain dispersions analogous to those of SAP alloys; namely, ones where the mean free path between oxides is less than . Unfortunately, however, it is very difficult to produce extremely fine dispersions of oxides in metals other than those which naturally form refractory oxide skins. There are several approaches to this problem including such procedures as mechanical mixing, internal oxidation, reduction of mixed oxides, and metal deposition from solution. Work at the Lewis Research Center has shown that metal powders 0.1p or finer could be produced by ball milling, when selected grinding aids were utilized.' Because these unusually fine powders were available, it was an initial objective of this study to determine if by mixing of these fine Ni powders with various amounts of MgO (0.05) a fine dispersion of MgO in Ni comparable to those in Al-Al203 might be achieved. A second objective was then to attempt to relate the parameters of structure to 1800°F stress-rupture strength of the alloys. Nickel powders of 1-, 0.4-, and 0.2-p average particle size were combined with 0.05- average particle size MgO powder. This oxide was added in quantities of 4, 12, and 20 vol pct. The mixtures were hot pressed and extruded at 2100°F.

Jan 1, 1962

By J. J. Demo

The effect of aluminum additions on the coating vale and corrosion resistance of Cr-Fe diffusiou coalings on a mild steel substvate has been studied. Aluminum additions up to 2 wt pct increase the chromium penetration rate while further additions retard it. The apparent cor$lict between these data and metallogyapkic ineasurements, which show a continuially increasing coaling thickness with aluminum addition, is discrissed. Compavisorz of corrosion resistance on the basis of equal thickness of tlre entire coating measured mnetal- ALTHOUGH ferrous metal articles are cheap and widely used, they are often quickly degraded by corrosion. To prevent or slow down the corrosion process, lographically is misleading; equal thickness of the cor-rosion-resistant portion of the coating is a bette.v basis of conzpavison. Inter difision coefFicients for Cr-Al-Fe coatings of different aluminum content have been detevmined and found to dary logarithmically when plotted againnst chromium concentvation. A general method of calculating diffusion profiles for different lrealment limes and surfuce coucentralions IS described. many types of coating are applied to steel.' Among these are diffusion coatings, formed by high-temperature diffusion of selected elements into the surface, which then becomes the coating Diffusion coatings are metallurgically bonded to the substrate and show a continuously varying concentration gradient from surface to substrate. Generally, these coatings have the advantage of adhering to the substrate upon deformation of the composite. Moreover, when chromium is one of the diffusion elements, a mild steel substrate

Jan 1, 1968

By B. M. Bird

ONE of the problems studied by the U. S. Bureau of Mines in cooperation with the University of Washington has been the re-treatment of table middlings. Hydraulic classification has given the best results. Instead of using the classifier to prepare the feed to the tables, as has been the practise for many years in ore dressing, it is used to separate part of a middling product that cannot be re-treated successfully on the table. Middlings are desirable in a table plant because the separation according to specific gravity is incomplete; that is, in the products of the table there is always an overlapping of free particles of coal and refuse that can be distinguished with heavy liquids such as are used in the float-and-sink test. The causes of this overlapping may be divided into two groups, those outside the table separation itself and those inherent in the table separation. The first of these groups includes, among other causes, the following: (1) poor adjustments of the table, (2) overloading or underloading the table, (3) irregularities in the quantity and quality of the feed, (4) irregularities in the power and water supply, and (5) a vertical danc-ing motion of the table deck due to weak foundations. These causes of overlapping are largely unnecessary in a properly designed and constructed plant; but whenever they are present they materially affect the character of the middling product, and hence the problem of re-treatment. The other group includes three additional causes: (6) small differences in specific gravity between coal and impurities, (7) a size-specific-gravity relationship of the coal and refuse particles in the table feed such that the sizing action of the table opposes the separation according to the specific gravity, and (8) shapes of particles that prevent a separation. The sixth, small differences in specific gravity, may be a very important reason for an incomplete separation. The change in specific gravity from coal to shale is always gradual and the designation of one part as coal and another part as refuse is arbitrary. If some specific gravity, such as 1.45, is chosen as the dividing point between washed coal and refuse,

Jan 1, 1928

By H. Kahata, I. Iwasaki, Y. Takahasi

A combined process of segregation roasting-flota-tion or magnetic separation was developed to recover nickel from lateritic iron ores and oxidized nickel ores. An ore was mixed with a halide, such as sodium or calcium chloride, and a solid reductant, and roasted, whereby the nickel content was segregated out as discrete metallic particles. Either by magnetic separation, or by flotation using a sulfhydryl collector together with a heavy metal salt as an activator, the metallic nickel could be concentrated, Effects of such variables as the types and amounts of the halide and solid reductant addition and of the roasting conditions were extensively investigated. The concentration results on several types of ores from Japan, the Philippines, and New Caledonia are presented. Laterite is a residual product of rock decay in tropical and subtropical regions, and consists mainly of hydrated oxides of iron and alumina. Those derived from serpentine sometimes become enriched in nickel, cobalt, and chromium contents. Oxidized nickel ores are of the similar origin, but their nickel as well as silica contents are higher due to gamierite-type silicates. Apparently, nickel enrichment is more pronounced in the transition region between the surface layer of iron laterite and the underlying serpentine. Iron laterites often contain over 50% iron, and their reserve is reported to exceed 22 billion tons, corresponding approximately to 20% of the world iron ore reserve.1 It is readily apparent, therefore, why the iron laterites have attracted much attention of the steel industry as a potential source of iron ores. Numerous attempts to remove nickel and chromium as byproducts, have been reported in literature.' Worldwide discoveries of high-grade iron ore deposits in recent years have inevitably lessened the interests in iron laterites. However, in view of the tremendous potential for their gross value and supplies of nickel, cobalt, chromium, and alumina along with iron, the problem remains as a challenge. Much of the chromium in laterites is present in the form of relatively coarse particles of chromite, and various classification methods have successfully been applied for its removal.2,3 The nickel, however, is intimately associated with limonite, and ordinary concentration techniques are totally ineffective. Much attention has, therefore, been given to hydro-metallurgical or pyrometallurgical means. Yet, all the known processes appear to have limitations either economically or for the use of products as iron raw materials due to a high residual content of nickel. Some attempts have been made to pre-roast laterites or oxidized nickel ores, particularly with sulfidizing agents, and to remove nickel either by magnetic separation,' or by flotation.4 It is apparent that any such concentration process would require grain growth of nickel during roasting for effective separation. Oxidized copper ores are reported to be concentrated by the segregation roasting-flotation process,5 in which the ores are roasted with a chloridizing agent and a carbonaceous reductant in order to promote the growth of metallic copper through repeated cycles of copper chloride volatilization and its reduction on the solid reductant surfaces. Examination of a vapor pressure-temperature diagram of various metal chlorides indicates that a separation of nickel from iron may be effected by a similar process. In fact, the segregation roasting of laterites was reported to increase the extraction of nickel by the ammonia leach process, as compared to the ordinary reduction roasting.6 In the present article some of the preliminary experimental results of the segregation roasting, followed by either flotation or magnetic separation, on laterites and oxidized nickel ores are reported. The effects of various parameters in the roasting as well as in the concentration steps are discussed. MATERIALS AND METHODS An oxidized nickel ore from Thio, New Caledonia, and three laterites from Homonhon, the Philippines, Wakasa and Miyagawa, Japan, were selected for the

Jan 1, 1967