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By John C. Machisak

Employment and related injury experience of the coking industry in the United States for 1957 contained in this publication is summarized under three general sections: (A) General injury experience: Tables 1 to 9: Current and comparable statistics on operating data, number, frequency, and degree of severity of injuries and major accident agencies involved in the cause of Injuries. Data are presented for the industry as a whole, for each type of oven, and for the States in which coke was produced.

Jan 1, 1959

By L. A. Roe

Magnetic separation of iron ores is one of the fastest-growing segments of the minerals beneficiation industry. The tonnage of taconite ores processed annually by magnetic separation will, in a few years, reach 100 million. Magnetic separation occupies an attractive position in the field of ore beneficiation. It is a simple yet effective method, used for some 150 years and steadily growing more important. This type of beneficiation orginated in 1792, when William Ful-larton was issued a British patent covering the separation of iron ore by magnetic attraction. What is magnetism, and why are some materials capable of being magnetized and others not The study involves many unknowns, and even a partial answer to these questions would be a dissertation in solid state physics and perhaps other fields of science. But the last two decades have revealed basic facts as to why certain materials are magnetic and what happens to them when they are magnetized. Some of the newer studies in solid state physics have developed a theory that can be applied to studies of magnetism. It is claimed that magnetism stems fundamentally from the spin of electrons in atoms that tend to go in pairs, spinning in opposite directions. The atom as a whole can act as a magnet only when there is an imbalance of electronic spin. Whenever an atom has an odd number of electrons, therefore, this imbalance exists. This neutralizing effect explains why a piece of material that contains atomic magnets is not necessarily magnetic. The physicists tell us that iron is composed of many small magnetized regions called domains, which consist individually of millions of atoms. The piece of iron becomes magnetized when an external force lines up these domains in the same direction. Fundamental data developed by physicists working in fields far removed from minerals beneficiation are now available for developing better magnetic separators for ore processing. More Data Needed on Magnetic Properties of Minerals: There is less information on magnetic properties of minerals than there is for certain aspects of magnetic separator design. When the data on magnetic properties is available, it is often directed toward the study of powders for tape recorders and other highly scientific endeavors that are of little use to the beneficiation engineer. W. R. Crane's table of tractive forces, published in 1902, is still a guide in the study of magnetic minerals. Bits of other information regarding electrostatic conductivity, dielectric constant values, and permeability of various minerals have also appeared but are of small practical value in magnetic separation of ore. It is extremely important to obtain pure mineral specimens for making investigations and to record results that may be of use in studies of magnetic processes. Reference to the large volume of data developed by those concerned with analysis and design of permanent magnets soon reveals that these people have extensively evaluated the effect of various impurities on magnetic properties. Much of the science of the ferrite industry is based upon spinel-type structures which are varied by substitution of selected elements or even subtraction of elements, leaving vacant sites in the space lattice. Magnetic separators are used to beneficiate a wide variety of industrial minerals. In this application the relatively large volumes of nonmagnetics are usually the commercial products. The amount of mag-

Jan 1, 1959

By J. B. Gayle

The merits of the various methods for dry-quenching coke have been the subject of numerous publications and almost equally numerous controversies for the past 40 years.5/ Most investigators have concluded that dry quenching is advantageous. Some have based their arguments on the improved physical properties of the resultant cokes. Others have claimed little or no improvement and have based their arguments on the economies acquired from the recovery and utilization of sensible heat. The extent to which the method of quenching influences the properties of the resultant cokes is of importance in connection with the operation of both commercial and experimental ovens. On the other hand, the recovery and utilization of sensible heat are economic problems related solely to commercial oven operation and- depend on the method of dry quenching used and the demand for a low intensity energy source. The scope of the present Bureau of Mines investigation has been limited to a comparative study of the properties of wet- and dry-quenched cokes produced from six coals and blends carbonized at flue temperatures of 2, 000° and 2,400° F. in the Tuscaloosa oven.

Jan 1, 1959

By H. L. Miaw, A. M. Gaudin, D. W. Fuerstenau

A quantitative method for evaluating density of slime coatings has been developed and applied to formation of iron oxide slime coatings on quartz and on corundum. Slime coating density is related to flotation recovery and to properties of the electrical double layer at mineral surfaces. IN spite of considerable study, the nature of slime coatings in flotation is still not completely understood. However, phenomena that control floc-culation and dispersion of colloidal systems are now interpreted in terms of electrical double layers.",' Colloids will flocculate even though the particles carry the same charge, but when two dispersed colloids of opposite charge are mixed. flocculation ensues even more rapidly. Analogous phenomena seem responsible for slime coating on minerals in flotation systems. To shed new light on the issue it was considered desirable to devise a tool that would measure slime coatings. The usual method has been to examine photographs of presumably representative surfaces, after. an intervening washing in running water. But such an examination is non-quantitative, and the changes in chemical environment represented by the washing may have removed the slime coatings that existed during flotation. To provide the possibility for a correlation with electrical double layer phenomena, the experiments were made with quartz, corundum, and iron oxide, for which elec-trokinetic data are available.'-" Since the properties of the electrical double layers of these oxides depend on the pH of the solution, pH will be the most important variable. Furthermore, because the zero point of charge for silica, iron oxide, and alumina occurs at pH 3.7, 8, and 9.5, respectively, the relative charge on the slime and mineral can be changed over wide ranges. Because of its practical importance in quartz flotation, iron oxide powder was chosen as the slime. Also, its uniform composition, contrasting color, and ease of analysis make experimentation simple. In this investigation, correlation was sought between the effect on flotation recovery of slime addition and slime coating density. Materials and Methods Details are available in a thesis by Miaw." The quartz was selected from pure Brazilian crystalline quartz, crushed, sized (65/150 mesh) acid-cleaned, washed, and stored in conductivity water. The corundum (synthetic alumina of high purity prepared by Linde Co., Chicago) was crushed, sized (65/100 mesh) deslimed, boiled in nitric acid, washed, and stored in conductivity water. The iron oxide slime, reagent-grade ferric oxide (—400 mesh) from Allied Chemical & Dye Corp., was heated to 160°C, cooled, and stored in a vacuum desiccator. In the electron microscope the slime particles appeared to be about 0.3µ in size, but their large specific surface (87,900 cm per g, by gas-adsorption method, using krypton) suggests that the actual particles are smaller than 0.3r. Had they been perfect nonporous spheres, they would have had a diameter of 0.13µ.

Jan 1, 1959

Coal Division Industrial Minerals Division Minerals Beneficiation Division Mining, Geology and Geophysics Division Established as a Society February 26, 1957 OFFICERS AND COMMITTEES J W Woomer, President A B Cummins, President-elect S D Michaelson, Past President C E Lawall, Eastern Regional Vice-President D W Scott, Central Regional Vice-President 3 D Forrester, Western Regional Vice-President R B Ladoo, Treasurer John Cameron Fox, Secretary

Jan 1, 1959

By H. C. Carpenter

Data are presented comparing results obtained with 17 different catalysts in hydrogenating crude shale oil to gasoline in single-pass operation. A method is described for predicting the maximum yield of gasoline obtainable at constant pressure for each catalyst from results of a limited number of experiments at different temperatures. Operating variables have considerable influence on yields and properties of products. With most of the catalysts, at operating temperatures below 890° F. liquid yield exceeded 100 volume-percent. Above this temperature the volume of liquid product decreased rapidly. Maximum gasoline production in most instances was achieved at a temperature higher than that at which the maximum volume of liquid product was produced.

Jan 1, 1959

By O. Q. Leone

Excellent metal quality, with lower power requirement, is attained in electrorefining titanium by using internal heating of the fused-salt bath. An internal heater provides more effective heat utilization, simplifies structural components in cell design, and prolongs cell life by eliminating direct application of heat to the cell container. This Bureau of Mines report covers one phase of the research in progress at the Electrometallurgical Experiment Station at Boulder City, Nev., for improving the techniques and lowering the total power requirement for electro-refining titanium metal.

Jan 1, 1959

By S. L. May

The Bureau of Mines has developed several methods for extracting tantalum and columbium (niobium) and the rare-earth compounds from ores and concentrates. A cooperative agreement was made by the Bureau with Porter Bros. Corporation of Idaho to process 200 pounds of its euxenite concentrate by methods that had been developed at the Albany, Oreg., Metallurgy Research Center. The euxenite concentrate was processed to extract and purify the valuable metals by chlorination, solvent extraction, and hydrometallurgical techniques. Chlorination was used to convert the valuable constituents into chlorides and to partly separate them. Solvent extraction techniques were used to separate the tantalum from the columbium. The rare-earth and uranium compounds were purified by hydrometallurgical methods.

Jan 1, 1959

By John J. Mulligan

The creeks draining Cape Mountain, on the western tip of Seward Peninsula, Alaska, comprise the Cape Mountain tin-placer district. Because of the war-caused shortage of tin, the Bureau of Mines in 1943 conducted a churn-drill placer reconnaissance to explore the district. Favorable indications were found, and plans were made for further investigation of the deposits; the plans were abandoned when tin again became plentiful. In July 1951 the Zenda Gold Mining Co. was granted a Defense Minerals Administration (Defense Minerals Exploration Administration after October 1951) loan to continue exploration of the more favorable areas indicated by results of the Bureau's investigation. Equipment was moved to the area in the fall and winter of 1951-52. During the 1952 field season, 209 churn-drill holes totaling 7,521 linear feet and 10 test shafts totaling 96 linear feet were sunk on the Cape Creek drainage. Work was resumed in 1953, when 56 churn-drill holes totaling 3,157 linear feet were drilled on Boulder Creek. The company planned to drill Goodwin Gulch and Goodwin Creek, but no further work was done owing to lack of capital.

Jan 1, 1959

By R. F. Stewart

A key step in changing coals to fluid fuels and chemicals is the conversion of coal to synthesis gas by gasification with steam and oxygen. As oxygen represents one of the largest single expenses in gasification, its cost is a vital factor in the economy of the process. At present, the most economical method for producing tonnage oxygen is by the conventional rectification of liquefied air. Several alternate methods have been proposed for producing oxygen from air: (1) methods based on physical or chemical sorption of oxygen from air by liquids or solids or (2) the oxidation of certain inorganic com-pounds to higher oxides unstable at higher temperature levels. Economic limitations are discussed by which these methods may be evaluated. Chelated metals of the salcomine type are promising chemical sorbents of oxygen from air. This report covers a study of the reversible sorption of oxygen by salcomine and other chelates. The presence of water in the salcomine structure was verified; it is the loss of this water that causes slow deterioration of salcomine during cycling.

Jan 1, 1959

By H. Dolezal

A laboratory study of acid-ferrous sulfate treatment of low-grade manganese ores from the Cuyuna range, Minnesota resulted in 93-percent extraction of manganese as manganese sulfate with consumption of 3.8 pounds of H2S04 per pound of extracted manganese. Two types of ore were treated in consecutive stages. The first are contained carbonate minerals of manganese and iron, both soluble in H2S04 solution. The second ore contained manganese oxide minerals, insoluble in straight acid solution but soluble in the ferrous sulfate solution obtained from treating the first ore. Leaching data were obtained by countercurrent percolation of coarse (minus-1/2-inch) ore particles at room temperature and by agitating minus-65-mesh ore particles in heated solution. Extraction of manganese and acid consumption were the same, but the percolation leach required 6 days compared with 1 hour for hot agitation. Variations in the size of ore particles treated, leaching time, acid concentration, solution temperatures, and method of applying ferrous sulfate solution to the oxide ore were studied. The effects of several reagents for removing iron from solution and improving filtration were also studied.

Jan 1, 1959

By B. W. Naugle

This report describes the carbonizing properties of coals from the principal beds in Cambria County, Pa. Samples of coals from Upper and Lower Freeport and Upper and Lower Kittanning beds having estimated minable reserves of 50-million tons or more were studied by the Bureau of Mines. Cambria County coals rank either as medium-or low-volatile bituminous. A preparation study indicated that all coals tested in this county, except one sample from the Lower Freeport bed, were responsive to cleaning and would yield a product with satisfactory chemical properties for metallurgical coal. All coals tested from Cambria County yielded strong coke; however, they expand excessively when carbonized singly, and should be used only as minor constituents in metallurgical coking blends when carbonized in slot-type ovens.

Jan 1, 1959

By O. F. Kammerer, W. E. Miller, D. H. Gurinsky, J. Sadofsky, J. R. Weeks

Zirconium and titanium inhibit solution mass transfer of steels by liquid bismuth, mercury, and lead. It is shown that in bismuth and mercury, these adsorb on the surface of the steels and subsequently react with nitrogen and possibly carbon from the steels to form inert, adherent surface layers of ZrN, TiN, or TiN + Tic. Data are presented which describe the condition under which thase deposits form. These inhibitors decrease the solution rate of iron into bismuth, and require a higher supersaturation for precipitation of iron from bismuth. USE of the low-melting heavy metals (bismuth, lead, mercury, and their alloys) as coolants has been limited because solution mass transfer of steels occurs in these liquids; i. e., iron dissolves in the hot sections of the heat transfer circuit and deposits in the colder sections. The rate of solution of iron and the temperature coefficient of solubility are sufficiently great to cause complete or partial stoppage by the deposition in the coldest section of a closed circuit in finite time, even though the actual solubilities are extremely low. In the development of the mercury vapor turbine by the General Electric Co., Nerad and his associates1 discovered that the addition of as little as 1 ppm Ti or Zr to magnesium-deoxidized mercury reduced the mass transfer of ferrous alloys by mercury to a negligible amount. Reid2 reported that titanium was detected chemically on the surface of steels contacted with this mercury alloy in amounts varying from 2.0 to 2.6 mg per sq in., the greatest amount being found in the hottest portion of the circuit. Reid stated that the titanium forms the intermetallic compound Fe2Ti by reaction with iron on the surface of the steels. This compound was presumed to be highly insoluble in mercury. More recently, El-gert and Egan3 have reported a greater than 100-fold reduction in the rate of mass transfer of a 5 pet Cr steel by liquid bismuth upon the addition of titanium (in excess of 50 ppm) and magnesium (350 ppm) in the liquid metal, during experiments performed in thermal convection loops* over the temperature differential 700° to 615° C. Also, Shep-ard and his associates' have reported that the addition of titanium to liquid bismuth and Pb-Bi eutec-tic produced a marked decrease in the rates of solution of both iron and chromium from type 410 steel capsules under static conditions. This inhibiting effect increased with repeated reuse of the capsules. Tests performed in this laboratory under carefully controlled conditions have shown that the addition of zirconium and magnesium, or titanium and magnesium, to liquid bismuth or lead greatly reduces the rate of mass transfer of chromium alloy steels and carbon steels in thermal convection loops with a maximum temperature of 550°C.5-9 The present paper will review the data obtained to date at this laboratory on the behavior of iron and steels in contact with liquid bismuth alloys containing titanium or zirconium, and will attempt to explain the role of the above additives in reducing solution mass transfer. Reaction between the Zirconium or Titanium Dissolved In Liquid Bismuth and an Iron or Steel Surface Reaction between Zirconium Dissolved in Bismuth and the Surface of Pure Iron-—A small pure iron crucible (analyzed by the supplier to contain 0.8 ppm N was contacted with bismuth containing approximately 0.1 pet Mg and varying amounts of a radioactive zirconium tracer. The crucible was then inverted at the temperature of contact. The thin residual layer of adherent bismuth was dissolved in cold, concentrated nitric acid. The crucible surface and the solidified bismuth were then analyzed for radioactive zirconium. An analysis of the activity loss on the crucible surface and the weight loss of the crucible during the nitric acid treatment showed that the acid treatment removed the zirconium that had originally been dissolved in the adherent bismuth, but not any zirconium that may have reacted with the crucible surface. The crucible was then pickled in warm aqua regia to remove all surface activity, hydrogen-fired at 600°C, and recontacted with a new liquid alloy. The results of the experiments contacted 1 hr at 450°C show, Fig. 1, a Langmuir-type adsorption with an adsorption free energy of approximately 17 keal per g atom Zr.5 This deposit was estimated to contain 1 atom of zirconium for each 7 to 8 iron atoms on the crucible surface, assuming a surface roughness factor of the pickled crucibles to be five. Increasing the temperature to 520°C caused consi-

Jan 1, 1959

By J. E. Forciea, O. E. Palasvirta, L. G. Hendrickson

AH pilot and commercial plants working with Mesabi Range taconite employ wet magnetic separation. Progress is being made with a dry magnetic process, but this has not yet been applied to taconite except in the laboratory and pilot plants. Flowsheets in all five plants are similar, including multiple stages of grinding, each followed by magnetic separation, which rejects a finished tailing. The flowsheet in Fig. 1 is used in the preliminary and commercial plants of the Erie and Reserve mining companies and in Unit C of Oliver's Pilotac plant. At Erie the desliming operation is omitted. In the Reserve plants two ball mills are used with each rod mill. Pilotac uses flowsheet 2 in Unit A-B and has also tested flowsheet 3. Principal differences in the three flowsheets are the number of grinding stages and the type of roughing. The terms open-circuit roughing and closed-circuit roughing are best defined by the diagrams. Special Test Data Given in Table I: For the Erie and Reserve commercial plants, Table I reflects routine conditions. Pilotac, the experimental plant, has been run with several flowsheets, including those followed at Erie and Reserve's commercial operations. Pilotac data for these last two flowsheets are similar to commercial plant results and are not repeated in Table I; statistics are given, however, for special test conditions. using other flowsheets. when the objective was to 'to extra-grade concentrate, Variations Among Taconites: Although crude ore tributary to these plants is generally classified as taconite, there are important differences in mineralogy and fineness of dissemination.

Jan 1, 1959

Jan 1, 1959

By K. G. Gorling, S. J. Wallden, N. B. Lindvall

It is the policy of The Metollurgical Society to provide, in the TRANSACTIONS OF THE METALLURGICAL SOCIETY OF AIME, a prompt and accurate medium for publication of reports of significant new research in both the scientific and engineering aspects of metallurgy. Papers submitted to the Society are judged by competent reviewers according to established criteria for technical merit, accuracy, originality, and presentation. STAFF: Editorial Director, Rixford A. Beals; Associate Editor, James J. Burke; Assistants, L. Capria and R. K. Larkin. PUBLICATIONS COMMITTEE OF THE METALLURGICAL SOCIETY: A. W. Thornton, Choirmon; Dennis Carney, John Chipman, J. C. Fulton, J. H. Hollomon, H. tl. Kellogg, A. E. Lee, R. Maddin, J. D. Sullivan, and O. Swan. Review and selection of manuscripts is under the supervision of the following Publications Committees: Extractive Metallurgy Division T. B. King. Cha~rmon; S. J. Dickenson, R. P. Hermsdorf, R. Schuhmann, Jr.. and P. T. Stroup. Institute of Metals Division: Robert Maddin, Chairman. F. Lincoln Vogel, Jr., Vice-chairman, W. A. Backofen, R. W. Balluffi, J. H. Bechtold, M. B. Bever, R. S. Busk, C. G. Goetzel, Paul Gordon, C. D. Graham. Jr., Robert F. Hehe-mann, R. I. Jaffee, F. E. Jaumot, Jr., lrving R. Kramer, A. J. Leno, Horold Margolin, C. J. McHorgue, Russell A. Meussner, J. 6. Newkirk, H. W. Paxton, G. E. Pell~ssier, I. S. Servi, Alan U. Seybolt, A. J. Sholer, and Sack Wahsburn. Iron and Steel Division: J. C. Fulton, Chairman; T. B King, F. C. Langenberg, W. O. Philbrook, and T. B. Winkler. Published bimonthly by the American Institute of Mining Metallurgical and Petroleum Engineers Inc., 29 West 39th Street, New York 18, N. Y. Telephonne pennsylvania 6-9220.Petroleum Subscription Engineers$20 per year for non-AIME members in United States and North South and Central 6-9220.SubscriptionAmerica $25 toreign; $5 for AIME members. Single copies, $4.00, iinalo copies Southfpr;ign,andCentral $5 00. The AIME 'is $25not responsible for any statement made or opinion expressed in its publications Copyright 1958 1958 by the American Institute of Mining, Metallurgical, and Petroleum Engineers, Inc. . Registered coble address, AIME New York . . . Indexed in Engineering Index, Industrial Arts Index, ...and Chemical Abstracts . . . Application for second class mail privileges IS pending at New Yark, N. Y. Volume 212, Number 2.

Jan 1, 1959

By J. H. Field

The sulfur dioxide emitted in low concentrations in flue gases from the combustion of sulfur-containing coals and fuel oils is a significant factor in contamination of the atmosphere with sulfur dioxide. A review of methods for treating gases containing high concentrations of sulfur dioxide shows that they are seldom satisfactory for purifying flue gases. Processes developed specifically for treating flue gases using liquid absorbents are costly and may cause localized pollution, because the cooled flue gases can settle in the vicinity of the stack. Bench-scale research is being conducted to investigate the use of dry absorbents for sulfur dioxide removal at temperature levels of about 250°- 300° F. and 600°-650° F. Alkalized alumina has been found effective for treating simulated flue gas and Is regenerable by hydrogen, carbon monoxide, or producer gas. Other metallic oxides have been tested as absorbents also. Chemically impregnated activated carbons removed sulfur dioxide from the gas at 265° F. Vanadium pentoxide is effective as a catalyst for oxidizing of sulfur dioxide in the simulated flue gas at temperatures lower than have been used commercially for gases with higher concentrations of sulfur dioxide. Conversions of sulfur dioxide to trioxide wore studied as a function of temp- erature over a range of about 570° to 750° F.

Jan 1, 1959

By Arnold B. Hubbard

This report presents a hydrogenolysis study undertaken to obtain information on the constitution of the kerogen or organic material in Colorado oil shale and to determine some of the properties of the hydrogenolysis products. The high yield of hydrogenolysis products was separated, so far as possible, into type compounds; a number were identified. The results thus obtained were used as a basis for proposing the possible existence of certain structures in kerogen. To the authors' knowledge, few or no hydrogenolysis studies have been made of Colorado oil-shale kerogen by others. However, this method has been used in studying the constitution of coal. In general, the coal studies involved treating pulverized coal at different temperatures and hydrogen pressures with different catalysts. In some instances different solvents were used during the treatments.

Jan 1, 1959

By J. J. Demeter

As part of its work on converting coal to fluid fuels, the Federal Bureau of Mines has been studying the synthesis of liquid fuels from carbon monoxide and hydrogen by Fischer-Tropsch synthesis. A fluidized bed of nitrided, fused-iron catalyst has been operated successfully to produce high yields of oxygenated compounds. Trouble-free operation continued for over 800 hours, and the test was terminated voluntarily. About 85 percent of the fresh feed was converted when the unit was operated at a space velocity of 500 hr.-1, a 12:1 recycle-to-fresh-feed-gas ratio, a 300-p. s. i. g. pressure, and a temperature of 252° C. When operating at a fresh-feed-gas space velocity of 1,000 hr.-l and a 9:1 ratio of recycle to fresh gas, conversion of fresh feed was 68 percent, and the product yield was 235.9 grams per cubic meter of synthesis gas converted. The oxygenate and C5 and heavier hydrocarbon yield was 110.6 grams per cubic meter of gas converted, 83 percent of this was oxygenates. The atom ratio of N:Fe of the catalyst, initially 0.455, decreased to 0.288 by the end of the 800-hour experiment. Nevertheless, the yield of oxygenated compounds per cubic meter of H2 + CO converted at the end of the run was approximately the same as that obtained 500 hours earlier with identical operating conditions. X-ray analysis of the discharged catalyst indicated that only ?-iron carbonitride was present. Sieve analysis of the discharged catalyst indicated that only 2 percent of fines was produced during the reduction, nitriding, and synthesis.

Jan 1, 1959

By Lloyd H. Banning

ELECTRIC smelting tests were conducted at the Northwest Electro-development Experiment Station, Albany, Oreg., to develop a feasible process for producing silicomanganese from siliceous manganiferous material. The Jackson County, Oreg., material used was massive and contained rhodonite as the most abundant mineral. Both raw and beneficiated materials were tested; various proportions and types of fluxes and reductants were used to make up the furnace charges. The silicomanganese product was used successfully in manufacturing various steels at industrial plants. The manganese content of the samples ranged from 23 to 28 percent; silica plus alumina content was as high as 55 percent-about four times the maximum specification for Metallurgical-grade ore. Sink-float laboratory tests indicated that the manganiferous material was amenable to beneficiation. Over 2 tons of rhodonite concentrate was prepared for smelting tests in a sink-float operation. Only the minus-3/4-inch, plus-8-mesh fraction was fed to a heavy-medium cone; over 97 percent of the manganese was recovered in the sink product, which contained 32.4 percent manganese and 44 percent silica plus alumina. About 25 percent of the silica was removed in the float product.

Jan 1, 1959