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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

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 M. G. Zabetakis

This publication presents a simplified graphic method for determining the explosibility of mine atmospheres under mine-fire conditions from mine- atmosphere composition data. Sometimes it is necessary to seal part of a mine during a fire to exclude air and thus extinguish the fire. Unfortunately, liberation of methane and formation of hydrogen and carbon monoxide in the sealed area may create an ex- plosive or flammable atmosphere if enough oxygen is present to support combustion. On the other hand, the oxygen concentration may be reduced through combustion processes and the concentration of inert gases (nitrogen and carbon dioxide) increased enough to render the atmosphere within the sealed area non-explosive. Before an area is unsealed, it is extremely important to know if the sealed atmosphere contains Flammable gases in proportions that might form explosive mixtures when air is introduced. If an explosive mixture forms and the fire is rekindled, a gas explosion will result. Various experimental methods may be used to determine the explosibility of a particular mine atmosphere; however, these methods usually are impracticable in the field.

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 Russell W. Hunt

The cave man of ages past took his wife-and family from the cave pointing to a fire he had built and beating on his breast said, "Look what I have done". Today man is taking his family back to a cave saying, "Come enter in because of what I have done". At the close of World War II Germany said if they had gone underground one year earlier with more of their operations, the war could have lasted four years longer with perhaps much of Britain devastated. The protection of the home front no longer rests with the soldier in actual combat. The battle will be won at home with the most careful kind of protection against missiles. After Nagasaki-Hiroshima Sir Winston Churchill said in substance "Up to now the Almighty has mercifully withheld from man the knowledge of these terrible weapons of destruction."

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 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

By A. F. Henderson, C. F. Cornell, A. F. Dunyon, D. A. Dahlstrom

Ossi E. Palasvirta (Development Engineer, Oliver Iron Mining Diu., U. S. Steel Gorp.)—The authors are to be congratulated for their interesting article, which thoroughly illustrates the variables inherent in filtration of taconite concentrate. The work and the conclusions based thereon largely parallel the test work done by the writer at the Pilotac plant" and the experience gained with a commercial size agitating disk filter in the same plant. At Pilotac, however, a thorough study was also made of the effect of depolarizing (demagnetizing) the filter feed, and it is the purpose of this discussion to comment on the merits of depolarization of the magnetite concentrate prior to filtering. The work at Pilotac was done in three phases: 1) preliminary laboratory testing with a circular filter leaf of 0.047 sq ft, followed by 2) plant testing using a 4-ft diam, single-disk agitating filter that was purchased on the basis of the pilot tests on the 4-ft model. In the laboratory tests depolarization was achieved by slowly withdrawing' batches of thickened concentrate from a coil producing an alternating field of about 300 oersteds. In plant tests the standard Pilotac procedure' was employed, wherein the pulp falls freely through the depolarizing coil. The preliminary tests in the laboratory at first seemed to indicate that although depolarization of the filter feed decreases the cake moisture, it also tends to decrease the thickness of the cake, thus decreasing filtering rate. The tests with the 4-ft disk filter soon showed, however, that the compactness of the cake, attained during the form period because of depolarization, permitted a considerable decrease in drying time without any sacrifice in final moisture content. Thus, the filter could be operated at a much higher speed, and the overall capacity was higher than with magnetized feed. Because of the great compactness of the cake there was little shrinkage during the drying period, which prevented cracking and subsequent loss in vacuum. This in turn permitted operation with as thick a feed pulp as the diaphragm pumps could handle, eliminating the necessity of pulp density control. On the basis of these findings, the 6-ft agitating disk filter has been operated at 2 rpm, using feed pulps varying from 65 to 73 pct solids. Initially Saran 601 was used as medium, but it was later replaced with a relatively open, tight-twist nylon cloth. Filtering rates up to 750 lb per ft- er hr can be attained with feeds averaging about 70 pct- 270 mesh, and there is no trouble because of cracking. The cake moistures vary between 8.5 and 9.5 pct. To recapitulate, the merits of depolarizing the filter feed may be summed up as follows: 1) The well dispersed pulp shows less tendency to settle in the filter tank. 2) The homogeneous filter pool results in more even cake formation. 3) Because of absence of flocs, great compactness of cake is attained during the form period. 4) The cake does not tend to crack during the drying period. 5) A drier cake is produced. 6) A shorter drying period is necessary, permitting higher operating speed, which in turn results in increased capacity. 7) Density of the feed pulp can be kept as high as the equipment can handle. This increases capacity, since it is directly proportional to the percentage of solids in the pool. A few tests were also made to study the effect of chemical flocculants on filtration efficiency. Results showed that the effects of chemical and magnetic floc-culation were quite similar. Thus the use of a floccu-lant would impair rather than improve the filtering of magnetite concentrate. A. F. Henderson, C. F. Cornell, A. F. Dunyon and D. A. Dahlstrom (authors' reply)—We want to thank O. E. Palasvirta for his comments, particularly in view of the encouraging results obtained with demagnetized taconite concentrate. In our studies an attempt was made to evaluate the effects of depolarizing the feed to the plant filters by passing the slurry through a coil, similar to the method described by Palasvirta. Unfortunately, in our experiments there were no startling improvements in performance level, neither cake rate increase nor cake moisture reduction. However, when slow filter cycle speeds were employed, the filter cake tended to crack and the vacuum level dropped, resulting in an increase in cake moisture content. When demagnetized feed was used during slow speeds, no cake cracking was evidenced and the vacuum level remained constant. Thus the depolarizing coil was found necessary only in cases of cracking. It should be noted that most of our test work concerned a feed of 85 to 90 pct —335 mesh and about 60 pct by weight solids concentration. This contrasts with 70 pct —270 mesh and 65 to 73 pct by weight solids as noted by Palasvirta. Reviewing both sets of results, it might be concluded that depolarizing may be successfully employed to alleviate cake cracking tendencies and may markedly improve cake rates and moistures on the coarser taconite concentrates. Further investigations may disclose the exact relationship of grind and pulp density to the depolarizing action.

Jan 1, 1959

By K. U. Snowden, J. N. Greenwood

EARLY studies by Gough and sopwith' have shown that the fatigue resistance of certain metals increased when the test was carried out in a partial vacuum; lead showed this effect to a marked degree. This communication describes surface deformation differences between high-purity lead fatigued in air and in a vacuum of approximately 5 X l0-3 mm Hg. Both air and vacuum tests were carried out by the same alternating flexure machine at a frequency of 500 cpm. Flat cantilever-bend specimens with tapered sides were cut from strip, annealed at 100°C, and chemically polished.

Jan 1, 1959

By H. I. Aaronson

The nucleation of pearlite at proeutectoid ferrite is inhibited, to an increasing extent, at the following locations: At twin boundary-nucleated ferrite, between closely spaced ferrite sideplates, and at intragranular plates. These effects are discussed in terms of the influence of transformation strain energies and of the interfacial free energy of austen-ite:ferrite boundaries on the rate of pearlite nucleation. The growth of pearlite into the interiors of austenite grains from the region of the grain boundaries is markedly restricted when low reaction temperatures and large austenite grain sizes permit the development of interlocking networks of intragranular ferrite plates. PREVIOUS investigators have made extensive studies of the interactions which occur between the proeutectoid ferrite and the pearlite reactions from the viewpoint of the mechanisms through which pearlite interferes with the nucleation and growth of proeutectoid ferrite.1-3 In the present investigation, the processes through which proeutectoid ferrite (hereafter termed simply "ferrite") can reduce the rate of formation of pearlite have been explored in some detail. A steel with a relatively low carbon content, in which the ferrite reaction can compete successfully with the pearlite reaction over a wide range of reaction temperature, and exceptionally coarse-grained specimens, which further emphasize the role of the ferrite reaction, have been employed for most of this work. A brief examination also has been made, however, of the effects of smaller austenite grain sizes upon these processes. Experimental Procedure The steel employed had the following composition: 0.29 pet C, 0.76 pet Mn, 0.25 pet si, 0,007 pet S, and 0.005 pct P. This alloy was homogenized for 48 hr at 1250°C. The investigation was performed

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 D. Turnbull, J. E. May

THE (110) [001] texture in silicon iron is of considerable interest both from the technological and scientific points of view. Its occurrence was reported more than 20 years ago.1-4 The texture develops by means of secondary re crystallizatjon5 and can be very strong, that is, greater than 90 pct alignment even thouh the primary re crystallization texture is weak or complex. This behavior is in contradistinction to the face-centered metals which develop their strong secondary recrystalliza-tion texture from a strong primary recrystalliza-tion texture.', The microstructural changes accompanying the (110) [001] texture formation in silicon iron are as follows: When properly prepared cold-rolled sheet (i.e., 0.015 in. thick) is annealed at about 800°C, primary recrystallization occurs and a fairly stable fine-grained primary recrystallized matrix of about 0.02-mm-diam grain size is produced. The material at this stage does not have the strong (110) [110] texture. As the temperature is raised to about 900°C, relatively large grains appear in the finegrained matrix and they grow at the expense of the smaller grains to many times the sheet thickness. In time the complete sample is consumed by these large grains. This process of the growth of relatively few grains (about one in 105 primary grains) at the expense of many grains is called secondary recrystallization. Since all the secondary grains are of essentially (110) [001.] orientation, the strong texture is developed by this secondary recrystallization process. Theories of the (110) [001] texture in polycrystal-line silicon iron have been proposed by Decker and Harker and by Dunn.Decker and Harker have shown that grains initially in the (110) [001] orientation will upon annealing after cold-rolling, re-crystallize back to the initial orientation. To account for the sharp texture in silicon iron they propose that (110) [001] grains become more highly strained than grains in other orientations and therefore recrystallize first. They are then the lowest energy grains and can consume their higher energy neighbors. Grains in orientations other than (110)

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

By Jasper D. Ward

The Indiana Limestone Company has developed an insulated, thin and comparatively light-weight pane 1 suitable for use as a spandrel panel in a curtain wall. The panel is about four inches thick and is composed of limestone backed with insulation. The inner surface of the insulation is protected with asbestos-cement board or a metal pan, depending on the type of insulation, building-code requirements and appearance (if the surface is left exposed). The limestone is cut to the size of the spandrel openings and the insulation and backup is applied in the mill ready to be shipped and in- stalled in the wall grid, A mortarless and waterproof joint with the metal frame components is achieved through the use of neoprene, thiokol, and caulking, The limestone is "dirt-proofed" (waterproofed) in the mill to slow down discoloration. The panel weighs more than some presently used materials. However, ILCO's architects and engineers have found that curtain wall systems capable of withstanding imposed wind loads are made up of sections large enough to carry this extra load of stone with little or no modification to the size of the metal frame. Limestone, a traditionally sound material, can be used in this new way without losing any of its natural qualities of dimensional stability, resistance to fire, and permanence.

Jan 1, 1959

By J. B. Watts

"THE Mine Engineering Department at Gaspe Copper is staffed by a chief engineer, assist-ant engineer, research engineer, chief surveyor, four instrument men, chief bonus clerk, draftsman, and a helper pool of four permanent men plus one or two students in the summer. The men are grouped according to function for organization purposes. Routine services provided by the Mine Engineering Department in-elude ail surface and underground surveying and mapping, preparation of working drawings, compilation of engineering reports, recommendations on ventilation, testing the mine air for carbon monoxide, research on mine equipment and its use, and the calculation of incentive bonus. Demand jobs from departments other than the Mine Department .are done on request. Such jobs may be in the plantsite, the Town of Murdochville, or at the shipping points at Gaspe harbour or the St. Lawrence river."

Jan 1, 1959