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By David J. Kusler

This report describes a rapid, reliable, and relatively simple method developed by the Bureau of Mines Pyrometallurgy Laboratory at Bruceton, Pa., for determining lime (calcium oxide) and magnesia (magnesium oxide) in various materials containing these constituents in greater than trace amounts. Optionally, titania (titanium dioxide) may be determined for the same sample. The accuracy of the method, suitable for most purposes, is shown by comparing the Bureau results with those obtained by accepted procedures. The method has been applied satisfactorily to the routine analysis of blast-furnace slags, for which purpose it was primarily developed, and to other calcareous compositions. In the Pyrometallurgy Laboratory it has replaced the standard methods previously used to determine lime and magnesia, and has been in general use by that laboratory for the past several years. The analysis time, generally under 3 hours, is considerably less than required by standard methods.

Jan 1, 1960

By Byron E. Blair

This report describes procedures for using a high-speed camera to study blasting phenomena. Both quantitative and qualitative information can be obtained, provided that proper interpretations of the projected two-dimensional images are made. Geometrical relationships between object and image displacements are given in terms of horizontal and vertical angles of the camera optic axis with respect to the quarry face. Correction factors are given for obtaining true object displacements from image displacements in the camera film plane. The time of initial rock movement also is considered, and the control-ling factors of camera speed, scale factor, minimum increment of projection measurement, etc., are evaluated in terms of minimum time intervals. The high-speed camera and associated equipment are described, and field measurements and laboratory data analysis techniques are outlined. An analysis of a typical high-speed motion picture is made, and the application of the necessary correction factors is illustrated.

Jan 1, 1960

By J. B. Gayle

The removal of coal particles from a slurry by flotation is made possible by the formation of stable aggregates with air bubbles of suitable sizes. The formation of such aggregates is theoretically possible only for certain favorable combinations of the solid-liquid-gas interfacial tensions. Because interfacial tensions involving solid phases are not conveniently measurable, a related variable, the contact angle, frequently is used as a measure of the floatability of various materials. Zero angles indicate nonfloatable substances, and large angles indicate substances having a high degree of floatability. During a study of contact angles for coal and substances related to coal in their similarity of response to various physical and chemical treatments, particularly flotation, carbonization, and oxidation, the reproducibility of replicate determinations taken within a 4-hour period was found to be much better than that for comparable results taken over a longer period of time. Consideration of possible causes for these differences led to an investigation of the effects of temperature variations on contact angles. References to literature revealed only a small amount of information, some of it apparently conflicting. Specifically, Sutherland and Wark4/ found that temperature variations "within limits" did not appreciably influence the angles measured for galena conditioned with potassium ethyl xanthate. On the other hand, McGlashan and McLeod5/ presented preliminary data showing that for sphalerite conditioned with potassium ethyl xanthate the angle is maximum at 25° to 35° C., depending on the pH of the system.

Jan 1, 1960

By F. E. Block

This investigation was made as part of a larger program to develop basically new methods for preparing yttrium metal in high-purity form. It was performed under a cooperative agreement between the U.S. Atomic Energy Commission (AEC) and the Federal Bureau of Mines. Laboratory-scale tests were made to devise methods for preparing high-purity, anhydrous yttrium trichloride, for reducing the yttrium trichloride with sodium or lithium, and for consolidating the resulting yttrium sponge into ingots.

Jan 1, 1960

By P. C. Good

High-purity chromium was prepared in massive form by the electrolysis of chromium trioxide solution at high temperatures. The metal thus obtained, containing 50 to 150 p.p.m. of oxygen, 20 p.p.m. of nitrogen, and traces of metallic impurities, could be hot-worked to rod and sheet and drawn to wire ductile at room temperatures. Optimum concentrations and operating conditions were established for the deposition of chromium from chromic acid baths containing sulfate, fluoride, and silicofluoride ions. Current efficiencies of 13 percent were attained with baths containing sulfate ion, and efficiencies of 40 to 44 percent with baths containing fluoride and silicofluoride ions. Cation exchange resins were used for removing metallic impurities from chromic acid solutions containing sulfate ion; solutions containing fluoride and silicofluoride ions were purified by recrystallization.

Jan 1, 1960

By I. Iwasaki

In recent years the rapid depletion of high-grade iron ores and the demand by blast furnace operators for increasingly low-silica ores have stimulated interest in flotation studies of low-grade iron ores, such as wash-ore tailings and oxidized taconites. Four processes have been reported for the flotation separation of these iron ores--anionic and cationic collection of the iron oxides, cationic collection of siliceous gangue, and anionic collection of activated siliceous gangue (5).5/ The effectiveness of any one method, however, depends largely on the mineralogical composition and on the physical structure of the sample; hence, a comprehensive study of the floatability of the individual minerals occurring in these materials is essential. A review of the literature shows that the floatability of hematite and magnetite has been frequently investigated, whereas very little corresponding information is available for goethite, or for its more earthy form, limonite, both of which are abundant in the Mesabi and Cuyuna ores (19). The purpose of this investigation was to formulate general information on the floatability of goethite. Vacuum flotation, contact angle measurement, and simplified flotation tests using a modified Hallimond tube were used. The experimental results were correlated with the electrokinetic properties of goethite as determined by streaming potential measurement. The results were used to interpret the batch flotation tests made on an artificial mixture of quartz and goethite.

Jan 1, 1960

By V. A. Nieberlein

This paper presents the results of research undertaken to recover titanium and columbium by low-temperature chlorination of low-grade columbium-bearing ilmenite concentrates, and to simultaneously remove chlorinated impurities from the volatile chlorides without resort to distillation. Coke-reduced ilmenite was chlorinated at 400° to 500° C., and the resulting TiC14 was free of most impurities before condensation. A heated purification column was used wherein various packing materials reacted chemically or physically with the impurities which passed through them in the vapor phase. A nearly water-white TiC14 product was obtained directly. The principal impurities in the titanium tetrachloride were: 0.02 percent Fe, 0.01 percent V, 0.05 percent A1, 0.04 percent Si, and 0.07 percent Cb. This is a less pure product than commercial TiC14. Most of the columbium was recovered as crude CbC15, requiring further refining.

Jan 1, 1960

By C. J. Walker

The ever-increasing use off natural underground formations for storing natural gas has focused attention on the behavior of such storage formations under varying operating conditions. The need for a means of evaluating in¬dividual wells and groups of wells has become manifest. It is essential that industry and others be able to determine the rates of flow that can be ex¬pected from a given well or group of wells under different conditions and to ascertain whether certain wells are deteriorating. Such questions need more exact answers now than ever before because of the vital role underground gas storage plays in the industrial and domestic consumption of natural gas. The Bureau of Mines--in cooperation with the American Gas Association--has main¬tained an active interest in gas-well testing because of the implications of such test procedures on the consumption and efficient production of natural gas. A basis for testing gas wells was provided by the back-pressure method of Rawlins and Schellhardt (12).4/ They showed that for normal gas wells there is a consistent relationship between rates of delivery of gas and corresponding pressures when the formation pressures are used as the basis of interpretation, The equation for this relationship is as follows: Q = C (Pf2 - Ps2)n where; Q = rate of flow, generally expressed in cubic feet per 24 hours. C = a coefficient.

Jan 1, 1960

By R. F. Tenney

The performances of four anthracite-burning stokers have been observed under identical 74-hp. steam boilers. Fifty runs of 12 and 24 hours' duration were made in accordance with the test code of the American Society of Mechanical Engineers (ASME). The capacity of each stoker for burning anthracite has been determined, the heat efficiency at each fuel rate has been computed, and the various significant items of hear loss have been estimated. The operating data and results from each run are tabulated in this report in the form used in the test code. The heat efficiencies and most significant operating data for each run are also presented graphically for each stoker to establish the trends with increasing boiler outputs, The tests show that rice anthracite can be burned on stokers adapted to its use at heat-conversion efficiencies of 82 percent or more under continuous firing. These high efficiencies are maintained with fuel inputs 30 percent higher and lower than the peak efficiency rate. Moreover, a heat efficiency of 70 percent or more is obtained at 50 percent of the optimum fuel rate, even though the excess air into the furnace cannot be held below 150 percent.

Jan 1, 1960

By Walter W. Fowkes

Leonardite is a coallike substance, similar in structure and composition to lignitic coal and believed to be derived from lignitic coal by the process of natural oxidation. Leonardite is little known outside lignite-producing areas and has been developed commercially only to a minor extent. The higher oxygen content and less compact structure of leonardite, compared with lignite, make it undesirable as a fuel but indicate that it has potential as a source of chemicals and for other nonfuel uses. It is a convenient source of humic acids. The United States has a large natural reserve of leonardite; furthermore, it can be produced in the laboratory under controlled conditions. The significant elemental difference between leonardite and lignite is the oxygen content (leonardite, 28-29 percent; lignite, 19-20 percent). The higher oxygen content of leonardite is due entirely to a Larger number of carboxylic acid groups. This fact explains the 17-Cold increase in alkali solubility of leonardite. Spectral studies indicate that the material is mixed salts of humic acids.

Jan 1, 1960

By D. D. Walker

Scheelite, the most abundant tungsten mineral in the Philipsburg region of Montana, is found in replacement deposits and along fissures and cracks in limestone at various distances from contacts with acidic igneous rocks. It also occurs at the limestone-igneous contacts, but typical garnet tactites are developed in only a few places in the region. The most favorable host rocks for scheelite mineralization are the Jefferson, Hasmark, and Madison limestones. Scheelite is exposed in float, outcrops, and surface and mine workings along a 2-mile-wide belt extending southwest from Lost Creek beyond Silver Lake, a distance of 15 miles or more. (See fig. 1.) Some scheelite is found in veins formerly mined for silver. Powellite and molybdenite occasionally are present with the scheelite. Hubnerite occurs in quartz veins in the Black Pine area 10 miles northwest of Philipsburg. These quartz veins occur in the quartzites of the Precambrian Spokane formation. Tungsten production in the region has come almost exclusively from scheelite deposits, both lode and placer. During a 6-year period beginning in 1943 a total of 142.0 tons of 63-percent W03 concentrate was produced by H & H Mines Co. In the early 1950's, the Trigger mine produced 4,000 tons of 1-percent W03 ore and the Tip Top 650 tons of 2.0-percent W03 ore and 2,906 tons of 2.2-percent ore. There has been sporadic production from some of the smaller properties in the area.

Jan 1, 1960

By John Nagy

A study was made in the Bureau of Mines experimental coal mine of factors affecting gas ignition by a cutoff explosive charge. Experiments showed that, although gas could be ignited under some circumstances, the probability under normal mining conditions would be low. The use of permissible explosives, relatively short-delay intervals in firing adjacent holes, blasting to a 6-inch kerf, and reasonable care in the placement of the holes favor safe blasting and are current practice in mining. The experiments also showed that the weight of the charge is not a primary factor in the ignition of gas by a cutoff charge. The quenching action of a first charge on the igniting action of a second was verified in a supplementary study. Related experiments have shown that gas at the face may be ignited by a single charge of explosive when fired with a light coal burden. Permissible explosives were less hazardous under these conditions than nonpermissible explosives. The frequency of gas ignition in cutoff and single-charge experiments increased as the linear distance between the sheared face and the opposing mine rib increased.

Jan 1, 1960

By John C. Holtz

"The Federal Bureau of Mines serves the mining industry by approving equipment that is designed to prevent explosion, fire, shock, or toxic hazards in mines when such equipment is used and maintained in a proper manner, through research, consultation, testing, and inspection, the Bureau studies machinery and component parts submitted by manufacturers and others. Before receiving the Bureau's approval as permissible for safe use in mines, equipment must pass exacting tests and must meet strict requirements established through research and experience and listed in the Bureau's various permissibility schedules. An important phase of the Bureau's research is the testing of diesel engines.Mobile diesel-powered equipment can be used safely in underground noncoal mines and tunnels when mechanical ventilation is provided to dilute and remove the exhaust gas and to replenish oxygen in the underground atmosphere. Safe ventilation is determined by suitable tests of each engine used in a diesel machine. This ventilation cannot be predicted safely, accurately, and economically from any general empirical relationship.In determining safe ventilation, the quantities of carbon dioxide, carbon monoxide, and oxides of nitrogen generated by a diesel engine must be ascertained. These quantities are related to the displacement of the engine, its speed of operation, the design of the combustion chamber, and the fuel:air ratio needed to produce useful power. At overrich fuel:air ratios, all diesel engines generate excessive quantities of toxic carbon monoxide and smoke. The results of engine tests are used to determine a maximum fuel-injection rate at or below which carbon monoxide can be controlled by a reasonable ventilation and smoke is essentially eliminated. Toxic oxides of nitrogen are related to fuel:air ratio and the design of the combustion chamber. Their concentration in the exhaust cannot be controlled by engine adjustments, and each engine appears to have individual characteristics concerning formation of these oxides. Production of oxides of nitrogen frequently is the most important factor in determining safe ventilation."

Oct 1, 1959

By Michael Sokaski, M. R. Geer, H. F. Yancey

This report is one of a series describing investigations by the Federal Bureau of Mines of the performance of various types of coal - cleaning equipment ; other reports in the series are listed in the bibliography . The information in these reports is useful to the coal industry and the manufacturers of coal - cleaning equipment in several ways : First , it assists the coalpreparation engineer who is planning a new plant to select the type of process best suited to the requirements by enabling him to forecast the yield and quality of clean coal obtainable with each type of equipment . Second , the information serves as a yardstick by which the performance of a plant can be judged and thus helps determine whether it is operating at satisfactory efficiency . Both these functions promote better coal - preparation practice ; that is , they help provide coal of more suitable quality for the market and likewise minimize the waste of good coal . This serves the interest of conservation with which the Bureau is vitally concerned . The present report deals with three plants using the Tromp dense - medium process , named after its inventor , K. F. Tromp , who developed the process in the Netherlands in 1936.5/ Selection of this particular dense -medium process for investigation was entirely a matter of convenience , and reports dealing with other dense -medium systems are planned for the future . Two baths are employed in one of the plants investigated . The first of these , handling 6- to 3 - inch coal , exhibited an exceptionally sharp separation between coal and impurity . This was characterized by an error area of 12 and a probable error of 0.023 . In the second bath , treating refuse from the

Jul 1, 1960

By T. N. McVay

The various applications of beryllium and its compounds in atomic - energy technology and a growing recognition of possible increased utilization of the metal in the aircraft and space - missile fields have resulted in increased interest in domestic and world reserves of beryllium . Unfortunately, little dependable data on beryllium resources and reserves are available , as past consumption of the element has been small and only limited prospecting and exploration work has been done . The scarcity of resource information is attributed partly to the difficulty of recognizing beryllium minerals in the field . These minerals frequently do not have distinctive characteristics of specific gravity, color , or other physical properties , that enable ready identification by the average prospector . This is particularly true of fine - grained minerals . As a result , a simple field test for identifying beryllium- bearing rock is needed . Recognizing this , technologists of the Federal Bureau of Mines investigated several of the proposed qualitative chemical tests for beryllium . This report describes various modifications of one of these methods to make it more suitable for use in the field . In the modified method , duplicate samples are fluxed -- one with potassium bifluoride and one with potassium bisulfate -- followed by dissolution of salts in water , conversion of the solution to an alkaline condition, addition of morin , and examination of the solution for fluorescence under short -wave ultraviolet light . This method provides a fast , dependable field test for beryllium minerals containing as little as 0.2 percent beryl or its equivalent . The test involves no radiation hazards , and it can be performed by persons having no technical training ; therefore , it should be useful to prospectors in discovering beryllium mineralization .

Jul 1, 1960

By E. J. Ostrowski, P. L. Woolf, J. P. Morris, Norwood B. Melcher

By injecting natural gas through auxiliary tuyeres into the smelting zone of the Bureau of Mines ' experimental blast furnace in January 1959 , the investigators succeeded in reducing the coke consumption by approximately one - third that of the base period . This caused a 30 - percent increase in pig iron production with no increase in wind rate . The maximum gas addition in these experiments was 4,665 cubic feet per ton of metal produced . Sharp reduction in gas consumption occurred when high hot blast and high wind rates were used , although the gas injection rate in percent of air blown remained constant . As the heat energy produced by burning natural gas to carbon monoxide and hydrogen is much less than burning coke to carbon monoxide , greater blast temperatures were required during the test runs . The gases produced from the methane were , however , more effective reductants ; so it was possible to increase the production rate while reducing the total heat requirements per ton of metal produced . During a base period with an all - sinter burden , before introduction of natural gas , a coke rate of 1,484 pounds per net ton of pig iron was attained , using an average blast temperature of 1,518 ° F. Gas was introduced gradually over a two -week period until an average 7 percent of the air blown was reached . During this period , the wind rate was adjusted downward to maintain a constant flow of gas in the bosh . The production rate of the furnace remained relatively constant . The quality of pig iron, however , improved as the sulfur load on the furnace was reduced as a result of the substitution of gas for coke . Blast temperatures were increased during this period from 1,518 ° F. to 1,939 ° F. , when the maximum gas addition was reached .

Jul 1, 1960

By J. S. Tosh

The Federal Bureau of Mines has investigated the equilibrium of the system potassium carbonate (K2C03) potassium bicarbonate (KHCO3) potassium bisulfide (KHS) carbon dioxide (C02) hydrogen sulfide (H2S) water (H20). Partial pressures of hydrogen sulfide, carbon dioxide, and water vapor were measured at 70° to 130° C. over solutions of 20-, 30-, and 40-percent-equivalent potassium carbonate containing from 20 to 3,000 grains of equivalent hydrogen sulfide per gallon of solution. This study was made to obtain equilibrium data for evaluating the feasibility of using solutions of hot potassium carbonate for removing, hydrogen sulfide from gas mixtures. The equilibrium partial pressure of hydrogen sulfide may be correlated with the ratio of the molal concentrations of the solutes (KHC03) (KHS)/ (K2CO3). The relationship is shown graphically for the 30- and 40-percent solutions. Once this ratio is determined, the partial pressure of hydrogen sulfide can be obtained from the curves. The equilibrium data show that effective removal of both carbon dioxide and hydrogen sulfide can be achieved simultaneously with hot solutions of potassium carbonate.

Jan 1, 1960

By Carl Rampacek, W. A. McKinney

The feasibility of leaching calcareous and siliceous oxidized copper ores by downward percolation with dilute acid was investigated in the laboratory and in a small continuous plant operated by the Federal Bureau of Mines . The crushed ore was leached in deep columns with solutions containing 1 or 5 percent sulfuric acid to dissolve the oxidized copper . Bench - scale laboratory tests on two calcareous ores from the same deposit indicated that a maximum copper extraction , about 72 percent , could be expected from heap leaching a feed as coarse as 1 inch . Laboratory tests on a siliceous ore showed that almost 70 percent of the copper could be extracted by leaching a 1 / 4 - inch feed . The bench - scale tests were supplemented by larger continuous runs wherein the copper was recovered from the leach liquors by precipitation on detinned scrap iron . Leaching the calcareous ore for approximately 10 days recovered 62 percent of the total copper . The sulfuric acid consumption was 9.6 pounds per pound of copper recovered . Treatment of the siliceous ore recovered 62.5 percent of the total copper in a 2.5 - day leach and the acid consumption was 3.7 pounds per pound of copper recovered . Cement copper products that assayed over 71 percent copper were obtained from the leach solutions by precipitation on scrap iron . The bench - scale and continuous tests demonstrated that downward percolation leaching of the calcareous ores was technically feasible but not economically practicable because of high acid consumption by the gangue . Leaching of the siliceous ore was rapid and the acid and water requirements were nominal . The downward percolation leach procedure is simple and requires a minimum of plant equipment .

Jul 1, 1960

By F. R. Cattoir, D. H. Baker

Fused - salt electrorefining has been successfully applied to the purification of vanadium metal . The electrolyte used in this refining technique was sodium chloride to which had been added 3 to 6 percent vanadium as vanadium dichloride . The average deposition current efficiency was 91 percent . Oxygen and nitrogen , the impurities in commercially produced vanadium metal , were reduced by two - thirds of the amount contained in the feed material . Hardness of the vanadium- metal product was reduced from an initial 97 Rockwell B ( RB ) to a minimum of 35 Rg . The reduction of these impurities markedly improved the plasticity of the final product obtained by melting the crystalline cell metal into small ingots . These ingots could be given a 99 - percent cold reduction by rolling before edge cracking appeared . Growing interest in high - purity vanadium and the industrial need for purer metals and improved alloys for use under high temperatures and high speeds have demanded the elimination and/or control of impurities . Accordingly, research to eliminate or control the undesirable impurities has been expanded .

Jul 1, 1960

By Oren C. Baptist

Umiat field contains the largest accumulation of oil discovered so far in Naval Petroleum Reserve No. 4 in Arctic Alaska. The Umiat anticline was tested with 11 wells; 6 produced oil in varying quantities. Behavior of the wells during testing was unpredictable. For example, one well was abandoned as a dry hole after all tests failed to recover any oil, yet an offset well, only 200 feet from the dry hole, produced 400 barrels of oil a day. The main oil reservoirs are less than 1,000 feet deep and are in the permanently frozen zone (permafrost). Reservoir pressures are low, and most primary production will be by expansion of gas-in-solution in the oil. Because of the unusual reservoir conditions and the difficulties encountered in drilling and completing the wells, the Department of the Navy asked the Federal Bureau of Mines to make laboratory studies of the reservoir sand to determine the cause of well plugging and to provide laboratory information, to be used as an aid in estimating oil recovery from frozen reservoir rocks under solution-gas expansion from low-saturation pressure conditions.

Jan 1, 1960