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By Arnlf Muan, Bert Phillips

The quenching technique has been used for- a study of phase velntiorzs within the composition triangle 2CaO.Fe2O3-FeO.Fe2O3 Fe2O3 of the system Ca-Fe-O. Desired total compositions of sanzples were attained by weighing of starting materials in required proportions and keeping them in sealed 80 pct Pt 20 pct Rh tubes during equilibration .runs. The liquidus surface has been delineated. the existence of two ternary compounds has been established, and seven ternary inwariant situations have been determined. ONE unit within the research program on refractory oxides in progress in our laboratories is the study of phase relations in the system Ca-Fe-Si-O. The present paper deals with the ternary system 2CaOFe2O3-FeO.Fe2O3-Fe2O3, which is only a small part of the enormously complex quaternary system. Many of the phases occurring in iron ore sinter products have compositions which can be closely approximated within this ternary system, and a knowledge of stability relations existing among these phases may be expected to be a useful guide for improving sintering operations. Two fundamentally different experimental approach es are commonly used in studies of systems containing iron oxides, both permitting control of the oxidation state of Fe. One method consists in keeping constant the oxygen partial pressure of the gas phase in equilibrium with condensed phases (liquid and crystalline). In the other method, which is the one used in the present investigation, the total composition of condensed phases is kept essentially constant by keeping the samples in a gas-tight container. The details of this experimental procedure will be described in a later section. PREVIOUS WORK Extensive studies of phase relations in the bounding binary system FeOFe2O3-Fe2O3 have been reported by Greig, Posnjak, Merwin, and Sosman,' by Darken and Gurry,2, 3 and recently by Phillips and Muan.4 A diagram summarizing the results of these studies is shown in Fig. 1. Particular attention is

Jan 1, 1961

By J. W. Town

As part of the Federal Bureau of Mines titanium resources examination program, samples from seven deposits in the Pacific Northwest were tested for amenability to various beneficiation techniques. The samples obtained by the Bureau's Office of Mineral Resources at Spokane, Washington represent a large potential source of titanium. This report summarizes the results of tests at the Bureau's Metallurgy Research Center, Albany, Oregon. Recoveries from tabling placer samples were about 50 percent at grades of 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50 30 percent titanium dioxide. Flotation was the most effective method for concentrating the fine ilmenite in clay samples; recoveries of approximately 50

Jan 1, 1961

By J. J. Wallace

This report describes the initial phase of Bureau of Mines research in the hydraulic mining of bituminous coal. The mining site and equipment are described, and the test procedures and results obtained with a bar-mounted monitor are given. Tests showed that hard Pittsburgh-bed coal can be mined hydraulically from a solid face at water pressures of 4,000 pounds per square inch.4 Coal was penetrated to a depth of 4 feet in 20 seconds with 225 gallons of water per minute coming from a 3/8-inch nozzle at 4,000 pounds per square inch pressure. Some difficulty was encountered in cutting the binders occurring in the coal; it was not possible Lu penetrate directly the overlying draw slate.

Jan 1, 1961

By John Chipman

THE equilibrium between titanium in liquid iron and titanium oxides has been studied by Hadley and Derge.' They have shown that a minimum occurs in the oxygen content of the metal between 0.1 and 1.0 pct Ti, but its exact level was not fixed. The oxide phase in this minimum range was principally TiO, containing some iron oxide. On the other hand, for concentrations above 5 pct Ti the oxide phase was TiO and the oxygen content of the metal increased rapidly with increasing titanium content. From their observations and the free energy of Ti0 and TiOz reported by Kelley and ah,' it is possible to derive approximate values for the activity coefficients of titanium and oxygen in liquid iron-titanium alloys and the conditions for equilibrium in steel deoxidation. Neglecting possible departures from the stoichio-metric composition, the condition of equilibrium with Ti0 may be expressed as follows: TiO= Ti_ + C) log K = log NTl + log [% O] + log yTi + log fQ Here as a matter of convenience the titanium concentration is expressed in mol fraction while that of oxygen is in weight percent. The activity coefficients are yTi and fo. The value of log fo approaches zero as the concentration of titanium approaches zero, while that of log yTi approaches a limiting value of In Fig. 1 the sum of log NTi + log [% 0] is plotted for mol fractions of titanium between 0.05 and 0.50. The smooth extrapolation gives a value of —4.15 which corresponds to log K — log y:i . We therefore have the equation: According to the data of Kelley and Mah,' the free energy of formation of Ti0 at 1900°K is -82,400 cal. The free energy of solution of half a mol of oxygen in iron, taking 1 pct 0 as the standard state, is -29,300 cal. From these we write: From these equations the activity coefficient of titanium at infinite dilution in iron is found to have a value of 0.011 or log y°. = -1.96. This is only an approximate value but is certainly better than the estimated 0.05 in Basic Open Hearth Steelmaking To obtain approximate values for the activity coefficient at intermediate concentrations, it is as- sumed that log yTi(l is constant and equal to -1.96. This corresponds to a value of E;: = 3 In yTi/aNTi = 9.0 which is not unreasonable We now have the value for the activity of titanium and the percentage of oxygen in equilibrium with TiO. It is therefore a simple matter to calculate the activity coefficient of oxygen which is shown in Fig. 2. The effect of titanium is rather large, being comparable to that of vanadium, but not so large as has been reported for aluminum. The slope of the line at low concentrations corresponds to E: = aln yo/ aNTi=-0.37. At concentrations below 1 pct Ti the deoxidation constant and oxygen content for equilibrium with TiO, can be calculated from the foregoing data and the free energy of formation of TiO,, which according to Kelley and Mah is -144,600 cal at 1900°K. The free energy of solution of oxygen has been given; that of Ti to form a dilute solution with 1 pct Ti as the standard state is RT ln (0.5585 y:i/47.9) = -34,800 cal. From these data we find (for concentrations in wt pct): TiO, = Ti + 2 -0; hFTgO0= + 51,200 cal log if =-5.89 The interaction coefficients, concentrations being expressed as wt pct, are e;: = alogfTi/a[% Ti] = +0.048 and e:' = a logfo,/a[ojTi] = -0.187. The calculation gives the following results which, in view of the impurity of the oxide phase, must be regarded as approximate:

Jan 1, 1961

By J. E. Miller

This paper reports experimental determinations by the Bureau of Mines of compressibility factors to 4,000 pounds per square inch absolute (p.s.i.a.) for helium at temperatures from -10° to 130° F. and for 16 helium-nitrogen mixtures at 70° F. This information is needed for computing accurate discharge volumes and is necessary for determining an average-density value for use in orifice-meter formulas. In thermodynamic calculations, several functions of the compressibility factor with pressure and temperature are required. The data in the original publications (6, 8)5 of this study have been reexamined and have been given a more comprehensive treatment. The recalculated compressibility factors are higher by approximately 0.2 percent because in the earlier work a linear relationship between the compressibility factor of helium and pressure was assumed.

Jan 1, 1961

By A. R. Orban, R. B. Engdahl, J. D. Hummell

The initial phase of a research program on smoke abatement from Bessemer converters is described. In work sponsored by the American Iron and Steel Institute, a 300-lb experimental Bessemer converter was assembled to simulate blowing conditions in a commercial vessel. Measurements of smoke and dust were also made in the field on a 30-ton commercial vessel. During normal blows the dust loading from the laboratory converter averaged 0.51 lb per 1000 lb of exhaust gas. This was similar to the exhaust-gas loading of a commercial vessel. The addition of hydrogen to the blast gas of the laboratory converter caused a decided decrease in smoke density. Smoke was also reduced markedly when methane or ammonia was added instead of hydrogen. The research is continuing on a bench-scale investigation of the mechanism of smoke formation in the converter process. DURING the past 2 years, on behalf of the American Iron and Steel Institute, Battelle has been conducting a research program on the control of emissions from pneumatic steelmaking processes. The objective of the research program is to discover a practical method for reducing to an unobjectionable level the emission of smoke and dust from Bessemer converters. PRELIMINARY INVESTIGATION Although conceivably some new collecting technique may be devised which would be economically practicable for cleaning Bessemer gases, no such system based on presently known principles seems feasible because of the extremely large volume of high-temperature gases involved. Hence, the research is being directed toward prevention of smoke formation at the source. A thorough review was first made of former work to determine the present status of the cleaning of converter gases. No published work was found on work done in the United States on collecting smoke or on preventing its formation in the bottom-blown, acid-Bessemer converter. In Europe, however, a number of investigations have been made on the basic-Bessemer converter. Kosmider, Neuhaus, and Kratzenstein1 conducted tests on a 20-ton converter to obtain characteristic data for dust removal and the utilization of waste heat. They concluded that because of the submicron size of the dust, special equipment would be necessary to clean the exhaust gases. Dehne2 conducted a large number of smoke-abatement experiments at Duisburg-Huckingen in a 36-ton Thomas converter discharging into a stack. A number of wet-scrubbing and dry collectors were tried unsuccessfully. A waste-heat boiler and electrostatic collector with necessary gas precleaners was felt to be the best solution for this particular plant. Meldau and Laufhutte3 determined that the particle size was all below 1 µ in the waste gas of a bottom-blown converter. Sel'kin and zadalya4 describe the use of oxygen-water mixtures injected into a molten bath in refining open-hearth steel. They claim that with use of oxygen-water mixtures the amount of dust formed was reduced between 33.3 and 20 pct of its previous level, and emission of brown smoke almost ceased. Pepperhoff and passov5 attempted unsuccessfully to find some correlation between the optical absorption of the smoke, the flame emission, and the composition of the metal in a Thomas converter in order to determine automatically the metallurgical state in the melt. In a recent U. S. Patent (NO. 2,831,762)' issued to two Austrian inventors, Kemmetmuller and Rinesch, the inventors claim a process for treating the exhaust gases from a converter. By their method the inventors claim that the exhaust gases from the converter are cooled immediately after leaving the converter to a degree that oxidation of the metal vapors and metal particles to form Fe2O3 is inhibited in the presence of surplus oxygen. Gledhill, Carnall, and sargent7 report on cleaning the gases from oxygen lancing of pig iron in the ladle. They claim the Pease-Anthony Venturi scrubber removed 99.5 + pct of the smoke, thereby reducing the concentration to 0.1 to 0.2 grain per cu ft, which resulted in a colorless stack gas after the evaporation of water. Fischer and wahlster8 developed a small basic converter and compared the metallurgical behavior of the blow with that of a large converter. Later work by Kosmider, Neuhaus, and Hardt9 on the use of steam for reduction of smoke from an oxygen-enriched converter confirmed that the cooling effect of steam is detrimental to production. From review of all of the published information on the subject, it was concluded that a practical solution to the smoke-elimination problem had not been found. Accordingly, it was deemed desirable to investigate the feasibility of preventing the initial formation of smoke in the converter.

Jan 1, 1961

By H. E. Peterson

Rhenium occurs in very small quantities (12).4 In order for the Federal Bureau of Mines to conduct an investigation of rhenium sources and methods of extraction, it was necessary to devise improved techniques for detecting and measuring minute quantities of the metal. A modification of the procedure of Malouf and White (46) was developed which can be used to detect rhenium in concentrations as small as 0.1 part per million and can be used to measure quantities of 1.0 part per million. It can be used for the analysis of siliceous and calcareous ores, of molybdenite concentrates, of fumes, of flue dusts, and of other metallurgical products. Development of the method involved devising an amine extraction procedure for separating rhenium from all interfering elements except tungsten and a selective distillation procedure for separating rhenium from tungsten. Adoption of these separation procedures permits use of large samples and precise determination of rhenium by colorimetric analysis of the thiocyanate complex of rhenium by means of a spectrophotometer.

Jan 1, 1961

By C. S. Finney, John Mitchell

The decline of the beehive coking industry was inevitable, but it had filled the needs and economy of its day. A beehive plant required neither large capital investment to construct nor an elaborate and expensive organization to run. The ovens were built near mines from which large quantities of easily-won coking coal of excellent quality could be taken, and handling and preparation costs were thus at a minimum. The beehive process undoubtedly produced fine metallurgical coke, and low yields were considered to be the price that had to be paid for a superior product. Few could have foreseen that the time would come when lack of satisfactory coking coal would force most of the beehive plants in the Connellsville district, for example, to stay idle; and if there were those like Belden who cried out against the enormous waste which was leading to exhaustion of the country's best coking coals, there were many more to whom conservation was almost the negation of what has since become popularly known as the spirit of free enterprise. As for the recovery of such by-products as tar, light oil, and ammonia compounds, throughout much of the beehive era there was little economic incentive to move away from a tried and trusted carbonization method simply to produce materials for which no great market existed anyway. With the twentieth century came changes that were to bring an end to the predominance of beehive coking. Large new steel-producing corporations were formed whose operations were integrated to include not only the making and marketing of iron or steel but also the mining of coal and ore from their own properties, the quarrying of their own limestone and dolomite, and the production of coke at or near their blast furnaces. As the steel industry expanded so did the geographic center of production move westward. By 1893 it had moved from east-central to western Pennsylvania, and by 1923 was located to the north and center of Ohio. This western movement led, of course, to the utilization of the poorer quality coking coals of Illinois, Indiana and Ohio. These coals could not be carbonized to produce an acceptable metallurgical coke in the beehive oven, but could be so treated in the by-product oven. By World War I the technological and economic limitations of the beehive oven as a coke producer were being widely recognized. After the war the number of beehive ovens in existence dropped steadily to a low of 10,816 in 1938, in which year the industry produced only some 800,000 tons of coke out of a total US production of 32.5 million tons. The demands of the second World War led to the rehabilitation of many ovens which had not been used for years, and in 1941, for the first time since 1929, beehive ovens produced more than 10 pet of the country's total coke output. Production fell off again after 1945, but the war in Korea made it necessary once more to utilize all available carbonizing capacity so that by 1951 there were 20,458 ovens with an annual coke capacity of 13.9 million tons in existence. Since that time the iron and steel industry has expanded and modernized its by-product coking facilities, and by the end of 1958 only 64 pet of the 8682 beehive ovens still left were capable of being operated. Because beehive ovens are cheap and easy to build and can be closed down and started up with no great damage to brickwork or refractory, it is likely that they will always have a place, albeit a minor one, in the coking industry. The future role of the beehive oven would seem to be precisely that predicted forty years ago by R. S. McBride of the US Geological Survey. Writing with considerable prescience, McBride declared: "A by-product coke-oven plant requires an elaborate organization and a large investment per unit of coke produced per day. Operators of such plants cannot afford to close them down and start them up with every minor change in market conditions. It is not altogether a question whether beehive coke or by-product coke can be produced at a lower price at any particular time. Often by-product coke will be produced and sold at less than cost simply in order to maintain an organization and give some measure of financial return upon the large investment, which would otherwise

Jan 1, 1961

By R. J. Brison, W. C. Bleimeister

The International Salt Company has long been interested in finding an efficient process for the removal of impurities from rock salt, and particularly from the rock salt produced at the Detroit mine. Methods which have been used previously at the Detroit mine included both hand sorting and differential crushing in a Bradford breaker with rejection of the oversize. Neither of these methods was adequately effective. The development of a new process for removal of impurities from rock salt has been described in the preceding article." Basically, the process consists of exposure of crude rock salt to radiant heating which selectively heats the impure particles. Subsequently the heated particles are removed by adhesion to a heat sensitive-coating on a conveyor belt. This method was found to be effective in improving both the quality and appearance of rock salt by the rejection of the dark, impure particles. The first commercial unit employing the new thermoadhesive method of dry separation of minerals was installed at the Detroit mine of International Salt Company in Detroit, Mich. (Fig. l). This unit was first put into operation in March 1957. The purpose of the Detroit installation was 1) to serve as a pilot plant for evaluating the process on a commercial scale and 2) to produce marketable quantities of rock salt of improved quality and ap- pearance. The design of this plant was based on the results and information obtained from a 1-tph pilot plant at Battelle Memorial Institute. DESCRIPTION OF PLANT Location: The separation plant was installed underground near the crushing and screening plant, for this was the most suitable location from the standpoint of material handling. Furthermore, ample space was availabe at this location. Because the process requires a relatively constant temperature, the uniform year-around temperature of the mine (57°F) gave an added advantage to an underground operation. Feeding: The rock salt is conveyed to a surge bin, from which it is fed to the heating unit by a conveyor. The feed-rate control consists simply of an adjustable gate at the bottom of the surge bin. The plant may be fed either No. 1 grade of rock salt (0.279 to 0.375 in.) or No. 2 grade (0.375 to 0.500 in.) with a maximum input capacity of 500 tons per 15-hour day. Heating Unit: The heating unit (Fig. 2) consists of a panel of infrared lamps suspended inside a low-speed revolving screen. The radiant-heat panel, which is curved for most effective utilization of the heat, holds 240 infrared lamps of standard industrial type, each rated at 500 watts. The position of the panel is adjustable so that it can be placed centrally over and to within 6 in. of the salt bed on the screen. The entire heat panel is suspended by rollers in ¦ R. J. Brison and O. F. Tangel: Development of a Thermo-adhesive Method for Dry Separation of Minerals.

Jan 1, 1961

By Stephan I. Zajac, Roger A. Blais, John B. Stubbins

THE iron deposits of central Labrador occur within a relatively small area, herein called the Knob Lake Iron Range, in which a northwest-trending series of low hills and ridges defines the height-of-land at the boundary between provinces of Quebec and Newfound-land. Approximately two-thirds of the deposits are in Quebec and the remainder in Labrador, with several deposits straddling the inter-provincial boundary. These deposits are being exploited in open-pit mines by the Iron Ore Company of Canada centered at Schefferville, Quebec. Since 1954 this company has produced more than 56 million tons of iron ore to become Canada's leading iron ore producer. With indicated reserves of more than 375 million tons of direct-shipping ore and large tonnages of iron formation amenable to beneficiation, this mining district is assured of a long life. This paper describes the Knob Lake iron ores and their geological settings and stresses the features that lead to a better understanding of their origin. The

Jan 1, 1961

By N. J. Grant, Masao Adachi

A number of Cu-SiO, and Cu-A1203 alloys of low oxide content, produced by internal oxidation of copper-silicon and copper-aluminum dilute solid solutions, were exposed at temperatures up to 1050°C for fairly long times to bring about partial or total re crystallization. The creep-rupture properties of these re crystallized alloys were compared to those in the as-extruded condition at 450° C. Some of the alloys were cold worked after re crystallization to note changes in creep-rupture properties, also at 450OC. SINCE the introduction of the SAP alloy in 1949,~ many studies have been carried out on similar oxide and intermetallic dispersion hardened alloys to determine properties and to establish the mechanisms involved in the strengthening process which led to stable, high-temperature behavior.'-' To date, it has been indicated that, however achieved, the structure should be composed of a continuous ductile metal matrix in which is dispersed a fine, submicron size, hard, insoluble second phase (or at least, essentially insoluble at temperatures very near the melting point), with a submicron or near submicron interparticle spacing. Stored energy, obtained by a high strain rate deformation process appears desirable, as an additional strengthening means beyond pure dispersion.=

Jan 1, 1961

By J. A. Boyle

In the Frick District of U, So Steel Corporation, we have had more than 37 years of experience in the use of multiple-fan ventilation systems, in our coal mines. In our Colonial field, with a long belt installation, we have mined 85 million tons of coal with the use of the multiple fan system of ventilation. In our Palmer field, with the use of the same arrangement, we have mined 90 million tons of coal--a total of 175 million tons without one accident attributable to improper mine ventilation. The same system, fundamentally, has been installed in our expanding Robena operations and at its present stage of development we are using eight fans to ventilate this area. To date we have mined 55 million tons of coal with very encouraging results and again without any accidents attributable to ventilation.

Jan 1, 1961

By James Westfield

Following is a brief resume of the Division's activities that have had a favorable effect on health, safety, and the reduction of injuries at coal mines: 1. The Federal Mine Safety Code for Bituminous Coal and Lignite Mines of the United States was issued originally by the Director of the Bureau of Mines on July 24, 1946, after consulting with management and labor representatives of the coal-mining industry. The code has been used by Federal coal-mine inspectors while inspecting bituminous-coal and lignite mines as a basis for determining the existence of unhealthful and unsafe conditions and practices in these mines. A revised code was issued by the Secretary of the Interior on October 8, 1953, after further consultations with representatives of management and mine workers and was incorporated by reference in the 1952 and subsequent bituminous-coal wage agreements. The agreement of May 29, 1946, between the Secretary of the Interior, acting as Coal Mines Administrator under authority of Executive Order 9728, and the United Mine Workers of America, covering bituminous-coal and lignite mines in Government possession, charged Federal coal-mine inspectors with the responsibility of making periodic investigations of the mines and reporting to the Coal Mines Administrator any violations of the Federal Mine Safety Code. Federal coal-mine inspectors also had temporary authority to close mines found to be imminently dangerous, but such authority under Executive Order 9728 was removed on June 30, 1947, when Government control of the mines was terminated.

Jan 1, 1961

By A. W. Ruff

In the last ten years large gains have been made in the field of blasting. These gains have been both in the theoretical and in the practical application of explosives. One of the most publicized changes in the practical application of commercial explosives is the now-prevalent use of ammonium nitrate and fuel oil. The new water-compatible mixture of ammonium nitrate and TNT should also have a large field of application. Most of the theoretical gains have been concerned with the actual rock breakage obtained with explosives. In the last ten years, large gains have been made in the field of blasting. These gains have been both in the theoretical and in the practical application of explosives. One of the most publicized changes in the practical application of commercial explosives is the now prevalent use of ammonium nitrate and fuel oil. The new water-compatible mixture of ammonium nitrate and TNT should also have a large field of application. Most of the theoretical gains have been concerned with the actual rock breakage obtained with explosives. EXPANDING-GAS-BUBBLE THEORY There has been an outstanding change in the conception of how an explosive produces rock failure. The early theory which explained rock breakage was correct for some of the first force-producing agents such as quicklime. When a drillhole was filled with quicklime and water added, the material expanded and steam was generated. The expanding material and the steam exerted a slowly increasing pressure on the sides of the drillhole. The force broke the rock by splitting. Because a great quantity of gas was produced by the deflagration of gunpowder, the same process of the gas pressure splitting the rock was assumed to take place. Even after 80 years of use, the rock-breaking action of all high explosives was thought to be caused entirely by the expanding gas bubble which tore and split the rock. Fig. 1 shows a vertical section through an exploding spherical charge of high explosive. It illustrates the early theory which attributed the entire breakage to the expanding gas bubble. The basic idea of this theory is that the breakage started at the explosive charge and progressed toward the free face. REFLECTED-WAVE THEORY me expanding-gas- bubble theory has gradually been replaced by the reflected-wave theory. The reflected-wave theory explains rock failure by explosives in the following manner: The enormously high gas pressure in the drillhole produces fracturing of the rock on the sides of the drillhole. The fracturing around a 1 1/2-in. diam drillhole is usually confined to an area with about a 6-in. diam. In the fractured area, the pressure of the gas is reduced until the force on the walls is no longer capable of fracturing the rock. Although the gas pressure does not continue to fracture the rock, the pressure imposes a high impact stress on the wall rock. In addition, a pressure or seismic pulse is produced in the rock. The pulse is probably entirely a compression pulse when originally produced in the rock. But, with distance, part of the energy of the compression pulse is transformed into a tension pulse which follows the compression pulse. The explosive charges and burdens used in conventional mine blasting are such that the tension pulse of the original wave is probably too small to be considered in a practical evaluation of the theory. The compression pulse is transmitted through the rock with no associated fracturing.

Jan 1, 1961

By R. W. Lewis

The Federal Bureau of Mines Boulder City Metallurgy Research Laboratory conducted experiments in order to develop a spectrochemical method for determining the concentrations of impurities In high-purity tungsten. This report presents a procedure, developed by these experiments, for determining 19 impurities in high-purity tungsten. Metal samples were thermally converted to the oxide, mixed with graphite, which was prepared and mixed with an internal-standard element, and excited in a d.c. arc. Sixteen of the impurity elements were determined with one set of conditions, using germanium as an internal standard. Lanthanum was used as an internal standard in the tests for boron and chromium. Molybdenum required the substitution of sodium chloride for the graphite and the use of copper electrodes. Data on the precision of the method are included in this report. The coefficients of variation vary considerably but average about 15 percent. Higher concentrations of impurities than those investigated may be determined with some modifications of the testing procedure, provided attention is given to the possibility of interelement interferences.

Jan 1, 1961

By W. M. Dressel

The objective of the research reported in this publication of the Federal Bureau of Mines was to devise a mineral dressing procedure that would concentrate zinc silicate minerals from certain deposits in southwestern Missouri. The best flotation results were obtained by batch laboratory flotation using sulfidizing agents and ethoxylated cocoamine. The flotation concentrate contained 70 percent of the zinc at a grade of 47.8 percent. Gravity concentration tests showed that 55 percent of the zinc could be recovered at a grade of 48.3 percent.

Jan 1, 1961

By Robert K. Koch

The reactions of alumina and alumina monohydrate with wet hydrogen fluoride gas were studied by the Federal Bureau of Mines to determine the feasibility of producing commercial-grade aluminum fluoride from offgases generated by pyrohydrolysis of siliceous fluorspars. The test results showed than an aluminum fluoride reactor operating at maximum efficiency could retain 96 percent of the fluorine contained in off-gases generated by pyrohydrolysis of siliceous fluorspar. The requirements are a reactor temperature of 200° C. and a reactor entrance gas containing 5 mole-percent hydrogen fluoride. Partial pressure equilibrium constants were determined for the reaction of alumina monohydrate and wet hydrogen fluoride gas from 200° to 350° C. and for the reaction of alumina and wet hydrogen fluoride gas from 350° to 700° C. Both reactions are reversible, and they proceed in directions that are dependent upon the temperature and the relative HF:H2O concentration. Logarithms of the equilibrium constants were used to plot the reaction isobars; these can be used to calculate the theoretical maximum efficiency of a reactor processing wet hydrogen fluoride gas between 200° and 700° C. The theoretical maximum efficiency decreases with increasing temperature.

Jan 1, 1961

By D. Bienstock

In connection with air-pollution studies, the Bureau of Mines is cooperating with the U.S. Public Health Service in investigating the use of solids for removing sulfur dioxide in concentrations of less than 0.5 percent from combustion and waste gases. Removal of sulfur dioxide at flue-gas tempera¬tures would no longer result in the cooling of scrubbed gas, which is inherent to liquid scrubbing processes used exclusively in industry today. Results are reported of extensive investigation, using metallic oxides as absorbents, adsorbents, and oxidation catalysts at 130° and 330° C. (temperatures at which flue gas may be treated in powerplant practice). The most active absorbents tested were the oxides of manganese, cobalt, copper, and alkalized alumina; 23 to 33 grams of sulfur dioxidn were removed by 100 grams of absorbent at 130° C., while scrubbing more than 90 percent of the sulfur dioxide from a simulated flue gas, and 19 to 61 grams of sulfur dioxide were removed at 330° C. A more detailed study is reported on absorption and regeneration, using manganese oxides and alkalized alumina. Adsorption of sulfur dioxide on activated carbons and molecular sieves at elevated temperatures is considerably less efficient than removal by absorption--a maximum of 7 to 8 grams of sulfur dioxide could be removed with 100 grams of adsorbent at 130° C. A potash-promoted vanadium pentoxide is effective in converting sulfur dioxide to trioxide; complete conversion in a simulated flue gas containing 0.35 percent sulfur dioxide was obtained at 365° C. Pilot-plant and cost studies are being made by the Bureau to determine the economic feasibility of removing on an industrial scale the sulfur dioxide present in gases in low concentrations.

Jan 1, 1961

By C. E. Westley, R. R. Beebe

Recent works by Plaksh et al.,1,2 Glembotsky,3 and others have renewed interest in the effects of oxidation on the surface activity of the sulfides. Since considerable supporting data are available on galena-potassium ethyl xanthate, this system is being studied at South Dakota School of Mines and Technology by contact angle measurement, using the technique of McGlashan and McLeod.4 The contact-angle method is well adapted to investigation of the influence of small amounts of oxygen on the establishment of a stable contact angle on galena in potassium ethyl xanthate solution. Samples of massive galena containing less than 0.001 pct Cu, 0.001 pct Ag, and 0.01 pct Zn are mounted in castable plastic and ground and polished manually in a glove box containing the desired proportions of oxygen and purified nitrogen. Oxygen and nitrogen contents of the test atmosphere are determined with an Orsatt analyzer. In this way a reproducible surface is created in contact with whatever oxygen concentration is desired. Water and all reagents are prepared and stored in the test atmosphere. An absorbent is used to control carbon dioxide that might be present. Final polishing is done with levigated alumina on a glass plate. The prepared sample is placed in the test solution and transferred to the contact angle apparatus in a sealed box, and the test is conducted while both sample and solution are maintained under a slight positive pressure of the test atmosphere. Table I gives the results of contact angle measurements made at various 02-Nz concentrations.5 Each value of contact angle is the average of at least six individual measurements made with different bubbles at different locations on the sample surface. A period of 20 to 25 min has been found by preliminary tests to be sufficient to permit develop- ment of maximum angle, and all measurements are made after at least this much time has elapsed. Exposure of prepared samples to pure water under the test atmosphere before exposure to the xanthate results in a small but measureable and consistent reduction in contact angle. This is particularly true in the oxygen-deficient atmospheres; for example, at 2.2 pct O2 such water contact reduces the average angle about 8" from that obtained by immediate testing in xanthate. The general trend of increasing contact angle with increasing oxygen concentration corresponds to the results of Plaksin et a12 The absence of diminish-ment of contact angle at very high oxygen concentration has been attributed to the high concentration of xanthate per unit of galena surface: At oxygen concentrations below 1 pct (the limit of accuracy of the Orsatt analyzer), no contact angle is obtained. Furthermore, no contact angle is obtained at any oxygen concentration in the absence of xanthate. This result seems to be in disagreement with those cited by Plaksin.1 Further work on the interaction of galena and potassium ethyl xanthate or a similar collector as influenced by oxygen is contemplated. The true nature of the interrelation is as yet unknown. For example, it is not known whether the governing oxygen reaction is with the mineral, with the reagent, or with both.

Jan 1, 1961

By LeRoy Kienitz

There may be someone here who is not required to run his equipment at its maximum capacity. There may be some fortunate enough to have more crushers than needed, wider conveyor belts than required, and other mill equipment equally oversize. If so, then this paper will have no interest for him; but if most of you are in the situation we in the aggregate producing industry are in, then you probably wish to crowd your mill equipment to its limit. When you do this you must watch for block-up and overloads of all sorts. You need more eyes than you have to guard the critical points. The human eyes that now do nothing much, but watch should be freed for more productive work.

Jan 1, 1961