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By J. P. Capp

This experiment, one of a series on underground gasification of coal, was an investigation by the Federal Bureau of Mines of hydraulic fracturing as a means of increasing the air acceptance of a coalbed to permit introducing combustion air and removing product gases. Specific objectives of the investigation included: (1) Fracturing a coalbed; (2) determining the distance the coal was physically affected; (3) ascertaining the effect of the fracture on air acceptance of the coalbed; and (4) gasifying the coal. The coal was fractured with a fluid consisting of 15,000 lb. of sand mixed with 10,000 gal. of fuel oil and 5,000 gal. of kerosine, injected at pressures up to 900 p.s.i.g. and rates up to 425 g.p.m. The oil served as the fracturing medium, and the sand as a propping agent to hold the fracture open. From the fracture point, (the place in the bed where the fluid was injected), the fracture extended 200 ft. or more along the face cleats, somewhat less along the butt. cleats, and was confined to the coalbed. At the fracture point, the bed accepted about 500 std. c.f.m. of air, which was an etghtyfold increase. Fracture effects were extensive, as airflow was noted from old mine workings and outcrops 600 to 800 ft. from the fracture point. It is probable the actual fracture was much less than 600 ft. and that normal coalbed permeability beyond the fracture limits was responsible for this flow. This indicated that effects of the fracture extended beyond the area of coal physically affected. Although no attempt was made to gasify coal more than 200 ft. away, these effects plus the natural permeability of the bed likely would permit combustion beyond the outer limit of the fracture. As these experiments continued for more than 2 years, and greater air acceptance due to the fracture was observed at the beginning of each test, it is apparent that the effects of the fracturing persist for a considerable time.

Jan 1, 1960

By Robert W. Smith

Computation of the thermodynamic properties of the reaction products in the deflagration of explosive gas mixtures has been a most valuable guide regarding the possible kinetic mechanisms of homogeneous combustion processes. Knowledge of the physically possible end states is indispensable for understanding observed deviations from equilibrium in heterogeneous combustion. However such information on dust flames is entirely lacking. To complement a Federal Bureau of Mines study of stationary graphite dust flames burning in pure oxygen,6/ this report gives examples, at atmospheric pressure and room temperature, of composition profiles in an idealized oxygen-dust flame, with both mass and enthalpy being preserved. Similar profiles can be obtained from the data of the paper for elevated temperature and pressure.

Jan 1, 1960

By R. M. Becker

THIS IS a progress report on a study of the application of statistical practice to mine and mineral sampling undertaken by the Federal Bureau of Mines to provide sound theoretical and practical data for use of the mineral engineering professions. One of the problems in mine sampling is determining the reliability of the results. For certain types of sampling data (random data) the reliability of the results can be stated mathematically. For other types of data there is no known means of quantitatively expressing reliability. In applying measures of reliability to a set of random data, some knowledge or assumption of the characteristics of the particular data is necessary. In many fields these characteristics are well known. However, in mining, where the data are in assays, these characteristics are not well known.

Jan 1, 1961

By R. L. Marovelli

ANTICIPATING the eventual use of the huge tonnages of nonmagnetic taconites of the Mesabi range of the United States, the Federal Bureau of Mines is classifying and evaluating these deposits in detail. This introductory report describes work begun in 1954 as part of a long-range program to sample, classify, and evaluate important occurrences of nonmagnetic taconite on the Mesabi, range. Included in this report are brief discussions of the geology, history, and potential of the Mesabi range district and mining industry, together with a more detailed presentation of the sampling and metallurgical evaluation of these nonmagnetic taconite deposits. A total of 898 field samples was collected. Most of these were taken in the region between Grand Rapids and Chisholm, Minn., but a few came from the area between Chisholm and Buhl, Minn. Of the total samples, 865 were from open pit bank faces where the greater vertical distances presented by the cherty members facilitated the taking of a large number of samples. Conversely, the narrow face presented by the slaty members confined and limited the areas from which samples were taken. In addition, 33 of the field samples were taken from rock dumps in order to determine, in a preliminary way, the characteristics of these materials.

Jan 1, 1961

By E. L. Litchfield

This report of work by the Federal Bureau of Mines has two primary objectives: A survey of the present status and usefulness of the minimum ignition-energy concept, and the presentation of recent data that are believed to bear on the safety problem associated with the ignition of combustible gases by electric discharges. The minimum ignition-energy concept has widespread applicability, especially to safety. The primary obstacle in making theoretical calculations of the requisite ignition energy is the lack of data on chemical kinetics and flame hydrodynamics. The new data on electrical ignition are representative of the great increase in knowledge that can be achieved by proper utilization of geometrical and electrical characteristics associated with the ignition source. CONCEPT OF MINIMUM IGNITION ENERGY The basic concept of a minimum ignition energy (the minimum amount of energy required to cause ignition) follows quite naturally from general physical principles and from the stability (lack of chemical reaction) of the gaseous mixture under the initial conditions. It also follows that if, as a first condition, lossless, instantaneous, and spatially localized energy can be injected and, as a second condition, the relaxation time for conversion of this type of energy to the type required for the reaction is short compared to some characteristic time scale of the ignition phenomenon, the energy requirements will be essentially independent of the type of energy source. Even if condition one cannot be fulfilled, it is sometimes possible to estimate the energy content of the gas required for ignition, and under these circumstances, condition one is fulfilled in effect. There are several instances where results can be interpreted for circumstances that effectively satisfy conditions one and two; these will be discussed later.

Jan 1, 1960

By L. J. Kane

Chemical processes using coal often require economical removal of dust from high-temperature gases. Laboratory-scale investigations by the Federal Bureau of Mines have shown that an aluminum silicate fiber is suitable for filtering dust from gases at 1,800° F. The effects of the bulk density of the filter, rate of gas-flow, concentration of dust in the filter, fiber diameter, depth of filter, and concentration of dust in the feed gas on removal efficiency, pressure drop, and capacity of the filter to hold dust were studied. The laboratory filters were difficult to construct because the fibers were longer than the tube diameter. This caused irregular distribution of fiber that permitted dust-laden gases to leak through channels developed in the filter. Leaks also formed between the filter and the tube wall, but this was minimized by improved filter design. However, edge leaks and leaks through channels in the filter probably would be insignificant in properly constructed filters of industrial size. As the concentration of dust in the filter increased, the efficiency of the low-density filters decreased, contrary to expectations, probably because a higher percentage of the dust passed through channels that developed in the filter. The efficiency of high-density filters, however, increased with the concentration of dust in the filter. Results indicate that loosely packed filters would have a longer life than tightly packed filters at the expense of efficiency. As regeneration or replacement of stationary filters is difficult and expensive, loose filters would be best for filtering gases containing much dust. Gases containing little dust may be cleaned with tightly packed filters to obtain higher efficiency. For either type of filter, precleaning with cyclone separators or other means is advisable.

Jan 1, 1960

By Henry H. Ginsberg

The effectiveness of 0.01 pct. molybdenum, as ammonium molybdate impregnated on coal, on the hydrogenation of a high-volatile bituminous C coal at 8,000 p.s.i.g. and 460° to 480° C. has been studied in a pilot plant by the Federal Bureau of Mines. Under these conditions, the Bureau obtained 98 to 99 pct. conversion5/ of coal to liquids and gases at throughputs of 29 to 101 lb. of m.a.f. coal per cubic foot of reaction space per hour. At 460° C. the indicated yield of oil ranged from 63 pct. (based on m.a.f. coal) at a throughput of 35 lb./c.f.h. (pounds per cubic foot per hour) to 68.5 pct. at a throughput of 58 lb./c.f.h., and the yield of gaseous hydro-carbons ranged from 25.5 to 19 pct. at the same throughputs. The maximum measured yield of oil boiling under 325° C. was 47 pct.

Jan 1, 1960

By Henry H. Ginsberg

The Federal Bureau of Mines made pilot plant investigations of the process requirements necessary to produce heavy fuel oil by the liquid-phase hydrogenation of bituminous coal. The investigation was carried out in three separate series of experiments. The first series studied the effect of temperature and contact time on product distribution at 3,500 p.s.i.g. and 420° to 480° C. in the presence of 0.1 wt.-pct../ stannous sulfide plus 0.05 wt.-pct. iodoform based on gross coal. As a result of increased contact times and temperatures, the conversion-6/ and yield of hydrocarbon gas increased, the viscosity of product oil decreased, and elimination of oxygen, nitrogen, and sulfur from coal increased. The yield of oil did not indicate any definite trend with changes in temperature and contact time. The yield of oil ranged from 76 to 85 pct. for Pittsburgh coal and from 60 to 85 pct. for Rock Springs coal. Asphaltenes in the product oil ranged from 17 to 38 pct. of the total oil for Pittsburgh coal and from 12 to 22 pct. for Rock Springs coal. Fuel oils meeting Bunker C or American Society for Testing Materials (ASTM) Grade 6 specifications were produced with Rock Springs coal at 0.2- to 1.0-hr. contact time and 440° to 480° C. and with Pittsburgh coal at 0.3- to 1.0-hr. contact time and 420° to 460° C. In the second series of experiments tin, nickel, iron, and zinc were evaluated as catalysts for the hydrogenation of Rock Springs coal to heavy fuel oil at 3,500 p.s.i.g. and 460° C. Using the apparent conversion of coal as criterion of catalyst activity, at a contact time of 0.45 hr. tin was the most effective catalyst; nickel and iron were nearly as effective, but the use of zinc resulted in much lower conversion. When the contact time was increased to 0.80 hr., the apparent conversion of coal was essentially the same for each of the catalysts. When the yield of oil boiling below 3550 C. was used as criterion of catalyst activity, at 0.45 hr. the order of activity was tin, iron, nickel, and zinc; at 0.80 hr. tin was far superior and the others were essentially equal. The product oils contained from 8 to 20 pct. asphaltenes.

Jan 1, 1960

By K. C. Dean

A semiquantitative test for the presence and identification of cesium and rubidium in rocks, clays, and mineral waters has been developed by the Bureau of Mines. The test can be used in the field, as a guide for the prospector, geologist, or mining engineer engaged in location or development [w]ork. It comprises two simple spot tests of a solution prepared from the [m]ineral sample. Phosphomolybdic acid, added to a drop of the test solution, [d]etects cesium, rubidium, and potassium in quantities as low as 60 parts per [m]illion. Silicomolybdic acid, added to a second drop of test solution, enables the operator to distinguish between cesium and/or rubidium and potassium. Test procedures, equipment requirements, and limitations of the method are described in this report. Cesium and rubidium were discovered in 1860 and 1861 by Bunsen and Kirchhoff with a spectroscope. The elements usually occur together, particularly in granite and granitic pegmatites. Rubidium does not occur as an essential constituent of any known mineral, yet it is found as a minor element in so many minerals that rubidium is 16th in abundance in the earth's crust. Cesium, which ranks as the 37th most abundant element, is the principal component of pollucite and a minor element in a wide variety of minerals.

Jan 1, 1960

By Alla D. Mah

No experimental heat-of-formation value has been reported in the literature for cerium sesquioxide. The heat of formation of bismuth sesquioxide has not been determined in recent years, and the older value was subject to large uncertainty. Accordingly, the heats of combustion of cerium sesquioxide and bismuth metal were measured by the Federal Bureau of Mines. The heats of formation were: ?H°298.15 = -427.01 ± 0.70 kcal. /mole for cerium sesquioxide and ?H°298.15 = -137.16 ± 0.30 kcal./mole for bismuth sesquioxide. The free energy of formation was estimated for cerium sesquioxide and accurately calculated for bismuth sesquioxide. The data were compared with values in the literature.

Jan 1, 1961

By E. C. Tarpley

The Federal Bureau of Mines has studied solvent extraction as a means of concentrating the mineral components in coal. Solubilities of a number of American coals were determined using abietic acid as a solvent. The effect of rank on solubility was investigated, and maximum solubility was found with coals of intermediate rank. Vitrinite is the most soluble petrographic component; fusinite, micrinitc, and exinite are nearly insoluble. Spore exines also have a low solubility. Abietic acid is a hydrogen donor and reduces pyrite to ferrous sulfide. Mild hydrogenation of high-molecular-weight fragments of the coal structure to those of lower molecular-weight probably contributes to the solvent action. Even where solubility of the coal substance exceeds 90 percent, contamination of the mineral matter with coal makes identification of the mineral components difficult. Further separation might be possible by the application of float and sink techniques to the residue. INTRODUCTION Work n the solvent extraction of coal is conducted to recover commercially useful products and to characterize coal;. and obtain information on their structure. Some coals, particularly those of low rank, contain waxes, resins, and humic acids which can be removed by solvent extraction and find varied industrial uses. In World War II, solvent extraction of coal was conducted on a commercial scale in Germany to obtain a low-ash feed material for hydrogenation and to produce electrodes carbon for the aluminum industry.4 5/

Jan 1, 1960

By R. V. Lundquist

Lime-soda sinters, made and processed for recovering alumina and soda, consisted of several types of compound structures differing from the ideal dicalcium silicate and sodium aluminate. Many or these compound structures were causes for low alumina recovery and contributed to the relation or leach slurries. Presence or free lime, whether in the sinter or released by hydrolysis of sinter compounds, contributed to relation of leach slurries. Free lime tends to establish the initial viscosity assumed by a leach slurry. Previous investigations by the Bureau of Mines (1, 4)4/ and by other laboratories (5) have demonstrated the technical applicability of the lime-soda sinter process to the recovery of alumina from aluminum silicate materials. The basic concept of the process is sintering aluminum silicate materials with limestone and soda ash for the production of dicalcium silicate and sodium aluminate and then extracting the sodium aluminate by leaching the sinter in causticized liquors. Alumina is precipitated from the pregnant liquors by carbonating with carbon dioxide. Reaction in the sintering operation may be represented by the following simplified equation: A1203?SiO + 2CaCO3 + Na2C03 = 2Ca0?SiO + Na20?Al203 + 3C02

Jan 1, 1960

By Charles K. Rose

The Cebolla Creek titaniferous iron deposits near Powderhorn in southern Gunnison County, Colo., were examined by the Federal Bureau of Mines as part of an overall program to investigate the Nation's titanium and iron resources. The deposits occur around the periphery of the Iron Hill stock, which underlies an area of about 12 square miles. Concentrations of magnetite, ilmenite, and perovskite arc localized along fractures in the pyroxenite stock. Mineralogical studies of composite surface samples collected in 1956 showed that most of the iron is present in ilmenite-bearing magnetite. Perovskite is the chief titanium mineral in the magnetite-rich and augite-rich types, and sphene is the principal titanium mineral in the placer material. The mica-rich rock contains approximately equal amounts of perovskite, ilmenite, and sphene.

Jan 1, 1960

By M. G. Zabetakis

At ordinary temperatures and pressures methyl ethyl ketone (MEK)-air mixtures containing between 2.0 and 11 vol.-pct. MEK and methyl isobutyl ketone (MIBK)-air mixtures containing between 1.5 and 7.5 vol.-pct. MIBK are flammable. However, MEK-bromochloromethane (BCM)-air mixtures containing at least 6.2 vol.-pct. BCM and MIBK-BCM-air mixtures containing at least 7.0 vol.-pct. BCM are nonflammable. Also, MEK-BCM-air and MIBK-BCM-air mixtures containing less than 18.7 vol.-pct. oxygen are nonflammable. To assure the formation of nonflammable mixtures when mixed with air, MEK-BCM vapor mixtures must contain at least 1.6 vol. BCM per volume MEK, and MIBK-BCM vapor mixtures must contain at least 2.8 vol. BCM per volume of MIBK; these quantities of BCM would be produced by liquid mixtures containing 55 vol.-pct. BCM in the first case and 60 vol.-pct. in the second. An MIBK-BCM-trimethylene chlorobromide mixture containing equal volumes of each liquid forms nonflammable mixtures with air at ordinary temperatures and pressures. The same is true of a liquid mixture containing 34.6 pct. (liquid volume) BCM, 34.b pct. perchloroethylene, 15.4 pct. MIBK, 7.7 pct. toluene, 3.85 pct. ethyl amyl ketone, and 3.85 pct. trimethylene bromide.

Jan 1, 1960

By W. H. Oppelt

The Federal Bureau of Mines investigated combustion of lignite in domes-tic heating equipment to obtain information on equipment performance and to evaluate testing procedures. Three types of domestic heating equipment were tested, ranging from a hand-tilled, magazine-type space heater to a ram-type overfeed stoker. Lignite was readily burned in each of the three units under various test conditions. Burnoff rates determined by adding weighed charges to the magazine were found to be in error because of shrinkage of the lignite when only a portion of the magazine capacity was consumed during a test. More reliable burnoff rates could be determined by carbon-nitrogen balances. A hand-fired magazine-type space heater (Booker heater) was operated without the furnace attachment at efficiencies to 75 pct. One test series was run with minimum supervision under conditions encountered in actual household operation. No mechanical trouble was encountered.

Jan 1, 1960

By F. R. Cattoir

The Federal Bureau of Mines refined chromium from an aqueous electrolytic process in molten sodium chloride-chromium chloride electrolytes. Oxygen and nitrogen contents were reduced by a factor of 10 to 40, but most other impurities were little changed. The product usually contained a little more iron than the feed. Since iron was entering the bath from the iron pot and the graphite liner at a nearly constant rate, contamination of the chromium deposits by it was more serious at low currents and deposition rates. A few runs in an iron cell with a nickel liner yielded chromium containing one half as much iron as the feed, but up to 1.5 pct. nickel. In all cases the anode feed lay in the bottom of the container, which itself was used as the anode connection. With a 12-in. cell, variations in applied voltage from 0.05 to 1.5, in current from less than 10 to over 100 a., and in initial cathode current densities from less than 100 to over 2,000 a./sq.ft. had little or no effect upon the analysis of the metal produced) except for iron content. Changes in bath analysis from 3 to 11 pct. chromium were also without effect. These changes did bring about large differences in the physical forms of the crystals obtained. The thick heavy crystals produced at low voltage and current contained voids which made them difficult to leach free of chlorides. Easiest to leach were the thin leaf-like crystals obtained at around 1 v.

Jan 1, 1960

By N. E. Hanna

As part of a program for improving, the safety of permissible explosives, the Federal Bureau of Mines has undertaken an investigation to establish the ability of sodium chloride to reduce the incendivity of permissible explosives to firedamp atmospheres. A motivating influence for this investigation has been the comparatively extensive experience of British and other European investigators, who used sodium chloride as a component of their permitted explosives (1, 5, 6 7).5/ In the United States research and development work of this type has been less extensive, although sodium chloride has been added to permissible explosives as a cooling agent (9) for many years. The results of the first phase of this investigation were presented in a previous paper (8), which established that adding up to 10 percent sodium chloride to permissible explosives reduces the likelihood of ignition of firedamp in the gallery test; however, the results were somewhat inconsistent, and the conclusions were qualified. Accordingly, the investigation was continued with a study of the effect of added sodium chloride as a function of the quantity added and of the particle size of the salt.

Jan 1, 1960

By R. V. Lundquist

A method was developed by the Federal Bureau of Mines for evaluating viscosity data from slurries obtained in leaching sinters from the lime soda sinter process for extracting alumina from aluminous silicates. The logarithm of the viscosity was observed to be a linear function with time. The slope of the plotted line provides a means for evaluating viscosity behavior in a lime soda sinter blurry and also a means for comparing gelation characteristics directly with other variables in the lime soda sinter process. This report presents one aspect of a continuing study by the Bureau of Mines on methods for treating siliceous aluminum ores. It is one of the many programs of the Bureau concerned with conservation, development, and use of our domestic minerals resources. Previous investigations of lime soda processes, both by the Bureau4-7/ and industrial concerns, have demonstrated that sintered materials containing CaO, Na2O, A1203, and S102 in various combinations exhibit a tendency to gel or set when mixed with water or other extraction solutions. Gelling prevents satisfactory recovery of alumina and in extreme cases prevents operation of an extraction plant.

Jan 1, 1960

By W. A. McKinney

A sample of oxidized copper ore from a large deposit located in Pinal County, Ariz., about 50 miles northeast of Tucson, was treated by the Federal Bureau of Mines in a small-scale continuous pilot plant by a procedure which comprised acid curing complemented by water leaching and countercurrent decantation washing in a series of drag classifiers. A feed was prepared by pugging minus 1/4-in, ore with concentrated sulfuric acid and about 10 pct, of eater, followed by curing in batches for about 24 hr. The cured ore was fed continuously to a leach drum, where it was mixed with advance solution from the countercurrent washing system to dissolve the sulfated copper. The pulp was thickened and washed in four Esperanza-type classifiers, using a flocculating agent to obtain rapid settling and thickening. The leached ore pulps thickened satisfactorily in the drag classifiers when about 0.8 lb. of a polyacrylamide flocculant per ton of dry feed was used. Clear overflow liquors were obtained, and classifier rake products containing about 60 pct. solids were produced, As much as 90 lb./hr. of ore was treated in the plant, with a recovery of 60 pct. of the total copper or 80 pct, of the acid-soluble copper when 2 tons of water per ton of feed was used in washing. The acid consumption was 4.3 lb./lb. of copper recovered. On the basis of the maximum feed rate employed and the effective pulp-settling area of the classifiers, a total of 1 sq. ft. of pool area was required per ton of dry feed per day for the thickening and washing operations. The washing efficiency in the test was 95 pct.

Jan 1, 1960

By S. L. Ausmus

The work covered in this report is a continuation of an earlier feasibility study by the Federal Bureau of Mines and points out improvements in the skull-melting method for casting reactive metals such as titanium, zirconium, and hafnium. Machined graphite molds with laminated sections can be reused many times. Large tube sections can be produced by spin casting. Graphite powder is the best expendable mold material, but binders for this use must be compounded carefully. The effects of current and furnace atmosphere on the dependent variables of the casting technique are shown. Because of developments in casting technology for titanium which eliminate the basic problems of melting and pouring the metal, opportunities for improvement in the method have increased. The mold material and gate and riser configurations require particular attention. The limits of application of the casting method have yet to be defined. New knowledge in anyone of these areas could result in marked improvements and simplifications in casting methods.

Jan 1, 1960