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By R. Barany

The heats of formation of seven substances were determined by solution calorimetry. At 298.15° K, the heat of formation of lithium sulfate from lithium, rhombic sulfur, and oxygen was -343.1 ± 0.7 kcal/mole, and the heat of formation of lithium sulfate monohydrate from lithium, rhombic sulfur, oxy-gen, and hydrogen was -414.3 ± 0.7 kcal/mo1e. For the silicates, the heats of formation at 298.15° K from the elements were kaliophilite, -503.8 ± 0.5 kcal/mole; leucite, -721.6 ± 0,8 kcal/mole; eucryptite, -505,2 ± 0.6 kcal/mole; alpha-spodumene, -727.9 ± 0.9 kcal/mole; and beta-spodumene, -721.1 ± 0.9 kcal/mole. The corresponding heats of formation at 298.15° K from the constituent oxides were kaliophilite, -42.7 ± 1.1 kca1/mole; leucite, -42.8 ± 1.1 kcal/mole; eucryptite, -16.1 ± 0.7 kcal/mole; alpha-spodumene, -21.0 ± 0.7 kcal/mo1e; and beta-spodumene, -14.3 ± 0.7 kcal/mo1e.

Jan 1, 1966

By A. W. Deurbrouck

The Bureau of Mines analyzed 13 samples collected from three Randolph County coalbeds. The Peerless and Sewell bed samples were generally of metallurgical quality as received from the mines or could be easily upgraded. How-ever, the Lower Kittanning coa1bed samples proved to be quite inimical to upgrading to metallurgical quality.

Jan 1, 1966

By E. K. Kleespies

The Bureau of Mines demonstrated a technique for electrowinning titanium from titanium nitride and titanium dioxide. Titanium-nickel-copper metal solutions containing 26 to 61 weight-percent titanium were prepared by electrolyzing titanium nitride in molten mixtures of potassium fluotitanate) and sodium chloride or barium chloride and depositing titanium on nickel-copper cathodes. A titanium-nickel alloy was prepared by electrolyzing titanium dioxide in an electrolyte of potassium fluotitanate) sodium fluoride) and calcium fluoride and depositing titanium on solid nickel cathodes. This alloy contained 21 weight-percent titanium and had a combined oxygen-carbon content of less than 0.1 weight-percent. A compartmented cell confined the oxide feed near the anode and inhibited oxygen contamination of the metal.

Jan 1, 1966

By Robert K. Koch

The Bureau of Mines investigated separating HF from HF-SiF4-H2O mixtures by passing the mixed gases through a sodium fluoride slurry in an airlift scrubber and forming a mixed precipitate of NaHF2 and Na2SiF6. The oven-dried precipitate was thermally dissociated in two stages. The first stage was carried out at 400° C and dissociated NaHF2 to NaF and HF. Condensation and analysis of the evolved HF proved it to be 97 to 99 weight-percent HF containing 0.79 to 0.99 weight-percent H2O and 10 to 93 ppm silicon. The second stage was carried out at 700° C and dissociated Na2SiF6 to NaF (for recycle) and SiF4. The quantity of HF recovered from gaseous HF-H2O-air mixtures decreased with increasing relative H2O concentrations. Air was beneficial when scrubbing extremely dilute wet HF gases. At HF partial pressures of 0.24 and 0.013 mm Hg in the scrubber entrance gases, HF partial pressures of 6.2 x 10-4 and 9 x 10-6 mm Hg were obtained, respectively, in the scrubber exit gases. Scrubber efficiencies were 99.7 and 99.3 percent.

Jan 1, 1966

By Oliver Q. Leone

Electrorefining tests using titanium-nitrogen alloys as anode material showed that no significant quantity of nitrogen was transferred to the cathode deposit. The nitrogen of the anode remained in the scale, and the titanium-nitrogen alloy was anodically insoluble in the electrolyte when the nitrogen content was 11 weight-percent.

Jan 1, 1966

By Ralph Husack

The Bureau of Mines investigated the effect of gamma radiation on reactions between Pennsylvania anthracite and fluorine and chlorine. In the tests with fluorine about 90 percent of the coal reacted at 350° C to form volatile products whether or not irradiation was employed. Up to 0.8 ml of liquid products per gram of anthracite was collected. Among the 25 com-pounds indicated by gas chromatography, fluoroform and l,l-difluoroethylene were tentatively identified from their relative retention times and perfluoro-cyclopentane from its infrared spectrum. In addition, a clear, hard, wax, probably a fluorocarbon, was formed at 45° C in both the presence and absence of radiation. With chlorine there was no significant difference due to radiation, and preliminary tests indicated that the chlorine reacted more with the organic matter of anthracite at 200° C than with inorganic matter. At 400° C the results were inconclusive because of excessive corrosion in the reaction vessel.

Jan 1, 1966

By G. E. Johnson

Batch tests of coals and coal-derived materials were made by the Bureau of Mines to determine their effectiveness in removing organic contaminants (COD or chemical oxygen demand, comprising those organic compounds that can be chemically oxidized, and ABS or alkylbenzene sulfonate, common household detergents) from the final effluent of secondary-treated waste waters. The adsorptive capacities of flyashes, coals, including at least one sample of each rank found in this country, pretreated coals, and miscellaneous materials including commercial chars and coke, were determined and compared with that of granular activated carbon. The coals, though not as effective as activated carbon, possess an economic advantage--they are relatively inexpensive, and they can still be burned as fuel without any loss of fuel value after use in waste¬water treatment. A hvcb coal was found to be one of the best, having about one-fourth the capacity of activated carbon for COD, adsorbing about 4 percent of its weight before it became saturated. Several coals contained constituents that added to the COD content of the treated water. Thus knowledge of the performance of the coal is necessary to insure selection of a proper coal as adsorbent.

Jan 1, 1966

By Robert W. Ageton

The Bureau of Mines investigated the in situ vertical component of the rock stress in the rib of the haulage drift on the 6100-level of the Star mine, Burke, Idaho, using the flatjack and borehole deformation methods. The estimate of the vertical component of stress about 2 feet into the rib at a station along the haulage drift on the 6100-level of the Star mine by the flatjack method is approximately 5,875 psi, whereas the borehole deformation procedure at this station yielded a value of 5,500 psi for the same depth into the rib. The test zone is approximately 5,625 feet below the surface.No attempt was made to extrapolate stress estimates beyond the depth of the flatjack installation.

Jan 1, 1967

By Thomas R. Bur

The strain and pressure gage methods for evaluating the relative performance of explosives in rock were compared. This comparison was based on a study of the responses of strain and pressure gages to explosion-generated seismic waves. Several explosives) representing a wide range of detonation pressures) were used. In general the relative performance of these explosives) as determined from amplitude) impulse parameter) and energy parameter measurements) is the same if the compressive portion of the strain pulse and the comparable portion of the pressure pulse are considered. Other similarities and differences of the two methods are also discussed.

Jan 1, 1967

By J. A. Ruppert

The Bureau of Mines investigated methods of refining iron-contaminated zinc to marketable quality and developed a laboratory-scale process in which aluminum, added as a refining agent, reacted with the iron, forming solid Fe2Al which floated to the surface of the melt. Solids were separated by both filtration and centrifugation, using a unique type of "dipping" centrifuge devised during the work. Typical zinc recovery was 95 percent, and iron content of the metal was lowered from 0.37 to 0.02 percent.

Jan 1, 1967

By E. A. Sondreal

The Bureau of Mines investigated the use of lignite char for producing carbon disulfide; CS2 production rates were as high as when wood charcoal was used as raw material. The maximum space velocity for CS2 produced in the bench-scale study was 9,280 hour-1, reacting sulfur and lignite char at 792° C. The reaction temperature and the temperature at which the char was carbonized were the two most important factors in determining CS2 production rates. Increasing the carbonization temperature in nitrogen from 400° to 900° C advanced the temperature at which carbon disulfide was first produced from 550° to 850° C. The average activation energy for reacting chars with sulfur was 44,000 cal/g mole. The reaction was first order with respect to the partial pressure of sulfur. Increasing the rate of sulfur admission caused a decrease in rate of production at otherwise similar conditions. Rates were not affected by either char size or sodium carbonate catalysis. High space velocities at moderate temperatures using inexpensive lignite chars could offer an economic advantage in the manufacture of carbon disulfide provided that yields were attractive.

Jan 1, 1967

By Ernest L. Corp

First in a projected series on the use of flexible liners for support of underground mine openings, this report presents information obtained from an extensive review of the literature on this subject. It also includes results of some preliminary test work by the Bureau of Mines. Investigations thus far indicate that flexible liners offer numerous advantages over rigid-type sup-ports, By deforming in the direction of the applied stress, the stresses are redistributed from the liner to the surrounding material. The corresponding buildup of passive resistance in the direction of diametric extension causes an equalization of stresses around the liner, thereby enabling the liner to carry loads in a more efficient manner. However, additional experimental data are needed to establish design criteria that will permit maximum utilization of the flexible liner concept in mining. Testing of small-scale models, accompanied by measurement of free-field stresses in material surrounding the model, is recommended as the most suit-able approach to the problem. The experimental procedures necessary to such an approach are outlined in detail and a statistical design for the experiments is proposed. The report also describes a device developed by the Bureau for measuring free-field soil pressures to 1,000 psi and a technique for evaluating the response of the device.

Jan 1, 1967

By Robert E. Wood

The compressibility factors, Z, of helium, nitrogen, and helium-nitrogen mixtures in the three-dimensional space of temperature, pressure, and gas composition have been related to the Leiden form of the virial equation of state. The dependency of virial coefficients through the fifth on temperature and gas composition has been established for the temperature range 133.15° to 748.15° K. Compressibility factors, Z, have been computed from the equation of state and tabulated as functions of gas composition, pressure, and temperature. Tabular values of Z are presented for 30.00 through 100.00 percent helium for temperatures from 240° through 700° R for pressures from 14.696 through 3,050 psia and for temperatures from 720° through 1,300° R for pressures from 14.696 through 1,500 psia. Tabular values of Z are presented at increments of 5.00 percent helium and 20° R, and, for pressures greater than 50 psia, at increments of 50 psi.

Jan 1, 1967

By D. E. Wolfson

The Bureau of Mines carbonized 35 coal samples from Logan and Mingo Counties) W. Va., at 900° C using the Bureau of Mines-American Gas Association method, and determined yields of products and physical properties of cokes. Twenty samples represented the No.5 Block, Stockton, Chilton, Cedar Grove, Lower Cedar Grove, Alma, No. 2 Gas, and Eagle beds in Logan County, and 15 samples represented the Coalburg, Buffalo Creek, Winifrede, Cedar Grove, Lower Cedar Grove, Alma, and No.2 Gas beds in Mingo County, W. Va, Chemical analyses were determined for all coals. All coals in both counties rank as high-volatile A bituminous. Most of the coals are chemically suitable for metallurgical coals. Coals with accept-able ash and sulfur contents can be used as major constituents in coking blends with higher rank coal to yield coke with satisfactory properties for blast furnace use.

Jan 1, 1967

By F. X. Tartaron

Behavior of hard-burned quicklime was compared with that of soft-burned quicklime in an oxygen converter utilizing oxygen blowing in a rotating cylindrical vessel, set at a 30° to 60° angle to the horizontal and operated at a predetermined speed of rotation. Four pairs of tests were made) each comparing hard lime with soft lime. Three of the pairs differed from one another in the quantity of lime employed) and the fourth differed in blowing time, All four pairs showed an increase in yield when soft lime was used. Three of the pairs revealed that the ratio of the oxygen consumed with soft lime to the oxygen consumed with hard lime was the same as the ratio of metal yield with soft lime to the metal yield with hard lime. The fourth pair contained an error and could not be included. Finally, a close inverse relation was found between the combined iron in the slag and the combined lime in the slag, which can be expressed by the equation pct Fe = 52.67 -0,906 (pct CaO).

Jan 1, 1967

By R. W. Van Dolah

The Bureau of Mines t.ced its investigations into sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) to define the scaling law for safe separation from detonating AN-FO. Both missile- and non-missile-producing AN-FO donors, weighing up to 5,400 pounds, were employed with acceptors of the same size. The usual cube-root scaling law was not confirmed; exponents for the relationship S = f(Wx) for AN were 0.51 with non¬missile-producing donors and 0.61 for missile-producing donors. For AN-FO an exponent of 0.80 was indicated in the missile-producing case. AN-F0 in polyethylene bags appeared somewhat more easily initiated than bulk AN-FO. The efficacy of barricades in protecting AN charges was investigated. detonation distances were reduced from one-third to one-seventh when filled barricades were employed. The investigation was extended to dynamite with both types of donors. With 1,600-pound missile-producing donors and an equivalent weight of dynamite, initiation would be expected in 50 percent of the trials at 167 feet. The corresponding value in the non-missile case was 67 feet. The data developed in this program of sympathetic detonation will allow the development of a rational set of safe separation distances for AN, AN-FO, and explosives.

Jan 1, 1966

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindablity index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions3 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous of coal as delivered is a check on the practical results obtained in the coal.

Jan 1, 1967

By H. G. Iverson

Solid state reactions of manganese with silica were investigated in high-temperature tests. Reactions of 0.5 to 4.0 moles manganese (Mn) with 1 mole silica (SiO2) at 1,100° C and of 2.0 Mn:SiO2 mole-ratio mixtures at 1,000° to 1,150° C yielded products consisting of a slag phase and a metallic phase. At 1,100° C, the slag phase from reactions of the low Mn:SiO2 mole-ratio mixtures was composed of SiO2 and rhodonite (MnSiO3), and the slag phase from the high Mn:SiO2 mixtures was composed of MnSiOs and tephroite (Mn2SiO4). The metallic phase from the corresponding low Mn:SiO2 mole-ratio reactants consisted of two manganese silicides, Mn5Si3 and Mn3Si; from the high Mn:SiOg mixtures, it was Mn and the manganese silicide (Mn5Si). For the higher mole ratios of MnSiO2 the manganese content in the metallic phase increased, while the manganese and silica contents of the slag phase remained nearly constant. The slags did not contain free or uncombined manganese oxide (MuO). For the 2.5 to 4.0 Mn:SiO2 mole-ratio mixtures reacted at 1,100° C, the maximum quantities of silica reduced and of the manganese in the slag appeared to become asymptotical at about 41 and 48 percent, respectively. A brominating procedure was developed that was highly selective in removing the metallic constituents from the reaction product, leaving the slag phase as residue. X-ray diffraction patterns were obtained on prepared silicides Mn5Si, Mn3Si, and MnSi.

Jan 1, 1967

By Murray Weintraub

In an investigation of the incineration of combustible wastes, the Bureau of Mines studied the effect of dimensional parameters, process variables, and fuel properties on the operation of an incinerator that consisted of a single cylindrical combustion chamber in which all combustion air was supplied tangentially above the fuel. Construction and operation of three designs of such a device proved that the tangential overfire air design is effective in providing efficient combustion and low concentration of particulate matter in the effluent gas. A correlation was found that related burning rate with air rate, chamber diameter, and inlet port diameter. In one of the incinerator models, ignition was by radiation from a preheated surface. The temperature of this surface was required to be 1,400° to 1,600° F to insure ignition of moist refuse; however, this had little effect on combustion rates. In the combustion of moist refuse, evaporation of the water proceeded through the fuel bed as a wave, with an ignition wave following the evaporation.

Jan 1, 1967

By C. Q. Cupps

n view of increased interest in secondary recovery of oil in the Cut Bank field, Montana, a review has been made of unpublished data obtained during a 1943-44 study of reservoir oil characteristics in this field. Considerable uncertainty was attached to interpretations of subsurface oil sample analyses from six Cut Bank zone wells, one Lander sand well, and one Moulton sand well, because of adverse sampling conditions and wide range in the data. Much of this uncertainty has been removed by this review which has shown two of the Cut Bank zone samples and the Moulton sand sample to be representative of the reservoir oils. Estimates of original reservoir oil characteristics derived from differential-liberation analyses of these samples show that the oil in the Cut Bank zone was initially saturated at the gas-oil contact pres-sure, 750 psia, and the oil in the Moulton sand was undersaturated with a saturation pressure of only 380 psia. The rest of the samples were indicated to be nonrepresentative of the reservoir oils because of a disproportional vaporization of heavier components of the solution gas. The vaporization of these components is believed to be a cumulative effect of contact of the oil with bypassing, light-gravity gas which had been liberated at higher pressures from solution in oil farther back in the formation, or which had come from the gas cap, rather than from the singular effect of gas evolution caused by excessively low bottom-hole pressures. Change of oil composition caused by the latter was found to conform closely to that occurring during a differential liberation of gas in the laboratory.

Jan 1, 1967