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By A. R. Taylor

This report describes the design, construction, and operation of a low temperature adiabatic calorimeter for measuring heat capacities of solids or liquids from 60° to 300° K. A brief discussion of the basic theory involved in chemical thermodynamics and the problems involved in obtaining accurate experimental data is presented. The operation of the calorimeter was tested by measuring the heat capacity of a sample of benzoic acid obtained from the National Bureau of Standards over a temperature range of 60° to 300° K. The measured heat capacity values of the benzoic acid compared favorably with similar values obtained by the Bureau of Standards, the maximum deviation being 0.5 percent. THEORY A brief discussion of the basic theory involved in chemical thermodynamics will illustrate the applications of heat capacity data and the problems involved in obtaining accurate experimental data.

Jan 1, 1962

By Maria I. De Rosa

The U.S. Bureau of Mines performed experiments to determine the hydrogen cyanide (HCN) concentrations and smoke particle characteristics during the combustion of flexible polyurethane foams and other nitrogen-containing materials, for the development of a test parameter. The experiments were conducted in an approximately 2O-L furnace at set furnace temperatures of 250° and 1,000° C for a 14-min duration, with an airflow through the furnace of 10 L/min. The variables studied as a function of time were the gaseous and aerosol HCN concentrations, the smoke particles average diameter (dg) and particle concentration (no), and the product of the smoke particle diameter and concentration (dgno). Carbon monoxide, carbon dioxide, and oxygen concentrations, sample mass weight loss, and furnace temperatures were also studied; analyses of nitrogen and cyanate content of the material were carried out. Results show that dgno correlates directly with the HCN concentrations, which depend on the nitrogen and cyanate contents of the material.

Jan 1, 2010

By K. E. Soroka

More than 500 fires are now burning in abandoned coal waste banks and coal deposits in the United States. Once established, such fires can burn for decades, and extinguishing them by conventional methods such as surface sealing to exclude air, excavation to remove fuel, or flushing to cool the fire zone is usually difficult and always expensive. Burnout Control, a technique developed by the Bureau of Mines for the control of abandoned coal fires, involves the accelerated combustion of coal in place with total management of the heat and fumes produced. A burning waste bank or mine is placed under negative pressure relative to the atmosphere, and heat and combustion products are drawn from the combustion zone through an exhaust ventilation system. Heat produced appears as sensible heat in the exhaust, at temperatures as high as 1,0000 C (1,832° F), and could be recovered for the production of steam, hot water, process heat, or electricity. The Bureau's first held field demonstration of Burnout Control was at Calamity Hollow in Allegheny County, PA (near Pittsburgh). Calamity Hollow was the site of an underground mine in the 1900's and was surface mined in the 1940's. In the winter of 1961-62, a fire of undetermined origin was discovered in the exposed coal. In 1963, the Bureau constructed a trench barrier around the fire and a surface seal over the affected area. The fire was isolated but not completely extinguished. In 1979, when the Bureau began work on the Calamity Hollow Mine Fire Project to demonstrate controlled burnout, the fire was still smoldering on the hot side of the trench barrier. The project, which was begun in December 1979 and ended in July 1982, consisted of the design, construction, operation, and subsequent dismantling of a Burnout Control ventilation system. This report is the fifth in a five-part series that describes the Calamity Hollow Mine Fire Project. The first report, part 1, describes the design and construction of the field installation. Part 2 will present the results of a continuous 4-month burnout operation. (Because part 2 involves the analysis of a substantial body of data, it will not be published until after publication of parts 1, 3, 4, and 5.) Part 3 describes the instrumentation used to control and monitor the progress of the burnout operation. Parts 4 and 5 deal with the closeout phase of the field demonstration. Part 4 describes the procedure used to quench the fire, and this part (part 5) describes the final excavation and backfilling of the heated zones. The reports in this series document the Calamity Hollow controlled burnout demonstration which showed that (1) controlled in situ combustion is a feasible method for controlling underground fires in abandoned mines, (2) the resultant thermal exhaust output is sufficient for energy utilization, and (3) water injection-fume exhaustion is a potentially effective method for cooling large underground fire zones. Further investigations of both Burnout Control and the water-injection-fume exhaustion quenching procedure are planned.

Jan 1, 1986

By H. M. Harris

The Bureau of Mines investigated chlorination of domestic ilmenites in a fluidized coke bed at temperatures of 950° to 1,150° C. Objectives were to develop an effective process for producing TiC14 suitable for TiO2 pigment and to reduce pollution by collecting and treating waste byproduct chlorides. The reactor for these tests was a 10.2-cm-diam quartz tube heated externally by electrical resistance heaters. It contained coke beds of from 35.6 to 82.5 cm in depth that were fluidized by 13 to 25 l/min of chlorine. Ilmenite concentrate powders were introduced at the bottom of the fluid-bed reactor, using the chlorine gas stream as a carrier. Test results showed that greater than 90 pct of the ilmenite reacted at optimum conditions and recovery of TiC14 ranged from 95 to 99 pct of stoichiometric. A temperature-controlled cyclone was used to remove high-boiling-point chlorides such as MnCl2, MgCl2, and FeCl2, and also collected fine unreacted ilmenite and coke dust. Impure TiC14 and FeC13 were separated by collecting the, iron chloride in a condenser con-trolled at 200° C. Titanium tetrachloride vapor was cleaned by passage-through a salt-column filter followed by condensation in water-cooled and refrigerated condensers. Liquid TiC14 was purified further by well-known industrial methods to meet specifications for pigment-grade chloride. Integrated tests were conducted in which chlorine, produced by dechlorination of FeC13 with oxygen, was recycled and used directly in a fluidized-bed chlorinator.

Jan 1, 1976

By P. L. Woolf, N. Bernstein, M. M. Fine

Continuous experimentation utilizing a 3- by 36 - foot rotary kiln was conducted to demonstrate the feasibility of simultaneous induration and reduction of magnetic taconite concentrate . Lignite , or lignite - anthracite mixtures , and green magnetite pellets (64.2 percent Fe , dry basis ) were heated in a rotary kiln to about 2,100 ° F. After separation from excess reductant , the product pellets were found to be highly reduced and acceptably hard . A total of 140 tons of prereduced pellets with an average Fe content of 79.0 percent was produced at Minneapolis and smelted in the Bureau's experimental blast furnace at Bruceton , Pa . Two additional supplies of prereduced pellets were obtained from The Steel Company of Canada , Ltd. , Hamilton , Ontario , which contained 83.8 and 91.3 percent Fe , respectively . Smelting of prereduced pellets was compared with that of unreduced pellets obtained from The Hilton Mines , Shawville , Quebec , and from the Erie Mining Co. , Hoyt Lakes , Minn . Blast furnace tests established that a substantial decrease in coke rates and higher production result from the use of prereduced pellets .

Jan 1, 1964

By E. O. Binyon

"Corundum and andalusite were discovered in August 1944 on what is now known as the Blue Metal group of claims. The property, comprising five unpatented lode claims, is situated 20 Miles northwest of Yerington in the Buckskin Mining District, Douglas County, Nevada, An engineer of the. Bureau of nines examined the property on November 1, 1944, and recommended a small: amount of drifting and crosscutting to determine more definitely the extent and character of the ore deposit. The work that had been done by the owners was for sampling purposes only and was confined to a few small pits on the outcrop, and no effort had been made. to delimit the ore zone. Samples taken from the best surface showings were sent to the experimental station in Salt Lake City for beneficiation tests. The results of the preliminary test work appeared favorable, and upon the strength of them and the recommendations made by the Bureau, 2.5 miles of access road was approved and completed early in 1945. Exploration was started on June 24 and completed September 26, 1945.In its program of exploration of mineral deposits, the Bureau of Mines has as its primary objective the more effective utilization of our mines resources to the end that they make the greatest possible contribution to national security and economy. It is the policy of the Bureau to publish the facts developed by each exploratory project as soon as practicable after its conclusion. The Mining Branch, Lowell B. Moon, chief, conducts preliminary examinations, performs the actual exploratory work, and prepares the final report. The Metallurgical Branch, R. G. Knickerbocker, chief, analyzes samples and performs beneficiation tests. Both these branches are under the supervision of Dr. R. S. Dean, assistant director.This paper is one of many reporting on various aspects of the Bureau of Mines program initiated in August 1939 by passage of the Strategic Minerals act, the scope of which was. greatly expanded by subsequent legislation.Some of these papers were published as war minerals reports, others as bulletins, technical papers, reports of investigations, and information circulars of the Bureau of Mines or• in, technical journals.The Bureau's program at first included separate investigations by the Mining and metallurgical Divisions, but these were consolidated under Assistant Director R. S. Dean beginning July 1, 1942. Mining and metallurgical investigations carried on in three regional organizations more closely integrated thereafter by a staff of specialists, who reviewed findings made in the field and in Bureau Laboratories, considered proposals for additional work, revised reports for publication, and served as advisors to the assistant director."

Aug 1, 1946

By John C. Edwards

The Bureau of Mines developed a mathematical model to predict the oxygen requirements for a miner evacuating a mine. The model accounts for variations in the miner's escape speed with mine airway height, and for the empirically determined expressions for the weight-specific oxygen uptake rate for upright walking, stooped walking (duck-walking), and crawling. A Fortran computer program that is user oriented was prepared based upon the model's constitutive equations. Specific instructions for utilizing the program, as well as applications to miner evacuation from a mine, are presented.

Jan 1, 1986

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 D. L. Paulson

Electric furnace smelting of blister copper directly from copper precipitates (cement copper) was investigated by the Federal Bureau of Mines. Copper concentrations in five different lots of cement copper in the investigation ranged from 62.5 to 82.5 wt-pct. Laboratory-scale smelting tests were made in a 50-kva electric-arc furnace to establish the reductant and flux requirements. Best recoveries were realized by adding 60 pct of the carbon required to combine with the contained oxygen in the cement copper. Operating parameters established during the laboratory-scale smelting tests were used successfully in smelting 20 tons of cement copper during 12 pilot-scale tests in an 800-kva electric-arc furnace. Over 98 pct of the contained copper was recovered as blister-grade metal. The projected energy consumption for a commercial-size furnace was 380 kwhr per ton of cold charge.

Jan 1, 1978

By George L. Gates

It is generally recognized that if the lose and contamination of the fluid content of a core specimen from an oil- and gas-bearing formation in a well were eliminated, the value of core analysis would be increased greatly. In an effort to obtain uncontaminated cores, extensive field tests were carried out in the Mercy field, San Jacinto County, Tex., with the Carter pressure core barrel and an oil-base drilling fluid having very low rates of filtration as measured by the standard A.P.I. drilling-fluid filter teat. A tracer was added to the drilling fluid filter test. A tracer was added to the drilling fluid to provide a means for quantitatively measuring the volume of oil filtrate in the cores. Unfortunately, as stated in the report on the Mercy tests, very little oil nand was penetrated in coring the well; and because the performance of the pressure core barrel was not entirely satisfactory, the tests did not provide a complete answer to the question: Does a filtrate from an oil-base drilling fluid enter cores., and how does it affect the results of the core analyses?

Jan 1, 1950

By R. W. Van Dolah

An investigation was made of the distances over which sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) might be expected. Large-scale gap tests used two types of AN-FO donor charges in three sizes with AN, both at ambient and elevated temperatures, and AN-FO acceptor charges. Donor sizes were varied to test the validity of a scaling law commonly used in quantity distance tables. The up-and-down experimental design was chosen to determine the 50-percent initiation point efficiently. The acceptor charges were instrumented to indicate initiation and to determine detonation velocity. Other electronic techniques for measuring the rate of growth, stability of detonation, and detonation pressures were employed. Air shock and fragment velocities between charges were measured by electronic and photographic methods, and determination of side-on air-blast pressures and impulse duration were made for about half the shots. Separation distances between donor and acceptor were found to be larger than anticipated both for the AN and the AN-FO. With AN-FO acceptors and a 16-gage steel faced donor, one initiation occurred at a separation of 53 feet or nearly 16-charge diameters; with AN, initiation occurred at 4 to 5-1/2- charge diameters.

Jan 1, 1966

By Edward L. Tullis

Numerous widely distributed pegmatites of the southern Black Hills of South Dakota contain small amounts of beryl, and two minor deposits are known in the northern Black Hills. Few mines have produced more than 50 tons, and the current, rate of production for the area is about 100 tons annually. Total production, since the first records, is 2,358 tons. Most of the deposits contain less than 1 percent beryl, although the beryl zones in several deposits contain 2 percent beryl or more. Estimated reserves of beryl total 11,824 tons, and an additional 234 tons has been measured; there are other unestimated reserves. The pegmatites are in a belt about the margin of the Harney Peak batholith in the southern Black Hills, although they fail into three districts. The most important, from the point of view of production and reserves, is the Keystone district. Many deposits also are found in the vicinity of Custer and Pringle. Small amounts of beryl occur in the dikes near Hill City. A little beryl has been produced from the Tinton district in the northern Black Hills, and an undeveloped dike has been discovered on Whitewood Peak near Deadwood. The beryl-bearing pegmatites are principally coarse-grained intergrowths or massive segregations of feldspar, quartz, and mica. Some of them contain notable amounts of lithium minerals, as well as some tantalite, columbite, and cassiterite.

Jan 1, 1952

By Robert Lee Stahl

Comprehensive field tests were made in the Gas Hills, Wyo., to determine whether surface geophysical techniques could be used to detect and delineate faults in marginal uranium deposits. The tests were made on property owned by Federal American Partners, Gas Hills, Wyo., and included seismic refraction, self-potential, induced polarization, magnetometer, electrical resistivity, airborne infrared thermal scanning, and airborne photography. Of the several geophysical techniques tested in the field, horizontal resistivity profiling with electrode spacings in the range of 25 to 50 feet was most diagnostic of faults. The method is quick, cheap, accurate, and one that can be easily used by personnel employed by mining companies to detect and delineate faults.

Jan 1, 1973

By J. B. Zink

The Bureau of Mines developed a spectrochemical method to determine six constituents in coal ash in the following concentration ranges: silica 9 to 63 percent, alumina 7.5 to 35 percent, ferric oxide 2 to 30 percent, calcium oxide 1 to 29 percent, magnesium oxide 0.5 to 6 percent, and titanium oxide 0.5 to 4 percent. Samples of coal ash are fused with a mixture of lithium tetraborate and vanadium pentoxide. The resulting beads are crushed, mixed with powdered graphite, and briquetted. The pellets are analyzed spectrographically, using controlled high-voltage spark excitation. Vanadium serves as the internal standard. Effects due to matrix variations are minimized by fusion with lithium tetraborate. Intensity ratios of selected analytical lines are determined photometrically, Concentrations are read from analytical curves, prepared from synthetic standards, relating log intensity ratios to log concentration. A combustion procedure is used to determine sulfur tri-oxide. The method is most useful when large numbers of coal ashes must be analyzed but a high degree of accuracy is not essential.

Jan 1, 1967

By J. P. Powell

The application of secondary producing methods for recovering additional oil from known fields has been recognized for many years as important to the economy of the nation. One of the most successful secondary methods is waterflooding, which conserves our natural resources by preventing premature abandoment of stripper leases and revitalizing previously abandoned areas. Waterflooding as a secondary-recovery method was introduced into the Midcontinent region in 1931, and its use as such has become widespread. As with most new methods, the most favorable fields and leases received primary attention, whereas those with viscous oil or less favorable sand characteristics were bypassed. Numerous reports3 4 5 6/ have been published giving the results of individual waterflooding projects, In this report, attention is directed to the effect of a single factor, the viscosity of the oil produced,

Jan 1, 1959

By A. S. Swanson

The Babb fault vein in Crittenden and Livingston Counties, Ky. (fig. 1), is one of an extensive series of such veins in the Western Kentucky and Southern Illinois fluorspar district. First operated in 1904, the production to May 1, 1944, was estimated at 143,000 tons of fluorite ore. There are five mines (fig. 2) on the Babb fault zone - Guill ,Kentucky Babb, Delhi-Babb, Eagle-Babb and Howard-Barnes. The Bureau of Mines developed four of these properties by core drilling from July 9, 1943, to May 1, 1944. During that period a total of 8,177.8 feet of diamond drilling was completed in 28 holes.

Jan 1, 1950

By H. S. Auvil

[Coals of low-volatile rank cannot be coked without admixing large proportions of high-volatile coal in the usual type of byproduct-coke oven, because they expand excessively and exert side thrust, which ruins the oven walls. Some medium-volatile coals also give trouble. Since high-rank coals produce a strong, blocky coke, it is desirable to have the rank as high as practicable, particularly in the manufacture of foundry coke. Accordingly, it has become the practice to mix or blend high-volatile shrinking, coals with as much low-volatile coal as possible and still have a mixture that will not deform the walls or cause difficulty in pushing the coke. Occasionally, the safe limit of low-volatile coal has been exceeded and ovens have been damaged. It is desirable, therefore, to rave a reliable method of determining the expanding tendencies of mixtures before they are charged into the ovens. Furthermore, coal charges somewhat in its properties as mining progresses, and therefore, mixtures found to be safe at one time may cease to be so subsequently, particularly if nearly the maximum allowable percentage of low-volatile coal is being used.]

Jan 1, 1938

By Robert H. Townsend

The following paper discusses the mining, transportation, and crushing methods, with costs, at the San Andreas plant of the Calaveras Cement Co. It is one of a series, prepared for and published by the U. S. Bureau of Mine describing methods used in cement-rock quarries throughout the country. These papers are designed to disseminate technical information regarding the methods used. The cost tabulations represent operating expenditures only and not total cost. It is recognized that publication of total costs mightin some instances cause embarrassment to individual producers as well as to the industry as a hole. On the other hand, operating costs are essential to the technical discussion and study of the methods employed. The attention of the reader is specifically called to this differentiation in order that no misunderstanding of the scope of the cost-tabulations shall ensue.

Jan 1, 1933

By A. F. Baker

Laboratory flotation of synthetic coal-pyrite mixtures and high-pyritic-sulfur coal indicated that ferric chloride (FeCl3), aluminum chloride (AIC13), chromium chloride (CrCl3), and cupric sulfate (CuSO4) are potential pyrite depressants. For each metal salt there appeared to be a range of pH values and optimum concentration for selectively depressing pyrite in coal flotation. Pyrite was depressed in the pH range from 4.5 to 7.0 with ferric chloride, from 5.8 to 7.0 with aluminum chloride, from 6.4 to 7.1 with chromium chloride, and from 6.4 to 7.4 with cupric sulfate. Best separation of pyrite from coal was achieved in flotation solutions containing from 2 X 10-5 to 5 x 10-5 mole/ liter of each salt. In solutions containing excess salt concentrations, coal was also depressed. These Bureau of Mines tests demonstrated on a laboratory scale that, in solutions containing 4 X 10-5 mole/liter ferric chloride and from 1 x 10-4 to 2 x 10-4 mole/liter sodium hydroxide, the pyritic sulfur content of a Lower Freeport bed coal sample could be reduced from about 2.51 percent to less than 0.60 percent with recoveries of over 83 percent. The depression of pyrite appears to be due to the adsorption of positively charged colloidal metal hydroxide at the pyrite-solution interface. This hypothesis is supported by zeta potential determinations which showed that suspended coal and pyrite particles in solutions containing metal salts are positively charged in the pH range where depression occurs.

Jan 1, 1971

By M. S. Seehra, R. S. Pandurangi

"The interaction of amorphous silica particles with several hydrogen bonding agents (H2O,, C2H,OH, C,H,NO) was investigated by monitoring the changes in the bulk and surface IR vibrational modes of silica using photoacoustic spectroscopy, It is argued that the intensity of the silanol band at 3747 cm-1 provides (an inverse) quantitative measure of the interaction of surface groups, along with the shift in the broad hydroxyl band, the interaction following the order C,H,NO > C2H2OH > H2O.The use of IR spectroscopy to study the adsorption on solid surfaces is well documented in the literature,"" For example, hydroxylation of a clean silica surface results in the formation of the free silanol group Si-OH, with a sharp IR band near 3747 cm-1. Further hydroxylation produces a broad band near 3500 cm-1, which is believed to result from various hydrogen-bonded silanol bands leading to a multilayered surface structure of few nm.3-6 Earlier studies had indicated a relationship between the surface silanol band and various chemical activities of silica such as cytotoxicity,7-9 catalysis,10-12 and others.13 Recent studies from our group14-in which the intensity of the silanol band and cytotoxicity of silica, heat-treated at various temperatures up to 1095°C, were investigated-have provided a strong correlation between cytotoxicity and intensity of the silanol band.Coating of silica by PVPNO (polyvinyl-2-pyridine N-oxide with the empirical formula C7H8N0), a strong hydrogen bonding agent, is known to reduce the cytotoxicity of silica, presumably by chemically blocking the silanol groups from phospholipids.15 This interaction of the hydrogen bonding agents with the silica can be studied by IR spectroscopy, and Knozinger16 and Rouxlet and Semples17 have used transmission IR spectroscopy to study the effect of various chemicals on the surface IR modes of silica. However, one of the major disadvantages of transmission IR spectroscopy is that the sample preparation (grinding and mixing with KBr and pelletizing) usually distorts the surface modes (see, e.g., Ref. 14) and there is always a doubt about the effect of the sample preparation on the measured properties, In recent years, photoacoustic (PA) spectroscopy has become the technique of choice for studying the IR spectra of samples in their natural state, since no sample preparation is necessary.18,19 Moreover, according to a recent paper,20 the relative intensity of the surface modes in PA spectroscopy of silica particles is much higher than that in transmission FT-IR spectroscopy. Consequently PA spectroscopy is ideal for studying the surface chemistry, In this work, we have used PA spectroscopy to investigate the interaction of three hydrogen bonding agents (C7H8NO, C2H5OH, and H20) with the silica surface by monitoring changes in the surface IR modes, Our results show that the surface IR modes get perturbed to a larger extent than the bulk IR modes in interaction with the hydrogen bonding agents, Moreover, whereas in the earlier studies, the shift of the broad silanol band near 3500 cm-1 was used as a measure of the interaction with hydrogen bonding agents,16,17 here we show that the relative decrease in the intensity of the sharp silanol band near 3747 cm-1 also serves as a quantitative parameter for the relative surface coverage and surface modification, Details of this work are given below,The Cab-O-Sil samples of silica used here were obtained from the Cabot Corporation of Tuscola, IL, In our earlier studies,14,20 we have shown these particles to be amorphous and about 0.05 am in size, For coverage of these particles with H20 and C2H50H, the following procedure was employed. About 5 mg of silica was mixed with 50 mL of the liquid (H2O or C2H5OH) and refluxed for one hour, The remaining liquid was allowed to evap¬orate to dryness and 1 mg of the treated sample was used to collect the PA spectra. In the case of PVPNO, the amount that binds to Cab-O-Sil is taken from the data on quar"

Mar 1, 1992