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By Vance G. Leak

A technique for recovering copper and steel from metallic scrap has been developed by the Bureau of Mines based on preferential melting in molten salt baths at 1,150° to 1,250° C, The molten salt, preferably barium chloride or calcium chloride, both minimizes oxidation of the metals and promotes heat transfer. Cleanest separations (0.01 percent copper remaining in iron) have been achieved by pretreatment (dipping or spraying) with sodium sulphate or sodium silicate, which alters and coats the surface of the iron to inhibit the alloying or brazing with copper. An economic evaluation of the process was carried out on six combinations of sweating media and inhibiting reagents. On the basis of the postulated model, a cost of about $0.20 per pound of copper recovered has been determined for the sweating treatment operation.

Jan 1, 1973

By Terry L. Muldoon

The Bureau of Mines conducted an investigation to quantify microphone response variations that could result when the microphone is worn by a worker, as with a personal noise dosimeter, and to suggest an optimum placement and orientation of the microphone for noise exposure measurements. Previous studies have shown no significant variations in a diffuse field. This investigation, therefore, was conducted in the free-field conditions of an anechoic chamber using an anthropometric dummy as a subject, and broad band noise as the acoustic stimulus. This investigation established that, in a free field, the wearer's body does significantly affect microphone response; the response variations are a function of azimuth, and location and orientation of the microphone. Results suggest that locating the microphone on top of the subject's shoulder, oriented parallel to the body axis, should yield data comparable to that obtained using a sound-level meter.

Jan 1, 1973

By H. B. Carroll

This Bureau of Mines report evaluates the performance of commercially available portable instrumentation for the detection of carbon monoxide, carbon dioxide, oxygen, and methane at conditions simulating an industrial work atmosphere. Portable instrumentation included in the study was gas-detection tubes (length-of-stain and color intensity), catalytic detector, liquid absorption detectors, paramagnetic oxygen detector, galvanic detector, and pelement or hot-wire methane detectors. Evaluation of the instruments was in atmospheres with 50 and 80 percent relative humidities at 75° F and containing test gas concentrations of 0.1, 0.25, 0.50, 1.0, 1.5, and 2.0 times the thresh-old limit value. Correlation of the results from the portable gao analyzer with measurement from the standard instruments was made by calculating and plotting an estimated line of regression, prediction, and confidence limits and the correlation coefficient for each detector system. Relative humidity in the 50-to 80-percent range did not appear to contribute to instrumental uncertainties in either performance or operation. Considerable deviation in detection precision between the portable gas-detection systems and the standard systems was established, especially at the lower gas concentration levels. The main difference or inconsistency in toxic gas concentrations determined with length-of-stain tubes resulted from the observer's interpretation of the results rather than difference in the tubes themselves.

Jan 1, 1973

By Green R. E.

The removal of silica from commercial iron oxide concentrates by dissolution with sodium hydroxide was investigated by the Bureau of Mines as a means for producing supergrade concentrates. The effects of strength of solution, temperature, and digestion time on the extraction of silica were evaluated using eight iron oxide concentrates. Silica extraction from the eight concentrates was enhanced by autoclave leaching in the temperature range of 150° to 250° C and varied from 70 to 95 pct depending on the concentrate used. Superconcentrates containing less than 2 pct Si02 and more than 69 pct Fe were made only when magnetite concentrates were leached in the autoclave. The investigation showed that it is not difficult to obtain a supergrade product if the gangue is mainly quartz.

Jan 1, 1973

By C. A. Komar

Laboratory-scale hydraulic fracture tests were conducted by the Bureau of Mines on directionally oriented sandstone material, along with measurements of directional rock properties such as tensile strength, permeability, ultrasonic velocity, and dynamic elastic constants. In these tests, fracture orientation was determined as a function of various combinations of stress, rock saturation, rate of borehole pressurization, and direction of minimum tensile strength relative to minimum horizontal compressive stress. The objective of the experiment was to investigate whether horizontal stresses always controlled the orientation of induced vertical hydraulic fractures, or if under conditions of small differences in stress and/or slow borehole pressurization rates, the induced fracture direction was influenced by directional properties of the rock matrix. This study shows that the expected influence of horizontal earth stress on the orientation of an induced hydraulic fracture becomes negligible when¬ever the magnitude of the difference between the compressive stresses is 200 psi or less. When this occurs, fracture orientation is controlled by the directional properties of the rock--primarily permeability and tensile strength.

Jan 1, 1973

By L. Cheng

This report describes a laboratory investigation of the effectiveness of low-pressure steam and a steam-water spray sequence for the collection of airborne respirable (<10 µm) coal dust. Comparison of present results to previous results obtained with water spray alone indicates that the use of steam in a steam-spray sequence increases the collection efficiency by about 14 percent over that obtained by water spray alone. However, the use of steam to collect airborne dust requires cooling the steam-dust mixture in order to achieve condensation of the steam, and steam does not appear to be an attractive approach for collecting airborne dust in underground coal mining operations.

Jan 1, 1974

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 E. G. Valdez

Laboratory research demonstrated that ceramic wall and floor tile can be produced from electric furnace phosphorus slags composed of calcium silicates. Grinding the slag in a pebble mill, followed by magnetic removal of deleterious magnetite, produced a raw material that could be compounded and formed into wall tile by dry pressing, sintering, and glazing. The effects of process variables such as forming pressure and sintering temperature were investigated. Wall tile bodies produced by this method were comparable to commercial tile. The tiles were readily glazed to a smooth shiny finish and met ASTM Specifications C34-62 for structural clay load-bearing tile. The estimated cost of producing wall tile by this method compared favorably with the retail market value for similar wall tile. Addition of borax or other additives to the ground slag followed by dry pressing and firing likewise produced a commercial grade of floor tile.

Jan 1, 1974

By J. A. Cavallaro

This Bureau of Mines report describes the preparation characteristics of 10 coal samples collected from the significant coal-producing mines of Lucas, Mahaska, Marion, Monroe, and Wapello Counties in Iowa, with special emphasis on physical desulfurization. All 10 samples were of high sulfur content as received, ranging from 4.2 to 10.4 percent; the organic sulfur content ranged from 0.8 to 3.8 percent. The pyritic sulfur content of the samples could be appreciably reduced by crushing and washing and provided pyritic sulfur reductions ranging from 36 to 75 percent. Crushing to 3/8-inch top size and removing the sink 1.60 specific gravity material would provide float coal products containing 3.5 to 6.0 percent sulfur. However, these coals could be burned at utility plants utilizing SO2 removal processes with efficiencies ranging from 70 to 88 percent and still be in compliance with the current Federal SO2 emission regulations for stationary sources.

Jan 1, 1973

By H. W. Leavenworth

Research was conducted by the Bureau of Mines to develop a technique to grow metallic fibers from a sulfide mineral. In this research, chalcopyrite (CuFeS2) was made sulfur deficient, and the remaining sulfur partitioned to the iron in the mineral to liberate metallic copper, or to the copper to liberate metallic iron. The metals formed on the surface as fibers and in the interior as spherical particles. Fiber growth is very fast. Lengths of 3 to 4 cm form in a matter of minutes, and the diameter of individual fibers is less than 1 µm. The mechanism of fiber growth is explained, and the reactions are reversible as predicted. Copper fibers can be made to grow from the surface at 400° C or to dissolve back onto the solid surface and be replaced by iron fibers at 625° C. Growth and dissolution can also be controlled to form copper/iron duplex fibers.

Jan 1, 1974

By J. M. Stuve

Thermodynamic properties were determined by the Bureau of Mines for the intermetallic compound, TiA13. Heat capacities were obtained from 5 to 303 K by adiabatic calorimetry. The derived value of S2 1s is 22.08±0.07 cal/deg¬mole. Enthalpies relative to 298 K were obtained from 298 to 1,413 K by copper-block drop calorimetry. No anomalous thermal behavior was noted in the temperature ranges investigated. Low- and high-temperature data were combined with a known enthalpy of formation at 298 K to give values of enthalpy of formation and Gibbs energy formation, 0 to 1,400 K.

Jan 1, 1974

By H. E. Perlee

Mathematical expressions are derived for the histories of the pressure, flame radius, mass fraction burned, and burned and unburned gas temperatures associated with a spherical flame propagating concentrically in a spherical vessel. The equations are solved numerically for a 9.5 pct CH4/air mixture using the best available information for the burning velocity, expansion ratio, and specific heat ratio. Calculated histories are in complete accord with experimental measurements. The accuracy of calculated histories is determined relative to errors in the system parameters, and it is found that 10 pct errors in either the burning velocity or the expansion ratio results in a 40-pct error in the pressure history. A 10-pct error in either burned or unburned specific heat ratio results in a 22-pct error &apos;in the pressure history. It was further established that the usual assumption of constant specific heat ratio is unacceptable, but equating the burned and unburned specific heat ratios result in no apparent error in the histories. The cubic law (P = Kt3 + Po) is derived and discussed, and it is found that the law is valid only during the early period (P<2 atm) of flame growth.

Jan 1, 1974

By R. W. Watson

This Bureau of Mines report summarizes some recent results on the sensitivity of various experimental explosive systems using ammonium nitrate (AN) as the oxidizing agent. The sensitivity survey included drop-weight and friction testing and sensitivity to initiation by projectile impact and a No.8 blasting cap. It was found that certain types of AN prills can result in cap-sensitive mixtures when combined with No.2 diesel fuel (Fa); prilled AN mixed with nitromethane also result in cap-sensitive mixtures. Mixtures of AN prills and neat 1-and 2-nitropropane were not cap-sensitive, and the use of powdered or grained aluminum in AN-FO did not adversely affect the sensitivity except possibly to increase its sensitivity to friction.

Jan 1, 1974

By Manuel Gomez

A computerized moving average technique was developed to interpolate coal seam characteristics between sample points. The interpolative method coupled with multivariate regression analysis and simulation procedures was used to forecast coal properties not readily obtained from an analysis of drill core samples. Coal property forecasts were of two kinds: (1) specific mine property forecasts that are suitable for mine product control and yield a good approximation of the local variation along both the vertical and horizontal axes of the seam, and (2) regional estimates where much of the local seam variation is smoothed out, but the general trends are maintained. Forecasts of the volatile matter, ash, total sulfur, and the heating value for part of the Pittsburgh seam located in Ohio, Pennsylvania, and West Virginia were in good agreement with independent evaluation data. Spatial configuration for preparation characteristics, particularly, the effect of crushing on sulfur release, low-and high-temperature carbonization properties, the Hardgrove grindability index, the coal hardness index, gasification variables, and hydrogenation factors were constructed for the same area of the Pittsburgh seam. These forecasts may be developed from drill core data collected in the exploration phase of mining. The results, which may take the form of a series of maps, are useful to mining, chemical, and combustion engineers, to economists and mine managers, as well as to coal users for mine design, economic analyses, energy forecasts, utilization studies, mine product control, and environmental control and programming.

Jan 1, 1974

By Daniel C. Boteler

Data from 68 entrained-bed carbonization tests were treated statistically by the Bureau of Mines, and several useful relationships were developed among the major variables. Nine coals, ranging in rank from lignite A to high-volatile A bituminous, were carbonized in two entrained-bed carbonization pilot plants. The carbonizing reactors employed were vertically mounted cylinders, internally heated, refractory-lined, and 10 inches ID. The range of carbonization temperatures was from 825° to 1,600° F. Using a regression-analysis computer program, empirical equations were developed by which carbonization temperature, air-to-coal ratio, devolatilization of coal, char yield, and volatile matter content of product char may be predicted.

Jan 1, 1973

By L. A. Haas

In this Bureau of Mines investigation, conditions were determined to form an iron sulfide adherent coating with a metallic golden luster on steel upon anaerobic heat treatment with sulfur. The sulfide formation rate was determined in the temperature range of 105° to 500° C with reaction times up to 68 hours. The optimum temperature and time to form an adhering decorative coating on mild steel was in the range of 105° C for about 70 hours to 285° C for 1 hour. The golden coating consisted of an inner layer of pyrrhotite and an outer layer of pyrite. At temperatures higher than about 300° C, the outer layer thickness decreased owing to the decomposition of pyrite to pyrrhotite.. Small quantities (<0.5 wt-pct) of petroleum oil accelerated the sulfide growth rate. The sulfide coating decreased the corrosion rate of steel in a neutral aqueous medium by a factor of two. The dissolution of pyrite in water was dependent on particle size and surface area with the flat pyrite coatings exhibiting the lowest dissolution rate.

Jan 1, 1974

By J. B. Janus

In connection with the purchase of coal under specifications for Government use, the Bureau of Mines in this report has compiled data on 81 mines located in 15 States. This annual report lists analytical data on the composition and quality of tipple and delivered samples of coal collected during fiscal year 1973. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for most of the coalbeds listed. The deliveries were sampled at destination in accordance with instructions issued by the Bureau of Mines. All samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1973

By D. W. Richardson

This Bureau of Mines publication provides the enthalpy of formation of malachite [Cua(COs)(OH)2] as determined by hydrochloric acid solution calorimetry. At 298.15 K the enthalpy of formation from the component oxides is -15.l0±0.30 kcal/mole and from the elements, -251.9±0.5 kcal/mole.

Jan 1, 1974

By David L. Veith

Caustic scrubbing followed by silica flotation with cationic ether primary amine proved effective in upgrading commercial magnetic concentrates to supergrade products containing 2 percent SiO2, or less. Samples representing 41 million long tons per year of commercial magnetic concentrates from the Lake Superior region were tested by the Bureau of Mines. Bench-scale and pilot plant research indicated an estimated potential of 32 million long tons per year of superconcentrates to be available. Two pilot plant investigations yielded superconcentrates containing 1.1 and 1.9 percent SiO2 that were derived from commercial concentrates containing 7.0 and 4.2 percent SiO2, respectively. Corresponding iron recoveries were 90 and 93 percent at reagent costs of just over 33 cents per long ton of superconcentrates produced. Additional sources evaluated on a bench scale resulted in iron recoveries of 72 to 95 percent in products containing 1.7 to 2.0 percent Si02. Although reagent cost ranged up to 60 cents per long ton of superconcentrate, it is probable that these costs would be reduced in plant applications where benefits are derived from material and reagent recycle.

Jan 1, 1974

By Laurance L. Oden

The Bureau of Mines is developing melting data for binary combinations of the alkaline earth fluorides and yttria to facilitate the formulation of slag compositions. The present report deals with the SrF2-Y2O3 system for which liquidus and solidus temperatures and solid solubilities were determined. The information is presented as the phase diagram. The phase diagram was constructed from information obtained by ceramogra¬phy, X-ray diffraction, thermal analysis, and electron probe microanalysis of small specimens encapsulated in platinum-20 percent rhodium or molybdenum ampoules. The data indicate a simple eutectic system with limited terminal solid solubilities. The eutectic temperature is 1,457°±5° C, and the eutectic composition is 4±1 mole-pct Y203. Strontium fluoride containing up to 2 wt-pct 0 2 was studied to determine the effects of oxygen contamination. Oxygen levels in excess of 0.2 wt-pct resulted in eutectic formation between SrF2 and SrO. The eutectic composition is between 0.2 and 0.7 wt-pct 02, and the eutectic temperature is 1,447°±5° C. No intermediate oxyfluoride phases were detected.

Jan 1, 1974