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By F. E. Joyce

This paper describes the development of a process for producing manganese and iron pellet concentrates from low-grade manganiferous iron ores of the Cuyuna range by a two-stage sulfatization-reduction roast. First, the manganese minerals (7.5 percent manganese) were converted to water-soluble manganese sulfate by roasting in sulfur oxide gases at 700° C, then, the hematitic iron minerals (31 percent iron) in the hot sulfatized are were reduced to magnetite with simulated reformed natural gas in the temperature range of 350° to 425° C. Batch tests were made in a 3-inch-ID by 6-inch-long, gas-heated, stainless steel retort, and continuous countercurrent experiments were performed in a 2-inch-ID by 10-foot-long, electrically heated shaft furnace. Manganese sulfate was removed from the roasted product by leaching with water, and over 90 percent of the manganese was recovered in an oxide product (65 percent manganese) obtained by precipitation, drying, and thelmal decomposition of the sulfate. An iron oxide concentrate (60 percent iron) with an iron recovery of 75 percent was obtained from the water-insoluble residue by magnetic separation.

Jan 1, 1973

By D. S. Burgess

This report summarizes the incidents that preceded the December 9, 1970, propane-air explosion in Port Hudson, Mo., and then attempts to establish the nature of the explosion from the ensuing events. Special emphasis is given to possible ignition sources, the distribution of flammable vapors, and the analysis of blast damage. Both near-and far-field damage indicated that this explosion may be attributed to the detonation of propane in air with an energy release equivalent to that from about 50 tons of detonating TNT.

Jan 1, 1973

By Walter W. Fisher

A study of copper cementation on iron was initiated to determine the effect that deposited copper has upon subsequent cementation. A microscopic investigation of cementation on an iron surface showed that cupric ion precipitates predominately on a growing copper deposit attached to the iron surface. A kinetic study of the cementation process in a revolving drum showed that the cementation rate is enhanced by the copper deposit attached to the iron surface and by the discrete copper particles of a cement copper slurry. The kinetic study also indicated that the character of the deposit is affected by the major anion in the solution. The cementation process is visualized to occur as a series of electrochemical cells in which cupric ion precipitates on copper dendrites attached to the iron surface.

Jan 1, 1973

By A. G. Kim

Methane and other hydrocarbon gases, byproducts of coalification, are emitted from coal at widely varying rates and often present ventilation problems during mining. The air in some coal mines apparently contains no methane. To determine if coals from mines which bid no history of detectable gas emission contained adsorbed methane, samples of coal at the shaft bottom and at an active face were obtained and placed in sealed metal cylinders. The atmosphere around the coal was sampled and analysed by gas chromatography. Methane, ethane, ethylene, propane, propylene, and butane were found to have been desorbed from these coals. Hydrogen and helium were also detected. An estimate of the amount of residual gas per ton A coal indicated that coal samples from the active face generally contained more adsorbed gas than coal samples obtained from the shaft bottom, although in both instances the total amount of gas was relatively small.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By Mark I. Copeland

The Bureau of Mines investigated the effect of up to 1 wt-pct of copper and silicon on the heat treatment response and hardness, tensile, and impact properties of hot-rolled medium-carbon steels. The steels were prepared by induction melting and fabricated into plates by forging and rolling. The tensile strength of 0.2-wt-pct carbon steels containing 0.3 wt-pct silicon was affected significantly by copper in both the hot-rolled and heat-treated (600° C) conditions, whereas the tensile strength of the 0.3-wt-pct carbon steels was less affected. A 600° C treatment was considered optimum as a post-rolling treatment to strengthen the steels by copper precipitation. Strengthening of 0.2-wt-pct carbon steels by silicon was reduced by increasing copper contents.. Optimum impact strengths occurred at about 0.3 wt-pct silicon in 0.2-wt-pct carbon steels containing 0.6 and 0.8 wt-pct copper. The impact strengths were lowest for 0.2-wt-pct carbon steels containing over 0.8 wt-pct copper and greater than 0.3 wt-pct silicon, especially in the heat-treated condition. Copper and silicon solutes and copper precipitates strengthened the steels. This effect was augmented slightly by strengthening through grain refinement by these solutes.

Jan 1, 1973

By M. Hertzberg

Results of a comprehensive study of the absolute spectral radiance of the infrared emissions from methane-air explosions are reported. The spectral growth of these expanding flames were recorded with a time resolution of 1 msec in the spectral range of 1.7 to 5.0 µm. Time-resolved spectra were obtained for methane-air mixtures as a function of stoichiometry, nitrogen dilution, and Halon dilution, in a 9-liter vessel under different venting conditions. Data are also presented for coal dust-air explosions. Temperatures, obtained from the absolute radiances and from a band ratio technique for methane-air, are internally consistent and are generally 50° to 200°K below adiabatic flame temperatures. All near limit mixtures gave essentially the same flame temperatures (1,500° to 1,600° K) regardless of whether the limit was obtained by dilution with excess air, excess methane, excess nitrogen, or Halon. The coal dust explosion spectrum is essentially a blackbody continuum at 1,500° K with some selective emission at 4.4 µm from hotter CO2. The data are analyzed in terms of the radiative dynamics of a sperically expanding flame zone. The importance of radiative transport is assessed. An equation is derived which relates the instantaneous fraction of combustion power radiated to adiabatic variables.

Jan 1, 1973

By Stanley C. Rhoads

The Bureau of Mines investigated the complete ternary system K2 HfF6¬K2ZrF6-l.25 weight-percent HF at 40° C. In addition, solubility curves have been established at 25°, 30°, 500, 60°, and 70° C. These solubility data implemented a study of hafnium enrichment in feed solutions for liquid-liquid extraction processes.. Selected K2HfF6-K2 ZrF6-1.25 weight-percent HF mixtures were equilibrated in a constant temperature bath. Compositions of the equilibrated solutions and wet residues were established from combined hafnium and zirconium oxide and total fluorine analyses. All solubility curves were essentially parallel on triangular coordinates. At 40° C, the solid phase of the K2HfF6-K2ZrF6-1.25 percent HF system is a series of solid solution hydrates with K2HfF6-H20 and K2ZrF6.3H2O segments existing at the respective extremes. Since this system contains K2HfF6-H20 and K2ZrF6.3H20 segments, it is not ideal for simple separation of high-purity K2HfF6 from K2HfF6-K2ZrF6 mixtures by recrystallization. However, it would be useful for producing hafnium-enriched feed solutions from zircon concentrates for liquid-liquid extraction of hafnium from zirconium.

Jan 1, 1973

By Robert I. Fujimoto

The work described was conducted to develop standards for the application of wire rope clips on wire rope. These standards include optimum number of clips and clip nut torques for wire rope sizes 1/4 through 2-1/4 inches, when used for forming an eye attachment in wire rope. Wire rope test specimens with clip attachments were load tested on tensile testing machines to determine an effective combination of clip nut torques and number of clips for each size of wire rope to develop efficiencies above 90 percent of the catalog ultimate rope strength.

Jan 1, 1973

By Charles Findlay

As one of its projects for degasification of major panels of coal prior to mining within them, the Bureau of Mines conducted methane emission studies during development of a set of three headings 1,800 feet in a major coal panel (2,700 by 3,500 feet) which had been completely isolated by sets of main headings for 12 months in the Federal No. 2 mine (Pittsburgh coalbed) in northern West Virginia. Similar emission studies were conducted in the development of two sets of main headings in virgin coal areas nearby. Comparing the two sets of data indicated that the isolated coal panel had been degasified by approximately 70 percent.

Jan 1, 1973

By H. H. Fields

The Bureau of Mines is in the process of degasifying a virgin area in northern West Virginia from the base of an 839-foot-deep vertical borehole¬. An in situ gas pressure hole 199 feet long, and seven degasification holes ranging in depth from 500 to 850 feet (average 618 feet) were drilled in an 8-foot-thick virgin Pittsburgh coalbed from the enlarged (14-foot-diameter) bottom of this borehole. The in situ pressure at the back end of the hole and the range of gas and water flows from degasification holes as they were completed and closed off were 203 psi, 79,000 to 257,000 cfd (average 160,000 cfd), and 5 to 8 gpm per hole (average 6.8 gpm), respectively. Twenty-four hours after the seven holes were connected through individual water traps to a common collector for natural venting of the gas through pipes to the atmos¬phere, the total gas and water flows and the in situ pressure dropped, respec¬tively, to 971,000 cfd, 1.3 gpm, and 18 psi. Eighty days later the correspond¬ing values dropped to 529,000 cfd, 0.50 gpm, and 13 psi. After 180 days of degasification, 91 million cubic feet of gas had been removed from the affected virgin area. This represents 60 to 70 percent of the gas calculated to be contained in the area of coal affected by the holes.

Jan 1, 1973

By A. W. Hall

A nuclear method was developed for continuously and automatically deter-mining the moisture content of coal flowing through a bin. Fast neutrons from a 1 curie americium-beryllium source penetrate the coal, are thermalized (slowed down) by hydrogen in the moisture, and are counted by a thermal neutron detector. The difference between the number of these thermal neutrons and those thermalized by dry coal (in a reference drum) is a measure of the moisture content of the coal. A materials handling system was developed and in tests at a commercial coal preparation plant, moisture in coal was monitored continuously within 0.2 percent of values determined by conventional means. The meter responded rapidly to change in moisture content, making it adaptable to automatic process control, and was operated for 1 year without malfunction or recalibration. Shielding of the source by the coal kept the neutron flux level at the bin wall less than 1 milliroentgen per hour, a safe level for personnel.

Jan 1, 1973

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 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 B. V. Johnson

The Federal Bureau of Mines has conducted research in support of the National Aeronautical and Space Administration's (NASA) Apollo program to acquire fundamental scientific and engineering knowledge of lunar-mineral resources for NASA's Office of Advanced Research and Technology. Equipment and techniques were developed to conduct soil shear tests in a simulated lunar environment. Shear tests performed with this equipment in ultrahigh vacuum and controlled laboratory atmosphere showed that simulated lunar soil increased in strength in the simulated lunar environment.

Jan 1, 1973

By I. Liebman

A Bureau of Mines study is in progress to determine the effectiveness of passive water barriers in suppressing coal-dust explosions. A 2.9-ft3-capacity water-filled plastic tub was found effective in suppressing dust explosions propagating at speeds of 250 to over 1,000 ft/sec. Work directed at determining the limitations of water barriers showed that the passive water barrier technique is also feasible for the suppression of weak dust explosions propagating at speeds of 100 to 250 ft/sec. For relatively slow accelerating flames, dynamic wind forces appear to be the important quantity governing fragmentation of the plastic tub and subsequent water release and dispersion, whereas dynamic impulse appears to be the significant quantity for rapidly accelerating flames. The acoustic approximation (relation between static pressure and flame or wind speed) is shown to be valid in a long single mine entry. This relationship appears to be useful in predicting the regions within a long single entry where passive water barriers are effective in quenching a dust explosion.

Jan 1, 1974

By Charles C. Boley

Using bench-and pilot-scale coking facilities, the Bureau of Mines produced experimental coke from blends of char with Sunnyside coal (high-volatile A bituminous) from Carbon County, Utah. At bench scale, additions of char made from lignite improved resultant cokes when concentrations of up to 60 pct were used in the blends. At pilot scale (500-pound movable-wall oven), four chars made by entrained-bed carbonization techniques from the parent Sunnyside coal and from a North Dakota lignite were used in two-component blends with the Sunnsyide coal. Chars from Sunnyside coal had volatile matter contents of 5.8, 9.8, and 16.0 pct, moisture-free basis; the char from the lignite had 16.6 pct. In twenty-five 500-pound tests, improvement in coke quality was observed from all blends at char concentrations to 17.5 pct. The best coke, produced from a concentration of 12.5 to 15 pct of S.8-pct volatile char, exhibited physical properties approaching those of an industrial coke produced from Sunnyside coal blended with three higher rank blending coals. Studies were also made of the effects on coke quality of char source, of particle size, of comparative use of char and of a blending coal, and of prolonged coal storage.

Jan 1, 1973

By Richard E. Thill

Elastic wave velocities and moduli were determined by both the pulse and resonance methods in a large number of specimens of St. Cloud Gray Granodiorite and Tennessee marble under the same moisture, temperature, and stress environment. Long cylinders were first tested by the resonance method to obtain longitudinal bar and torsional wave velocity. The cylinders were then sectioned in half and tested by the pulse method to obtain the transient pulse velocity. These velocities were later used to obtain various moduli for comparison. Statistical comparisons between the Young's, shear, and bulk moduli and Poisson's ratios obtained independently by the pulse and resonance methods indicate that the methods do not give equivalent results in nearly isotropic rock. The amount of difference varies for each modulus, with the least difference (less than 5 pct) occurring in the shear modulus and the greatest difference (as high as 34 pct) in the bulk modulus. Moduli determinations in aluminum show much closer agreement between the pulse and resonance methods than in rock. The discrepancy in pulse and resonance results probably is caused by frequency dispersion effects and by differences in error sensitivity in the various formulas used to calculate the moduli.

Jan 1, 1974

By Laxman S. Sundae

A Bureau of Mines investigation was conducted to determine the effect of specimen volume on the apparent tensile strength of disks of St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite. The investigation used a technique developed by the Bureau to determine apparent tensile strength. Because the test specimens were selected without macroscopic defects, that is, cracks, joints, and planes of weakness, the strength variations are solely due to microscopic features. Several replications of each test were performed. Data for each set of specimens were fitted to a power law of the form y = axb, where y = apparent tensile strength, x = specimen volume, and a and b are constants. This power law is essentially a form of Weibull's theory. The average coefficients of correlation for St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite were 0.85, 0.53, and 0.78, respecitvely. In all cases a decrease in strength with increasing volume was noted; in the extreme case, a decrease of 40 pct was noted with an elevenfold increase in volume. The decrease in strength with increasing specimen volume is explained in terms of Weibull's theory.

Jan 1, 1974

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