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By James J. Snodgrass

The Bureau of Mines designed and constructed a series of calibration models for geophysical borehole logging. A nominal hole diameter of 3 inches was selected as representative of typical core holes drilled for mining and engineering purposes, although additional hole diameters of 2, 5, and 8 inches are provided in one of the models for determination of empirical correction factors for variations in hole diameter. The physical properties of the models were determined by laboratory analyses of drill core samples and evaluated statistically for reliability. This report outlines the location of the models, elements of design and construction, and results of the laboratory tests. The models are available at the Denver Federal Center, Denver, Colo., for use by Government agencies and private industry to calibrate logging equipment for measurements of density, sonic velocity, magnetic susceptibility, and electrical resistivity.

Jan 1, 1976

By Philip C. Good

Unweathered low-grade calcareous phosphate rock of about 20 percent P205 grade was beneficiated by a procedure in which contained carbonates were decomposed by calcination at about 1,000° C. On quenching the hot calcined rock in water, major impurities passed into a slime phase which was mechanically separated from a coarser concentrate fraction. Phosphate rock of two major types was beneficiated in batch-scale studies yielding concentrates containing 31.3 to 38.5 percent P205 at recoveries ranging from 54.8 to 86.0 percent. The samples were from two major deposits in India. Processing information gained was utilized in extending the work to a continuous-flow system, processing phosphate rock at rates up to 157 kilograms per hour. Superphosphate exceeding 16 percent water-soluble P205 was prepared from concentrate derived from continuous-flow processing.

Jan 1, 1976

By Y. Miron

Previous studies at the Bureau of Mines outlined the hazards of ammonium nitrate-fuel oil (AN-FO) mixtures in the presence of pyrite-bearing ores. The recent trend in the mining industry to strengthen AN-FO by the addition of aluminum metal raised the question regarding the effect of aluminum in AN-FO in the presence of pyrite-bearing ore. Laboratory work, similar to that done previously, demonstrated that the temperature of a self-sustaining reaction in the presence of AN-FO ore-aluminum is not lower than that for a comparable AN-FO-ore mixture. However, as might be expected from known thermochemical data, once initiated, the resulting reactions between AN-FO, aluminum, and pyrite are much more vigorous than those observed for AN-FO and pyrites alone. The temperature required to produce a self-sustained reaction for the combinations tested in this study is 250°±20° F while in the previous Bureau study, reactions were noted, in some instances, at 150° F. The different pyritic ores may be the cause of this variation.

Jan 1, 1976

By Edward D. Thimons

Inflatable stoppings are currently marketed for production use, and numerous mining companies have become interested in using such stoppings in rescue and recovery operations. The Bureau of Mines therefore evaluated the concept of using inflatable stoppings in emergency situations. The stoppings tested by the Bureau were 12-foot-diameter spheres inflated with a blower operated by a small battery pack. Experiments were conducted with the stoppings in a full-scale wooden mine model to evaluate their ability to withstand sliding or slipping at various internal and differential pressures, puncture resistance, various inflation techniques; and internal leakage from the stoppings. The stoppings were then installed and tested in the Bureau's Safety Research Coal Mine at Bruceton, Pa., to determine their effectiveness as mine air barriers. Despite some encouraging results obtained with the model and in-mine studies, the stoppings did not perform well in two operating metal mines where they proved difficult to erect and inadequate as air barriers.

Jan 1, 1976

By H. C. Ko

Calorimetric determinations of low-temperature heat capacities and standard enthalpy of formation were made by the Federal Bureau of Mines for basic aluminum sulfite, A1203?2.0S02?5.3H20. The standard values of entropy (S°), enthalpy of formation (?Hf°), and calculated Gibbs energy of formation (?Gf°) at 298.15 K are 85.2±0.1 cal/deg-mole, -943.1±1.2 kcal/mole, and -820.7±1.2 kcal/mole, respectively.

Jan 1, 1976

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 E. F. Ferrell

Gold was recovered from scrap electronic 60-40 (tin-lead) solders by drossing with aluminum or zinc at elevated temperatures. The gold, together with other metallic impurities, collected in the dross phase which could then be separated from the molten solder by skimming or filtering. Drossing upgraded the gold concentration by a factor of 10. Further upgrading was achieved by a combination of steps including an oxidation roast and either a combined cyanidation-amalgamation treatment or an aqua regia leach. The gold was then recovered in highly concentrated form from the aqua regia or cyanide solutions by cementation and from the amalgam by volatilization or dissolution of the mercury. The solder was purified by reaction with NaOH to remove dissolved aluminum or with SnCl2 to remove dissolved zinc.

Jan 1, 1976

By Israel Liebman

The Bureau of Mines developed three types of passive water barriers for suppressing slow-moving coal dust explosions. One type is a modification of a conventional tub barrier and depends on the dynamic pressure generated ahead of an explosion to tilt the tub to release its water and suppress the explosion. The other two barriers operate in response to an increase in static pressure developed ahead of the explosion. Tests indicate the first barrier begins to release its water at air speeds as low as 50 ft/sec, and the second and third barriers will operate at a rise in static pressure as little as 0.5 psi. All three barriers were found to be effective in suppressing coal dust explosions propagating at speeds as low as 100 ft/sec. A plan is described for installing a water barrier in a working mine on a trial basis.

Jan 1, 1976

By Martin Hertzberg

This Bureau of Mines study concerns the use of the tube bundle method as a sensitive and reliable detector of mine fires. The method involves the pneumatic, sequential sampling of many points in a system through branching tube bundles that lead to a single analytic station of high sensitivity, good reliability, and convenient location. Two serious limitations inhibit its use: the relatively slow response times for long lengths of narrow sampling tubes and the wall-diffusion losses for submicrometer smoke particulates. These limitations were quantitatively evaluated by measuring tube transit times and smoke particulate transmissions as a function of tube length, diameter, and pressure drop. The comparison of the data with theory offered the challenge of extending the classical, incompressible flow solutions to the two compressible cases: isothermal and adiabatic. New equations were derived for these cases, and the measured transit time data gave reasonable agreement with calculated solutions in both the laminar and turbulent regimes. The measured transmission losses of smoke particulates from several combustion sources compared favorably with those expected from Brownian diffusion losses to the interior walls of the sampling tubes. Traveltime and smoke transmission graphs are provided and, pump power requirements are estimated.

Jan 1, 1976

By Seth C. Schaefer

The Federal Bureau of Mines studied the Gibbs free energies of formation of chromous fluoride (CrF2), chromic fluoride (CrF3), and chromium (II,III) fluorides (CrF2.40 and CrF2.45) with high-temperature galvanic cells employing calcium fluoride doped with 1 mole-pct yttrium fluoride as the electrolyte. Free-energy changes were obtained from open-circuit potential measurements for the following cells: Cr, CrF2 // CaF2 // NiF2, Ni (a) NiO, NiF2 // CaF2 // CrF3 , Cr203 (b) CrF2 , CrF2.40 // CaF2 // NiF2, Ni (c) and CrF2 ?45 , CrF3 // CaF2 // NiF2, Ni (d) with the following overall reactions Cr(s) + NiF2 (s) = Ni(s) + CrF2 (s) (1) 3NiO(s) + 2CrF3 (s) = 3NiF2 (s) + Cr203 (s) (2) 5CrF2 (s) + NiF2 (s) = 5CrF2.4O (s) + Ni(s) (3) and 3.64CrF2.45 + NiF2 (s) = 3.64CrF3 (s) + Ni (s) . (4) These results were combined with the best available literature values of ?Gf° of NiF2, NiO, and Cr203 to deduce Gibbs free energies of formation for the chromium fluorides expressed as follows: ?Gf°(CrF2) = -179.31 + 24.33 X 10-3T ± 0.43 kcal-mole. (5) (858.1 - 964.9 K) ?Gf° (CrF3) _ -226.16 + 1.82 X 10-3T ± 0.79 kcal/mole (6) (880.8 - 957.8 K) ?Gf°(CrF2.40) _ -213.65 + 32.14 X 10-3T ± 0.44 kcal/mole (7) (0053.9 - 936.8 K) and ?Gf°(CrF2.45) _ -176.17 - 12.67 X 10-3T ± 0.80 kcal/mole (8) (875.1 - 937.6 K). Free energies and equilibrium fluorine pressures for three univariant and one bivariant equilibria are illustrated.

Jan 1, 1976

By M. J. Sapko

The pressure and flame development of the methane-air-nitrogen system was investigated in the Bureau's l2-foot-diameter sphere to define buoyancy effects and to develop relationships for predicting venting requirements. Pressure rise (?P) is defined as a function of time (t) and nitrogen dilution and is shown to deviate noticeably from the cubic law (?P = kt3), depending upon the period of combustion and the mixture composition. Corresponding flame speed (Sf) and burning velocity (Su) data are given which show that Sf is time dependent and that Na dilution has a greater effect than air dilution in inhibiting the flame propagation. The Su data agree with "accepted" values and are unique in that they are based on much larger flames than those used in other investigations. Downward propagation limits are shown to depend mainly upon buoyant forces, which can affect the burning of even stoichiometric CH4-air systems. Theoretical expressions, based on the mixture burning velocity and expansion ratio, are given for predicting the venting requirements for ignitions of hydrocarbon-air-nitrogen mixtures in spherical or cubical enclosures.

Jan 1, 1976

By Edward D. Thimons

Several types of inflatable stoppings, developed under Bureau of Mines contract for use as mine air barriers during underground production, have been tested by the Bureau. All of the stoppings tested showed significant internal leakage initially but, in all but one stopping, the leaks were sealed with limited effort The stoppings were tested underground in two western noncoal mines under production conditions. The results from the Colorado molybdenum mine showed the stoppings to be generally unsatisfactory for daily mine usage if they are deployed near blasting areas or in locations where near-perfect air seals are required. They were very susceptible to blast damage and seldom were better than 90 percent efficient as air barriers. However, stoppings tested in the New Mexico uranium mine were located substantially distant from any blasting. Because slight leakage past the stoppings was acceptable, they proved very satisfactory in that application.

Jan 1, 1976

By Mark I. Copeland

Bureau of Mines researchers investigated the combined effect of copper and tin additions on the mechanical properties of hot-rolled steels. Wrought steels containing 0.2 wt-pct C and up to 0.2 and 1.0 wt-pct Sn and Cu, respectively, were made and evaluated by conducting tensile and impact tests and electron-beam microprobe and electron microscopy examination. Tin additions did not significantly affect the tensile properties of steel at different copper contents in the hot-rolled condition. Tin lowered the copper content at which strengthening by copper precipitation normally starts, 0.8 wt-pct, and decreased the strength of steel aged at 1,022° F (550° C). The most adverse effect of tin was lowering the notch toughness of steels at most copper contents.

Jan 1, 1976

By Wallace W. Roepke

The Bureau of Mines studied the cutting characteristics of point-attack bits to reduce airborne respirable dust and energy during cutting. Linear cutting of two coal types using four bit types at three depths of cut with three space-depth ratios was performed with a modified horizontal milling machine using an optical particle-size monitor for respirable dust sampling. The cutting action of one bit on a rotary hardhead mining machine was mathematically analyzed and compared with the results of the linear cutting test. Airborne respirable dust per unit mass cut (specific dust) was found to be a monotonically increasing function of specific energy. Specific dust and energy decrease with increasing depth of cut. The amount of nonairborne respirable dust was 100 to 1,000 times greater than the airborne dust. The plumb-bob bit produced the most airborne respirable dust and the highest specific energy of the four bits tested. Rotary cutting was a greater dust producer and energy consumer than linear cutting because of the constantly changing depth of cut, space-depth ratio, and attack angle of the bit relative to the horizontal bedding planes. A new cutting technique is proposed to minimize the existing problems of the rotary cutting machines by providing greater production, reduced dust, and minimized methane ignition potential at the face.

Jan 1, 1976

By Daryl R. Tweeton

The Bureau of Mines compared the effects of surface-active chemicals with those of pure water on core-drilling rock and quartz and on fracturing quartz. The objectives were to determine if these chemicals assist drilling and fracturing rock and if zeta potential control was worth pursuing as an aid to full-scale drilling. All tests were performed in the laboratory. No significant increases in drilling rates were observed for 1 to 10,000 ppm Al (as AlC13) in flushing water when drilling microcline or serpentine, nor for 1 to 10,000 ppm Mg (as MgC12) when drilling microcline or marble. Concentrations near those giving a zero zeta potential were used with microcline and marble. A 50-pct rate increase was observed for drilling quartz in 0.7 ppm oleylammonium acetate, which gave a zero zeta potential. No other concentrations were used. No effect on the tensile strength of quartz thread in 0.05 ppm Al (as AlC13), which gave a zero zeta potential, was observed. Heptanol, reported to give a zero zeta potential on quartz, did not reduce the bending strength of small quartz bars below that in water. These generally negative findings raise doubt about the usefulness of zeta potential control in full-scale drilling. The results, combined with previous studies, suggest that controlling physical properties of drilling fluids, such as viscosity, is more useful than altering chemical properties.

Jan 1, 1976

By Raymond M. Stateham

Calculations based on data obtained from measurements of smoke from coal-fired powerplants predict that infrared imagers will be useful tools for smoke vision. Infrared imagers operating in the 3-to 5-um spectral region have been evaluated for this purpose. A mine opening 110 meters long was filled with smoke from burning coal, and two men, wearing breathing apparatuses, moved through the smoke to serve as targets. The men were detected and identified at 80 meters.

Jan 1, 1976

By A. E. Gooch

The Bureau of Mines conducted research in an attempt to provide a more sound basis for recommending improved artificial support during deepening of the main shaft of the Lucky Friday mine in the Coeur d'Alene mining district of northern Idaho. Field measurements of closure across the short axis of the 13-by 26-foot shaft were as high as 16 inches. Elastic/plastic finite-element (F/E) analyses were made, reducing the values of large-scale in situ rock mass properties until field closure measurements generally corresponded to displacements in the F/E analyses. Resulting plots of rock mass displacements, stresses, and areas of plastic failure display the results of creating openings (shaft, in this case) in deep mines in difficult ground conditions requiring artificial support.

Jan 1, 1976

By W. L. Staker

The Bureau of Mines investigated the use of shredded automobile scrap for copper cementation. Air agitation was used to improve the cementation rate and prevent excessive buildup of copper on the iron. The pieces of scrap were too large to be properly evaluated in the laboratory; therefore, a pilot scale test unit was constructed and the process tested at field locations. Pregnant solution was obtained from industrial leaching operations, processed in the test unit and the barren solution and cement copper were returned to the plant process stream. The test results showed that the air-agitated launder containing auto-mobile scrap was an effective means for recovering copper from leach solutions. A continuous l4-day test run was made without a noticeable decrease in cementation efficiency. The most suitable scrap product was obtained from incinerated automobile hulks shredded in a hammer type of shredder. However, it was necessary to remove small pieces such as nuts and bolts because they interfered with the discharge of the copper product.

Jan 1, 1976

By J. M. Stuve

Low temperature and high-temperature calorimetric measurements were made by the Federal Bureau of Mines on high-purity samples of Re02(s) and Re03(s) to determine heat capacities and enthalpies. The temperature range of heat capacity measurements was 5 to 310 K for Re02 and 8 to 309 K for Re03. High-temperature enthalpy measurements alone were determined for pure Re207(s,1). The derived standard entropies are S°298 = 11.43±0.01 cal/deg mole for Re02(s) and S298 = 16.55±0.02 cal/deg mole for Re03(s). High-temperature enthalpy equations expressed in calories per mole are as follows: Re02 (s) , H-H298.15 = 16.002T + 1.600 X 10-3T2 + 3.522 X 105T-1 - 6,095 (298 to 1,400 K); Re03 (s) , H-H298.15 = 20.293T + 3.238 X 10-3T2 + 3.950 X 105 T-1 - 7,664 (298 to 1,000 K); Re207 (s) , H-H298.15 = 38.437T + 10.309 X 10-3T2 + 4.315 X 105 T-1 - 13,824 (298 to 413 K); Re207 (s) , H-H298.15 = 30.181 + 17.713 X 10-3T2 - 10,612 (413 to 600 K) ; Re207 (1) , H-H298.19 = 66.101T - 10,092 (600 to 700 K). Gibbs energy of formation (?Gf°) data and related functions over the temperature ranges investigated are tabulated for the three oxides.

Jan 1, 1976

By R. H. Jefferson

An electrochemical method to selectively determine sulfur dioxide in the presence of sulfur trioxide was investigated. A hydrophobic gas-permeable membrane separates the gas sample solution from an internal filling solution containing a fixed quantity of chloride ion and a sufficiently large excess of sodium bisulfite so that its concentration may be considered constant. Sulfur dioxide diffuses through the membrane to dissolve in the internal filling solution and liberates an equivalent quantity of hydrogen ions. The electromotive force between a precision-ground, flat-ended pH electrode, which acts as the sensing element, and a chloride sensing electrode, which acts as the reference element, gives a direct measure of S02 in the gas sample solution. Calibration curves in water, tetrachloromercurate (TCM) , and citrate buffer absorption solutions were closely parallel with slopes in their linear segments, ranging from 57 to 52 mv/decade of S02 concentration. The slopes compare reasonably well with the theoretically expected slope of 58 millivolts at 21° C. The water standard curve was linear with respect to the logarithm of S02 concentration from 1 to 1,000 ppm S02; the TCM standard curve was linear from 10 to 2,000 ppm S02; and the citrate standard curve was linear from 30 to 5,000 ppm S02' The high efficiency and nontoxicity of citrate favor it as a substitute for the conventionally used TCM in the absorption solution.

Jan 1, 1976