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By Dale E. Wittmer

Nonoxide ceramic materials could substitute for high-temperature alloy steels containing imported critical and strategic materials such as cobalt, chromium, and nickel if their high-temperature properties can be improved. An important result of this substitution would be a reduction of the Nation&apos;s need for imports of critical and strategic materials. In this Bureau of Mines investigation, the primary objective was to produce high-purity u1trafine (particles <5 ~m equivalent spherical diameter (ESD)) alpha-silicon carbide (a-SiC) powders with improved high-temperature properties using the Bureau&apos;s patented turbo-milling process. A secondary objective was to determine the feasibility of using polymer mill construction materials as a means of eliminating metal contamination from the turbomill. U1trafine a-SiC powders with BET (Brunauer-Emmett-Te11er) surface areas from 30 to 35 m2/g (~0.06 ~m particle ESD) were produced in an all-polymer turbomi11. These high-purity powders (with I-pct Band I-pct C additions) hot-pressed to greater than 99 pct of their optimal density and exhibited properties commensurate with those of commercially available a-SiC. The most promising of the construction materials tested for the major wear surfaces of the turbomi11 was u1trahigh-mo1ecu1ar-weight (UHMW) polyethylene, a polymer thermoplastic.

Jan 1, 1984

By A. Y. Lee

Prior work at the Bureau of Mines resulted in the successful development of a bench-scale, combination electrorefining-electrowinning method for recycling the lead from scrap batteries using waste fluosilicic acid (H2SiF6) as electrolyte. This paper describes larger scale experiments. Anodes cast from scrap battery lead were electrorefined in a 20-L multielectrode cell for 3 to 7 days. The anodes, containing 2 to 2.5 pct antimony, were ideal for obtaining firm and adherent slime blankets. Cathode deposits, assaying 99.99 pct Pb, were obtained, with current efficiencies near 99 pct. Sludge leaching was done in 100-L tanks followed by filtering in 61 cm square vacuum pan filtersu Lead of greater than 99.99-pct purity was recovered from the filtrate by electrowinning in a 20-L multielectrode cell using insoluble Pb02-Ti (lead dioxide-coated titanium) anodes and pure lead cathodes. The fluo-silicic acid electrolyte depleted in lead was repeatedly recycled to leach more sludge, and there was no problem with impurity buildup. The amount of Pb02 formed on the anodes during electrowinning was less than 1 pct of the total lead deposited on the cathodes, as long as the phosphorus concentration in the electrolyte was greater than 1.3 giL. Emissions of lead in air were less than 10 ~g/m3, well below the proposed OSHA limit of 50 ~g/m3.

Jan 1, 1984

By R. D. Brown

This Bureau of Mines report describes a new methodology for identifying and sorting scrap metals using two modern portable instruments: a thermoelectric sorter and a hand-held emission spectroscope. The method, tested on a 27-sample stainless steel and superalloy array, makes it possible to group and/or identify a typical mixture of high-value metal scrap in two or three steps, whereas as many as seven or eight steps are needed to perform the same separations using chemical spot tests. A portable fluorescent X-ray analyzer identified 19 of the 27 alloys in the sample array by name or type; these alloys are included in the microprocessor memory. The remaining alloys were identified by using the analyzer in its elemental analysis mode and comparing the results wit.h alloy specification chemistry.

Jan 1, 1984

By G. K. Derby

The Bureau of Mines investigated methods for removing dragline bucket wire rope terminations with the objective of finding efficient methods that are safer than the method most commonly used at U.S. surface mines, which is to use the explosive impact of a projectile fired from a cannon to remove the rope termination. Removal of a wire rope termination for repair or replacement requires separation of the wedge and socket that lock together to secure the rope end. The Bureau investigated currently used methods and improved upon and tested two safer alternate methods for removing wire rope terminations. A cannon test program was conducted, using 40-and 50-gr primer (detonating) cord, to establish the possible force produced with a 4-in-bore cannon and a 55-lb projectile. Wedge and socket units supplied from cooperating mines were separated under controlled conditions to establish data on separation force requirements. The two alternate methods investigated were use of the force generated by (1) a pendulum ram and by (2) a portable hydraulic pusher. Both methods are capable of providing sufficient force to effect wedge and socket separations on draglines with up to 78-yd3 buckets under normal conditions.

Jan 1, 1984

By M. L. Glenn

The Bureau of Mines is conducting research on substitutes for chromium-containing alloys in order to conserve imported critical and strategic materials. Part of this research concentrates on finding low-chromium substitutes for heat-resisting stainless steels for the temperature range 600° to 800° C. Ferritic alloys are emphasized that have oxidation resistance provided by chromium contents as low as 10 pct and stress rupture strength provided by the precipitation of the chi(X)-phase intermetallic compound, (Fe36Cr12 (Mo, Ti)10). Initially, research was concentrated on selecting an alloy composition having a minimum chromium content with strengthening provided by the X-phase. An Fe-(10-12 pct)Cr-6 pct Mo-(1.5-2.0 pct)Ti alloy was selected. After the alloy selection, the tensile, stress rupture, and oxidation properties were determined. Stress rupture properties were found to be similar to those of 304 stainless steel. However, the alloys possessed brittleness during both stress rupture and tensile testing, possibly as a result of too high a content of molybdenum and titanium. Higher than expected oxidation rates were found that may be caused by the high molybdenum content.

Jan 1, 1984

By R. H. Grau, A. Sainato, S. J. Schatzel, T. M. Kohler, A. T. Iannacchione

This Bureau of Mines research study found gas emission rates from an advancing face, and flows and pressure of gas from an exploration drill hole were dependent upon the geology of salt encountered in a domal salt mine. Normal production-grade "pure" salt adjacent to an anomalous&apos; zone was found to have a methane emission rate of less than 5 ft3/ ton (0.1 m3/t) of mined salt from a room advanced by a continuous miner. Extremely low gas flows [less the 4 ft3/h (0.1 m3/h)] and lack of pressure buildup were also observed from this normal salt in a 154-ft (47-m) exploration drill hole. These data indicate that methane emissions should not be a problem when mining in this type of salt. In the adjacent anomalous zone, methane emission rates ranged from 15 to 70 ft3/ton (0.4 to 1.8 m3/t) of mined salt from an advancing face. Gas flows of approximately 42 ft3/h (1.2 m3/h), and pressures in excess of 900 psig (6,200 kPa) were observed in an exploration drill hole when the anomalous zone was encountered. This information suggests a greater methane emission hazard from the anomalous zone than from the associated normal salt. If this trend of increasing emissions problems associated with anomalous zones of salt is common with similar anomalous zones encountered or observed in other domal salt mines, then special control strategies should be employed to minimize this potential mining hazard.

Jan 1, 1984

By Martin Hertzberg

In this Bureau of Mines study, an equation is derived for the limit burning velocity for divergent, spherical propagation from an ignition kernel of radius, r: (Su)e = ( ) . For flame propagation into a preexisting, stretching velocity gradient of magnitude dv/dx, the limit velocity is (Su)e = (a dv/dx)1/2. These formulations are shown to be equivalent to the fluid dynamic concepts of Damkoh1er, Kar10-vitz, and Markstein. Existing data for the b10woff limits of flames are shown to give excellent agreement with those concepts provided that proper account is taken of two dilution effects: composition dilution caused by entrainment and velocity gradient dilution caused by flow expansion. Approximate flow-field solutions are also derived for the unburned gas motion above an upward propagating, spherical flame kernel in buoyancy-induced flows. It is shown that;, the upward hemisphere propagates toward a stagnation plane in a counterflow configuration involving the balance between the combustion force, which accelerates the cold gas upward, and the buoyancy force that accelerates the cold gas downward. The position of the stagnation plane above the upward propagating hemisphere is related to the ratio of the buoyant velocity, vb, to the burning velocity, Suo Extinction of the upward propagating wave occurs by flame stretch in that counterflow configuration when n = Vb/Su begins to exceed the expansion ratio, Pu/Pb&apos; and the wave is blown off by its own buoyancy-induced flow field.

Jan 1, 1984

By P. R. Bremmer

As part of a program to devise alternative technologies for producing alumina from domestic resources, the Bureau of Mines investigated the leaching of calcined kaolinitic clay to form basic aluminum chloride solutions. Bench-scale experiments were conducted for single-stage batch leaching with AICl3 solution and three-stage countercurrent leaching with substoichiometric HCI. Variable conditions of clay calcination and leaching were studied to determine their effects on aluminum extraction and pregnant liquor composition,

Jan 1, 1984

By John Durkin

Electromagnetic narrow-band signals were transmitted through the earth at 27 coal mines located throughout the United States. From those Bureau of Mines tests, apparent earth conductivity values were derived based upon a homogeneous half-space model of the earth. The derived conductivity values were found to be inversely proportional to the transmitted frequency and mine depth. A linear regression model relating the logarithm of the conductivity to the mine depth was formulated, and the results indicate that the mine depth can be an adequate predictor of the apparent earth conductivity above coal mines. Apparent earth conductivity was found to decrease with mine depth.

Jan 1, 1984

By John Durkin

Electromagnetic narrow-band signals were transmitted through the earth at 27 coal mines located throughout the United States. From those Bureau of Mines tests, apparent earth conductivity values were derived based upon a homogeneous half-space model of the earth. The derived conductivity values were found to be inversely proportional to the transmitted frequency and mine depth. A linear regression model relating the logarithm of the conductivity to the mine depth was formulated, and the results indicate that the mine depth can be an adequate predictor of the apparent earth conductivity above coal mines. Apparent earth conductivity was found to decrease with mine depth.

Jan 1, 1984

By G. J. Slavens

The Bureau of Mines has devised technology to recover cobalt, nickel, and byproduct copper from domestic lateritic material using an oxidative, ammoniacal ammonium sulfate leach. Nickel, cobalt, and copper were recovered by solvent extraction and electrowinning. To reduce the cost and complexity of cobalt recovery, an alternate method using lig-nite to extract Co3+ was investigated as reported herein. In the first 25 BV (bed volumes) of solution contacted with lignite, 97 wt pct of the Co3+ was extracted in & downflow column at pH 9.3. After 85 BV, the lignite was loaded to 1.5 wt pct Co3+ and further ex-traction was minimal. The lignite extracted cobaltic ammine complexes rather than cobalt ions and was nonselective as to other -metal cations and ammonium ions. Deleterious cations and 80 wt pct of the nonammine ammonium ions were removed prior to acid elution of the lignite. The removal of the ammines prior to elution to produce an ammonium-ion-freeCo3+ eluate was only partially successful. Thus Co3+ removal from ammoniacal solutions by lignite is technically difficult and economically unfeasible. It was also determined that reduction of Co3+ to Co2+ occurred during the extraction-elution process.

Jan 1, 1984

By Robert C. Gabler

Three filter cloth fabrics commonly used in drains for coal waste embankments were tested by the Bureau of Mines for clogging behavior and deterioration under simulated field conditions. The objective was to provide guidelines for the mining industry for the proper selection and use of filter cloths to assure safer embankments at mine waste disposal sites. The filter cloths were tested with three coal waste samples in stand-pipes used to simulate coal mine waste disposal environments. Two of the cloths showed a tendency to become clogged with fines from the wastes. One waste caused clogging by precipitating an iron-silicon compound on the test cloths. No apparent cloth deterioration resulted from exposures to the simulated coal waste environments. (The exposures ranged from 2 to 12 months.) In other tests, exposures to waters in the pH range of 2 to 12 and to reagents used in coal-preparation plants resulted in insignificant or no deterioration, as measured by tensile strength. However, long exposures to sunlight (ranging from 4.6 to 6 months) caused major deterioration in two of the cloths (86-and 98-pct losses in tensile strength) and slight deterioration in the third cloth (9-pct loss in strength).

Jan 1, 1984

By D. R. Tesarik

To ensure the stability ofa tailings pond embankment, the height of the phreatic surface must be kept at or below a safe level. In this investigation, the Bureau of Mines analyzed various horizontal drain designs for tailings embankments to determine their effects on location of the phreatic surface. This report describes the investigation, and it includes 21 dimensionless graphs that can be used to estimate the drain spacing and length dimensions necessary to ensure the stability of embankments of various configurations. Analyses were based on the use of two computer codes, a three-dimensional finite-element code and a two-dimensional finite-difference code. The computer-generated results were compared with results obtained from a laboratory embankment model, other laboratory test results, and piezomet-ric data from two actual tailings embankments. Nearly the same phreatic surface locations were predicted using either of the computer codes. For one of the actual embankments studied, the predicted phreatic surface location was slightly higher than the measured location; for the other, the predicted location closely followed the actual surface trend. Phreatic surfaces of the laboratory model were slightly higher than the code-gener-ated locations, and the differences grew larger as drain length increased or drain spacing decreased.

Jan 1, 1984

By Don B. Hunter

The Bureau of Mines investigated the extraction of alumina from calcined kaolin by leaching with boiling RCI in a train of three 50-gal continuous, stirred reactors. Slurry discharged from the reactors con-tained an excessive amount of fines, which impeded solid-liquid separation. Autogenous grinding of coarse solids that accumulated in the reactors was the source of the fines. This report describes modifications to the reactors and to the operations that led to decreased fines generation and improved solid-liquid separation. Modifications to the reactors included custom-made impellers, the addition of a baffle system, a subsurface slurry discharge system, and slower rotation of the impellers. Concurrent testing of a continuous horizontal belt filter showed that the form filtration rates were increased from 350 to almost 1,000 Ib/h+ ft-2 when the modified reactors were used.

Jan 1, 1984

By H. W. Kilau

The Bureau of Mines tested chromium-bearing waste slags from industrial stainless steel and other chrome alloy operations to determine their chromium leachability characteristics under acid precipitation conditions and to devise measures to prevent any pollution originating from this source. Two critical slag composition factors were found to control the chromium leachability: (1) CaO:Si02 ratio and (2) magnesium content. Above a 2.0 CaO:Si02 ratio, chromium exists in slag as CaO·Cr203, which can be vulnerable to leaching by acid precipitation especially if oxi-dized to CaCr04 when exposed to the environment over an extended period. Maximum chromium leachability from industrial slags occurred when the composition of the slag had about a 2.0 CaO:Si02 ratio. Between a 1.0 and 2.0 CaO:Si02 ratio, in the presence of sufficient magnesium, MgO ·Cr203 was formed, which is very resistant to oxidation and to dissolution by simulated acid precipitation. Addition of magnesium silicates to molten slag to fix the chromium in the MgO·Cr203 form was successful in preventing chromium leaching in simulated acid rain solutions. Experiments showed olivine and waste taconite tailings were suitable for this purpose. Olivine addition to a waste slag having a composition vulnerable to leaching (CaO:Si02 > 2) reduced the chromium leachability more than 80 pct.

Jan 1, 1984

By L. E. Schultze

The Bureau of Mines has devised techniques to recover lithium from geothermal brines as the chloride. More than 99 pct of the lithium was precipitated from a brine containing 170 mg/L Li by adding a solution of AICl3 and increasing the pH to 7.5 with lime slurry. The Li-Al precipitate was dissolved in HCl and sparged with gaseous HCI to recover the AlCl3; this resulted in a solution containing LiCl and CaCI2. The solution was evaporated at 1000 C to obtain a mixture of the chlorides from which 97 pct of the lithium was recovered and 90 pct of the calcium was rejected by leaching with tetrahydrofuran. The LiCl recovered by evaporation of the tetrahydrofuran was purified by dissolution in water and treatment with oxalic acid. The final LiCl solution contained 89 pct of the lithium originally present in the brine and had a purity of 99.9 pet.

Jan 1, 1984

By J. G. Groetsch

Municipal solid waste (MSW) contains about 8 pct ferrous metallics which are typically recovered by magnetic separators at municipal resource recovery facilities. At present, only about 182,500 ton/yr of MSW magnetics are being processed for remelting out of the -11 MMton/yr discarded. The Sn in MSW magnetics makes this material difficult to recycle to the steel industry. An electrolytic method using stannous fluoborate-fluoboric acid for removing Sn was evaluated. Optimum concentrations of Sn in the electrolyte and the effects of impurities such as Al, Cu, Fe, and Pb on Sn recovery from the electrolyte were evaluated. Operating parameters were 60 to 65 g/L fluoboric acid and 20 to 30 g/L Sn using stainless steel electrodes at a current density of 60 A/ft2. Tests were run with postconsumer scrap4 and MSW magnetics. Good results were obtained with MSW magnetics, after pretreatment by reshredding, magnetic separation, and air classification. The final Sn content of the MSW magnetics scrap was reduced from 0.18 to 0.017 wt pct. Heat and solvent treatments of MSW magnetics to remove coatings did not significantly improve Sn removal beyond that obtained with material that had only been mechanically pretreated.

Jan 1, 1984

By R. W. Watson

At the request of the Mine Safety and Health Administration (MSHA) the Bureau of Mines evaluated the potential hazards of three compressed oxygen self-contained self-rescuers (SCSR&apos;s) designed for use in under-ground coal mines. The evaluation followed the lines used in a similar investigation of chemical self-rescuers and involved laboratory experiments as well as field trials designed to simulate a mining environment. They included bullet impact, bonfire, feeder-breaker impact and feed-through, and mining machine runover tests. The work showed that the units were not inherently unsafe but that under certain conditions of extreme abuse they can present a potential ignition or explosion hazard. This, coupled with a survey of reported damage on SCSR&apos;s currently deployed in underground mines, which indicated a relatively high frequency of incidents leading to the destruc-tion of the units, led to new recommendations on the deployment of SCSR&apos;s. The recommendations formulated by MSHA state that the units should be either properly worn by the miner, stored in heavy containers, or otherwise protected from situations in which they might be accidentally ruptured or destroyed, such as runover by mobile mining equipment.

Jan 1, 1984

By Victor Spironello

The Bureau of Mines is studying cupola ironmel technology with the objectives of conserving high-quality raw materials through substitution and productivity. In the research re-ported here, a ize was modified by a gas-fired melting and/or ing chamber into the stack above the level of the coke bed, for study as a prototype for a coal-fired melting chamber. The modified cupola, in which natural gas was used to partially replace foundry coke, was evaluated in several trial runs. Data were obtained on furnace performance, metal and slag chemistry, and scrubber waters as particulates. Results of the modified ion were compared to those of conventional cupola operation. Although this research was preliminary--since the ultimate goal is to use pulverized coal instead of yielded ample evidence that the melting rate of a cupola can be icantly increased with less than a increase in energy input. Other evidence suggests that melting of low-density scrap can be enhanced and that scrap containing undesirable and/or oxidizable elements can be appreciably upgraded. This work is continuing and will include the use of pulverized coal of low rank to assist in melting.

Jan 1, 1984

By J. V. Scalera

Because of U.S. dependency on imported critical metals, the Bureau of Mines has conducted research to evaluate the possible substitution of nitrided low-alloy steels for higher chromium-containing alloys. The corrosion data for nitrided steels are limited primarily to the Soviet literature. The objective of this study was to determine the corrosion properties of six commercially nitrided low-alloy steels in a 5-wt % NaCl solution at pH 4. Weight-loss tests indicated that, in deaerated test solutions, most of the nitrided steels were less corrosion resist-ant than nontreated steels. However, electrochemical tests indicated that under more oxidizing conditions, nitrided materials are converted to a passive state with a significantly reduced corrosion rate. Elec-trochemical tests performed in an aerated environment confirmed the passivity of the samples in an oxidizing environment.

Jan 1, 1984