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By J. P. Bennett

Based on previous Bureau of Mines research indicating that improved high-temperature properties could be achieved for periclase refractories through chemical additions, the Bureau investigated the properties of full-size bricks produced from chemically modified periclase refractory grains and the suitability of making such chemical additions to Mg(OH)2 slurries prior to production of the periclase grains. In full-size brick testing, strength values, both hot and cold, for the optimized bricks were superior to those for a commercial 98-wt-pct-MgO refractory. The best results were obtained for a natural magnesite with an adjusted CaO:Si02 (C:S) ratio of 3.0 and a 1.0-wt-pct addition of Zr02 and for a seawater periclase with an adjusted C:S ratio of 2.5 and a 0.5-wt-pct addition of Mn02. For samples produced from chemically modified Mg(OH)2 slurries, additions of both Mn02 and Zr02 and an increase in C:S ratios produced significant increases in hot flexural strength, similar to those resulting from chemical additions made to periclase grains. The most effective modifications were additions of Mn02 to brine-derived periclases having a C:S ratio adjusted to 3.0. These results on chemically modified magnesia refractories indicate that such material could potentially substitute for magnesiachrome refractories containing imported chromite.

Jan 1, 1984

By D. J. MacDonald

The Bureau of Mines has conducted bench-scale investigations leading to the design of an integrated process for producing reactor-grade zir-conium oxide (Zr02) from zircon sand, which avoids the air pollution, water pollution, fire hazard, and odor problems associated with the hexone-thiocyanate process. The integrated process consists of three steps: production of crude zirconyl sulfate solution, solvent extraction, and production of Zr02 from strip liquor. This report describes the solvent extraction step. Multistage, countercurrent liquid-liquid extraction with a tertiary amine in kerosine was used to separate zirconium from a dilute H2S04 solution containing hafnium and other impurities. Process steps de-scribed include extraction from an aqueous feed solution to form a hafnium-contaminated, zirconium-bearing organic-phase solution, scrubbing to separate zirconium from coextracted hafnium, stripping to transfer hafnium-free zirconium into an aqueous strip liquor, chloride-loading to produce a chloride-bearing organic solution, scrubbing with the chloride-loaded organic solution to remove traces of uranium impur-ity from the zirconium-bearing strip liquor, and regeneration to pre-pare the organic solution for reuse. These steps were performed simul-taneously in steady-state, bench-scale experiments. Zirconium recovery of up to 93 pct was achieved. Results of an economic evaluation are included.

Jan 1, 1984

By J. P. Bennett

The Bureau of Mines is investigating the acid resistance of ceramic materials to identify construction materials for emerging technology in chemical and metallurgical processes. Eight commercial ceramic materials, including two red shale, two fireclay, a silica, a silicon carbide, a carbon, and a high-alumina brick, were evaluated. Samples were exposed to 40 wt pct HN03 at 70° and 90° C and 60 wt pct HN03 at 50°, 70°, and 90° C for time periods of 110 days. Statistically significant changes in cold crushing strength were generally small or not detected, except for a strength drop in the high-alumina brick, which decreased in strength when exposed to the chosen acid concentrations at 90° C. Vol-ume and weight changes were also measured. The leach rates of Al, Ca, Fe, K, Mg, Na, Si, and Ti were monitored. Increasing temperature or a decrease in the acid concentration resulted in an increased ion leach rate. Of the conditions tested, the most severe corrosion occurred at 90° C for a 40-wt-pct-HN03 solution. The silica brick had the best overall acid-resistant properties, followed by a red shale and a fire-clay brick. The carbon and silicon carbide bricks are not recommended for service.

Jan 1, 1984

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 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 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 R. E. Green

The Bureau of Mines undertook a bench-scale study of three different types of oxidized taconites3 from the Lake Superior district to improve the dispersion-selective flocculation-desliming process for beneficiating these materials. The response-surface contours of the effects of dissolved ionic species in the water and of three dispersion systems on the selective flocculation process were studied. Results of metallurgical data and chemical analyses of the aqueous phase showed that the water quality affects the performance of the selective flocculation process.

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 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 W. K. Tolley

This report presents data collected during research by the Bureau of Mines on corrosion of grinding media. Corrosion rates of eight alloys commonly used in grinding media were tested in synthetic mill water using an ultrasonic grinding device especially designed for this work. Electro-chemical measurements showed variations in corrosion rates for these alloys between 9.8 mpy for medium-carbon steels and 0.14 mpy for high chromium white irons. Bureau data are discussed along with data from the literature to indicate that corrosion causes less than 10 pct of the wear of grinding media in commercial grinding mills. A comparison of corrosion rates for various types of grinding media shows that alloying elements and electrochemically active inclusions in steel affect the corrosion behavior of the media.

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 E. Morrice

The Bureau of Mines investigated methods for beneficiating platinum-palladium ores from the Stillwater Complex, Montana. Results of bench-scale and pilot-scale studies employing froth flotation to recover sulfide concentrates containing platinum-palladium values from a serpentinized ore are presented. Best results in the pilot mill were obtained with a sodium isobutyl xanthate-normal dodecyl mercaptan col-lector combination at a natural pH of 8.2. A rougher concentrate con-taining 1.7 oz/ton Pt and 4.7 oz/ton Pd was prepared. Recoveries of platinum and palladium were 96 pet and 86 pet, respectively. Batch cleaner flotation of rougher concentrates yielded concentrates contain-ing 3.7 oz/ton Pt and 9.8 oz/ton Pd.

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

By T. E. Ackman

Scale inhibitors and slow-release polymers were tested by the Bureau of Mines at mine drainage treatment facilities. The scale inhibitors were investigated to determine their effectiveness in controlling gypsum (CaSO4) scale; the polymers were investigated to determine their effectiveness for increasing settling rates of suspended iron hydroxide. Two types of scale inhibitors were tested at a site having a severe CaSO4 scaling problem. Both proved to be effective in controlling scale formation; in addition, one caused the dissolution of CaSO4 deposits. Slow-release polymers were tested at three mine drainage treatment facilities. These gelatinous polymeric flocculants were found to be convenient and easy to use, but only effective when pH could be controlled.

Jan 1, 1984

By S. C. Rhoads

The Bureau of Mines is investigating low-chromium alloy substitutes for type 304 stainless steel (type 304 SS). The purpose of the research is to reduce the chromium content in austenitic stainless steels used for corrosion-resistant applications. Nine Fe-9Cr-12Ni alloys containing additions of 0 to 5 pct Mo, 0 to 2 pct V, and 0 to 2 pct Cu were selected for evaluation. All of the experimental alloys containing 5 pct Mo and an alloy containing 2Mo-2V-2Cu possessed structure and tensile strengths similar to those of type 304 SSe Alloys containing SMo-2V and SMo-2V-2Cu had ac-ceptable welding properties as measured by the Varestraint test. Alloys containing at least 2 pct Mo had cQrrosion resistance comparable to that of type 304 SS in solutions of nitric acid, phosphoric acid, acetic acid, and citric acid. In chlorides, all the experimental alloys were susceptible to localized corrosion and stress corrosion cracking similar to that of type 304 SSe The corrosion properties were established by weight-loss tests, electrochemical polarization tests, and stress-corrosion cracking tests. An Fe-9Cr-12Ni-SMo-2V alloy and an Fe-9Cr-12Ni-SMo-2V-2Cu alloy had a combination of welding properties, tensile properties, and corrosion resistances that were most comparable to those of 304 SS.

Jan 1, 1984

By M. M. Tilman

The Bureau of Mines evaluated corrosion resistance of Split Set friction rock stabilizer mine roof bolts to aid in better prediction of useful service life. Electrochemical corrosion testing was conducted utilizing an automated corrosion measurement system. Natural and/or synthetic mine waters from four uranium and two copper mines were the test media for the two types of high-strength, low-alloy (HSLA) steels from which Split Set stabilizers are manufactured, and for galvanized steel. Tests were conducted with waters of minimum and maximum dissolved oxygen content at in-mine water temperatures. Retrieved Split Set stabilizers were also evaluated for property changes. Galvanized steel was found to be far superior to the unprotected steel in general corrosion resistance; limited tests indicate little ten.dency to pitting, contrary to behavior for the uncoated steel. Copper-bearing HSLA steel was slightly more corrosion resistant than non-copper-bearing HSLA steel. Statistical analyses resulted in development of equations relating dissolved oxygen, chloride, sulfate, and magnesium contents of mine waters to corrosion rates of the two HSLA steels (nongalvanized). An equation was developed that relates corrosion rates of galvanized steel to mine water temperature and dissolved oxygen content. Variable conditions in mine environments make corrosion damage difficult to predict and emphasize the need for corrosion prevention and control.

Jan 1, 1984

By Arthur V. Petty

The Bureau of Mines has researched the utilization of mining and pro-cessing wastes as raw materials for the production of glass-ceramic pipe. Characterization of various wastes as to occurrence and chemical composition is reported. A computer program was developed and used to identify waste materials and mixes that would result in glass melts from which glass-ceramics could be produced after cooling and subsequent heat treatments. The production of abrasion-resistant pipe from inexpensive and readily available domestic resources could offer an economical substitute for high-alloy steels containing the critical and strategic materials cobalt and chromium.

Jan 1, 1984