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By Charles L. Kusik

As part of an effort to establish processes that could be exploited in case of adverse changes in international chromium production and trading patterns, this study was sponsored by the Federal Emergency Management Agency (formerly the Federal Preparedness Agency) through the Bureau of Mines, to experimentally determine the feasibility of recovering chromium from critical scrap metals containing significant quantities of this element. Based on a conceptual pyrometallurgical chromium recovery flowsheet developed at Arthur D. Little, Inc., the experimental program described in this report demonstrated key process steps for the recovery of chromium as ferrochromium in a batch process. The process involves oxidation of chromium into a slag phase, subsequent separation of the slag phase from the remaining metal, followed by reduction of chromium from the slag phase to produce ferrochromium.

Jan 1, 1981

By R. E. Peterson

The Bureau of Mines has undertaken beneficiation investigations on samples representing large tonnages of oxidized taconites in order to develop and evaluate applicable technologies for producing iron oxide concentrates from these materials. Information derived from the investigations can be used to expand the domestic iron raw-materials base and to establish the impact these taconite deposits may have on future national iron ore requirements. This report describes a process that includes reduction roasting, magnetic separation, and flotation, applied to a western Mesabi Range sample taken near Coleraine, Minn. The sample contained 36.8 pct iron and 46.0 pct silica, and represented 0.5 to 1 billion tons of crude material. An average of 962 lb/hr of oxidized taconite was roasted with 33 lb/hr of lignite in a 35-foot-long rotary kiln. Pulverized lignite and natural gas maintained the kiln operating temperature at 850° C. The roasted taconite was beneficiated by magnetic separation and cationic flotation in a 900-lb/hr pilot plant and yielded a product analyzing 68.1 pct iron and 4.6 pct silica, and containing 82.4 pct of the iron in the kiln feed.

Jan 1, 1981

By Joseph A. Perry

One goal of the Bureau of Mines is to develop technology tp insure a dependable supply of minerals to the United States. To support this goal, the Bureau's Albany Research Center has modified a commercial atomic absorption spectrophotometer to rapidly determine trace levels of mercury by cold-vapor atomic absorption spectrophotometry. Such diverse materials as ores, mill products, stream water, sediments, and flue dust have been analyzed. A very high dynamic range of 0.2 ng/ml to 1 µg/ml of mercury in solutions is routinely analyzed by this instrument.

Jan 1, 1981

By Donald A. Wilson

As part of a continuing effort to maximize metal recovery from domestic secondary resources, the Bureau of Mines investigated a process for recovering the metallic portion of scrap alkaline batteries. A pyrometallurgical method for recovering nickel and cadmium from Ni-Cd scrap batteries previously developed on a laboratory scale, was scaled up to 25-and 43-pound charges. The method employed reduction and/or decomposition in a retort using a minimum of 2.5 percent carbon as a reductant. Metallic cadmium was distilled at atmospheric pressure and a minimum of 900° C. Purity of the recovered cadmium was 99.8 percent minimum and the nickel-iron residue contained less than 0.02 percent cadmium.

Jan 1, 1981

By A. T. Iannacchione

Roof-rock instability in advancing sections of underground coal mines is a major contributing factor to accidents resulting in fatalities and injuries. Such roof-rock conditions can also result in loss of production due to additional cleanup time and increased amounts of reject material. The Bureau of Mines is investigating fundamental geologic factors affecting coal mine roof-rock instability in order to develop techniques to predict zones of potential unstable roof-rock. Two distinct directional trends of unstable shale roof-rock in a mine working the Upper Kittanning Coalbed are delineated: one trend is associated with the sandstone-shale transition zone, the other with a fault system. The unstable shale roof-rock associated with the transition zone, a consequence of differential compaction, is comprised of slickensided roof-rock. Whereas, the unstable shale roof-rock associated with the fault system, a consequence of structural deformation of the strata, is comprised of fault planes. These faults, small in comparison to the sandstone-shale transition zone, are difficult to delineate with a standard drilling program. Trends of the transition zone associated with the sedimentary facies change are projected into unmined portions of the coalbed with the aid of exploration core data.

Jan 1, 1981

By Benjamin W. Haynes

Materials from phosphate rock mining and processing were analyzed for fluorine and uranium content as part of the Bureau of Mines program to more effectively recover resources from mining and mineral processing reject materials. The analysis of both feed and waste materials generated in the beneficiation and acidulation of phosphate rock was performed to obtain information on the disposition and concentration of these elements in phosphate rock processing streams. Fluorine was determined by a distillation-titration method and by ion chromatography. Uranium was determined by the dibenzoylmethane (DBM) method, the reliability being confirmed by roundrobin analysis of samples within Bureau of Mines research centers. National Bureau of Standards (NBS) Standard Reference Material (SRM) 120b-Phosphate Rock was also analyzed for fluorine and uranium to verify procedures and results. Fluorine values ranged from 0.3 wt-pct in gypsum filter cake to 3.7 wt-pct in phosphate rock concentrate. Uranium ranged from less than 5 µg/g in gypsum filter cake to 200 µg/g in a dried clay slime.

Jan 1, 1981

By G. L. Finfinger, J. Cervik, L. J. Prosser

The Bureau of Mines has completed an underground degasification project in which an underground piping system was used to transport methane from the coalbed to the surface. In a 10-month period four horizontal holes were drilled to an average depth of 1,450 feet. All four holes were surveyed vertically and azimuthally. In 991 days of degasification, 255 MMcf of gas was drained from the coalbed. The underground piping system proved to be a safe and effective means of transporting methane from the coalbed to the surface.

Jan 1, 1981

By L. J. Prosser

The Bureau of Mines has completed an underground degasification project in which an underground piping system was used to transport methane from the coalbed to the surface. In a la-month period four horizontal holes were drilled to an average depth of 1,450 feet. All four holes were surveyed vertically and azimuthally. In 991 days of degasification, 255 MMcf of gas was drained from the coalbed. The underground piping system proved to be a safe and effective means of transporting methane from the coalbed to the surface.

Jan 1, 1981

By Philip A. Holland

The Bureau of Mines has developed a method for determining helium in water for use in sampling and analyzing surface and subsurface waters for geochemical survey work. The accuracy of the analytical method is within ±10 percent for samples containing above 20 x 10-8 cm3 He (STP)/cm3 H20. The minimum detectable helium-in-water concentration is calculated to be 2 x 10-8 cm3 He (STP)/cm3 water. Water samples are collected in 500-cm3 stainless steel cylinders. The dissolved gases are extracted into a cylinder of equal volume containing a known quantity of neon. The resulting gas mixture is subsequently analyzed for helium and neon-21 by mass spectrometry. The volume of helium in the sample is calculated from the mass spectrometric determination of the helium-to-neon-21 ratio, the known quantity of neon used, and the extraction efficiency of helium.

Jan 1, 1981

By Nicholas P. Kripakov

The U.S. Bureau of Mines examined the applicability of existing material models to solve practical geotechnical mining-related problems by solving a yielding pillar stability problem considering confining effects on strength. Numerical difficulties normally encountered with modeling strain softening behavior were eased with a simplified computational procedure using a quasi-elastic approach to account for residual strength after initial failure. Although in agreement with a confined-core pillar design method using actual mine conditions that include mine layout geometry, overburden geology, and rock properties of the deposit and surrounding structure, the results cannot be verified because measured field data are not available at this writing.

Jan 1, 1981

By L. E. Schultze

As part of its goal of maintaining an adequate supply of minerals to meet national economic and strategic needs, the Bureau of Mines devised a processing sequence for recovering uranium from carbonaceous ores. Uranium extractions of 97 pct were obtained by contacting the ore with a solution containing 400 grams of ferric sulfate hydrate in 200 ml water for 3 hr at boiling temperature (96° C). Uranium was recovered from the leaching solution by solvent extraction with tri-issooctyl amine. The barren ferric sulfate solution was recycled to the leaching system. The leaching process resulted in no detectable dissolution of carbonaceous material from the ore. Work on the project was terminated in 1978 because of a transfer of responsibility to the U.S. Department of Energy.

Jan 1, 1981

By R. R. Backer

The Bureau of Mines, in cooperation with Washington Irrigation and Development Co. (WIDCO), evaluated the dewatering of fine coal-refuse slurry using chemicals and various types and combinations of drains in natural earth impoundments. About 40 lb of lime and 2 lb of polymer per ton of dry solids were mixed with the underflow from the preparation-plant thickener. Clear, free water was immediately liberated from the slurry. The percent solids by weight of the slurry increased from about 17 to 30 immediately, and after 5 days increased to 45 wt-pct. This indicates a threefold reduction in total volume after 5 days from 172 cu ft/ton solids originally to 56 cu ft/ton solids.

Jan 1, 1981

By T. L. Hebble

The Bureau of Mines investigated a hydrometallurgical procedure to recover Co, Ni, and Cu from an electrolytic zinc industrial copper filter cake. The copper filter cake is presently unmarketable or of low value because economic and environmentally acceptable processing technology is lacking. Research by the Bureau of Mines has developed a multistage process for recovering or recycling over 93 pct of the Zn, Cd, Cu, Co, and Ni from this material. The stages involved are (1) wet sizing, (2) H2S04 leaching of undersized material, (3) H2S04-Mn02 leaching of H2S04 leach residue, (4) selective precipitation of As, Cu, and Co-Ni products, and (5) precipitation of manganese for recycling to the leach circuit. The final process residue is only 1.6 wt-pct of the initial cake and consists of lead sulfate.

Jan 1, 1981

By J. W. Walkiewicz

The Bureau of Mines investigated alloys containing mischmetal (MM), cobalt, copper, magnesium, and iron for use in permanent magnets in place of the scarce samarium-cobalt alloys. The magnetic properties of MM-Co, MM-Co-Cu, MM-Co-Cu-Mg, and MM-Co-Cu-Fe-Mg alloys were evaluated. Magnets were fabricated by powder metallurgy consisting of arc-melting the metals, crushing and grinding the resultant alloys, alining and compacting the powder, and sintering the compacts. Magnetic values of MHc = 4.7 kOe, BHc = 4.07 kOe, Br = 6.81 kG, and (BH)max = 10.0 MGOe were obtained with a MM-Co alloy containing 36±0.5 wt-pct MM. By substituting copper and magnesium for part of the cobalt, the values for MHc and BHc were increased to 29.0 kOe and 5.89 kOe, respectively. This intrinsic coercivity value exceeded that of Sm-Co alloy obtained in our laboratory. The addition of iron to MM-Co-Cu-Mg alloys resulted in an increase of Br to 6.90 kG and (BH)max to 10.3 MGOe. Copper and magnesium contents of these alloys were optimized to obtain maximum values of MHc.

Jan 1, 1981

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

By C. D. Litton

Submicrometer particle concentrations and average particle sizes were monitored for four full-scale sealed coal fires in the multiple-entry section of the Bruceton Experimental Mine. The data from these tests indicate that there exists a very good correlation between the submicrometer particle concentrations and the maximum temperatures measured within the coalbed. As the maximum coalbed temperature decreases with time after sealing, the submicrometer particle concentrations show a corresponding reduction. This particle-temperature correlation is in sharp contrast to the gas concentration data obtained, for which essentially no correlation exists with the measured coal-bed temperatures. The results of these full-scale tests indicate that the measurement of submicrometer particle concentrations may be a more realistic approach to determining the status of underground sealed fire areas.

Jan 1, 1981

By R. K. Koch

The Bureau of Mines produced several series of titanium castings in order to investigate the feasibility of producing commercial-grade titanium castings in bentonite-bonded olivine or zircon sand molds. The use of these molds for titanium casting was investigated as a possible alternative to the industrially used rammed graphite process. Parameters investigated were mold mixtures, mulling, gating, venting, drying, and mold washing. The investigators found that castings with superior ductility and fatigue life, compared with rammed graphite castings, could be made by fume-free pro-cesses in molds bonded by western bentonite, using either olivine or zircon sand. Zircon molds were satisfactory for both light-and heavy-sectioned castings. However, olivine molds were suitable only for light-sectioned castings because the mold-metal reaction became excessive during the pouring of heavy-sectioned castings.

Jan 1, 1981

By Seth C. Schaefer

The Bureau of Mines has determined the standard Gibbs energies (AGf°) of CoS1.035 (cobalt sulfide) and Ni2.515S2 (nickel sulfide) with high-temperature galvanic cells using stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, CoS1.035, CoO, S02(g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt, with the overall cell reaction C0S1.035(c) + 1.535 02(g, 0.0114 atm) = CoO(c) + 1.035 S02(g)¬ These results, combined with the best available data for ?Gf° of CoO and S02 from the literature, give the standard Gibbs energy of formation of CoS1.035 for the reaction Co(c) + 0 5175 S2(g) = CoS1.035(c) ?Gf° = -38.890 + 18.87 x 10-3T ± 0.185 kcal/mole (866.0 - 1,104.9 K), where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, N12.515S2, NiO, S02(g, 1 atm)//Zr02//02(g, 0.0122 atm), Pt, with the overall cell reaction Ni2.515S2(c) + 3.2575 02(g, 0.0122 atm) = 2.515 NiO(c) + 2 S02(g). Combination of these results with data for ?Gfo of NiO and S02 from the literature yields the standard Gibbs energy of formation of Ni2.515S2 for the reaction 2.515 Ni(c) + S2(g) = Ni2.S1SS2(c) ?Gf° -65.377 + 24.67 x 10-3T ± 0.541 kcal/mole (968.6 -1,053.7 K).

Jan 1, 1981

By A. V. Petty

In accordance with its objective to maximize minerals recovery from secondary domestic resources, Bureau of Mines conducted research on recycling chrome refractory wastes. Since 20 pct of the U.S. demand for imported chromite is used in the production of refractories, primarily for the steel, copper, and glass industries, samples of used chrome-containing refractories from copper converter and reverberatory furnaces were investigated to determine their potential for recycling. The samples were beneficiated using a combination of wet magnetic separation, flotation, and leaching techniques, and the concentrates were reformed into briquets for refractory evaluation. Small refractory test specimens produced from the beneficiated concentrates gave modulus of rupture values at 1,350° C comparable to those of commercial mag-chrome brick of similar composition; however, grinding the waste refractories to at least minus 65-mesh was required in order to liberate the metallic copper. Most of the copper was easily recovered using conventional beneficiation techniques, but the finely ground chrome concentrate would require briquetting, calcining, and crushing to produce a coarse grain suitable for recycling into secondary mag-chrome refractories.

Jan 1, 1981

By J. H. Maysilles

The Bureau of Mines is conducting research on various technologies to recover alumina from domestic resources for feedstock to existing aluminum smelting capacity as a means to reduce dependence on imported bauxite, which represents 93 pct of U.S. aluminum requirements. One of the more promising technologies being investigated is the hydrochloric acid leaching of kaolinitic clay. In the hydrochloric acid leaching technology, alumina is recovered from iron-free aluminum chloride leach liquor and separated from impurity elements by sparging the liquor with HC1 gas to crystallize aluminum chloride hexahydrate (ACH). A large-scale crystallizer with a 336-gallon usable volume was constructed and operated to obtain engineering and design data for potential scale up and to demonstrate the ability of the technology to produce specification grade alumina. Test campaigns involving about 1,400 hours of operation were completed. ACH meeting all chemical purity requirements could not be produced by a single crystallization, but was produced by recrystallizing the product from the calcined kaolin clay leach liquor. Product crystals with a size distribution of more than 80 pct plus 100 mesh and 65 pct plus 65 mesh were made at a rate of 10 pounds of ACH/(hr)(ft3). The zirconium tube heat exchanger used to maintain constant process temperature operated with an over-all heat transfer coefficient of 420 to 500 BTU/(hr)(ft2)(°F).

Jan 1, 1981