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By W. C. McLaughlin

Under a cooperative agreement, the Bureau of Mines, Magma Copper Co., and ASARCO, Inc., tested backfilled ground support systems at t.wo elevations in Magma's San Manuel, AZ, mine. The tests were mainly for guidance in designing the loading crosscuts of the new ASARCO Sacaton underground mine. Two-piece, wide-flange steel sets for 8-by 8-ft (2.44-by 2.44-m) and 11-by II-ft (3.36-by 3.36-m) openings were designed. Set spacing was 3 ft (0.91 m) and 5 ft (1.52 m), respectively. After erection, the sets were lagged with various test materials. The void between the lining and the ground was backfilled with sand and pea gravel. Instruments measuring strain (used to determine changes in stress) were placed beneath the sets and in the backfill. Results indicate the backfilled sets in the smaller drift (2315 grizzly level, panels 6 and 7) of 8-by 8-ft (2.44-by 2.44-m) cross section are a viable permanent support system, lower in cost than the standard formed concrete. Results are inconclusive in 2615 grizzly level, panels 5 and 6, where wide-flange steel sets were used with 5-ft (1.52-m) long concrete gob lagging of T-design.

Jan 1, 1983

By B. W. Madsen

A modified transpiration apparatus was devised by the Bureau of Mines to permit rapid and accurate measure of the vapor transport and vapor diffusion coefficients of antimony sulfide (Sb2S3) and other compounds at temperatures to 1,045 K. The apparatus was equipped with dual condensers and valves to switch the flow of vapor in a fraction of a second from one condenser to the other, thus allowing short-interval sampling under equilibrium conditions. Reliability of the technique was established by measuring the vapor pressure of ZnC12 as a function of temperature and comparing the results with published data. As part of an investigation of the vapor concentrations and species of accessory element sulfides associated with copper and zinc smelting, the apparatus was used to measure the rate of vapor transport and diffusion coefficients of vapor over liquid Sb2S3 as a function of temperature between 870 and 1,045 K. The calculated vapor density was combined with published direct measurements of vapor pressure to calculate the average molecular weight of the gaseous species. Average molecular weight of the vapor in equilibrium with Sb2S3 ranged from 286 to 112 g/mol over the temperature range studied.

Jan 1, 1983

By R. R. Lowery

An analysis of three 1-1/4-diam manufactured wire ropes of 6x19 classification was done to identify and describe reference conditions of new rope. Reference condition is of value when examining tested or retired ropes. Measurements of strand and rope pitch and of wire and rope diameter confirmed adherence of all ropes to those construction specifications. Mechanical properties of strength and ductility were determined by accepted methods for the ropes and wires from the ropes. Individual wires from one rope failed to meet minimum wire ductility values. Wire chemical composition varied in average carbon levels, from 0.70 to 0.78 wt pct, and in manganese content, from 0.45 to 0.80 wt pct. One manufacturer's product contained 1 to 3 wt pct Ni and Cr. Heavily wrought pearlitic steel microstructures were porous and contained inclusions. Cold work variations were evidenced by wrought grain width. Recorded anomalies reflected the condition of the manu-factured products. The report provides data that compare the three wire ropes studied, but cannot verify the effects that these conditions or anomalies have on rope service life.

Jan 1, 1983

By August J. Kwitowski

This report presents the results of a joint Bureau of Mines-U.S. Department of Energy project that evaluated a newly developed low-coal mining system: the 4M miniminer system. The evaluation took place from April through October 1981 and determined potential health, safety, and productivity factors for the mining system using the surface test facilities at Bruceton, PA. The planning, testing, results of testing, and a summary evaluation of the 4M miniminer system are included in the report. The miniminer system was found to be a very good concept with future potential for safe, healthful, and economic production in thin-seam mining. The mining system was also judged to have considerable potential for use in some coal seams that are presently considered unminable by other existing mining equipment. The preproduction, prototype version of the miniminer system that was tested suffered from several safety and production problems. These problems are also described, along with suggested remedies.

Jan 1, 1989

By S. C. Termes

The Bureau of Mines conducted research on the flocculation of various minerals with insoluble cross-linked starch xanthate (ISX) to determine its potential as a beneficiation technique for low-grade, highly dissem-inated ores and for selective desliming. Covellite, chalcocite, pyrite, pyrrhotite, chalcopyrite, bornite, sphalerite, galena, and molybdenite fines flocculate with ISX. Floc formation, floc size, and settling rate are dependent on pH, with the pH dependence differing for each mineral. Quartz is not flocculated by ISX. Experiments to obtain selective flocculation of sulfides from quartz were attempted. Good selectivity was only obtained for the bornite-quartz system. postflocculation separations resulted in flocculated bornite in grades as high as 92 pet. Evidence is presented that the flocculation of many of the sulfide minerals with ISX may involve covalent bonding of the xanthate group to lattice metal site(s).

Jan 1, 1983

By S. C. Termes, P. E. Richardson, R. L. Wilfong

"The Bureau of Mines conducted research on the flocculation of various minerals with insoluble cross-linked starch xanthate (ISX) to determine its potential as a beneficiation technique for low-grade, highly disseminated ores and for selective desliming. Covellite, chalcocite, pyrite, pyrrhotite, chalcopyrite, bornite, sphalerite, galena, and molybdenite fines flocculate with ISX. Floc formation, floc size, and settling rate are dependent on pH, with the pH dependence differing for each mineral. Quartz is not flocculated by ISX. Experiments to obtain selective flocculation of sulfides from quartz were attempted. Good selectivity was only obtained for the bornite-quartz system. Post flocculation separations resulted in flocculated bornite in grades as high as 92 pct. Evidence is presented that the flocculation of many of the sulfide minerals with ISX may involve covalent bonding of the xanthate group to lattice metal site(s). INTRODUCTIONBecause of the increasing interest in selective flocculation as a beneficiation technique for low-grade, highly disseminated ores and for selective desliming, the Bureau of Mines has been investigating the flocculation behavior of several cross-linked starch derivatives containing chelating groups. This report dis cusses the flocculation of sulfide mineral fines by insoluble cross-linked starch xanthate (ISX).Polymeric materials such as ISX, which contain a chelating group of known re¬activity towards specific mineral surfaces, were first proposed by Slater, Clark, and Kitchener (1), 3 Kitchener (2), and Attia and Kitchener (3) as selective flocculants for mineral fines with particle aggregation possible through a bridging mechanism. ISX appeared to be attractive as a sulfide mineral flocculant because (1) alkyl xanthates are known to react selectively with sulfide minerals"

Jan 1, 1983

By Bruce D. Hanson

The Bureau of Mines conducted a series of ignition tests with two types of conical bits (plumb bob and pencil) used on continuous mining machines, to determine their ignition potential at various bit speeds, cut depths, and wear conditions. The tests were conducted using single bits mounted on a 34-in-diam drum in a Bureau ignition test facility. The bits impacted blocks of Berea sandstone in a 6.5 pet methane atmosphere at various bit speeds and cut depths. In a new condition, the plumb bob bits were considerably more incendive than the pencil bits, causing ignitions in 32 of 35 tests at 60 rpm, compared with ignitiolls in 2 of 22 tests for the pencil bits. The results from new bit testing also show that reduction of bit tip velocity to 180 fpm does not eliminate ignition potential. When subjected to progressive wear, bits of both types were more incendive when they were locked in place, unable to rotate, than when they were free to rotate.

Jan 1, 1983

By J. M. Riley

The Bureau of Mines investigated a promising new technology for recovering A1203 from alunite to support the Bureau's alumina miniplant project. Results are presented for a study of the technical feasibility of treating alunite crushing and grinding reject fines for recovery of A1203. Alunite pellets having sufficient strength and resistance to degradation were produced by combining fines and coarse alunite with a KOH binder. The best pellets were prepared, in a laboratory pelletizer, by adding 1 pct KOH as a 5-pct solution to a mixture of 40 pct alunite dust (98 pct minus 65 mesh) and 60 pct coarse alunite (minus 20 plus 65 mesh). Calcines suitable for K2SO4 and A1203 recovery were produced by reducing dehydrated alunite pellets with sulfur in a laboratory shaft furnace for 4 h at 600° C, followed by air oxidation of the reduced calcine for 1 h at 600° C. This report presents design calculations, schematic diagrams, and discussions of the essential features of a proposed process research unit (PRU)--a continuous, 6-lb/h alunite shaft furnace--for studying the process.

Jan 1, 1983

By Jack L. Henry, Davis E. Traut, L. R. Penner

The Bureau of Mines conducted solvent extraction batch tests to evaluate the usefulness of neodecanoic acid ( NDA) for extracting Co 3+ from ammoniacal leach liquors high in ammonium sulfate . This work is an outgrowth of previous Bureau research in which technology was devised for the recovery of cobalt , nickel , and byproduct copper from domestic laterites . The previously devised technology uses an oxidative ammoniacal sulfate leach to treat the laterite , and nickel and copper are then recovered from the leach solution by solvent extraction and electrowinning . This report deals with the subsequent solvent extraction of cobalt from the nickel - copper raffinate solution . The results showed that about 70 pct of the contained Co 3+ can be extracted batchwise at pH 8 using NDA ( a 10 - carbon - chain highly branched carboxylic acid ) . However , NDA had a solubility of approximately 0.6 to 0.8 g / L in aqueous raffinate following extraction , and this high solubility makes it impractical for use with alkaline solutions that are low in cobalt . In addition , the extracted cobalt species ( predominately cobaltic hexammine ) is not amenable to the electrolytic recovery of cobalt metal because of its extreme stability . This fundamental prob-

Jan 1, 1965

By R. P. Walters, M. J. Lynch, D. R. Flinn

The Bureau of Mines evaluated tthhee feasibility of substituting platinum- coated metals for bulk platinum shapes as a means for conserving platinum . Platinum coatings were prepared using four different methods of electrodeposition , then tested and evaluated . In order for platinum coatings to be useful in process environments , they must be thick , adherent , stress - free , and pore - free . The Bureau evaluated direct - current , current reversal , cathode shielding , and pulsed- current plating techniques for producing a pore-free platinum electrodeposit from a molten cyanide bath . Aqueous corrosion tests of Fe - 10Cr substrates coated with approximately 25 μm of platinum showed that pulse plating yielded the most corrosion- resistant and , hence , the most pore -free coatings . The morphology of coating cross sections was in all cases columnar . The average grain size of pulse -plated deposits was independent of thickness , while all other plating techniques produced grains that increased in size as the coatings became thicker . It is believed that the constant grain size in the pulse - plated deposits resulted from better mass transport during the electrodeposition .

Jan 1, 1965

By T. L. Turner, Daniel T. Rogers

As part of a program to investigate technology for the extraction of studied HNO3 alumina from abundant domestic ores , the Bureau of Mines leaching of calcined Georgia kaolinitic clay . In this investigation , iron impurities were removed from the aluminum nitrate pregnant leach liquor by solvent extraction , and the purified liquor was evaporated to prepare a suitably concentrated crystallizer feed liquor . Aluminum nitrate nonahydrate was crystallized from the liquor to separate the aluminum from undesirable trace elements and excess water . Continuous crystallization at 40 ° C in a pilot plant vacuum evaporative unit was performed for 5 days to observe the effects of impurity buildup under minimum bleed- stream conditions . Liquor feed rate was 26 lb/h and AAll (( NNOO33 )) 33..99HH22O0 ((AANNNN)) crystal production rate was 17 lb/h . Fe 203 and Cr203 were not effectively separated from the crystals , and P205 , MgO , and K20 impurities must be removed by recrystallization . Other impurities did not excessively contaminate the crystals . Washing the crystals with water or aqueous HNO3 gave an equivalent increase in crystal purity levels by displacing mother liquor . Theoretical equations , applicable to any continuous evaporative crystallization of developed to produce material balances for engineering ANN , were applications .

Jan 1, 1965

By Dwight L. Sawyer, Roy T. Sorensen

The Bureau of Mines has investigated the recovery of alumina by hydrochloric acid leaching of calcined kaolinitic clay . Bench- scale studies indicated that horizontal belt filtration was a pprraaccttiiccaall method for separating the siliceous residue from aluminum chloride liquor generated in the leaching step . Miniplant -scale continuous testing was performed to evaluate the filter circuits and to compare filtration response of different calcined kaolin feed materials and of different agitatorbaffle designs in the leaching reactors . Soluble alumina recovery with a single filter ranged from 94 pct with minus 10 -mesh feed more than 96 pct with minus 35-mesh or misted feed . Process advantages were confirmed for the calcined misted kaolin feed material prepared by a Bureau-developed misting process . With two filters in series , an overall filtration rate of 100 lb solids /hr.ft - 2 of filter area was attained with a soluble alumina recovery of more than 99 pct . More than 99.5 pct alumina recovery was obtained with a thickener and a two - filter circuit for either the minus 35-mesh or the misted feed . Modifications in leaching reactor design made to decrease particle- toparticle attrition were successful and significantly increased filtration rates and decreased flocculant requirements .

Jan 1, 1965

By V. E. Edlund

As part of its efforts to devise new and improved methods for recovering lithium from unconventional resources , the Bureau of Mines investigated a lime -gypsum- roast , water- leach technique for processing lithiumenriched ( 0.01-0.68 pct Li ) clays . This report presents the results of a study of the technical feasibility of extracting lithium from raw material representative of clay beds associated with the McDermitt Caldera complex in Nevada and Oregon . prepared from water used Pellets suitable for bench-scale roasting studies were mixtures of minus 200 -mesh clay , limestone , and gypsum , with as the pelletizing agent . Roasting pelletized charges at 900 ° to 1,000° C temperatures for 1- to 4-h periods produced calcines that leached readily , yielding water - soluble lithium sulfate ( Li₂SO4 ) . A 5-3-3 ( weight ratio ) mix of clay , limestone , and gypsum produced calcines with the best leaching characteristics . More than 91 pct of the contained lithium was extracted from pelletized mix batches roasted in covered refractory boats . Lithium recovery decreased to about 87 pct when the mix was roasted under dynamic conditions in a gas - fired rotary furnace . A reaction mechanism was postulated which indicated that dilution and loss of SO2 and oxygen in the combustion exhaust adversely affected the leachability of the dynamically roasted calcine .

Jan 1, 1983

By Richard S. Olsen

Prior work by the Bureau of Mines demonstrated a feed preparation method that eliminates the formation of slime during leaching of calcined kaolinitic clay and makes leached residues fast settling and easy to filter. Nitric acid leaching rates determined for calcined kaolinitic clay prepared by this method were found to correspond to a zero-order reaction model for both batch and continuous, stirred-tank leach-ing. A rate constant of 0.136 min-1 was determined. Separation of solid residues from the reacted slurry was examined, and filtration rates were determined. Permeabilities of the flocculated, leached residues were around 51 darcys, or 5.0 x 10-7 cm2 for laminar flow through 4-ft-deep beds.

Jan 1, 1983

By C. O. Ruud, R. E. Siemens, D. Chandra

The mineralogical constitution of a lateritic ore dictates the type of metallurgical process that can be used to extract valuable metals such as nickel and cobalt . To provide needed mineralogical information on the interrelationships of the metals contained in domestic laterites , the Bureau of Mines awarded a grant to Denver Research Institute to study the transition - type , low - grade laterites found in northern California and southern Oregon . For comparison , limonitic - type laterites from New Caledonia and the Philippines were also studied . X-ray diffraction , electron microscopy , electron beam analysis , and conventional petrography were used to determine the mineralogical associations of nickel and cobalt in the laterites . Results showed that for both laterite types studied most of the nickel and minor amounts of cobalt are associated with the mineral geothite ( FeO ( OH ) ) . Most of the cobalt and minor amounts of nickel are associated with a mixed manganese oxide (wad ) mineral .

Jan 1, 1983

By J. E. Schiller

The Bureau of Mines is investigating methods to treat waste water that contains cyanide. This report describes a new method that removes heavy metals and all forms of cyanide. In the first step, hydrogen peroxide and sodium thiosulfate are added at pH 7 to 9 in a 1:2 molar ratio to convert free and weakly complexed cyanide to nontoxic thiocyanate. Then steryldimethylbenzylammonium chloride is added to precipitate ferro-cyanide, and finally, ferric sulfate is added as a sweep floc and sequestrant for heavy metals. After the suspended solids settle, the water is polished by filtering. The water initially contained 1 to 5 mg/L Fe, 1 to 5 mg/L Cu, and 10 to 30 mg/L total cyanide; the level of each of these constituents was reduced to less than 0.02 mg/L.

Jan 1, 1983

By R. E. Siemens, Gary L. Hundley

The Bureau of Mines has devised and demonstrated a process for recovering Ni and Co from low-grade domestic laterites . The process consists of four mmaajjoorr steps : ( 1 ) reduction roast , ( 2 ) ammoniacal leach , ( 3 ) solvent extraction , and ( 4 ) electrowinning . Several solid - liquid separation steps are required that affect the economics of the overall process . In this study , two techniques for solid - liquid separation , centrifugation and thickening , were investigated . This report presents the results of ( 1 ) laboratory and pilot plant studies to determine parameters for sizing centrifuges and thickeners and ( 2 ) an economic study of the two techniques , based on the requirements of a commercial - size ( 5,000 - tpd ) laterite processing plant . Sizing and other equipment - related recommendations , based on data from the Bureau's studies , were obtained from commercial manufacturers . The costs of thickening and centrifugation , including all the unit operations affected , were determined by the Bureau's process evaluation group . The total operating costs for separation using the two techniques ( including depreciation on the capital cost of equipment ) were found to be quite close : $ 17.26 per ton of laterite for centrifugation and $ 18.15 per ton of laterite for thickening . For centrifugal separation , the greatest cost was found to be the initial capital cost for the separation equipment ; using thickeners , the greatest cost was for reagent recovery .

Jan 1, 1983

By Arthur V. Petty

The Bureau of Mines has investigated the effect of refractory oxide additions, introduced in soluble form, on the refractory properties of 42-, 58-, and 70-pct-A1203 brick. Brick having porosities ranging from 12 to 16 pct were impregnated with solutions containing chrome, chrome-iron, zirconium, calcium, magnesium, cobalt, nickel, tin, and manganese ions. Additions of some of these ions provided dramatic improvements to such properties as hot modulus of rupture, hot load, and particularly slag resistance. These improvements can be related to reduction of porosity, amorphous grain boundary phases, formation of more refractory bond phases, and reduction of the wettability of Al203-containing refractories by metallurgical slags. Fifty-eight-percent-AI203 brick, impregnated with chrome, showed hot modulus of rupture, hot load, and slag resistance two to five times better than those of untreated 70-pct-AI203 brick. This could result in reducing the Nation's dependence on imported refractory-grade bauxite generally required for high-A1203 brick, as domestic alumina resouces could be used to produce the improved refractories.

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 Lester M. Adams

In 1980, the Bureau of Mines surveyed a group of mine seals in Randolph County, WV, to evaluate their effectiveness for reducing toxic pollutants in mine water discharges. The survey focused on 11 block wet mine seals, but mine seals of several other types were also examined. The seals were installed in 1966 and 1967 in abandoned drift portals by the Federal Water Quality Administration (FWQA), a predecessor of the Environmental Protection Agency (EPA), in cooperation with the Bureau of Mines and other Federal and State agencies, in a project known as Elkins Mine Drainage Pollution Control Demonstration Project. The seals were designed to prevent air from entering the mine portals while allowing mine water to flow out. It was believed that by preventing air from entering inactive or abandoned mines, the formation of toxic pollutants and acid mine drainage (AMD) could be reduced. Evaluation of the seals was based on water flow measurements, water analyses, and visual observations. The Bureau's 1980 data were compared with past data collected by the EPA. Several leaks and failures were observed in the clay seals, as evidenced by apparent blowouts and the absence of vegetation where the mine water surfaced. Analyses of the 1980 data indicated some improvement in the quality of water discharged from many of the wet air seals.

Jan 1, 1984