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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 Rolland L. Blake

The Bureau of Mines investigated the mineralogy, tonnage, and beneficiating characteristics of oxidized (nonmagnetic) taconite iron resources of the Western Mesabi Range as part of its program to insure adequate future domestic mineral supplies. Magnetic taconite currently provides about 95 pct of Mesabi production, but the large tonnages of oxidized taconite between the magnetic deposits will be needed to help meet future domestic demand for iron ore. Three bulk samples that represent large tonnages from the Western Mesabi Range were selected to determine their mineral composition and liberation by light optical microscopy and to test their beneficiating response. This report describes the mineralogy and liberation characteristics of the three samples of the Biwabik Iron-Formation for 26.5 mi (42.7 kID) from Keewatin to Grand Rapids, MN. (Details of response to beneficia-tion were reported previously.) The samples represent mostly material from the Lower Cherty Member of the Biwabik-Iron Formation, although one sample included some Upper Cherty Member. Minerals of all three samples were quartz (chert), hematite, goethite, and minor to trace amounts of magnetite, iron carbonate, and iron silicates. It was concluded that the oxidized taconites of the Western Mesabi Range represent a subeconomic indicated resource that can be selectively mined and beneficiated as a future large source of iron feed for steelmaking.

Jan 1, 1983

By H. William Zeller

The Bureau of Mines is conducting research to determine whether the use of chemical surfactants improves respirable coal dust control and is evaluating laboratory test criteria for selecting effective surfactants. This publication presents the results from wetting effectiveness tests with emphasis on the capillary rise test. The test variables investigated included coal particle size, type of surfactant, surfactant concentration, test duration, and mineral con-tent of the water. In addition to the rise test, measurements of con-tact angle, zeta potential, and sink time for various coal and surfactant combinations were conducted. No significant correlations among the four wetting tests were observed, a surprising result which implies that each test type measures specific aspects of the wetting phenomenon and also that each test type should only be used to select surfactants for specific applications. For example, the rise test shows solution penetration into porous materials, and the sink test discriminates among surfactants for dispersing finely ground materials into suspension. Another important conclusion is that combinations of agents retain their individual wetting properties, allowing mixtures to be for-mulated to perform well in both rise and sink tests.

Jan 1, 1983

By D. E. Shanks

The Bureau of Mines surveyed a variety of inorganic ion-exchange materials to determine their suitability for removing valuable accessory elements and troublesome contaminants from metallurgical process and waste streams. Most of the materials, which included molecular sieves, heteropolyacid salts, and hydrous metal oxides, did not give adequate separations, did not have the necessary stability in strong acids or bases, or were not in a physical form suitable for ion-exchange use. Many of the suitable inorganic materials, especially the hydrous oxides, were capable of cation exchange with high capacity only in basic conditions, which caused hydrolysis of most of the cations tested. Multivalent anions, such as arsenate and phosphate, were easily removed from acidic solutions by hydrous oxides. Hydrous zirconia was the best material for this purpose. Multivalent anions were not easily des orbed because of compound formation; therefore, conventional ion-exchange techniques could not be employed. As an alternative approach, hydrous ferric hydroxide was used as a filter material to remove arsenate and phosphate from acid solutions. One gram of arsenic was removed from solution for each 20 g of ferric hydroxide. Ferric hydroxide is preferable to hydrous zirconia for use as a filter material because of low cost.

Jan 1, 1983

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 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 M. Hayashi

The Bureau of Mines conducted laboratory studies on low-grade vanadiferous silicates from the Pumpkin Buttes and Nine Mile Lake deposits of Wyoming to examine techniques for extracting vanadium and uranium. Recovery from low-grade sources such as these could contribute to future vanadium production and reduce reliance on vanadium imports. The Pumpkin Buttes samples contained 0.03 to 0.04 pct V205 and 0.06 to 0.12 pct U308; the Nine Mile Lake samples contained 0.02 to 1.0 pct V205 and 0.06 to 0.19 pct U308" Leaching the Pumpkin Buttes samples for 18 h at 800 C with addition of 200 lb/ton H2S04 resulted in recoverey of 80 pct of the vanadium contained in the samples. The Nine Mile Lake samples were readily leached, yielding 78 to 94 pct of the vanadium after 3 h at 800 C with addition of 100 lb/ton H2S04, A solvent extraction procedure was used to selectively recover urani-um from Pumpkin Buttes and Nine Mile Lake leach solutions and to recover vanadium from the raffinates. In batch shakeout tests, Alamine 336 recovered over 95 pct of the uranium from leach solution adjusted to pH 1. Di-2-ethylhexyl phosphoric acid and Cyanex 272 recovered vanadium from the uranium raffinate after reduction and adjustment to pH 2; vanadium extractions of up to 96 pet and 92 pct, respectively, were achieved.

Jan 1, 1985

By Timothy A. Clancy

In support of research on forming ceramics from mining and processing wastes, the Bureau of Mines tested various commercial refractories to evaluate their resistance to melts of these wastes. Sixteen refractories of various types were exposed in slag erosion tests to two siliceous waste melts with Si02/CaO ratios of 4.0 and 2.2, The extent and nature of slag attack were then determined for each refractory. The nature of slag attack was investigated through scanning electron micrographs and microprobe elemental distributions. The refractories that performed best in resisting attack by the melts were high-alumina types, and of the refractories tested, the most resistant was a 90-pct-Al203, 10-pct-Cr203 refractory.

Jan 1, 1983

By P. M. Brown

The Bureau of Mines is investigating a dewatering technique for coal-clay waste that uses a flocculant, polyethylene oxide (PEO). This flocculant forms strong stable flocs that can be dewatered on a static screen. A field test unit (FTU) using this technique was operated at approximately 400 gal/min, using a waste stream from the flotation circuit of a coal preparation plant. Consolidated coal-clay material con-taining 55 to 60 pct solids was produced when the flotation circuit slurries of 2.7 to 8 pct solids were treated with 0.1 to 0.3 Ib PEO per ton of solids. The FTU was also operated at 64.5 and 87.5 gal/min using a portion of the underflow slurry from the preparation plant's thickener. Consolidated coal-clay material containing 55 to 60 pct solids was produced when the thickener underflow slurries of 19 to 24 pct solids were treated with 0.08 to 0.2 Ib PEO per ton of solids. PED-treated materials continued to dewater when placed in a pit.

Jan 1, 1983

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 G. B. Atkinson

The Bureau of Mines investigated a method for increasing the leaching rate of bulk superalloy scrap to facilitate recycling and recovery of critical metals such as Ni, Co, and Cr. Three superalloys were investi- gated, the cast-nickel-base superalloy IN-738, the wrought-nickel-base superalloy Rene-41, and the cast-cobalt-base superalloy Mar-M-509. Superalloys melted with 20, 30, 40, and 50 pct Al metal to form inter- metallic compounds were easily crushed to a convenient particle size and reacted rapidly with acid solutions which dissolved the metals. For example, leaching 1/2-in pieces of unalloyed IN-738 with excess 6N HC1 at 95° C for 2 h dissolved about 0.5 pct, while leaching 10 g of minus 20-mesh 30 pct Al-70 pct IN-738 with excess 6N HC1 at 95° C for 2 h dis- solved 96.2 pct.

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 K. J. Ladwig

The Bureau of Mines conducted a field investigation of the water quality in inundated underground coal mines in the Northern Anthracite Field, eastern Pennsylvania. Water samples were collected at multiple depths from nine abandoned mine shafts in the Wyoming Basin, ranging from 68 to 650 m (223 to 2,132 ft) in depth and intersecting as many as seven mined seams in a single shaft. The shafts were also monitored for fluid resistivity, fluid temperature, Eh, and pH using downhole instrumentation. The monitoring program showed that the formerly highly acidic mine water is now slightly alkaline. Sulfate concentrations decreased as much as 74 pct in the flooded workings and 54 pct at a mine water discharge from values reported in 1964 and 1968, respectively. These data are consistent with the inhibition of pyrite oxidation and gradual flushing of oxidation products in flooded mine environments. The monitoring program also revealed significant vertical stratification in water quality in five of the nine shafts, each characterized by two easily recognizable zones. The transitions between zones were sharp, marked by rapid changes in Eh, pH, and ionic composition, the upper zones being less contaminated than the lower zones. The development of stratification appears to be a function of shallow localized flow conditions, arising primarily from the relative positions of mine openings and structural features of the coalbeds.

Jan 1, 1984

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 L. P. Kleinmann

To control the formation of acid drainage at its source, the Bureau of Mines has investigated the role of iron-oxidizing bacteria in the oxidation of pyrite. In laboratory tests, it was determined that Thio-bacillus ferrooxidans could be controlled in coal refuse using anionic surfactants, with an associated decrease in acid production of about 75 pet. Based on these results, large-scale tests were conducted at an 8-acre active coal refuse area in northern West Virginia and an 11-acre inactive refuse pile in southern West Virginia. Acid production was decreased 60 to 95 pet for 4 to 5 months after application of 55 gal/ acre of 30-pct sodium lauryl sulfate solution. To date, effluent surfactant concentrations have been extremely low. Either a hydroseeder or a road-watering truck can be used to apply the surfactant. Since the surfactant solution must reach the pyritic material to be effective, sites that have been reclaimed are generally not amenable to these procedures. A simple laboratory test is described that provides an estimate of adsorption potential; this can be used to calculate a safe application rate.

Jan 1, 1983