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By J. A. Eisele

The Bureau of Mines conducted bench-scale cyclic tests to determine the composition of recycled leach liquor in the Bureau?s proposed clay/HCl leach/ HCl sparge process for producing Al203 from clay. The data developed from these tests make it possible to synthesize leach liquors for predetermined steady-state operating conditions when conducting large-scale crystallization tests. The results of two sparge tests were compared. One was a 20-cycle test with a 36-pct-HCl concentration in the mother liquor; the other was a 10-cycle test with a 26-pct-HCl concentration in the mother liquor. The effect of impurity concentrations in the leach liquor on the purity of aluminum chloride (AlCl30?6H20) crystals was determined, but there was poor correlation between this data and results that have been obtained from miniplant-scale work.

Jan 1, 1980

By R. F. Farrell

A goal of the U.S. Department of the Interior, Bureau of Mines, is the advancement of minerals technology through the development of improved metals and minerals processing. In support of this goal, the Bureau of Mines has developed a general method for preparing solutions from a wide range of metal and mineral samples for chemical analysis. The development of the method from current knowledge of vessel material, pressure dissolution techniques, and the fluoride-boric acid reaction is given. The method uses 7 ml of a mixture of HC1-HNO3-HF acids in a ratio of 3.5:2:1.5 sealed in plastic bottles that act as pressure vessels when heated in a boiling water bath. A final volume of 100 ml is obtained by the addition of 93 ml of a 1. 5-pct H3BO3 solution to the bottles, which are reheated; precipitated fluorides as well as sample residue are dissolved by the fluoride-boric acid reaction. A copper slag and a steelmaking slag treated using this method were analyzed by atomic absorption spectroscopy yielding values for Si, Mg, Ca, AI, Fe, Mn, Na, As, Pb, Sb, and Zn very close to certified values with an average relative standard deviation of 2.13 pct. The low cost, reduction in preparation time, ease and safety of sample handling, conservation of reagents, and ability to dissolve volatile materials without loss make this method superior to traditional wet digestion techniques for many materials, and ideal for use with atomic absorption, and optical emission or X-ray emission spectroscopy.

Jan 1, 1980

By J. E. Schiller

The Bureau of Mines has investigated the surface charge of amphibole asbestos fibers and nonasbestiform cleavage fragments, as part of the Bureau's fundamental studies to provide new knowledge on the physical and chemical properties of the amphibole minerals. Microelectrophoresis was used to measure the electrophoretic mobilities, in water, of particles from six asbesti-from amphiboles and seven nonasbestiform amphiboles over the pH range of 5 through 9. The particles generally ranged in size from 2 to 5 µm wide by 10 to 30 µm long. The isoelectric point was determined for four of the minerals, and values were found to be between pH 3.5 and pH 5. The minerals studied had zeta potentials that generally ranged from -25 to -so mv in neutral solution. Attachment of colloidal positively charged AgI was also studied as a means of determining surface charge. Scanning electron microscopy of amphibole particles that had been in contact with aqueous AgI showed equal attachment of AgI to asbestos fibers and to cleavage fragments; the extent of AgI coating was the same for both. The electrophoretic mobilities of asbestos fibers were essentially the same as those of elongated cleavage fragments of the same aspect ratio (particle length divided by width). Blocky particles from both asbestiform and nonasbestiform specimens had lower mobilities.

Jan 1, 1980

By S. A. Matthes

This Bureau of Mines report describes analysis of a copper slag for 13 elements from a single sample solution by flame atomic absorption spectroscopy. Samples are dissolved with 7 ml of an HC1-HF-HN03 (3:1.5:2) mixture in heated plastic pressure vessels. A 1.5-pct boric acid solution is added to dissolve precipitated fluorides and to reduce matrix effects that interfere with atomic absorption analysis. Preparation time is less than 1 hour per batch of 10 samples. Total analysis time is less than 6 person-hours for 130 determinations with an average relative standard deviation of 1.83 pct for the 13 elements. Simple acid standards were used for all determinations. Values obtained by this method are in excellent agreement with values obtained by slower, more costly procedures.

Jan 1, 1980

By David E. Siskind

The Bureau of Mines studied airblast from surface mining to assess its damage and annoyance potential, and to determine safe levels and appropriate measurement techniques. Research results obtained from direct measurements of airblast-produced structure responses, damage, and analysis of instrument characteristics were combined with studies of sonic booms and human response to transient overpressures. Safe levels of airblast were found to be 134 dBL (0.1 Hz), 133 dBL (2 Hz), 129 dBL (6 Hz), and 105 dB C-slow. These four air-blast levels and measurement methods are equivalent in terms of structure response, and anyone could be used as a safe-level criterion. Of the four methods, only the 0.1-Hz high-pass linear method accurately measures the total airblast energy present; however, the other three were found to adequately quantify the structure response and also represent techniques that are readily available to industry. Where a single airblast measuring system must he used, the 2-Hz linear peak response is the best overall compromise. The human response and annoyance problem from airblast is probably caused primarily by wall rattling and the resulting secondary noises. Although these will not entirely be precluded by the recommended levels, they are low enough to preclude damage to residential structures and any possible human injury over the long term.

Jan 1, 1980

By K. Robert Dorman

This Bureau of Mines report describes laboratory and field experimentation in building mine ventilation stoppings, air-door frames, and fan bulkheads with a civil construction technique. Shotcrete is applied to a free-standing, three-dimensional wire-truss panel, which is easily cut and rapidly erected. In mines where shotcrete equipment is available, this technique should be faster and cheaper than conventional block-and-mortar or monolithic concrete construction.

Jan 1, 1980

By Arne Landsberg

Accessory metals, although valuable resources, present possible environmental concern in the smelting of base metals. The Bureau of Mines, U.S. Department of the Interior, has undertaken research to define the chemistry involving these metals. Arsenic in copper smelting is the first to be investigated. Roasting, the first step in many copper smelters, was chosen for initial investigation because of the potential for arsenic removal in this primary process. Simple, static-bed, vaporization experiments were devised to obtain the data in this study. Ancillary transpiration and mass spectrometry were also used to delineate conditions necessary for arsenic volatilization from a roaster feed. For nearly complete arsenic removal, a temperature of 650°-700° C, a reducing atmosphere including carbon monoxide, and a source of sulfur were found to be essential.

Jan 1, 1980

By Robert Blickensderfer

Equipment and procedure for the continuous roll bonding of metal strips are described. The reels, mill rolls, and furnace were located within a vacuum chamber capable of operation at a residual gas pressure of 1 x 10-4 to 1 x 10-5 torr. Several metals were successfully clad at rolling temperatures of 930° to 1,050° C in lengths up to 120 ft. The bimetals that were clad included stainless steel to carbon steel, molybdenum and nickel to stainless steel and carbon steel, and titanium to carbon steel. Bend tests of bond integrity are described, and microstructures of the interfaces are presented. The amounts of brittle intermetallic phases formed at the interface are minimized by this cladding method.

Jan 1, 1980

By G. W. Elger

The Bureau of Mines conducted laboratory and larger scale studies on samples of domestic perovskite and ilmenite ore concentrates to devise a procedure for recovering TiC from these ores. From the concentrates, mixtures of titanium and calcium carbides were produced. The carbides were then ground and reacted with water. This reaction decomposed the CaC2 to acetylene and hydrated lime and simultaneously liberated the TiC. Using a combination of elutriation and gravity-separation techniques to separate the hydrated lime, approximately 93 pct of the titanium was subsequently recovered as purified carbide containing 54 to 70 pct titanium with CaO content as low as 0,6 pct. This combination of techniques can be used to separate more than 90 pct of the CaO from the TiC. Therefore, this carbiding procedure is a viable method for treating titaniferous materials, including perovskite, that contain more than 20 pct CaO. Tests made in a static-bed reactor showed that for the reaction of TiC with elemental chlorine to produce titanium tetrachloride (TiCI4), a temperature of at least 940° F is desirable to achieve a suitable extraction of titanium in a laboratory chlorination reactor. In fluidized-bed tests at 840° F, 98 pct of the titanium contained in TiC was extracted.

Jan 1, 1980

The Bureau of Mines, U.S. Department of the Interior, devised a flotation technique for upgrading chromite in chromium ores and gravity concentrates. The technique consisted of cationic flotation of chromite from a slime-free pulp acidified to pH 2.5 or lower using H2S04 modifier. Flotation results showed that ore containing serpentine as the primary gangue mineral was more amenable to concentration by this technique than ore containing the readily floatable olivine as the primary gangue mineral. Rougher flotation of a chromite ore containing abundant serpertine increased the grade form 19 to 41 percent Cra03 at a chromite recovery of 89.6 percent. Rougher flotation of ore containing abundant olivine upgraded the chromite from 23.4 to 29.6 percent Cr203 at a recovery of 89.4 percent. The technique was also applied to chromite gravity concentrates to further upgrade chromite and to reject silicates. Flotation of a gravity concentrate containing 40.9 percent Cr203 and 4.4 percent SiO2 recovered 90 percent of the chromite in cleaner products containing 44.9 percent Cr203 and 0.63 percent Si02. The combined recovery by gravity and flotation was 87 percent. An economic evaluation of this technique will be undertaken to deter-mine its feasibility for commercial use.

Jan 1, 1980

By H. D. Jacobs

The Federal Bureau of Mines, as part of a program to insure future raw material needs for the iron and steel industry, undertook research to beneficiate the oxidized taconites from the western Mesabi range in Minnesota. The data presented were obtained by applying the Bureau-developed selective-flocculation/cationic-flotation process to the second of three oxidized taconite samples. These three samples are representative of an estimated 10 billion tons of ore analyzing 30 to 40 pct iron. The experimental work was performed in a 900-lb/hr pilot plant. Treating the ore sample (36.1 pct Fe) with the Bureau's process produced commercially acceptable concentrates averaging 63.5 pct Fe and 4.3 pct SiO2, with an average iron recovery of 84.6 pct.

Jan 1, 1980

By J. E. Pahlman

As part of its effort to reduce the need for strategic minerals through conservation and to reduce the capital and energy requirements of mineral processing, the Bureau of Mines has investigated a method for preparing ferrochromium alloys containing less than 2 percent carbon. This method will conserve chromium and should reduce the capital and energy requirements for chromite reduction. Reduced products containing less than 2 wt-pct C and as low as 0.01 wt-pct C were obtained by reacting pellets of chromite and carbonaceous reductant mixtures at pressures of 0.1 to 1 torr and temperatures of 1,230° to 1,320° C. The extent of reduction increased with increased temperature and decreased pressure; however, operating conditions were limited due to the onset of significant chromium vaporization at higher temperatures and lower pressures. Foundry coke, anthracite, and carbon black were found to be supe¬rior to graphite as reductants. The reduction of chromite to metallics was found to proceed via the carbide intermediates (Fe,Cr)7C3 and (Fe,Cr)23C6, No evidence of carbide intermediates Fe3C or Cr3C2 was found. Buttons of ferrochrome alloys were made by melting a mixture of reduced products with CaO and Si02 at 1,700° C for 20 minutes in an induction furnace,

Jan 1, 1980

By W. P. Diamond, J. R. Levine

The explosion hazard of methane-air mixtures has become an increasingly serious mine planning problem, and an advance assessment of methane gas potential can therefore be essential for a safe and economic mine development pro- gram. As part of its coal mine health and safety program, the Bureau of Mines has developed a simple, inexpensive test to measure the methane content of coal samples obtained from exploration cores. The gas content of coal per unit weight as determined by the direct method test can be used as a basis for a preliminary estimate of mine ventilation requirements, and to determine if degasification of the coalbed in advance of mining should be considered. Since the Bureau began measuring the gas content of coal samples in 1972, experience has led to equipment and procedural changes, the most significant of which has been the development of a ball mill for crushing the coal sample to release the residual gas at the end of the desorption test period. This revised procedure replaces the crushing box and graphical methods described in earlier Bureau publications. The results of 583 direct method tests are summarized in tabular form. These results include data on the gas content of 125 coalbeds in 15 States.

Jan 1, 1980

By Philip Thompson

The Bureau of Mines investigated a selective flocculation-flotation technique to remove insoluble slimes from low-grade potash ore in a continous 45-kilogram-per-hour (100-pound-per-hour) process investigation unit (PIU). This research is part of the Bureau's program to improve resource recovery from low-grade ores. Results showed that 84 percent of the insoluble slimes were removed from an ore containing 5.5 percent water-insolubles and 14 percent K20 using a Bureau-developed, cationic flocculant-glycol ester-diesel oil reagent. Subsequent potash flotation recovered 75 percent of the potash in a cleaner concentrate assaying 56 percent K20. Concentrate leaching upgraded the product to market specifications of 60 percent K2O. An economic evaluation by the Bureau suggested that the rate of return on investment, after taxes, should be about 20 percent for such an enterprise.

Jan 1, 1980

By L. A. Haas

The Bureau of Mines conducted bench-scale leaching tests with recycled spent copper electrolytes and copper-nickel mattes produced from the Minnesota Duluth Complex concentrates. This report describes the first stage of an overall two-stage leach operation. The objective of this research was to determine the matte-leach technology required to convert spent copper electrolyte into an enriched nickel liquor suitable for a nickel refinery and there-fore essentially free of copper, iron, and sulfuric acid. The experimental variables investigated were matte composition, particle size, spent electrolyte content, pulp concentration, oxygenation, temperature, and time. The time required to produce an enriched purified nickel liquor decreased with increasing pulp concentration, temperature, and oxygenation, but increased with increasing particle size and electrolyte copper and acid content. Nickel-rich (about 50 g/l) liquors at a pH of about 4 and containing less than 1 g/l of copper and iron were produced at 70° C by leaching minus 325-mesh low-iron (less than 5 pct) matte for 8 hours with spent electrolyte containing 22.4 g/l Cu, 28.9 g/l Ni, less than 0.1 g/l Fe, and 50 g/l H2S04 at a pulp concentration of 1 kg of matte per liter of spent electrolyteo Varying the nickel content of the spent electrolyte from 11 to 101 g/l appeared to have no appreciable influence on the matte leaching characteristics.

Jan 1, 1981

By C. F. Davidson

The Bureau of Mines studied the extraction of lithium from lithium-containing clays by chlorination with hydrogen chloride (HC1). In bench-scale laboratory investigations, HC1-H20 mixtures were used to selectively chlorinate lithium, but not calcium or magnesium, in lithium-containing clays. The addition of calcium carbonate to the clay was found to improve the lithium recovery. Reaction conditions found to affect the lithium recovery were ratio of clay to carbonate, reaction temperature, and HC1 concentration. The best conditions for selective chlorination of the lithium were 2:1 clay-carbonate, 750° C, and 20 wt-pct HC1. The experimental results and trends in lithium extraction are explained using thermodynamic relationships.

Jan 1, 1981

By V. R. Spironello

The Bureau of Mines is conducting studies of the slags related to ferrous technology to evaluate acceptable substitutes for the auxiliary flux, mineral fluorspar, in foundry operations. This work is directed toward the Bureau's goal of minimizing the Nation's dependence on scarce and critical minerals Comparative basic practice cupola (18-inch-ID) trials were made to evaluate a waste material called "used potlining," which contains significant levels of fluorine, sodium, and aluminum in various compounds. Used potlining is recovered from alumina reduction cells after its useful life, and was supplied by the Aluminum Co. of America (Alcoa) to the Bureau for evaluation. The material in the lump and pelletized form (with limestone) provided extremely fluid slags based on visual observation during cupola operation. No adverse effects were found on cupola performance, metal and slag chemistry, the environment, or mechanical properties of the castings produced. Fluorine recovery in the slag was equal to, or higher than, that of fluorspar; fluorine losses to the scrubber water and solids were lower. The acidity of the scrubber Hater was somewhat neutralized. No difference was observed in furnace-refractory attack, as determined by the level of magnesia in the slag and visual inspection. The recovery of sodium in the slag, presumably as the oxide, significantly increased slag fluidity, suggesting that less than equivalent fluorine may be required. There was no contamination of the gray iron by the aluminum from the used potlining. Used potlining was completely satisfactory as a substitute for fluorspar in cupola ironmelting.

Jan 1, 1981

By E. R. Cole

This Bureau of Mines investigation was prompted by the need forr a stable anode for electrowinning metals, particularly zinc and copper, from acid solutions. The polarization behavior of Pb-Ag (1 pct Ag) anodes in H2SO4 and fluoride solutions was determined as the first step in the development of such an anode. A Luggin capillary, dc power supply, high-impedance voltmeter, and other equipment standard to an electrochemical laboratory were used in this study. It was determined that during polarization, a relatively hard, stable coating of Pb02 was formed on the surface of the lead-silver anode and the rate of formation of this coating was considerably enhanced by the presence of fluoride ions in solution. Subsequent investigations at the Bureau of Mines Rolla Research Center resulted in the development of a Pb02-coated titanium (Pb02-Ti) anode. Results of this effort were presented in Bureau of Mines Report of Investigations 8111. Additional data resulting from extensive testing of the Pb02-Ti anodes, as well as process improvements and innovations, are included in this report. The anodes were considered generally unsatisfactory for zinc electrowinning because of lower conductivity, higher oxygen overvoltages, and shorter in-cell life as compared with the Pb-Ag anodes now being used in industry. However, the PbO2-Ti anodes were used successfully to oxidize waste chromium solutions and to electrowin copper.

Jan 1, 1981

By S. E. Khalafalla

The Bureau of Mines has used colloidal solutions of magnetite in a magnetic field to segregate nonmagnetic materials such as nonferrous scrap metals and to concentrate precious minerals. Conventional magnetic separation relies on the inherent magnetic susceptibility of the material to be separated and may be designated as magnetic separation of the first kind the medium of separation rather than the separated particles are made magnetizable, a new system of gravity separation results. In this new magnetic separation of the second kind, a magnetic fluid rather than air or water acts as the separation medium. The same force that attracts magnetic objects in separations of the first kind also attracts the entire separation medium in separations of the second kind, thereby creating a reactionary force of equal magnitude in the opposite direction. This force, sometimes called the levitation force, can be made to segregate nonmagnetic particles in a flowing stream according to their specific gravity. The technique has been applied to segregate nonferrous metals from automobile and appliance shredders and mixed scraps. The system has also been used to upgrade diamondiferous jig concentrates from certain river gravels in order to facilitate the sorting and recovery of their diamond content.

Jan 1, 1981

By Philip C. Good

The Bureau of Mines investigated the feasibility of utilizing low-grade phosphatic shale as a feed for phosphoric acid production. Present practice in the phosphate mining operations of southeastern Idaho is to remove and either stockpile or waste low-grade phosphatic shales as the high-grade phosphate beds are selectively mined. Acid digestion studies were performed on uncalcined shale and on shale calcined to remove free carbon to determine phosphoric acid quality, yield, and amenability to filtration. The untreated shale, containing 21.4 pct P205, was digested with sulfuric acid in a single-tank reactor to yield phosporic acid and gypsum residue. Although 96 pct P205 recovery was attained in digesting uncalcined shale, only the calcined product gave satisfactory filtration rates. Calcined shale yielded phosphoric acid recovery of about 93 pct of the contained P205. It was higher in impurities than commercially prepared acid derived from high-grade western phosphate rock. An acid filtration rate of 745 lb P205/ft2/day was attained. This value is lower than the rate of 900 lb P205/ft that is generally considered to be acceptable in industrial production of phosphoric acid from high-grade phosphate rock.

Jan 1, 1981