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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 Mark S. Stagg, Virgil J. Stachura, John W. Kopp, 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 any one 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 be 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 pre- clude damage to residential structures and any possible human injury over the long term.

Jan 1, 1965

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 Seth C. Schaefer

[As part of the Bureau of Mines effort to provide thermodynamic data for advancement of mineral resources technology, the standard Gibbs energies of formation (?G°f) of MnS (manganese sulfide) and Fe0.9 S (pyrrhotite) were investigated with a high-temperature galvanic cell employing stabilized Zr02 (zirconia) as the electrolyte. Potential measurements were obtained for the cell Pt, MnS, MnO, S02 (g, 1 atm)//Zr02//02(g, 0.0114 atm), Pt with the overall cell reaction MnS (s) + 1.5 02 (g, 0.0114 atm) = MnO (s) + S02 (g) . (1) These results give the standard Gibbs energy of formation of MnS for the reaction Mn (s) + 0.552 (g) = MnS (s) (2) ?G°f = -66.487 + 15.19 x 10-3T±0.207 kcal/mole (896.4 - 1,208.1 K) (3) where temperature (T) is expressed in kelvins. Similar measurements were obtained for the cell Pt, FeO .9S, Fe304 , S02 (g, 1 atm) //Zr02//02 (g, 0.0114 atm) , Pt with the overall cell reaction 10/3 FeO .9 S (s) + 16/3 02 (g, 0.0114 atm) = Fe.,04 (s) +10/3 S02 (g). (4) These results yield the standard Gibbs energy of formation for the reaction 0.9 Fe (s) + 0.5 S2 (g) = Fe0.9 S (s) (5) ?G°f = -35.229 + 12.67 x 1073T+-0.104 kcal/mole (839.5 - 1,086.6 K). (6) A third-law analysis of MnS data yields a standard enthalpy of formation (AH°f) for the reaction Mn (s) + S (rh) = MnS (s) (7) ?H°f298 = -51.16±0.21 kcal/mole (8) A similar third-law analysis for Fe0.9S data yields a ?29°f298 for the reaction 0.9 Fe(s) + S(rh) = FeO .9S(s) (9) ?HO\°f298 = -24.01±_0.15 kcal/mole. (10) ]

Jan 1, 1980

By V. R. Spironello

The Bureau of Mines is involved in research directed toward the conserva¬tion of important raw materials and the utilization of solid waste. Two of the objectives are to conserve high-quality coking coals used for foundry coke and to utilize waste materials of marginal quality but of high calorific value. These objectives are consistent with Bureau goals. Pilot plant cupola trials were made to evaluate the adequacy of various alternative fuels, and to determine to what extent they could replace the foundry coke in cupola charges. Information was obtained on furnace performance, metal and slag chemistry, environmental questions, and the properties of castings. It was shown that anthracite or bituminous coals can partially replace charge coke up to the 40 pet level. Briquetted materials prepared from fuel fines, and waste prod¬ucts or byproducts of high calorific value, all tend to break down on heating in a cupola so that their use must be restricted to below 20 pet replacement. In cases where pitch-bonded coal fines or petroleum coke were used, carbon pickup by the iron was inadequate for gray iron specifications. Although emphasis during this work was placed on basic slag practice, some acid practice results are included.

Jan 1, 1980

In Bureau of Mines research on recycling chrome refractory wastes, used refractories from argon-oxygen decarburization and electric steelmaking furnaces were beneficiated, concentrates were reformed into briquets, and modulus of rupture tests were conducted at 1,350° C. The test results indicated that the beneficiated minus 6-mesh material could be used for producing magnesia-chrome refractories.

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 G. R. Palmer

Using a fluidized, countercurrent multiple-compartment ion-exchange (MCIX) column previously developed by the Bureau of Mines, Bureau researchers have successfully extracted uranium from a simulated acidic in situ leach liquor that contained 150 ppm U30s? This successful demonstration of the MCIX system is reported, and the effects of varying the operating conditions on the performance of the system are also examined. Operating the MCIX system with a flow rate of 15 gpm/ft2 and an aqueous-to-resin flow ratio of 200:1, more than 90 percent of the uranium Has extracted, and a resin containing approximately 28 grams U308 per liter was produced. The absorption column used to investigate the operating variables was approximately 18 feet long with a 2-inch ID and was divided into compartments that were 1 foot long.

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 R. E. Simpson

Beginning in 1972, fully grouted resin bolts were used in underground mines. An estimated 20 million resin bolts will be installed in 1980 owing to their apparent support improvement in most roof-bolt applications. Inorganic cements were tested to replace the resin at a lower cost while retaining the advantages of a grouted bolt. Although other inorganic materials were considered, all but portland and gypsum cements were rejected for reasons of availability, performance, or cost. Portland and gypsum-type cements were tested by the Bureau of Mines to select a fast-hardening, low-cost material that would anchor a roof bolt adequately to meet safety standards. An alpha-gypsum cement, accelerated with potassium sulfate, was selected as the best material because it had adequate pull strength at a desired set time of less than 5 minutes and was readily available.

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 Anthony W. Sparks

The Bureau of Mines conducted tests designed to compare its breathing metabolic simulator (BMS) with other methods that are currently used to evaluate the performance of respiratory protective equipment. The BMS is a commercially developed device that uses a piston cylinder to simulate breath movement. Using a propane furnace that consumes oxygen and forms CO2, the BMS also simulates the respiratory metabolism of humans. The breathing and metabolic subsystems of the BMS are described in detail in this report. Results are compared from tests that used the BMS to evaluate respiratory equipment and from tests that used human subjects for the same purpose. The BMS was also tested against a pulsatile breathing machine (PBM) previously designed by the Bureau. Both machines were used to test respiratory equipment, and the test results are compared in this report. To illustrate typical applications of the BMS, the report briefly describes how the BMS was used to test two different types of closed-circuit respiratory apparatus, and the test results are presented. This research showed that BMS test results compared more closely to the results of tests that used human subjects than did results obtained using the PBM.

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

By Annie G. Smelley

As a part of research conducted in its mission to effect pollution abatement, the Bureau of Mines, U.S. Department of the Interior, is developing a dewatering technique that allows for disposal of clay wastes, for reuse of water now lost with clays, and for reclamation of mined land. The technique utilizes a high-molecular-weight nonionic polyethylene oxide polymer (PEO) that has the ability to flocculate and dewater materials containing clay wastes. In laboratory experiments, coal-clay waste, potash-clay brine slurry, phosphatic clay waste, uranium tailings, and talc tailings were successfully consolidated. Coal-clay was te was consolidated from 3-. 6 to 57 percent; potash-clay brine slurry was consolidated from 3.8 to 35 percent; phosphatic clay waste from 15.6 to 49 percent; uranium tailings from 15.4 to 67 percent; tailings from talc production from 9.7 to 53 percent; and an acidic Ti02 slurr slurry from 1.68 to 30 percent.

Jan 1, 1980

By B. W. Dunning

This paper describes studies conducted by the Bureau of Mines to achieve its goal of developing methods for increased recovery and utilization of valuable constituents in a wide variety of domestic and industrial wastes, In this particular study, 36 units of obsolete electronic equipment from military aircraft were disassembled into their modular components by hand to determine materials distribution. Further modular disassembly into individual parts was used to identify metal composition. After identifying the metals in some of the more difficult to dismantle modules, similar modules were grouped together, shredded, mechanically separated, and using metal composition data from hand separation, classified along with the hand-separated materials. Although this equipment is normally classified as law-value iron-bearing aluminum, data were obtained that indicated the potential for moderately higher value classification. The electronic units were classified as to precious metals, copper, iron, and aluminum contents, and scrap values were estimated.

Jan 1, 1980

By J. Bennetts

As part of its mission to develop technology that will help increase the supply of critical and strategic minerals from domestic resources, the Bureau of Mines has investigated methods for beneficiating platinum-group metal ores from the Stillwater complex, Montana. This report presents the result of a bench-scale study employing froth flotation to recover a sulfide concentrate containing platinum-palladium values from a mineralized gabbro. Best results were obtained with a flotation scheme utilizing a mercaptobenzothiazone collector and sulfuric acid. Rougher concentrates containing approximately 11 oz Pt-Pd/ton and 90 pct of the metal values in the ore were obtained. Subsequently, cleaner concentrates containing approximately 26 oz Pt-Pd/ton and between 80 to 85 pct of the Pt-Pd values in the ore were prepared.

Jan 1, 1980

As part of the Bureau of Mines subactivity in secondary resource recovery and to expand the Nation's mineral base, the Tuscaloosa Research Center made characterization and preliminary beneficiation studies of the waste residues from various coal-conversion processes: from pilot plant tests of the Synthane process for coal gasification, the Synthoil process for coal liquefaction, and the solvent-refined coal (SRC) process for sulfur removal from coal. Those coal conversion processes selected for this study were based on the availability of pilot plant samples. Physical, chemical, and mineralogical examinations of the wastes made to determine the mineral content prior to physical beneficiation tests indicated that in addition to significant quantities of carbon, some trace elements offer potential for concentration.

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 J. P. Hansen

In order to help assure an adequate domestic supply of minerals essential to the Nation's economy and and security by developing more efficient minerals extraction technologies, the Bureau of Mines Tuscaloosa Research Center examined the application of autogenous microgrinding to calcium carbonate minerals. Treatment of minus 8-mesh Alabama marble resulted in a product 80 pct minus 5 micrometers (µm) at a power consumption of 70 to 80 kwhr/ton, This study shows that coarse particles of calcium carbonate minerals are effective as the grinding media for the autogenous attrition grinding of these minerals. The minus 8- plus 30-mesh fraction is an effective grinding medium (sand) for particles smaller than 30 mesh. A 40-pct-solids slurry and a sand: marble ratio of 2.5 appeared to be near optimum. For residence times above 13 minutes, products were greater than 80 pet minus 5 µm and greater than 54 pct minus 2 µm. Power consumption was uniformly low, ranging from 50 to 100 kwhr/ton of product depending upon the feed rate. One marble sample from Georgia was shown to be the most persistent grinding medium, with losses of less than half those of the other materials tested.

Jan 1, 1980

By F. X. McCawley

The Bureau of Mines, in pursuing its goal of extending the life span of strategic materials, conducted field corrosion studies at the East Mesa Known Geothermal Resources Area (KGRA) in the Imperial Valley, Calif., to determine the optimum materials of construction for use in geothermal mineral energy resource recovery plants. These studies included characterization of geothermal environments and in situ corrosion testing. The corrosion resistance of 10 alloys exposed to 5 brine and steam process environments was evaluated using the low-salinity, high-temperature brine from geothermal well Mesa 6-1. Of these alloys, Hastelloy C-276, Hastelloy S, Incone1 625, titanium-2nickel, and 316 L stainless steel had excellent resistance to corrosion in all of the process environments; E-Brite 26-1 and 430 stainless steel had fair resistance. Although general corrosion rates for 4130 steel and 1020 carbon steel were substantially higher than those of the other iron-base alloys, these two alloys could prove useful in low-salinity process environments because of their low cost. Aluminum alloy 5005 was the least corrosion resistant alloy and pitted severely. Scales formed on all of the alloys in every process environment. Calcite, aragonite, and an amorphous silicate were the major components of the scales.

Jan 1, 1980