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By J. S. Dunning

One Federal Bureau of Mines research goal, to minimize requirements for domestically scarce mineral commodities through conservation and substitution, can be accomplished by utilizing more abundant elements such as iron, molybdenum, and titanium. An example of this research is the study of precipitation-hardening, iron-base alloys containing molybdenum and titanium, as substitutes for the high-tonnage stainless steels that are high in imported nickel and chromium. The precipitation hardened iron-base alloys are strengthened by a dispersion of the ternary Laves phase, Fe2 (Mo, Ti). Aluminum and chromium additions changed the solid solubility limits of molybdenum and titanium in a-iron and affected the composition of precipitating phases. A baseline composition of Fe-7Mo-2Ti was selected to study the effects of aluminum and chromium additions on the precipitation-hardening mechanism and microstructure and was also used in studies of mechanical properties and oxidation resistance. The study yielded workable, precipitation-hardening alloys, with elevated temperature strengths equivalent to or superior to types 304 and 316 stainless steels. Chromium and aluminum additions in combination were more effective in providing oxidation resistance than either addition was alone.

Jan 1, 1980

By J. M. Gomes

The Bureau of Mines has investigated the occurrence and recovery of by-product heavy minerals from sand and gravel operations as a means of assessing the Nation's resources. Sand samples from 63 locations in central and southern California were treated to yield heavy-mineral concentrates. The mineral compositions of the concentrates were characterized by chemical and mineralogical examinations. Additional large quantities of concentrates were prepared from selected deposits that contained significant quantities. Beneficiation studies were performed on these concentrates to recover individual mineral products. Gold was recovered by amalgamation; platinum-group metals and radioactive minerals by flotation; magnetite, ilmenite, and chromite by magnetic and high-tension separation techniques.

Jan 1, 1980

By J. M. Kuchta

The chemical and thermal criteria used for predicting the spontaneous combustion hazard are briefly reviewed and data are presented to characterize the gas desorptions and self-heating tendencies of 29 U.S. coals. Closed vessel desorption experiments showed that CO, CO2, and CH4 are the main gases evolved and that the CO, CO/?O2 index, and 02 absorption rate increase with decreasing rank and increasing oxygen content of the coal. In this Bureau of Mines report, the effects of temperature, moisture, and other variables are discussed together with the application of the data to the complex conditions encountered in a mining environment. An important finding is that the presence of CO alone in a mine is not necessarily an indication of a self-heating reaction of the coal. Based upon experiments conducted in an adiabatic-type calorimeter, the self-heating temperatures of lignite and subbituminous coals can be as low as 30° C, whereas the bituminous coals require a temperature of about 60° C or more. The self-heating hazard is greatest when the coals are dried and exposed to a high humidity condition, apparently as a result of the "heat-of-wetting." Generally, the hazard is greatest with the western coals of the United States.

Jan 1, 1980

By W. H. Eddy

The Bureau of Mines used several laboratory batch flotation schemes combined with magnetic separation to investigate the feasibility of recovering potash feldspar and glass sands from molybdenite tailings. Four molybdenite tailings or prospective tailings were used as test samples. Feldspar concentrates containing from 10.7 pct to 12.0 pct K2O were recovered from three of the four samples. The alkali content of the fourth sample met the grade for a mixed feldspar. All the feldspar concentrates contained iron in excess of the 0.10-pct-Fe203 specification for most uses. Electron-beam microprobe examination of the feldspar concentrates showed the presence of an iron-bearing potash feldspar in quantities that were excessive with respect to most iron specifications. However, a high-quality glass sand was produced from all of the samples.

Jan 1, 1980

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 D. Harry Chambers

The Bureau of Mines, through a memorandum of agreement with the Department of Defense, conducted research to recover silver from aircraft scrap. Silver was recovered by an electrolytic method from stainless steel honeycomb sections separated from the aircraft. These sections had been constructed by sandwiching a stainless steel honeycomb core between stainless steel sheets and then brazing the assembly with a silver alloy. Over 300 pounds of silver was used in the B-58 bomber, concentrated in certain honeycomb sections of the aircraft. Following shredding of the aircraft parts, an average of 95 percent (ranging 67 to 100 percent) of the silver was recovered in a single electro-refining step. After the electrorefined product was magnetically cleaned, purity of the recovered silver was greater than 99.3 percent.

Jan 1, 1980

By R. Blickensderfer

Maintaining an adequate supply of minerals and metals to meet national economic and strategic needs is the overall goal of the Bureau of Mines, U.S. Department of the Interior. One method of achieving this goal is to conserve scarce metals by cladding a plentiful base metal, such as iron, with a scarcer metal. To investigate cladding, a vacuum-rolling mill capable of rolling bimetal specimens at temperatures to 1,300° C in a residual gas pressure of 2 x 10-5 torr was established. Metals that were successfully bonded to iron included stainless steels, chromium, nickel, nickel alloys, copper, and several refractory metals including molybdenum and titanium. The effects of the rolling temperature, reduction in thickness, rolling speed, and residual air pressure on bonding strength and bend ductility of the bimetals were determined. Optimum rolling conditions produced bimetals with bond shear strength essentially equal to that of the iron base metal.

Jan 1, 1980

By H. D. Jacobs

The Bureau of Mines undertook a research program to insure an adequate supply of iron raw materials for future iron and steel making needs. A sample was obtained of oxidized taconite from the western Mesabi Range in Minnesota, and the metallurgical response of the taconite to beneficiation by a process that included selective flocculation-desliming-cationic flotation was evaluated. The sample contained 35.3 pct iron and represented approximately 2 billion tons of crude material. Selective flocculation and flotation were evaluated in a pilot plant with a feed rate of 900 Ib/hr. Concentrates averaging 61.7 pet iron and 5.1 pet silica were obtained, with an accompanying iron recovery of 67.2 pet. About 83 pct of the process water requirements were reclaimed from the slime and froth tailing and then recycled.

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 James H. Russell

The Bureau of Mines, U.S. Department of the Interior, in cooperation with the Department of Energy, has attempted to increase the activity of nickel catalysts for converting synthesis gas, derived from coal, to a substitute natural gas. This report describes the effects of low-level additions of B, Ca, Ce, Co, Mn, Mo, Pd, Re, Ti, Y, Zn, and Zr on the methanation activity of Raney nickel. The methanation rate at 320° C and the resistance to poisoning by 2 ppm H2S were used to compare catalysts. The effects of the additions were small, and the experimental variances were large, necessitating the use of statistical methods to identify significant effects. Co, Ti, Y, and Zn improved the resistance to H2S poisoning, but only Co improved the methanation rate In some individual catalysts containing Ca, Mo, or Mn, both the methanation rate and resistance to H2S poisoning were improved.

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 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