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By Laird Crocker

A goal of the Federal Bureau of Mines is to minimize the undersirable environmental conflicts and impacts associated with mineral processing operations. To help reach this goal the Bureau operated a citrate-process pilot plant for the removal of sulfur dioxide from lead smelter sintering machine waste gases to test the process. The process uses a carboxylate solution such as citric acid to absorb sulfur dioxide from waste gases. The absorbed sulfur dioxide is subsequently reacted with hydrogen sulfide to precipitate sulfur and regenerate the solution for recycle. Nominal capacity of the pilot plant was 1,000 scfm of 0.5 vol-pct sulfur dioxide gas. The pilot plant was operated for over 5,400 hr and produced about 55 net tons of sulfur. The operation demonstrated that (1) 99 pct of the sulfur dioxide could be removed from lead smelter sintering machining waste gases containing from 0.1 to 0.6 vol-pct sulfur dioxide, (2) sulfur precipitation and solution regeneration with hydrogen sulfide in conventional stirred vessels was readily controlled, (3) precipitated sulfur could be continuously recovered as a 99.S-pct-pure product by flotation and melting, and (4) 78 dry-vol-pct hydrogen sulfide gas could be produced from pilot-plant product sulfur, natural gas, and steam.

Jan 1, 1979

By William J. Karwoski

To improve rock-burst control in deep vein mining, a field demonstration has been carried out by the Bureau of Mines to test a new rock-burst control concept--rock preconditioning in advance of mining. The procedure is to fracture the major rock-burst-prone zone during the development of each level before production mining. This allows initial mining to begin in a preconditioned zone and later mining from the level below to end in a prefractured or preconditioned pillar zone that is relatively burst-free. This full-scale field demonstration was carried out On the 7700 level of the Hecla Mining Co.'s Star-Morning mine. An expected burst-prone zone along the main vein between 7 and 10 crosscuts, some 250 feet long by 40 feet above and below the level, was preconditioned by blasting a fanlike ring of drilled holes from each crosscut. The drill holes, up to 100 feet long and 4 inches in diameter, were loaded with high explosives and shot. About 4,550 feet of drilling and 9,000 pounds of explosives were involved in the effort. Comparison of preshot and postshot data from monitoring instrumentation indicated that the blasting did fracture the rock in the planned zone and did result in an immediate stress decrease and softening of rock. The field data compared favorably with predicted results from a finite-element computer model simulation of the destressing. Based on observations made during mining and on the data from the Hecla rock-burst monitoring system, there is no doubt that this preconditioning in advance of mining demonstration resulted in much-improved rock-burst control during first-floor mining. It was also concluded that preconditioning the vein was more effective than preconditioning the wall rock.

Jan 1, 1979

By M. M. Tilman

Etchants containing hexavalent chromium and sulfuric acid are used in a variety of surface-finishing operations. When the resultant spent solutions are discarded, substantial quantities of chromium are lost and pollution prob¬lems are created. To minimize the undesirable environmental effects while improving metal and minerals recycling technology, the Bureau of Mines is con¬ducting research on a method for the economic inplant recycling of these waste etchants. Trivalent chromium, produced when the etchant reacts with a substrate, is oxidized in the anode chamber of a diaphragm cell; other metals, dissolved during the etching operation, are transferred to the catholyte. When waste brass etchants are treated in this manner, all of the trivalent chromium is oxidized and more than 40 percent of the copper and zinc is removed. Similar copper removal and chromium oxidation are achieved with waste printed circuit board etchants and rinse waters from plastic etching operations. The electrical energy needed to regenerate 1 kg sodium dichromate is less than 9 kwhr. Regenerated brass etchants evaluated by two companies equaled or exceeded the performance of fresh etchants.

Jan 1, 1979

By J. L. Holman

The Bureau of Mines has extended its previous development of cast Mn-Cu damping alloys to powder metallurgy (P/M) consolidation of alloys containing 55 to 75 wt-pct Mn. Blends of minus 200-mesh elemental powders were compacted cold in directional and isostatic presses. With 1 pct binder, typical green densities ranged between 76 and 80 pct of theoretical when pressing at 30 or 48 tsi. Green strength increased with compacting pressure and copper content. As-sintered tensile strengths ranged to 60,000 psi fox a hydrogen, sintered 60Mn-40Cu alloy, along with 5-pct elongation. Sintered densities ranged between 90 and 96 pct of theoretical. Sintering (a as effective when holding for 1 hr at maximum temperatures of 900° to 1,040` C, dependent on composition. Strength and ductility were considerably lower than for equiva¬lent cast alloys. When aged to the damping condition, alloys containing 60 to 70 pct Mn exhibited >40 pct specific damping capacity (SDC) at 5,000-psi stress, considerably higher than values reported for equivalent cast material. Effects of 1 or 3 pct Sn or Zn additions on SDC and other properties were assessed. Trials were conducted on consolidating rings and gears of the 65Mn-35Cu alloy on industrial-type P/M equipment.

Jan 1, 1979

By J. T. McLendon

As part of its research project in developing improved refractory materials for metallurgical applications, the Federal Bureau of Mines obtained hot modulus of rupture data at 1,500°,1,550°, and 1,600° C on samples of 13 refractory periclase materials produced from seawater, lake brines, and natural magnesite. The periclase samples also were characterized to establish chemical and mineralogical composition and microstructure. The results indicated that a high MgO content does not necessarily assure good hot strength and that an optimum and varying CaO-Si02 ratio exists for each individual periclase sample.

Jan 1, 1979

By I. Liebman

Two triggered barrier systems and several extinguishing agents were tested against coal dust explosion propagating in the main entry of the Bureau of Mines Experimental Mine at Bruceton, Pa. One system used a high-pressure cylinder to propel the extinguishant; the second system used pressurized nitro-gas or Halon 1301 (CF3Br) in a low-pressure system to power the disperser. The relative efficiencies of the extinguishants were determined by compar¬ing calculated concentrations of the extinguishant clouds present in the mine during suppressing of the explosions. Results showed the following trend of increasing effectiveness: Purple-K (KHC03)<water<hybrids consisting of foam or water combined with Halon 1301<Halon alone. On a weight basis, water was two to three times as efficient as Purple-K, whereas the hybrids and Halon alone were only marginally superior to water. Maximum efficiency of an extinguishant is attained by high rates of discharge from the barrier and by minimizing the time interval between onset of discharge and flame arrival to that necessary for discharge. Both the high- and low-pressure barrier systems were demonstrated to be capable of suppressing coal dust explosions; however, because of the potential hazard of the former, the low-pressure system is considered to be the most attractive prototype.

Jan 1, 1979

By Harold L. Rhodes

The Bureau of Mines has developed a method for determining the H2S content in natural gas samples. A gas chromatograph with a flame photometric detector was used to analyze samples with H2S concentrations ranging from 5,000 ppm to a minimum detectable limit of 0.01 ppm. A mass spectrometer was used to analyze samples containing H2S in amounts greater than 5,000 ppm. Methods are presented for preparing containers for H2S samples and for preparing standards using partial pressure and weighed standard methods, Sample collection techniques are discussed, as are analytical results which illustrate the loss of H2S while in the sample container and provide a basis for evaluating containers used for sampling and standard preparation.

Jan 1, 1979

By C. B. Davison

One goal of the Bureau of Mines is to conserve the Nation&apos;s mineral resources by developing improved performance materials. Consistent with this goal, the Bureau conducted studies on the formation of undesirable cristobalite in seven different fire clays used as refractories. The studies employed scanning electron micrography, chemical and X-ray analyses, and pyrometric cone equivalent determinations to examine the sample clays and determine the effect of thermal history and stablilizing additives on the amount of cristobalite in various calcines. This research has indicated that as fire clay calcining temperatures increased from 1390° to 1,490° C there was a gradual decrease in the percent of cristobalite present in the calcines and a progressive development of mullite crystallization. No cristobalite was found in fire clays calcined above 1,550° C, but cristobalite reappeared when the calcines were reheated to temperatures between 1,400° and 1,500° C. The research also revealed that additions of lithium fluoride (LiF) prevented formation of cristobalite in fire clay calcines.

Jan 1, 1979

By H. R. Beard

The Federal Bureau of Mines investigated the absorption of radium and thorium from waste uranium leach liquor by clays and other materials. This work was conducted in support of the Bureau&apos;s goal of minimizing the environ¬mental conflicts, impacts, and occupational hazards Associated with mining and mineral processing operations. Tailings and soil samples from Wyoming and Utah were contacted with tailings liquors to determine the degree of absorp¬tion. Absorption ranged from 0 to 99 percent for radium and from 0 to 31 per¬cent for thorium. Some samples, which readily absorbed radium, were contacted with various salt solutions that could be present in tailings solutions to determine their effectiveness as desorbents. The desorption of radium ranged from 0.06 to 100 percent. An alpha-spectrometric method was used to determine the radium and thorium, concentrations in the solutions and the solids.

Jan 1, 1979

By Jack Touseull

On November 15, 1972, the Bautsch mine, a lead-zinc mine in Paleozoic dolomites, experienced a massive rock failure involving 3 to 5 million tons. Because this failure was large and extended to the surface, it was included in the Federal Bureau of Mines investigations on "Massive Rock Failures." Analysis of the rock mechanics and mode of failure revealed that failure at the Bautsch mine was the result of the interrelationship of many factors. Factors related to the failure were found to be external and internal to the mining environment. Unlike internal factors, external factors were not apparent and, therefore, many external factors were investigated; some of which are not normally considered in rock mechanics analyses. External and internal factors determined to be of significant importance were: (1) precipitation, (2) fractures, (3) plastic clay layer, (4) topography, (5) rock alteration, (6) bedding, and (7) mining zone dimensions. Because of the conditions at the mine, failure could have been predicted without extensive instrumentation. Application of basic geologic and engineering principles to the internal and external factors could have predicted failure. Alternately, failure would, in all probability, have been delayed by years if, after 1962, mining had been curtailed in the area of failure.

Jan 1, 1980

By V. R. Spironello

The Bureau of Mines is involved in research directed toward the utilization of municipal solid waste. One of the primary objectives is the recycling of the magnetic fraction of municipal solid waste (raw refuse). This is consistent with one of the Bureau&apos;s goals, which is to minimize the requirements for mineral commodities by maximizing metals recovery from secondary domestic resources, In this investigation, cupola trials were made using combinations of refuse scrap with shredded automobile scrap under basic and acid slag practices. Furnace operating information and the behavior of alloying and tramp elements was obtained. The research showed that it is possible to utilize up to 60 percent refuse scrap in the cupola under basic practice and 30 percent under acid practice, Aluminum in refuse scrap, present in bimetallic cans, increased the recoveries of silicon and manganese charged to the cupola. Increased use of refuse scrap provided iron of lower sulfur. The alumina resulting from oxidation increased the slag volume. The aluminum and tin contents of the iron increased with increasing levels of refuse scrap in the charge. Lead was not a problem with respect to contamination of the iron. In basic practice, operation of the cupola was satisfactory since all slags were adequately fluid. In acid practice, operation became troublesome above the 45-percent level. Under both practices, the cupola iron melting rate decreased. Particulates in scrubber water and stack condensate samples contained lead, zinc, and tin, and the dust load increased. The tensile and transverse strengths of the iron produced under both practices are reported.

Jan 1, 1980

By T. O. Llewellyn

The Bureau of Mines conducted batch-?scale tests on a sample of parphyry copper mill tailings as part of a study to determine the feasibility of rutile recovery from this source. The tailings that were tested contained 0.75 percent titanium dioxide (Ti02), with about two-thirds of the Ti02 values occurring as rutile. Mineralogical studies indicated that about one-half of the Ti02 content could be considered recoverable. Beneficiation studies of the tailings showed that best flotation results were obtained when sulfides and carbonates were removed by bulk flotation prior to rutile flotation. Rutile flotation was most effective when a petroleum sulfonate collector was used in an acid circuit. From this basic method of flotation, two alternative procedures were developed. The first procedure was to size and grind the tailings to minus 200 mesh; deslime the total pulp; and then float the sulfides, carbonates, and rutile. The second procedure was the same, except that it did not include sizing and grinding. Flotation of the sized and ground tailings yielded rutile concentrates containing 43.1 percent Ti02 and 75.7 percent of the recoverable Ti02. Rutile concentrates floated from the tailings that were deslimed but not ground contained only 34.7 percent Ti02 and 69.4 percent of the recoverable Ti02.

Jan 1, 1980

By J. R. Cobble

As part of the Federal Bureau of Mines project to develop new or improved materials for metallurgical furnace applications, the Tuscaloosa (Ala.) Research Center has conducted research to develop a reproducible laboratory test for evaluating the resistance of refractories to molten slags. Tests were conducted with a slag representative of slag used to produce mineral wool. A rotating cylindrical furnace was lined with the brick being tested, and it was operated at temperatures up to 1,660° C for periods ranging from 8 to 32 hours. The effects of such variables as slag temperature, rotational velocity, charge rate, and contact time on refractory erosion were determined. The research demonstrated the reproducibility of the test procedure developed.

Jan 1, 1980

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 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 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 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 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