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By B. W. Jong

The U.S. Bureau of Mines investigated anhydrous chlorination and caustic-acid leaching processes to recover Ni, Co, Mo, and W from waste hydroprocessing catalysts. In batch laboratory-scale equipment, the chlorination process extracted 61 to 99 pet of the metals. Final recovery was 65 to 99 pct. The caustic-acid leaching process extracted 81 to 98 pct of the metals. Final recovery was 36 to 99 pct. Chlorination processing included roasting, chlorination, hydrolysis of metal chlorides for recovering Mo or W, water leaching of Ni or Co from the spent charge, purification, and solvent extraction or precipitation of Ni or Co from the purified solutions. Caustic-acid leach processing included NaOH leaching, solvent extraction of Mo or W from the NaOH leach liquor, H2S04 leaching of the NaOH leach residue, purification, and solvent extraction or precipitation of Ni or Co from the purified solution. The estimated fixed capital cost for a commercial-scale plant processing 39,000 Ibid of waste Ni-Mo-AI catalyst was $8 million for the chlorination process and $9.6 million for the caustic-acid leaching process. The estimated operating cost was about $0.20 and $0.40 per pound of the waste catalyst, respectively, for the two processes.

Jan 1, 1989

By Daniel C. Boteler

Data from 68 entrained-bed carbonization tests were treated statistically by the Bureau of Mines, and several useful relationships were developed among the major variables. Nine coals, ranging in rank from lignite A to high-volatile A bituminous, were carbonized in two entrained-bed carbonization pilot plants. The carbonizing reactors employed were vertically mounted cylinders, internally heated, refractory-lined, and 10 inches ID. The range of carbonization temperatures was from 825° to 1,600° F. Using a regression-analysis computer program, empirical equations were developed by which carbonization temperature, air-to-coal ratio, devolatilization of coal, char yield, and volatile matter content of product char may be predicted.

Jan 1, 1973

By Jalna R. Zatko

The Bureau of Mines, U.S. Department of the Interior, has developed a novel method of flocculation dewatering of phosphatic clay wastes using polyethylene oxide as the flocculant. Research was conducted to determine whether ethylene oxide gas was present in the air in the vicinity of disposed waste materials which had been flocculated with polyethylene oxide. Samples of clay waste materials containing polyethylene oxide were prepared in stoppered glass bottles in simulated disposal environments. Gaseous samples, removed over a 75-day period using an airtight syringe, were injected into a gas chromatograph that was capable of separating ethylene oxide from air. The presence of ethylene oxide gas was not detected in any sample. To determine possible degradation products of polyethylene oxide, the properties and reactions of ethylene oxide and its polymers were reviewed. Based upon the literature survey and experimental study, it was concluded that adverse environmental effects were not likely to result from the use of polyethylene oxide for flocculating phosphatic clay waste products.

Jan 1, 1980

By Ivette E. Torres

Many significant events that began in 1990-91 continued to have a profound impact in the world minerals economy in 1992. The dissolution of the U.S.S.R. and the formal breakup of the Council for Mutual Economic Assistance (CMEA) had significant effects far beyond the geographic boundaries of Europe and Central Eurasia. CMEA's network of economic interdependence had relied on central planning, a variety of subsidies, and barter agreements that allowed its members to function without the pressures of productivity and efficiency. In the mineral sector, many decisions had been made based on the need for military planning and technology competition with the market economy world. Because of inexpensive oil available through subsidies and technology assistance from the former U.S.S.R., industries III CMEA member countries had been able to function and maintain production to supply minerals and materials required to support the policies of the central plan. In 1992, most of the former CMEA countries decreased their output of many minerals. In some cases, the network of production that had been in place was severed. Political and economic instability, destruction of infrastructure, and new priorities were affecting other mineral industries in the area. In late 1991, 15 independent countries replaced the U.S.S.R. and in early 1991 the former CMEA countries found themselves trying to adjust to the realities of economic independence and the need to compete with former allies for survival. Although 11 of the 15 former Soviet republics joined in the Commonwealth of Independent States (CIS) in December 1991, in 1992, individual economic needs exceeded the needs of the Commonwealth III importance. As a result, new mineral trade patterns emerged as minerals were used as a source of much needed capital.

Jan 1, 1994

By P. A. Bloom

Arsenic-containing flue dusts are currently being stockpiled by several nonferrous smelters in the United States. These stockpiles are a source of environmental concern since the dusts can be transported by wind and contain water-soluble arsenic. The stockpiles also represent an alternate source of metals. To provide a quality environment, the Bureau of Mines investigated a process to make environmentally acceptable the discard of arsenic obtained from the treatment of arsenical flue dust. The process includes (1) leaching arsenic from a lead smelter copper dross flue dust, (2) fixing arsenic as an insoluble compound, and (3) recovering other metal values. Overall results of acid-leaching tests on lead-smelter flue dusts showed that H2S04 dissolved 80 to 90 percent of the As, Zn, and Cd, and up to 86 percent of the In. Pb, Ag, and Au remain in the residue, which can be recycled to the smelter. Indium was recovered from the strong acid leach solution by solvent extraction; arsenic was fixed in a stable form by precipitation with Fe2(S04)3 and CaO or CaC03.

Jan 1, 1982

Avoid errors in determining the amount of trace elements in overburden when core drilling samples, particularly as required by PL 95-87, the Surface Mining Control and Reclamation Act of 1977. Reason Metal additives present in certain drill stem joint lubricants appear to contaminate overburden samples. If these lubricants are used in assembling the drill string, they can interfere with the analytical methods used to establish concentration of trace metals. Errors In trace element determination appear to be as much as 30 times true concentration, and may falsely Indicate that the amount of trace element in the overburden exceeds the

Jan 1, 1981

Utilize innovative processing technology to prepare high-purity, ultrafine advanced ceramic powders with little or no contamination occurring during the milling process. Advanced ceramic materials made from these powders could substitute for high-temperature alloys containing critical materials such as chromium, cobalt, and nickel. Approach Modify and evaluate the Bureau's turbomill, developed earlier to grind a variety of ceramic raw materials (clay, mica, and talc), as a milling or size-reduction technique for hard and abrasive advanced ceramic powders, such as silicon carbide. Background Powders for producing ceramic materials, such as silicon carbide. silicon nitride, alumina, and zirconia, which arc being considered for use in severe applications requiring high-temperature and/or corrosion resistance, are very difficult to reduce to fine sizes for processing into finished parts. Traditional techniques of particle size reduction, such as ball milling and jet milling, are very energy intensive and/or slow. These traditional techniques often produce materials that have a nonuniform particle size distribution and are contaminated by the milling media or container.

Jan 1, 1989

By E. J. Kloos

Bureau of Mines-approved self-contained breathing apparatus of the compressed air demand type were evaluated for performance at low temperature. Apparatus durations, breathing resistances, and airflow rates were measured on machine tests at room temperature and -25° F. Man tests under actual wearing conditions verified the machine test results. Many serious functional changes in apparatus performance occurred at low temperature. Pressure regulators malfunctioned when diaphragms lost flexibility. Under certain conditions frozen condensed moisture sealed exhalation valves and fogged eyepieces. High-pressure leaks, not encountered at ordinary temperature, developed at low temperature. Tests results are discussed generally and specifically for each apparatus. Recommendations are given to obtain optimum performance from demand type breathing apparatus at low temperatures.

Jan 1, 1968

By John D. Corrick

A dilute sulfuric-acid leach was developed for extracting lead and copper from lead blast furnace mattes and the chemistry was defined. The possible application of Ferrobacillus ferrooxidans to the problem of salvaging lead and copper from blast furnace mattes was also investigated. Operating conditions were varied to determine their effect on the oxidation and hence extraction of lead and copper from the matte. Conditions varied were temperature, pH, reaction time, aeration in the slurry, and particle size of the matte. A set of optimum conditions were developed that resulted in maximum lead and copper sulfide oxidation. Tests employing these optimum conditions resulted in 82.3 percent of the lead and 98.7 percent of the copper being extracted by a dilute acid leach, while maximum lead and copper extracted using F. ferrooxidans was 69.8 percent of the lead and 78.4 percent of the copper. Tests conducted with a different sample of blast furnace matte indicated that the dilute acid leach might have wide application in extracting lead and copper from other such blast furnace mattes.

Jan 1, 1968

By Andrew J. Fergus

A study of the flotation characteristics of columbium-tantalum minerals was made by contact-angle and microflotation methods, and the findings were confirmed by flotation of two natural ores. In the contact-angle study conditions for collection of columbite, pyrochlore, and tantalite were determined for (1) sodium oleate with a sulfonate; (2) sodium isooctyl phosphate; (3) a short-chain primary amine; (4) a long-chain primary amine; and (5) a quaternary amine. These conditions were confirmed in microflotation tests. Information about collector action on common gangue minerals was also obtained by these two methods. In batch flotation tests on a pyrochlore ore and a columbite ore, it was demonstrated that collectors selected on the basis of contact-angle and micro-flotation studies would float columbium minerals from a complex natural ore. However, multiple cleaner and scavenger flotation steps will be necessary to produce commercial concentrates. From a pyrochlore ore containing 0.54 percent Cb2O5, a 44.4 percent Cb2O5 concentrate was made containing 36.4 percent of the total Cb2O5. For a columbite are the corresponding values were: 4.35, 54.6, and 67.1 percent. During the batch flotation study, wetting agents were found to aid in the gangue-ore mineral separations.

Jan 1, 1968

By Douglas Pollock, John Organiscak

Water spray characteristics, including droplet size and velocity, airborne dust capture potential, and induced airflow quantity for various spray nozzle designs were evaluated to provide basic information for improving spray applications. Water droplet size and velocity characteristics were initially measured by a Phase Doppler Particle Analyzer (PDPA) for hollow cone, full cone, flat fan, and air atomized spray nozzles at similar operating parameters. Airflow inducement and dust capture experiments were also conducted under the same operating parameters to examine any salient features of the spray nozzle type, droplet characteristics, induced airflow, and airborne dust capture. Test results indicate that there are trade offs between airflow inducement and dust capture efficiency. A spray nozzle with a wider discharge angle was observed to induce more airflow, but at reduced dust capture efficiencies. Increasing spray nozzle fluid pressure(s) generally reduced water droplet sizes with concurrent increases in droplet velocity, airflow inducement, and airborne dust capture. Placing a three-sided barrier around the spray nozzles normally reduced spray air induction and increased dust capture efficiency. A direct relationship between airborne dust capture efficiency and spray input power normalized per unit of airflow induced was ob- served. This information can be utilized to improve the performance of water sprays for reducing airborne dust levels.

Provide a strategy for calculating optimum distribution of selected sensors for detecting underground mine fires. Approach The Bureau of Mines performed research to determine adequate distribution of product-of-combustion (POC) fire sensors within mine entries. This placement strategy would improve the miner's chances for escape by locating sensors where they would most effectively, quickly, and efficiently detect fires resulting from coal or wood combustion. Spacing of Sensors Placement strategy guidelines were based on the performance of 160 F heat sensors with ideal operating characteristics which were placed at intervals of ten feet in underground mine entries. Data obtained from full-scale mine fires were used to estimate fire sizes and alarm activation times for the heat sensors. Various equations were then developed to determine spacing requirements for any fire detection system installed in entries of varying heights, widths, and ventilation rates.

Jan 1, 1983

By Stephen A. Hare, O&apos

The melting, casting, and welding of the Raney nickel alloy (42 pct Ni-58 pct A1), a methanation catalyst useful in coal gasification, were investigated. Melting was done in graphite crucibles by heating aluminum and adding nickel using a cryolite slag cover. Casting conditions were found to be optimum when the melt temperature ranged from 1,125° to 1,200° C and the mold temperature ranged from ambient to 250° C. Suitable mold materials were found to be quartz, heat-resistant glassware, olivine, and zircon. Welding of the alloy can be accomplished using tungsten inert gas process. Tensile strength of the alloy, in the as-cast condition, was found to be 2,000 1b/sq in with an impact strength of less than 1 ft-1b. The coefficient of thermal expansion was determined to be 18.4 x 10-6/° C after heat treatment.

Jan 1, 1977

By F. J. Smith, W. A. Gallagher, C. A. Herbert

"INTRODUCTION A fire started about 10 a.m., November 10, 1947, at the Kings mine, Princeton Mining Co., Princeton, Ind., about 1,800 feet inby the main shaft bottom on the main west haulage road at a point estimated to be 2 miles from the faces of the main west entries. No lives were lost, as 27 men escaped from the mine after a series of explosions, which necessitated sealing the mine on the surface. This information circular shows"" how adverse conditions might be overcome, when reopening a sealed mine, by expert planning and close cooperation on the part of various organizations. Conditions found in the mine after it was reopened were comparable to the worst that had been anticipated, yet the mine was recovered with comparatively little difficulty and a minimum of risk. The open workings in the mine covered a vast area, but most of the mine resumed production of coal after being sealed for only 37 days.The information contained herein also points to the desirability of adhering as closely as possible to a predetermined schedule of operations."

Feb 1, 1949

By Daniel Edelstein

Demand for arsenic trioxide increased markedly during 1984 as a result of increased use of arsenical wood preservatives and increased use of arsenicals in agriculture. The increase in agricultural demand was due to a return to production of land with-held from cotton planting under an agriculture program for acreage diversion for some 1983 crops. Supplies of arsenic trioxide were more than adequate to meet increased demand, and prices either declined from, or remained at, the low 1983 levels. In June, ASARCO Incorporated announced plans to close its Tacoma, WA, smelter by mid-1985. Domestic Data Coverage.-Refined arsenic trioxide was produced by two U.S. companies. The major producer voluntarily reported its production to the Bureau of Mines, but to prevent disclosure of proprietary data, the production data have been withheld.

Jan 1, 1985

By C. M. Frost

The hydrodesulfurization characteristics of a Venezuelan topped crude oil and a Venezuelan reduced crude oil were determined at temperatures from 740° to 850° F, pressures from 800 to 1,600 psig, and space velocities from 1.0 to 2.0 Vo/Vc/hr. Kinetic calculations showed that under these conditions the desulfurization reaction was first order with respect to sulfur and had an average activation energy of 32.5 kcal/mo1. Catalyst life tests made at 750° F, with pressures of 800, 1,200, and 1,600 psig and space velocities of 1.0 and 1.25 Vo/Ve/hr, showed that the decrease in the relative activity of the catalyst was a logarithmic function of time or volume of oil processed and the amount of vanadium deposited on the catalyst. Comparative tests made with residual fuels prepared from a Wilmington, Calif., crude oil and a Wyoming asphaltic crude oil showed that catalyst life may be extended by processing fuel oil with a low metal content, but it may be shortened by the presence of large amounts of asphalt in the feed.

Jan 1, 1971

By Michael J. Gallagher

Diamond-bit performance data accumulated by the Bureau of Mines in core-drilling limestone and dolomite show that the physical characteristics of the diamonds and the sizes and types of bits used are economically significant. An analysis of the data establishes one trend of particular significance to those engaged in core drilling: Bits set with small, low-quality drill bort are the most economical. Detailed analysis of the factors that affect diamond-bit performance, such as size and quality of diamonds, sizes and types of bits, percentage of core recovered, and physical characteristics of bit matrices are assessed in the tables, bar charts, and discussion.

Jan 1, 1958

By A. W. Henderson

Methods for converting WOCl4 to WCle were investigated in small-scale, laboratory apparatus to devise a method for preparing pure WCls suitable for conversion to tungsten metal. Chlorine, COCI2, and CCI4, alone and in combination with various forms of carbon, were tested as chlorinating agents at various temperatures. More than 95 percent conversion of WOCl4 to WCls was achieved with all reagents at 8000 C in the presence of activated carbon. Only CCl4 maintained its effectiveness in the absence of carbon at 800° C. The effectiveness of carbon was found to be related directly to its surface area.

Jan 1, 1968

By Harold F. Unger

The Bureau of Mines conducted drilling experiments in the laboratory with a commercially available percussive drill that has an independent rotational system. Eight rock types with a wide range of physical properties were drilled under several combinations of rotational speed, drilling thrust, and operating pressure. Penetration rates and energy per unit volume correlated well with the coefficient of rock strength as shown graphically. Size-distribution analyses of some of the drill cuttings show how particle size varies with rotation speed and rock hardness. In general, changing the rotational speed has a greater influence on the penetration rate in softer rocks, with penetration rate increasing with increasing rotational speed.

Jan 1, 1972

By F. N. Kissell, R. J. Bielicki

The Bureau of Mines found sulfur hexafluoride (SF6), released from a lecture bottle, to be an ideal gaseous tracer for studying mine ventilation systems. Air samples were collected in glass syringes and analyzed by electron-capture gas chromatography. In these studies, the lower limit of detection was about 1 part per billion by volume (ppb) of SF6 per part of air. Experiments conducted in a Pennsylvania limestone mine showed this technique useful in evaluating the effectiveness of auxiliary fans, measuring low flow velocities, probing the air circulating near a working face region where ventilation appeared to be poor, and estimating volumetric flow rates in airways of large cross-sectional area and having low flow velocities. This technique was also used in a western vein-type metal mine to measure the amount of return air being recirculated into the intake air due to leakage through old stoped areas.

Jan 1, 1974