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By W. M. Dressel

Over 2 million tons of steel furnace dust containing approximately 100,000 tons of zinc and 10,000 tons of lead are produced each year. Recycling of the dusts would conserve mineral resources, lessen land area requirements for disposal, decrease pollution problems, and aid in solving our balance of payment problem. Steelmaking dusts can be pelletized and thermally treated to remove lead and zinc and to reduce the iron oxide to form metallized pellets. In laboratory tests more than 99 pct of the zinc and 85 pct of the lead was volatilized from the dust by roasting at 1,000° C in carbon monoxide. The volatilized material can be collected and treated further for lead and zinc recovery. Reduction and volatilization of over 95 pct of the zinc and most of the lead was achieved by roasting self-reducing mixtures of steel furnace dusts and high carbon steelmaking wastes in an inert atmosphere at 1,100° C. Over 80 pct of the iron in the resulting pellets was metallized.

Jan 1, 1974

By W. H. Eddy

The Bureau of Mines conducted laboratory batch-and small-scale continuous flotation processing tests on waste granite fines from Georgia, to determine the feasibility of recovering usable feldspar and quartz products by flotation. Two flotation methods were utilized for the removal of biotite and other iron-bearing minerals: One was in an acid-cationic circuit, and the other in an alkaline-anionic-cationic circuit. Feldspar was recovered using an acid-cationic method. To produce commercial-grade feldspar and quartz products it was necessary to employ either two sequential froth flotation circuits or one froth flotation circuit supplemented by wet-magnetic separation techniques to remove iron contaminants. Continuous flotation processing yielded a commercial-grade feldspar concentrate containing, in percent, 3.8 Na20, 5.4 K20, and 1.10 CaO, with recoveries of 77.8, 70.3, and 64.4, respectively. The feldspar tailing was high-quality glass sand containing 98.2 percent SiO2 and 0.024 percent Fe2O3. About 42 percent of the quartz was recovered at glass sand specifications. An effective separation of, potash feldspar from the bulk feldspar concentrate was achieved by batch flotation in a mineral separation cell.

Jan 1, 1974

By J. J. Drost

The feasibility of basic oxygen furnace (BOF) offgas heat recuperation by preheating scrap was investigated on a pilot plant scale by the Bureau of Mines. In this study, offgases generated during the oxygen blowing of a molten pig iron and scrap charge were passed through a static bed of shredded auto scrap. Scrap quantities varying from 100 to 180 pounds and representing from 22 to 40 percent of the 450-pound BOF metallic charge were preheated in this manner. Average scrap bed temperatures of 1,650° F for 100 pounds of scrap and 1,150° F for 180 pounds of scrap have been achieved during the blows. As compared to cold scrap used in the normal BOF practice, it was found that by preheating scrap, usage could be increased by 43 percent. The thermal energy recovered by this preheating method can account for up to 44 percent of the energy necessary to melt the scrap.

Jan 1, 1974

By R. Blickensderfer

Test equipment that simulated frictional impacts between coal-cutter bits and mineral inclusions at a coal face during operation of a continuous coal mining machine was used by the Bureau of Mines in the laboratory to study the incendivity of impacts between various rocks, metals, and hard-metal alloys in an explosive mixture of air-7 pct natural gas. Quartzitic sandstone was found to be the most incendive of several rocks tested. Limestone concretions from a coal seam, known locally as "sulfur balls," sparked furiously but were not incendive. Among the metals tested, the type of steel used in commercial coal-cutter tools was the most incendive material tested. A l7-4PH stainless steel was less incendive and appears to be the most promising high-strength steel alloy, reasonably economical, for use in coal-cutter bits. Some hard-metal alloys, primarily titanium and zirconium diboride composites, were also evaluated as possible replacements for the conventional cobalt-bonded tungsten carbide used in the tip of coal-cutter bits. The metal-bonded diborides were generally less inc endive but more brittle than the conventional tungsten carbide. Carbonitride coatings on tool bits were also tested but found to have no advantage. The source of ignition during frictional impact between metal and rock was studied. Immediately after impact, a yellow flash was observed and a smear of metal near its melting point occurred on the rock. This hotspot on the rock, rather than the yellow flash or sparks or metal fragments, was observed to be the cause of the ignition.

Jan 1, 1974

By M. Shabbir

A study was made to determine the optimum conditions for precipitation of uranium from mill solutions using hydrogen peroxide. Precipitation tests were made on both synthetic and actual mill solutions. Parameters studied included amount of hydrogen peroxide, initial pH, reaction pH, time, and temperature. Also investigated was the effect of varied amounts of vanadium, molybdenum, and sulfate in the test solution on uranium precipitation and product quality. The optimum conditions for complete precipitation and high product quality were (1) the use of 150 percent of the stoichiometric requirement of hydrogen peroxide, (2) initial pH of 1.0, (3) reaction pH between 3.4 and 5.0, (4) 4 hours reaction time, and (5) ambient reaction temperature. The excess hydrogen peroxide requirement is partially dependent on the amount of impurities present in the feed solution. The hydrogen peroxide process appeared applicable to treatment of the several mill eluate and strip solutions tested. The experimental studies also indicated that the hydrogen peroxide technique gives substantially better product quality than that produced by ammonia precipitation.

Jan 1, 1974

By P. T. Brooks

A process for extracting 69 percent of the vanadium from weathered Nevada dolomitic shale containing about 1 percent V205 was developed on a laboratory scale by the Bureau of Mines. The process essentially is comprised of salt roasting, leaching with dilute sulfuric acid, solvent extraction, and precipitation of vanadium as ammonium metavanadate. Carbonaceous unweathered shale was less amenable to treatment. A preliminary cost estimate for mining and processing 1,500 tons per day of weathered shale indicated a production cost of about 1 dollar per lb of V205. Considering recent sales at nearly $1. 75 per lb of contained V205, larger scale testing to obtain more definitive process design and evaluation data may be warranted.

Jan 1, 1974

By Jack L. Henry

A laboratory and a pilot-plant-scale investigation has been conducted by the Bureau of Mines to examine possible sources of nitride defects in the production of magnesium-reduced titanium sponge. The production of alpha-stabilized nitride inclusions in hot-rolled titanium plate from air contamination of sponge during its manufacture has been experimentally demonstrated. Magnesium-reduced sponge prepared from air-contaminated magnesium or when contaminated by an air leak during reduction, vacuum distillation, or inert gas sweep, shows very large variations in nitrogen content. Refractory nitrides, delta TiN and epsilon Ti2N have been identified in this sponge. The highest incidence of inclusions resulted from sponge that was reduced by air-contaminated magnesium and from sponge subjected to air contamination during the vacuum distillation cycle and during helium sweep. Air contamination of sponge during the reduction cycle was not nearly as effective in producing inclusions. Tests showed that color and texture may not be reliable criteria for locating defects during sponge inspection. Maintenance of good vacuum-tight integrity, filtration of molten magnesium prior to charging into the reduction retort, and mechanical attrition of sponge to pulverize and disperse nitrides are suggested as practices to lower inclusion incidence in commercial titanium ingots.

Jan 1, 1974

By Jack L. Henry

The Bureau of Mines conducted seven pioneering experiments in a 12-inch-diameter Kroll reduction reactor to examine the feasibility of coreducing the chlorides of Ti, AI, and V to produce a homogeneous titanium alloy sponge. The coreduction studies proceeded in a normal manner, and the yields of sponge were comparable with those of pure titanium sponge made in the same reactor. Vanadium concentration was very uniform throughout the sponge cake when VC14 in solution in TiCl4 was fed into the molten magnesium. More difficulty was encountered in feeding solid VCl2 and AIC13. Vanadium and aluminum concentration in the sponge was not uniform, and mechanical difficulties were experienced with the small-scale screw feeder. Although the sponge varied in composition from region to region, the ingots prepared from it were uniform in composition.

Jan 1, 1974

By Russell R. McLellan

As part of an effort to develop new or improved placer mining technology in the Tertiary gold-bearing channel gravel of northern California, the Bureau of Mines conducted investigations at the old Badger Hill placer mine in Nevada County, Calif., to collect data and information regarding drilling and sampling methods and deposit characteristics. Sampling studies involved the collection and processing of 400 tons of large-and small-volume samples from drill holes, underground workings, surface pits, and blasthole rounds. A total of 355 samples averaging 2,296 pounds per sample provided reasonably accurate data for analysis of the gold distribution. These studies indicated that the bulk of the gold is within 40 feet of bedrock in stacked, lenticular zones of cemented gravel that are largely confined to the relatively narrow, meandering course of the deepest portion of the bedrock channel. Drilling studies involved the testing of truck-mounted rotary, buckett and vibratory drills, none of which proved to be a completely versatile tool for sampling quickly and reliably both consolidated and unconsolidated gravel..

Jan 1, 1974

By Mark I. Copeland

This study was conducted by the Bureau of Mines to determine the effect of steel reheating practices in burning natural gas on the amount of silicon required to prevent the formation of copper on steels containing up to 1 wt-pct Cu. Formation of copper, which causes surface hot shortness, was readily prevented by as little as 0.3 wt-pct Si and by 2 vol-pct excess oxygen in the furnace atmosphere when reheating steels containing up to 0.8 wt-pct Cu. Up to 0.8 wt-pct Si content and careful control of reheating conditions were necessary for steels containing 1 wt-pct Cu. Best conditions for these steels were reheating to 2,200° F (1,205° C) in burning gases containing 2 vol-pct excess oxygen, and then to higher temperatures in gases of 6 vol-pct excess oxygen. Slag and mold wash were not detrimental on steels reheated for 8 hr by a soaking-pit-type furnace schedule, but they were problematical on steels heated for 2 hr by a pusher-type furnace schedule. The effect of silicon contents on scaling rates also was determined.

Jan 1, 1974

By James J. Snodgrass

The Bureau of Mines has investigated vibration levels produced by blasting at four underground sites to establish how such factors as type of explosive, delay blasting, charge weight, and geology affect amplitudes of ground motion. A summary of the work is presented and the results of further analysis of the data are discussed. Square root scaling was found applicable to two of the underground sites and could be applied with minor error to all the sites. Comparison of empirical propagation equations in the different rock types indicates that although the site effect is apparent, the combined data may be used as a basis for engineering estimates of vibration amplitudes from subsurface blasting in many different rock types. Recommendations for predicting and minimizing vibration amplitudes from underground blasts are given.

Jan 1, 1974

By J. H. Weber

This Bureau of Mines publication describes the hardware system and software package for the semiautomatic acquisition and automatic processing of high-resolution mass spectrographic plates. The semiautomatic data acquisition allows a tenfold saving of time compared with manual data acquisition. Automatic processing of the high-resolution data to yield exact masses, intensity, and the corresponding empirical formulas is accomplished by efficient programming on a small, inexpensive, programmable calculator system.

Jan 1, 1974

By C. Daniel Kealy

Dissolved and suspended solids are present in the free water of tailings ponds. This Bureau of Mines study was designed to identify the influences of the slime zone in preventing these solids from reaching the environment outside the tailings pond. The finite-element method was used to determine the rate of discharge of subsurface water from the Van Stone tailings pond in northern Washington. The slime zone was sampled and tested for the first time, and results were interpreted and incorporated into the mathematical model. Computer results were verified by installing and monitoring piezometers in the field and by a simulated (16- by 1/2- by 3 foot) laboratory model. Output from the numerical model defined critical seepage zones and revealed that proper pond design and maintenance can reduce pond seepage losses to a minimum. Minimization of seepage requires maintaining the pond water level over the slime zone. Sufficient physical, chemical, and limnological data were collected and analyzed to conclude that the only realistic reflection of synergistic effects is obtained by study of the indigenous biota in combination with quantitative chemical and physical data. Proper planning and management of the milling and waste disposal operations are the key to minimal pollution.

Jan 1, 1974

By J. M. Stuve

Low-temperature adiabatic heat-capacity determinations were made by the Bureau of Mines in the temperature range from 5 to 300 K for the two crystalline modifications of zinc sulfide, sphalerite (ß) and wurtzite (a). The entropy at 298.15 K of sphalerite was evaluated as l4.02±0.04 cal/deg mole and wurtzite, l4.06±0.04 cal/deg mole.

Jan 1, 1974

By T. D. Ralston

This Bureau of Mines report presents a mathematical model for heterogeneously catalyzed chemical reactors operating under turbulent conditions. The model includes reaction kinetics on the catalyst surface as well as diffusion of the reacting components within the reactor. Three applications of the model to tube-wall methanation reactors are discussed. The first application is a computation of catalyst activity from measured reactor data. This result is then used in a reactor sizing problem and a problem of reactor simulation with recycle. In addition to the reactor model, a novel approach to solving the recycled reactor problem is given.

Jan 1, 1974

By C. Melvin Lepper

The Bureau of Mines has developed an improved earth resistivity field system which employs a novel technique for obtaining null measurements. The instrument is designed to operate reliably in high-noise environments such as those found in the vicinity of operating mines. The system consists of a low-frequency transmitter, a sensitive receiver and an external battery pack, each in its own case to provide protection from the elements. The receiver and transmitter units have self-contained recharge-able batteries to supply power to the circuitry and separate built-in battery chargers that operate on standard 115 Vac power. The system is portable and simple to operate. Measurement accuracy, reliability, and dynamic range are superior to most commercially available equipment even though less time and effort is required to make null readings. Unlike some commercial systems, long integration times are not required to enhance signal-to-noise ratio in areas of high background noise.

Jan 1, 1974

By F. W. Wood

The Bureau of Mines has sought clarification of the Ti-TiN system by studying the phases formed by diffusion reactions between titanium and titanium nitride. Reaction couples were prepared by embedding pockets of TiN powder in arc-melted buttons of titanium. Specimens were vacuum annealed at nominal temperatures of 800°, 950°, 1,200°, and 1,500° C. Metallographically mounted cross sections from reacted specimens and from some that were not annealed were examined optically, with an electron microprobe, with an election microscope, and by X-ray diffraction. Each annealed specimen contained a segregated core primarily of d-phase material, an ?-phase diffusion layer, an a-phase diffusion layer, and host metal. On the basis of corresponding microprobe analyses, and considering results of certain other research, a new phase diagram is proposed. It contains no qualitative innovations, only quantitative adjustments. Results were also analyzed from the viewpoint of diffusion behavior. Diffusion coefficients calculated for the ? phase were sufficiently scattered that the parameters are very tentative. Nevertheless, the diffusion behavior reported is in reasonable agreement with one of two prior studies if it is assumed that the earlier investigators were mistaken in their identification of the nitride phase in which the diffusion occurred.

Jan 1, 1974

By H. G. Lucas

A feeder screw supplied at constant pressure by a hopper-orifice arrangement was developed for feeding solids in size ranges up to several hundred micrometers at constant flow rates. Performance of the feeder was evaluated by measuring the flow rates obtained with 3-to 7-micrometer coal ash, 70 percent through 200-mesh coal, and minus 325-plus 400-mesh coal ash. Constant feed rates within a few percent of set values were achieved for half-hour periods for the larger particles and for 5-minute periods for the finer particles. Suggestions are given for feedstock preparation and feeder operation for optimum performance.

Jan 1, 1974

By D. E. Hirsch

The Bureau of Mines has developed a systematic procedure for separation, characterization, and semiquantitative analysis of high-boiling (350° to 550° C) distillates of crude oils. Isothermal and molecular distillation were used to prepare the 370° to 530° C distillate of Recluse, Wyo., crude oil. The distillate was separated into fractions by chemical treatment, silica-alumina gel adsorption, and gel permeation chromatography (GPC). The fractions were analyzed by use of GPC correlations and mass and nuclear magnetic resonance (NMR) spectrometry. The increased knowledge of petroleum composition obtained from the data will contribute to improved petroleum processing and utilization and energy conservation.

Jan 1, 1974

By F. E. Armstrong

An instrument using a gamma-ray backscatter technique for determining the weight-percent incombustibles content of coal dust and rock dust mixtures in coal mines has been built and tested. The unit gives a direct readout in per-cent incombustibles for coal mine dust mixtures containing between 50 and 100 percent incombustibles; calibration of the device requires using a sample of the rock dust employed; this is usually limestone but occasionally dolomite or gypsum. A small americium-24l source is used with a scintillation detector whose output feeds a rate meter. The source-detector geometry used was chosen to reduce the effects of variation in bulk density. Accuracy of the system is within ±3 percent for most mixtures. The instrument is portable and completely self-contained; the rechargeable batteries supply power for 300 to 400 determinations.

Jan 1, 1974