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By I. A. Jacobson

In a closely controlled laboratory retorting system for oil shale, a relationship was developed by the Bureau of Mines between the temperature in the retort and the weight ratio of ethylene to ethane in the gases produced. Reciprocal temperature was shown to be directly proportional to the log ([ethylene]/[ethane]). From this relationship a number, called retorting index, was developed. The retorting index has the dimension of temperature, but its magnitude depends on both temperature and residence time for the reactants in the heated zone in the oil-shale retort. The slopes of the lines relating reciprocal temperature and the logarithm of the ethylene-ethane ratios are nearly constant for each of the retorting processes for which data have been presented. The retorting index should be a valuable tool to control the operation of oil-shale retorts, either aboveground or in situ. If an optimum operating condition can be established, the maintenance of the optimum or the departure from it should be easily monitored by use of the index.

Jan 1, 1974

By John L. Reuss

A laboratory study was conducted by the Bureau of Mines to investigate the technical feasibility of decomposing hydrous magnesium chlorides by using a steam pyrohydrolysis technique. This procedure consisted of injecting steam into the atmosphere of a decomposition furnace containing samples of hydrous magnesium chloride and determining the rate of hydrolysis by measuring the rate of chloride evolution. The variables investigated were temperature, amount of water vapor in the decomposition atmosphere, and hydration stage of magnesium chloride. The application of steam was shown to accelerate both the rate and completeness of magnesium chloride decomposition reactions. For example, when magnesium chloride hexahydrate is exposed to a furnace temperature of 600' C in an air atmosphere for 20 minutes, the decomposition is 37 percent. Under identical conditions in a steam atmosphere, the decomposition is in excess of 70 percent. The magnesium oxide produced by the steam pyrohydrolysis of magnesium chloride dihydrate at 800° C contained 98 percent magnesium oxide. Based on magnesium oxide composition, this is equivalent to that of burned magnesite produced at temperatures in excess of 1,300° C. To demonstrate the quality of the product on a practical basis, metal reduction tests have shown it to be equivalent to reagent-grade magnesium oxide as a carbothermic reduction feed material.

Jan 1, 1974

By L. C. Marchant

Results of detailed analyses of four cores from the Threemile Canyon area in the P. R. Spring tar sand deposit in Utah are reported by the Bureau of Mines. The cores were obtained by the Utah Geological and Mineralogical Sur-vey as part of a l7-corehole evaluation program in the P. R. Spring, Hill Creek, and Rim Rock tar sand deposits. Average properties of the oil zone in the Threemile Canyon area as deter-mined from these cores are as follows: Oil saturation, 67.4 pet of pore volume; porosity, 29.2 pct; permeability before oil extraction, 133 millidarcies; and permeability after oil extraction, 2,855 millidarcies. Average net thickness of the oil zone is 23.8 ft and average depth to the top of the oil zone is 189 ft.

Jan 1, 1974

By J. J. Cummins

The Bureau of Mines heated at 150° to 350° C for 0.5 to 360. days Green River oil shale that had been previously extracted by benzene to provide information on in situ processing conditions, to determine the effect of low-temperature heating on the unconverted kerogen, and to determine the composition of benzene-soluble thermal products. The methods used in determining the composition of the soluble thermal products consisted of fractionation of the soluble material, elemental analysis of the soluble products, fractionation of the polar resins by ion-exchange chromatography, gas chromatographic analysis of [n]-alkanes3 and mass spectral analysis of the branched plus cyclic alkanes and aromatic oils. The methods used to determine the effect of low-temperature heating on the unconverted kerogen remaining in the oil shale heated residues consisted of carbon-hydrogen analysis, volatile material determination, carbon residue determination, and oxidation rate determination. In general, it was concluded that significant increases in the degradation of kerogen to oil occurred between the temperature range of 250° to 350° C; that the composition of the soluble products depends upon the temperature at which they are formed; and that the [n]-alkanes are pyrolytically degraded from the kerogen structure. In particular, the 250° C heating temperature is beneficial to the formation of branched plus cyclic alkanes. Also, the heated and unconverted oil shale kerogen and the soluble thermal products become more aromatic as the temperature increases from 150° to 350° C.

Jan 1, 1974

By M. L. Whisman

The Bureau of Mines developed and tested in the laboratory several innovative techniques for reclaiming used lubricating oil. These processes included percolation through both chemically treated clay and ion-exchange resins, distillation through batch and continuous wiped-wall vacuum apparatus, treatment with solvent extraction systems, and chemical removal of impurities with chelating agents. In each treatment, the criteria of evaluation was oil recovery and reduction of acidic and metallic components. Both vacuum distillation and solvent treatment ranked high in their abilities to remove acidic and metallic components of the used oil with good oil recoveries. A combination of the two techniques gave the best overall results in terms of quality evaluations made by established bench tests. The methods were not ranked according to economic practicablity.

Jan 1, 1974

By E. R. Cole

A lead smelting process that appears to present minimal pollution problems has been developed at the Bureau of Mines, Rolla Metallurgy Research Center. Ten and 100 g samples of PbS mill concentrates were vaporized at 1,000° to 1,100° C in a furnace with an inert gas atmosphere during a 2-hour period. The PbS vapor was transported by the inert carrier gas to the reduction zone of the furnace where it was reduced at the same temperature with excess hydrogen to metallic lead. Lead of 99.9 pct purity was produced. The H2S formed can be decomposed into elemental sulfur and water vapor by a modified Claus process. Approximately 90 pet of the Cu and 70 pct of the Ag and Zn remain in the residue and are potentially recoverable. More than 98 pct of the lead in the concentrates was extracted.

Jan 1, 1974

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