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By D. J. MacDonald

Wettability measurements and laboratory waterflood tests were compared under a wide variety of conditions. Experiments were conducted with synthetic and natural crude oils, treated and untreated outcrop and oilfield sandstone cores, and synthetic brines with and without caustic, detergent, or phosphate additives. Measurements were made on equilibrated and unequilibrated systems at 77° and 150° F. Wettability was evaluated by the Bureau of Mines method from capillary pressure curves determined with a centrifuge. The waterflood data were fitted by empirical curves; the parameters of the curves characterize primary and subordinate production and also give the ultimate oil recovery. Results showed that wettability measurements at 77° F were useful predictors of recovery efficiency in waterflood tests run at both temperatures. Oil recovery in the early stages of waterflooding increased with increasing water wettability; however, the ultimate recovery was highest at a slightly oil-wet condition. The oil displaced at highest speed in the centrifuge was correlated with ultimate recovery in waterflood tests. Chemical additives to the brine sometimes lowered wettability and also sometimes improved waterflood recovery, but wettability and recovery were not correlated with additives present. The effect of additives on recovery in waterflooding was best seen in water-oil ratio curves.

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 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 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 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 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

By W. T. Abel

The Bureau of Mines tested 48 materials for their ability to absorb H2S from hot simulated producer gas (1,000°-1,500° F). The material found best from the standpoint of absorption capacity, durability, and amenability to regeneration was sintered pellets of 75 percent fly ash-25 percent Fe203. The performance of this absorbent under simulated and actual conditions is described. The effect of absorbent composition, absorbent temperature, steam content of the gas, and tar vapors and dust in producer gas is discussed.

Jan 1, 1974

By T. O. Llewellyn

The Bureau of Mines investigated the use of a heavy liquid in combination with fluid cyclones to separate brucite from a Nevada ore on a continuous basis, using a mixture of dibromomethane and trichloroethylene having a density of 2.44 grams per cubic centimeter. Single-stage cyclone separation produced a concentrate that contained 84 percent of the total magnesia at a grade, on a calcined basis, of 95.6 percent MgO.

Jan 1, 1974

By E. D. Calvert

The room temperature tensile properties of commercially pure titanium and seven titanium alloys prepared by skull casting were determined in the as-cast and heat-treated conditions. Data were compared with property data from tensile tests on wrought alloys of the same compositions in the as-worked and heat-treated conditions. The alloys evaluated were Ti-5Al-2.5Sn, Ti-6Al-4V, Ti-6Al-4V-lSi, Ti-6A1-2Sn-4Zr-2Mo, Ti-6A1-6V-4Zr-4Mo, Ti-6A1-6V-2Sn, and Ti-11.5Mo-6Zr-4.5Sn. Test specimens were prepared from both static and centrifugal castings and from plate fabricated by forging and rolling vacuum-melted ingots. The data indicate that the alpha and alpha-beta alloys have strength properties in the as-cast condition that are reasonably close to the strength properties of their wrought counterparts in the as-worked condition. An exception to this was the Ti-6A1-6V-4Zr-4Mo alloy for which insufficient data were available to form any firm conclusions. Fine-grained cast structures of Beta III (Ti-11.5Mo-6Zr-4.5Sn) were shown to be generally stronger in the as-cast condition than the wrought alloy in the as-worked condition except for the yield strength of one structure that was unusually low. Heat treatment of this alloy produced properties that were unpredictable. Indications are, however, that optimization of heat treatment parameters for each cast structure could produce strength properties equal to that of wrought materials.

Jan 1, 1974

By H. O. Poppleton

This Bureau of Mines study was made to investigate a possible method for selectively removing the Si02 component of silicate minerals and ores. Of specific interest were aluminum ores and zircon. Methods are described for removing Si02 from these ores as volatile silicon sulfides by treating the ore with sulfur and carbon; with sulfur, carbon, and a reducing gas; or with sulfur compounds and carbon. Comparative results are also given for the desilication of some of the ores with carbon alone to form volatile silicon monoxide. The silica component can be removed partially from bauxites at temperatures above the sublimation temperature of SiS (940° C) by treatment with carbon, sulfur, and methane; however, it is more difficult to remove the silicon from kyanite, manganese silicate, red muds from aluminum processing, kaolinite, lateritic nickel ores, and zircon. Complete desilication requires temperatures ranging from 1,100° C for bauxite to 1,450° C for zircon. Although the high temperatures required and the undesirable metal sulfides produced eliminate practical application of this method using present technology, the Bureau is reporting this data so that they will be available to future investigators.

Jan 1, 1974