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By Thomas M. Garland

A field study was made by the Bureau of Mines in cooperation with oil companies to determine the feasibility of changing the injection profile of water-input wells after water breakthrough at producing oil wells. A secondary objective was to study the particle size and quantity of plugging material required to change the input profile and the methods of applying these materials. Fifty-three injection wells were treated with various amounts and types of plugging materials and the injection profile was definitely changed in most of the wells treated. Increased efficiency of water injection after treatment was indicated by tracer surveys and injection-well performance. There were some indications that the rate of water production was reduced and the rate of oil production was increased as a result of selective-plugging treatments, but ,s found that an immediate change in the rate of oil and water production did not normally occur. In many cases, beneficial results from a treatment may never be observed in the rate of oil or water production due to the many factors that affect the performance of producing and injection wells.

Jan 1, 1966

By Willard L. Hunter

The smelting of tin slags was undertaken at the Bureau of Mines Albany Metallurgy Research Center (AMRC) to produce crude columbium-tantalum ferro-alloy as a unit operation in the production of pure columbium and tantalum oxides or chlorides. Columbium and tantalum-rich alloy was prepared during short unrelated campaigns over a total period of 12 years. Tin slags from Malaya and the Congo (Geomines) were smelted. These slags were reduced by carbon in a small, single-phase, steel-making furnace} a larger three-phase, steelmaking furnace, and a three-phase, submerged-arc furnace, In all cases depleted slags were fluid and easily tapped from the furnace. However, unless diluted by iron additions, the metal product was a viscous, high-melting, heterogeneous mixture that could be removed from the furnace only by hand rabbling.

Jan 1, 1966

By D. C. Crowell

This publication presents the results of a laboratory investigation of displacement of gas by injection or imbibition of water into sandstone models under essentially isobaric conditions. A brief discussion of scaling requirements is included. The influence on residual gas saturation of independently varying the parameters of dimensional ratios of the porous media, rates and methods of flooding, surface tension, initial water saturation, and permeability is shown. Of these variables, increased initial water saturation and decreased surface tension reduced residual gas saturation significantly, whereas variations in flooding rate and dimensional ratios had no apparent effect. No correlation was evident between absolute permeability and residual gas saturation.

Jan 1, 1966

By John J. Mulligan

The Bureau of Mines investigated the tin deposits of the Cape Mountain area during July and August 1962 to test the effectiveness of detrital-cover sampling in permafrost areas as a relatively cheap and simple means of guiding mine development and exploration. Results indicate that systematic detrita1-cover sampling can be used effectively to delineate obscure deposits with sufficient accuracy to permit sampling with a minimum of trenching or drilling. Extensions of known outcroppings were traced in sufficient detail to guide lode sampling and several previously unknown tin-bearing lodes were found and sampled. Lode sampling was limited to the minimum needed to establish the reliability of detrital-cover sampling results. The results of previous lode and placer investigations are summarized and detrital-cover sampling methods and results are described in detail.

Jan 1, 1966

By W. L. Falke

This Bureau of Mines report illustrates critical path planning and scheduling techniques as applied to typical mining operations. Detailed examples of arrow diagramming and computer oriented applications of critical path methods are given. Program Evaluation and Review Technique (PERT) is discussed briefly in comparison to the Critical Path Method (CPM).

Jan 1, 1966

By Albert W. Deurbrouck

The preparation characteristics of the coals of Buchanan County, Va., are described in this Bureau of Mines report. Twenty-one samples ,,,ere collected from 9 coalbeds in the county. Of these samples 13 were of metallurgical quality as received, and 8 required some upgrading to provide acceptable products. In general, the coals were of low to medium ash and sulfur content, and ranked as medium-to high-volatile bituminous. In 1963, production in the county was in excess of 13 million tons, of which 2.2 million tons were mechanically cleaned.

Jan 1, 1966

By Norman G. Foster

The mass spectra of four tertiary butyl substituted thiophenes are reported. A comparison and contrast with earlier structure correlations made by API-RP48 mass spectroscopists is presented. The fragmentation routes of these types of molecules are discussed and explained in terms of existing theories in mass spectrometry. Low ionization voltage data are presented to support the mechanistic picture developed. Structures are inferred about some of the ions, and these are correlated with existing theories. Metastable peaks in the spectra are used to support the fragmentation paths. The presence of doubly charged ions in the spectra is noted and the possible implications toward mechanisms discussed. The general picture of simple, small fragments leaving the ion moiety upon further fragmentation is developed in detail. Some suggestions are presented for further work utilizing isotopically labeled molecules to establish firmly the general picture of fragmentations of the alkylthiophenes.

Jan 1, 1966

By John M. Gomes

Two molten salt systems were evaluated as electrolytes for the repetitive recovery of tungsten from tungsten oxide (W03) made by calcining commercial-grade ammonium paratungstate. Using a sodium chloride-sodium fluoride-potassium aluminum tetrafluoride electrolyte at 800° C, 1 pound of 99.8 percent tungsten was recovered for each 2.7 kilowatt-hours of energy consumed. The metal contained 1,100 ppm carbon, was in dendritic masses of spherical grains, and had an apparent bulk density of 5.41 g/cm3. T ngsten of 99.9 percent purity was won from a sodium pyrophosphate-sodium tetraborate-sodium chloride electrolyte at 1,000° C; 6.0 kilowatt-hours of energy was consumed for each pound of metal recovered. The metal contained 120 ppm carbon, was in dendritic masses of hexagonal acicular crystals, and had an apparent bulk density of 7.25 g/cm . Each metallic impurity--aluminum, calcium, copper, iron, nickel, and silicon--in the two tungsten products was 16 ppm or less.

Jan 1, 1966

By Arnold P. Pipilen

In a study of the principal factors affecting the transport of coal-water mixtures through a centrifugal pump and a pipeline, the interrelation between solids concentration, velocity, and pressure drop was established for a bituminous lump coal (minus 2 inch) in concentrations up to 48 weight-percent. An optimum concentration was found to exist for maximum capacity of a given pipe-line, and for minimum energy requirements per ton of coal. Coal size degradation by particle fracture took place in the pump; abrasion and attrition to form fines took place in both pump and line. A novel system of studying flow of solid-liquid mixtures in pipelines by the determination of relative sound intensities was developed.

Jan 1, 1966

By H. Leitch

In laboratory experiments, the Bureau of Mines investigated melting, quenching, and sulfuric acid leaching of alumina from mixtures of albite and anorthite, and from anorthosites containing 26 to 32 percent alumina. Variations in pouring temperature, quenching and leaching conditions, were studied with respect to the extraction of alumina and impurities. Virtually all of the alumina was dissolved by leaching melted and quenched California anorthosite in boiling 16-percent sulfuric acid solutions for 15 to 30 minutes. The leach solutions were readily separable from the solid residue by conventional thickening and filtration techniques. Only 2 to 5 grams of SiO2, Fe2O3, or CaO dissolved per 100 grams of alumina. The quantity of SiOz in solution varied inversely with the duration of the leach and with the concentration of the H2SO4 solution used. Melted and quenched Wyoming and Minnesota anorthosites with SiO2:CaO weight ratios of 4.3 and 3.2, respectively, were less amenable to sulfuric acid leaching than California anorthosite with an SiO2:CaO weight ratio of 5.3. However, excellent results were obtained on the Wyoming and Minnesota anorthosites by the addition of SiO2 to these materials before melting, in quantities sufficient to adjust the SiO2:CaO weight ratios of the furnace charges to between 4 and 6.

Jan 1, 1966

By R. W. Van Dolah

An investigation was made of the distances over which sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) might be expected. Large-scale gap tests used two types of AN-FO donor charges in three sizes with AN, both at ambient and elevated temperatures, and AN-FO acceptor charges. Donor sizes were varied to test the validity of a scaling law commonly used in quantity distance tables. The up-and-down experimental design was chosen to determine the 50-percent initiation point efficiently. The acceptor charges were instrumented to indicate initiation and to determine detonation velocity. Other electronic techniques for measuring the rate of growth, stability of detonation, and detonation pressures were employed. Air shock and fragment velocities between charges were measured by electronic and photographic methods, and determination of side-on air-blast pressures and impulse duration were made for about half the shots. Separation distances between donor and acceptor were found to be larger than anticipated both for the AN and the AN-FO. With AN-FO acceptors and a 16-gage steel faced donor, one initiation occurred at a separation of 53 feet or nearly 16-charge diameters; with AN, initiation occurred at 4 to 5-1/2- charge diameters.

Jan 1, 1966

By Galen G. Waddell

Dilation and contraction of the rock surrounding horizontal access open-ings of a deep mine were analyzed during stope advance to determine what type of measurements, made with relatively inexpensive instrumentation, would best reflect the rock behavior. A variety of instruments, mostly mechanical extensometers, were used. Detailed descriptions are given of Down-the-hole extensometers, floating rockbolt clusters, transit surveys, and other instruments and measuring techniques. Although all of the radial-deformation-rate graphs illustrated useful rock behavior data, the most informative graphs were compiled from data procured with the radial extensometers that penetrated, to various depths, the rock around the access openings. An analysis is given of measurement data on the rock around lateral drifts and across and adjacent to the nearly vertical vein of the Star mine, Burke, Idaho. Several useful relationships were found between the rock deformation rate and the stoping process. Information was produced on the elastic state of rock around an underground opening, effectiveness of stope support, rheology of rock, zone of influence around stopes, effectiveness of rockbolts, axis of maximum strain in a plane perpendicular to the long axis of the lateral, and other phenomena. This information could be of particular value in determining location, design, and support of underground openings.

Jan 1, 1966

By H. E. Perlee

Autoignition temperatures and limits of flammability of nine halogenated hydrocarbons in atmospheres of air, oxygen, and nitrogen tetroxide were measured in a modified standard autoignition apparatus and limit-of-flammability apparatus previously developed at the Bureau of Nines. Of the nine halogenated hydrocarbons investigates--bromochloromethane, bromotrifluoromethane, bromochlorodifluoromethane, 1,1,2-trichlorotrifluoroethane, 1-bromo-l-chloro-2,2,2-trifluoroethane, dibromodifluoromethane, l,2-dibromo-1,1,2,2-tetrafluoro-ethane, 1,1,1,3,3-pentachlorotrifluoropropane, and l-bromo-2,4-dichloro-1,1,2, 3,3,4-hexafluorobutane--two formed flammable mixtures with nitrogen tetroxide and six with oxygen; none formed flammable mixtures with air. Three of the halogenated hydrocarbons formed no flammable zones with any of the three oxidizing atmospheres. For those halogenated hydrocarbons that supported combustion in oxygen atmospheres, explosion pressures developed during constant-volume burning of mixtures near the middle of the flammable zone were observed to range from about 6 psig for dibromodifluoromethane to 158 psig for 1-bromo-1-chloro-2,2,2-trifluoroethane. In all cases, the calculated burning velocities of these mixtures were less than 8 in/sec.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted phosphate beneficiation studies to determine the influence of mineralogical and textural features on the recovery of phosphate from select bed and composite samples representing different phosphate rock types of the western Phosphoria Formation. Batch heavy-liquid tests showed that ore grade) pellet size, and type of interstitial material were significant parameters affecting concentrate grade and recovery. Recoveries at acid grade (31.5 percent P2O5) ranged from 98 to 56 percent. Liberation was essentially complete at 28 mesh, and recoveries tended to drop when overgrinding occurred.

Jan 1, 1966

By J. W. Town

The Bureau of Mines conducted petrographic classification and flotation studies to determine if acid-grade concentrates could be obtained from individual and composite samples from the Meade Peak member of the Phosphoria Formation, Idaho. The petrographic studies were made to determine the effect of compositional features on concentration of phosphates. The ore grade, ovule size, and clay content were the main features affecting grade and recovery of phosphate. Flotation results on roasted ore with a tall oil emulsion scheme showed that beds containing over 10 percent P2O5 could be beneficiated and composited with the two high-grade beds to produce a composite concentrate containing 31.9 percent 05 at 84.3 percent recovery. Treatment of these intermediate-grade phosphate beds by flotation increased ore reserves over 200 percent and increased the ore-to-waste ratio in the ore zone from 1:5.7 to 1:0.27.

Jan 1, 1966

By R. F. Abernethy

A modified Unterzaucher method was applied to the direct determination of oxygen in coal. Coal samples were pyrolyzed in a nitrogen atmosphere, and the gaseous oxygen compounds liberated were converted to carbon monoxide by a platinized-carbon catalyst at 9000 C. After passing over heated copper and through a tube containing soda-asbestos and magnesium perchlorate, the purified carbon monoxide was oxidized to carbon dioxide by iodine pentoxide--liberating an equivalent amount of iodine. The iodine was titrated with 0.02 ~ sodium thiosulfate; in a few tests the weight of carbon dioxide produced was determined. Direct oxygen determinations of coal included organic oxygen from the coal substance, plus a small quantity of inorganic oxygen derived principally from carbonate minerals and from combined water of silicates in the mineral matter. The influence of mineral matter on the direct oxygen determination was investigated by testing (1) untreated coal, (2) demineralized coal from which most of the mineral matter except pyrite was removed by treatment with hydrofluoric and hydrochloric acids, and (3) coal samples treated with dilute hydrochloric acid.

Jan 1, 1966

By R. L. Benner

The Bureau of Mines investigated the ZnO-Fe2O3-Fe3O4 system at 1,000°, 1,300°, and 1,400° C, with oxygen pressures between 1.0 and lx10-4 atmospheres. The results, divided into the thermodynamic properties as related to the spinel structure, and the thermodynamic properties as related to zinc concentrate roasting, were used to calculate the activities of ZnO, Fe2O4, and Fe3O4 within the spinel solid solution region of the ternary system, and the pseudo-binary activities of ZnFe2O4 and Fe304. The activities of both systems show large positive deviations from Raoult's Law, especially at high Fe3O4 concentrations. The free energies, the enthalpies, and the entropies of mixing for the binary system were calculated from the binary activities, and the entropies of mixing were compared with two statistical models, one representing an ideal solution, and one representing the mixing of a normal with an inverse spinel. The binary entropy of mixing seemed to be better represented by the latter statistical model, indicating that the tetrahedral and octahedral cations of the reactants tend to remain in the product, even at the high temperatures of the study. This comparison also indicated that the cations of the components are the major contributing factors to the thermodynamic properties.

Jan 1, 1966

By Willard L. Hunter

The Bureau of Mines studied the effect of temperature upon the reduction of chromite by carbon and the relative reducibility of chromites as a function of their composition. Ferric oxide was also studied to provide comparative data. Pellets weighing approximately 1 gram and containing 70 percent ferric oxide, chromic oxide, or chromite and 30 percent graphite were subjected to closely controlled temperatures under a flow of argon for 15 minutes. The amount of CO and CO2 evolved was measured, and the reduced sample was analyzed by X-ray diffraction techniques. The reduction of Fe2O3 was studied over a temperature range of 600° to 1,400° C, while the reduction of Cr2O5 and chromite was conducted from 9000 to 1,621° C. The temperature above which appreciable reduction of Cr203 by graphite took place was 1,125° C. The temperature at which significant reduction started for three of the four chromite samples was approximately the same, indicating that there was concurrent reduction of iron and chromium oxides in the chromite mineral rather than selective reduction of iron oxides followed by reduction of chromic oxide. Rhodesian chromite appeared to dissociate at a lower temperature with concurrent reduction of iron. Based on the temperature at Which chromite was 50 percent reduced in 15 minutes, Transvaal chromite reduced most easily, followed by Mouat, then by Kampersian, and finally by Rhodesian DFC material. Statistical analysis of test results indicated that the ferric iron content of chromites affects their reduction behavior more than any other constituent.

Jan 1, 1966

By Jack G. Croeni

A study was made by the Bureau of Mines to determine the influence of high energy-rate deformation on the structures and properties of low-carbon steel, stainless steel, titanium, titanium-6 percent aluminum-4 percent vanadium, beryllium, molybdenum, and tungsten. The purpose of this study was to determine relative formability, the effect of energy and temperature on metalworking parameters and resulting structures, and the properties of materials formed by this technique. Forming techniques were limited to upset forging and direct extrusion on pneumatic-mechanical forming machines. Results show that considerable grain refinement can be achieved by careful control of deformation and forming temperature by high energy-rate techniques. Significant improvements in strength were observed as a result of this refined structure. Approximate deformation resistance as a function of temperature was determined for a variety of materials.

Jan 1, 1966

By James W. Myers

The Bureau of Mines studied factors affecting ignition of coal mine refuse and on methods for control of burning. Laboratory experiments showed that air permeates more readily through segregated than through nonsegregated refuse and that air permeability is greater through coarse than through fine particle refuse. Minus 3-1/4-inch refuse ignites spontaneously more readily than minus 1/4-inch refuse. The burning of a 1,000-pound conical coal pile was con-trolled by capping with an 18-inch-thick layer of minus 1/4-inch refuse containing 37 percent combustible. In field trials, the burning of refuse at operating mines was controlled by capping with a layer of fine refuse. Water, applied as a spray or by injection, quenched surface flames and cooled the burning waste. Inspection of refuse piles at operating mines showed that the spontaneous ignition tendency is affected by the exposed surface relative to the total volume and the segregation of particles during dumping.

Jan 1, 1966