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By Jerry B. F. Champlin

The successful injection of liquids into subsurface permeable formations for production stimulation, storage, or waste disposal requires a rapid, precise, and accurate method of determining the permeability of porous solids. This report describes a method and apparatus, developed by the Bureau of Mines, that use the principle of specific-volume permeametry. Calibration of the apparatus over a wide range of permeabilities and standardization of several apparatus constants have eliminated many of the tedious calculations and problems of manipulation common to some other methods. Improvements in reproducibility and accuracy have resulted from reducing experimental measurements to one parameter--time. Specific permeabilities of reservoir rock samples are determined directly from a chart that relates elapsed time to a permeability equivalent to that determined by bubble-tube measurements.

Jan 1, 1962

By Michael G. Zabetakis

Investigation of gas explosions usually reveals that the combustible gases have come from transmission and storage facilities or from natural gas or oil wells. However, combustible gases such as methane and hydrogen can derive from biological processes. Hazardous situations have been created in the past by the use of abandoned mines for the disposal of sewage and rainwater, by the interconnection of storm and sanitary sewers, by sealing the openings in manhole covers when repaving the roadway over a sanitary sewer, and by the construction of buildings over or near garbage fill areas without adequately providing for the release of combustible gases.

Jan 1, 1962

By Lowell Stroud

This report is the third in a series presenting equilibrium vapor-liquid data for helium-bearing natural gases. The first two reports contained phase data for the gases processed for helium at the Bureau of Mines Amarillo and Exell, Tex., helium plants. The present report offers similar information for a lower-helium-content (0.75 mole-percent) natural gas to be processed in the Department of the Interior's long-range helium-conservation program. A windowed-cell apparatus was used to obtain 218 samples of equilibrium vapor and liquid phases at 73 experimental conditions ranging in temperature from -100° F to -275° F and in pressure from 100 to 500 psi. From the phase data, the condensation characteristics, helium solubility, and equilibrium-vaporization-coefficient data for helium, nitrogen, and methane were evaluated. The effect of using a. preliminary hydrocarbon trap upon the subsequent vapor-liquid compositions is reported. A brief comment regarding the composition effect of passing the gas through a gasoline-removal unit is also included.

Jan 1, 1963

By James S. Browning

The Bureau of Mines conducted laboratory batch and small-scale continuous selective flotation tests of barite-fluorspar ores from two deposits near Marion, Ky., to determine the technical feasibility of recovering commercial grade fluorspar and barite concentrates. The lignin sulfonate-sodium fluoride method of floating the fluorspar successfully produced acid-grade fluorspar concentrates. Flotation of the barite from the fluorspar tailing using petroleum sulfonate collector yielded concentrates suitable for use in compounding oil-well drilling mud. The fluorspar and barite recoveries were about 82 and 85 percent, respectively.

Jan 1, 1963

By D. Bienstock

To develop a rugged catalyst capable of withstanding hydraulic attrition resulting from the oil-circulation process for synthesizing liquid fuels, use of an iron catalyst containing an active coating surrounding an inert solid core of metal was investigated. This massive-iron catalyst in the form of steel shot and lathe turnings was activated by partial oxidation with steam at 600° C, impregnated with alkali, and reduced with hydrogen at 450° 6. The massive-iron catalysts were resistant to oxidation and spalling, and a 6-month catalyst life was attained. Higher operating temperatures could be employed than with fused iron oxide catalysts, resulting in greater gasoline yields. Because the lathe turnings pack with void volumes of 70 to 90 percent, it has become possible to employ a fixed bed without the danger of cementation that occurs with fused iron oxides.

Jan 1, 1963

By R. F. Zaffarano

Reservoir oil in the Greater Aneth area, Utah, part of the Paradox basin, was studied to detect variation in oil characteristics within the reservoir and to determine its relation to age of accumulation and fluid equilibrium. At least three subsurface oil samples were obtained from each of the four largest of five field divisions comprising a producing area of 45,000 acres. Height of the oil column in the Pennsylvanian Desert Creek zone is about 230 ft. In general, the oil characteristics were found to be uniform across the area, and averages were developed for use in engineering applications. Average saturation pressure was 1,780 psia; the oil was undersaturated at the initial reservoir pressure, 2,200 psia. Variation in saturation pressure shows a lack of complete fluid equilibrium and continuing diffusion of solution gas from the main body of the reservoir to two extensions linked by narrow arms. By assuming early accumulation, the time involved in this diffusion process was calculated to be about the same as the age of the reservoir formation. Cause of the concentration of gas in the main body is attributed to differential entrapment during accumulation of oil and gas from an exterior source.

Jan 1, 1963

By George H. Johnson

This report describes the procedures and summarizes the results of an investigation of surface subsidence above caving blocks at the San Manuel mine, San Manuel, Ariz., in order to obtain quantitative information on subsidence and ground movement caused by mining large volumes of ore. This investigation is one part of an overall study of rock mechanics being undertaken by the Bureau of Mines. Attention was given to the improvement of a rapid and precise method of surveying a large number of subsidence pins and cracks in the surface terrain. Photogrammetric methods were used as an adjunct to the triangulation subsidence surveying as well as in ordinary topographic work Maps of various kinds were prepared to show the results obtained. The computation of the survey notes was programed for an electronic digital computer at a saving of time and expense over the use of a desk calculator and trigonometric tables.

Jan 1, 1963

By Frank Parrish

History and performance data of 17 water-injection projects in Cooke and Grayson Counties in north Texas are presented for the purpose of studying and comparing operating practices and oil-recovery techniques. Water is injected into Strawn and Canyon sands of Pennsylvanian age. The principal formation flooded is the Strawn, which ranges in depth from 725 to 6,900 ft in the projects covered. Estimated ultimate recoveries range as follows: Primary, 22 to 494 bbl per acre ft; and secondary; 63 to 296 bbl per acre ft. These figures represent the following percentages of original oil in place: Primary, 10 to 46 pct; and secondary, 8 to 23 pct. Shallower projects; 725 to 1,500 ft in depth, had higher average primary and secondary recoveries than did deeper projects. Crude-oil gravity, which ranges from 20° to 45° API, was not relatable to yield of secondary recovery oil. Analysis of the data indicates that five-spot injection patterns will yield the highest percentage of oil remaining at start of flooding; that is, 28.8 pct for five-spot injection patterns, compared with 20.8 pct for line-drive patterns and 11.6 pct for random patterns. Waterflooding in this area appears to be very successful. Secondary recoveries of most projects are expected to nearly equal primary recoveries.

Jan 1, 1963

By Robert V. Berryhill

Reconnaissance studies of beach deposits along approximately 220 miles of the shoreline of Bristol Bay, Alaska, were made to determine if more detailed investigations were warranted. In addition to preliminary mapping of the deposits, samples were obtained from auger borings spaced at 1-mile intervals in key areas; shovel samples were collected to supplement the borings. Most samples were roughly concentrated in the field; magnetic separation tests, petrographic analyses, and determinations for radiometric equivalent uranium, gold, platinum, iron, and titanium were made in the Bureau of Mines laboratory at Juneau, Alaska. Spot samples from some beaches along the shores of the Alaska Peninsula indicate small deposits containing up to 10 percent recoverable titaniferous magnetite; some larger deposits were indicated to contain from 1 to 2 percent total heavy metal, principally as titaniferous magnetite. Significant amounts of other commercial minerals were not detected.

Jan 1, 1963

By J. P. Morris

An experimental blast furnace in normal operation was quenched by substituting cold nitrogen for the hot blast air. More than 2,200 samples from the stack, bosh, and hearth were taken; 500 of these were selected for detailed analysis. Deductions are made as to the patterns of burden movement and gas flow; the reduction of iron oxides, including a comparison of ore and sinter; and the behavior of sulfur above the smelting zone. Metal and slag beads from the bosh were analyzed, as were samples from the hearth metal and slag. A brief description of a petrographic examination of the quenched burden is included.

Jan 1, 1963

By Allan F. Smith

The influence of hydraulic fluids on spontaneous heating in bituminous coals is determined by measurement of the temperature increases produced in coal-fluid mixtures heated to a temperature sufficient for the initiation of self-heating. Similar tests on as-received coal samples and water-coal mixtures are compared with the results obtained for the various hydraulic fluids. Three of the four coals were sampled from coalbeds known to have a history of spontaneous heating. The data provide a basis for predicting the possible effects in gob or carbonaceous refuse of coal mines.

Jan 1, 1963

By James S. Browning

Recovery of fine mica from a sample of impounded tailing from the Dixie Mines, Inc., crushing and screening operations, Heflin, Ala., was investigated to determine if plant losses of mica could be reduced while econmically producing a commercially acceptable mica concentrate. Conventional wet-tabling and agglomerate-tabling methods yielded concentrates assaying about 95 percent mica from the tailing that contained 17 percent mica. Products containing about 98 percent mica and accounting for mica recoveries of 86 percent were obtained by flotation, using as reagents sulfuric acid, kerosene, and coco amine acetate (a mixture consisting chiefly of dodecyl and tetradecyl amine acetates). The results of the batch flotation tests were verified by tests in a small continuous flotation pilot plant.

Jan 1, 1963

By H. E. Powell

A laboratory investigation was conducted by the Bureau of Mines to study the magnetic characteristics and to measure the magnetic susceptibility of the mineral siderite. All susceptibility measurements were made by the method of Gouy on powdered samples and at room temperature. Specific susceptibilities of samples from 15 different locations, domestic and foreign, were determined. Values ranged from 66 to 103 (10-6) cgs electromagnetic units. The relation of susceptibility to mineral composition is discussed in this report. The specific susceptibilities of 76 minerals are tabulated in an appendix.

Jan 1, 1963

By Frank A. Peters

A series of evaluations is being made to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. These evaluations include the estimated operating and capital costs as well as recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The three processes considered in this evaluation are designed to leach alumina as aluminum sulfate from calcined clay with sulfuric acid and to remove the silica residue by filtration. The filtrate from leaching is then purified by one of the following methods: Removal of iron in electrolytic cells using mercury cathodes; removal of iron by chemical precipitation through the formation of an iron-manganese complex; or precipitation of the alumina from an aqueous-ethanol solution, leaving iron in solution. Both the operating and capital costs for these processes are higher than those for the Bayer process. For plants producing 1,000 tons of alumina a day, the estimated operating costs per ton of alumina are: Electrolytic iron-removal process........... $81.35 Chemical iron-.removal process............... 82.08 Ethanol purification process............... 86.17 The investment in mercury is not part of the operating cost since this cost is considered equivalent to catalyst cost which would not be shown. The estimated capital investments for 1,000- ton-per- day plants on a Marshall and Stevens chemical equipment index basis of 240.0 are: Electrolytic iron-removal process...... $116,775,500 Chemical iron-removal process............... 99,418,900 Ethanol purification process................ 94,210,200 These investments include the working capital but not the land for each of the processes. Included in the electrolytic iron-removal process is an investment of $4,859,400 for mercury. Investigation of other methods for removing iron, of the decomposition operation, and of the leaching operation could reduce these costs.

Jan 1, 1963

By Hillary W. St. Clair

This is an initial progress report on a theoretical study of the iron blast furnace. The purpose is to develop a thermochemical model that will simulate mathematically a real furnace. An analysis is made of the behavior of a hypothetical furnace, operating adiabatically on pure ferric oxide, graphitic carbon, and dry air. Relationships are derived for carbon consumption, gas composition, and reaction temperature for a furnace operating at steady state, and in which the smelting rate is slow enough for the gas and solids to approach thermal and chemical equilibrium. Analyses are made for two contrasting types of gas flow: (1) Nonturbulent flow, having no vertical mixing; and (2) turbulent flow, having perfect mixing during each step of the process. It is shown that some vertical mixing is essential for complete reduction of ferrous oxide and that the extent of vertical mixing is one of the critical factors in the behavior of the furnace, This analysis indicates that the thermochemical relationships in a blast furnace can probably be best simulated by a finite series of gas-solid reactors through which gas and solids flow countercurrently and in which the temperature and composition of gases and solids are assumed to be uniform. Any degree of vertical mixing can be approximated by the proper choice of the number of reactors.

Jan 1, 1963

By R. D. Berkenkotter

Titanium and iron assays obtained from cores of three diamond-drill holes from the Cebolla Creek titaniferous iron deposit were evaluated by statistical techniques to obtain information concerning the mineral characteristics of the deposit and to make a preliminary determination of sampling requirements for the deposit. A range of sample volumes representing sizes from one-sixth NX core 2 feet in length through full NX core 10 feet in length were prepared by split-ting the NX core with a diamond saw and combining pulverized splits. Results indicate the existence of at least two statistical populations having different average grades of iron and titanium. Each has an assay frequency distribution that is not normal but is highly peaked (leptokurtic). Frequency distributions of assays from specific altered zones of the drill holes appear to be normally distributed. Increasing the cross-sectional area of the sample unit to change assay volume did not result in significant changes either in assay values or the resulting frequency distributions of assays. However, when assay volume is increased by increasing sample interval, the shape of the assay frequency distribution changes, and a normal distribution of assays is approached. Positive correlation exists between titanium and iron assays. The degree of correlation, although very significant, is too low to use for prediction purposes. Although the amount of data from three widely separated drill holes is not sufficient to establish an average grade for this large deposit, it indicates a range of expected assay values and provides some information for determining requirements of future sampling for evaluation purposes.

Jan 1, 1963

By C. H. Schack, K. C. Dean

An investigation was made to devise and evaluate a flexible flotation method for beneficiating typical tactite types of calcareous scheelite - bearing ores ; these scheelite - bearing ores are available in large tonnages in deposits containing 0.2 to 0.3 pct tungsten trioxide . The objective was to achieve a high recovery of the tungsten in concentrates , containing a minimum of 10 pct WO3 , that would be suitable for chemical processing into high- quality synthetic scheelite . The principal problems encountered and resolved by bench- scale flotation tests on ore samples from five different deposits were to define the conditions and reagent combinations essential for ( 1 ) achieving selective flotation of a small amount of scheelite from a large amount of calcite and ( 2 ) controlling the effect of small amounts of calcium , magnesium , and iron salts in the ores and water used . The flotation process was evolved from batch tests and continuous runs in a pilot - scale mill with a capacity of 100 lb per hour . The flotation process comprised ( 1 ) removal of sulfide minerals , ( 2 ) conditioning the residual ore pulp with sodium carbonate , quebracho , and trisodium phosphate , and ( 3 ) rougher flotation and single - stage cleaning of a scheelite concentrate . In a pilot plant run , over 91 pct of the tungsten was recovered from ore containing 0.27 pct WO3 , in a concentrate containing 11.2 pct WO3 .

Jan 1, 1964

By Oliver Q. Leone

The effect of oxygen content in the anode metal on titanium electrorefining characteristics was studied. Increasing quantities of oxygen in the anode resulted in increased anode scale formation, decreased anode and cathode current efficiencies, lower titanium recovery efficiencies, and higher oxygen content of the cathode products. The titanium electrorefining process performed best when the anodes did not contain more than 0.5 percent oxygen, although anode dissolution was recorded for alloys containing up to 25 percent oxygen. Back emf affords a useful index of an alloy to electrorefining.

Jan 1, 1965

By F. W. Hoertel

The effects of certain process variables on the grain size, grain type, and microhardness of vapor-deposited tungsten were established, and the near-optimum parameters and the efficacy for the vapor deposition process were determined. No significant change in the grain size or microstructure resulted from ultrasonic vibration of the substrate during deposition, from variations in the hydrogen (H2) to tungsten hexafluoride (WF6) ratio, or from small increases in reaction-chamber pressure. Near-optimum conditions were continuous deposition at atmospheric pressure, a deposition rate of 2-mils thickness/square inch of substrate area/hour, a temperature of 5500 C, and a hydrogen to WF6 ratio of 4:1. The addition, individually, of about 2 volume-percent of butane, 24 volume-percent of carbon dioxide, or 4 volume-percent of propane to the hydrogen and WF6 mixture produced deposits with the finest grain size for each gas. A corresponding increase in microhardness accompanied the decrease in grain size. The addition of gases did not alter the columnar microstructure found in vapor-deposited tungsten.

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