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By Roy L. Wilfong

The thermal decomposition of the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of praseodymium, neodymium, and samarium was investigated thermogravimetrically in the temperature range 25° to 1,500° C. Each salt was decomposed at a heating rate of 2.5° C, per minute. The pyrolytic sequences have been identified and the temperatures of formation of inter-mediates, the minimum oxide formation temperatures, and values for loss on ignition have been determined. The nonstoichiometric ranges between Pr6011 and Pr203 and the extent of these ranges have been determined for oxides derived from the carbonate, nitrate, and oxalate salts of praseodymium. The alum and sulfate salts of praseodymium produced the sesquioxide without forming the intermediate non-stoichiometric oxides. The temperature limits of formation and regions of stability for the alums and sulfates were better defined than were those for the carbonates, nitrates, and oxalates. The minimum oxide formation temperature increased in the order of samarium, neodymium, and praseodymium irrespective of the anion.

Jan 1, 1962

By H. C. Fuller

Rhodonite, a manganese silicate, occurs as an important component of extensive veins in the San Juan district of Colorado. Recent work by the Bureau of Mines has demonstrated that typical ores of the area can be upgraded to about 30-percent manganese content. Because of their siliceous nature, such concentrates require further processing to convert the manganese into more usable forms. The investigation described in this report demonstrates the technical feasibility of producing silicomanganese from a rhodonitic concentrate by electric smelting methods. The rhodonitic concentrate used in the smelting research was prepared by dry high-intensity magnetic separation of ore from the Silver Queen vein. The concentrate contained 29 percent manganese, 2 percent iron, and 41 percent silica. The principal minerals in the concentrate were 35 percent rhodonite, 30 percent rhodochrosite, and 25 percent quartz and chalcedony. Limestone was used as the flux and coal was used as the reductant. These minerals were crushed and screened to minus 1/2-inch plus la-mesh size.

Jan 1, 1962

By L. H. Banning

This investigation was undertaken to obtain basic information necessary for the design and operation of a plant for recovering metallic values from nickeliferous laterite and serpentine of the Philippine Islands. It was divided into three parts: (1) Mineralogical studies and preliminary mineral dressing tests; (2) electric smelting of the ores, upgrading of ferronickel by blowing with oxygen, smelting laterite slag to produce crude iron, and the production of mild steel; and (3) nickel and cobalt recovery from upgraded ferronickel. Results of the investigation indicate that it should be feasible to recover nickel, iron, and possibly cobalt products from the laterite and ferro-nickel from the serpentine. Mineralogical studies were made on representative fractions of the laterite and serpentine tonnage samples and on five selected samples; mineral dressing tests were made only on laterite. The nickel occurs principally associated with hydrous iron oxides and chemically combined with serpentine; garnierite was the only discrete nickel mineral identified, and it was found in a highly decomposed serpentine. The bulk of the cobalt was found in wadlike manganese oxide material. Approximately twice as much chromite was found in the laterite as in the serpentine, By mineral dressing techniques, laterite was separated into two fractions: one fraction contained over 90 percent of the nickel and cobalt, and 83 percent of the iron; the other fraction contained 74 percent of the chromium. A cobalt concentrate (1.1 percent Co) was produced by a scrubbing and sizing procedure.

Jan 1, 1962

By J. R. Ross

A reconnaissance for sources of scandium and a metallurgical investigation of recovery methods for byproduct scandium from uranium mill solutions were conducted by the Bureau of Mines. The work on scandium was undertaken to obtain information on domestic resources and to explore and develop recovery procedures in consonance with the Bureau's long-range program for conservation and wise utilization of mineral resources. The element scandium is widely distributed in the earth's crust in trace amounts, but it seldom occurs as an important constituent in any mineral. An exception is thortveitite, (Sc,Y)2 Si207) a rare mineral that contains various amounts of scandium and yttrium and may contain up to 42 percent scandium oxide (SC203). Knowledge of the chemistry of scandium has expanded rapidly in recent years (1, 4, 9)4 but only fragmentary information is available about the metal because it is still largely a laboratory curiosity without established uses (2, 3). A recent study shows some of the physical proper-ties of the metal are (1) density of 3.05 grams per cubic centimeter) (2) melting point of 1,540° C, (3) hexagonal close-packed structure) (4) hardness of about 50 Brinell (500-kilogram load), and (5) an alloy behavior similar to yttrium and rare-earth metals (2). The price of $2,850 a pound for scandium oxide of 99.9 percent purity and $2,700 a pound for oxide of 99 percent purity reflects the scarcity and complex chemistry of the element.

Jan 1, 1962

By William R. Wayment

The objective of this investigation was to obtain data on friction-head losses of sand slurries during their transport in pipelines. The data ultimately will be used in designing hydraulic transport systems. Information that was incidental to the primary objective was gathered on degradation, changed percolation characteristics, and critical velocities of the slurries~ Tests were made in a closed-circuit pilot plant, with one type of tailing, through horizontal 2-, 3-, and 4-inch-pipe test sections at various pulp densities and flow velocities. Tests were made in a closed-circuit pilot plant, with one type of tailing, through horizontal 2-, 3-, and 4-inch-pipe test sections at various pulp densities and flow velocities. Approximately 2,000 tests were run in the pilot plant. The ranges of flow velocities used in the experiment were 2.8 to 19 f.p.s. in the 2-inch line, 4 to 14.5 f.p.s. in the 3-inch line, and 4 to 11 f.p.s. in the 4-inch line. Velocities were varied in increments of 0.5 f.p.s. through the entire velocity range in each pipe size. Densities were varied in 3-percent increments from 40 to 70 percent solids by weight except for one series of tests in the 2-inch line; in this series, densities were varied in 5-percent increments from 5 to 65 percent solids by weight.

Jan 1, 1962

By John D. Bardill

Data from extensive tests was obtained on friction-head losses of various sand slurries, composed of materials of different specific gravities and under varying transport conditions, to provide useful information for designing hydraulic transport systems. The tests were run in a pilot plant through 2-, 3-, and 4-inch lines with slurries composed of relatively pure barite and limestone solids. Available grinding and classification equipment did not permit attaining a comparable size distribution in the two materials tested, thus preventing direct correlation of friction-head loss values to physical properties or mineral composition. A total of 495 measurements were made of limestone slurries in the 2-, 3-, and 4-inch pipe test sections at flow velocities from 6 to 14 feet per second and pulp densities from 40 to 70 percent solids. A total of 640 measurements of barite slurries were made in the 3-and 4-inch pipe test sections at flow velocities between 7 and 14 f.p.s. and pulp densities ranging from 40 to 80 percent solids.

Jan 1, 1962

By J. F. Neill, O&apos

The manganiferous schists occurring in the vicinity of Kings Mountain, North and South Carolina, suggest significant tonnages of potential submarginal ores. Although some reconnaissance work in connection with these deposits has been reported, no recent information has been published. Evaluation of the schists as a possible domestic manganese resource has not always adequately considered the fact that the manganese content occurs quantitatively both as oxide and as the silicate, spessartite. The Bureau of Mines investigation herein reported includes preliminary studies to indicate the extent of manganese oxide mineralization and to deter-mine the amenability of the material to sulfur dioxide leaching. The field reconnaissance studies suggest a resource containing in one area an average of 6.4 percent manganese as oxide. The procurement of depth information was beyond the scope of the investigation.

Jan 1, 1962

By H. R. Shell

Fluorphlogopite mica was synthesized from inexpensive and abundant olivine, clay, feldspar, and sand (plus K2SiF6). The raw materials were melted in crucibles and in an internal resistance electric furnace. The melts yielded >95 percent mica. The major difficulty encountered was incomplete settling of the highly dispersed ferroalloy. This problem was not completely solved. Reducing agents tried in melts of 300 to 400 pounds were carbon, silicon, and silicon carbide. Carbon slowly reduced the iron of the raw materials, with much fuming. Silicon apparently was oxidized ahead of the melting and was ineffective under the conditions obtained. By far the best reducing agent was silicon carbide. With silicon carbide, fuming did not occur and ionic iron content of the mica flake approached 0 percent. However, even with SiC, the highly dispersed globular iron did not completely separate from the mica portion. The fluorphlogopite made during this investigation should be suitable for metallurgical use. A byproduct ferroalloy containing about 5 percent nickel, 3 to 5 percent chromium, and some cobalt was obtained. Because of the highly dispersed metallic ferroalloy, the mica was not deemed suitable for electrical or electronic uses.

Jan 1, 1962

By J. G. Croeni

The titanium-iridium alloy system was investigated to determine whether alloys of this system would merit further development as control-rod material for nuclear reactors. A study was made to determine the titanium-iridium phase diagram by using melting-point, thermal analyses, X-ray diffraction, dilatometric, electrical resistivity, and metallographic techniques. The titanium-iridium alloy system was investigated between 500° and 2,400° C. Results indicate the formation of two intermetallic compounds, Ti3Ir rind TiIr3, and one intermediate solid solution centered about the 50 atomic percent iridium composition. A eutectic reaction occurs at 1,475° C, and 19 atomic percent iridium. The Ti3Ir decomposes peritectically at 1,520° C. The intermediate solid solution exhibits a maxima of 2,140° C. at 50 atomic percent iridium. This phase is also believed to undergo an order-disorder transformation at 1,750° C. Another eutectic reaction takes place at 2,000" C. and 60 atomic percent iridium. The compound TiIr3 formed at 75 atomic percent iridium decomposes peritectically at 2,115° C. Further increases in iridium content result in the formation of an iridium-rich terminal solid solution. Information obtained below 900° C. in titanium-rich alloys indicates that iridium acts as a beta stabilizer in titanium, and the authors believe that a eutectoid decomposition of beta-titanium occurs near 500° C. and 10 atomic percent iridium.

Jan 1, 1962

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions 5/ issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and, if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1962

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 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 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 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