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By M. E. Tyrrell

Lightweight basic refractories suitable for use in some sections of the all-basic furnace were developed. Potential advantages of such refractories are lower weight, improved resistance to thermal shock, and less tendency to spall off the working face. Plant trials in positions not subject to heavy loading or severe erosion seem warranted. Forsterite (2MgO.SiO2), stabilized dolomite (2Ca0?SiO2 + MgO), and chrome-spinel [(Fe,Mg)0?(Cr,Al) 031 refractories were fabricated using bubbles as the principal component in the brick mixtures. Bubbles were blown from melts of the basic raw materials as they were tapped from a conducting-hearth arc-resistance furnace. The bubbles were graded, bonded with synthetic Forsterite plus mineralizers, dry-pressed, and fired to temperatures of 1,600° C. or over in a gas-fired kiln. Refractory properties of the bubble brick were compared with those of insulating refractories made by burning combustibles out or dense brick mixtures. Lightweight refractories fabricated of bubbles were one-third lighter in weight than dense bricks of like materials. Their mechanical strength was satisfactory, and their resistance to thermal shock was excellent. In tolerance to open-hearth slag and in resistance to thermal shock, the chrome-spinel bubble bricks wore the best of the refractories tested. Basic refractories of the insulating type were about 40 percent lighter in weight than dense commercial refractories, but they were mechanically weak and not suitable for superduty service.

Jan 1, 1962

By Robert K. Koch

Laboratory-scale studies on defluorination of natural and synthetic fluorspars by pyrohydrolysis at 1,500° C. were made to determine the feasibility of developing a process for producing hydrogen fluoride from siliceous fluorspars. It was found that the reaction (at 1,500° C.) is not promising for process development, even though a silica-free offgas can be generated. The primary difficulty is the low hydrogen fluoride content of the offgases; an HF content of 6 percent was the best achieved. Previous research by the Bureau of Mines has demonstrated that offgases averaging 27 percent hydrogen fluoride can be produced under carefully controlled conditions at 1,280° C. The lower temperature process is a better method for production of HF. However, charges in which the CaF to Si02 mole ratio varied from 0.4 to 2 could be processed with similar results. Also, combined alumina and ferric oxide contents up to 25 mole-percent did not noticeably alter the rate of defluorination. Therefore, virtually any natural siliceous fluorspar would respond in essentially the same manner when exposed to water vapor at 1,500° C.

Jan 1, 1962

By J. P. Capp

The Bureau of Mines conducted field-scale experiments in underground gasification of coal with oxygen-enriched air. A path about 140 feet long was linked at the rate of LO feet per day through a coalbed hydraulically fractured with a mixture of starch gel and sand. During the best gasification period, which extended for 2-1/2 days, 785,000 std. c.f. per day of 124-B.t.u. gas was produced. In other periods the heating value at times was almost 300 B.t.u. per std, c.f,, but sustained production of such gas was not achieved. During gasification, a total of 50 tons of coal was gasified and 114 tons of coal was carbonized. Approximately 12 million B, t .u. per foot of nominal path was recovered at the surface.

Jan 1, 1962

By Henry M. Harris

Low-carbon shales from 65 deposits and 11 sources of coal-mine waste in western Oregon and Washington were tested in a rotary kiln for their suitability as raw material for expanded aggregate. Shales from 41 sources bloated enough to produce crushed, expanded aggregates, weighing less than 65 pounds per cubic foot in the preliminary tests. The samples were judged on the basis of processing qualities, physical properties, and size and uniformity of the source. Nine low-carbon shale deposits and three coal-mine waste sources were selected for more extensive bloating tests and for examination of the expanded aggregates in concrete shapes. Composite samples from these 12 sources and from 2 commercial operations, when processed for testing in concrete shapes, had bulk densities ranging from 37.S to 72.9 pounds per cubic foot. Damp-cured concrete shapes made with these aggregates had bulk densities ranging from S6 to 119 pounds per cubic foot, and all but three of the lightweight concretes had crushing strengths ranging from 3,270 to 6,810 p.s.i. Properties of the lightweight concretes were compared with those of concrete shapes made with commercial aggregates, and with sand and gravel.

Jan 1, 1962

By L. O. Bacon

This Bureau of Mines report summarizes the results of laboratory work in the design of instrumentation for obtaining the dynamic tensile strength of rock at minimum loading. Minimum loading is defined as the lowest tensile loading by pulse reflection to cause fracturing. The instrumentation for obtaining dynamic tensile strengths of rock cores evolved into the use of a compressed-air pellet gun to impact one end of a rock core, suspended by wires, at increasing increments of air pressure. Maximum strain was measured on most or all of the impacts, and the strain at fracture of the core was obtained by extrapolating the pellet velocity-strain curve to the pellet velocity at fracture. Stress at tensile fracture was obtained from the maximum s train, and the dynamic Young's modulus was calculated from the rod velocity by using simple rod theory.

Jan 1, 1962

By Thomas L. McVay

The Bureau of Mines made laboratory batch and small-scale continuous flotation tests of a sample of pegmatite rock from a deposit of the Lithium Corporation of America, Inc., near Kings Mountain, N.C., to determine the feasibility of producing commercial-grade spodumene concentrates. Various reagents and flotation procedures were tested to determine the optimum conditions for floating the spodumene and retarding the gangue minerals. The best results were obtained when sodium fluoride and lignin sulfonate were used as the pulp conditioner and oleic acid was used as the spodumene collector. The continuous flotation tests indicated that commercial-grade. spodumene concentrates analyzing 6.4 pct. Li2O could be produced with recovery of 77 pct. of the lithia in the ore.

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 R. L. Crosby

From studies of wrought magnesium alloys containing rare-earth elements, data are presented on the mechanical properties of the alloys at room temperature and at temperatures of 100°, 200°, and 300° C. Results of studies of the solid-solubility of cerium and zirconium in magnesium as determined by electrical resistance measurements are also discussed and are compared with those of other investigators. The strength of magnesium-cerium alloys did not increase with the addition of vanadium and titanium dioxide. The addition of zirconium increased the tensile strength of the alloys as much as 10,000 p.s.i. at room temperature, but this increase diminished above 100° C.

Jan 1, 1962

By A. B. Whitehead

A spectrographic method for the determination of 18 impurities in cerium is presented. The carrier distillation technique is utilized to separate the spectra of impurities from the complex spectrum of cerium. Metal samples are ignited to the oxide, mixed with silver chloride carrier containing an internal standard, and excited with a 20-ampere direct-current arc. An additional exposure, made after carrier depletion, provides for the determination of refractory elements. Experiments to determine the best carrier, sample-carrier ratio, electrodes, arc current, exposure conditions, internal standards, and any matrix effect are described. The relative standard deviation of the method at the 20- and 200-part-per-million levels is about 25 and 15 percent, respectively. The average relative error is about 20 percent in the 10- to 1,000-part-per-million concentration range.

Jan 1, 1962

By M. E. Tyrrell

The purpose of the work leading to this report was two-fold: (1) To determine the properties of cemented tungsten carbide modified by the addition of one, two, and five percent of titanium diboride, and (2) to compare the properties of these mixtures when sintered, hot-pressed, and flash-welded (resistance-sintered). Minor additions of titanium diboride to mixtures of 94 percent WC and 6 percent Co decrease mechanical strength but increase oxidation resistance in proportion to the amount of the addition. One percent of titanium diboride increased the hardness by 2 Rockwell A units. Hot-pressing produced compacts with the highest density and the best mechanical strength, but losses of cobalt were high and grain growth was pronounced.

Jan 1, 1962

By David Burgess

Natural gas is a general term applied to the gas obtained from oil or gas wells. It is the most widely used of all gaseous fuels. The principal disadvantage in the use of this and other gaseous fuels is the difficulty encountered in the storage and transportation of large quantities in the gas state. Handling in the liquid state is possible, but reduced temperatures are required since methane (table 1) is the principal component of most natural gases that are used as fuels. Actually, liquid storage has been utilized both here and abroad;3 however, the Cleveland disaster4 has pointed out the need for a critical evaluation of the hazards involved in the storage of this cryogenic fuel. Accordingly, a program was undertaken to obtain basic data that could be used to assess these hazards. In this report, the factors to be considered in an evaluation of the fire and explosion hazards associated with any fuel are each discussed briefly. These factors are then used to assist in the design of experiments for the evaluation of the hazards associated with liquefied natural gas (LNG) relative to those associated with other common fuels. Experiments have been conducted on the vaporization of LNG, the mixing of LNG vapors with air, the effect of temperature and nitrogen dilution on the limits of flammability of methane in air, the burning rates of LNG and other fuels, flame radiation, and extinguishment of fires above liquid pools. Based on the results of these experiments, LNG can be stored safely in suitably designed above-ground tanks surrounded by earthen dikes in much the same manner as gasoline.

Jan 1, 1962

By W. W. Agey

This report summarizes results of bench-scale metallurgical studies by the Federal Bureau of Mines on three composite samples representative of the low-grade manganese ores purchased by the General Services Administration (GSA) and stockpiled at Deming, N. Mex., and Wenden, Ariz. Bench-scale flotation tests at the Salt Lake City Metallurgy Research Center showed that all three composites could be beneficiated by flotation to recover 88 to 90 percent of the manganese in concentrates that assayed from 38.5 to 39.0 percent Mn, 10 to 12 percent insoluble, 5 percent CaO, 3 to 5 percent Fe, and 1.3 to 1.7 percent combined Pb plus Zn plus Cu, Sintering studies indicated that specification-grade material could be made from these concentrates by sintering above 1,000° C, and adding either sodium or calcium chloride to the charge to insure removal of enough lead and zinc to meet the specifications.

Jan 1, 1962

By J. Robert Wells

The Bureau of Mines has developed a spectrochemical procedure for determining 19 impurity elements in high-purity titanium metal, titanium oxides, and titanium halides in which all samples are converted to titanium dioxide. Determination of these impurities was studied in the general concentration range of 0 to 1,000 p.p.m., but different determination limits were found for the various elements. The procedure is quantitative for 18 elements but semi-quantitative3 for beryllium and has an overall relative standard deviation of 15.8 percent. Two mixtures were used, one composed of graphite and lithium carbonate plus gallium oxide and the other of graphite and lithium carbonate plus germanium dioxide. Each mixture was blended mechanically with an equal weight of titanium dioxide. Lithium carbonate served as buffer-diluent. Gallium was the internal standard for 1 impurity element, germanium for 7, and titanium for the remaining 11.

Jan 1, 1962

By William J. Campbell

Evaluation by the Bureau of Mines of published expansion values for magnesium oxide shows significant variation in values, which may be attributed to sample variables, experimental errors, or systematic differences between measuring techniques. To eliminate the sample variable in measuring expansion, thermal expansion characteristics of a high-purity polycrystalline magnesium oxide were determined by 21 cooperating laboratories using one or more of the following techniques; X-ray camera, X-ray diffractometer, dilatometer, interferometer, and telemicroscope. All expansion values were corrected by the author to a single reference temperature of 25° C. Linear expansion was expressed as a power series in the form of the following equation. Expansion (percent) = [[ A + B (?t) + C (?t)2] ?t 104] The constants, A, B, and C, were determined by least square techniques for X-ray camera, X-ray diffractometer, and dilatometer data separately, and for combined data of all five techniques. Expansion values are tabulated from 26° C. to 1,400° C. in 2° C. intervals using constants derived from X-ray camera data. Below approximately 500° C., expansion values obtained by dilatometric and interferometric methods are significantly lower than those by X-ray methods; above 500° C., this bias decreases rapidly. Comparison of results within methods showed the least variance for X-ray camera results; dilatometer and X-ray diffractometer results have about the same variance. The average deviations, in percent, between observed and calculated expansion values among methods were approximately 10 percent from 100°C. to 300°C., 5 percent from 300°C. to 500°C., and 2 percent from 500°C. to 1,400°C. Maximum deviations were approximately twice as large in most instances.

Jan 1, 1962

By D. F. Walsh

A study of damping capacity was made on a number of magnesium-base alloys, commercial types and experimental compositions. Hardness and tensile properties were determined, and the microstructure of each alloy was examined. Alloys of low yield strength, in general, possessed high damping ability. A correlation was established between damping capacity and composition.

Jan 1, 1962

By L. F. Willmott

Pulverized high-volatile A bituminous coal was gasified with oxygen and superheated steam in a pressure-gasification pilot plant equipped for slurry feeding. The minimum ratio of water to pulverized coal that could be pumped satisfactorily as a slurry was about 1 to 1. Heating this slurry produced a suspension of coal in superheated steam having a steam-to-coal ratio greater than the 0.3 to 1 proportion that is considered optimum for pressure gasification of pulverized coal. A steam separator removed enough steam to provide ratios down to about 0.5 to 1, but a 0.3 to 1 ratio was not achieved. Gasification of Sewickley coal produced a synthesis gas containing about 36 percent H2, 46 percent CO, and 13 percent CO2, Gas output, gas composition, and coal and oxygen requirements were Virtually the same as for a pilot plant equipped for fluidized-coal feeding. Typical results from the slurry-fed plant at 300 psig were carbon gasified, 95 percent; coal requirement, 34 lb/M (thousand) std cu ft CO + H2 produced; oxygen requirement, 365 std cu ft/M std cu ft CO + H2 produced. The results showed that the two feeding methods are equally satisfactory from the standpoint of gasification. A choice between a fluidized-coal gasification process or a slurry gasification process depends on considerations relating to the coal-feeding phase itself, including capital and operating costs, manpower requirements, safety, and flexibility of operation.

Jan 1, 1962

By F. B. Petermann

The Bureau of Mines conducted electric furnace smelting tests on sintered flotation concentrate and siliceous log-washed are. The flotation concentrate was derived from the Maggie Canyon deposit of the Artillery Mountains area, Mohave County, Ariz., and contained, before sintering, 35.6 percent Mil and 19.4 percent Si02 + A1203. The log-washed ore was from the McGregor deposit of the Artillery Mountains area, Mohave County, Ariz., and contained 31.2 to 33.6 percent Mil, 19.5 to 27.6 percent Si02 + A1203, and 2.5 percent Pb. This work was undertaken to determine the most effective smelting technique for producing standard products from such nonspecification ore and concentrates. The objective was to collect data, using a small furnace, which would be reasonably accurate and permit extrapolation to large-scale practice for comparing with results on specification-grade are.

Jan 1, 1962

By A. A. Cochran

Methods of preparing small heats of steel containing radioisotopes were developed, and the techniques of stripping film autoradiography were used to detect and study the carbide and sulfide phases in titanium-bearing steels. Metallography had revealed areas of titanium sulfide and ferrite or pearlite adjacent to areas of titanium carbide and ferrite, and unidentified, irregular phases at the boundaries between these two areas. Sulfur 35 was used to deter-mine the extent of the titanium sulfide inclusions, and carbon 14 was used to delineate the titanium carbide phase. Individual radioactive areas were located with a resolution of approximately 10 microns. A general background exposure that was not correlated with microscopically visible phases was observed in the carbon 14 autoradiographs. The evidence from both sulfur 35 autoradiographs and carbon 14 autoradiographs indicated that the unidentified inclusions were sulfides rather than carbides. INTRODUCTION The use of radioisotopes to facilitate the work at the Rolla Metallurgy Research Center was expanded in fiscal year 1959 when the Bureau of Mines authorized the installation of an intermediate-level radioactivity laboratory. Before this time, sealed cobalt 60 sources had been employed for radiography, but no tracer work was done. The primary objective of the first experiments conducted in the new laboratory was to supplement physical metallurgy investigations of selected problems in steel research.

Jan 1, 1962

By M. M. Fine

This report describes a Bureau of Mines technical feasibility study of simultaneous reduction and induration of pelletized iron ore to make a product with superior qualities as blast-furnace feed. Highly reduced, physically competent pellets can be made from magnetite and specularite concentrates that contain small additions of bentonite as binder. In batch tests, pellets were dried, surrounded with solid fuel in crucibles, and heated to the reducing temperature. Total iron content of the best products was higher than 80 percent and crushing strength of 1/2-inch metallized pellets ranged up to 600 pounds or more. Comparative tests of several commercial oxide pellets showed a wide range in crushing strengths, but most values were less than 350 pounds. Continuous tests in a rotary kiln resulted in the same degree of reduction, but the pellets had lower crushing strengths because of the limitations in the maximum operating temperature of the small kiln.

Jan 1, 1962

By Charles Prasky

This report describes and appraises recent progress in the development of a differential sulfatizing process for recovering a ferrograde manganese oxide from low-grade manganiferous ferruginous materials in the Cuyuna range. Individual process steps were carried out successfully using a 20-inch-diameter shaft for continuous countercurrent sulfatization of the manganese, a multiple-compartment rotary drum for leaching the water-soluble manganese sulfate, a submerged-combustion evaporator for the recovery of monohydrate crystals of manganese sulfate, and a shaft furnace for the thermal decomposition of sulfate crystals for production of a ferrograde manganese oxide and a sulfur dioxide gas suitable for sulfatization of fresh are. Of the two general kinds of Cuyuna manganiferous materials--the carbonate slates and the oxidized ores--only the slates were studied at pilot scale.

Jan 1, 1963