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By S. J. Gasior

Pilot plant studies showed the technical feasibility of fluidized-bed operation for producing hydrogen and synthesis gas by the steam-iron process. A mixture of iron and iron oxide from 20-to 100-mesh was partially reduced with a simulated producer gas and then oxidized with steam and/or carbon dioxide. Results of tests show the effects of pressure, temperature, bed height, gas-to-solids ratio, type of iron oxide, and composition of gas on the gas and solids conversions during reduction and oxidation. A baffled free-fall solids system was also found operable. The short residence time of about 5 seconds limited conversion of the solids.

Jan 1, 1961

By A. F. Colombo

Laboratory-scale tests were conducted by the Bureau of Mines on an argillaceous Michigan copper ore and mill tailing to determine the feasibility of leaching with acidified ferric sulfate solutions. The ore and tailings, containing 1.24 and 0.24 percent copper, respectively, were from the White Pine Copper Co., Ontonagon County, Mich. The investigation showed that ferric sulfate leaching of the ore and tailings followed a predictable pattern. Thus, with 4 hours of leaching, up to 58 percent of the copper in the ore was extracted, but prolonged leaching (2 to 3 weeks) was required to dissolve more than 90 percent of the copper. Similarly, about 50 percent of the copper in the mill tailings sample was dissolved in a few hours, but 8 days or more were required for extractions of over 90 percent.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Perry County, Ky., are described in this Bureau of Mines report. Seven samples, representing the Hindman, Flag, Haddix, and Fire Clay beds, were carbonized by the Bureau of Mines-American Gas Association (BM-AGA) method, and yields of products and physical properties of cokes were determined. Carbonizing properties of blends of Flag and Fire Clay coals, with 20 and 30 percent Pocahontas No. 3 low-volatile coal from McDowell County, W. Va., also were determined. Expanding properties of the Flag and Fire Clay coals and their blends were determined in the Bureau of Mines sole-heated oven. The Perry County coals tested are high-volatile A bituminous in rank and, with the exception of the Hindman-bed sample, which contained excessive sulfur, were chemically suitable for metallurgical use. The three coals tested in the sole-heated oven contracted less than normal for Appalachian coals of similar rank, Blending the Fire Clay and Flag coals with 20 or 30 percent low-volatile coal increased coke strength appreciably but increased the expansion beyond normal limits for industrial blends.

Jan 1, 1962

By G. W. Birge

Carbonizing properties of the principal coal beds of Butler County, Pa., are described in this report by the Bureau of Mines. Eight samples, representing the Upper Freeport, Lower Freeport, Upper Kittanning, Middle Kittanning, Lower Kittanning, Clarion, and Brookville beds, were carbonized at 900° C. by the Bureau of Mines-American Gas Association (BM-AGA) method. Butler County coals rank as high-volatile A bituminous and are generally characterized by high sulfur content compared with Appalachian coals used for industrial coking. If cleaned, the Brookville and one sample of Upper Freeport coal would be acceptable as the major component of metallurgical coking blends. The other Butler County coals tested would be unsuitable for this purpose because of either excessive sulfur or poor coking properties.

Jan 1, 1962

By A. A. Berk

The Bureau of Mines devised a test nipple for the field study of corrosion in the condensate-return lines of Federal heating plants. Corrosion surveys, made with this device, showed that the deterioration of the piping was caused principally by carbonic acid in the steam condensate. Corrosion problems were brought under control when the carbonic acid concentration in the condensate was decreased. In many instances, this was effected by decreasing the total carbon dioxide content of the feedwater; in others, the condensate acidity was neutralized with volatile, alkaline chemicals. Filming treatment with octadecylamine, reported successful in controlling return-line corrosion in industry, was much less effective in Federal area-heating plants. Laboratory study by the Bureau disclosed that octadecylamine is unstable in heating systems. Analytical methods were developed for this chemical and its degradation products in heating-plant condensate. Field surveys, in using these methods, confirmed the instability of the filming material. Laboratory tests showed that the degradation products are not useful film formers. Since filming treatment has little effect on condensate corrosivity, the piping was corroded where it was not coated by the treatment chemical.

Jan 1, 1962

By D. W. Scott

Thermodynamics is a powerful tool for investigating rotational isomerism in substituted ethanes and related molecules. Accurate calorimetric data can be interpreted to give information, not only about the energy difference between conformations, but also about the shape of the potential barrier hindering rotation from one conformation to another. However, a deterrent to this use of thermodynamics is the labor required to calculate the contributions to the thermodynamic functions for assumed potential functions. Tables of thermo-dynamic contributions for appropriate potential functions can eliminate that labor and greatly facilitate the thermodynamic study of rotational isomerism. In this research, tables of contributions to the thermodynamic functions were compiled for two potential functions typical of some commonly encountered examples of rotational isomerism. TYPES OF POTENTIAL FUNCTIONS Potential function 1, illustrated in figure 1, A, has two equal minima higher than the third. It has the general shape of the barrier to internal rotation in n-butane, for example. The trans conformation of n-butane has the lowest energy, and the two skew or gauche conformations have equal but higher energy. Potential function2, illustrated in figure 1, B, has two equal minima lower than the third. It has the general shape of the barrier in 2-methylbutane, for example. The two C1 conformations of 2-methylbutane have equal energy much lower than the assumed Cs conformation, which has not been observed spectroscopically.

Jan 1, 1962

By W. H. Ode

An investigation of standard methods for determining ash in low-rank* coals showed that generally 60 to 95 percent of the total sulfur in the coal is retained in the ash as SO3. This large sulfur retention causes a positive error in the determined mount of ash of as much as 6 percentage points for the coals examined, although it usually is 2 to 3 percentage points for lignites and about 1 for subbituminous coals. Unless the sulfur content is low or unless a correction is made for the SO3 retained, the fixed carbon and oxygen have an equivalent negative error when determined by difference; also other inaccurate analytical values occur when the data are calculated on an ash- free bas is. No simple modification of the ashing procedure was found that would reduce the sulfur retention to a point where its effect on the ash determination would not be significant, Therefore, for accurate analytical work on law-rank coals, the SO3 should be deducted from the determined ash to obtain a "corrected" ash value.

Jan 1, 1962

By Gerald W. Elger

This report compares the quality of zirconium metal prepared by batch reduction of zirconium tetrachloride by (1) sodium, (2) magnesium, and (3) mixtures of sodium and magnesium. Criteria for quality are based on chemical analyses and hardness testing of zirconium arc-melted from sponge. The best quality zirconium with respect to low oxygen content and hardness numbers was prepared by reaction of zirconium tetrachloride with a mixture of sodium and magnesium. It was found that this reaction could be successfully carried out by two methods: (1) addition of sodium and magnesium before the initial reaction and (2) periodic injection of sodium during reaction of zirconium tetrachloride with magnesium. The largest quantity of metal was found to be recovered from experiments in which a mixture of sodium and magnesium was used. Magnesium appeared to be a better reductant than sodium because magnesium-reduced zirconium contained less oxygen and exhibited lower hardness numbers than sodium-reduced metal.

Jan 1, 1962

By E. L. Singleton

This Bureau of Mines investigation was initiated to study and establish some of the chemical and physical characteristics of the condensed Mno-Si02 system. To prevent oxidation of the manganous ion, I atmosphere of purified helium was used in the furnaces. Solidus-liquidus curves and invariant points were established from melting-point determinations and were supplemented from data obtained by the static-quenching method. Experimental findings and data are for the intermediate compounds of tephroite and rhodonite with their respective eutectics represented at 25.5 and 37.2 weight-percent silica. Tephroite melts congruently at 1,347° C., and rhodonite melts incongruently at 1,286° 8.. A metastable transformation was determined to exist at the 1,347° C. isotherm, the congruent melting point of tephroite. A composite X-ray-diffraction pattern was formulated for synthetic rhodonite. This investigation contributes fundamental data leading toward a better understanding of the more complex slag systems.

Jan 1, 1962

By V. E. Edlund

Pyrometallurgical studies by the Bureau of Mines demonstrated the feasibllity of sintering and smelting a low-grade flotation concentrate made by pilot-plant processing 10-percent manganese ore from the Maggie Canyon deposit, Mohave County, Ariz. Under optimum conditions 85 percent of the manganese in a flotation concentrate that assayed 36 percent manganese was recovered as standard ferromanganese. A blend of this flotation concentrate with high-grade dithionate pilot plant precipitate was similarly processed with a recovery of 90 percent of the manganese. Thorough mixing and pelletizing of the charge before treatment on the sinter hearth was necessary to produce a well agglomerated product by single pass sintering. Although satisfactory sinter was produced from a variety of material combinations, best results were obtained on a charge that contained 80 percent flotation concentrate and 20 percent return sinter fines. This combination was mixed with 6 percent coke, based on weight of concentrate; and 12 percent moisture. Sintering such a charge yielded a well agglomerated product containing over 80 percent coarse material, The results of standard crushing tests showed that the product was physically comparable to iron ore sinters and manganese nodules.

Jan 1, 1962

By R. O. Dannenberg

This report describes aperiments by the Bureau of Mines and reviews theoretical aspects of the use of organophosphate solvent extraction for recovering beryllium from sulfate leach liquors. The leach liquors were prepared by sulfuric acid leaching of lime-sintered low-tenor beryl flotation concentrates. The experimental work on sulfate leach liquors showed that the acidic esters of organophosphates extracted beryllium slowly but in preference to aluminum. Three common alkylphosphoric acids, di- (2-ethylhexyl) (EHPA), heptadecyl (HDPA), and dodecyl (DDPA), in order of decrmsing selectivity, yielded a partial separation of beryllium from aluminum.

Jan 1, 1962

By Heinz W. Sternberg

The literature on electrochemical treatment of coal is reviewed, and possible avenues of further research in this field are discussed in this report. Electrolytic reduction of finely distributed coal resulted in the addition of as many as 9 atoms of hydrogen to 100 atoms of carbon. Reduction of coal extracts at controlled potentials indicated the presence of condensed aromatic hydrocarbons and reducible quinones in coal. As much as 65 percent of low-rank coal can be made alkali soluble by electrochemical treatment. Higher rank coals gave smaller yields of alkali-soluble products. However, the nature of this reaction is not clear. The difficulty of reducing coal electrolytically is probably due to the insolubility of coal and not to any structural peculiarity. Reduction of coal by electrolytically generated radical anions appears to be a promising approach for further research.

Jan 1, 1962

By D. J. Stoops

The object of the research described in this paper was to investigate the effect of metallurgical and surface treatments on the corrosion behavior of arc-melted reactor-grade zirconium in cupric or ferric chloride solutions. An apparatus was constructed and specimens of various metallurgical conditions and surface treatments were tested for 6 days at 35° C., with aeration. Some correlations were observed between corrosion rate and the metal's condition and treatment, Specifically, the unattacked or least attacked specimens were those that had been etched as a final treatment before testing. The most severely attacked specimens were those that had been vacuum-annealed as a final treatment before testing. The moderately attacked specimens were those neither vacuum-annealed nor etched, but having a final surface treatment which left a cold-worked surface. Attack by cupric and ferric chloride was by pit- ting with no preference for grain boundaries, The corrosion scale was cow posed predominately of very fine zirconim particles, Particles from the FeC1,-corroded specimens were more pyrophoric than those from CuCl2-corroded specimens, and appeared to have a higher surface area to volume ratio. Comparison of results to those of previous investigators showed that at certain salt concentrations the more pure, reactor-grade zirconium was quite resistant to attack while the less pure, graphite-melted zirconium was severely attacked.

Jan 1, 1962

By G. L. Hopps

Various chemicals, including compounds of copper and lead, were added to a mixture of No. 2 and No. 6 fuel oils that was fired in an experimental furnace. Tests were made to determine (1) the effectiveness of these chemicals in removing soot deposits on probes devised to simulate heat-transfer surfaces in boilers and (2) the effectiveness of the chemicals in preventing the deposition of soot on the probe surface. Test conditions were regulated so that the temperature of the products of combustion adjacent to the probes was in the range of 625° to 700° F. The clean-metal temperatures of the air-cooled probes were comparable with the water-tube temperatures in boilers operated at 40 to 100 p.s,i.g. The dosages of the fuel oil additives used in these tests were generally larger than those usually recommended for most proprietary compounds.

Jan 1, 1962

By Kevin Malone

Chrysotile asbestos occurs in many counties in California, and a small production had been reported at times, but development of deposits had been disappointing. A reconnaissance survey by the Bureau of Mines indicated that several deposits in the serpentine belt in Shasta, Trinity, and Siskiyou Counties might contain enough asbestos of filler grade to supply the growing demand on the west coast. Accordingly from 1956 to 1958 parts of the Mount Eddy and Shasta View deposits were investigated by trenching and diamond drilling to determine their potential. The work comprised construction of roads, bulldozer trenching, excavation of areas for diamond drilling, sampling, and upping. The trenches were excavated to expose the surface extent of some of the asbestos-bearing areas, To determine the downward continuation of asbestos-bearing sections and to secure samples for test purposes, six diamond drill holes, totaling 1,738 linear feet, were drilled in two selected areas. The trenching and core-drilling indicated that the asbestos-bearing material occurs as ribs and lenses of varying thicknesses in a broad belt of serpentine, about 600 feet wide and several miles long,

Jan 1, 1962

By R. L. Lincoln

The effects of adding from 1 to 50 atomic percent (a/o) to vanadium were investigated by the Bureau of Mines. Properties studied included as-cast and annealed hardness, microstructure, fabricability at room temperature and elevated temperature, tensile strength, electrical resistivity, and oxidation resistance at 625° and 800° 2. Additions of small amounts of hafnium resulted in lessened as-cast hardness, decreased electrical resistivity, impaired roll- ability, increased oxidation resistance, and greater tensile strength. Larger amount of hafnium caused greater as-cast hardness, increased electrical resistivity, further impaired rollability, continued increase in oxidation resistance, and lessened tensile strength. INTRODUCTION The purpose of this study was to determine the effect of hafnium additions on the properties of vanadium and to learn if this binary alloy had any special or unusual properties. This investigation is a part of a larger research project in which new and expanded uses of vanadium are being sought. Domes tic vanadium is found frequently in combination with uranium, and because of the demand for uranium as a nuclear fuel, there now exists a surplus of vanadium-bearing minerals and vanadium pentoxide as a byproduct of uranium production. Primary principles of conservation demand that greater use be made of this readily available surplus; finding suitable metals to alloy with vanadium to enhance its properties is one way to increase its utilization. This report is the result of an investigation of the effects on the properties of vanadium when hafnium is added in amounts from 1 to 50 a/o.

Jan 1, 1962

By Robert S. Warfield

The Federal Bureau of mines and U.S. Geological Survey conducted exploratory investigations and geologic mapping in the Wishbone Hill district of the Matanuska coalfield almost continuously from 1942 through 1958. These investigations delineated reserves of high-volatile bituminous coal necessary to supply the rapidly expanding military and civilian requirements in the Anchorage area. This report describes the program conducted by the Bureau of Mines from 1949 through 1958, and briefly summarizes previous investigations, the results of which have already been published. The coal-bearing structure on both the north and south limbs of the prominent Wishbone Hill syncline was explored by 8,719 feet of churn drilling and 25,460 feet of diamond-core drilling. A total of 33 holes were drilled ranging in depth from 60 to 2,114 feet. To supplement the drilling operations, bulldozer and dragline trenching were undertaken at key locations; about 25,000 cubic yards of dragline trench were excavated in the vicinity of the old Premier mine.

Jan 1, 1962

By V. F. Swanson

As part of the Bureau of Mines titanium resources examination program, samples of altered rock (saprolite) and unaltered rock from the Roseland anorthosite near Roseland, Nelson County, Va., were tested for amenability to beneficiation by flotation. A flotation technique was developed to produce bulk concentrates of ilmenite, rutile, sphene, and leucoxene. It was necessary to first float apatite using oleic acid as the collector, in an alkaline pulp with dextrine as a titanium mineral depressant. The titanium minerals could then be floated from the apatite tailing, using fluosilicic acid to depress the remaining apatite, morin to depress ferromagnesian minerals (when present), and oleic acid as the collector. A bulk titanium mineral concentrate, analyzing 66.0 percent Ti02 and 0.08 percent P205, was obtained from a sample of the unaltered rock which contained 5.45 percent TiO2 and 2.81 percent P205. Overall recovery in the concentrate was 47.1 percent of the total TiO2 in the ore. About 55 to 65 percent of the saprolite sample was clay and was removed by attrition scrubbing and decantation. The apatite prefloat procedure was applied to the saprolite sands; subsequent titanium mine: 1 flotation recovered 72.2 percent of the Ti02 in a bulk concentrate containing 65.1 percent TiO2 and 0.20 percent P205.

Jan 1, 1962

By E. G. King

An earlier Bureau of Mines report4 provided low-temperature heat-capacity and entropy data for three sodium vanadates. This report continues the study of vanadates by presenting analogous data for three crystalline calcium vanadates - calcium metavanadate (CaV206), calcium pyrovanadate (Ca2V2O7), and calcium orthovanadate (Ca3V208). No similar data for these compounds have been published previously. MATERIALS All three vanadate samples were prepared by the Bureau of Mines by heating stoichiometric mixtures of reagent-grade calcium carbonate and vanadium pentoxide.5 Calcium metavanadate was prepared at 610° to 660° C. A stoichiometric mixture was heated for 17 days with intervening grindings, mixings, and adjustments of composition, as shown necessary by chemical analysis. The final analysis gave calcium oxide, 23.48 pct. (theoretical, 23.57 pct.) and vanadium pentoxide, 76.32 pct. (theoretical, 76.43 pct.). The sample also contained 0.11 pct. acid-insoluble matter. The X-ray diffracton pattern showed no lines of free calcium or vanadium oxides. No X-ray diffraction patterns were found in the literature for any of these substances.

Jan 1, 1961

By W. T. Benson

The Bureau of Mines has examined selected deposits of titanium minerals throughout the United States. The titaniferous magnetite deposits in the western San Gabriel Mountains, Los Angeles County, Calif., were among those selected for study, and in 1956-58 field work was conducted to determine the extent and character of the titaniferous magnetite deposits occurring in the area. This report describes this work and summarizes earlier work in the area by the Bureau and others. The titaniferous magnetite occurs disseminated as seams and lenticular pods in an anorthosite belt 4 to 6 miles wide that trends about. N. 80° W., extending from sec. 13, T. 3 N., R. 12 W., to the west boundary of R. 14 W., at which point the titaniferous magnetite-bearing rocks disappear beneath the sediments in the Santa Clara River Valley.

Jan 1, 1962