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By A. C. Rice

Investigation of a variety of mines to determine efficiency for rare- earth extraction has resulted in a solvent extraction technique wherein Primene 81-R,4 N-benzylheptadeeylamine (BHDA), and Primene JM-T give favorable extraction from sulfate solutions. Extraction from chloride, nitrate, and perchlorate solutions is negligible. Distribution coefficients for 10 rare-earth elements with Primene 81-R establish an extraction sequence beginning with lanthanum and proceeding through lutetium according to atomic number. Yttrium and ytterbium are exceptions in the extract ion sequence.

Jan 1, 1962

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 C. S. Tout

While investigating methods for determining the best temperatures for hot-working experimental stainless steels, the Bureau of Mines Albany Metallurgy Research Center developed a machine in which hot-twist tests could be made in a few minutes. This machine is similar to some used previously except that specimens are heated by induction instead of by radiation, and their temperature is measured by a calibrated radiation-detection unit instead of by a thermocouple. In. developing the technique for using the new machine, tests were made on specimens of medium-carbon steel, mild steel, and AISI (American Iron and Steel Institute) type 304 stainless steel. Tests also were made on as-cast specimens and preworked specimens of experimental AISI type 202, low austenitic stainless steel, and as-cast specimens of AISI type 301 experimental stainless steel. The optimum hot-working temperatures were determined for all types of steel tested. Also, data were gathered on the effects of test speed and temperature on torsional strength and the effect of twisting on tensile stress in the specimen.

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 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 T. T. Campbell

This investigation was undertaken by the Bureau of Mines to determine if high-purity ductile molybdenum of uniform quality can be prepared by bomb reduction techniques. Molybdenum trioxide (Mo03) and mixtures of molybdenum dioxide (Mo02) and trioxide were reduced by magnesium in closed steel bomb reactors. Very high pressures in excess of 5,000 p.s.i. developed during magnesium reductions of Mo03. The addition of calcium oxide to the bomb charges caused a significant reduction in pressure. Reaction efficiencies higher than 95 percent were obtained during magnesium reductions of either Mo03 or mixtures of Mo02 and Mo03, but high pressures were encountered when the charges contained from 30 to 60 percent Mo02. Reaction efficiencies were usually low (less than 80 percent) when the bomb charges contained more than 40 percent Mo02. The charges with the best composition considering operating pressure, yield, and purity contained from 10 to 30 percent Mo02. The addition of small amounts of carbon to the reaction charges was helpful because some deoxidation occurred during the reduction and also during subsequent arc-melting of the regulus metal. The purity of the bomb-reduced, arc-cast molybdenum metal ranged from 99.2 to 99.8 percent and in some instances the metal contained as little as 5 parts per million oxygen.

Jan 1, 1962

By Gerald V. Gibbs

As a part of the Bureau of Mines long-range program in asbestos, synthetic asbestiform compounds and minerals were prepared and described. Fundamental structural data on two such compounds are given in this report. Crystallographic data are provided for the synthetic isotypic compounds potassium-lead silicate, K2.Pb4 -Si8021 (I), and lead-aluminum silicate, Pb2. Pb4 .Al2Si6O21 (II). The space group symmetry 14/mmm was assigned provisionally to I and II on evidence of single crystal and piezoelectric measurements. A statistical evalua¬tion of indexed powder diffraction data revealed the cell edtes of I to be a 11.816 and c 7.932A and those of II to be a 11.723 and c 8.044A. The phases are uniaxial with observed refractive indices eD 1.790, an ?D,699 and eD 1.884, cusp 1,807, respectively. The atomic structure of I and II may be based on a complex of chains of silicon-oxygen tetrahedra lying along the c cell edge similar to the type of chain structure postulated by Pauling for scapolite. K2.Pb4.Si8021 and Pb2.Pb4 Al2Si6021 were first described by Geller and Bunting (5, 6)4 as fibrous compounds similar in crystal habit to asbestos. These authors gave powder diffraction data, although no attempt was made to find the cell edges or to index the powder diffraction patterns. Later, Shell and others (9) conducted a crystallochemical study of these fibrous silicates in search of a substitute for strategic asbestos. Their single crystal data revealed K2.Pb4 -Si8021 to be tetragonal body-centered with cell edges a 11.66, c 7.95 A. Pb2.Pb4 Al2Si6021 was concluded to be isotypic with K2.Pb4 -Si8021 on the basis of similar powder diffraction patterns, chemistry, and physical properties. No attempt was made, however, to index the powder diffraction record nor to determine the appropriate space group of either compound.

Jan 1, 1962

By C. J. Chindgren

Upgrading of commercial red cake and recovery of vanadium oxide from uranium-vanadium mill solutions were investigated by the Bureau of Mines. Alternative procedures potentially useful for manufacture of high-quality vanadium oxide at the mill site were explored and developed. The simplest and best procedure for converting commercial red cake containing about 10 percent combined sodium and potassium oxides (Na20) (K20) into a 98- to 99-percent vanadium pentoxide (V205 product appeared to be a metathesis in an ammoniacal solution of ammonium sulfate. Molybdenum, as well as the alkali metal oxides, was removed from the red cake by this procedure at a modest expenditure of labor and reagents. When preparing vanadium oxide of higher grade, it was necessary to dissolve the red cake and reprecipitate the vanadium as ammonium metavanadate. Calcination at 450° C, decomposed the metavanadate and yielded oxide of about 99.5 percent V205. By recyrstallizing the metavanadate before decomposition, an oxide product approaching 99.9-percent purity was obtained.

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 D. J. Bauer

A pure scandium solution was concentrated from 10-4 mole per liter to 0.5 mole per liter by continuous foam fractionation in a spaced, packed column. Recovery in the foam was 77 percent using a spaced, packed draining column with sodium n-methyl-n-"coconut oil acid" taurate as the surfactant. The technique was first studied batchwise in a small unpacked column to determine the more important variables. Optimum surfactant concentration was found to depend on scandium concentration. Extraction and, in general, enrichment ratios were highest in the 2.5 to 3.5 pH range at temperatures ranging from 50° to 70° C. An airflow rate of 136 ml./min. was satisfactory in the equipment used.

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 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 Mary F. Koehler

Continuing a program of thermochemical investigation of compounds of to ferroalloy elements, this paper contains ins values of the heats of formation of two sodium molybdates (Na2Mo04 and Na2Mo207) and three sodium tungstates (NO2W4, Na2W207, and NA2W207, and Na2W4013). The experimental method was solution calorimetry. The solution medium was sodium hydroxide solution, except that hydrofluoric acid solution was used for sodium tetratungstate. The heat of formation values are given with reference both to the constit¬uent elements and to the constituent oxides. These data are of prime impor¬tance in the thermodynamic consideration of these substances, as their accumulation includes the most difficult and time-consuming steps toward evaluating the free energies of formation and thus the potential reactivities and thermal stabilities. Except for values for sodium monomolybdate and monotungstate, no previous similar data were contained in literature sources.

Jan 1, 1962

By A. R. Taylor

This report describes the design, construction, and operation of a low temperature adiabatic calorimeter for measuring heat capacities of solids or liquids from 60° to 300° K. A brief discussion of the basic theory involved in chemical thermodynamics and the problems involved in obtaining accurate experimental data is presented. The operation of the calorimeter was tested by measuring the heat capacity of a sample of benzoic acid obtained from the National Bureau of Standards over a temperature range of 60° to 300° K. The measured heat capacity values of the benzoic acid compared favorably with similar values obtained by the Bureau of Standards, the maximum deviation being 0.5 percent. THEORY A brief discussion of the basic theory involved in chemical thermodynamics will illustrate the applications of heat capacity data and the problems involved in obtaining accurate experimental data.

Jan 1, 1962

By R. Lincoln

A surplus of vanadium has resulted from the tremendous output of uranium, of which vanadium is a byproduct. More knowledge of the properties and characteristics of vanadium as a pure metal has been needed so that industry can take advantage of its availability and use it according to the best principles of conservation. Besides the problem of utilization, there is the ever present need of finding new materials which will satisfy specific and demanding requirements of science and engineering; vanadium or one of its alloys may possess the latent potential for filling some of these needs. Thus this? research project was undertaken by the Bureau of Mines to determine and examine some of the physical and mechanical properties of pure vanadium. A corallary investigation was the determination of the effect of the interstitial contaminants, oxygen, nitrogen, and carbon, on unalloyed vanadium. The vanadium used for these determinations was principally the product of experimental production of the Bureau. The evaluation of this material, as small quantities became available, provided most of the data that have been obtained.

Jan 1, 1962

By R. S. Warfield

Following World War II, the rapid increase in both military and civilian activity in the area served by the Alaska Railroad stimulated interest in the availability of local sources of nonmetallic minerals that might be used for building materials. Except for abundant sand and gravel and some pumice, the construction industry of the area depended entirely on high-cost imports for building materials of mineral origin. Because continued rapid growth was anticipated, development and use of local sources of such materials was advocated by both military and civil authorities to reduce the high costs of con¬struction and bolster the unstable economy of the area. The U.S. Department of the Interior began a program On included examining the numerous deposits of nonmetallic minerals accessible to the Alaska Railroad to determine their possible use as raw materials for the construction industry. Preliminary field investigations were made by the Geological Survey. The more promising deposits were subsequently examined and sampled by Bureau of Mines engineers, and the samples were subjected to the laboratory tests necessary to indicate the chemical and physical characteristics of the raw materials or their products. Such field and laboratory investigations were conducted on clay, shale, argillite, limestone, gypsum, and pumice taken from various parts of the area. In initial phasees of the work, done irate 1948 through 1952, many of the deposits examined were suitable for proctoring building materials. Results of the work completed during that period have been published in a Bureau of Mines report3 giving general information and detailed data on more than 35 deposits that were investigated.

Jan 1, 1962

By Philip E. Niebuhr

A procedure, which can be performed in the field by nonanalytical personnel, is given for sensitive spot tests for detecting tellurium or selenium. The expressed need of a field test for detecting small amounts of tellurium, which may be accompanied by relatively large amounts of selenium, has led to the development of this method. Tellurium search has been impeded by the lack of a satisfactory test from the standpoint of sensitivity and specificity. A quantitative laboratory method exists, but it is expensive and relatively laborious. Several other qualitative tests are known, but they require unstable solutions, which must be freshly prepared for use, and a greater variety of laboratory equipment. The particular advantages of the test described are its simplicity and the stability of the reagents required, there-fore is is well adapted for field use. Also, this test was found to be of practical use in the analytical laboratory when screening samples, thereby reducing analytical costs. The roughly quantitative interpretation of the results can save time by indicating the approximate size of the sample taken for a quantitative determination.

Jan 1, 1962

By M. R. Geer

All the coal lands in Alaska are publicly owned, and the Federal Government is the principal consumer of coal. Therefore the Government has long been concerned with the wise utilization of the coal reserves of Alaska as well as with the availability of coals meeting the specifications for use in various Government installations. Coal preparation plays a key role in both of these areas of interest. The proper choice and operation of coal-washing equipment permits the mining of inferior deposits, minimizes waste of coal in preparation, and assures a prepared product of the best quality obtainable from the raw coal. Thus, from time to time, the Bureau of Mines has made washability examinations on most of the coals mined in Alaska. Generally, these examinations were made when new mines or new beds were opened, when construction of new preparation plants was being considered, or when the operation of existing plants could be improved by better knowledge of the raw coal. The purpose of this report is to bring together all the washability data available on the coals of the Matanuska Valley and Beluga River fields. The pattern of energy development for the rapidly growing Anchorage area is not clear at this time. Formerly coal was the only fuel available for large-scale space heating and power generation. More recently both oil and natural gas have entered the market, and several hydroelectric projects have been completed. Additional major hydroelectric projects are being considered. The role that will be played by coal in this competitive energy market is uncertain. However I if coal is the fuel used in future power plants or industrial installations, the information contained in this report will be useful in indicating the quality of the coals that can be supplied and in selecting proper preparation techniques.

Jan 1, 1962