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By Henry C. Meeves

The nonpegmatitic sources of beryllium in Arizona, Colorado, New Mexico, Utah, and four adjacent states investigated by the Bureau of Mines are described. The investigations included 155 properties from which over 6,200 rock samples were collected; more than 5,500 samples were analyzed by the nuclear beryllium-detection technique. Twenty-four of the properties examined had rock containing more than 0.10 percent BeO. Many of the beryllium determinations were made in the field with portable detection instruments by direct scanning of outcrops and by testing samples of rock brought to the instrument. The large domestic resources of low-grade nonpegmatitic beryllium ore in Utah, which were discovered by private enterprise and which respond favorably to small-scale treatment processes, may come into commercial use and thus reduce the dependence of the United States on imported beryl.

Jan 1, 1966

By Walter Kawa

Coals of various rank were reacted by the Bureau of Nines in plasma jets generated from argon and argon-hydrogen mixtures containing up to 33 volume-percent hydrogen. Average plasma temperatures ranged from about 3,400° to 12,000° C. Products were a solid residue and a gas containing hydrogen, methane, acetylene, diacetylene, and oxides of carbon. The highest yield of acetylene obtained with argon plasmas was 15 percent by weight of moisture- and ash-free coal. The data indicated that acetylene yields of 40 percent or higher can be obtained from the reaction of coal in argon-hydrogen plasmas, although results from these experiments could not be correlated with operating variables because of low recoveries plasma contained sufficient energy to heat the coal to temperatures as high 9,000 or 10,000° C, but complete devolatilization did not occur in any experiment.

Jan 1, 1966

By S. E. Khalafallo

The Bureau of Mines investigated the kinetics of reduction of wustite and magnetite with carbon monoxide. A mechanism was postulated wherein the interaction between gaseous and absorbed carbon monoxide appears to be the rate-determining process. This mechanism fully accounts for the experimental rate equation JL.h relates th velocity of reduction to the pressure of the reducing gas at constant temperature. It also explains the variability of the heat of activation of the reduction process with the state of aggregation of the oxide material. The integrated rate equation is in perfect agreement with the experimental reduction-time curves.

Jan 1, 1966

By Jr. Koch

Statistical methods applied at the Bureau of Mines Denver Mining Research Center to data from metallic ore bodies were used to evaluate lignite reserves from core data and to predict the extent of lignite horizons in some Texas lignite beds. Six lignite seam units were studied using data from 361 drill holes. The data indicate a total of 214.2 million tons of lignite in the area examined, and probable reserves of 113 million tons in an area 2,000 feet beyond the limits established by the drill holes. It was demonstrated that lignite reserves present in lenticular beds could be reliably determined by statistical techniques, and that core drilling could be optimized to maximum information with minimum drill holes. The technique described is applicable to other coal beds.

Jan 1, 1966

By Bernard Porter

The densities of LiF, NaF, and KF, of binary mixtures of these alkali fluorides, and of binary mixtures of UF4, ThF4, YF3, LaF3, and CeF with each of tie alkali fluorides were measured as functions of the melt composition and temperature. Molar volumes at 1,000° C were calculated for all the mixtures. Binary systems containing LiF exhibited molar volume ideality. Binary fluoride systems containing either NaF or KF as the alkali fluoride exhibit positive deviations from molar volume additivity. However, molar volumes in the NaF-KF system are ideal.

Jan 1, 1966

By Donald W. Mitchell

Certification tests for urethane-foam systems and techniques for apply-ing foam safely in mines are described. Fire hazard from foam exists if flame propagates beyond the ignition source or penetrates the foam. Foam that passes the certification tests can be applied on stoppings, continuous sections of ribs of relatively wide passageways (with no foam on the roof), short sections of roof such as overcasts, roof cavities, and intersections (with no foam on the ribs), and between buntons on one wall of a shaft. Foam on the ribs and adjoining roof presents a fire hazard. Stoppings covered with foam passing the certification tests are resistant to penetration of heat, flame, and smoke than similar stopping without foam. Flame propagation can be arrested by water sprays. Spontaneous ignition of foam can be prevented.

Jan 1, 1966

By James Paone

The Bureau of Mines studied the behavior of rocks at the initial state of crater formation that results from the stresses created under a drill bit to determine which mechanical properties of rock are important in rock fragmentation by drilling. Although a definite relation between the drilling strength and relevant mechanical properties has not been established, maximum yield strength of rock is apparently a parameter of drillability of rock. The strengths of rock were considered from the Mohr-Coulomb criterion from which the surface of failure was constructed. The results from previous tri-axial tests on Solenhofen limestone were adopted to verify the criterion of failure. Inelastic behavior of some rock types was observed under a low-velocity impact of a hemispherical bit and under static indentation with a similar bit. Quantitative determinations of strengths of Solenhofen limestone) Indiana limestone, and Tennessee marble were made under static indentation. The maximum yield strength estimated from the average stress over the indented area was used as the crushing strength of rock under a drill bit.

Jan 1, 1966

By Jr. Karr

The Bureau of Mines studied the influence of carbonization method, temperature, and carrier gas on the composition of eight different low-temperature tars produced from a Colorado subbituminous coal. A fluidized bed was compared with an entrained bed, temperature was varied from 500° C to 650° C, and external heating using recycle gas as the carrier gas was compared with internal heating using oxygen-containing gas. The entrained bed yielded significantly more m-cresol and m-ethylphenol, indicating that thermodynamic equilibrium was more nearly approached in the system. Increasing the temperature greatly increased the yield of benzenes and naphthalenes, while paraffins, olefins, and total tar acids were reduced. Using oxygen in the carrier gas decreased the yield of low-boiling phenols and increased that of paraffins and olefins at 650° C.

Jan 1, 1966

By R. O. Dannenberg

This Bureau of Mines report describes the results of research to develop a process for recovering additional beryllium from a commercial mill waste product, fluoferrate leach residue. Forty-five percent of the total beryllium in the leach residue was recovered in a beryllia product assaying over 98 pct Be0 by a process comprising (1) leaching with 1 N sulfuric acid, (2) adjusting the acidity of the leach liquor to pH 2, (3) extracting the beryllium with di-2-ethylhexyl phosphoric acid (EHPA), (4) stripping the loaded extract with sodium hydroxide solution, (5) boiling the sodium beryllate strip solution to precipitate beryllium hydroxide, and (6) calcining the beryllium hydroxide. Calculated reagent requirements per pound of Be° recovered by a proposed flowsheet were 28.1 lb sulfuric acid, 0.04 lb flocculent, 0.15 lb EHPA, 0.06 lb isodecanol (IDA), 0.22 gal kerosine, and 6.3 lb sodium hydroxide.

Jan 1, 1966

By Lars Osen

The Bureau of Mines investigated (1) the effect of torsion on yield and ultimate strengths of bolts when the torsion is applied first and tensile load is applied independently of torsion and (2) various methods of increasing the tension-torque ratio and/or narrowing the data spread of the tension-torque relationship. A special torsional attachment was fabricated to attach to a universal testing machine to independently subject rock bolts to combined tensile and torsional loads. It was found that initially installed torsion is nullified during tensile loading and the tensile yield and ultimate strengths are not significantly reduced. Lubricating various components of a bolt assembly or using hardened washers will improve the tension-torque relationship during conventional installation; however, the torsional load is not nullified during this type of loading. Hence, a bolt is subjected to a combined stress throughout the loading cycle; the yield point will thus be lowered compared with the pure tensile yield if care is not taken during installation to stay below the torsional yield.

Jan 1, 1966

By Harry R. Nicholls

Preliminary tests on presplitting rock in the presence of an in situ static stress field were undertaken to study the influence of a horizontal static stress field on the creation of a vertical presplit fracture plane. These tests indicated that it is easier to fracture the rock parallel to the in situ maximum compressive stress than in other directions. Instrumented shots indicate that the interaction of stress waves generated by the detonating charges is probably responsible for starting tensile fractures between shotholes and that expanding gases may propagate these initial cracks by a wedging action. The hole spacing for presplitting appears to be equal to the half wavelength of the stress wave. However, wider hole spacing appears feasible if the initial fracture is started by closer hole spacing.

Jan 1, 1966

By M. H. Stanczyk

The Bureau of Mines made bench-scale laboratory tests on a sample of typical Florida phosphate slime to determine alumina and phosphate extractions obtainable by agitation leaching, by baking and curing, and by a leach-electrolysis scheme. Recovery of mineral values from leached slime pulps by resin-in-pulp ion exchange contact and the reaction of the leached pulps to filtration, flocculation, and settling were also investigated. The best extractions of alumina and phosphate were obtained by (l) agitation leaching with sulfuric, hydrochloric, or nitric acid at an elevated temperature or (2) curing or baking the slime with sulfuric acid. Alumina extractions ranged from 80.8 to 90.0 percent and phosphate extractions ranged from 93.3 to 98.4 percent when the slime was leached at 90° C with sulfuric, hydrochloric, or nitric acids. Baking the slime with sulfuric acid at 200° C for 4 hours yielded an alumina extraction of 92.3 percent and a phosphate extraction of 97.0 percent, whereas curing with sulfuric acid at 100° C for 24 hours gave slightly higher alumina and phosphate extractions. Flocculation and settling properties of the slime were virtually unaffected in all cases. Filter area requirements, although somewhat improved as compared to untreated slime, remained relatively high. The lowest filter area requirement obtained was 44 square feet per ton of dry solids treated per day. Contacting leached slime pulps with ion exchange resins depleted the leach pulps of solubilized values; however, the filtration and settling properties of the barren pulps were unaffected. A leach-electrolysis scheme resulted in some concentration of solubilized phosphorus, but the method showed little promise of being commercially feasible.

Jan 1, 1966

By P. E. Churchward

The Bureau of Mines developed a process using amines for recovering tungsten as ammonium paratungstate from alkaline leach liquors without producing synthetic scheelite as an intermediate product. Over 90 pct of the tungsten in low-grade scheelite or ferberite concen-trate was recovered as ammonium paratungstate by (l) autoclave leaching the concentrate with Na2CO3, (2) solvent extraction of the acidified leach liquor with kerosine solutions of either a quaternary amine (Aliquat 336) or a primary amine (Primene JM-T), (3) stripping the tungsten values from the quaternary amine with ammoniacal NH4C1 or from the primary amine with NH4OH, and (4) crystallization of ammonium paratungstate from the strip liquor. Reagent consumption in pounds per pound of W03 recovered was, for the quater¬nary amine, 3 Na2CO3, 3.5 H2SO4 , 2.2 NH4Cl, 1 NH3, and 0.4 glacial acetic acid; for the primary amine, it was 3 Na2CO3, 3.5 H2SO4, .06 NH4Cl, and 0.9 NH3. Both reagents extract molybdenum along with tungsten. Silicate and phosphate are partly extracted and contaminate the product; leach liquors containing these impurities require preliminary purification.

Jan 1, 1966

By H. M. Smith

Data from the Bureau of Mines routine method for the analysis of crude petroleum are used to characterize crude oils. Some data are used directly while other data are used to calculate the aromatic) naphthene) and paraffin contents of the distillation fractions and the correlation index of the paraffin-naphthene portion of the fractions. The calculated properties show significant differences in composition between crude oils. The methods of calculation and interpretation of data are explained and illustrated.

Jan 1, 1966

By C. L. Klingman

The Bureau of Mines tested eight commercially available, activated charcoals experimentally to compare the following characteristics: capacity for adsorption of nitrogen at 77° K and 170 atmospheres' pressure, surface area, carbon tetrachloride adsorption capacity, hardness, and density. The nitrogen adsorption test was devised to simulate plant conditions occurring in the final step of purification in Bureau helium faciliti.es. The remaining tests were patterned after empirical acceptance tests that are widely used throughout the adsorbent industry. Surface area and carbon tetrachloride adsorption correlated well with nitrogen adsorption. The samples with low density generally had better adsorption qualities than those of higher density. The carbon tetrachloride test appeared to be the most practical for selecting a charcoal to be purchased, but an attrition, or hardness test should also be run to be sure the charcoal will not crumble in use.

Jan 1, 1966

By L. C. Marchont

This Bureau of Mines report tabulates data on nitrogen-gas reservoirs and isolated occurrences of inert gases in several Williston basin oilfields. Recoverable reserves of nitrogen gas in the Minnelusa nitrogen interval within the areas of five oilfields on the Nesson anticline in North Dakota are estimated at about 1.27 trillion standard cubic feet, based on computer analyses of logs from over 300 wells. This volume of nitrogen represents a large source of high-pressure inert gas and warrants consideration of possible application in oil-production operations. Drill-stem tests made in two of the fields indicated that nitrogen can be produced at rates up to 28 million cubic feet per day.

Jan 1, 1966

By Stephen D. Hill

The Bureau of Mines devised and constructed a modified Knudsen effusion apparatus, permitting a constant measure of the weight of effusing vapor, to determine the equilibrium vapor pressure of metal halides at temperatures up to 1,200° K and over the pressure range 10-5 to 10-2 torr. The reliability of the apparatus was established by determining the vapor pressure of potassium chloride. After correcting for partial dimerization of the vapor, data obtained on solid KCl between 750° and 950° K can be expressed by the following equation:

Jan 1, 1966

By R. E. Cumings

The Bureau of Mines made electrorefining tests in inert-atmosphere, molten salt cells to develop methods for the preparation of high-purity molybdenum. Seven of the electrolytes investigated were suitable for the preparation of refined metal. The electrolytes were composed of molybdenum chloride in alkali chlorides or mixtures of alkali and alkaline-earth chlorides. An electrolyte composed of potassium chloride and potassium hexachloro-molybdate was selected for a larger scale, more detailed study on the basis of its ease of preparation, its ability to retain the molybdenum salt, and the type of deposits obtained. High-purity molybdenum in the 99.99-percent-purity range was successfully prepared as dense plate up to 80 mils thick and as dendritic crystals. The temperature of electrolysis and the current density were major factors in determining whether plate or dendritic crystals of molybdenum were obtained.

Jan 1, 1966

By Jr. Norman

The Bureau of Mines investigated the thermoelectric properties of yttrium selenides and tellurides from room temperature to 900° C. X-ray crystallographic data were determined for the yttrium-selenium and yttrium-tellurium compounds that were orthorhombic with a cubic substructure. The yttrium selenides and tellurides exhibited semimetallic to insulator conduction properties with figures of merit of 10-9 to 10-4 °C-1. The mono-selenide and monotelluride behavior was partially degenerate; unsatisfied bonds were the source of the large number of charge carriers. The higher stoichiometry selenide compounds were intrinsic semiconductors) but with high electrical resistivities. A critical defect or impurity ionization energy for carrier activation appeared to exist in the majority of telluride compounds. Mobility and energy band determinations are required to interpret completely the observed effects in most of the compounds studied.

Jan 1, 1966

By J. G. Donaldson

Binary alloys of molybdenum and tungsten were prepared by the Bureau of Mines in laboratory-scale experiments by hydrogen reduction of their vaporized hexafluorides. Near-optimum deposition parameters were determined, and the nature of the deposited alloys was investigated. Dense, homogeneous alloys were codeposited between 650° and 750° C with a reduction efficiency of more than 75 percent. The alloy composition was uniform when the hydrogen ratio in the gas feed mixture did not exceed 3 times the stoichiometric requirement. Regulating the proportions of the metal hexafluorides in the gas feed provided a large degree of control over the composition of the deposit. Hardness of the deposits varied directly with the proportion of excess hydro,,,, in the gas feed and with the weight-percent of tungsten in the alloy. Hardness was not affected by deposition temperature over the range 650° to 750° C for specimens of similar composition. Extreme brittleness and unsuitable physical shapes of the alloys prevented tensile strength measurements.

Jan 1, 1966