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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 Elton L. Litchfield

The techniques for direct initiation of detonation, developed by the Bureau of Mines, have been applied to gaseous mixtures of oxygen with methane, 'thane, propane, butane, or hexane. An exploding wire was used as the initiation source to determine minimum stored electrical energies required to effect detonation of mixtures between one-half and two times the stoichiometric fuel ratios. Detonations were obtained in the most easily initiated mixtures of ethane, propane, butane, and hexane for initiation energies between 24 and 33 joules at 1 atm and 28-43 joules at 0.5 atm initial pressure. Methane mixtures, at 1 atm, were not observed to detonate when initiated with up to 484 joules.

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 R. E. Stiles

The modified perchloric--EDTA method devised by the Bureau of Mines for the determination of copper in high-grade samples gives results that are more precise and more accurate than those from the classical sulfuric-iodometric method. Although the perchloric--EDTA method is more costly than the conventional method, the savings in time alone largely offsets this difference. Specifically, the modifications wade in the more conventional procedure comprise (1) use of perchloric acid instead of sulfuric acid for dissolution of copper minerals, (2) precipitation of copper as copper sulfide from dilute perchloric acid solution, (3) wet oxidation and dissolution of the precipitated copper sulfide, (4) use of larger amounts of indicator than those employed in the Schwarzenbach method of titrating low-tenor copper solutions with disodium ethylenedinitri10-tetraacetate and murexide indicator, and (5) use of refrigeration to partially stabilize aqueous solutions of the indicator.

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

By R. F. Kendall

Only a limited number of mass and infrared reference spectra of high purity unsaturated hydrocarbons and oxygenates are presently available in the literature. To aid Bureau of Mines research programs requiring such references, 64 mass spectra and 70 infrared spectra were obtained and are reported. The individual compounds, acquired from commercial sources, were purified by preparatory gas chromatography. Purity determinations were made using a combination of analytical gas chromatography, microhydrogenation, and catalytic deoxygenation. These spectra will aid spectroscopists in the identification of compounds of the types reported.

Jan 1, 1966

By J. V. Batty

The Bureau of Mines devised techniques involving the use of beta-and gamma-ray-emitting radioisotopes and successfully adapted these techniques to the density of mineralized flotation froths) the rate of flow of finely ground ore pulps) and the residence time of pulps in processing circuits. Specifically, the water and mineral loads of flotation froths were continuously measured by determining the proportion of a constant-strength beam of beta rays that was absorbed by the froth column. Continuous measurement of the rate of flow of an ore pulp was accomplished by measuring the changing width of a free-falling stream of the pulp with a collimated beam of beta rays. The residence time of solids in conditioning and resin-in-pulp circuits was accurately measured by following the progress through these circuits of a portion of the pulp that had been tagged with the gamma-emitting Ag110 radioisotope.

Jan 1, 1966

By N. H. Coates

The Bureau of Mines determined average film coefficients of heat transfer for helium flowing through smooth, water-cooled tubes at Reynolds numbers of 5,000 to 25,000, helium inlet temperatures of 1,600° to 2,600° F, average temperature difference across the helium film of 800° to 1,300° F, and heat flux to 215,000 Btu/(hr)(sq ft). Since helium was the only gas used, the ranges of values for physical properties of the fluid are limited--thermal conductivity from 0.15 to 0.20 Btu/(hr)(sq ft)(O F/ft), viscosity from 0.082 to 0.104 lb/(ft)(hr), and Prandtl number from 0.63 to 0.68. Four equations, three of them dimensionless, correlate these coefficients with other properties of the helium--bulk temperature, film temperature, dimensionless parameters based on temperature, and the ratio of wall temperature to bulk temperature.

Jan 1, 1966

By J. M. Kuchta

The Bureau of Mines used laminar hot air jets of l/8- to 3/4-inch diam-eter to determine the hot gas ignition temperatures of various combustible vapor-air mixtures. The combustibles were n-hexane, n-octane, n-decane, a hydrocarbon jet fuel (JP-6), and an adipate ester aircraft engine oil (MIL-L- 7808). Minimum ignition temperatures occurred at a fuel to air weight ratio of about 0.5 and were not greatly sensitive to variations of fuel concentra¬tion. Moderate variations of jet velocity also had little influence on these ignition temperatures. However, these temperatures decreased with increase in heat source dimensions (jet diameter). The hot gas ignition temperatures of the combustibles were not necessarily much greater than corresponding autoignition and wire ignition temperatures when the size (,F the heat source and the ignition criterion were the same.

Jan 1, 1966

By J. E. Zeilinger

The technical feasibility of using energy from explosive ignitions of coal dust to pump water was .demonstrated in an exploratory investigation. Ignition of small amounts of pulverized coal that were dispersed in air over columns of water pumped up to 5.3 gallons of water per cycle when operated against a head of 30.75 feet. Water displacement was accomplished by either manual or automatic operation through a single cycle, and by automatic operation through a continuous series of cycles of I-minute duration. Operating through single cycles, slurries containing up to 3 pounds of coal and 4.6 gallons of water were also pumped. Possible uses of an efficient coal-fired pump would include pumping water for irrigation purposes, removing water from mines, transporting coal from mines in the form of a slurry, and pumping water to elevated reservoirs at electric powerplants so that it could be used to generate electricity during peak periods of demand.

Jan 1, 1966