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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 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 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

By Verne E. Hooker

The Bureau of Mines conducted a preliminary investigation to determine the state of stress in crystalline rock outcrops near Atlanta, Ga. The secondary principal stresses in a horizontal plane near the surface are compressive and are 500 to 3,000 psi. The maximum compressive stress is northeast-southwest in the Stone Mountain-Lithonia district but changes to northwest-southeast near Douglasville. The elastic constants were determined from data obtained by static and dynamic laboratory methods and in situ velocity measurements. Results show Young's modulus to be dependent upon both stress level and anisotropy in the rock. Average secant moduli obtained from triaxial tests were used to compute the applied stress from borehole deformation measurements.

Jan 1, 1966

By L. B. Pankratzt

The heat capacity of dimo1ybdenum carbide (Mo2C) was measured from 51° to 298° K, and the entropy at 298.15° K was evaluated. Heat content measurements above 298.15° It were conducted for dimolybdenum carbide (M0caY) and monotantalum carbide (TaC). The results were combined with known heats of formation and the 298.15° K entropy for TaC to obtain values of the heat and free energy of formation from 298.15° K to 1,400° K for MoaC and from 298.15°K to 1,800° K for TaC.

Jan 1, 1966

By L. B. Pankratzt

The heat content above 298.15° K of ferroelectric lithium columbate (LiCbO3) was measured to 1,770° K. The Curie temperature was determined to be 1,450° K, the melting point 1,540° K, and the heat of fusion 16.94 kcal/mole. Heat content and entropy increments have been tabulated for the temperature range from i98.15° to 1,800° K. Heat contents are also given in equation form.

Jan 1, 1966

By Jerry W. Ramsey

The Bureau of Mines studied two Pennsylvania anthracites using low-temperature carbon dioxide adsorption. A modified form of the Brunauer-Emmett-Teller equation was used to calculate specific surface areas. Two mesh sizes of each anthracite were used to determine how gamma irradiation at 106 and 108 rads, both in vacuum and in the presence of air, affected the carbon dioxide surface areas. Results show that anthracites have a system of pores that are essentially all interconnected rather than isolated; that anthracites differ from one another in specific surface, which may correlate with density; and that irradiation in vacuum has no discernible effect on specific surface of anthracite, but irradiation in air does produce changes in specific surface.

Jan 1, 1966

By E. J. Kloos

The Bureau of Mines devised a new machine-test method for measuring carbon dioxide inspired by a wearer of self-contained breathing apparatus. The new method compares favorably in speed and precision with standard man-tests in which the apparatus is tested while actually worn, and is scheduled for use in future approval tests for facepiece carbon dioxide 'measurements. However, man-tests will still be used to measure the efficiency of the carbon dioxide sorbent materials in closed-circuit breathing apparatus.

Jan 1, 1966

By R. L. Crosby

Microscopical and X-ray diffraction techniques were used to identify two intermediate phases in that part of the solid region of the magnesium-cerium system between and Mg3Ce. Previous literature had reported only one intermediate phase for this region, 1)12t chemical analysis determined the approximate composition of the two compounds to be Mg23Ce2 and Mg17Ce2. The range in composition of the two intermediate phases was found to be limited to less than 0.3 atomic percent cerium. The study did not determine the crystal structure of Mg17Ce2, but that of Mg23Ce2 is tetragonal with a = 10.33 A and c = 19.51 A.

Jan 1, 1966

By Jr. Hazen

Relationships that may exist between assays and sample interval lengths when using unequal sample intervals in mine sampling have been investigated as part of the larger research problem of adapting statistical methods to the analysis of weighted average grades. The theoretical relationship between the amount of difference in the weighted and unweighted average grade of ore and the size of the correlation coefficient between assay value and sample interval length was found to be linear. Numerous examples of actual field sample and assay data, which have been obtained by using unequal sample intervals, are documented, and the differences between weighted and unweighted average grades of ore and the correlation coefficients between assays and sample interval lengths have been computed and plotted on graphs. Differences between these actual field data and the expected theoretical linear relationship are examined. It is hypothesized that the use of unequal sample intervals in mine sampling is, in fact, stratified sampling in a statistical context. The sampler establishes stratification by selecting unequal sample intervals on the basis of differences in lithology, changes in rock type, characteristics of mineralization, or differences in metal content. Statistically} methods currently used in mine sampling, involving unequal sample intervals, fail to consider differences in the inherent variances in grade of ore within the various strata established by using unequal sample intervals. Consequently the strata are sampled with different precision. This difference in precision of sampling between strata may account for much of the deviation between the plotted points representing actual field sampling data and the theoretical linear relationship between the amount of the difference between weighted and unweighted average grade of ore and the size of correlation coefficient between assays and sample interval lengths.

Jan 1, 1966