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By Robert M. Becker

Part 5, the last of this series, deals with the theoretical confirmation and application of results developed in parts 1 and 2. The bulk-sampling variances of Hassialis and Kassel and Guy are compared with those in part 2, both as to formulation and as applied to ores and coal. The results provide confirmation for much of the development in part 2. Examples are presented for determining the reliability of bulk samples with respect to various measurable characteristics. These characteristics include, for example, assays for elements or compounds and particle surface area. The bulk samples considered consist either of a given weight, a given volume, or a given number of particles. In addition to problems of sample reliability, some of these examples may also be applicable to quality control. Several possible applications of results developed in parts 1 and 2 are outlined. These include tests for random data, degree-of-mixing indices, and particle-fineness indices.

Jan 1, 1966

By R. L. Benner

A compound stability diagram was constructed by the Bureau of Mines for the Zn-Fe-S-O system to show the phases that should be thermodynamically stable at various temperatures, oxygen pressures, and SO2 pressures. The diagram was demonstrated to have good qualitative value for predicting stable phases that may, in turn, be related to the recovery of zinc in the leaching phase of the electrolytic zinc process. The study showed that roasting temperature is the most Significant variable in preventing roaster formation of zinc ferrite, which is directly related to subsequent extraction of zinc in the leaching step.

Jan 1, 1966

By Lippe D. Sadwin

A high-speed streak camera method for making equation of state measurements (shock and particle velocities) on samples of rock under dynamic load conditions is described. Experimental data are given for tests on 12 samples representing 5 rock types. Analysis of these data shows that the method is practical and that good reproducibility of results can be obtained. The pressure range covered in the tests was from 1 to 50 kilobars.

Jan 1, 1966

By F. E. Griffith

Cost data are given for five methods of secondary backfilling of strip mines previously partially backfilled. The operations were conducted in north-central Pennsylvania; an average of 600 linear feet of highwall were backfilled in each trial. Major obstacles and the relative merits of the methods are discussed.

Jan 1, 1966

By R. W. Van Dolah

An attempt has been made in this investigation to define the conditions under which ammonium nitrate (AN) might detonate as a result of involvement in fire. The initiation of detonation by shocks derived from explosives or from projectile impact was investigated as a function of temperature and charge diameter. A new technique was devised to investigate the burning of raw and contaminated AN under pressure. No transition, to detonation in AN was obtained in the burning experiments. The critical diameter for detonation of fertilizer-grade AN was found to be quite small when the AN was at temperatures just below melting point; this indicates that initiation of detonation may be less difficult at elevated temperatures but such initiation by gas-phase detonation was shown to be unlikely. Transition from burning to detonation was obtained with AN intimately mixed with fuels that included polyethyl-ene, paper, and fuel oil when these were contained in vessels with restricted vents. However, the experimental results supported by an analytical study indicate that the initiation of detonation in AN from fire exposure in normal storage and from transportation incidents is quite improbable. The detonation of AN in recent incidents more likely may have resulted from the effects of adjacent explosions.

Jan 1, 1966

By James F. Devine

The radial, vertical, and transverse components of particle velocity were recorded by Bureau of Mines investigators along gage arrays extending in one or two directions for 145 to 3,170 feet at five quarries. Of the 39 quarry blasts, 12 were instantaneous blasts, 5 were of the one hole per delay type, using millisecond delayed caps, and 22 were multiple hole per delay type employing millisecond delay detonating fuse connectors. Charge weight per hole ranged from 8 to 1,500 pounds, and the charge weight per delay interval, including the instantaneous blasts, ranged from 25 to 4,620 pounds.

Jan 1, 1966

By P. L. Weston

The Bureau of Mines used high-temperature reduction roasting, magnetic separation, acid-leaching, and autoclave precipitation processes to recover iron and manganese from brown Cuyana range ores of Minnesota. Wet magnetic separation concentrated over 90 percent of the iron in 3 of 4 ores as high grade products analyzing 74 to 85 percent iron, 2.5 to 6 percent manganese, and 3 to 10 percent SiO2. The nonmagnetic fractions were leached with dilute sulfuric acid extracting 83 to 93 percent of the contained manganese and small amounts of iron. The leach solutions contained Mn-to-Fe and Mn-to-SiO2 ratios favorable enough for possible consumption in metallurgical mane operations. Exceptionally pure Mn solutions were achieved by pressure precipitation of the remaining iron in an autoclave followed by lime precipitation of silica and alumina.

Jan 1, 1966

By James Paone

The Bureau of Mines made drillability studies with impregnated diamond bits in the laboratory on 7 rock types and in the field on 21 different rock types. Results indicate that drill parameters of rotational speed, thrust, and torque must produce sufficient applied forces to induce stress levels that cause continuous failure in rock to achieve efficient penetration rates. Higher rotational speeds appear to be more effective in drilling relatively harder rocks, although the increased speed causes more bit wear; increases in thrust result in higher drilling rates but not linearly; and up to a critical value a linear relation exists between torque and penetration rate for a specific rock type. Penetration rates with impregnated bits show a trend similar to that obtained with surface-set bits for rock under 25,000 psi compressive strength.

Jan 1, 1966

By H. R. Babitzke

To develop alloys suitable for use at elevated temperatures, columbium and tantalum were combined with tungsten, hafnium, vanadium, zirconium, and titanium, and the resulting alloys were evaluated with respect to fabricability, hardness, Electrical resistivity, strength at elevated temperatures, oxidation resistance, and bend transition. Of the 23 compositions tested, Cb-2OHf-5W-10Ti exhibited superior high-temperature properties. A recrystallized sample of this alloy was fabricable at room temperature, had a strength of 44,000 psi at 1,200° C, and had an oxidation rate of only 7.7 mg/cm2/hr at 1,000° C.

Jan 1, 1966

By Jr. Hazen

This report documents 653 sets of sample data involving 78,366 assays obtained from past exploration for various minerals and metals. Most of these data have been taken from published reports describing exploration projects, conducted jointly by the Bureau of Mines and the Geological Survey, for the Strategic Minerals Program from 1940 through 1949. Means and standard deviations have been computed for the exploration assay data and have been plotted on graphs for 22 minerals and metals. A mathematical model, based on the binomial distribution, has been developed to explain the configuration of the plots of the exploration means and standard deviations. The two statistics, mean and standard deviation, which describe assay data, have been used for simulating probability models. These probability models then have been combined with the binomial model of the exploration assays and related to the sequential decision process associated with exploration drilling for mineral deposits. These probability regions can be used to form the basis for sequentially predicting the probable range of the average grade of mineral or metal that may be expected as an exploration drilling program is continued after the initial discovery of mineralization has been made.

Jan 1, 1966

By G. W. Weems

The Bureau of Mines combined preconcentrating techniques and mass spectrometry to develop a parts-per-billion general analysis of impurities in helium. The impurities are preconcentrated using a Bureau trace-impurity analyzer; 35-mm Hg pressure of helium is left in the concentration trap to sweep the impurities into the mass spectrometry and provide a 10-mm Hg sample pressure.

Jan 1, 1966

By I. L. Nichols

Volatilization of cesium from pollucite ore was investigated as an initial step in the production of purified cesium metal or cesium salts. High recovery of cesium and rubidium as chloride sublimates was accomplished by 2-hour roasts in a tube furnace using charges containing 1 part ore, 2 parts limestone, and 0.23 part calcium chloride. Recoveries of cesium in the sublimate product were 89.1, 92.9, and 95.2 pct, respectively, using 1,100° C and vacuum, 1,250° C with an air sweep, and 1,250° C without an air sweep. Most of the lithium, sodium, and potassium sublimed with the cesium and rubidium, but virtually none of the calcium, aluminum, and silicon in the charges was volatilized.

Jan 1, 1966

By C. I. Pierce

The Bureau of Mines used an electrolytic tank model to investigate the response of guard electrodes of different dimensions under different simulated reservoir conditions. Sandstone disks from the Berea and Connellsville Formations were used as resistive beds in the model, and agar gel or water was used as conductive beds. In the experiments, bed thickness, hole diameter, mud resistivity, and bed resistivity were varied. The guard electrode is an excellent tool for determining true bed resistivity in the thin-bedded oil reservoirs of the Appalachian area. Vertical resolution and resistivity values are good when there is little or no invasion. Resistivity values are near true bed resistivity in beds thicker than about six hole diameters when the electrode-to-hole-diameter ratio is close to 1. However, low-resistivity muds cause false peaks to appear on the logs near bed boundaries in thick beds, and for resistive beds having a thickness approximately three to five times the hole diameter, apparent resistivities tend to be excessively high when mud resistivity is low.

Jan 1, 1966

By R. Barany

The heats of the glass-crystal transformation of nepheline (Na0.7794K0.2206AlSiO4) and wollastonite (CaSiO3) and the heat of formation of nepheline at 298.15° K were determined by solution calorimetry. For the glass-crystal transformations, the heat values were -9.0 ± 0.3 kcal/mole for nepheline and -8.1 ± 0.2 kcal/mole for wollastonite. The heat of formation of nepheline was -34.8 ± 0.6 kcal/mole from the oxides and -501.0 ± 0.5 kcal/mole from the elements.

Jan 1, 1966

By P. C. Good

Work was done to determine conditions necessary for efficient electrodeposition of aluminum from fused chloride electrolytes. Aluminum was deposited from a molten chloride salt electrolyte over a temperature range of 150° to 750° C. At lower temperatures in a heat-resistant glass cell, aluminum was deposited on stainless steel and on aluminum cathodes. The deposit was recovered in the form of light, feathery dendrites that could not be consolidated. At 750° C, molten aluminum was deposited at cathode current efficiencies as high as 90 to 100 percent on titanium diboride cathodes and in molten aluminum cathodes. Nitride-bonded silicon carbide was the best cell material, although porcelain was also used. The electrolyte consisted of a mixture of sodium and potassium chlorides in 1 to 1 mole ratio, containing aluminum chloride in concentrations ranging from 2 to 30 weight-percent in cells holding up to 1,000 grams of electrolyte. Generally favorable results were attained in studies made at temperatures greater than the melting point of aluminum.

Jan 1, 1966

By J. W. Stevenson

The Bureau of Mines investigated the influence that atmospheric pressure changes exert in a gassy coal mil on a ventilating air current with a system of bleeder entries. During the season when abnormal barometric fluctuations usually occur, recording instruments monitored the air current ventilating an active coal-producing area. It HL he rate of coal production caused a more significant change in methane concentration than did barometric change. The hazard that accompanies methane release due to expansion of the gob gases during atmospheric lows was minimized by the effective bleeder system.

Jan 1, 1966

By Willis Beckering

The Bureau of Mines designed a cell having four variable compartments in series to facilitate analysis of multicomponent mixtures. Use of the cell considerably decreases the time required for differential absorption analyses. A solution of a major component is placed in each compartment, and the light absorbed by each of these components is varied by increasing or decreasing the path length of the appropriate cell. Simple calculations then establish the amount of the component present. In analyzing unknown mixtures, compensation is made for compounds known to be present, and the differential spectrum representing components not accounted for is recorded and analyzed.

Jan 1, 1966

By Albert F. Baker

Techniques were developed and circuitry was assembled for measuring the total and volume resistances to the flow of electric current through solid specimens of anthracite. The two-, three-, and four-terminal test methods demonstrated the extreme sensitivity of resistivity to differences in anthracite characteristics and showed response to changes resulting from variations in structure, temperature, and moisture content.

Jan 1, 1966

By D. G. Kesterkel

Low-melting thoriurnrbase binary alloys or metal solutions were prepared by two different techniques involving the electrolysis of ThO2 dissolved in fluoride melts. Experiments were performed at 950° to 1,250° C using electrolytes containing ThF4 and various alkali and alkaline earth fluorides. In the first method, electroreduction of ThO2 and deposition of thorium on a nickel or iron cathode formed a molten alloy that dripped off and collected on the bottom of the cell, or in a tungsten cup. An electrocodeposition technique was used to prepare thorium-base alloys or solutions containing nickel, iron, chromium, or manganese. Electrolytic reduction of the component metal oxides and simultaneous deposition of the two metals on a tungsten cathode yielded a liquid alloy product. Complementary experiments were performed on the fused fluoride electrowinning of dendritic thorium from Th02 at 1,075° to 1,200° C in which thorium crystals were recovered and arc-melted into buttons. Major contaminants were aluminum, carbon, copper, iron, oxygen, and silicon, totaling 0.2 percent.

Jan 1, 1966

By Rogers F. Davis

The Bureau of Mines developed a new method for the determination of oxides of nitrogen in diesel exhaust gas. The procedure, a modification of the Saltzman method, uses a NO2 absorbent for the diesel exhaust gas; the colorless absorbent becomes purple on contact with N~. When used properly this procedure gives satisfactory results in 2 hours, whereas the standard phenoldisulfonic acid method required approximately 8 hours. The new method is not satisfactory for determination of oxides of nitrogen in the overrich fuel to air ratio range.

Jan 1, 1966