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By R. J. Heemstra

A method was developed for calibrating photographic emulsions and retrieving working curves for emission spectrography. The values obtained from a digital readout or a recorder chart of a comparator-microphotometer are converted to light intensity values using an emulsion characteristic curve derived from a quartic polynomial preliminary curve. The characteristic curve, consisting of Seidel transform versus the logarithm of intensity, is split into two cubic polynomials at the zero value of the transform, resulting in eight emulsion calibration coefficients. These methods allow use of the calibration curves even at very small and very high intensities, thus extending the range of analysis. Use of a small computer allows rapid calculations. A computer program was written to formulate, code, and file each working curve along with its statistical error. Proper coding of the input data permits the direct printout of the concentration of the elements under investigation.

Jan 1, 1970

By D. S. Burgess

An investigation of the hazard of spillage of liquefied natural gas (LNG) onto water is described. About 2,000 gallons of LNG were consumed in various tests. The initial vaporization rate of LNG following spillage was found to be 0.037 lb/ft2 sec; when the spill was confined, this vaporization rate was moderated after about 20 seconds by the growth of an ice layer on the water surface; when the spill was unconfined, a coherent ice floe was not observed and the vaporization rate was essentially time independent. The maximum diameter (in feet) of the spreading LNG pool was found to be given by 6.25 Wo 1/3, where Wo is the weight of LNG in pounds, Downwind of a natural gas source, time-averaged methane concentrations were given in good approximation by standard air pollution equations. However, peak concentrations were as much as twentyfold higher than average, adding an additional factor to the assessment of hazard. The effect of layering by the cold vaporized natural gas was similar to the effect of a temperature inversion on normal gases in the atmosphere. Small-scale explosions were observed on pouring LNG onto a water surface; no single explanation seems pertinent to all of the incidents observed.

Jan 1, 1970

By Frank G. Horino

This report presents a method of utilizing the Coulomb strength criteria for estimating the strength and stability of pillars and pit slopes containing planes of weakness. It is assumed that the Coulomb theory, as a special case of the Mohr envelope, is a satisfactory first approximation of failure in uniaxial compression or triaxial loading with low lateral loads. Accepting this assumption for brittle materials, an expression for the strength decrease of rock pillars containing a plane of weakness or fracture at any angle of orientation is derived. As few as six samples (three solid cores and three fractured cores at a failure-oriented angle) are required for testing uniaxially and triaxially to statistically determine the coefficients of friction and the shear strengths of both the solid rock and the fracture plane and the range of failure angles of the fracture plane. Interpretation of the data shows that the mean normal stress and maximum shear stress technique of analyzing the data is superior for solid core and that shear and normal stress values using angles of failure should be used for fractured specimens with failure-oriented angles. Plots of either the strength or strength ratios against fracture angles obtained from oriented drill core samples give a useful first approximation of strength decrease due to fracture. Using the same test conditions for both fractured and unfractured material increases the validity of the tests.

Jan 1, 1970

By Mary H. Brown

The heats of formation of oxalic acid and sodium, potassium oxalates, and lithium oxalates were related by solution calorimetry to the heat of formation of (COOH)2.2H20, a value believed to be reliable as reported in the literature. The following heats of formation were determined: (COOH)2(a), -198.1±0.1; (COOH)2(ß), -197.8±0.1; UAW,, -328.7±0.4; Na2C204 -316.2±0.1; K2C204, -321.9±0.2; and K2C204-H20, -393.5±0.2 kcal/mole. The heat of the crystalline transformation (COOH)2(a) ? (COOH)2(ß) was determined to be 0.30±0.02 kcal/mole at 298.15° K.

Jan 1, 1970

By Oleg Terichow

The Bureau of Mines studied the penetration of a slender cylindrical tube into a sand bed, simulating seafloor material under the application of a static load. The factorial experimental design was based on three factors: tube diameter, geometry of penetrating bit, and seawater saturation of sand, all of which were found to be significant in influencing the depth of penetration. The geometry of the penetrating bit, or shoe, is of major significance in the mechanics of penetration and should be considered the most important factor for additional study. Linear regression analyses of the load-penetration data show that the relationship is linear.

Jan 1, 1970

By Roy F. Abernethy

This report describes a method developed by the Bureau of Mines for the determination of beryllium in coal ash. Samples are put into solution by standard wet chemical procedures. Interfering elements are complexed with Na2EDTA, and the beryllium is separated by extraction of its acetyl acetone complex with chloroform or carbon tetrachloride. Final determination is made with Beryllon II.

Jan 1, 1970

By M. M. Tilman

The Bureau of Mines investigated the precipitation strengthening of lead¬-base alloys containing 0.5 through 4 weight-percent combined Cd plus Sb. The Cd and Sb were alloyed in a 1-to-1 atomic ratio which maintained compositions along the quasi-binary section Pb-CdSb. Tensile properties, creep rates, and stress-rupture values were obtained on alloys in the aged condition. The highest tensile strength was observed in an alloy of Pb-3 CdSb, After aging for 6 months at 90°±3° F, this alloy had a mean tensile strength of 8,950 psi with 15-percent elongation. An aged alloy of Pb-1 CdSb exhibited a steady state creep rate of 1.2 X 10-3 percent per day at a stress of 500 psi and a temperature of 90°±3° F. Times to rupture at stresses up to 4,000 psi and at a temperature of 90°±3° F were obtained for some compositions.

Jan 1, 1970

By Oliver C. Fursman

The Bureau of Mines undertook this investigation to study methods of utilizing red mud residues from production of alumina from bauxite. Pilot-plant tests were conducted using Jamaican and Surinam red muds. Both the carbon-lime-soda sinter process and electric-arc smelting with coke and limestone were employed to recover iron and alumina. Alumina recoveries of 85 to 90 percent were obtained by the sinter process; although iron recovery was about 80 percent, the magnetic product was finely divided and difficult to separate from the gangue. Smelting red muds in the electric-arc furnace produced a pig iron with 98-percent recovery of iron; up to 84 percent of the A1203 was recovered by leaching the calcium aluminate slag with Na2C03 solution. A titania product assaying 96 percent TiO2 was recovered from the nonmagnetic portion of Surinam red mud sinter by extraction with H2SO4. Leached calcium aluminate slags and brown mud (from the combination Bayer process) are possible raw materials in the manufacture of portland cement.

Jan 1, 1970

By E. F. Ferrell

Electrowon molybdenum powders and a commercial hydrogen-reduced powder, all with different minor impurities, were investigated by the Bureau of Mines with respect to inherent properties, to fabrication techniques, and to proper-ties of the fabricated sheet. Compared with the commercial hydrogen-reduced powder, the electrowon powders had a larger particle size, a greater flow rate, a higher apparent density, and a lower oxygen content. Sheet materials prepared from the two types of powders showed similar mechanical properties, under the same conditions of heat treatments, except for low-temperature ductility. Yield strengths varied with carbon content, heat treatment, and test temperature.

Jan 1, 1970

By Alfred E. Schwaneke

A versatile torsion creep tester was instrumented with electromechanical and servomechanical components to operate automatically and unattended, producing digital printed outputs. The apparatus uses an electrical system for applying torsional stresses, and a unique angular transducer as a null detector operating a servocontrolled strain measuring system with the digital readout. The tester is designed to measure the creep in single-crystal or polycrystalline zinc, zinc alloys, magnesium, magnesium alloys, or other metals and alloys. Applied stresses may be varied from zero up to 2,000 psi in the outermost fibers of a 1/8-inch-diameter, 4-inch-long specimen. Strain readings to 0.001 degree, equivalent to a strain of 2.73 X 10-7, may be made automatically from one every 5 seconds to one per month. The apparatus has provisions for programed temperature control and special atmospheres or vacuum operation. A discussion of applications of the system to other mechanical testing apparatus is included.

Jan 1, 1970

By J. Grumer

The Bureau of Mines, under the sponsorship of the Space Nuclear Propulsion Office, conducted a laboratory-scale hydrogen safety study which determined several combustion characteristics of hydrogen diffusion flames. Experiments show that ambient air may enter the top of a hydrogen flare stack when the hydrogen flow is low. A new concept, supported by photographic evidence, predicts that diffusion flames burning in air on a wide, upright pipe (stack) and fed with slow, upward flows of buoyant gas will induce a downward flow of air along the walls of the pipe that can support combustion within the pipe. Predicted flamedip limits agree roughly with experimental values determined on 6-, 12-, and 18-inch-diameter stacks and increase with increasing stack diameter. Measurements were made of the limiting flow at which a hydrogen diffusion flame blows out in still air. By means of an empirical application of the critical boundary 8 velocity gradient concept, these data lead to a blowout limit of about 10 reciprocal seconds for a hydrogen diffusion flame. Burning rates of large hydrogen diffusion flames ranging from about 0.03 to 1 ft/sec were used to predict approximate flame heights on flare stacks. Temperatures of larger hydrogen diffusion flames up to about 3,600° F were observed, but the most representative value appears to be about 2,600° F. It was found that crosswinds do not strip significant amounts of unburned hydrogen from its diffusion flame and that water-cooled flare stacks are not likely to be damaged when flame is blown back into them by opposing winds.

Jan 1, 1970

By Garrett R. Hyde

Sintered yttria and sintered dysprosia can be used to make single-component thermistors having typical thermistor geometries and operable in the temperature range 500° to 1,200° C. However, at these temperatures, instability of platinum electrodes can contribute a slight aging effect if the thermistor is kept near 1,200° C for long periods. Typical characteristics at 500° C for an yttria disk thermistor 12 mm in diameter and 2 mm thick are a resistance of 12.4 megohms and a temperature coefficient of resistance of -3.8 percent per degree C. Typical characteristics at 500° C for a dysprosia thermistor of the same dimensions are a resistance of 1.84 kohms and a temperature coefficient of resistance of -1.6 percent per degree C.

Jan 1, 1970

By I. D. Shah

The Bureau of Mines investigated the sequence of principal chemical reactions taking place during the roasting of covellite (CuS). Practically all covellite is converted to digenite (Cul.SS) before oxidation to Cu20 begins. Part of the Cu2O is then converted to CuO, which in turn forms CuS04 through CuO?CuS04 as an intermediary. CuS04 and CuO'CuS04 decompose at 600° to 700° C to yield CuO and S03 (g) as final products. An overall mechanism is proposed for chemical reactions occurring at different interfaces of partially oxidized CuS pellets.

Jan 1, 1970

By Roy L. Wilfong

Surface area measurements were conducted on cadmium sulfide powders following thermal treatments at temperatures up to 500° C and treatment times up to 1 week. Thermal treatments at temperatures up to 300° C produced no significant changes in the surface area of the powders even after 1 week of exposure. At 500° C some decomposition of the cadmium sulfide occurred.

Jan 1, 1970

By John P. Hansen

Batches of red or brown iron ore concentrates, weighing 100 or 200 grams, were reduced with gaseous reductants in a laboratory-sized fluidized-bed reactor. Using a loss of weight technique, the rates of reduction were measured and the effects of temperature, gas consumption, and gas flow rates were determined. Below about 725° C the rate of reduction was controlled by the chemical reaction at the reduction interface having an activation energy of about 10 kcal/g mole. Above about 725° C the rate of reduction appeared to be controlled by the flow of the gaseous reductant and therefore to be directly proportional to the flow rate. Above 725° C, hydrogen reduced the iron ore much faster than carbon monoxide. In gas mixtures, carbon monoxide or nitrogen reduced the hydrogen partial pressure and lowered the reaction rate proportionally. When present in large concentrations, carbon monoxide had a serious inhibiting effect on the reduction rate, probably owing to carburization and sintering of the reduced iron.

Jan 1, 1970

By James J. Olson

The Bureau of Mines recorded both particle accelerations and velocities from one-stick and production blasts at Eagle-Picher Industries' Shullsburg mine, Shullsburg, Wis., to test the effectiveness of square root scaling in grouping underground blast vibrations and to determine the effects of rock type and mine geometry on blast vibrations. Although the charge weights of subsequent delay periods sometimes exceeded the charge weight of the zero-delay period, both acceleration and velocity records showed that the zero-delay portion of the Shullsburg production blasts produced the highest vibration amplitudes. Because of the restricted range of charge weights in the Shullsburg experiments, no statistical determination of an appropriate scaling factor could be made. However, the square root scaled peak particle velocity data from the Shullsburg production blasts grouped well within the approximate band-width of vibration data obtained by the Bureau from quarry blasts in many different rock types. This indicates that scaling by some factor, perhaps the square root or cube root of the charge weight, may be an effective way to group and study vibration data from underground blasts. Further research is needed to determine which scaling factor is best for underground blasting.

Jan 1, 1970

By Henry M. Harris

The roll forming of oxide powders was studied in a Bureau of Mines investigation to find the conditions and parameters required to make satisfactory ceramic strip. High-quality porous or dense alumina, zirconia, and porcelain shapes were made by sintering strip roll-formed at room temperature from powders containing minor amounts of binder and water. Strips with thicknesses of 0.04 to 0.08 inch and bulk densities from 40 to 90 percent of theoretical densities were made. The parameters most important to formability were particle size, condition of the powders, and roll gap. Other factors affecting quality were speed and surface condition of the rolls, amount and type of binder, water content, and sintering conditions. Ceramic strip was formed at rates up to 78 feet/minute, which is 13 to 23 times faster than reported by previous investigators, and forming was done in a simple and inexpensive roll unit. Reshaping the strip was possible by cutting, grinding, shearing, and stamping. The following innovations were developed that allow roll processing not normally possible with ceramic powders: (1) Fine-sized powders were made into strip by preparing these as partially sintered granules; (2) thick strip was formed by pressure feeding powders into the rolls; (3) flexible strip was made using a rubber-base bonding agent; (4) corrugated strip was formed on shaped rolls; and (5) porcelain strip was densified and reduced in thickness by rerolling while hot.

Jan 1, 1970

By H. J. Heinen

Malononitrile [CH2(CN)2J, which forms a carbanion in basic solutions, was investigated as a potential leachant for gold and was shown to be an effective extractant in alkaline pulps. Malononitrile was comparable to equal molar quantities of sodium cyanide (NaCN) in leaching gold from an oxide ore and yielded 10 to 20 percent higher recovery in leaching a refractory carbonaceous ore, although dissolution was slower with malononitrile than with cyanide. Complete recovery of the gold from the pregnant solutions was achieved by coprecipitation with a lead salt on zinc dust; the leachant was shown to be capable of regeneration and recycling a limited number of times. Addition of an anion-exchange resin to the carbonaceous pulp containing malononitri1e increased gold recovery from 67 to 95 percent. Some malononitrile derivatives were also shown to be gold solvents.

Jan 1, 1970

By Kenneth H. Johnston

Information on oil and water production, volume of water injected, core analyses, and well completion data was collected on 28 Red Fork sand water-flood projects for comparison and evaluation of results. An average water injection efficiency of 35 percent, an average water-injected to oil-produced ratio of 16.8:1, and an average loss outside the flood pattern of approximately 45 percent of the injected fluid resulted in an oil recovery to January 1, 1969, of only 5.6 percent of the pore volume, or 9.1 percent of the initial stock-tank oil in place. The principal causes of poor oil recovery from these projects are the losses of large quantities of injection water from the flood patterns through oriented, natural fracture systems or zones of high permeability and excessive channeling of injection fluids from input wells to oil wells. For more efficient operation and a higher percentage of oil recovery from the Red Fork sand and other low-permeability-sand waterflood projects, directional orientation of both induced-and natural-fracture systems should be determined during early development. The success of a low-permeability-sand waterflood project depends to a large extent upon the orientation of the injection wells with the fracture system.

Jan 1, 1970

By J. E. Murphy

Purification of samarium metal by sublimation and by vaporization from a low-melting metal flux, at the same temperature, were compared. Vaporization proved more effective for removing impurities such as magnesium, calcium, and manganese. Recovery of samarium, however, is more rapid by sublimation because of its constant rate of distillation.

Jan 1, 1970