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By Robert E. Barieau

This report gives the principles of the method used by the Helium Research Center of the Bureau of Mines when solving nonlinear-regression problems and contains the mathematical equations necessary to accomplish the following objectives: the evaluation of the parameters in such a way that the sum of the weighted squares of the residuals of an experimental observable is a true minimum, regardless of the functional relationship between the variables and these parameters; and the evaluation of all variances and covariances of the parameters by means of the usual approximation of the law for the propagation of errors.

Jan 1, 1967

By F. X. Tartaron

Behavior of hard-burned quicklime was compared with that of soft-burned quicklime in an oxygen converter utilizing oxygen blowing in a rotating cylindrical vessel, set at a 30° to 60° angle to the horizontal and operated at a predetermined speed of rotation. Four pairs of tests were made) each comparing hard lime with soft lime. Three of the pairs differed from one another in the quantity of lime employed) and the fourth differed in blowing time, All four pairs showed an increase in yield when soft lime was used. Three of the pairs revealed that the ratio of the oxygen consumed with soft lime to the oxygen consumed with hard lime was the same as the ratio of metal yield with soft lime to the metal yield with hard lime. The fourth pair contained an error and could not be included. Finally, a close inverse relation was found between the combined iron in the slag and the combined lime in the slag, which can be expressed by the equation pct Fe = 52.67 -0,906 (pct CaO).

Jan 1, 1967

By J. M. Stuve

Standard heats of formation (AH°p) of YbCl3 (c) and TmCl3 (c) were measured by solution calorimetry. Heat of solution data are given for ytterbium and thulium metals and corresponding anhydrous trichlorides in 4.360 molal hydrochloric acid. The derived standard heats of formation of YbCl3 (c) and TmCl3 (c) were -229,370 ±720 and -235,820 ±400 cal/mole, respectively, at 298.15° K. The resulting heats of formation for YbC13 and TmCl3 are about 1 kcal and 6.3 kcal more negative than previously published values.

Jan 1, 1967

By R. W. Van Dolah

The Bureau of Mines t.ced its investigations into sympathetic detonation of ammonium nitrate (AN) and ammonium nitrate-fuel oil (AN-FO) to define the scaling law for safe separation from detonating AN-FO. Both missile- and non-missile-producing AN-FO donors, weighing up to 5,400 pounds, were employed with acceptors of the same size. The usual cube-root scaling law was not confirmed; exponents for the relationship S = f(Wx) for AN were 0.51 with non¬missile-producing donors and 0.61 for missile-producing donors. For AN-FO an exponent of 0.80 was indicated in the missile-producing case. AN-F0 in polyethylene bags appeared somewhat more easily initiated than bulk AN-FO. The efficacy of barricades in protecting AN charges was investigated. detonation distances were reduced from one-third to one-seventh when filled barricades were employed. The investigation was extended to dynamite with both types of donors. With 1,600-pound missile-producing donors and an equivalent weight of dynamite, initiation would be expected in 50 percent of the trials at 167 feet. The corresponding value in the non-missile case was 67 feet. The data developed in this program of sympathetic detonation will allow the development of a rational set of safe separation distances for AN, AN-FO, and explosives.

Jan 1, 1966

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindablity index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions3 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous of coal as delivered is a check on the practical results obtained in the coal.

Jan 1, 1967

By H. G. Iverson

Solid state reactions of manganese with silica were investigated in high-temperature tests. Reactions of 0.5 to 4.0 moles manganese (Mn) with 1 mole silica (SiO2) at 1,100° C and of 2.0 Mn:SiO2 mole-ratio mixtures at 1,000° to 1,150° C yielded products consisting of a slag phase and a metallic phase. At 1,100° C, the slag phase from reactions of the low Mn:SiO2 mole-ratio mixtures was composed of SiO2 and rhodonite (MnSiO3), and the slag phase from the high Mn:SiO2 mixtures was composed of MnSiOs and tephroite (Mn2SiO4). The metallic phase from the corresponding low Mn:SiO2 mole-ratio reactants consisted of two manganese silicides, Mn5Si3 and Mn3Si; from the high Mn:SiOg mixtures, it was Mn and the manganese silicide (Mn5Si). For the higher mole ratios of MnSiO2 the manganese content in the metallic phase increased, while the manganese and silica contents of the slag phase remained nearly constant. The slags did not contain free or uncombined manganese oxide (MuO). For the 2.5 to 4.0 Mn:SiO2 mole-ratio mixtures reacted at 1,100° C, the maximum quantities of silica reduced and of the manganese in the slag appeared to become asymptotical at about 41 and 48 percent, respectively. A brominating procedure was developed that was highly selective in removing the metallic constituents from the reaction product, leaving the slag phase as residue. X-ray diffraction patterns were obtained on prepared silicides Mn5Si, Mn3Si, and MnSi.

Jan 1, 1967

By P. G. Barnard

The Bureau of Mines investigated the effects of various additions of rare-earth metals or rare-earth oxides on the mechanical properties of cast and wrought plain-carbon steels. Rare-earth metals, as misch metal, were added to medium-carbon steel in amounts to 0.70 weight-percent; rare-earth oxides, as a commercial mixture, were added in amounts to 1.50 weight-percent. The melting and casting of conditioned steels were done in a vacuum-induction furnace, to avoid formation of oxides from the melting atmosphere and to pro-vide better control over chemical composition. At room temperature, data for tensile strength, yield strength, elongation, and hardness of cast and wrought steels were obtained by standard testing equipment and procedures. Impact tests were conducted on as-cast steel specimens. The greatest amount of tensile ductility and impact strength was obtained in as-cast steel with 0.50 to 0.70 weight-percent misch metal additions. No significant improvement on mechanical properties was indicated in wrought steels containing rare-earth metal additions in the range from 0.10 to 0.70 weight-percent. In general, the rare-earth oxide additions up to 1.50 weight-percent had little effect on the tensile properties of steel in the cast, wrought and annealed, or wrought and normalized condition.

Jan 1, 1967

By Murray Weintraub

In an investigation of the incineration of combustible wastes, the Bureau of Mines studied the effect of dimensional parameters, process variables, and fuel properties on the operation of an incinerator that consisted of a single cylindrical combustion chamber in which all combustion air was supplied tangentially above the fuel. Construction and operation of three designs of such a device proved that the tangential overfire air design is effective in providing efficient combustion and low concentration of particulate matter in the effluent gas. A correlation was found that related burning rate with air rate, chamber diameter, and inlet port diameter. In one of the incinerator models, ignition was by radiation from a preheated surface. The temperature of this surface was required to be 1,400° to 1,600° F to insure ignition of moist refuse; however, this had little effect on combustion rates. In the combustion of moist refuse, evaporation of the water proceeded through the fuel bed as a wave, with an ignition wave following the evaporation.

Jan 1, 1967

By C. Q. Cupps

n view of increased interest in secondary recovery of oil in the Cut Bank field, Montana, a review has been made of unpublished data obtained during a 1943-44 study of reservoir oil characteristics in this field. Considerable uncertainty was attached to interpretations of subsurface oil sample analyses from six Cut Bank zone wells, one Lander sand well, and one Moulton sand well, because of adverse sampling conditions and wide range in the data. Much of this uncertainty has been removed by this review which has shown two of the Cut Bank zone samples and the Moulton sand sample to be representative of the reservoir oils. Estimates of original reservoir oil characteristics derived from differential-liberation analyses of these samples show that the oil in the Cut Bank zone was initially saturated at the gas-oil contact pres-sure, 750 psia, and the oil in the Moulton sand was undersaturated with a saturation pressure of only 380 psia. The rest of the samples were indicated to be nonrepresentative of the reservoir oils because of a disproportional vaporization of heavier components of the solution gas. The vaporization of these components is believed to be a cumulative effect of contact of the oil with bypassing, light-gravity gas which had been liberated at higher pressures from solution in oil farther back in the formation, or which had come from the gas cap, rather than from the singular effect of gas evolution caused by excessively low bottom-hole pressures. Change of oil composition caused by the latter was found to conform closely to that occurring during a differential liberation of gas in the laboratory.

Jan 1, 1967

By R. J. Heemstra

A continuous flowing paper electrophoresis cell was used to separate petroleum and petroleum extracts into characteristic patterns. The electrophoresis of Bachaquero, Lagunillas, Boscan, and Gibson petroleums in nitro-benzene and acetic acid-based electrolytes was investigated. The extent of separation in the patterns was studied by measuring the metal and porphyrin contents of the effluents. Qualitative separations were achieved in some systems, whereas either system demonstrated only a high degree of electrophoretic migration.

Jan 1, 1967

By Jr. Hill

Laboratory metallurgical treatments of three high-iron bauxite ores from Arkansas were conducted to determine the relative effectiveness of experimental methods for recovering alumina and a commercially acceptable iron concentrate. The standard for evaluating recoveries from experimental processes was the Al2O3 recovery from Bayer digests of the crude ores; recoveries from digestion of the three ores were 74.1, 87.4, and 88.7 percent. Flotation, magnetic separation, or various combinations of digestion, calcination, and reduction-sintering, leaching, and magnetic separation of leach residues failed to produce Al2O3 recoveries as high as the standard. A high-iron-bearing fraction, containing between 68 and 78 percent of the total iron, was produced in a three-phase treatment involving a caustic, lime reduction-sinter of the crude ore, water extraction of Al2O3 from the sinter, and magnetic separation of the leach residue.

Jan 1, 1967

By John S. Berber

To improve the economics of low-temperature carbonization of coal, the Bureau of Mines is conducting research on the upgrading of the product tar to marketable chemicals. This report describes experiments on the catalytic hydrodealkylation, followed by catalytic vapor-phase oxidation of the dealkylate to phthalic and maleic anhydrides, of mixed residues from the urea adduction of lignite-neutral oil fraction and on the catalytic thermal dealkylation of high-boiling tar acids. The hydrodealkylation experiments were conducted at pressures from 1,000 to 1,750 psig and at temperatures from 600° to 1,000° F. The oxidation was, in all cases, at atmospheric pressure and 9500 F. Maximum yield of maleic anhydride, based on the liquid feed to the hydrodealky1ation unit, was 12.2 percent at 750° F and 1,500 psig; that of phthalic anhydirde was 6.9 percent at 650° F and 1,500 psig. Maximum yield of combined anhydrides was 18.8 percent at 650° F and 1,500 psig. The non-dealkylated feed material, upon oxidation, yielded 8.9 percent and 3.8 percent maleic anhydride and phthalic anhydride, respectively.

Jan 1, 1967

By Leo A. Schrider

A prediction for oil recovery from a pilot waterflood in the Kane oil- field, located in Elk, Forest, and McKean Counties, Pa., was made and compared to actual field performance. Water-injection and production histories, well logs, other field data, and results from laboratory tests of core material were used in this analysis. Performance of the pilot waterflood, initiated in January 1963, was predicted using a modified Craig, Geffen, and Morse calculation technique. Maximum recovery from this low permeable, preferentially oil-wet formation was predicted to be about 22,500 barrels of oil after 300,000 barrels of water had been injected into the pilot waterflood area. After additional field data were collected it became necessary to reevaluate the pilot waterflood area. The gas saturation prior to the waterflood was estimated to have been 20 percent, based on an assumption regarding the required volume of water injected to initiate oil production. In view of the actual field performance, a gas saturation of 13 percent is indicated. When this gas saturation and the method originally proposed by Craig and others are used) the predicted results are more representative. In December 1965, field performance was further analyzed using a hyperbolic-decline curve as presented by Arps. Based upon this evaluation method, the pilot water flood in the Kane sand should produce 37,000 to 42,000 barrels of oil with the injection of 300,000 barrels of water into the pattern. By continuing this secondary-recovery project to a reasonable economic limit, ultimate oil recovery may be as much as 50,000 to 55,000 barrels, or 129 to 142 barrels per acre-foot from 36.5 acres.

Jan 1, 1967

By W. P. Haynes

To evaluate the potential use of battery-powered vehicles, the Bureau of Mines studied the performance of a battery-powered truck propelled by a 9.6 kw dc motor in considerable detail under various driving conditions. Some of the factors investigated were: Gear ratios, payload (1,468 lb maximum), road grade, stops made per mile, and charging time. With the exception of some difficulty with brush wear, operation and maintenance of the truck was generally trouble-free. On range tests carrying an 868-lb payload a distance of about 50 miles at an average speed of about 19 mph in normal driving, the Bureau's battery-powered truck averaged 1.6 to 1.9 miles per ac kwhr input. Stop-and-go tests indicated that prospects for the use of battery-powered trucks in house delivery service within city limits are good; performance of the Bureau truck was sufficiently high for that type of service. The estimated power cost of 2.65 cents per mile while making 10 stops per mile was attractively low from the standpoint of fuel costs.

Jan 1, 1967

By Jr. Koch

As a part of a larger study of the distribution of metals within ore deposits, the geometry of distribution of gold, silver, lead, copper, and zinc in five veins of the Fresnillo mine, Zacatecas, Mexico, was established. The purpose was to obtain basic data necessary for evaluation of geological theories about processes of vein formation and useful for practical mining applications in ore estimation and prediction of ore beyond present workings. The Bureau of Mines investigation comprised statistical analysis of 64,000 assay values from some 16,000 mine samples. The samples were taken at 2-meter intervals in drifts exposing the veins through a vertical range of some 750 meters. Within individual veins, the metals are distributed in dome¬like patterns with highest metal contents tending Lo occur in oreshoots at the centers of the developed parts of the veins. However, in the block of ground containing all five veins, base metals define mathematical domes with highest contents near the center; precious metals define mathematical basins or troughs with low contents near the center. The ratio of silver assay values to lead assay values corresponds to two geographically distinct types of mineralization: one in which silver is closely related to lead, and another in which silver is independent of lead. Other metal ratios also vary regularly from one place to another. The statistical methods employed in this study would be useful for other geologists or engineers who need to analyze large amounts of assay or similar numerical data.

Jan 1, 1967

By Jack Smith

New turbine blades designed to resist ash erosion were tested by the Bureau of Mines in a pilot-scale coal-fired gas turbine. After a total of 1,963 hours, the rotor blades were only slightly eroded; and they had an estimated useful life of 20,000 to 30,000 hours. Changes in aerodynamic design of the blades successfully concentrated the ash at the outer casing, but stepped sidewalls for the rotor drum and wear strips at the bases of the rotor blades are still needed to minimize wear at these points. Stepped sidewalls and wear strips did not adequately protect the stator blades. Ash slightly eroded their leading edges, above the inserts, and cut notches into their trailing edges near the bases. Stator blade life was estimated at 5,000 to 7,500 hours. Blade erosion in these tests was less severe than with previous designs, but more efficient combustors and ash separators are required to reduce the amount and size of ash entering the turbine, to achieve acceptable blade life for commercial operation.

Jan 1, 1967

By David E. Nicholson

In a Bureau of Mines investigation of the dynamic compaction of mine hydraulic backfills, two basic forms of mechanical vibration inducers were used and compared for effectiveness of compaction. Internal compaction, using concrete probe vibrators of various sizes, and external compaction, using plate vibrators} were studied and evaluated for use in underground stopes. An aluminum plate, which was light and displaced sufficient volume to remain afloat in fluid fill, and a steel plate were both used in the external compaction tests. Efficiency of compaction was better in studies conducted with internal probe vibrators. Tests were conducted in an underground backfilled stope with three different-sized probe vibrators (2-, 4-, and 6-inch-diameter) to determine an approximate area of influence. Results showed the areas of influence to be approximately 3, 4, and 5 feet in diameter, respectively, for the three different probes. Physical properties of hydraulic slurries were determined; preferred grain-size distributions, water exudation properties, and water contents of hydraulic slurries are reported. The best compaction results were obtained with moderately well-graded, fully saturated backfills, with slow rates of water exudation, which were capable of remaining in a semifluid state during the compaction process.

Jan 1, 1967

By J. W. Town

Recrystallization studies on chrome-bearing spinel materials were made by the Bureau of Mines to determine the effects of certain fluxing agents and cooling rates on the chromium-to-iron ratio of recrystallized spinel. Statistically designed and evaluated tests showed that the ratio of chromium to iron in naturally occurring chrome spinel could be increased from 1.5 to 1 to over 7 to 1 and that the ratio of chromium to iron in the chrome-spinel in a stain-less steel slag could be raised to over 18 to 1. Silica, magnesia, and lime had significant positive effects, while alumina had a significant negative effect. Cooling rates of 200 C per hour in a programmed spiral globar electric furnace were satisfactory for growing crystals of recoverable size.

Jan 1, 1967

By Robert E. Barieau

General expressions for evaluating practically all the thermodynamic properties of a fluid from a single equation of state are derived. Most of the formulas are expressed in terms of the compressibility factor, with this factor being an explicit function of the temperature and the molal density. Similar expressions are given using reduced variables.

Jan 1, 1967

By T. Estelle Gardner

Heat-capacity measurements were made over the range 8° to 350° K on beryllium sulfate dihydrate and beryllium sulfate tetrahydrate using an adiabatic calorimeter. No anomalies were noted in the curve for either compound. Smooth values of heat capacity, entropy, enthalpy function, and free-energy function were calculated from the heat-capacity data at 10° K intervals and at 273.15° and 298.15° K. The entropy values calculated at 298.15° K were 39.01 ± 0.12 entropy units (eu) for the dihydrate and 55.68 ± 0.17 eu for the tetrahydrate.

Jan 1, 1967