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By J. J. Demeter

Anthracite from the four producing regions in Pennsylvania was both ashed in the laboratory and burned on a chain-grate stoker to determine the sulfur-retention properties of its ash. The retention of sulfur in laboratory-prepared anthracite ash was shown to be related to ashing temperature and to the amounts of sulfur and calcium present in the coal. At the usual laboratory ashing temperature of 750° C sulfur retention ranged from 0.8 to 13.2 percent of the total coal sulfur. Sulfur retention in the ash was negligible, o to 0.3 percent, at 1,200° C, which is the thermal decomposition temperature of calcium sulfate; thus calcium sulfate does not form and cannot serve as a sulfur-retaining agent. In several tests the anthracite was mixed with 6 or 10 percent dolomite prior to firing in the chain-grate stoker. The dolomite did not improve sulfur retention owing to the high temperature in the fuel bed. Sulfur retention was, however, related to the unburned carbon in the ash. The relationship of the percentage of original coal sulfur retained in the ash (Y) to the percentage of the original carbon in the coal remaining in the ash (X) is expressed by Y = -0.579 + 0.914X. The percentage of sulfur retained is almost directly proportionate to the percentage of original coal carbon in the ash.

Jan 1, 1968

By Kenneth H. Johnston

Information and data necessary for research on improving methods of oil recovery from low-permeability reservoirs and for comparison and evaluation of performance of such reservoirs with those producing from more permeable sands were obtained. Core analyses, well logs, production tests, well stimulation techniques, primary and secondary production records, and data on two water-flood projects were examined for wells producing from the Bartlesville sand, West Avant field, Osage County, Okla. Overall recovery from the study area was generally poor with only 9.0 percent of the pore volume recovered to January 1, 1968. Larger fracture treatments (8,000 to 12,000 gal) could have resulted in an increase in primary oil recovery. Secondary recovery by water-flooding accounted for only 1.9 percent of the pore volume because of the inability to control the large volume of injection fluid that escaped from the flood patterns and the excessive volumes of water produced with the oil. Future waterflood development in other low-permeability reservoirs should include the drilling of new input wells, use of injectivity surveys to locate possible natural fracture systems, or zones of high permeability, and control of injection fluids by altering flood patterns and/or plugging of the more permeable zones.

Jan 1, 1968

By H. G. Iverson

An investigation was conducted on the conditions affecting the precipitation of aluminum by autoclaving synthetic solutions containing Na2SO4, Al2(SO4)3, H2SO4, and H2O. Virtually all of the alumina could be precipitated as natroalunite (NaAl3(SO4)2 (OH)6). This product could be readily filtered and dried. Results are reported in terms of alumina precipitated in this compound and not in terms of alumina itself. Solutions of ~ 0.30, ~ 0.60, and ~ 0.80 mole/liter A1203 and various concentrations of H2SO4 and Na2S04 were investigated. The optimum time and temperature for autoclaving were 20 to 30 minutes at 200° C. The highest yields of natroalunite were obtained from solutions containing little H2SO4 and ~ 2 moles Na2SO4 per mole A1202. Acid in quantities of 0.3 to 0.5 mole/mole of alumina in solution depressed the yield to 90 percent or less. In differential thermal analysis, at 1,000° C the natroalunite precipitate decomposed without melting to yield SO, and SO2 gases, a solid composed of Na2SO4, and gamma and alpha Al203. Continued heating to 1,200° C produced No SO, and alpha A1303. Water-leaching of this product removed the Na2S04 and left a final residue of alpha A1203.

Jan 1, 1968

By John B. Shutack

In an effort to improve the performance of the explosive-anchored rock bolt, the Bureau of Mines studied the effect of the detonation velocity of the explosive and type of charge (linear or nonlinear) on the fracturing tendency of the anchor tube. Also, different types of tubing were compared to determine the one most suitable for use as an anchor tube. The Bruceton up-and-down method was applied in tests in which steel shooting blocks having boreholes ranging from 1-3/8 to 2-1/8 inches in diameter were used. Of the four types of tubing evaluated, a welded A-178 tubing that was drawn over a mandrel and renormalized gave the most promising results. The A-179 seamless tubing that is normally used with the explosive bolt was the most inferior. Both types, however, gave significantly better anchorage than the conventional shell when tested in both laboratory and underground experiments. Within the range of velocities studied (5,000 to 7,000 m/sec), the type of explosive showed no significant effect on anchor-tube performance. In general; linear explosive charges provided better anchorage than nonlinear charges.

Jan 1, 1968

By R. E. Thill

The ultrasonic pulse measurement system described measures velocities of longitudinal (compressional) and shear waves in rock to give values that can be used with density values to determine the dynamic elastic constants of rock. A special feature of this pulse measurement system is its unique acoustical bench that minimizes errors in pulse transit times that are commonly associated with coupling, sample alinement, and sample orientation. Some special features of the acoustical bench are its highly versatile transducer cartridges, a pneumatic ram coupling device, an orientation mechanism, and a vacuum chuck sample holder. The lathe-bed-like construction of the acoustical bench assures automatic alinement of samples and versatility in accommodating samples of various shapes and sizes.

Jan 1, 1968

By Robert A. Bradburn

The Bureau of Mines has developed a miniature, portable two-level oxygen-deficiency alarm and produced three prototype models. Each operates from a 4.2-v dc power source, and the highest current drain of any model is 80 ma. An electrochemical cell, which produces an electrical output in proportion to the partial pressure of oxygen to which it is exposed, is used as an oxygen detector. The output of the cell is applied to an electronic circuit that detects two different levels of oxygen percentage below that of normal air, and produces distinct audible signals at these levels. The hazard alarm mode is activated when the oxygen percentage first drops below normal and produces a 500-cps "beep" tone with an intermittency of 1 cps. The danger mode produces a continuous 500-cps audible signal when the oxygen percentage drops still lower.

Jan 1, 1968

By F. E. Brantley

Optimum autoclaving conditions were determined for separation of iron and manganese values from pregnant leach liquor produced in extracting manganese from low-grade umber are. The umber was leached with a synthetic anolyte similar to a recycle solution, used in manganese electrolysis cell operations, that had been renewed with ferrous sulfate and sulfuric acid. The equipment used and results obtained are presented for the several conditions employed. The kinetics of the separation were studied. Rate equations were derived for the formation of solid ammonium-manganese sulfate, (NH4)2 Mn2 (S04)3.

Jan 1, 1968

By L. H. Adami

Heats of formation were obtained for four anhydrous crystalline sodium borates by hydrochloric acid solution calorimetry. The heats of formation at 298.15° K from the elements are NAB02, -233.2 ±0.6 kcal/mole; Na2B07, -786.4 ±1.0 kcal/mole; NaB305, -549.9 ±0.8 kcal/mole; and Na2B6013, -1,412.5 ±2.0 kcal/mole, The heats of formation from the constituent oxides are NaB02, -31.5 ±0.8 kcal/mole; Na2B407, -78.8 ±1.3 kcal/mole; NaB305, -44.1 ±0.8 kcal/mole; and Na2B8013, -96.7 ±1.5 kcal/mole.

Jan 1, 1968

By Martin H. Stanczyk

Bench scale, laboratory batch attrition grinding tests were made of a coarse commercial kaolin in a stainless steel, 5-inch-diameter attrition grinding machine to study the effect of a number of basic operating variables on particle size reduction and electric energy consumption. The results of the investigation showed that the more important operating variables influencing the efficiency of kaolin comminution and energy consumption requirements were type, size, and shape of grinding media, grinding media to clay weight ratio, peripheral rotor speed, clay slip pulp density, degree of pulp dispersion, and the angular arrangement of the rotor and stator bars. The tests also indicated that variables having less influence on grinding efficiency and energy consumption were pulp temperature, design of rotor cage, rotor clearance, rotor-stator bar interval, addition agents, pulp level, degree of pulp aeration, and chamber liners. The research showed that grinding media had the greatest influence on abrasion of machine parts and that spherical-shaped grinding media were superior to sharp angular or long bladed media with respect to media degradation, machine abrasion as well as grinding efficiency.

Jan 1, 1968

By W. L. Acherman

The Bureau of Mines found the chemical and galvanic corrosion behavior of the TZM and molybdenum-30 tungsten alloys to be generally equal or superior to that of unalloyed molybdenum in many aqueous solutions of acids, bases, and salts. Notable exceptions occurred in 1 [N] nitric acid, where both alloys corroded appreciably faster than molybdenum. In mercuric chloride solutions, the TZM alloy was susceptible to a type of crevice corrosion which was not due to differential aeration. The alloys were usually not adversely affected by con-tact with dissimilar metals in galvanic couple experiments, but the dissimilar metals sometimes corroded galvanically. Both alloys were resistant to substitute ocean water spray at 60° C.

Jan 1, 1968

By W. S. Sanner

Grinding experiments were conducted to determine the finest anthracite particles that could be produced in a ball mill. Continuous and batch tests were run in a dry-grinding ball mill. Batch grinding produced the finest coal particles. They averaged 2.2 microns in diameter and were 99.0 percent smaller than 37 microns. Continuous grinding yielded a product 6.1 microns in diameter, with 96 percent smaller than 37 microns.

Jan 1, 1968

By John R. Hoskins

The Bureau of Mines conducted an investigation to more exactly define the influence of some end conditions on the laboratory-determined uniaxial compressive strength of rock samples. Limestone, marble, sandstone, and granite were used to provide a range of specimen modulus of elasticity from 2.7 X 106 psi to 10 x 106 psi. Four variables were studied: Nonparallelism and surface texture of specimen ends were the specimen variables investigated; the end platen size and the adjustable or spherical head friction were the machine variables studied. It was concluded that the loading ends of small laboratory models and samples should be prepared with surface irregularities that do not vary from a plane surface by more than 0.001 inch. It was also concluded that nonparallelism of the specimen ends should not exceed 8 minutes for a rigid head load or 15 minutes for an adjusting head load. The measured compressive strength of specimens prepared with these tolerances will be statistically the same with any diameter or thickness of platen and any degree of head friction if initial alinement of the specimen is assured.

Jan 1, 1968

By John Ward Smith

The Bureau of Mines drilled Wyoming Corehole No. 1 in Sweetwater County, Wyo., to sample Green River Formation oil shale. Core obtained was assayed for oil yield to determine richness and stratigraphic distribution of oil shale in the deposit. Oil shale in place at Wyoming No. 1 site represents over 200 million barrels of oil per square mile. Additional data useful in evaluating the deposit, including generalized stratigraphy and mineralogy, detailed lithologic descriptions of the core, rock specific gravity, and bore-hole logs, are presented with the oil-yield data. The sampled Wyoming oil shale resembles Mahogany-zone oil shale in rock properties and gross mineralogy. A statistically derived equation relating shale density to oil yield for the Wyoming deposit compares with a similar relationship valid for the better known Mahogany-zone oil shales in Colorado and Utah. A density log from Wyoming Corehole No. 1 is calibrated for direct oil-yield logging. The alternating rich and lean beds of shale at this site may permit creating the permeability necessary for direct production of shale oil from the shale in place.

Jan 1, 1968

By Elbridge W. Gresseth

Rock deformational structures in a deep mine were analyzed by petrofabric techniques to learn (1) the relative magnitude and direction of the principal stresses involved in tectonic deformations prior to mining, (2) the preferred orientation of rock planar discontinuities which define rock anistropy prior to mining, and (3) the relationship of mining-induced rock failure to inherent rock stresses and inherent rock anisotropy. Rock fabric elements used for petrofabric analysis consisted of bedding planes, faults, joints, fractures, foliation, sericite plane (001), quartz axis [0001], quartz deformation lamellae, and microfractures. Structures and structural symmetries from different areas within the mine and from different scales of observation were compared to learn the nature of rock anisotropy and the orientation of the principal stresses defined by rock deformations. Analysis of such fabric as regional and macroscopic faults, b-c joints, quartz [0001], sericite (001), and microfractures, indicate that during the epochs of tectonic deformation, the maximum and minimum principal stresses were horizontally oriented and acted along northwest and northeast axes, respectively. This condition of regional stress appears to have continued during folding and the associated period of faulting. The most recent tectonic deformation represents a rotation of the minimum principal stresses into a vertical position, as shown by the development of a tensile joint system, quartz deformation lamellae, and microfractures. Good interscale correlation and statistical homogeneity of tectonic fabric indicate a stress field homogeneity in this area during tectonic deformation. Rock physical anisotropy is genetically associated with tectonic fabric and consists of preferentially oriented planar discontinuities intersecting along a nearly vertical axis. The mining-induced deformations were correlated with the inherent rock anisotropy which either directly controls or greatly affects their development. This phase of rock deformation shows a greater degree of stress field heterogeneity than was the case with tectonic deformations This is explained as a result of nonconfinement afforded by underground openings and the increase in ground stresses due to mining activity"

Jan 1, 1968

By J. E. Zeilinger

This Bureau of Mines report describes the preparation characteristics of the significant coalbeds of Clarion County, Pa. Of the 15 samples collected, 1 was of metallurgical quality as received, 4 could be sufficiently upgraded to provide acceptable products, and the remaining 10 samples could not be upgraded to metallurgical quality because their sulfur contents could not be lowered to meet the standard. For steam or power generation, 1 sample was of low sulfur content as received, 1 sample could be upgraded to low sulfur content, and 10 samples could be upgraded to medium sulfur content. The original sulfur content of the remaining three samples can be appreciably reduced by removal of the sink 1.58 specific gravity material; however, these coals would be classified as medium sulfur coals both before and after removal of the sink material.

Jan 1, 1968

By J. O. Winget

Amino acids were investigated in conjunction with rare-earth separation by ion exchange to determine whether they can be utilized effectively as retaining agents for metals separation using ethylenediaminetetraacetic acid (EDTA) eluant at 85° to 90° C. Hydroxyethylethylenediaminetriacetic acid (REDTA) and diethylenetriamine pentaacetic acid (DTPA) were the most effective amino acids investigated. Elements of atomic numbers 39 and 57 through 68 were effectively retained, whereas elements of atomic numbers 69 through 71 passed through the retaining-agent band. Utilization of REDTA or DTPA retaining agents allows an increase of 75 percent in the EDTA eluant concentration over that possible with hydrogen-or copper-retaining ions without precipitation occurring. Eighty-five percent recovery of the EDTA eluant collected before rare-earth breakthrough and during elution of lutetium, ytterbium, and thulium, and essentially complete recovery of the REDTA or DTPA retaining agents, are possible without extensive processing.

Jan 1, 1968

By Leland E. Paulson

This investigation examined the feasibility of altering the inorganic component of North Dakota lignite by ion exchange. Lignite of specific size consist was washed with various ionic solutions and examined for evidence of exchange. Ions of higher valance substituted preferentially at equivalent concentrations. Results indicate that a major portion of the inorganic material associated with lignite is combined in exchangeable form with the organic component. Particle size of the treated coal is a critical factor in determining the rate of exchange. The data indicate that monovalent ions are easily replaced by divalent and trivalent ions, and the presence of ionic material in slurries containing finely divided lignite significantly increases filtration rates.

Jan 1, 1968

By Robert M. Becker

A multistage probability model for assessing the reliability of mineral samples following any number of stages of sample reduction is presented. Sample reduction is the process of alternately crushing or grinding and sampling mineral particles prior to assaying. The final multistage model developed accurately describes the ideal sample reduction practice. This model is based on previously developed and experimentally tested models for a single stage of sampling. The problem is approached through the probability distributions for the various stages of sampling. The probability distribution, moments, and moment relationships for a single stage of sampling are first reviewed, and the useful concept of unit moments is defined. In presenting the models for two stages of sampling, emphasis is placed on the physical description of the sample reduction process which leads quite naturally to its mathematical representation. In this representation, crushing or particle-size reduction between the stages of sampling is viewed as a random process with respect to the number and proportion of particles of the various kinds produced. The physical and mathematical description is extended to more than two stages of sample reduction, and the first three moments for any number of stages are developed. In common sample reduction practice the effects of a finite population (finite amount of material) at each stage of sampling appear to be important in describing the variance contribution of each stage. This is also true for the third moment about the mean. An example is cited in which the skewness increases by more than an order of magnitude when several stages of sampling are considered. This is largely due to the dependence of the multistage third moment about the mean on the variance. In general the model and results should be useful in helping to understand, control, and reduce the random errors that arise in the sample reduction process.

Jan 1, 1968

By D. H. Chambers

Digestion studies were undertaken to develop a method for the rapid dissolution of high-temperature ferroalloy scrap. Laboratory tests showed: (1) dissolution of alloy scrap with ferric ion as the leaching agent was a moderately rapid method of digestion; (2) the dissolution process can be considered as a typical reaction of a metal with chlorine gas, although evidence was obtained to show dissolution as a two-step process, one step as the reduction of ferric ion by the soluble alloy constituents and the other as the oxidation of ferrous ion with chlorine gas; and (3) the attack of ferric ion on the alloy was a function of alloy composition, ferric to ferrous ion ratio, and area of contact between leach solution and alloy. The exceedingly complex nature of alloy compositions and dissolution products generally precluded satisfactory analytical determinations. Results of moderate accuracy were obtained using complex modifications of standard analytical and spectrographic techniques.

Jan 1, 1968

By R. W. Freedman

The gas chromatographic method, devised by the Bureau of Mines for analyzing routine mine air samples, was compared with the infrared method used for confirmatory determination of methane in mine air. While maintaining the specificity of the infrared method for methane determination, the gas chromatographic method is more precise, much more rapidly performed, and more convenient.

Jan 1, 1968