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By Daniel C. Boteler

Data from 68 entrained-bed carbonization tests were treated statistically by the Bureau of Mines, and several useful relationships were developed among the major variables. Nine coals, ranging in rank from lignite A to high-volatile A bituminous, were carbonized in two entrained-bed carbonization pilot plants. The carbonizing reactors employed were vertically mounted cylinders, internally heated, refractory-lined, and 10 inches ID. The range of carbonization temperatures was from 825° to 1,600° F. Using a regression-analysis computer program, empirical equations were developed by which carbonization temperature, air-to-coal ratio, devolatilization of coal, char yield, and volatile matter content of product char may be predicted.

Jan 1, 1973

By C. M. Frost

Crude shale oil produced during in situ retorting by the Bureau of Mines at Rock Springs, Wyo., was refined by three schemes. In the first, the crude oil was fractionated to raw naphtha and 400° F+ residuum. The residuum was hydrogenated over cobalt molybdate catalyst at 815° F and 1,100 psig. The blended raw and 160°-400° F hydrogenated naphthas were hydrodenitrified and then catalytically reformed. The 400° F+ hydrogenated oil was catalytically cracked. In the second scheme, the crude was hydrogenated over nickel-tungsten catalyst at 800° F and 1,500 psig. The hydrogenated fractions were processed by methods used in the first scheme. The third scheme resembled the second but, prior to hydrogenation, the crude was "hydrostabilized" over cobalt molybdate at 500° F and 500 psig. Yields of reformate and cat-cracked gasoline as volume-percents of the crude, and research-method octane numbers (with 3 ml TEL) for the three methods were as follows: First method, 32 pet reformate, 90 octane; 19.5 pct cracked gasoline, 99.2 octane. Second method, 29 pet reformate, 81.1 octane; 21.3 pct cracked gasoline, 99.6 octane. Third method, 28.2 pet reformate, 86 octane; 28.7 pct cracked gasoline, 95.9 octane.

Jan 1, 1974

By Fun-Den Wang

Finite-element structural analyses were performed to determine the stress distribution and displacements around a single rectangular coal mine opening in a multilayered rock system. The effects of changes in mechanical properties of roof and coal layers, roof layer and mine opening geometry, horizontal-to-vertical load ratio, and structural geologic features on the stress distribution about the opening were studied. Variability in the stiffness and relative thickness of the immediate roof layers can produce a considerable difference in the stress distribution about the opening as compared with that of a homogeneous material. Changes in opening width and horizontal-to-vertical load ratio have different effects on the stress distribution about the opening depending on the composition of the roof layers. In general, where a stiff layer exists in the roof at the surface of the opening, the stresses are higher in the roof and ribs around the opening. Horizontal changes in facies in the roof layers produced by structural geologic features can also greatly alter the stress distribution about the opening compared with the simple layered cases.

Jan 1, 1974

By Laxman S. Sundae

A Bureau of Mines investigation was conducted to determine the effect of specimen volume on the apparent tensile strength of disks of St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite. The investigation used a technique developed by the Bureau to determine apparent tensile strength. Because the test specimens were selected without macroscopic defects, that is, cracks, joints, and planes of weakness, the strength variations are solely due to microscopic features. Several replications of each test were performed. Data for each set of specimens were fitted to a power law of the form y = axb, where y = apparent tensile strength, x = specimen volume, and a and b are constants. This power law is essentially a form of Weibull's theory. The average coefficients of correlation for St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite were 0.85, 0.53, and 0.78, respecitvely. In all cases a decrease in strength with increasing volume was noted; in the extreme case, a decrease of 40 pct was noted with an elevenfold increase in volume. The decrease in strength with increasing specimen volume is explained in terms of Weibull's theory.

Jan 1, 1974

By L. A. Haas

In this Bureau of Mines investigation, conditions were determined to form an iron sulfide adherent coating with a metallic golden luster on steel upon anaerobic heat treatment with sulfur. The sulfide formation rate was determined in the temperature range of 105° to 500° C with reaction times up to 68 hours. The optimum temperature and time to form an adhering decorative coating on mild steel was in the range of 105° C for about 70 hours to 285° C for 1 hour. The golden coating consisted of an inner layer of pyrrhotite and an outer layer of pyrite. At temperatures higher than about 300° C, the outer layer thickness decreased owing to the decomposition of pyrite to pyrrhotite.. Small quantities (<0.5 wt-pct) of petroleum oil accelerated the sulfide growth rate. The sulfide coating decreased the corrosion rate of steel in a neutral aqueous medium by a factor of two. The dissolution of pyrite in water was dependent on particle size and surface area with the flat pyrite coatings exhibiting the lowest dissolution rate.

Jan 1, 1974

By J. B. Janus

In connection with the purchase of coal under specifications for Government use, the Bureau of Mines in this report has compiled data on 81 mines located in 15 States. This annual report lists analytical data on the composition and quality of tipple and delivered samples of coal collected during fiscal year 1973. Tipple samples were collected by Bureau of Mines engineers at tipples as coal was being loaded into railroad cars or trucks. Ultimate analyses are given for most of the coalbeds listed. The deliveries were sampled at destination in accordance with instructions issued by the Bureau of Mines. All samples were analyzed in the Bureau laboratory at Pittsburgh.

Jan 1, 1973

By R. P. Vinson, Abdurrahman Cetinbas, Joseph Cervik, M. G. Zabetakis

The periphery of longwall panels in the Pocahontas No. 3 coalbed is characterized by a zone of reduced permeability that inhibits the natural drainage of methane. A residual gas pressure of 105 psig was measured after 1 year in an isolated block of coal measuring 340 by 1,100 feet. The buildup of gas pressure within such large blocks causes methane problems during plowing operations. However, natural drainage holes drilled during development have been found to reduce the gas content of the coal in this coalbed by over 90 percent. The effect of water infusion on dust during plowing operations was investigated using existing methane drainage holes. These holes were cleaned of debris and a pipe was grouted into the hole for water infusion of the panel. Both total and respirable dust levels were reduced by 40 to 79 percent. Water infusion of the panel proved more effective than did the use of a plow-mounted spray sys tem.

Jan 1, 1974

By Abdurrahman Cetinbas

The periphery of longwall panels in the Pocahontas No.3 coalbed is characterized by a zone of reduced permeability that inhibits the natural drainage of methane. A residual gas pressure of 105 psig was measured after 1 year in an isolated block of coal measuring 340 by 1,100 feet. The buildup of gas pressure within such large blocks causes methane problems during plowing operations. However, natural drainage holes drilled during development have been found to reduce the gas content of the coal in this coalbed by over 90 percent. The effect of water infusion on dust during plowing operations was investigated using existing methane drainage holes. These holes were cleaned of debris and a pipe was grouted into the hole for water infusion of the panel. Both total and respirable dust levels were reduced by 40 to 79 percent. Water infusion of the panel proved more effective than did the use of a plow-mounted spray system.

Jan 1, 1974

By John R. M. Hill

The Bureau of Mines performed elastic-plastic, finite-element analyses to investigate the support performance of hydraulic backfill. A mathematical model was developed for two vertically adjacent stopes separated by a sill pillar. An exact duplicate of a working stope was not intended; however, the model did simulate a working stope to the extent that field measurements from an active stope could be used for comparative purposes. Using a predetermined mining sequence, the computer analysis simulated the mining operation as a series of incremental cut-and-fill steps. Computer results included a complete history of stope closure and pillar stresses throughout the mining sequence. With the mining sequence and rock properties held constant, three separate analyses were made using varying backfill properties. These cases included no fill,-low-to-medium-quality fill, and medium-to-high-quality fill. Results of these analyses show decreases in stope closure and pillar stresses as the backfill quality increases, thus reducing the possible occurrence of rock bursts. Predicted stresses within the backfill compare favorably with field measurements. A relationship between maximum stress normal to the stope wall and the ratio of relative fill stiffness to relative rock stiffness was also indicated.

Jan 1, 1974

By D. W. Richardson

This Bureau of Mines publication provides the enthalpy of formation of malachite [Cua(COs)(OH)2] as determined by hydrochloric acid solution calorimetry. At 298.15 K the enthalpy of formation from the component oxides is -15.l0±0.30 kcal/mole and from the elements, -251.9±0.5 kcal/mole.

Jan 1, 1974

By David L. Veith

Caustic scrubbing followed by silica flotation with cationic ether primary amine proved effective in upgrading commercial magnetic concentrates to supergrade products containing 2 percent SiO2, or less. Samples representing 41 million long tons per year of commercial magnetic concentrates from the Lake Superior region were tested by the Bureau of Mines. Bench-scale and pilot plant research indicated an estimated potential of 32 million long tons per year of superconcentrates to be available. Two pilot plant investigations yielded superconcentrates containing 1.1 and 1.9 percent SiO2 that were derived from commercial concentrates containing 7.0 and 4.2 percent SiO2, respectively. Corresponding iron recoveries were 90 and 93 percent at reagent costs of just over 33 cents per long ton of superconcentrates produced. Additional sources evaluated on a bench scale resulted in iron recoveries of 72 to 95 percent in products containing 1.7 to 2.0 percent Si02. Although reagent cost ranged up to 60 cents per long ton of superconcentrate, it is probable that these costs would be reduced in plant applications where benefits are derived from material and reagent recycle.

Jan 1, 1974

By Laurance L. Oden

The Bureau of Mines is developing melting data for binary combinations of the alkaline earth fluorides and yttria to facilitate the formulation of slag compositions. The present report deals with the SrF2-Y2O3 system for which liquidus and solidus temperatures and solid solubilities were determined. The information is presented as the phase diagram. The phase diagram was constructed from information obtained by ceramogra¬phy, X-ray diffraction, thermal analysis, and electron probe microanalysis of small specimens encapsulated in platinum-20 percent rhodium or molybdenum ampoules. The data indicate a simple eutectic system with limited terminal solid solubilities. The eutectic temperature is 1,457°±5° C, and the eutectic composition is 4±1 mole-pct Y203. Strontium fluoride containing up to 2 wt-pct 0 2 was studied to determine the effects of oxygen contamination. Oxygen levels in excess of 0.2 wt-pct resulted in eutectic formation between SrF2 and SrO. The eutectic composition is between 0.2 and 0.7 wt-pct 02, and the eutectic temperature is 1,447°±5° C. No intermediate oxyfluoride phases were detected.

Jan 1, 1974

By C. C. Hwang

The Bureau of Mines formulated a method for calculating the concentration of entrained dust from a dust deposit by a turbulent gas stream. In particular, a diffusion equation is used to calculate dust concentrations in a channel following an explosion. Dust leaving the channel walls was treated as originating from stationary or moving, and single or multiple material sources. Formulas and sample computations for various types of dust sources in circular and rectangular channels are given, based on experimental entrainment rates. The analysis predicts the dust concentration as a function of time and channel space. The results appear to agree with the physical characteristics of explosion-driven dust dispersion in a O.6-m-diameter, 50-m-long explosion tunnel. The analysis is also applied to simultaneous and consecutive dispersion of coal and rock dust from simulated coal mine surfaces (walls, floor, roof, and ribs).

Jan 1, 1974

By Thomas O. Meyer

Laboratory test results are presented for the determination of elastic modulus made with the NX borehole jack. Determinations were made in massive pieces of aluminum so as to satisfy conditions of linear elasticity, homogeneity, and isotropy. Results indicate a large discrepancy (approximately 200 percent) betwen material modulus as determined by laboratory block-loading tests and that indicated by the jack under relatively ideal circumstances. Effects due to interface friction, finite block size, incomplete plate-bore contact, and other factors were examined and found not to be significant. Finite element results indicate that assumed loading conditions for the jack differ from those actually occurring, at least in materials of high elastic modulus (approximately 10 million psi), such as quartzite.

Jan 1, 1974

By P. G. Pigott

This investigation by the Bureau of Mines demonstrated that building bricks can be produced by the steam-curing process from various types of industrial mineral wastes. Wastes, utilized to produce bricks, consisted of copper mill tailings, roofing granule fines, asbestos fines, and zinc mill tailings. Bonding of the wastes with either Ca(OH)2 or portland cement resulted in building bricks that met ASTM specification C73-67 for grade SW and MW bricks when evaluated in accordance with ASTM designation C67-66 on sampling and testing of brick. An economic evaluation of the process indicates the total operating cost per 1,000 bricks is about $36.

Jan 1, 1974

By G. J. Conroy

This Bureau of Mines study was initiated to determine whether or not a large-scale investigation of 400-Hz applications in coal mines was justified as a means of increasing safety in operations due to size and weight reductions in portable and other mining machinery. Potential uses for 400-Hz power in mining operations are explored, and cost and size comparisons with 60-Hz systems are made. The use of variable-frequency motor drive is suggested for conveyors. The conclusion was reached that there is no significant potential safety increase due to a general size and weight reduction, as the fact of such general reduction cannot be demonstrated.

Jan 1, 1974

By George A. Savanick

Coal mine roof shales fracture preferentially at slickensided surfaces because of weak or nonexistent adhesion between two slickensided rock surfaces. The purpose of this Bureau of Mines research was to characterize chemically the thin film of smooth, glossy material that makes up the slickenside. This material was analyzed by electron spectroscopy and ion scattering spectrometry while in place on the rock surface and by standard methods of quantitative chemical analysis on concentrate removed from the rock. These analyses showed that the chemistry and mineralogy of the slickensides are similar to that of the adjacent shale.

Jan 1, 1974

By H. B. Carroll

The Bureau of Mines has designed and built a controlled-environment test chamber specifically for instrument evaluation in simulated work atmospheres. The atmosphere inside the 300-liter stainless steel chamber can be controlled at any selected temperature and relative humidity in the range of 2° to 93° C and 20 to 95 percent, respectively. Instruments placed inside the test chamber are subjected to an atmosphere at a preset temperature and humidity containing various concentrations of toxic gases such as CO, C02, NO, NO2, S02, and H2S. Toxic gas losses resulting from wall reactions, monitoring instruments, and instruments under evaluation are compensated by the use of a dynamic gas blending system.

Jan 1, 1973

By Edward L. Burwell

The Bureau of Mines conducted laboratory experiments to determine the change during retorting in the apparent permeability and the degree of compaction of beds of broken oil shale. Grades of oil shale studied ranged from 20.6 to 46.7 gallons of oil per ton (gpt), and the simulated overburden pressures applied to the shale were from 300 to 900 psi. Linear regression analysis of the data produced equations describing the response of the oil shale. Oil shales of approximately 20 gpt experience only minor apparent permeability reductions under test conditions, but richer shales (30 to 50 gpt) lose essentially all permeability. The permeability reductions were accompanied by corresponding decreases in bed height that ranged up to 37 percent of the original bed height.

Jan 1, 1974

By Gordon E. Fletcher

This Bureau of Mines report outlines the atomic absorption analysis of oilfield brines for barium, calcium, copper, iron, lead lithium, magnesium, manganese, potassium, sodium, strontium, and zinc, using the method of additions. The advantages of using atomic absorption are discussed. The method of additions was chosen to overcome large matrix interferences usually found in brines; techniques of overcoming chemical, ionization, and background interferences are also described. The method was used to analyze several hundred oilfield brines and found to be rapid and reasonably accurate. A solvent extraction method was used to concentrate lead, copper, zinc, and iron in low-level samples.

Jan 1, 1974