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By J. M. Stuve

Low-temperature heat capacities and the enthalpy of formation were deter-mined calorimetrically by the Bureau of Mines for CuO?CuS04. The derived standard entropy (S°298.15) was 40.36±0.04 cal/deg-mole, and the enthalpy of formation (?H°f) was -219.l±0.3 kcal/g-mole. A large thermal anomaly was observed in the heat capacity of CuO?CuS04 at 20±0.1 K. Gibbs energy of formation data are tabulated up to 1,200 K. Construction details of a precision low-temperature adiabatic calorimeter capable of determining heat capacities of solids in the temperature range 5 to 320 K are given. A calibrated miniature germanium resistance thermometer was incorporated into the calorimeter to extend the range of accurate measurements below 15 K. High-resistance dc heater windings were used throughout the cryostat to reduce heat conduction of inner connecting wires.

Jan 1, 1975

By C. O. Hawk

Distillable oils derived from coal were desulfurized and hydrogenated at 2,500 psig in a two-step vapor-phase catalytic operation to give a product rich in saturated cyclic hydrocarbons. The first step was mainly a desulfurization at 400 C, the second a saturation at 300 C. One of the oils used as feed stock was from low-temperature carbonization of a bituminous coal, the other was from the liquid-phase hydrogenation of coal in the Bureau's pilot plant. The product from the saturation step was distilled to remove the light ends and high-boiling residue and to recover a fraction having acceptable properties with respect to heating value, density, freezing point, viscosity, and boiling range according to specifications suggested by the Air Force for ultra-high-speed aircraft fuel. Quantities of the fuel fraction available were too small for the thermal stability test approved by the Air Force. The experiments, performed on laboratory scale, comprised mostly a study of the effect of varying the oil feed rate (at constant oil-to-hydrogen ratio) on the yield of the desired fuel fraction. The yield of the fuel fraction made from low-temperature carbonization oil was a little more than 1 percent of the weight of coal carbonized; that from coal-hydrogenation oil was about 12 percent of the weight of coal hydrogenated. A few attempts to do both desulfurization and saturation in one operation with sulfur resistant catalysts, developed for vapor-phase hydrogenation or hydroforming, were unsuccessful. By leaving the low-boiling ends in both feed stocks to desulfurization, another product was obtained: a low-sulfur aromatic cut boiling below 200 C. This material would be suitable as a solvent or a chemical raw material.

Jan 1, 1965

By D. Bienstock

Using a nitrided fused-iron catalyst, the Bureau of Mines investigated the Fischer-Tropsch reaction in the oil-circulation process. The nitrided iron was quite stable and permitted the longest run obtained thus far in the oil-circulation process without the need for reactivating the catalyst--3,700 hours of operation. The effects of several operating variables--temperature, pressure, gas-recycle ratio, space velocity, synthesis-gas composition, and synthesis with and without reflux of oil to the reactor--on the production of oxygenates were studied. The importance of removing reflux oil and of high gas recycle in increasing the oxygenate content was shown. A finished gasoline containing 28 percent by weight alcohols was produced. The research octane number (RON) was 92.9 clear, increasing to 98.5 with the addition of one milliliter of tetraethyl lead (TEL). INTRODUCTION The Federal Bureau of Mines has been engaged since 1944 in a research and development program on the synthesis of gasoline from coal. Gasification of coal with steam and oxygen to yield a "synthesis gas"--a mixture of carbon monoxide and hydrogen--is being investigated at Morgantown, W. Va., and the synthesis of gasoline by catalytically reacting carbon monoxide and hydrogen over iron by the Fischer-Tropsch reaction is being investigated at Bruceton, Pa.

Jan 1, 1960

By Gerald T. Homce

A system capable of monitoring a mine electrical power system to detect incipient electrical component failure could significantly improve power system safety and availability. The U.S. Bureau of Mines funded a contract with The Pennsylvania State University (Penn State) to establish the theoretical and technical framework for such a system. This report briefly outlines the contract, reviewing related Bureau and Penn State work prior to its award, and describes support work carried out by the Bureau. The main focus of the report is on research efforts by Penn State and subsequent results. An existing algorithm for incipient-failure detection and classification was studied, and recommendations are made to improve its performance. In addition, mathematical models of cable-connected motor systems and deteriorating motors were developed and implemented on computers. These models and laboratory tests were used to study and document relationships between component deterioration and electrical terminal effects. The project was supported by the U.S. Navy and the nature of its interest in the application of failure prediction techniques is also included.

Jan 1, 1989

By B. J. Moore

This publication contains routine analyses and related source data for 278 natural gas samples from 14 States. All of the samples were collected during calendar year 1973 as part of a continuous survey of the free world for occurrences of helium in natural gas. This survey has been conducted in the United States by the Bureau of Mines since 1917. In late 1965, the survey was expanded to include foreign gasfields. The analyses published herein were made by mass spectrometer and a special helium analysis apparatus, which are described in Bureau of Mines Bulletins 4862 and 576.3 Fifteen previous publications have presented the results of 10,201 gas analyses prior to 1973. The first three, Bulletins 486,4 576,6 and 617,6 contain analyses and related source data on 5,218 gas samples collected from 1917 through 1960. The other 12 publications,7 which were issued as information circulars, supplement the three bulletins and contain 4,983 analyses of samples collected since 1960. This publication is the 13th publication supplementing the three bulletins.

Jan 1, 1974

By Kenneth G. Broadhead

The objective of this rare-earth oxalate study by the Bureau of Mines was to determine systematically by radiochemical techniques what effects, if any, could be attributed to the several variables--temperature, digestion time, acid concentration, rare-earth concentration, oxalic acid concentration, stirring, and the presence of other rare-earth ions. A Latin Square experimental design was used to evaluate statistically some of the variables. Precipitation losses ranged from near zero to about 7 percent, and mineral acid and rare-earth concentration were the predominant factors affecting completeness of precipitation. Quantitative oxalate precipitation of the rare-earth elements was achieved by controlling the experimental conditions as follows: (1) Maintaining rare-earth concentrations above 0.01M; (2) stirring the mixture several minutes after precipitation; (3) using an adequate (two to five-fold) excess of oxalic acid; (4) precipitating at room or iced temperature and digesting for at least 1 hour; (5) avoiding an excess of mineral acid and, if possible, maintaining the pH above 2.0; and (6) avoiding excess complexing agents such as EDTA (ethylenediaminetetraacetic acid). In the past 20 years research aimed at developing more efficient separation and purification techniques applicable to the rare-earth elements and yttrium has been extensive. Common to most of these procedures has been the use of oxalic acid to precipitate this group of elements selectively. However, this particular use of oxalic acid has a much earlier origin; its application in precipitating yttrium was first reported by Mosander (8)4 in 1843. Despite long and popular employment of this technique, only limited and somewhat conflicting data are available regarding the many factors affecting the degree of rare-earth oxalate precipitations.

Jan 1, 1961

By Charles V. Jude

This U.S. Bureau of Mines report presents a review and evaluation of existing and new backfilling materials and methods for their applicability to the problem of gate road stress reduction in deep retreat longwall coal mines. Candidate backfill materials include pulverized coal combustion fly ash, flue gas desulfurization, and fluidized bed combustion by-products from coal-fired electric power generation plants. Properties of both backfill and its component materials are presented, with particular emphasis on the unconfined compressive strength and elastic modulus of backfill mixtures. Hydraulic mix designs discussed in this report include high-water content slurry and low-water content paste fills. Three gate road stress-transfer-modification concepts are proposed to reduce abutment stresses in gate road systems. The first concept, packwalling, involves packwall construction behind the headgate shield inby the face and adjacent to the headgate pillars. The second concept, gob-filling, involves infilling a strip of gob inset from and parallel to the headgate using paste injection methods patterned after a technology recently developed in Europe. In the third concept, entry-filling, slurry fill methods are used to fill abandoned gate roads and crosscut entries inby the face.

Jan 1, 1995

By C. N. Adams

The purpose of this investigation was to evaluate the physical and mechanical properties of high-purity titanium made by two processes. Sodium-reduced metal with 58 Brinell hardness number (B.h.n.) and electrorefined metal with 60 B.h.n. and 70 B.h.n. were used. Titanium of these hardness levels did not work-harden excessively, and beyond 40 percent cold work the hardening effect was not great. Rapid softening occurred when the metal was annealed at temperature between 300° and 600° C. Full annealing, as determined by property and microstructure studies, was accomplished after 30 minutes at 700° C. A recrystallization diagram is presented which is based on determinations of annealed grain size as a function of rolling reduction and annealing time. For reductions of less than 20 percent, exaggerated grain growth occurred during annealing; for reductions greater than 20 percent, the variation in grain size for each annealing temperature was minor.

Jan 1, 1961

By John W. Buch

This is the first progress report to be released on the anthracite, mechanical mining research and engineering development program of the Bureau of Mines. This phase of Bureau work, which was initiated as an aid to stimulating wartime production of anthracite, has been continued after the war to assist primarily in improving the general economic position of the anthracite industry. Field work was started in. the 1945 fiscal year with the cooperation of an advisory committee representing management, labor, and the Commonwealth of Pennsylvania. For a beginning, several matters were suggested by members of this advisory committee as being worthy of investigation, and sections of underground mines yore offered for test purposes. Among the suggestions accepted for investigation was the problem of increasing the rate of advance for driving gangways in thin, steeply pitching anthracite beds 4 to 6 feet thick and pitching 60 degrees or more. The problem was undertaken as a field study, and this report relates to accomplishments on this project to June 30, 1947.

Jan 1, 1949

By Charles Vaught

The U.S. Bureau of Mines evaluated the self-contained self-rescuer (SCSR) donning proficiency of 243 miners. These workers were from eight underground coal mines in the eastern United States. The objectives of the study were (1) to gather information on skill levels, since all miners in the study had prior instruction and opportunity to practice donning the apparatus, and (2) to summarize a quality control procedure useful in conducting periodic evaluations of donning proficiency. The sampling procedure used proved to be both reasonable and efficient in gathering information on training effectiveness_ It also provided a good statistical base for making informed site-specific decisions regarding SCSR training needs. Results from the observed samples at each of the eight mines indicate a wide variability across sites. The rate at which miners failed to isolate their lungs varied from 33 to 40.0 pct. Concomitantly, proficiency rates (miners either performing adequately or demonstrating a perfect 3+3 sequence) ranged from 13.3 to 63.3 pct.

Jan 1, 1991

By Jack Mantel

The goal of this 42-month contract was to increase safety in low-seam underground coal mines through development and in-mine evaluation of a temporary roof support system for roof drills and floor-riding operator compartments for a loader and shuttle car. The program was performed in three phases. During Phase I, state-of-the-art canopy technology was investigated, and preliminary design and mock-up evaluations were performed for temporary roof supports for single-and dual-boom bolters and for transverse-mounted floor-riding canopies for a shuttle car and coal loading machine. The shuttle car and loader canopies were approved for further development, and the design, fabrication, testing, and certification were completed in Phase II. In Phase III, the Bureau of Mines furnished an FMC 6L shuttle car fur use in the evaluation of the canopy for 45 shifts. The shuttle car canopy was evaluated at Virginia Crews Coal Company in West Virginia. Efforts to secure an evaluation site for the loader canopy were unsuccessful. The loader canopy was shipped to Bruceton for possible future evaluation.

Jan 1, 1985

By R. V. Lundquist

Aeration in water slurries and controlled drying of manganous hydroxide produced from dithionate leaching of Artillery Peak manganese ores from Arizona were investigated by the Bureau of Mines at its Electrometallurgical Experiment Station, Boulder City, Nev., to determine whether a simple process could be developed for converting this product into a battery-grade manganese dioxide. The properties of manganese dioxide prepared by the thermal decomposition of manganous nitrate were investigated also. Manganese dioxide suitable for use in batteries was not obtained from the dithionate leach product, but some of the factors controlling its oxidation were isolated. Aging of manganous hydroxide was of major importance in retarding its oxidation by aeration. Sodium hydroxide and sodium silicate promoted oxidation by drying. Optimum quantities were about 0.85 mol of sodium hydroxide and 0.2 mol of sodium silicate per mol of manganese, and drying temperatures of 200° C. produced yields of manganese dioxide up to 90 percent of the manganese present. Higher temperatures and concentrations of reagents carried oxidation of manganese beyond its tetravalent state.

Jan 1, 1957

By Hillary W. St. Clair

This report describes an experimental method for determining parameters for the rate of reaction of CO2 with solid carbon. The method involves the simulation of a flow reactor by a mathematical model based on a hypothetical multistage reactor which permits calculation of the analyses of effluent gas and carbon consumed as functions of the flow rate and duration of the reaction. The method is applied to experimental data on the reaction of coke with CO2 in fluidized-bed and fixed-bed flow reactors. A method is described whereby two parameters may be determined simultaneously. The method involves a reiterative procedure that finds the values of the parameters that minimize the sum of squares of deviation between calculated and observed analyses of the effluent gas.

Jan 1, 1971

By A. B. Needham

Graphite is a raw .material of considerable importance in both waxy and peace. Two types of graphite, classified according to particle size as flake and fines, are used, but the former is in much greater demand. The principal wartime use of graphite is in the manufacture of crucibles for melting brass and special alloys of copper and steel. Other uses in both peace and war are as lubricants, for foundry facings, and in paints, electrodes, batteries, motor and generator brushes, and a variety of other commodities. . This paper describes the operations of the Southwestern Graphite Co. of Los Angeles, Calif., which produces both flake and fine graphite from a property in Burnet County, Tex.

Jan 1, 1946

By C. J. Walker

The Bureau of Mines undertook a theoretical and laboratory study to determine the feasibility of using ethylene as a tracer for natural gas in underground gas-storage reservoirs. The study indicated that ethylene was a useful gas tracer in underground gas storages. Tracer losses were not excessive. Laboratory tests were conducted at pressures as high as 500 psia in both wet and dry consolidated-sandstone cores, evaluating tracer loss with gas blends containing natural gas with different concentrations of ethylene tracer. Under certain conditions losses were less than 17 percent.

Jan 1, 1966

By W. S. Wright, A. W. Tolonen

"INTRODUCTION The Mount Andrew iron deposit on Kasaan Peninsula, Prince of Wales Island, Southeastern Alaska, was examined in August 1942 by an engineer 4/ of the Bureau of Mines accompanied by geologists 5/ of the Federal Geological Survey. From October 20 to 27, 1942, two engineers 6/ of the Bureau of Mines made a further preliminary examination and took three large samples of magnetite and magnetite-copper ore for metallurgical testing. During the stunner of 1942 an investigation of the Mount Andrew-Stevenson-Mamie area, including topographic and geologic mapping and a magnetic survey, was made by geologist 7/ the Federal Geologically Survey. On May 31 and June 2, 1943, two Bureau of Mines engineers 8/ conducted a preliminary examination in which special attention was directed to trails, camp, and drill sites. They were accompanied on May 31 by L. A. Warner of the Geological Survey.During the period from September 1943 through September 1944 Bureau of Mines engineers 9/ completed a thorough investigation which included trenching, core drilling, and sampling. A Federal Geological Survey representative 10/ examined all trenches and cores for geological data.LOCATION AND ACCESSIBILITYThe deposit is situated at latitude 55º 31' N. and longitude 132º 18' W. on the north side of Kasaan Bay on Prince of Wales Island, Southeastern Alaska. The general location is shown on figures 1 and 2. The deposit is 5 miles southwest of the village of Kasaan and by water, 27 miles northwest of Ketchikan; the main tunnel portal is 7/8 mile north of the Mount Andrew landing on Kassan Bay."

Nov 1, 1947

By K. Zipf, Z. T. Bieniawski

"An extensive mixed-mode fracture toughness testing programme was conducted on coal from three coal fields. A special mixed-mode testing fixture for coal and other geologic materials was developed together with reliable specimen preparation procedures. Dynamic modulus measurements made on each of the 116 fracture toughness specimens showed that these coals exhibit certain degrees of anisotropy. The fracture toughness testing programme systematically varied the loading rate, specimen orientation and fracture loading mode. Loading rate did not significantly effect the fracture toughness over the quasi-static range tested. Orientation did have a significant effect on measured fracture toughness. In the coals tested, the divider orientation and arrester orientation had higher fracture toughness than the short transverse orientation. Data showed that one orientation could have almost twice the fracture toughness as another. The fracture toughness testing enabled certain evaluations of three mixed-mode fracture theories: maximum tangential stress, maximum energy release rate and strain energy density theory. Due to the extreme heterogeneity of the coals tested, definitive conclusions regarding the best mixed-mode fracture theory are not possible; however, data do tend to support the strain energy density theory. INTRODUCTIONThe major aim of this research is to ·develop a fundamental understanding of how fine· fragments of coal (respirable dust) are generated during a fracture process. In a related paper [l], a hypothesis was presented for the mechanism of fine fragment formation during a generic coal material/cutting tool interaction. In this hypothesis, fine fragments are created during coal material/cutting tool interactions that are best described as general mixed-mode fracture processes. Data are required on the mixed-mode fracture behaviour of coal, the physical character of the newly-created fracture surfaces and the character of the inherent flaw structure of the coal material. Accordingly, a test programme was designed that provided some information in each of these areas. The testing effort seeks to measure critical fracture toughness under mixed-mode loadings as a material parameter characterizing in part the tendency of various coals to generate undesirable quantities of fines and respirable dust."

Jan 1, 1990

By Arne Landsberg

A study of the chlorination kinetics of germanium, silicon, iron, tungsten, molybdenum, columbium, and tantalum has been made to determine the effects of temperature, chlorine concentration, geometric surface area and gamma radiation. The reaction products were volatile at the temperatures used this making it possible to follow the reaction rates by weight loss of the solid. Chlorination rates of germanium, silicon, and iron were found to be directly proportional to chlorine concentration while the rates for tungsten, molybdenum, columbium, and tantalum were proportional to the 0.5 to 0.6 power of chlorine concentration. A good correlation of reaction rate and geometric surface areas was not obtained because the true surface area of the samples could not be measured. Intense gamma radiation had no effect on reaction rates. The Arrhenius activation energies determined over the temperatures used are as follows: Germanium, 27 kcal/mole (233°-241° C); silicon 33 kcaL/mole (375°-517° C); iron, cold rolled, 20 kcal/mGle (259°-325° C) annealed, 21 kcal/mole (293°-337° C); tungsten, 43 kcal/mole (617-776° C); molybdenum, 37 kcal/mole (445°-4910 C); columbium) 34 kcal/mole (229°?255° C); and tantalum, 29 kcal/mole (370°-449° C).

Jan 1, 1965

By Steven J. Page

The Bureau of Mines used fiber-laden air to test two identical fibrous aerosol monitors (FAM) in order to establish the FAM-optical count correlation. The FAM is a unique instrument developed by GCA Corp. (GCA) to measure real-time fibrous aerosol concentrations. It will also respond to particulates that have sufficient shape irregularities to possess fiber characteristics such as the 3:1 length: diameter (L:D) aspect ratio. Results of the Bureau's laboratory tests showed that the FAM response is linearly correlated to concentration data obtained using the optical membrane filter count technique approved by the National Institute for Occupational Safety and Health (NIOSH), U.S. Department of Health, Education, and Welfare. A plot of the FAM-optical count correlation showed that FAM concentration readings are generally well within ±25 pct of the optical membrane filter count. Initial tests to estimate the best ratio control setting of the FAM for 5-µm fiber-length discrimination were performed using one instrument only (the ratio control setting determines the minimum threshold fiber length that will be detected by the FAM). The estimated setting was then used to correlate both FAM units. The result was a 65 pct difference in correlation between the two units. It appears that the major factor responsible for this difference was the internal adjustment of the photomultiplier detector sensitivity for each of the two FAM units.

Jan 1, 1980

By J. H. Tylczak

The Bureau of Mines studied the effect of alloy additions on abrasive wear of low-alloy steels. A dry-sand, rubber-wheel abrasion test appa-ratus using ASTM G65-Sl procedure B was used for the abrasive wear tests. Eighty-six material heat-treatment combinations were abrasion tested. Results of these tests were analyzed statistically using regression analysis to see if additions of Cr, Mn, Mo, Ni, Si, AI, Cu, and S were significant in affecting the abrasive wear rate of low-alloy steels. Regression analysis was also used to confirm hardness and C affect on the abrasive wear rate of these steels. It was found that for all the steels taken as a group, increased amounts of Mn significantly reduced the wear rate, while increased amounts of Mo and S1 increased the wear rate. Analysis also confirmed previous research done by others, that increasing hardness and amounts of C reduced the wear rate. For the hardened steels taken as a class, only increasing amounts of C and Mn reduced the wear rate, while increases in Si increased the wear rate. In the class of unhardened steels, increases in C, Mn, and S re-duced the wear rate, whereas increases in Mo increased the wear rate. The steels with the best resistance to wear were two hardened experimen-tal steels similar to AISI 1055 and AISI 107S.

Jan 1, 1986