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By W. E. Robinson

Differences in the composition or chemical structure of the organic material in samples of Uinta Basin (Utah) oil shale were studied relative to stratigraphic position within the Green River Formation. This involved a systematic study of the soluble organic material and the insoluble organic material (kerogen) present in the samples. Emphasis was placed upon the distribution of the alkanes (normal and isoprenoid compounds) in the soluble extracts and upon the aromaticity of the kerogen. Significant differences exist in the chemical composition of the organic material from various strata within the Uinta Basin, some of which were related to burial depth but most were related to source material variations, environmental differences, or other factors. The Uinta Basin samples differed significantly from Piceance Creek Basin and Green River Basin samples in the large amount of soluble extract they contained.

Jan 1, 1975

By Larry P. Jackson

As part of the current research effort in shale-oil chemistry conducted by the Federal Bureau of Mines, reduced chlorophyllins were prepared and pyrolyzed in an effort to identify the role of plant pigments and their decomposition products in the nitrogenous compounds found in the product of oil-shale pyrolysis. The properties of the chlorophyllin pyrolysates were related to the composition of the reduced chlorophyllins with particular emphasis on the amount and types of nitrogen compounds formed. A comparison based on the types of nitrogen compounds present was made betvJeen shale oil and the chlorophyll in pyrolsates. In order to make this comparison, a sample of shale-oil light distillate was separated into polar and nonpolar fractions, and a careful examination of the polar fraction was conducted to obtain an accurate picture of the types of nitrogen compounds present. The information gathered from these studies was used to evaluate reduced chlorophyllin as a model of oil-shale kerogen insofar as the production of nitrogen compounds was concerned. The results indicate that the reduced chlorophyllin does yield nitrogen products which are directly related to the nitrogenous compounds in shale oil, and it therefore represents a good model of shale-oil kerogen.

Jan 1, 1975

By John F. Papp

The Bureau of Mines has sampled microstructure of low-pressure flat flames by mass spectrometer for normal methane-oxygen-argon and for methane-oxygen-argon-bromotrifluoromethane flames. The physical and chemical phenomena, and the method of analysis of mole fraction data to evaluate net reaction rates are here considered in detail. Included is a computer program listing with output on one flame. Chemical species considered are CH4 , CO, CO2, H, H20, OH, Ar, H2, O2 , O, H2CO, CH3 , CF3Br, HF, HBr, Br, CH3Br, HCO, F2CO, CH2 CF2 , H02.

Jan 1, 1975

By Patrick J. Cain

The fatigue-failure characteristics under high-frequency (10 KHz) cyclic loading were determined for a marble, granite, and quartzite. The rock speci-mens were cyclicly loaded (using a high-power piezoelectric sonic transducer) at a constant strain amplitude generated by forming a longitudinal standing stress (strain) wave in the cylindrical test specimen. The number of load cycles required to fail each rock type at a given strain amplitude was deter-mined. The fatigue fractures were tensile in nature and the fracture load amplitudes were as low as 30 pct of the static tensile strength. Also the internal heating of the rock caused by the material damping (internal friction) was measured. The damping and internal heat generation in the specimens was analyzed to show that nearly all of the power input can be accounted for as a change in enthalpy in the specimen. Using these results the thermal strain in the rock was calculated to evaluate its contribution to fatigue failure. The thermal strain was found to range up to 30 pct of the dynamic strain amplitude depending on the load amplitude and the number of load cycles. The specific energy required for failure was determined and possible applications of the high-frequency fatigue fragmentation process are discussed.

Jan 1, 1975

By P. R. Tisot

The structural response of propped oil shale fractures was determined for each of two different grades of Green River oil shales (38.0 and 29.0 gpt) as they were heated in an inert atmosphere from ambient to subretorting temperatures (below those required for rapid pyrolysis of the organic matter). Small oil shale cores were propped apart by 3-mm glass beads to simulate a small cross section of a propped oil shale fracture between an injection and a producing well. These specimens were then heated at a uniform bate up to 800° F in a specially designed test cell under stress levels from 100 to 1,000 psi in biaxial and in triaxial confinement. Under the conditions of heat and compressive stress utilized in this study, all of the propped fractures in the two oil shales underwent structural deformation ranging from partial to complete collapse, as evidenced by proppant embedment. Structural collapse of induced fractures would in turn result in serious impairment or complete loss of the fracture flow capacities of the specimens. Results from this Bureau of Mines study indicate that underground retorting of Green River oil shale may be seriously impaired by loss of permeability when utilizing propped fractures in oil shales assaying more than 28 gpt.

Jan 1, 1975

By P. W. Jeran, C. D. Sullivan, C. M. McCulloch

A series of geological surveys were completed in six coal mines in connection with a Bureau of Mines research program on methane control. The aim of these surveys was twofold: First, to study the overall geology of the coalbed, and second to use the resulting data to evaluate the influence of the geological characteristics of the coalbed on safe and efficient coal extraction. This report explains the advantages of geologic maps and fence diagrams in coal mining, and how the knowledge gained from such geologic investigations of mines can help control many underground problems.

Jan 1, 1975

By C. M. McCulloch

A series of geological surveys were completed in six coal mines in connection with a Bureau of Mines research program on methane control. The aim of these surveys was twofold: First, to study the overall geology of the coalbed, and second to use the resulting data to evaluate the influence of the geological characteristics of the coalbed on safe and efficient coal extraction. This report explains the advantages of geologic maps and fence diagrams in coal mining, and how the knowledge gained from such geologic investigations of mines can help control many underground problems.

Jan 1, 1975

By B. Dimitriades

The Bureau of Mines measured the reactivities of 19 hydrocarbons known to be prominently present in automotive exhaust and ambient air in a smog chamber. Results agreed well with those obtained using two other smog chambers. Reactivity scales were developed for hydrocarbons and aldehydes using the results of this work and those of a previous study. Application of the reactivity scales to automotive exhaust samples gave fair agreement between predicted and observed rate-of-N02-formation values; however, predicted and observed ozone yields were neither in agreement nor did they correlate well. This lack of correlation for ozone yield was attributed to the inappropriateness of (1) the individual component reactivity data, (2) the reactivity classification scheme used, and (3) the linear summation method. In seeking to understand this problem and to develop more appropriate reactivity scales, the data were examined from a reaction mechanism standpoint, and further studies were suggested.

Jan 1, 1975

By C. A. Wilson

The Bureau of Mines started a continuing program to investigate and evaluate analytical techniques to assist governmental agencies to select simple, rapid, reliable methods for crude oil spill identification. Six crude oil samples were analyzed to evaluate gas-liquid chromatography, atomic absorption spectrophotometry, infrared spectoscopy, sulfur and nitrogren determinations, mass spectrometry, nuclear magnetic resonance spectroscopy, and ultraviolet spectrophotometry. Samples were studied from the following selected fields: El Morgan, Egypt; Duri, Indonesia; Minagish, Kuwait; Bachaquero, Venezuela; Gach Saran, Iran; and Prudhoe Bay, Alaska. These samples were chosen to represent high-production fields that are likely to be involved in oceanic transport. Over 50 years of Bureau of Mines analytical research on petroleum served as the basis for evaluation of the experimental results to determine which of the methods are effective techniques to identify crude oil spills. Gas-liquid chromatographic analysis, atomic absorption spectrophotometric analysis, and sulfur-nitrogen determinations are recommended as the most useful of the techniques investigated.

Jan 1, 1975

By Maurice Deul, Herbert H. Fields, John H. Perry

The Bureau of Mines has been promoting health and safety in mining since its establishment in 1910. One area of research covers methane control in coalbeds; this report describes a multipurpose borehole used for both degasification and the production of commercial-quality gas. The multipurpose borehole was drilled into a barrier pillar, and seven horizontal degasification holes and one pressure point hole were drilled radially out from its perimeter. On January 28, 1974, after 505 days of degasification, a compressor was installed to the exhaust stack of the multipurpose borehole (2), and pipeline--quality gas was introduced into a commercial pipeline. As of February 4, 1975, over 171 million cubic feet of gas had been purchased by the gas company. The in situ pressure at a depth of 200 feet into the coalbed and the average gas flow and water flow from the degasification holes as they were completed and closed off were 203 psig, 1,200,000 cfd, and 6.8 gpm, respectively. Twenty-four hours after the seven holes were connected through individual pipes to the atmosphere, the total gas and water flows and the in situ pressure dropped, respectively, to 971,000 cfd, 1.3 gpm, and 18 psig. Five hundred days later, the corresponding values were 620,000 cfd, 0.15 gpm, and 10.5 psig. Daily flows have been as high as 800,000 cfd, and as low as 360,000 cfd, during the last 500 days. On February 4, 1975, after 882 days of degasification, 576 million cubic feet of gas had been removed from the Pittsburgh coalbed; apparently a much larger area of virgin coal is being degasified than is defined by the holes. This study indicates that horizontal boreholes drilled into a coalbed from the bottom of any shaft will effectively remove gas from the Pittsburgh coalbed.

Jan 1, 1975

By Herbert H. Fields

The Bureau of Mines has been promoting health and safety in mining since its establishment in 1910. One area of research covers methane control in coalbeds; this report describes a multipurpose borehole used for both degasification and the production of commercial-quality gas. The multipurpose borehole was drilled into a barrier pillar, and seven horizontal degasification holes and one pressure point hole were drilled radially out from its perimeter. On January 28, 1974, after 505 days of degasification, a compressor was installed to the exhaust stack of the multipurpose borehole (1), and pipeline--quality gas was introduced into a commercial pipe-line. As of February 4, 1975, over 171 million cubic feet of gas had been purchased by the gas company. The in situ pressure at a depth of 200 feet into the coalbed and the average gas flow and water flow from the degasification holes as they were completed and closed off were 203 psig, 1,200,000 cfd, and 6.8 gpm, respectively. Twenty-four hours after the seven holes were connected through individual pipes to the atmosphere, the total gas and water flows and the in situ pressure dropped, respectively, to 971,000 cfd, 1.3 gpm, and 18 psig. Five hundred days later, the corresponding values were 620,000 cfd, 0.15 gpm, and 10.5 psig. Daily flows have been as high as 800,000 cfd, and as low as 360,000 cfd, during the last 500 days. On February 4, 1975, after 882 days of degasification, 576 million cubic feet of gas had been removed from the Pittsburgh coalbed; apparently a much larger area of virgin coal is being degasified than is defined by the holes. This study indicates that horizontal boreholes drilled into a coalbed from the bottom of any shaft will effectively remove gas from the Pittsburgh coalbed,

Jan 1, 1975

By Ann G. Kim

Methane in coal constitutes a serious hazard in coal mining. Draining the methane in advance of mining can mitigate this hazard, conserve energy, and offer economic benefits. This Bureau of Mines report evaluates the Pittsburgh coalbed in Greene County, Pa., to determine if advance drainage is feasible. The gas content of virgin reserves in Greene County is estimated at 100 to 200 ft3/ton, a total of over 370 billion ft3 of gas in an area approximately 310 mi2. Because of the similarity to natural gas, drained coalbed gas could be recovered and added to pipeline supplies of natural gas. The value of conserved gas would offset the cost of drainage and extend energy resources.

Jan 1, 1975

By R. E. Siemens

A process is being developed by the Bureau of Mines to selectively recover nickel and cobalt from low-grade domestic laterites. In laboratory evaluation of the process, the oxides in the laterite were selectively reduced with carbon monoxide at temperatures from 350° to 600° C. For material containing more than about 5 percent magnesia, pyrite additions or post-reduction heat treatments were necessary to achieve satisfactory nickel and cobalt extraction for this range of reduction temperatures. Multistage leaching of the reduced material at ambient temperature and pressure in the presence of oxygen, ammonium sulfate, and ammonium hydroxide extracted up to about 90 and 85 percent of the contained nickel and cobalt, respectively. The nickel was selectively recovered from the leach solution by solvent extraction and was then stripped from the loaded organic with dilute sulfuric acid to provide a nickel-rich electrolyte. Treatment of the raffinate with hydrogen sulfide resulted in the recovery of cobalt as a sulfide. The only contaminant in solution was magnesium which was removed by ion exchange or precipitation. In this process the energy requirements are relatively low and except for minor operation losses, only coke and oxygen are consumed.

Jan 1, 1975

By Oleg Terichow

Electrophoretic mobility measurements were made by the Bureau of Mines on samples of a Florida phosphate slime to determine the optimum conditions of coagulation and settling in an aluminum sulfate solution. Addition of anthracite to promote mutual coagulation demonstrated the practicability of heterocoagulation by reduction of the repulsive effect of double layers. By proper selection of the electrolyte and its concentration, the reduction of the double layers to a net zero point of charge causes the predominance of Van der Waals' forces of attraction leading to the coagulation and rapid settling of both particle systems, as is predicted by the Derjaguin-Landau-Verwey-Overbeek theory of colloidal stability. Confirmation was found in the microfiltration tests where a modified Carman equation was applied to evaluate the specific filter bed resistance.

Jan 1, 1975

By Joan C. Biordi

[Composition profiles for atomic, radical, and stable species, as well as temperature and area expansion ratio profiles, have been determined for a nearly stoichiometric CH4-02-Ar flame and one to which 0.3 percent CF5Br inhibitor had been added. Net reaction rate profiles were calculated for all the observed species. For the normal flame, these and the mole fraction profiles gave rate coefficient information about the elementary reactions in the methane flame, for example, CH. + 0 4- H2CO 0 H, k4 = 1.05 X 1014CM3 mole-1sec-1 for 1,550§T 0,725' K; CO + OH 4 C02 + H, k6= 4.7 X 1011 for 1,350{T X1,750° K. Comparison between the inhibited and normal flame showed that A] and [CH3] were significantly reduced at the lower temperatures in the inhibited flame even though in the hot gas region the [E] [OH!, and [0] were essentially the same in both flames. The CF3Br disappears very early in the flame, relative to the fuel, and the reaction primarily responsible for its disappearance is H v CF3Br 4 HBr + CF3, where k7 is found to be 2.2 X 1014 exp(-9460/RT) for 700-1,550° K. Reaction of the inhibitor with methyl radicals provides for the relatively small amounts of CH3Br observed, but CH3 + Br2 - CHs Br + Br must also occur. The HBr formed reacts rapidly with H atoms to form H2 and Br, but the reaction is soon "balanced" in the flame as may be demonstrated by calculation of the equilibrium constant at various temperatures. The fluoro-carbon fragment produced in reaction (7) also reacts rapidly, in part with methyl radicals to give the observed elimination product CH2CF2 Later in the flame, above -1,400' K, F2CO is formed from the reaction CH2CF2 + 0 P F2CO + CH2 and k., -1.5 X 1013 at 1,600° K. The rather slow decay of carbonyl fluoride is attributed to reaction with H atoms according to the sequence F2CO I H - HF + FCO and FCO + H HF + CO.]

Jan 1, 1975

By L. A. Johnson

This Bureau of Mines report presents the analysis of three cores from the Asphalt Wash area of the P.R. Spring tar sand deposit of northeastern Utah. Two tar sand zones are indicated in the Asphalt Wash Area. Total net thickness of the tar sand ranges from 23 to 39 ft, with occurrences between 56 and 263 ft in depth. The sand has average porosity of 24.7 pct of bulk volume, average permeability before and after extraction of 87.5 and 596 md, respectively, and average oil saturation of 58.1 pct of pore volume. Oil gravity averages 10.9° API.

Jan 1, 1975

By G. L. Gates

The waters used to waterflood the Wilmington oilfield were studied by the Bureau of Mines, in cooperation with the city of Long Beach, Calif. Increases in the pressure of the injection wells indicated that they were being plugged by materials suspended in the waters. This study was made to identify the suspended materials, determine their origin, and find methods of preventing their formation. The suspended oil-coated materials were iron sulfide, barium sulfate, calcium carbonate, clay, and sand (or silica). Results indicated that the sulfide, which was as high as 90 milligrams per liter, was the product of sulfate-reducing bacteria. The injection of ocean water increased the sulfate content of the waters in the petroleum reservoirs from 3 to 250 milligrams per liter, thereby furnishing sulfate for growth of the bacteria. The waters were supersaturated with barium sulfate. Laboratory tests showed that sulfide could be removed from the waters by adding iron at a cost of 1 to 2 mills per barrel. The solubility of iron sulfide and calcium orthophosphate in the injection waters was also determined.

Jan 1, 1975

By Alan H. Goode

The advancement of high-temperature drilling fluid technology for application in geothermal environments is part of the Bureau of Mines program for more efficient development of our Nation's energy resources. The bentonite constituent of water-base drilling fluids is sensitive to destabilization by high-temperature and salinity. A substitute material for bentonite, phosphate slime, which is reported to be saline resistant, was considered. These studies show that spray-dried slime suspensions have more favorable rheological behavior, but poorer filtration properties, as compared with bentonite suspensions.

Jan 1, 1975

By Richard J. Leary

The inputs of capital and labor to support future iron ore production were developed by the Bureau of Mines from projections of iron demand and estimates of capital and labor requirements. Trends in technologic change and the organization of production were analyzed. Labor requirement schedules for iron ore mining and beneficiating were constructed from aggregate inter-temporal trends and 1970 cross-sectional analysis of mines and mills. A sup-ply schedule of the capital requirement for mine-mill-pellet plants was developed from U.S. and Canadian experience. The structure of demand for iron to the year 2000 was examined as well as the availability of resources. Projections of capital and labor requirements to 2000 were constructed under two international patterns of iron ore supply to the United States. The most likely model is for a continuation of the 70 percent United States-30 percent foreign shares, expanding at an average 2.0 percent growth rate to 2000, and supported by a cumulative gross capital investment of $3.8 billion constant 1967 dollars and a labor force in the United States of 29,800 by 2000. The information content of projections is discussed, and the possible effects of international forces on supply are considered. A generalized methodology for estimating capital and labor requirements in other mineral industries also is included.

Jan 1, 1975

By R. H. Sprute

Extensive Bureau of Mines laboratory testing has shown that electrokinetic densification can be an effective method for dewatering and consolidating unclassified metal mine mill tailings. The report describes results of a limited field test of this technique. Eighteen-cubic-yard concrete model stopes, 18 feet long by 6 feet deep by 56 inches wide, were filled with unclassified tailings slurry from a metal mine in the Coeur d'Alene, Idaho, district. Five different tests were performed. They showed that a strong, dense, dewatered fill can be obtained in a reasonably short time using electrokinetics, with typical power consumption of 25 to 30 kW-hr/yd3 of densified fill. At present power costs in the Coeur d 'Alene district, this would amount to 10 to 12 cents/yd3.

Jan 1, 1975