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By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Paolo Ciambelli, Lenore Rainey

"The evolution during oxidation of the internal structure of soot and carbon black particles was studied using high-resolution transmission electron microscopy (HRTEM) and an image analysis system. Increasing ordering to the carbon structure with increasing oxidation is observed. Measures of the increased order are increases in the fractional coverage of a cross section of the particles with a layered structure, a decrease in the mean interlayer spacing, and a decrease in the spread of the interlayer spacing. The changing structure of the carbon black impacts its properties, such as the rate of oxidation.There is considerable interest in the study of the structural changes of carbonaceous materials as a function of oxidation. Davis et al.1 measured the variation of carbon dioxide surface area of various coals as a function of residence time in a flow reactor. HRTEM measurements revealed that crystallite dimensions and interlayer spacings are altered by combustion. Ishiguro et al.2 showed that oxidation alters the structure of diesel soot. The aim of our current research is to develop a better understanding of the microstructural reordering of carbon blacks with implications to their properties. The carbon blacks used in this research have already been studied and their reactivities as a function of oxidation measured.3The methodology used in this work has already been described in detail elsewhere.4 This paper presents an application to quantify the structural changes of carbon black particles as a function of oxidation and graphitization. The technique used is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, chars, etc., possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure. The carbon structure has been variously described as turbostratic5 or as crumpled sheets6 to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as the composition of the source of the carbonaceous material. The value of electron micros¬copy in studying the morphology of such materials has been well established,2,7,8 although only a few attempts toward quantification have been made.The sample observed was carbon black CB330 from De¬gussa. One set of carbon black samples were oxidized in a thermo-gravimetric analyzer (TGA) in air at 575 0C, so that the conversion varied from 0 to 96%. Another set of carbon black samples were graphitized (Graphpac-GB by ALLTECH) and then oxidized in the TGA at 680 °C until 92% burnout was reached. The latter samples are called GB 0% and GB 92%, respectively.For the HRTEM observation a small portion of each sample was ultrasonically dispersed in ethanol. The suspension was deposited dropwise on a copper TEM grid coated with a lacey carbon film. The examination of the samples was carried out on areas that extend over the holes in the supporting film in order to avoid interference from the amorphous carbon background film An oriented gold crystal was used as a calibration standard and subjected to the same techniques as the carbon black samples."

Jan 1, 1998

By R. L. Schmidt

Research conducted over the past 20 years in France, Great Britain, and the United States on the use of the large-hole burn cut has established cer¬tain advantages for this system. Advantages include longer pull and more complete fragmentation from blast rounds. However, research is needed to establish a set of parameters for optimum performance. As part of the Bureau of Mines Advancing Mining Technology for Marginal Resources program, the Twin Cities Mining Research Center, Twin Cities, Minn., acquired a horizontal rotary drill capable of boring holes up to 24 in. in diameter. This was used for a series of underground experiments at White Pine mine, White Pine, Mich., during 1973. Exceptional results were obtained with a 12-1/4-in void hole that yielded up to 18 ft of pull in a 10- by 20-ft drift, Fragmentation was excellent, and the compactness of the muck pile facilitated loading.

Jan 1, 1975

The following are abstracts from papers presented at the 4th Symposium on Respirable Dust in the Mineral Industries and· were produced through research funding under the Generic Mineral Technology Center for Respirable Dust. Full articles appear in the proceedings published in July 1996 in Applied Occupational and Environmental Hygiene. (Volume 11, Number 7). The two addresses included in the proceedings point to the progress, prospects, problems, and perspectives on control of respirable dust and dust-related disease in the mineral industries. The symposium papers deal with respirable dust issues that are longstanding such as characterization, health effects, control of airborne coal dust, new and emerging issues such as iron toxicity, diesel particulates, and sampling. The papers were grouped into the following topics: continuous dust monitoring, encompassing the development of a fixed-site monitor that will provide continuous information on instantaneous and time-weighted respirable dust concentrations; mechanisms involved in the generation of dusts in mine environments, important for dust control at the source; characterization and control of diesel emissions (particularly diesel particulates) in mine atmospheres; mining systems effects and models; dust control in mine working faces and in milling environments; characterization of the physical, chemical mineralogical, and biological properties of the dust and their relevance to health effects and sampling; dust-lung interactions, encompassing results from several biomedical studies dealing with acute and chronic inhalation of airborne dusts and associated lung responses; the role of iron in causing lung injury; and therapeutic strategies for ·the control of pulmonary disease. All papers submitted to the organizers were peer-reviewed. In the proceedings, we have not differentiated among the platform and poster papers; rather, they have been grouped into the above topical areas. Taken together, these papers reveal significant progress in the control of dust generation, characterization of dust, understanding of dust-lung interaction, and mining and milling practices to reduce dust exposure - all essential for reducing dust-related occupational hazards at the workplace.

Jan 1, 1998

By N. A. C. Smith

One of the most important considerations in any manufacturing industry is the production of stable material, that is, material which will not change in quality before it reaches the consumer. The manufacturer of gasoline, the refiner of crude petroleum, is handicapped in this respect by the varying nature of his raw material, but as far as it is commercially practicable, he has endeavored to improve his product, and in most cases he has been eminently successful. It sometimes happens, however, that a gasoline that is apparently normal when first made, will In time deposit small quantities of a gummy substance. The present Investigation was undertaken in the hope that it would throw some light on these gums and indicate how their formation might be prevented.

Jan 1, 1922

By E. J. Kloos

The Bureau of Mines devised a new machine-test method for measuring carbon dioxide inspired by a wearer of self-contained breathing apparatus. The new method compares favorably in speed and precision with standard man-tests in which the apparatus is tested while actually worn, and is scheduled for use in future approval tests for facepiece carbon dioxide 'measurements. However, man-tests will still be used to measure the efficiency of the carbon dioxide sorbent materials in closed-circuit breathing apparatus.

Jan 1, 1966

By L. Cheng, M. S. Seehra, P. S. Raghoottama

The four major IR bands of a-quartz at 1080, 797, 693 and 488 cm-1 are studied at room temperature by FTIR-Photoacoustic Spectroscopy. Using Rosencwaig-Gersho theory, equations for the PAS signal q for the thermally thin and thermally thick cases are derived and it is shown how thin to thick transition occurs and leads to saturation as the sample mass is increased. For sample mass < 2 mg, q is proportional to sample mass thus defining the region for quantitative analysis. The dependence of q on the chopping frequency f is found to vary as q f-n with n ? 0.9 for quartz, in good agreement with the RG theory.

Jan 1, 1989

By Robert Blickensderfer

Equipment and procedure for the continuous roll bonding of metal strips are described. The reels, mill rolls, and furnace were located within a vacuum chamber capable of operation at a residual gas pressure of 1 x 10-4 to 1 x 10-5 torr. Several metals were successfully clad at rolling temperatures of 930° to 1,050° C in lengths up to 120 ft. The bimetals that were clad included stainless steel to carbon steel, molybdenum and nickel to stainless steel and carbon steel, and titanium to carbon steel. Bend tests of bond integrity are described, and microstructures of the interfaces are presented. The amounts of brittle intermetallic phases formed at the interface are minimized by this cladding method.

Jan 1, 1980

By David J. MacDonald

Stability constants, that is, equilibrium constants for complex-formation reactions, have been determined by a titrimetric method for complexes formed by the transition metal ions Ni2+, Cu2+, Zn2+, and Cd2+ with the structurally analogous bidentate ligands N-ethylethylenediamine and 2-(ethylthio)-ethylamine. The sulfur containing ligand was found to be the weaker of the two chelating agents for each of the four metals. Absorption spectra of the individual complexes have been determined in order to calculate their crystal field stabilization energies. The combined results suggest a linear relation between free energy of chelation and ionic radius of the metal ion.

Jan 1, 1972

By Sathit Tandanand

This report presents a Bureau of Mines study on the time-dependent behavior of coal measure rocks for future implementation in stability analysis and safety evaluation of in-mine rock structures. This initial study focused on moisture adsorption rate and strength degradation of shales in Pennsylvanian coal-bearing strata in the Illinois Basin. A reaction of clay minerals in Illinois shales with atmospheric water vapor was hypothesized as the adsorption and strength degradation mechanism. Part of energy exchange between shales and the environment was attributed to a free energy controlled by pore pressure of the rock and partial pressure in the environment. The relationships between adsorption versus time and strength degradation versus moisture content were derived and correlated with the experimental data. Partial saturation at various levels of relative humidity occurs within approximately 2 weeks at room temperature. The strength of shales tested decreases linearly with increasing moisture content. When the moisture exceeds 7 pct of the dry weight, these Illinois shales become unstable. To this end, the moisture content is a good predictor of rock strength for shales.

Jan 1, 1987

By C. C. Merrill

Columbium, tantalum, titanium, and zirconium are present in solid waste products generated by the chlorination of rutile used for production of titanium tetrachloride (TiC14). The columbium and tantalum were separated from titanium and zirconium by liquid-liquid extraction techniques using a secondary amine. Salts of these elements are in a leach liquor produced by water leaching of mineral waste from the chlorination of rutile. This waste, produced at the rate of approximately 50,000 tons per year, is about 40 wt pct water soluble. Leach liquors, separated by filtration, were further separated into a solid fraction and a liquid fraction by pressure hydrolysis, The solid fraction containing Cb, Ta, Ti, and Zr was dissolved in HC1-HF and used as a feed solution. Columbium and tantalum were removed from the organic extractant with 1 [N] HC1. A miniature 10-stage reactor showed that the columbium and tantalum present in solution could be separated with a continuous flow.

Jan 1, 1972

By B. W. Gandrud

In the summer of 1950, Bureau of Mines engineers visited a number of coal-preparation plants in western Europe and Great Britain to obtain information on European and British coal-cleaning and froth-flotation practices. In view of the growing importance of froth flotation as a process for cleaning fine sizes of coal, it was felt that such data and information would be of value in this country, for, although froth flotation has been adopted for use in a few of our plants, it has not as yet been employed as extensively as in British and European preparation plants. Many of the important coal beds in western Europe, especially in the Ruhr Valley of Germany and in the Dutch coal-mining region of Limburg, Netherlands, are very friable, with the result that the run-of-mine product contains a large proportion of the sizes too fine to be treated successfully by any other method than froth flotation. Furthermore, the relatively high cost of producing coal from these beds has for many years made it economically feasible and desirable to treat the fines by froth flotation, especially in the coking-coal fields.

Jan 1, 1951

By M. L. Whisman

Several commercial processes for reclaiming used lubricating oil were duplicated on a laboratory bench scale. Laboratory tests were selected and in some instances modified to determine the physical properties of each oil produced. In addition, the hydrocarbon composition of some samples was determined using a liquid chromatographic technique, and compared with the composition of new oil in order to determine the severity of the re-refining technique. Selected samples of reprocessed oil were reformulated with an additive package for further estimates of quality as determined by wear, corrosion, foaming, and oxidation stability tests. Additionally, several samples of commercially re-refined oil and new oil were obtained and physical properties were determined for comparative studies.

Jan 1, 1974

By Thomas P. Holden, Todd M. Ruff

Problem: An average of three workers a year are killed in surface mining operations when a piece of haulage equipment collides with another smaller vehicle or a worker on foot. Another three workers are killed each year when haulage equipment backs over the edge of a dump point or stockpile. Devices to monitor the blind areas of mining equipment are needed to provide a warning to operators when a vehicle, person, or change in terrain is near the equipment. Method: A proximity warning system (PWS) based on the global positioning system (GPS) and peer-to-peer communication has been developed to prevent collisions between mining equipment, small vehicles, and stationary structures. Results: A final system was demonstrated using one off-highway haul truck, three smaller vehicles, and various stationary structures at a surface mining operation. The system successfully displayed the location of nearby vehicles and stationary structures and provided visual and audible warnings to the equipment operator when they were within a preset distance. Summary: Many surface mining operations already use GPS technology on their mobile equipment for tracking and dispatch. Our tests have shown that it is feasible to add proximity warning to these existing systems as a safety feature. Larger scale and long-term tests are needed to prove the technology adequately. Impact on Industry: A PWSs that incorporates a combination of technologies could significantly reduce accidents that involve collisions or driving over an edge at surface mining operations.

By D. E. Shanks

The Bureau of Mines investigated the effects of HCI concentration and solution temperature on the solubility and crystal form of the chlorides of Co, Mn, and Ni when sparged with HCI gas at temperatures of 20°, 40°, and 60° C. Increasing HCI concentration in solution caused the chlo-rides of Co, Mn, and Ni to crystallize (salt out) because of the common ion effect. The salting-out crystallization was most effective for NiCI2, which had a solubility of 0.7 pct at 20° C and maximum HCI concentration. COCl2 salted out to a minimum solubility of 9.4 pct at 20° C and 22 pct HCI concentration and increased in solubility at greater HCI concentrations because of the formation of chloride complexes. MnCl2 was intermediate in behavior. The effect of temperature on solubility was greatest for CoCl2 and least for NiCI2, 15 and 7 pct change, respectively, over the temperature range of 20° to 60° C. The salted-out chlorides of cobalt and nickel formed the hexahydrates and those of manganese formed the tetrahydrate in saturated metal chlo-ride solutions at 20° C and low concentrations of HCI. Increasing the temperature or the HCI concentration caused a 108s in waters of hydra-tion. At 60° C, the salted-out crystals of NiCl2 formed the tetrahydrate in HCI concentrations up to 18 pct and the dihydrate at higher concentrations, while cobalt and manganese chlorides formed the dihydrates, even in water.

Jan 1, 1985

Increase the recycling of critical and strategic materials by simplifying the indentification and segregation of scrap. Background Because the United States is dl-most totally dependent on imports of such critical metals as chromium, cobalt and nickel, Bureau of Mines research has been directed towards conserving these metals by increasing the recycling of the complex scrap materials that contain them. Experienced scrap sorters, using the traditional techniques of object recognition, spark tests, chemical spot tests, color, apparent density, and magnetic properties, can adequately sort a wide variety of alloy groups. However, the complex nature of new materials entering the scrap market has made sorting both more difficult and more important. Some new alloys contain so many components that separation by discrete alloys becomes a prerequisite for effective recycling. The Bureau has completed Investigations on two methods for rapidly sorting complex scrap mixtures. One method uses a combination of two low-cost instruments. The other uses a single sorting instrument. Both approaches are reported.

Jan 1, 1986

Provide an operator cab to assure protection, comfortable use of controls, and good visibility. Approach A cab which raises and lowers by pivoting about d horizontal axis was Installed on two S&S cleanup tractors and tested in two underground working mines. How It Works Hydraulic cylinders actuated by a lever inside the cab cause the cab to pivot about a horizontal axis. This action raises or lowers the cab height. The total cab excursion is 14 inches. A release valve in the hydraulic system allows the cab to lower automatically if struck by a roof load or overhead obstruction. The pivoting action of the cab is engineered so that the operator maintains comfortable use of all controls at all cab heights. The movement is such that the angular relationship of the operator&apos;s ankles With the tram and brake foot controls IS consistently within 90 to 100 degrees. Figure 1 outlines the approximate position of the operator at three cab elevations.

Jan 1, 1977

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 R. K. Clifford

Chalcopyrite (CuFeSz) concentrates produced on the Lead Belt of Missouri typically contain 28 pct Cu and from 0.5 to 1.5 pct each of nickel and cobalt. Most of the nickel and cobalt are present as the mineral siegenite, (Ni,Co)3S4, almost none of which is recovered presently. The Bureau of Mines, U.S. Department of the Interior, has been conducting research on the chalcopyrite to produce a marketable fraction enriched in cobalt and nickel. Ferric chloride leaching of various chalcopyrite (copper) concentrates has yielded residues containing from 10.2 to 16.2 pct Ni and 8.3 to 11.4 pct Co with recoveries of approximately 79 pct. In another approach, laboratory froth-flotation tests have been conducted to investigate the effects of regrinding, roasting, baking, and steaming prior to flotation, with a variety of reagents. The best laboratory results were obtained after regrinding the copper concentrate to 94 pct minus 400 mesh and floating the chalcopyrite at natural pH (6.5) with 0.48 pound of sodium diethyldithiophosphate and 0.01 pound of sodium cyanide per ton of concentrate. This procedure yielded a tailings assaying 20.4 pct Cu, 5.2 pct Ni, and 3.45 pct Co. The tailings contained 67.2 pct of the nickel and cobalt and 15.9 pct of the copper originally in the copper concentrate; the remainder of the values reported to the flotation concentrate, which analyzed 29.6 pct Cu. To verify the laboratory flotation results, a 60 kg/hr process demonstration unit (PDU) was constructed in the Cominco American Magmont mill, Bixby, Mo.

Jan 1, 1978

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 R. S. Olsen

The Bureau of Mines is engaged in a continuing research effort toward the recovery of alumina from kaolinitic clay and other nonbauxitic domestic minerals. Hydrochloric acid extraction of calcined clay is among the acid processes under consideration. Although aluminum is easily leached from calcined clay, the presence of fines and slimes in the leached residue has hindered the application of this and other acid leaching processes. A clay feed preparation method was therefore developed that eliminated the slimy nature and the separation problems normally associated with leached clay residues. The preparation process consists of crushing the raw clay to minus 20 mesh, dampening the crushed clay with a fine water mist while tumbling on a rotating disk, and calcining the misted clay at 750° C. The misting process increases residue settling rates threefold to 9 cm/min (18 ft/hr) and filtration rates by two orders of magnitude. Leaching-kinetics were determined for misted clay feeds in a batch, stirred-tank reactor. Rapid leaching occurred during the first 85 to 90 pct of the extraction. The linear relationship of extraction to time during this initial phase corresponded to a zero order reaction with a rate constant of around 10 pct/min.

Jan 1, 1981