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By Árpád B. Palotás, Adel F. Sarofim, John B. Vander Sande, Lenore Rainey Christian, J. Feldermann

"Interest in the fine structure of soots and carbon blacks is motivated by a variety of possible applications. The structure provides information on the origins of the particles and on their adsorptive and reactive properties. This paper describes a method for quantification of the structure of soots and carbon blacks based on direct electron microscopic observation followed by image analysis of these materials. High-resolution transmission electron microscopy (HRTEM) provides a very detailed observation of particle structure. The differences in soot structure, because of its complexity, may not be easily quantifiable with the human eye; therefore, high-level computer software has been used to manipulate HRTEM images. This technique involves the application of fast Fourier transforms (FFT) to single particles and the measurement of characteristic parameters such as interplanar spacings and crystallite sizes from these particles. The methodology and application of this characterization technique are presented here. Results are shown for dif¬ferent samples obtained from soot and carbon black particles selected to illustrate the capabilities of the methodology. Quantitative information can be obtained on structural characteristics, e.g., interplanar spacing, circularity, orientation, elongation, and length distribution of lattice fringes, as well as on the fractional coverage of the extracted pattern. c 1996 Wiley-Liss, Inc.This paper presents a combination of techniques for recognizing and classifying different carbonaceous materials, using their structural morphology. A new method to assess and quantify the parameters which define such structures is proposed and discussed. The technique 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, cokes, chars, etc. possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure (Buseck and Bo-Jun, 1985; Buseck et al., 1987). The carbon structure has been variously described as turbostratic (Oberlin, 1989) or as crumpled sheets (Rouzaud et al., 1991) 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 on the composition of the source of the carbonaceous material. The value of the electron microscope in studying the morphology of such materials has been well-established, and abundant information is available (Ishiguro et al., 1991; Lahaye and Prado, 1978; Buseck, 1992).The use of HRTEM has brought further insight into this matter. Qualitative assessment of the structural order of such materials has been attempted over a long period of time in order to differentiate between various sources or treatments. There is, to date, no successful method available for quantifying the structural characteristics of various carbonaceous materials. This paper presents a technique which is able to recognize dif-ferent materials and to quantify the structural parameters of those materials using HRTEM and computational image analysis, including pattern recognition techniques.In the case of perfectly ordered graphitic crystals, electron diffraction is widely used for obtaining details on structure. Analysis of diffraction patterns can reveal parameters such as interplanar spacing, d002, crystallite size along the c-axis, Lc, crystal size in the plane of the layers, L., mean number of crystallites, Nc, etc.Complicated electron microscopy methods such as defocusing, tilted illumination, axial illumination, etc., often have to be used in order to characterize complex materials such as randomly oriented crystals in soots and carbons. Obtaining the right fo"

Jan 1, 1998

By J. S. Kennedy, M. M. Fine

"INTRODUCTION Barite is one of the major industrial minerals whose production has increased considerably in the last 10 years. In 1935 domestic production of barite was 218,075 tons and. had increased by 1944 to 515,136 tons. 3/ Most of the primary uses for barite and barite products were developed before 1935, so the increase in barite production reflects the growth of industry in general rather than any recent developments in barite technology.The principal uses for ground and crushed barrite are as a weighting agent in heavy drilling fluids, as a filler in rubber and other materials, as a pigment and extender in paints, and as a flux in glass melt. In addition, a considerable' quantity of barite serves as the raw material for the manufacture of lithopone and barium chemicals.Specifications for barrite vary widely and depend primarily on the use to which the material is put. The primary requisites for barite used in heavy drilling muds -are that it have a minimum specific gravity of 4.2 and be very,low in soluble salts. A minimun barium sulfate content of 92 percent may be specified; but this is less important than the gravity. 4/ In addition before consumption the material must be ground to '92 percent minus 325-mesh. 5/ Lithopone and chemical manufacturers require a minimum of 94 Percent barium sulfate, a maximum of 1.0 percent iron oxide, and not more than a trace of fluorine. 6/ Barite used as fillers in light-colored products should be of fairly high grade, but the filler used in dark products may be considerably lower grade.Glass barite should contain a minimum of 96 percent barium sulfate, not more than 3 percent moisture, a maxium of 0.2 to 0.4 percent iron oxide, and not more than a trace of titanium oxide. Particle size is a matter of some importance in glass barite, also. 7/"

May 1, 1948

By A. J. Kraemer

This report on research and experimentation by the Federal Bureau of Mines on technologic and scientific problems of the petroleum and natural gas industries presents a resume of work from July 1, 1953, to June 30, 1956. The preceding report, for the fiscal year ended June 30, 1953,3/ indicated continuation of the Bureau's program of petroleum and natural gas research of world-wide significance, which began in 1910. The petroleum and natural gas research of the Bureau of Mines is divided into five main categories: (1) Production of petroleum and natural gas, (2) transportation and storage, (3) petroleum chemistry and refining, (4) thermodynamics, and (5) economics.

Jan 1, 1959

By Alla D. Mah

Titanium forms several compounds with oxygen and also is able to dissolve interstitially about 33 atomic percent of oxygen. Starting with titanium dioxide, reduction becomes increasingly difficult as oxygen is removed; and the final step, be reduction of the titanium-oxygen interstitial solutions, is by far the most difficult. The possibility of reducing titanium oxide, or of purifying titanium containing oxygen, by treatment with certain more volatile metals has been a subject of considerable interest. Theoretical appraisal of the limitations of this possibility, however, has been hampered by lack of adequate information on the thermodynamic properties of the titanium-oxygen solutions. The purpose of the present work was to remedy this difficulty by expanding the thermodynamic knowledge regarding these solutions. The experimental work involved three types of calorimetry and furnished the following information: (1) Heats of formation of 11 titanium-oxygen solutions, in the range of 0 to 10 wt.-percent oxygen, were determined at 298.15° K. As a byproduct, an improved value of the heat of formation of rutile was obtained, which, in turn, led to improved values of the heats of formation of the lower titanium-oxygen compounds. (2) Low-temperature heat-capacity data and entropies at 298.15°K in were determined for 2 representative titanium-oxygen interstitial solutions. (3) High-temperature heat-content data were obtained for 2 titanium-oxygen interstitial solutions to about 1,600° K.

Jan 1, 1957

By Clarence Hall, J. J. Rutledge

Many of the fatal accidents in coal mines have resulted from the Explosives used in Use of explosives for breaking down the coal. These accidents have resulted both from the use of explo- sives that were not suitable and from the careless or improper use of suitable explosives. Investigation has shown that one of the commonest causes of dis- astrous explosions in the coal mines in this country has been a blown- out shot of black blasting powder or dynamite. The dangers that attend the use of these explosives were perceived several years ago, and in consequence the attention of powder manufacturers was directed to the production of explosives that would be less liable to ignite inflammable gas or dust. The manufacturers have been so successful in their efforts that it is now possible to obtain explosives which yield much shorter and quicker flames than black blasting powder or dynamite, and hence are much less dangerous to use in fiery or dusty coal mines. of explosives. To find out which of the many grades of short-flame explosives Government tests have the qualities that render an explosive most effective and least dangerous for mining coal, the United States Government established a testing station at Pitts- burgh, Pa., in 1908. This station is now under the charge of the Federal Bureau of Mines. Before the station was opened a state- ment of the requirements that the explosives in question would have to satisfy was drawn up and sent to manufacturers. A number of these sent explosives to be tested, and on May 15, 1909, a list of the explosives that had passed the tests was published. Since that date other brands of explosives have been tested and three more lists have been issued. The latest list, published in Miners' Cir- cular 2, Bureau of Mines, contained the names of no less than 71 explosives that had passed the tests prior to January 1, 1911.

Jan 1, 1912

By T. M. Romslo

"The Keystone and St. George properties are in the so-called Johnson Camp area and adjoin a property that in recent years has become a steady producer of low-to medium-grade copper-zinc ores. The Keystone Copper Co. was active intermittently from 1908 to 1938 and during 1926 to 1937 produced a recorded 1,100 tons of 5 percent copper ore. There is no evidence that ore has been produced from the St. George property.In the Johnson Camp area both igneous and sedimentary rocks ranging in age from pre-Cambrian to Quaternary are exposed. The ore bodies are in the Paleozoic rocks and occur principally in the Abrigo formation, which is composed mainly of limestones and shales. The rocks of the productive zones are metamorphosed and are cut by systems of fractures and faults. Chalcopyrite and sphalerite, the principal ore minerals, replace altered limestones to form deposits locally called mantos and chimneys.Investigation of the Keystone and St. George deposits by the Bureau of Mines included topographical and geological mapping of the surface and the underground workings and diamond drilling from the surface. A total of 10,067.8 feet was drilled in 22 holes. The drilling started November 13, 1947, and was completed August 19, 1948.This report records factual information obtained during the course of the investigation."

Jul 1, 1949

By B. W. Gandrud

The upper part of the Alabama deposits of crystalline graphite consists of an oxidized ore derived from the underlying unoxidized ore through prolonged Weathering. The degree of oxidation in different sections and at different depths within the bed is not uniform. The original ore is hard and blue-gray; the weathered product is soft and brown and is the only part that has been mined to any extent. Samples of both oxidized and unoxidized ores were obtained from two of the large graphite deposits of Clay County. Three additional samples of oxidized ore were obtained from different portions of a third property in the same region. In this report, ores 1 to 5 are of oxidized material and ores 6 and 7 of unoxidized.

Jan 1, 1934

By B. P. Martinez

A process for regenerating spent pickle liquor is proposed in which some of the water is evaporated at atmospheric pressure and ferrous sulfate is precipitated as monohydrate crystals..Equilibrium conditions are set for a slurry of crystals in a mother liquor containing 5 percent FeS04 and 45 percent E2S04, by weight, and boiling at about 235° F. The slurry is pumped continuously to a filter, and the mother liquor from the filter is pumped back for reuse in the pickling tanks. The net result of the process is to remove ferrous sulfate in the regeneration plant at the same rate ac it is produced in the pickling tanks. This process is integrated with the steel-pickling operation and controlled by the pickling requirements for particular steels. Spent pickle liquor is removed for regeneration continuously from both batch and continuous picklers at higher acid concentrations than would be dumped to waste because no acid is neutralized or discarded. However, the process is not designed to keep a sulfuric acid concentration stronger than 25 percent in any pickling tank. To retain flexibility in the pickling operation, all acid makeup is added to the pickling tanks. Rinse waters are used as water makeup for the pickling tanks. To further minimize waste of acid in the rinse waters, improvements of rinsing practices are outlined.

Jan 1, 1953

A prototype EM Location System was fabricated and tested at the Geneva Mine near Dragerton, Utah. This system consisted of six manpack transmitters and six manpack receivers covering the frequency band from 900 Hz to 2900 Hz as well as a six channel receiver designed for use in a helicopter. Tests showed that EM signals from lightweight (314 lb) transmitters could be detected both on the surface and from a helicopter through -2 as much as 1650 ft of relatively high conductivity (2 X 10 mhos/m) over- burden. Furthermore, the resulting field strength profiles could be used to determine source location to within 150 ft of the actual surveyed location in the mine. Modifications were made to a Monitoring, Locating and Communications System being tested at the Bruceton Mine, Pittsburgh, Pennsylvania. These modifications have improved the performance and quality of the paging and voice telephony mode of the system. Subsurface receiver modifications have improved reception of voice downlink signals.

Jan 7, 1973

By K. E. Stanfield

The oil yields of sections of Green River oil shale in Colorado, Utah, and Wyoming are presented as part of a continuing project to determine oil-shale reserves in the United States. Oil-yield logs, based upon analyses obtained from 1945 through 1952, are presented to show the thickness and richness of 202 sections of Green River oil shale. The logs are based on analyses of approximately 20,500 samples, representing 179,000 feet of shale, which were made by the Bureau of Mines, and upon analyses, representing approximately 26,000 feet of shale, which were made by other agencies. The samples consisted of cores from a Bureau of Mines coring program in U. S. Naval Oil-Shale Reserve 1, Garfield County, Colo., and cores, drill cuttings, and channel samples provided by other agencies, chiefly oil companies. Most of the samples of oil shale from Utah and Wyoming were derived from oil-well drilling operations. As a result, the oil-shale sections were widely scattered and were not extensive or reliable enough to be representative of the significant deposits of Green River oil shale in these States. The oil-shale sections for Colorado, however, were more comprehensive, and a number of the sections were used in a previous report as a basis for estimating oil-shale reserves in Colorado. The present report does not give estimates of oil-shale reserves but is limited to presentation of oil-shale analyses that may be used for future reserve estimates. Other sections of Green River oil shale are being analyzed, and the results will be published in subsequent reports.

Jan 1, 1954

By J. B. Vander Sande, L. C. Rainey, P. Bolsaitis, B. Dirsa

"The structure and composition of silica-rich particles recovered by lavage from the lungs of three active miners with different medical histories were studied using high-resolution electron microscopy and chemical microanalysis. The results arc compared to the similarly determined structure and composition of respirable-size mineral particles obtained from roof-bolter dust-box samples from two coal mines of widely different bulk quartz concentrations. The results show that the lungs of the miners contain silica-based particles with structures not found in the mine samples. Also, the particle structures and compositions found in the macrophages were different in each of the miners. The rau.lu suggest the possibility that intracellular processes may affect the susceptibility of individuals to silica-induced pneumoconiosis. The cytotoxic and fibrogenic potentials of mine dusts result from the activity of their individual components. Whether this effect is additive or even mass (i.e., dose) related is questionable and has been the subject of many investigations. Particle size and size distribution of various constituent minerals, the surface structure and properties of individual particles, and the self-cleaning capability of the lung (i.e., the capacity of the macrophage system) may, among other variables, affect the pathogenic changes induced by dusts lodged inside lungs. Extensive epidemiological investigations conducted on miners from different coalmining districts, where equivalent dust exposures have been shown to result in vastly different frequencies of lung disease incidence, also confirm this hypothesis (1) In a recent study, Ferrer et al. (2) used energy-dispersive X-ray analysis (EDXA) to investigate the inorganic element content in pleura and lung in reference, silica exposed non-pneumoconiosis, and silicotic populations. Constant depositions of silicon and calcium were detected in visceral pleura, parietal pleura, and lung of the refence group and in visceral pleura and lung of the exposed non-pneumoconiosis and silicotic groups. Comparison of the silicon content in pleura between silicotic and exposed non-pneumoconiosis subjects showed a nonsignificant probability of difference, whereas there were no differences with respect to the silicon content in lungs."

Dec 1, 1995

By R. F. Droullard

The Bureau of Mines has developed test facilities for use in a research program that deals with radiation hazards in mining. This report describes the radon test chamber located at the Denver Research Center and the Twilight experimental mine located near Uravan, CO.

Jan 1, 1984

By R. D. Rosenkranz

The Bureau of Mines has investigated the availability of copper from 272 deposits in market economy countries. The deposits studied have demonstrated resources totaling 413 million metric tons of contained copper and account for more than 90 pct of the reserve base for market economy countries. Using data gathered as part of its Minerals Availability Program, the Bureau performed geologic, engineering, and economic evaluations in order to determine the copper production potential of each deposit. At the 1981 copper market price of $0.85/lb, the deposits studied could economically produce an estimated 88 million metric tons of copper (allowing for profit computed at a 15-pct rate of return), primarily from mines operating at the time of the study (1981). At this price, producing mines in market economy countries could economically produce only 2.1 million metric tons of refined copper per year. However, actual 1981 production was 6.2 million metric tons, indicating that many mines continued to operate even though they were unable to cover all production costs. For U.S. producing mines, the estimated average cost of production per pound (including profit at a 15-pct rate of return) was $0.15 higher than the average cost in other market economy countries.

Jan 1, 1983

By W. E. Tournay

In accordance with a cooperative agreement between the Bureau of Mines, United States Department of the Interior, and the Linde Air Products Co., an investigation was made at the Bureau Explosives Testing Station, Bruceton, Pa., to develop suitable test methods for evaluating the performance and sensitivity characteristics of liquid-oxygen explosives. This report presents the results of the investigation. The unique nature of liquid-oxygen explosives necessitated both modification of standard techniques and development of entirely new test methods. The latter requirement was due to the fact that differences exist in the kind of information that must be developed for studying relative safety and performance properties of these explosives compared to that of fixed explosives.

Jan 1, 1949

By Howard E. Rollman

South Central United States, an area including Arkansas, Kansas, Louisiana, Mississippi, Missouri, Oklahoma, and Texas, is a net exporter of refractories. Nearly $45 million of these materials was shipped in 1954 from plants in the area, compared with area consumption of $18.5 million. About 88 percent of all refractories production is concentrated in Missouri. The prevalent consumption pattern, however, is one of localized shortages. For example, although Texas uses more than half of the refractories consumed in the South Central United States, production of refractories in Texas is relatively small. Also, the apparent self-sufficiency of the area is in terms of value produced rather than in terms of products consumed. Nearly all of the $6,425,000 nonclay refractories consumed in the area were shipped from other States. Local resources possibly could be developed for making refractories to serve markets that currently are being supplied from outside the area. Since other industries are growing rapidly in the area, the market for refractories is expected to continue to grow--more rapidly than the national market. The Missouri refractories industry is economically important nationally. Nearly one-fourth of the clay refractories produced in the United States are made in Missouri. Moreover, Missouri produces most of the higher grade clay refractories, about 62 percent of the high-alumina refractories, and 85 percent of the superduty refractories. The competitive position of the Missouri refractories industry is strong. The national market for clay refractories and the market in the South Central United States are expected to continue to grow. The ratio of net income to the value of refractories shipped in Missouri is larger than the national average.

Jan 1, 1960

By John J. Mulligan

Coalbeds were discovered in outcroppings of the Beacon group of sediments on the north end of the Willett Range ( altitude 77 ° 11 ' S , longitude 160 ° 20 ' E ) , Victoria Land , Antarctica , in December 1960 during an investigation undertaken as part of the U.S. Antarctic Research Program under the auspices of the National Science Foundation . Three separate exposures of coal or coaly material were found . Two of the exposures contain , respectively , eight and four beds of hard , compact , finely banded attrital coal ranging in thickness from 8 feet downward to a few inches , and reported to range in rank from mediumvolatile bituminous to semianthracite . The coals are associated with carbonaceous shales containing an abundant assemblage of fossil plants resembling those associated with the Permian coals of Australia and other Gondwana areas . The third exposure , apparently somewhat higher in the stratigraphic sequence , contains only coaly plant fragments scattered through a thin conglomerate and overlying sandstones . A sandstone bed that overlies these coal - bearing sandstones contains abundant logs and fragments of silicified wood . Preservation of features is poor , but one segment of a silicified stem suggests comparison with Rhexoxylon , a gymnospermous tree that usually is considered indicative of Triassic age . The Beacon sediments in this area have been invaded , broken , and uplifted by a massive series of diabase sills and dikes greater in volume than the intruded sediments . The heat emitted by these intrusives must have advanced the metamorphic development of the coals . However , there is no evidence of alteration to graphite , and coal found in direct contact with a diabase sill contains no vesicles or other usual evidences of natural coking . Either the pressure of overlying rocks inhibited the development of coke , or the coals had been metamorphosed beyond the coke forming stage before the igneous intrusion .

Jan 1, 1963

By Herbert Cremer

The United States,-the largest nickel consumer in the world, produces virtually no nickel from domestic ores. Dependence upon outside nickel - sources and increasing strategic, importance of nickel focused the attention of the United States on deposits within its boundries. The most likely domestic sources of nickel are low-grade oxide and silicate deposits, such as the Cle Clum deposit, Kittitas County, Wash., and the Riddle deposit, Douglas County, Oreg. The Federal Bureau of Mines, Northwest Electrodevelopment Laboratory, Albany, Oreg. has been investigating electric smelting of low-grade oxide and silicate nickel ores. These smelting studies have been on selective reduction to produce low-carbon ferronickel. Selective reduction is based upon the relative reducibility of: nickel, iron, and chromium, in the order named, when the charge contains insufficient carbon or other reductants to reduce the entire quantity of these metals present in the ore.

Jan 1, 1954

By Michael E. Henderson

The U.S. Bureau of Mines (BOM) constructed the Hydraulic Transport Research Facility (HTRF) to investigate the hydraulic parameters relating to the transport of coarse coal. To achieve these goals in a timely and efficient manner, the Bureau contracted to Boeing Services International, Inc. (BSI) the responsibility of operating the HTRF and providing technical support. This data report is a summary of the testing and data results for the period from 6 September to 9 September 1983. The testing covered herein is for coarse 2-in by 0 (minus 50 mm) Pittsburgh Seam run-of-mine (ROM) coal in a 12-in (300 mm) pipeline, at velocities ranging from 8 to 16 ft/s (2.4 to 4.9 m/s) and at concentrations ranging from 15 to 50 pct.

Jan 1, 1985

By Roy L. Grant

The Bureau of Mines investigated the up-and-down method with factorial designs to determine if shorter, and therefore less costly, trial sequences could be used. Although sequences of 50 trials are usually recommended, sequences of 20 trials were arbitrarily chosen for the experiments with permissible coal mine explosives described in this report. These explosives were fired from a cannon pointed into a flammable natural gas-air atmosphere at the Bureau of Mines Explosives Research Center gallery to ascertain their safety properties. The investigation demonstrated that the shorter sequences led to useful conclusions with a reduction in cost of the experimental program.

Jan 1, 1967

By A. M. Evans, J. H. Soulé

"INTRODUCTION Deposits of iron ore in Cherokee County, Tex., have been worked at various times in the pact, and the ore has been smelted in small local blast furnaces.Recently it was proposed to establish a charcoal blast furnace with a wood distillation plant to produce charcoal for fuel and byproducts. Financial assistance from the Reconstruction Finance Corporation was sought by George Easley and associates to enable them to purchase, move, and erect the furnace and build the required accessory plants. The furnace was to be moved from Pembroke, Fla.In August 1941, the Bureau of Mines was asked by the Office of Production Management to check the development work of Easley and associates and to ascertain (1) the iron-ore reserves, (2) the cost of mining ore and delivering it to the blast furnace, and (3) the grade and character of the ore. The Bureau of Mines was advised, while the investigation was in progress, that approximately 1,000,000 long tons of measured reserves would be sufficient to demonstrate the feasibility of operating the properties.Although deposits of iron ore are widely distributed in Cherokee County, only the Pryor Mountain, Banks and Cherokee, J. P. Acker, and Citizens State Bank tracts were sampled thoroughly by the Bureau of Mines. The iron-ore rights on these are owned by the New Birmingham Development Co., the Cherokee Development Co., or by individuals. Options to lease the ore rights were obtained by Easley, who obtained options on the Hawes Peach Orchard and Bradford tracts, also, which were examined only cursorily by the Bureau."

Aug 1, 1947