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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 H. Kato, G. Asai, R. Blickensderfer, R. Siemens

Some relationships were established among crystallographic orientation , rollability , deformation texture , annealing behavior , slip planes , and ductile- brittle bend transition temperature of molybdenum single crystals . Six large molybdenum single crystals obtained from an ingot melted by electron beam were oriented by X - ray diffraction and rolled on crystallographic planes of low indices in a known direction . During room temperature rolling , cleavage occurred on 100 type planes . At 300 ° C the crystals were rolled to 95- percent reduction in thickness . The crystals ( 001 ) [ 110 ] and ( 011 ) [ 100 ] were most easily rolled . Pole figures were used to correlate the deformation textures of the rolled crystals with the initial crystallographic orientation . Several of the textures which developed could be explained as a rotation about a < 110 > axis of symmetry . The cube crystal ( 001 ) [ 100 ] retained much of its " cubic " orientation . The (001 ) [ 110 ] crystal developed the simplest texture , whereas the ( 211 ) [ 113 ] and ( 211 ) [ 120 ] crystals developed the most complex textures . The 1 - hour recrystallization temperature of the crystal ( 211 ) [ 113 ] was 700 ° C , which is about 300 ° C lower than that of commercial polycrystalline molybdenum . The poles of the slip planes ( as determined from gross slip lines at relatively low magnification ) tended to lie within 20 to 60 degrees of the pole of the rolling plane . The Knoop hardness was slightly dependent upon crystallographic orientation but more dependent upon rolling direction . The ductile- brittle bend transition temperature was dependent upon the rolling orientation and the dislocation density .

Jan 1, 1964

By Lindsly. Ben E.

"The recovery or partial recovery of the oil remaining in oil sands after the usual methods of production have become unprofitable is perhaps the greatest problem in the petroleum industry today. The amount of this oil remaining in the sand is variously estimated by those familiar with the subject to be 25 to 90 per cent of the original content.2Lewis3 states, ""The estimate of 80 to 90 per cent of the oil left underground does not seem incredible.""It is estimated by the writer that approximately 91 per cent of the oil originally held in the Elliott pool, was still in the formation on January 1, 1924, and that it would take at least 12 years, at the 1923 rate of production, to further reduce this quantity by one per cent of the original content.The progress made in the oil industry during the past few years relative to the prevention of evaporation losses; to improvement in cracking processes, whereby the gasoline yield from many crudes has been doubled and trebled; to the increased recovery of gasoline from natural gas; and many other developments, remarkable as they are, can be applied only to that comparatively small portion of petroleum products which are raised to the surface. A device or process which would cut development costs to one-half would probably result in a much smaller profit to the oil industry, than the profit derived from an additional 10 per cent recovery of the total amount of oil in a pool. Various methods have been used and many others proposed, for the increase of oil recovery from normally depleted sands.In France, oil sands are being mined by means of shafts and galleries. In other places, notably the Bradford, Pennsylvania field, the yield has been increased by means of water flooding, wherein water is introduced into the sand to displace oil, and drive it to producing wells."

Oct 1, 1926

By ARCH L. FOSTER

The rapid increase in the mmber of automobiles during the last 25 years has resulted in the insistent and growing demand for better roads of more permanent construction. Some form of State license for the operation of automobiles has been in effect almost from the time of the first "self-propelled" vehicle, and some part of the revenue derived from the sale of these licenses has been applied to the maintenance and construction of roads. However, to obtain funds with which to build their present highway systems, the individual States have resorted to the taxation of gasoline. The first State to adopt a gasoline tax was Oregon, the law becoming effective February 25, 1919. By 1928, all of the States except two had levied taxes on gasoline at rates varying from 2 to 5 cents per gallon. New York and Massachusetts passed gasoline tax laws which became effective in 1929. Regulations governing the quality and the methods of handling gasoline and other petroleum products sold in the States have also been adopted by 29 States; many of these laws antedate the adoption of a gasoline tax. The variations in motor fuel speci- fications and methods of test have been pronounced in the several States. The Bureau of Mines, in making certain technical studies of the rasolines marketed throughout the United States, the results of which are reported in its semiannual motor gasoline surveys and other reports, has had occasion to obtain and compile all of the present (April 1, 1931) tax and pection laws of the several States which relate to motor fuel and other petroleum products. To facilitate the use of this material and to obviate the need in most cases of reading the complete text of the laws as published by the States, the pertinent information was arranged in tabular form for cly reference. 3 Although digests of States gasoline tax laws' are available and copies of the complete laws can be obtained from the State agancies in charge of the enforcement of gasoline tax and inspection laws, it is believed that

Jan 1, 1932

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 Walter W. Kaufman

This User&apos;s Manual, extracted from information contained in the Final Report for the above referenced project, outlines test procedures to measure the braking capabilities of underground non-coal rubber-tired mining equipment. Methods to interpret test results, recommendations for safe braking capabilities, and basic techniques to improve braking systems and road surfaces are also discussed. Possible applications for runaway vehicle protective devices other than braking systems are reviewed. Also included is a listing of mining equipment and brake component manufacturers who supply the majority of equipment to the United States non-coal mining industry. In conjunction with this list of manufacturers, a general tabulation of brake related specifications appears for vehicles observed during stopping tests conducted underground.

Jan 1, 1977

By D. S. Colby

The productive capacity of natural-gasoline and cycle plants in the United States as of January 1, 1952 was 811,596 barrels per day, an increase of 163,691 barrels per day since the last survey on January 1, 1950. The rate of growth during these 2 years has been 12 percent per year s only slightly below the maximum rate, recorded from 1948-50. This survey, for the first time, presents capacity data on a barrel rather than a gallon basis. Also, for the first time, a break-down of capacity by products has been obtained. The combined LP-gas producing capacity of plants and fractionators equaled 382,790 barrels per day, 47 percent of the total industry capacity tor all products. During January 1952, LP-gas and natural gasoline and other products were each produced at the rate of 76 percent of the January 1 capacity.

Jan 1, 1952

By W. R. K. Wu

This Bureau of Mines report presents a statistical study of the repeat abilities of coal-plasticity parameters obtained in the tests with the Gieseler plastometer and the Audibert-Arnu and Hoffmann dilatometers. Repeatability is expressed in terms of one or two standard deviations for the differences between duplicates. The statistical method employed here is summarized. Results are tabulated for the temperature and nontemperature parameters of the three tests.

Jan 1, 1970

Comparative tests of four coals used industrially for coke production have been made by three laboratories of the Federal Bureau of Mines, each using its standard equipment and procedures for evaluating coal for coking. Two of the coals were blends used in the western and eastern sections of the United States, the third was a strongly coking coal widely used for producing coke in Alabama, and the fourth was a blend typical of those used for producing foundry coke in the Birmingham district. The coals used and the cokes produced from them covered a wide range of chemical and physical properties. The tests used at all three laboratories for determining the physical properties of the cokes were made according to ASTM (American Society for Testing Materials) methods. The excellent agreement found for the physical properties of the cokes indicated that, for the coals tested, the BM-AGA (Bureau of Mines-American Gas Association) 18-inch circular retort used at Pittsburgh, Pa" the 14-inch slot-type oven used at Denver, Colo., and the 17-inch slot-type oven used at Tuscaloosa, Ala., were substantially equivalent for evaluating coals for production of coke. Thus, added value is given to data obtained previously and independently at these three Bureau laboratories. INTRODUCTION Laboratory equipment to produce coke for evaluation has not been standardized by the industry. The results obtained with anyone design of equipment have been regarded as showing only the relative values of coal to produce coke of the requisite quality. Few systematic studies have been made to correlate results obtained in different types of equipment. Results of one, in which the Bureau of Mines participated, were published recently.2/ This

Jan 1, 1961

By Hal J. Kelly

A picture of the ceramic industrial potential of the Pacific Northwest States is presented by reviewing the present ceramic industries, raw-material resources, and current market demands. A resume is given of the industrial plants manufacturing ceramic ware as well as available information on raw-material resources. No attempt was made to prospect for new deposits but rather to evaluate, insofar as possible, those already known. Since much of the industry is concentrated on the Pacific coast, most of the information available on resources concerns deposits in that area. Large, undeveloped districts in Montana and Idaho, however, offer promise of larger reserves of ceramic raw materials. Average annual production, some operating costs, and annual power consumption are given for each of the plants. Production and some cost figures are listed to show the limited nature of the present industry and to suggest fields open for new development.

Jan 1, 1956

By J. F. McIlwain

As part of its goal to minimize the requirements for critical materials, the Federal Bureau of Mines has investigated the consolidation of an iron-base superalloy (20 pct Cr, 5 pct each Ni and Mn, 1 pct each C, W, Mo, and Cb, and the balance Fe) and its modifications by powder metallurgy (P/M) techniques. Vacuum-atomized, prealloyed powder was used. Consolidation was by sintering of cold-pressed alloy powder, or by forging plus rolling or extrusion of canned powder. Several commercial lubricants were evaluated in the pressing operation. At 50-tsi compacting pressure with up to 3 wt-pct lubricant, green strengths did not exceed 1,000 psi. Powder sintered just below the solidus temperature attained a tensile strength of 69,000 psi and 4 pct elongation. Liquid-phase sintering produced higher densities, lower tensile strengths, and nil ductility. Canned powder was forged and rolled at 1,200° C, yielding a 100-hr rup¬ture strength of 9,800 psi at 815° C and a room-temperature tensile strength of >130,000 psi at 6 pct elongation. Heat treatment of modified P/M iron-base alloy containing 0.63 pct C resulted in a 100-hr rupture strength of 17,000 psi. Oxidation resistance at 805° to 815° C of the forged and rolled P/M iron-base alloy was similar to that of the cast iron-base alloy and supe¬rior to conventional stainless steels.

Jan 1, 1981

By D. E. Shanks

This U.S. Bureau of Mines (USBM) research simplified an earlier hydrogen chloride (HCI) leach-sparge process developed by the USBM to recover reduction-grade alumina from domestic kaolin clay. Improvements were made by decreasing the initial leaching acid concentration from 25 to 20 pet, decreasing the leaching time from 1 to 2 h to 15 to 30 min, eliminating the solvent extraction step for Fe removal, and eliminating the step to recover the AI content of the bleedstream circuit. A 10-cycle bench-scale experiment of the simplified process showed that the ferric chloride (FeC13) concentration built up to 9.3 g/L in the recycle stream. This did not interfere with any of the unit operations or final alumina product purity because Fe forms stable soluble chloride complexes when sparged with HCI and is easily washed from the large aluminum chloride hexahydrate (ACH) crystals. The reduced leaching time and acid concentration did not decrease Al extraction.

Jan 1, 2010

By Raymond P. Maloney

The Bureau of Mines investigated the White Mountain mercury deposit, in the Kuskokwim River Basin, to better determine the extent of mercury mineralization and to encourage its development by private industry. A program of diamond drilling, augering, bulldozer trenching, and sampling was carried on during four field seasons, from 1960 to 1963, inclusive. Significant amounts of cinnabar, with only trace amounts of arsenic and antimony, occur in dolomite over an area about 4,000 feet long and 1,500 feet wide. The deposit differs from other mercury deposits in the Kuskokwim River Basin by the absence of silica-carbonate and rhyolite intrusives. Small-scale mining was started in 1963 as the result of Bureau investigation and continued during the summers of 1964 and 1965. The investigations indicate that open pit mining might be the most feasible method of working this deposit.

Jan 1, 1967

By E. C. Lane

This paper is the first part of a report giving the results of the Bureau of Mines&apos; twenty-third semiannual survey of motor gasoline marketed in the United States. A companion report, Part II, is in preparation and will give a more detailed discussion of the whole survey. Results of the determination of copper-strip corrosion, color, sulphur content, copper-dish evaporation residue, and gum content as given by the Bureau of Mines steam-oven method will be presented in the second paper, which will also include the prevailing retail price and the tax at the time the sample was taken. This paper deals specifically with data relative to gravity, Reid vapor pressure,5 and distillation (method 100.13).6 The samples tested were divided into "competitive-price gasolines" and "premium-price motor fuels," a method of presentation that was begun with the twenty-second semiannual survey.7 A total of 312 samples were collected from service station pumps in 20 cities throughout the United States. Of this number of samples, 207 were "competitive-price gasolines" and 105 were "premium-price motor fuels." All of the samples were collected in March, 1931, and analyzed at the Petroleum Experiment Station of the United States Bureau of Miner at Bartlesville, Okla.

Jan 1, 1931

By Walter Wood, J. T. H. Cannarella, H. F. Yancey, R. E. Zane

More than 50,000,000 tons of bituminous coal and probably about the same quantity of anthracite are cleaned annually in the United States by wet methods. The water, fine coal, and impurities from the water used for washing ordinarily are recovered by moans of various forms of settling tanks. Settling and clarification may be hastened markedly, thereby greatly increasing the capacity of clarification equipment already installed, by the addition of substances to the washery water that cause the fine particles in suspension to agglomerate and thus settle more rapidly. This phenomenon, although well known and applied in other fields, has been used at only a few coal washeries in the United States. It is widely employed, however, as an aid in the recovery or disposal of fine coal or impurities, as a means of preventing, stream pollution, and to enable reuse of washery water at many plants in Europe. Pioneering work in the United States has been done principally by two companies -- the Pittsburgh Coal Co., in Pennsylvania, 6/ and the Pacific Coast Coal Co., in Washington.

Feb 1, 1940

By C. W. Owings

"Coal may be and has been hauled safely at approximately the same cost with permissible2 storage-battery locomotives as with trolley, cable-reel, crab-reel, or nonpermissible storage-battery locomotives. While in general, thinking mining men readily admit the relative safety of the permissible storage-battery locomotive there are some persons who question the safety of this type; however, the greatest opposition to the widespread use of storage-battery locomotives is from those who believe them to be more expensive to operate and to be more expensive in first cost than the trolley or cable-reel locomotive. Data collected during a comprehensive study- of storage-battery and wired transmission of power in some Pennsylvania and West Virginia coal mines indicate that there is but little difference between the cost of hauling with cable-reel or with storage-battery locomotives. It would appear that if this fact were mere generally known mine operators of the more progressive type would install such equipment and avail themselves of greater safety in hauling coal.The need for greater safety in haulage in coal mines is readily understood when it is considered that during the 12 month period, July 1, 1929 to June 30, 1930, trolley or cable reel gathering locomotives caused four explosions in which 407 lives were endangered, 11 persons were injured, and 30 lives were lost. Still another disaster was averted by the vigilance of a fire boss, who discovered a stratum of gas 3 feet thick at the top of an entry into which a gathering locomotive was about to enter. Other explosions not resulting in any fatality probably have not been reported. In addition numerous fires have been caused by trolley or cable-reel locomotives, and these fires probably would have been avoided had permissible storage-battery locomotives been used."

Nov 1, 1930

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 E. J. Lintner

This paper is one of a series being prepared by the United States Bureau of Mines describing clay mining, crushing and grinding methods, and costs, at various operations throughout the United States. These papers are designed to disseminate technical information regarding methods used. The, cost tabulations represent local operating expenditures only and not total production costs. It is recognized that publication of total production costs may in many instances cause embarrassment to the individual operator as well as to the industry as a whole. On the other hand, operating costs are essential to the technical discussion and study of the methods employed. The attention of the reader is specifically called to this differentiation in order that no misunderstanding of the scope of the cost tabulation shall ensue. The following report deals specifically with the methods employed by the Evans Pipe Co., Uhrichsville, Tuscarawas County, Ohio. The author wishes to acknowledge the assistance of the following company officials: T. J. Evans, II, president; T. J. Evans III, vice president and general manager; and L. P. Young, general superintendent.

Jan 1, 1936

By J. J. Hoeppner

Lignite samples were collected so as to be widely representative of the extensive deposits in the western north-central area. These were carbonized at temperatures ranging from 450° to 550° C., according, to a standardized procedure. In general, product yields varied; extremes obtained on selected samples show char recoveries on the moisture- and ash-free basis as 56.7 percent for slack lignite or "leonardite" to 80.8 percent for a concentrate of the fusain component from a typical face sample; normal lignite samples averaged approximately 70 percent. Tar-plus-light-oil yields ranged from 3.3 percent for the fusain concentrate to 11.0 percent for a normal sample, averaging approximately 8 percent; gas recoveries varied more widely both in yield and in composition, ranging, from 10.0 percent to 27.7 percent, the latter being from leonardite and quite high in carbon dioxide. Sampling was conducted with the view of representing, as nearly as possible, all beds delineated by Brant (2);4/ many are necessarily missing since collection was confined largely to worked deposits. Data presented in this report indicate a general uniformity of North-Central lignite in respect to low-temperature carbonization, with a few possible exceptions of a local nature. When processed according to the indicated conditions, maximum tar yield may be realized with minimum loss of recoverable heating value of the original coal. Natural weathering of lignite, however, does affect tar yield adversely and should be held to a practical minimum in any commercial operation.

Jan 1, 1956

By D. J. Parker

Ability to signal the hoisting engineer in shaft mines is of utmost importance from the standpoint of safety and economy. The problem of signalling from the cages and especially from the moving cages has received too little attention from mine operators; however, this problem has been given considerable thought and attention by at least one large metal-mining company in Utah which has devised successful, economical, and safe systems of signalling from the cage whether it is moving or at rest. A Report of Investigations on "Methods used in Utah for signalling mine hoists from moving cages," by C. A. Allen, then a metal-mining engineer in the Bureau of Mines, was issued in June, 1920. As this report contains interesting history of systems of signalling from moving mine hoists, and describes several systems then in use, it is here quoted in full.

Jan 1, 1929