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By H. W. Wainwright

.1. The purification pilot plant and the equipment, solution, and gas cycle used for removing hydrogen sulfide and carbon dioxide are described. 2. As sulfur recovery is necessary in any large Fischer-Tropsch plant, pilot-plant runs were made at 300 p.s.i.g. to study the efficiency of tri-ethanolamine solutions in removing selectively hydrogen sulfide from gases containing varying amounts of carbon dioxide. 3. Aqueous solutions of TEA of 20, 30; 35, and 50 percent were investi¬gated. Data indicate that 30 to 35 percent is the optimum concentration if both selectivity and economy are considered. Slightly better selectivity is obtained with the.20 percent solution, but steam consumption is greater owing to the higher solution rates. Results from our pilot plant runs indicate that a 50 percent solution not only produces an acid gas of lower hydrogen sulfide content but also requires high solution rates to effect hydrogen sulfide purification. 4. Data from 37 runs using TEA are presented in tabular form. In addition, the data are correlated and presented in three sets of curves. By using these curves, it is possible to calculate the compositions of the purified and acid gases for various raw gas mixtures. 5. In cooperation with the Southern Natural Gas Co., investigations were carried out at 300 p.s.i.g. on the simultaneous removal of hydrogen sulfide and carbon dioxide, from gases using various concentrations of diethanolamine. 6. Data from 17 runs employing 20, 30, and 40 percent DEA are reported in both tabular and graphic form. 7. A comparison of the data from one DEA run made at 200 p.s.i.g. with those from the runs operating at 30O p.s.i.g. shows float the absorption capacity of the solution, and, hence, the steam requirements per gallon are about the sage for both pressures. .The only real advantage of the higher pressure is the additional volume of gas that can be treated. 8. The quantity of steam needed to reactivate fouled TEA and DEA solutions increased as the reactivator pressure was increased about 1,0 to 1.1 pounds of steam was required for each gallon of circulating solution when the reactivator was operated at 5 p.s.i.g. 9. A curve is included that shows the effect of the hydrogen sulfide con-centration in a lean 35 percent TEA solution on the hydrogen sulfide content of the purified gas and on steam consumption for reactivation. 10. Both TEA and DEA reduced the organic sulfur content of the raw synthesis gas considerably. Analyses of the lean amine solutions showed a gradual build up of sulfur compounds, indicating that the compounds formed by the amines and organic sulfur do not break down under the ordinary operating conditions of the reactivator. 11. Considerable operating difficulty was encountered in the pilot plant owing to foaming of the amine solutions. Laboratory experiments in which the effectiveness of certain antifoam agents was studied showed Alkaterge C to be most promising for the particular conditions studied.

Jan 1, 1952

By D. M. Lewis, J. K. H. Ma, Y. Rojanasakul, J. Y. C. Ma, J. H. Kang, V. Castronova

"Tetrandrine is a bisbenzylisoquinoline alkaloid which has been shown to exhibit antifibrotic activity against silicosis. Tetrandrine is characterized by its strong binding to alveolar macrophages and inhibition of particle-induced respiratory burst activity in these phagocytes. In contrast, tubocurine and tubocurarine are structurally similar to tetrandrine but exhibit little effect on fibrosis or activation of alveolar macrophages. The objective of the present study was to test the effect of tetrandrine on macrophage production of monokines in response to occupational dusts, and to determine tetrandrine's effect on monokine-medicated cell growth using a mouse thymocyte proliferation assay and lipopolysaccharide (LPS) as a positive control. Stimulation of alveolar macrophages by respirable silica dust resulted in a release of monokines which caused a fourfold increase in thymocyte proliferation. Coal dust, on the other hand, had no effect on macrophage production of this cytokine. Tetrandrine was found to exhibit a dose-dependent inhibition of monokine release from both silica and LPS-stimulated alveolar macrophages. In experiments where thymocytes were directly treated with tetrandrine, a dose-dependent inhibition of thymocyte proliferation was noted with both interleukin-1- (IL-1) specific and nonspecific mitogenic (concanavalin A) actions. In contrast to the inhibitory potency of tetrandrine, tubocurarine was found to have no effect on either the production of monokines by LPS-stimulated alveolar macrophages or IL-I-mediated thymocyte proliferation. These results provide a correlation between the ant:fibrotic effect of tetrandrine and inhibition of macrophage activation. INTRODUCTIONThe pathogenesis of chronic pulmonary fibrosis caused by inhalation of occupational dusts has been associated with abnormal activation of alveolar macrophages such as the release of various cytokines capable of inducing fibroblast proliferation and collagen synthesis. These macrophage-derived cytokines include interleukin-1 (IL-1), tumor necrosis factor (TNF), platelet-derived growth factor (PDGF), transforming growth factor-B (TGF-(B), macrophage derived growth factor (MDGF), and interferon [1, 2].Interleukin-1 is a major macrophage-derived cytokine that has been shown to exhibit multiple biological effects on a variety of target cells. It is known to cause leukocyte [3, 4] and endothelial cell activation [5, 6], and to affect the synthesis and maintenance of the extracellular matrix by stimulation of fibroblast proliferation [7-9], synthesis of collagens [10] and gluco-saminoglycans [11], and prostaglandin E2 production [12]. In addition, IL-1 plays an important role in the initiation of an immune response through its direct activation of lymphocytes and stimulation of the production of other cytokines, such as interferons and hemopoietic colony-stimulating factors, needed for the expression of an immune response [13]. As a major cytokine in the immune-inflammatory sequela, IL-1 is also produced by epidermal, epithelial, lymphoid, and vascular tissues after infection, injury, or antigenic challenge [14]. Agents such as lipopolysaccharide (LPS), phorbol myristate acetate (PMA), immune complexes, and particulates are known to activate the synthesis and release of IL-1 by monocytes and macrophages [15]. These substances also trigger intracellular signals leading to altered arachidonic acid metabolism. Although the mechanism is still not clear, prostaglandins have been shown to suppress IL-1 translation via the induction of cyclic adenosine-monophosphate (CAMP), whereas leukotrienes produce a positive signal for IL-1 production [13]."

Mar 1, 1992

By Raymond F. Helinski, Linda J. McWilliams, Sean Gallagher, Thomas R. Battenhouse, August J. Kwitowski, John R. Bartels, Dean H. Ambrose

This report examines the boom arm vertical speed for roof bolting machines to study a moving boom arm appendage at different speeds during different work scenarios. The goal of this study is to determine the impact of the appendage speed on the likelihood of the operator's hand, arm, head, or leg making contact, such as touching the moving appendage. The overall research goal is to reduce workers' risks to injury from exposure to underground mining machinery. Accident investigation reports from the Mine Safety and Health Administration do not usually contain enough information to aid in studying this problem, and lab experiments with human subjects are not feasible because of safety issues. As an alternative, researchers used a unique computer simulation model that uses a virtual human, vision tracking, and generates random virtual human motions and risky work behaviors. By using specialized software to simulate the computer model, researchers accurately identified potential hazards of tasks where it is not possible to perform experiments with human subjects. Results of a frequency distribution analytic approach show that, regardless of other variables, contact incidents were always greater when the boom was moving up, always greater on the hand, and always greater or the boom arm part of the machine. The reason why the subject experiences more contacts when the boom arm is moving up rather than down is that more risky behaviors occur during drilling and bolting when the boom is ascending. Results of a cross-tabulation analytic approach show that the 25th-percentile operators experienced more contacts than other operator sizes and had most of their contacts during a boom speed of 13 in/sec. The hand-on-boom behavior during drilling and bolting tasks experienced more contacts than other work behaviors, and both tasks had most of their contacts during speed 13 in/sec. The 60-in seam experienced more contacts than other seam heights and had most of the contacts during speed 16 in/sec. For univariate logistic regression models, seam height is the most important predictor of the probability of a contact. However, a multivariate logistic regression model predicted contacts are more likely with the both-knee work posture in the 60-in seam, a 25th-percentile operator compared to a 55th-percentile operator, and speeds 16 and 22 in/sec compared to 7 in/sec. Results of a survival analytic approach suggest that controlling the boom speed is the most important factor in determining the risk of an operator making contact. Based on the data collected, boom speeds greater than13 in/sec result in a substantial increase in risk to the roof bolter operator making contact. Speeds less than or equal to 13 in/sec are associated with a more modest relative risk of making contact, which represents a decrease in potential hazard. Virtual operator's response time has little effect on the number of contacts experienced. The mining industry can use the information in this study to reduce the likelihood that roof bolter operators will experience injury due to contact with a moving roof bolting machine's boom arm.

Jan 5, 2005

By R. D. Leitch, W. P. Yant

"In the course of another investigation4 during 1926 and 1927, samples of water collected from a few abandoned coal mines indicated that their drainage was usually lower in acidity than water from active mines in the same locality. In order to determine whether this condition might have a bearing on the advisability of sealing abandoned mines, a number of such mines were visited, samples of drainage were collected, and as much information- as possible was obtained from officials of the mining companies and older residents of the district. The results of this work are the basis of the present report.The authors are indebted to E. W. Robertson, F. F. Spowart, J. H. Nagle, and W. D. Adams of the Northwest Mining & Exchange Co.; E. M. Fasset, Fred Lane, Wm. Humphreys, and Dr. T. A. Hutchison of Brockway, Pa.; C. W. .Faulk of the Shawmut Mining Co.; James Hau of Kersey, Pa., and to others for information received; and to Dr. R. R. Sayers of the Bureau of Mines, under whose direction the work was conducted.The Lower Kittanning is the most important bed in the locality studied. A great many of the abandoned mines examined are in this bed, and nearly all of the present active ones are. The Upper Freeport bed is also mined to some extent, and a number of the abandoned mines formerly worked this bed. As only three active mines are now (1927) working the Upper Freeport, the comparison of acidities is necessarily limited. Of these three, one had been idle since 1922 until shortly before it was sampled.The location of most of the mines was already known from previous work, but some of them had to be located by following up streams known to contain acid waters. A sample of the- outflow was collected in self-sealing bottles known as ""citrate bottles"" for the determination of dissolved oxygen by the Winkler method.5 Another sample was taken for the determination of acidity according to standard methods of water analysis.6 Ferrous iron was determined at the mine or very soon after taking the sample by titrating with a standard solution of potassium permanganate in acid solution. The hydrogen-ion value was determined by a standard double-wedge comparator.7From the total acidity values in each sample, which are the most important values, the total iron was calculated on the assumption that acidity as sulphuric acid was due to dissolved ferrous sulphate. This assumption is commonly made for mine waters, but is inaccurate to the extent that free acid is already present, and some of the iron is present as ferric, rather than ferrous, sulphate. The amount of ferrous sulphate may be a rough measure of the extent to which oxygen is lacking within the mine. The permanganate titrations just mentioned showed what part of this total iron was in combination as ferrous sulphate, and the difference .was assumed to be that in combination as ferric sulphate, after correcting for the amount of free acid already formed as shown by the titration values."

Oct 1, 1928

By R. R. Sayers

"According to the dictionary,3 an accident is an event that takes place without one's foresight or expectation, often an undesigned, sudden, and unforeseen occurrence of an afflictive or unfortunate character. However, actual experience with accidents, the second most important cause of death in the United States,4 and a more extensive and scientific inventigation of their causes indicate that from 75 to 90 per cent of accidents are avoidable.5 This is borne out by the results of a three-year study of the accident records of 64,000 motor vehicle operators in New York6 which show that certain drivers are prone to accidents, that accident experience is traceable to certain causes, and that accidents don't just ""happen,"" It is estimated that 97,000 persons were killed by accidents in the United States in 1929 and 15,000,000 were injured. Of these about 23,000 deaths were due to so-called industrial accidents. In a list of accident rates by industries, compiled by the National Safety Council7 from reports of member establishments, mining heads the list, in both frequency (74.43 per 1,000,000 man-hours worked) and severity (9.9 days lost per 1,000 man-hours worked). These figures are very much higher than for any other industry; theindustries showing figures most comparable to mining are meat packing with a frequency rate of 55.94 and a severity rate of 1.47, construction with a frequency rate of 50.41 and a severity rate of 4.62, and refrigeration with a frequency rate of 43.35 and a severity rate of 3.04.While there is no way to determine the actual cost of all accidents from a monetary standpoint, estimates indicate that the cost will run into hundreds of millions of dollars annually.Cost of accidents in metal mines.- The United States Bureau of Mines obtains accurate figures on the number of lost-time nonfatal accidents as well as fatal accidents in the metal-mining industry.8 In 1926 the metal mines employed 127,823 men; 430 men were killed and 30,350 men received lost-time but nonfatal injuries as a result of accidents. Each of these fatal and nonfatal injuries averaged 114 days lost time, computing a fatality as 6,000 days lost time. This is equivalent to 3,523,944 days time lost due to accident, or at $5 per day per man, to a wage loss of $17,619,720. Deducting one-ninth of this figure for compensation paid, the metal miner loses in wage annually about $15,700,000, or about $122 per individual. This average loss per individual includes the cost of fatal accidents reckoned at 6,000 days or $30,000, but even if the loss in time due to fatal accidents be deducted, the average cost to each individual metal miner each year for nonfatal accidents is about $32. Estimating the loss to the metal-mine employer as about the same as that to the employee, the annual cost of metal-mine accidents to the employer is about $15,700,000 and to the employer and miner is $31,400,000."

Oct 1, 1930

By Donald R. Johnson

Apparatus providing simultaneous differential thermal analysis, thermo-gravimetry, and evolved gas analysis, has been developed by the Bureau of Mines specifically for thermal study of oil shale and other solid, natural fuels. The apparatus is described in detail, and simultaneous analyses on a single sample of an oil shale mineral, nahcolite, and a thermal analysis demonstration compound, calcium oxalate monohydrate, are presented to demonstrate the instrument's capabilities.

Jan 1, 1970

By H. R. Shell

Fluorphlogopite mica was synthesized from inexpensive and abundant olivine, clay, feldspar, and sand (plus K2SiF6). The raw materials were melted in crucibles and in an internal resistance electric furnace. The melts yielded >95 percent mica. The major difficulty encountered was incomplete settling of the highly dispersed ferroalloy. This problem was not completely solved. Reducing agents tried in melts of 300 to 400 pounds were carbon, silicon, and silicon carbide. Carbon slowly reduced the iron of the raw materials, with much fuming. Silicon apparently was oxidized ahead of the melting and was ineffective under the conditions obtained. By far the best reducing agent was silicon carbide. With silicon carbide, fuming did not occur and ionic iron content of the mica flake approached 0 percent. However, even with SiC, the highly dispersed globular iron did not completely separate from the mica portion. The fluorphlogopite made during this investigation should be suitable for metallurgical use. A byproduct ferroalloy containing about 5 percent nickel, 3 to 5 percent chromium, and some cobalt was obtained. Because of the highly dispersed metallic ferroalloy, the mica was not deemed suitable for electrical or electronic uses.

Jan 1, 1962

By R. L. Rough

Photoelastic, wire resistance, and borehole-deformation gages were used to measure the in situ strains when an outcropping Black Hand Sandstone Formation in Hocking State Forest, Hocking County, Ohio, was overcored to stress-relieve the surrounding sandstone. Strains transmitted to the photo-elastic gage did not produce isochromatic patterns suitable for quantitative analysis. Strain readings from the wire resistance gage indicated tensile-strain loading during overcoring; readings from the strain-gage bridges in the borehole-deformation gage indicated compressive-strain relaxation during overcoring. The magnitude and orientation of the computed stress fields obtained from both gages were comparable when the corresponding tensile and compressive elastic moduli were applied. Stresses computed from deformation and resistance gages at depths to 5 feet showed the maximum stresses to range from 1.042 to 2.121 times greater than the minimum stresses. The bearings of principal stresses calculated from the deformation gage readings varied between N 61° E and N 83° E; the wire resistance strain gage bearing computations varied between N 68° E and N 82° E. Measurements of in situ strain in sandstone were shown to have promise but to require further development in field technique that could likely be achieved through experience.

Jan 1, 1971

By Bradley V. Johnson

This publication summarizes the in-house and contract research and development projects conducted since 1974 by the Bureau of Mines for the control of noise and vibrations from surface mine blasting.

Jan 1, 1982

By D. Harrington

The code of hoisting signals for use in mines hoisting from one level, as suggested in this publication, is submitted to induce consideration of this subject by representative groups of the coal-mining industry, such as the lithe Inspectors Institute of America, National Coal Association, American Mining Congress, and others, as well as to -furnish a code of signals for use in those mines operated in States that do not have regulatory hoisting codes in their mining laws, or regulations. The signal codes described in this publication apply only to mines hoisting from one level and to slope mines. Mines that hoist from more than one level are referred to Bureau of Mines Information Circular 7289 Suggested Hoisting-Signal Code For Metal Mine Shafts, which suggests signals for hoisting from various levels or stations.

Jan 1, 1944

By C. H. Herty

As the problem of inclusions in steel has become increasingly important, more and more attention has been paid to the source of the oxide inclusions in steel. In killed steels the oxide inclusions are traceable to the reaction of deoxidizers with the iron oxide dissolved in the steel during the refining period of the open-hearth heat. In a large class of steel known as "rimming steel" the action of the steel during solidification depends entirely on the gas evolved, and this evolution in turn is controlled by the amount of iron oxide in the liquid steel in the mold. It is therefore of great importance to be able to determine the amount of iron oxide dissolved in steel and to devise methods for the control of iron oxide in any class of steel. The object of the present investigation was to obtain a true value of the oxygen content of liquid steel. If the steel has not been deoxidized, the greater percentage of the oxygen is present as iron oxide in solution.

Jan 1, 1932

By Harold L. Rhodes

The Bureau of Mines has developed a method for determining the H2S content in natural gas samples. A gas chromatograph with a flame photometric detector was used to analyze samples with H2S concentrations ranging from 5,000 ppm to a minimum detectable limit of 0.01 ppm. A mass spectrometer was used to analyze samples containing H2S in amounts greater than 5,000 ppm. Methods are presented for preparing containers for H2S samples and for preparing standards using partial pressure and weighed standard methods, Sample collection techniques are discussed, as are analytical results which illustrate the loss of H2S while in the sample container and provide a basis for evaluating containers used for sampling and standard preparation.

Jan 1, 1979

By Donald J. Barnes

There are no producing or developing mines in the study area. The only mineral production was stone from a basalt deposit near Indian View Point. Cinders and sand and gravel have been produced from deposits within 1/2 mi (0.8 km) of the boundary. Stone, sand and gravel, and cinder deposits inside the area are not considered resources because equal or better quality material is found closer to markets. The study area has no known oil and gas, coal, geothermal, or other energy related deposits. However, in 1982 application was filed on 25,000 acres (10,125 ha) of petroleum and on 15,000 acres; (6,0/5 ha) of geothermal leases.

Jan 1, 1983

By J. L. Eakin, J. P. Powell

"The increased costs of exploration and drilling of new oil fields and the continued success of water flooding in nearly depleted oil fields have created a demand for information on the results obtained from individual projects. The Bureau of Mines has published several reports concerning water-flood activity in the Midcontinent area and at the request of the industry has continued to collect and disseminate this information. This report was written in response to these requests. It describes in detail the water-flooding projects in Anderson, Franklin, Linn, and Miami Counties, Kans., and includes methods of water treating and the results obtained. The production histories of each county and many water-flood projects are shown graphically from the date of the first development. Maps of most of the major projects, showing their status as of January 1, 1953 are presented also.The practice of injecting water to stimulate oil production was legalized in Kansas in 1935, and the first water-flooding project authorized in this four-county area was initiated by the Texas Co. in December 1935 in Linn County. Forty-nine projects2/ initiated in the area to January 1953 are estimated to have recovered approximately 10 million barrels of oil that would not have been produced by methods used previously. About 7,900 productive acres had been, or are, flooded by these projects, and approximately 136 million barrels of water had been injected.These four counties in the eastern Kansas shallow production area3/ were an important factor in the early history of the Kansas oil and gas industry. This position has been maintained from the very beginning through the early period of vacuum and air injection and into the era of water flooding. The location of the area and the relative position of the four counties and water-flooding areas in each are shown in figure 1.The first drilling for oil in this area in 1860 resulted from investigations of the existence, and use by the Indians, of so-called tar or oil springs. The first wells drilled were nonproductive, and the impending Civil War caused the search for oil to be discontinued. In 1884 a few shallow oil wells were drilled near Paola, and completion of several gas wells near that city led to subsequent drilling of an oil well, which was completed in June 1885, having an initial flow of 10 barrels of oil daily.In 1904 the original Paola gas field became a good oil-producing field. In 1905 the Rantoul field in Franklin and Miami Counties was opened; and drilling activity spread throughout the adjoining area, resulting in development of several shallow oil pools in Linn and Anderson Counties. The first ""shoestring"" pool in eastern Kansas to produce oil was probably the Paola or Pressonville shoestring, which was discovered in 1917. The rate of oil production from the area declined until 1919, when the Centerville shoestring pool was discovered. Discovery of the Colony gas field in 1921 was followed within a few months by drilling of the Garnett and Garnett and bush City shoestring pools. The Schermerhorn pool (now part of the Centerville field) s discovered in 1927, and the Kincaid shoestring pool was first drilled in 1931. The oil-production histories of the individual counties are discussed separately."

Jun 1, 1953

By Knox Van Dyke, Vincent Castranova, Lixin Wu, Mark J. Reasor, James M. Antonini

"One of the proposed mechanisms involved in the pathogenesis of silicosis is that inhaled silica dust activates a ""respiratory burst"" in pulmonary phagocytes, such as macrophages and neutrophils. This increase in oxidative metabolism results in enhanced generation of reactive oxygen species which if produced in excess, would overwhelm natural defense mechanisms and cause damage to the lung parenchyma. This damage would then result in scarring, fibrosis, and decreased gas exchange.Weiss and LoBuglio' have listed several oxygen species produced by phagocytes which may be involved in cellular injury. These oxidants include superoxide anion, hydrogen, peroxide, hydroxyl radical, and hypochlorous acid. Superoxide anion (0;) is generated from molecular oxygen by the plasma membrane bound enzyme NADPH oxidase according to the following reaction:Once generated, superoxide anion can form hydrogen peroxide:In the presence of myeloperoxidase and halide, hydrogen peroxide can form hypochlorous acid:Superoxide and hydrogen peroxide can also form highly reactive hydroxyl radicals. Hydroxyl radicals can be generated slowly by the Haber-Weiss reaction:In addition. hydroxyl radical production can be catalyzed via the Fenton reaction:Hydroxyl radicals can also be generated from the reaction of superoxide and hypochlorous acid as follows:Recent investigations suggest that, in addition to the reactive oxygen species discussed above, nitric oxide may be a potential mediator of silica-induced toxicity.2-4 Nitric oxide (NO') can be generated by the cytosolic enzyme nitric oxide synthase according to the following reaction:NO synthase exists in two forms. i.e.. a constitutive. Ca2+-calmodulin-dependent form and an inducible. Ca2+-calmodulin-independent form. In pulmonary phagocytes. the activity of the constitutive form of NO synthase is low. However. NO synthase can be induced in macrophages and neutrophils by a variety of stimulants such as lipopolysaccharide. interferon y. chemotactic peptide, platelet activating factor, or leukotriene B4.3.5Once generated. nitric oxide can combine with superoxide anion to form peroxynitrite as follows:Peroxynitrite is a potent oxidizing agent. In addition, peroxynitrite can form peroxynitrous acid. which in turn can produce hydroxyl radical and nitrogen dioxide (all of which exhibit strong oxidizing potential) by the following reactions:Oxygen metabolites have been shown to cause lung damage in vivo.6 Such damage includes edema. leakiness of the alveolar endothelial/epithelial barriers, and airway constriction.7 Superoxide and hydrogen peroxide have been associated with membrane damage and cell lysis.8 These oxidants have also been associated with alteration of cytoskeletal structures at cell-cell junctions and elevation of transepithelial conductance in cultured monolayers.9 Macrophages or neutrophils can be stimulated by bacteria or phorbol myristate acetate to produce sufficient oxidant levels to lyse lymphoma cells.10 This cell killing is inhibited by catalase but is unaffected by superoxide dismutase. hydroxyl radical scavengers. or azide. i.e., an inhibitor of peroxidase. This implicates hydrogen peroxide as the active oxidant. Similarly. Weiss et al.11 have reported that hydrogen peroxide is critical in the death of cultured endothelial cells due to neutrophil activation. In addition. hydroxyl radicals generated by monocytes have been associated with cell injury.12 Lastly. peroxynitrite has been shown to oxidize sulfhydryl groups and to inactivate proteinase inhibitor making the lung more susceptible to damage caused by phagocytotic enzymes.' Therefore. a strong case can be made that activated pulmonary macrophages and neutrophils are capable of causing oxidant injury. This chapter presents in vitro and in vivo data indicating that silica is associated with the production of reactive oxygen species from these pulmonary phagocytes."

Jan 1, 1998

By B. R. Mohal, F. F. Aplan, S. Chander

"ABSTRACTThe wetting behavior of coal has been determined in the presence of nonyl and octyl series of nonionic surfactants containing polyethoxy groups of different sizes. The wetting behavior was determined by a modified Walker technique and contact angle measurements. The results show that the wetting rate of coal varies with coal rank, structure of the hydrocarbon chain and number of ethoxy groups in the hydrophilic group of the surfactant. A close relationship has been observed between the wetting rates and the short-time advancing contact angles.INTRODUCTIONNonionic surfactants are used in many applications to improve wettability of solids. They can be used as dispersing agents [ 1 ] or dust suppressants [ 2-5 ] and to control the flotation, flocculation, filtration and flowability of particulates. This study was undertaken to study the effect of a series of nonionic surfactants on the wetting behavior of coal. Two series of surfactants, namely, ethoxylated nonyl and octyl phenols were used. The nonyl phenol series contains a linear hydrocarbon chain containing nine carbon atoms ( CH3( CH2 )8-C6H4,- ( OC2H, ) n, where n is the number of ethoxy groups) . The octyl phenol series contains a branched hydrocarbon chain containing eight carbon atoms ( ( CH3 ) 3CCH2C ( CH3)2-C6H4- ( OC2H4) n ).Initial wetting rates — modified Walker techniqueWalker et al. [ 6 ] developed a sink test to determine the wettability of coal particles. In this technique, coal particles are dropped individually onto the surface of surfactant solutions of different concentrations, and the most dilute concentration in which coal would sink ""instantaneously"" is determined. This technique is a variation of a procedure initially developed by Draves and Clarkson [ 7 to determine the effect of surfactants on wettability of cotton fibers. In this procedure commonly known as the Draves test, the concentration of a surfactant required to give a 'sink time' of 25 s is determined.Other investigators have used slight variations of the Walker method to study the wetting of fine particles [ 8-12 ] , by measuring the time for wetting a given amount of powder. There are differences in the manner in which the time of wetting is measured, however. Some investigators measure the time for the last trace of coal to disappear [ 8,11 ] whereas others determine the time for the vast majority of particles to sink [ 10 ] . Some investigators report a wetting rate [ 11 ] which is a value calculated on the basis of the time for the 'last traces of particles to sink'. The differences in choice of criterion for wetting can result in different values for wetting rates as illustrated in Fig. 1 which is based upon our measurements of the amount of powder wetted as a function of time. The procedure for wetting rate measurements is described in the next section. The technique in which time for disappearance of the 'last traces of particles' is determined gives the smallest value for the wetting rate, while the technique in which the time for wetting of the 'vast majority' of particles is determined will give intermediate rates. The terms 'last traces of particles' and 'vast majority of particles' are usually not defined explicitly and can lead to large differences in wetting rates measured by different investigators. Since our measurements show that the wetting rates for an assembly of powder decreases with time, we have used the initial wetting rates to compare the wetting behavior of coal in solutions of different surfactants."

Mar 1, 1989

By Raja V. Ramani, Wilson Miola

"The potential health effects of quartz-bearing airborne dust in mine and mill atmospheres point to the need for the quantification of quartz content in the source material for determining the source-sink relationships and for choosing applicable control measures. While a standard method exists from a regulatory point of view for the sampling of coal mine atmospheres for determining (i) respirable dust concentrations and (ii) the amount of quartz in the samples, there is no generally accepted standard method for quartz analysis in bulk samples of coal and host rocks. Generally, the bulk sample is reduced to a powder for producing quartz analysis samples. Extensive controls arc necessary to ensure representativeness of the analysis samples when these are very minute fractions of the bulk samples. Since the amount of analysis sample is not limited, alternative methods for quartz analysis may also be tried. It is, however, necessary to adopt a procedure which will satisfy several statistical requirements to guarantee representativeness of the quartz analysis samples.In this paper, the important factors in the preparation of quartz analysis samples from the host rocks and bulk samples are discussed. The method developed to prepare the analysis samples is outlined. The results of application of the procedures are presented. The procedure developed for quartz analysis sample preparation is based on sound statistical foundations. The procedure has been validated for reproducibility and homogeneity.The current methods used for quartz analysis in powders are the P-7 infrared spectrometry and quantitative X-Ray Diffraction (XRD). Both have similar restrictions concerning the sample characteristics and operational problems, which arc intrinsic to radiation beams, device geometry, mechanics and controls of the radiation behavior. Although improvements can be made in the spectrometers and diffractometers, some of the most important steps are the procedures for analysis sample preparation from bulk samples and for calibration of the instruments. The sample preparation process is often referred to as one of grinding and sizing the bulk sample to generate the powder for the scanning devices. The particle sizes are referred to and their influence emphasized but the representativeness of the sample is assumed. Assuring sample representativeness during the sample preparation procedures is critical.For the sampling of airborne respirable dust in coal mines, the collection devices, the collection procedures and the analysis procedures are defined. This is not true for bulk samples where weights must be reduced thousands of times to generate the analysis samples for the scanning devices. The specifications to be developed may include bulk sample amount, sample reduction procedures, sample particle size distribution and sample amounts. However, the common problem of insufficient sample amount which is often encountered with mine airborne dust samples need not exist for bulk samples. Further, the same bulk sample can yield analysis samples for several experiments. The latter, of course, requires sample homogeneity.Three concepts are important in the selection of any procedure for sample preparation and analysis. These arc accuracy, reproducibility and representativeness. The adopted procedure has to guarantee a homogeneous sample representative of the population, a defined level of accuracy and reproducibility. Important statistical concepts are embedded in these requirements, particularly with respect to estimation and dispersion errors. Accuracy and reproducibility are totally different though not independent concepts. Estimation is related to accuracy and the true value. Dispersion is related to reproducibility and is measured by the classical statistical standard deviation of the distribution of a series of measurements or analysis performed over the same lot or analysis sample. The dispersion variance (or dispersion error) does not tell a"

Mar 1, 1992

By C. P. Fang, V. A. Marple, K. L. Rubow, P. H. McMurry

"It has been known for some time that sizes of aqueous particles may be affected by flow-induced relative humidity (RH) changes. The RH of air flowing through an impactor decreases as a result of pressure drop through the impactor and increases because of aerodynamic cooling within the high-speed jets, as illustrated in Figure 1. Because the sizes of aqueous particles depend on RH, the impaction stage on which such particles are collected may be different from the stage where they ought to be col¬lected, based on the particle size at the sampler inlet.Fuchs (1980) reviewed literature on water vapor condensation in impactors. The reviewed impactors operated at jet velocities of 100-250 m/s. Particle size increases ow¬ing to water vapor condensation were found in all cases. In one case (Khorguani et al., 1970), it was found that very small droplets (Dp <_ 0.02 um) containing sodium chloride and silver iodide were collected in an impactor with a cut point of 0.32 µm and a jet velocity of 100 m/s. Fuchs believed that such particles could not be captured in an impactor without having been enlarged by condensation. Winkler (1974) sampled at¬mospheric dust with a rectangular nozzle impactor that had a nozzle cross section of 0.3 x 15 mm, a cut size of 0.4 um, and an average jet velocity of 100 m/s. No adhesive was used on the impaction plate. The collection efficiency increased as air humidity was increased from 20% to 100%. The effect was especially noticeable in the increased collection efficiency for hygroscopic particles, and was attributed to condensation.Extensive theoretical and experimental research work on the distortion of the particle size distributions in impactors was done by Biswas and coworkers (1985, 1987). The impactors employed in the study were a low-pressure impactor with high jet velocity stages (Hering et al., 1978, 1979) and a conventional six-stage impactor, Sierra's model 226, operated in the incompressible regime. Ammonium sulfate aerosols were chosen for the study. In the low-pressure impactor, an orifice operating at a Mach number of 1 causes a sudden pressure drop, significantly reducing the RH in the next two stages (stages 5 and 6). This results in a 0.15-um diameter ammonium sulfate droplet shrinking to about 0.07 um at stage 5 when the inlet RH is 95%. In stage 7, the tempera¬ture drop is considerable because the jet speed is sonic. For an inlet RH of 95%, a 0.03 um droplet grows to about 0.06 um. However, the same size droplet at an inlet RH of 25% grows to only 0.04 um. For the Sierra model 226 cascade impactor that is operated with a Mach number of 0.27 at the last stage (stage VI), it was found that for an inlet RH of about 67%, particle growth would occur in stage VI. At 80% RH, both stages V and VI were affected. Biswas et al. (1987) stated that Mach number alone does not determine the size biasing; the type of aerosol, the inlet conditions, the temperature and pressure ratio, and the impactor geometry (throat length, jet-to-plate distance, etc.) must be considered for each stage in evaluating the distortion of the particle size distribution."

Mar 1, 1992

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 Nar S. Dalal, Xianglin Shi, Val Vallyathan

"INTRODOCTIONIn an earlier communication 1 from our laboratory it was reported that mechanical crushing of coal and quartz under normal air atmosphere generates of free radicals on the particle surfaces, and that these radicals decay with time, hence pointing to a higher toxicity of fresh dusts in relationship to pneumoconiosis and silicosis. More recently Fubini et al.2 have also reported the detection by electron spin resonance (ESR) of the formation of SiO. and Si-type of radicals from quartz particles crushed under atmospheric conditions. In agreement with earlier ESR studies on single crystals of quartz crushed under high vacuum ( -10-10 torr>3 and subsequent exposure to air,3 and to other gases,4 these radicals were identified2 as being formed by the homolytic cleavage of the Si-0-Si bonds and the reactions of the Si• and SiO- radical with atmosphere. Fubini et al.2 also suggested that these radicals might be involved in the mechanism of the fibrotic action by silica, either by transforming the particle surface into a selective oxidating agent or as an initiator of a sequence of reactions leading to fibrosis. Earlier Gabor and Anca5 bad reported that lipid ·peroxidation caused by free radicals on the silica surface might be involved in the red blood cell membrane damage. Thus far, however, no parallel cytotoxicity, fibrogenicity, and free radica1 studies on a given quartz dust sample have been reported, except for some earlier work from our laboratory.1·6·7 We now present more recent results obtained from parallel cytotoxicity, fibrogenicity, and free radica1 measurements on a freshly made quartz dust. The dust's free radica1 content was measured using ESR spectroscopy while its cytotoxicity potential was estimated via hemolysis. Hemolysis was employed as the toxicity test because it is a widely used method for estimating the potential of a dust for disrupting the cell membrane. 8 The fibrotic potential was followed by measuring the dust-induced lipid peroxidation, using linoleic acid as a model lipid. As discussed below, the results obtained suggest new clues to the mechanism of the quartzrelated cytotoxicity and fibrogenicity. MATERIALS AND METHODSReagentsCrystalline quartz particles with a size range of 0.2-2.5 mm were obtained from the Generic Respirable Dust Technology Center, Pennsylvania State University, University Park, Pennsylvania. These particles were crushed in air to obtain quartz dust samples with particle sizes smaller than 20 microns. We chose to work with a dust with mixed particle sizes, rather than a specific range, as an effort to simulate the mining atmosphere. An agate mortar-pestle arrangement was used for the crushing and grinding because of the close similarity of the structure of agate to that of quartz. Diethylenetriaminepentaacetic acid (DETAPAC) were purchased from Sigma. All other chemica1s were purchased from Fisher or Aldrich.Hemolysls ExperimentsHemolytic activity of silica was measured, following an established procedure,9 as the amount of hemoglobin released from a 2 % suspension of sheep erythrocytes after incubation with 10 mg of silica dust for one hour at 37 °C. The hemoglobin release was estimated via the absorbance at 540 nm using a Gioford spectrophotometer. The procedure was calibrated by substituting the silica dust by a phosphate buffer solution as a negative control (background) and O.S % Triton-X-100 as a positive control (100% hemolysis). The percentage of hemolysis was calculated as follows:"

Jan 1, 1990