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By M. S. Seehra, R. S. Pandurangi

"The interaction of amorphous silica particles with several hydrogen bonding agents (H2O,, C2H,OH, C,H,NO) was investigated by monitoring the changes in the bulk and surface IR vibrational modes of silica using photoacoustic spectroscopy, It is argued that the intensity of the silanol band at 3747 cm-1 provides (an inverse) quantitative measure of the interaction of surface groups, along with the shift in the broad hydroxyl band, the interaction following the order C,H,NO > C2H2OH > H2O.The use of IR spectroscopy to study the adsorption on solid surfaces is well documented in the literature,"" For example, hydroxylation of a clean silica surface results in the formation of the free silanol group Si-OH, with a sharp IR band near 3747 cm-1. Further hydroxylation produces a broad band near 3500 cm-1, which is believed to result from various hydrogen-bonded silanol bands leading to a multilayered surface structure of few nm.3-6 Earlier studies had indicated a relationship between the surface silanol band and various chemical activities of silica such as cytotoxicity,7-9 catalysis,10-12 and others.13 Recent studies from our group14-in which the intensity of the silanol band and cytotoxicity of silica, heat-treated at various temperatures up to 1095°C, were investigated-have provided a strong correlation between cytotoxicity and intensity of the silanol band.Coating of silica by PVPNO (polyvinyl-2-pyridine N-oxide with the empirical formula C7H8N0), a strong hydrogen bonding agent, is known to reduce the cytotoxicity of silica, presumably by chemically blocking the silanol groups from phospholipids.15 This interaction of the hydrogen bonding agents with the silica can be studied by IR spectroscopy, and Knozinger16 and Rouxlet and Semples17 have used transmission IR spectroscopy to study the effect of various chemicals on the surface IR modes of silica. However, one of the major disadvantages of transmission IR spectroscopy is that the sample preparation (grinding and mixing with KBr and pelletizing) usually distorts the surface modes (see, e.g., Ref. 14) and there is always a doubt about the effect of the sample preparation on the measured properties, In recent years, photoacoustic (PA) spectroscopy has become the technique of choice for studying the IR spectra of samples in their natural state, since no sample preparation is necessary.18,19 Moreover, according to a recent paper,20 the relative intensity of the surface modes in PA spectroscopy of silica particles is much higher than that in transmission FT-IR spectroscopy. Consequently PA spectroscopy is ideal for studying the surface chemistry, In this work, we have used PA spectroscopy to investigate the interaction of three hydrogen bonding agents (C7H8NO, C2H5OH, and H20) with the silica surface by monitoring changes in the surface IR modes, Our results show that the surface IR modes get perturbed to a larger extent than the bulk IR modes in interaction with the hydrogen bonding agents, Moreover, whereas in the earlier studies, the shift of the broad silanol band near 3500 cm-1 was used as a measure of the interaction with hydrogen bonding agents,16,17 here we show that the relative decrease in the intensity of the sharp silanol band near 3747 cm-1 also serves as a quantitative parameter for the relative surface coverage and surface modification, Details of this work are given below,The Cab-O-Sil samples of silica used here were obtained from the Cabot Corporation of Tuscola, IL, In our earlier studies,14,20 we have shown these particles to be amorphous and about 0.05 am in size, For coverage of these particles with H20 and C2H50H, the following procedure was employed. About 5 mg of silica was mixed with 50 mL of the liquid (H2O or C2H5OH) and refluxed for one hour, The remaining liquid was allowed to evap¬orate to dryness and 1 mg of the treated sample was used to collect the PA spectra. In the case of PVPNO, the amount that binds to Cab-O-Sil is taken from the data on quar"

Mar 1, 1992

By C. H. Fisher

Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils4 such as gasoline, kerosene, and neutral oils from coal-tar distillates. Despite its long use, however, there is no general agreement as to optimum conditions and concentration of acid, and numerous methods and modifications have been recommended. In most cases, treatment of the neutral oil with 80 to 90 percent sulphuric acid, followed by distillation to the original endpoint to remove olefin polymers, is recommended for the estimation of unsaturated hydrocarbons. The distillate thus obtained is taken as olefin-free oil and used in later stages of the anlysis. Aromatic hydrocarbons generally are determined in the olefin-free oil by suphonation with more concentrated acid (96 to 100 percent and fuming sulphuric acid are recommended), the hydrocarbons not attacked and removed as water-soluble sulphonic acids being considered as saturated hydrocarbons. In some cases the saturates are examined further by differentiating between cyclic (naphthenes) and acyclic hydrocarbons (paraffins), Generally this is achieved by physical methods, although strong sulphuric acid is known to react preferentially with some types of saturated hydrocarbons. It was the purpose of the present work to make a general study of this type of analysis and to investigate the reactions of hydrocarbons under conditions often used in analyses that employ sulphuric acid reagents. Since previous work is not in good agreement, the optimum concentrations of acid for the different stages of the analysis were determined. Several sulphuric acid methods previously recommended and new modifications were compared, two synthetic solutions being used as the reference oil. The results obtained are presented below under separate headings.

Jan 1, 1937

By J. C. Barrett

Bureau of Mines research on the arc welding characteristics of titanium was initiated in 1948. Little was known about the art except that the easily contaminated metal required more protection from the atmosphere during welding than most other metals. Chambers were designed and built within which titanium could be welded with adequate inert gas protection. Welds were made and their properties studied, and prototype items were made successfully. This report, presenting a resume of the titanium arc-welding experiments undertaken by the Bureau of Mines, demonstrates that the process is successful if conducted under proper conditions and describes the welding of prototypes. INTRODUCTION The Bureau of Mines' first report on methods of joining titanium covered the subject of spot welding,4/ outlining the conditions necessary for producing spot welds in ductile titanium consolidated by powder metallurgy methods and describing the characteristics of such welds. This report embraces the field of fusion weld-ing of titanium and traces the development of suitable methods and equipment for producing such welds.

Jan 1, 1956

By B. W. Jong

The Bureau of Mines studied reinforcement of sulfur concretes using glass, polyester, and aramid fibers. The objective of this research was to determine the feasibility of fiber-reinforcing the sulfur concrete to enhance the flexural properties. Optimum fiber sulfur concrete compositions were formulated with a cement-to-fiber ratio of 9.0:1 for glass-fiber and polyester-fiber sulfur concretes and 12.1:1 for aramid-fiber sulfur concretes. Test samples were prepared using techniques developed by the Bureau of Mines. Flexural strength values of up to 50 pct of compressive strength values were achieved with fiber additions. With non-fiber-reinforced sulfur concrete, the values ranged up to 20 pct. The impact strength and fracture toughness of sulfur concretes were increased sig-nificantly by reinforcement with glass or with aramid fiber and were adversely affected by use of polyester fiber. Strain tolerance was doubled and failure mode was shifted from catastrophic to noncatastrophic type by adding glass fiber. The glass-fiber and aramid-fiber sulfur concretes are resistant to acid corrosion and have proved durable in freeze-thaw cycles. This laboratory and field evaluation has shown that fiber reinforcement of sulfur concrete is feasible and that it enhances the flexural properties.

Jan 1, 1985

By Edward E. Johnson

The principal purpose of this study was the development of an engineering and economic model of a hypothetical large-scale open pit gold mining operation. The guiding concept in developing the model was the idea that, through study of a number of such models, it would be possible to evaluate a mineral property and to make reasonable estimates of the benefits to be derived from research in mining and metallurgy. The model by use of a computer is able to produce results easily and quickly when cost factors are varied. Cost factors may be varied as a result of assumptions of improved technology or of assumptions of assuming different approaches or methods to accomplish a particular segment of the mining or processing operation. The discounted cash flow rate of return was used to measure the effect of changes in costs or expected revenue. In this study, assumptions based on past processing practices were made in an effort to reduce costs of processing the ore These assumptions were: (1) Eliminating the low-grade cyanide circuit; (2) reducing the quantity of material to be processed by screening after crushing; and (3) using a combination of assumptions (1) and (2). All three assumptions resulted in reduced capital investment and operating cost that caused substantial increases in the rate of return.

Jan 1, 1968

By Cleo G. Rall

The value of brine analyses in the study of petroleum-engineering problems was recognized early in the history of petroleum. The Bureau of Mines before 1928 had indicated in several reports.3/ ways in which analyses might be used. Because of the confusion resulting from attempts to correlate the work of different chemists using greatly varying methods of analysis and systems of computation and expression of results, a paper presenting the methods used by the Bureau of Mines was prepared and published in 1928. This system of determining the characteristic constituents of oil-field waters and of calculating and reporting results has been widely adopted by the petroleum industry. The earliest and most obvious use of water analyses is determination of the source of water infiltrating into petroleum and natural-gas wells. For this purpose it is necessary that an analysis of the connate water of the formation from which the oil is produced be available and that an analysis of the contaminated water be made. By comparing these analyses with those of connate waters from formations higher in the structure, the formation from which the infiltrating water comes may be identified.

Jan 1, 1953

By Yael Miron

The presence of pyrite (FeS2) in coal can cause or contribute to several problems for the coal mining industry. These problems, which include spontaneous combustion, roof falls, floor heave, and accidental explosions in coal surface mining when ammonium nitrate fuel oil (ANFO) explosives are used, result from pyrite oxidation. Pyrite oxidizes exothermically in the presence of air and moisture to form a large variety of products, including hydrated ferrous and ferric sulfates, and sulfuric acid. Some of the products are reactive chemicals and strong oxidants. The volume of many of these oxidation products exceeds the original volume of the pyrite; as a result, the adjacent coal disintegrates and its surface increases, rendering it more susceptible to oxidation. The heat from pyrite oxidation raises the temperature of the adjacent coal, accelerating the oxidation and self-heating rates of the coal. These combined chemical, physical, and thermal effects are the cause of the aforementioned problems. When ANFO is used in surface coal mines and contacts ferrous sulfate, a highly exothermic reaction ensiles. Additional hazards are fires or explosions caused by the frictional ignition of methane when the pyrite in the coal is struck by a cutting bit during mining.

Jan 1, 1994

By N. A. C. Smith

This report on the physical and chemical properties of typical crude oils of southern Louisiana and southern Texas is the seventh in a series of preliminary chapters of a bulletin covering the producing districts of the United States. Preceding reports* may be obtained from the Bureau of Mines on request. The details of the methods used in this survey in collecting samples and making laboratory tests have been discussed in the first three papers. A method of summarizing and interpreting the laboratory data has also been given, but most of the crudes included in the present report differ so radically from those previously reported, that it has been found advantageous to adopt a somewhat different method in making summaries. This method is described in detail later. If any errors or omissions are noted by readers, it is hoped that these will be brought to the attention of the Bureau of Mines, for correction before the appearance of the final bulletin.

Jan 1, 1922

By H. W. Kilau

The U.S. Bureau of Mines is evaluating water spray additives for the purpose of improving respirable dust control during coal mining operations, with particular emphasis on the longwall shearer. Recent field tests of surfactant-polymer reagents at two production longwall operations have shown favorable respirable dust reductions compared with water sprays containing no additive. Gravimetric dust samples obtained by a technician downwind of the shearer while following or preceding the machine showed dust reductions in the range of about 40% to 60% for some of the reagent formulations compared with using water alone. Three polymers were tested: two polyethylene oxide compounds of different molecular weight and hydroxypropyl methylcellulose (HPMC). All were effective for dust reduction, and two were cost effective when used in combination with sodium di(2-ethylhexyl) sulfosuccinate surfactant. How-ever, the use of these reagents requires the longwall operator to be more aware of headgate dust control. Experimental evidence indicates that dust captured by reagent-treated sprays at the shearer can be reemitted in the headgate area if stagcloader-crusher sprays and other dust controls are inadequate.

Jan 1, 2010

By A. F. Baker

Laboratory flotation of synthetic coal-pyrite mixtures and high-pyritic-sulfur coal indicated that ferric chloride (FeCl3), aluminum chloride (AIC13), chromium chloride (CrCl3), and cupric sulfate (CuSO4) are potential pyrite depressants. For each metal salt there appeared to be a range of pH values and optimum concentration for selectively depressing pyrite in coal flotation. Pyrite was depressed in the pH range from 4.5 to 7.0 with ferric chloride, from 5.8 to 7.0 with aluminum chloride, from 6.4 to 7.1 with chromium chloride, and from 6.4 to 7.4 with cupric sulfate. Best separation of pyrite from coal was achieved in flotation solutions containing from 2 X 10-5 to 5 x 10-5 mole/ liter of each salt. In solutions containing excess salt concentrations, coal was also depressed. These Bureau of Mines tests demonstrated on a laboratory scale that, in solutions containing 4 X 10-5 mole/liter ferric chloride and from 1 x 10-4 to 2 x 10-4 mole/liter sodium hydroxide, the pyritic sulfur content of a Lower Freeport bed coal sample could be reduced from about 2.51 percent to less than 0.60 percent with recoveries of over 83 percent. The depression of pyrite appears to be due to the adsorption of positively charged colloidal metal hydroxide at the pyrite-solution interface. This hypothesis is supported by zeta potential determinations which showed that suspended coal and pyrite particles in solutions containing metal salts are positively charged in the pH range where depression occurs.

Jan 1, 1971

By D. L. Paulson

Electric furnace smelting of blister copper directly from copper precipitates (cement copper) was investigated by the Federal Bureau of Mines. Copper concentrations in five different lots of cement copper in the investigation ranged from 62.5 to 82.5 wt-pct. Laboratory-scale smelting tests were made in a 50-kva electric-arc furnace to establish the reductant and flux requirements. Best recoveries were realized by adding 60 pct of the carbon required to combine with the contained oxygen in the cement copper. Operating parameters established during the laboratory-scale smelting tests were used successfully in smelting 20 tons of cement copper during 12 pilot-scale tests in an 800-kva electric-arc furnace. Over 98 pct of the contained copper was recovered as blister-grade metal. The projected energy consumption for a commercial-size furnace was 380 kwhr per ton of cold charge.

Jan 1, 1978

By Cecil E. Lester

Since the advent of coal mining, the minimal lighting in the under¬ground working place has been an obstacle to the safe and efficient performance of the miner's many tasks. Compounding this problem is the fact that the machines being operated in the working place are so large that the vertical and horizontal clearances around the machinery are severely limited. Consequently, in these poorly lighted and congested working places, the machine operator is unable to utilize his peripheral vision. He cannot see hazards as they develop and, too often, cannot react in time to avoid serious injury or death to himself or his fellow miners. The greatest hazard to miners inby the last open crosscut is from falls of roof which are often preceded by warning signs such as falling rock fragments, roof supports taking weight, or a sudden reduction in the height of the working place. These warning signs often go undectected because the machine operator's attention is focused on the small circle of light emitted from his cap lamp. Congress recognized the illumination deficiencies, and, in the Federal Coal Mine Health and Safety Act of 1969, charged the Secretary of the Interior with the authority and responsibility for development and promulgation of minimum standards for illuminating working places in coal mines. These standards have been developed and, as stated in the April 1, 1976 Notice, Federal Register, Volume 41, No. 64, will be promulgated on October 1, 1976, as mandatory regulations under Section 75.1719, Title 30, Code of Federal Regulations. The regulations require that the designated surfaces within the miner's normal field of vision be illuminated to 0.06 foot-lamberts while self¬propelled mining equipment is being operated in the working places. The term "working place" is defined in the Act as "the area of a coal mine inby the last open crosscut".

Jan 1, 1976

By John W. Thatcher

A demountable X-ray tube vacuum spectrograph was designed by the Bureau of Mines for the determination of long-wavelength X-ray spectra from the light elements. This instrument was operated for both secondary and combined primary-secondary excitation of the aluminum K-series. There was an increased analytical sensitivity for elements in period 3, and an indication that with improved X-ray tubes or direct election excitation of the sample, X-ray determination of elements in period 2 is also possible.

Jan 1, 1965

By Peter C. Wood

This report describes research directed toward the preparation of chemical oxygen (02) sources which exhibited improved 02 storage and reaction characteristics when compared to potassium superoxide (KO2). The initial focus of the research was the preparation of calcium superoxide (Ca(02)2) by the disproportionation of calcium peroxide diperoxyhydrate. The Ca(02)2) was characterized by chemical, thermal, and x-ray analyses. Several methods for scaling up the Ca(02)2 synthesis process were studied. Next, the reactivity of Ca(02)2 toward humidified carbon dioxide (C02) was evaluated and was compare o that of K02 under flow-test conditions approximating those existing in portable breathing apparatus. The reactivities of mixtures of K02 and Ca(02)2 or lithium peroxide towards humidified CO2 were also studied. Finally, an analysis of two commercial, K02-based, self-contained self-rescuers was conducted to determine the potential weight and volume savings which would be possible if Ca(02)2 or a mixture of K02 and Ca(02)2 were used as a replacement for K02.

Jan 1, 1983

By Earl F. Hastings

The Pilgrim mine, operated by the Pioneer Gold Mining Co., is 9-1/2 miles west of Chloride in the Pilgrim mining district on the eastern slope of the Black Mountains, or River Range, Mohave County, Ariz. In March 1937, 100 tons of gold ore per day were being mined and milled at the property by a total force of 5i men. Climatic conditions allow year-round operations. Due to present activity in the county there is an ample supply of labor for the requirements of the mine. The Pilgrim is the only producing property within s radius of 6 miles; recently, however, the South Pilgrim Mining Co. has launched a development campaign on claims that adjoin the Pioneer Co. property to the south.

Jan 1, 1937

By William A. Sloan

"In smelting operations, finely divided material called ""flue dust"" is carried by the moving gases from the roasters and furnaces; it is partly settled and recovered in the flue system. The flue dust from copper smelters contains a high percentage of copper, usually some gold and silver, and occasionally other valuable metals. It is too valuable to throw away and in present practice is returned to the smelting furnaces for re-treatment. A part of this material again passes out with the gases and forms a circulating dust load in the system. The dust that passesout of the stacks into the atmosphere is an important source of loss in copper smelting. Loss of values also occurs by dust being blown away while in transit from the flues back to the furnace, and of course the greater the amount of rehandling the greater this loss.Dust carried in the gas currents causes corrosion of the roof arches in reverberatory furnaces. Returning flue dust to the furnace increases the quantity of suspended dust. Corrosion reduces the life of the arches and shortens the length of furnace campaigns; also the corrosion of arches limits the temperature at which a furnace may be operated. Every ton of material that must be re-treated in the furnaces reduces correspondingly the amount of new ore or concentrates that could be smelted.As the present tendency is toward finer grinding in flotation plants smaller particles will need to be treated at the smelters, increasing the difficulty of preventing losses in flue dusts. Many schemes and processes for a more economical method of treating flue dust have been proposed or tried, but in the main none of them has been successful."

May 1, 1928

By H. A. Doerner

"During the year which has passed since the last progress report on reduction of zinc by natural gas,3 the laboratory experiments on this investigation have been completed. In this concluding report, the whole subject will be reviewed and additional data presented.Chemical ReactionsIn a thermodynamic study of zinc smelting, Maier 4 discussed the use of methane for reducing zinc oxide, and predicted equilibria at various temperatures for the sore important reactions. The study has been extended to include the following list.Maier predicted that 870°C. would be the critical temperature above which reaction (1) would take precedence over reaction (2) and that reaction (1) at equilibria would be substantially complete at or above 927°C. A subsequent papers described experimental verification of these predictions and gave data on reaction rates under various conditions.It methane is passed through a heated bed of zinc oxide at a low enough rate reactions (1), (3), and (4) reach an equilibrium which can be expressed by reaction (10). The equilibrium concentrations for the products of this reaction in the temperature range 900° to 1100°C. were calculated by applying the thermodynamic constants to the stoichiometric relations. 6 The results of these calculations are listed in table 1 and shown graphically in figures 1, A and B. These data have major importance, and experimental work has shown that they are subtantially correct."

Dec 1, 1934

By J. W. Town

Recrystallization studies on chrome-bearing spinel materials were made by the Bureau of Mines to determine the effects of certain fluxing agents and cooling rates on the chromium-to-iron ratio of recrystallized spinel. Statistically designed and evaluated tests showed that the ratio of chromium to iron in naturally occurring chrome spinel could be increased from 1.5 to 1 to over 7 to 1 and that the ratio of chromium to iron in the chrome-spinel in a stain-less steel slag could be raised to over 18 to 1. Silica, magnesia, and lime had significant positive effects, while alumina had a significant negative effect. Cooling rates of 200 C per hour in a programmed spiral globar electric furnace were satisfactory for growing crystals of recoverable size.

Jan 1, 1967

By M. L. Wouden

In the late 1970's, the Bureau of Mines began to examine the criteria for reestablishing vegetative cover on coal strip mine spoils near Glenrock, WY. A 9-acre plot, consisting of (1) spoils covered with topsoil, (2) spoils without topsoil, and (3) spoils treated with sewage sludge, was constructed. These plots were seeded with Tegmar intermediate wheatgrass (Agropyron intermedium), Fairway crested wheatgrass (A. cristatum), and Critana thickspike wheatgrass (A. dasystachyum). After 5 yr, the topsoil had about 70 pct plant coverage. Revegetated spoils, without topsoil addition, averaged approximately 30 pct plant coverage, and sewage sludge-treated spoils had about 45 pct plant coverage. Comparison of grass types showed the intermediate wheatgrass produced greater surface coverage.

Jan 1, 1986

By John R. Dudo

The Bureau of Mines Morgantown Petroleum Research Laboratory, with the cooperation of the Penn York Oil Company, cored the Dewdrop, Bradford Third, Lewis Run, and Sartwell sands in the Sartwell oilfield, McKean County, Pa. This report contains a review of the geology and depositional history of the field and an evaluation of the feasibility of secondary recovery of oil from the Bradford Third and Sartwell sands by waterflood or gas drive. Core analysis, geologic data, and electrical and radioactivity logs were used to evaluate the reservoir characteristics. Reservoir geometry, rock properties, fluid characteristics and saturations, and relative permeability-saturation relationships were used to assess the floodability of these two sands. The results of this study indicate that between 53,000 and 61,000 barrels of oil can be recovered by water or gas injection. The success of a waterflood or gas drive will depend on the field injection rates of the reservoirs comprising this oilfield. Following an economic evaluation, additional field work is recommended to further test the floodability of the reservoir.

Jan 1, 1967