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By C. H. Fisher, Abner Eisner

"INTRODUCTION Sulphuric acid of various concentrations has long been used as a reagent in the determination of olefins and aromatics in hydrocarbon oils 4 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 60 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 differentiatingbetween 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."

Dec 1, 1937

By Paul M. Tyler

Graphite occurs in many places in the United States, but previous to 1914 the domestic production amounted to only 15 to 20 per cent of the natural graphite consumed in this country. Including artificial, graphite, the proportion was about 25 per cent. During the World War the production of both natural and artificial graphite increased until, in 1918 it, contributed more than one-half of the available supply, and since 1919 the proportion has not fallen below 40 per cent. Except during the war period, however, this apparently increasing independence has not been due to any large increase in production from domestic mines. It simply reflects a larger output of artificial graphite and reduced imports of Ceylon lung and chip, grades which have never been produced in substantial quantity in the United States. DOMESTIC DEPOSITS3 American graphite deposits, though numerous and often large, are characteristically low-grade. They constitute an abundant source of potential supply, but in normal times they have proved relatively costly to work, and even at the same price the various products have never been able wholly to displace certain imported qualities, notably crucible grades from Ceylon and pencil graphite from Mexico.

Jan 1, 1929

By Alton B. Cook

The practice of using partly depleted oil reservoirs for gas-storage operations is proving successful. Moreover, this practice provides a method of secondary oil recovery when gas is cycled at full-storage reservoir pressure. Because of the relative newness of this operation, a study was undertaken to assist engineers in developing improved gas-injection and production procedures and in calculating the amount of gas needed for completely repressuring reservoirs. This paper is the third in a series reporting the progress of a study by the Federal Bureau of Mines of reservoir performance during complete gas repressuring and gas cycling. A procedure for estimating secondary oil recovery by this method is also under study. One report (7)3/ describes the laboratory equipment. The other report (8) gives (1) data on the New York City field, Clay County, Tex., which has been converted to gas-storage operations; (2) laboratory data from research with a model oil reservoir, in which primary production, complete gas repressuring, and gas cycling for the New York City field were simulated; and (3) theory to explain reservoir performance during gas repressuring.

Jan 1, 1961

By E. S. Shedd

Misch metal was electrowon from a treated bastnasite concentrate in a REF3-LiF-BaF2 electrolyte at 950° C. The metal was prepared and tapped from a 1,000-ampere cell, and nearly 100-percent utilization of the rare-earth oxide was achieved. Prolonged operation in a smaller cell (40 amperes) indicated that the composition of the misch metal product was reasonably constant, and no significant increase of impurities, with the exception of carbon, was noted.

Jan 1, 1970

By Raghoottma S. Pandurangi, Mohindar S. Seehra

"The interaction of amorphous 1ilica particles with several hydrogen bonding agents (H2O, C2H5OH, C7H2NO) 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 or surface groups, along with the shift in the broad hydroxyl band, the interaction following the order C7H2NO > C2H5OH > H2O. Index Headings: Silica; Surface vibrational modes; Photoacoustic spectroscopy; Hydrogen bonding agents.INTRODUCTIONThe use of m spectroscopy to study the adsorption on solid surfaces is well documented in the literature.1 2 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.3-5 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 C7H8NO), 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 m spectroscopy, and Knozinger16 and Rouxlet and Semples11 have used transmission m 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, C2H50H, and H20) with the silica surface by monitoring changes in the surface m 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."

Jan 1, 1990

The U.S. Bureau of Mines (USBM) has developed a test procedure to compare the initiating strength of detonators by using adjustable-sensitivity liquid explosives. Various tests of detonator strength are currently used by the industry, but many of them do not quantify the ability of detonators to initiate detonation reactions in an explosive charge. The USBM used mixtures of nitromethane and ethylene diamine, the sensitivity being "fine-tuned" by 2-nitropropane. Military standard J-2, commercial No.6, and commercial No.8 detonators were evaluated using three test configurations: (1) axially immersed in the test explosive, (2) tip just touching surface of the explosive, and (3) immersed transversely in the explosive. Markedly different results were obtained for these three configurations, indicating that the directional effects are important. This explains why different detonator strength tests do not correlate well with each other. Some tests, such as the sand bomb and underwater, measure the total energy out-put, while other tests, such as the plate dent, test measure the energy in the axial direction. The USBM's test data indicate the importance of conducting the experimentation in the manner in which the detonator is actually intended to function.

Jan 1, 2010

By E. Morrice, R. D. Smith

Thermal expansion and electrical resistance measurements were made on cerium metal from 4° to 300° K. The apparatus developed , including a specimen holder and a cryostat system , are described along with the experimental techniques used in obtaining the measurements . The total linear thermal expansion Data at of 99.83 weight - percent cerium metal between 4 ° K and room temperature was 4.24 percent . The resistivity at 4° K was 7.0 x 10-6 ohm- centimeter . 4° K indicate a fundamental relationship between residual resistivity and purity of cerium metal . The effects of annealing and repeated thermal cycling on resistivity were determined .

Jan 1, 1964

By D. K. Deardorff, Laurance L. Oden, H. Kato, M. I. Copeland

The equilibrium relationship of hafnium and tantalum was studied to facilitate alloy and property investigations . The data obtained are presented graphically as the equilibrium diagram . Alloys were prepared from high - purity components by nonconsumabletungsten- electrode arc melting . Data for the equilibrium diagram were obtained by optical pyrometry , metallography , X- ray diffraction of heat treated specimens , X- ray diffraction using a high- temperature camera , and differential thermal analysis . During the investigations , a casting apparatus was constructed , and the existing melting - point apparatus was improved . The bcc allotrope of hafnium forms a continuous series of solid solutions , called beta , with tantalum which exhibit a minimum melting point at 20 wt pct tantalum and 2,110 ° C. At 24 wt pct tantalum and 1,050 ° C , hafnium- rich beta decomposes in a monotectoid reaction to yield alpha and tantalum- rich beta . The monotectoid isotherm extends from 5.5 to 60 wt pct tantalum . The twophase region , in which hafnium- rich and tantalum- rich beta solid solutions are immiscible , rises to a maximum temperature of 1,265 ° C at 38 wt pct tantalum . The solubility of hafnium in tantalum decreases from 40 wt pct at the monotectoid temperature to 20 wt pct at 750 ° C.

Jan 1, 1964

By Frank E. Cash

Published or available data on safety in quarries are few except those pertaining to blasting issued by manufacturers of explosives. During the past 25 years the quarrying industry (including various types of quarries producing many different materials) has had a markedly improved accident experience. The downward trend has not been phenomenal or has it been uniform from year to year, owing to occasional major disasters; but from the information at hand it appears that improvement during the 25-year period has been definite.

Jan 1, 1941

By T. W. Johnson

One of the common methods of increasing recovery of oil from partly depleted oil sands is to inject natural gas, air, or air-gas mixtures into the sand, thereby supplying energy to move oil into the well bore. Where natural gas is not available, air or an air-gas mixture is used as the repressuring medium. Air-gas mixtures are obtained from the casing-heads of oil-producing wells in the areas repressured with air or air-gas mixtures and consist usually of varying amounts of the hydrocarbon gases, nitrogen, oxygen, and carbon dioxide. Laboratory experiments have been conducted by the Bureau of Mines to determine the effect of air on crude oils.4/ In these experiments the crude oils were oxidized by the air, and the degree of oxidation depended not only upon the chemical composition of the crude oil but also upon the duration and method of contact between the oil and air, the temperature of the fluids and the concentration of the oxygen. When the crude oils were oxidized the following results and changes in the oils were obtained:

Jan 1, 1937

By Joseph M. Pugliese

This work was done by the Bureau of Mines to provide quarry operators with an uncomplicated, first-approximation method for designing blast patterns, considering geologic structure, and to show the valid use of the technique by comparing drill and blast pattern dimensions used in the quarry with those determined by the presented method. The author visited 12 limestone and dolomite quarries in Ohio (Adam, Crawford, and Highland Counties), Wisconsin (Milwaukee, Racine, and Waukesha Counties), and Minnesota (Fillmore, Olmsted, and Wabasha Counties); observed the blasting practices; studied the major geologic features; and after discussion with the quarry managers, foremen, and blasters, compared the quarry blasting patterns with those as calculated by the empirical formulas (after R. L. Ash), with geologic structural considerations. When geologic structure such as bedding, jointing, folding, and caves, as well as explosive properties and field performance characteristics are accounted for in a manner suggested by the research, the presented empirical formulas may be used as a good first approximation. The included steps in planning a blast design and generalized blast patterns should be of help to the quarry operator. Design changes are recommended for those quarries where problems are occurring.

Jan 1, 1972

By T. W. Johnson

One of the common methods of increasing recovery of oil from partly depleted oil sands is to inject natural gas, air, or air-gas mixtures into the sand, thereby supplying energy to move oil. into the well bore. Where natural gas is not available, air or an air-gas mixture is used as the repressuring medium. Air-gas mixtures are obtained from the casingheads of oil-producing wells in the areas repressured with air or air-gas mixtures and consist usually of varying amounts of the hydrocarbon gases, nitrogen, oxygen, and carbon dioxide. Laboratory experiments have been conducted by the Bureau of Mines to determine the effect of air on crude oils.4/ In these experiments the crude oils were oxidized by the air, and the degree of oxidation depended not only upon the chemical composition of the crude oil but also upon the duration and method of contact between the oil and air, the temperature of the fluids and the concentration of the oxygen. When the crude oils were oxidized the following results and changes in the oils were obtained:

Jan 1, 1937

By G. H. Martindill

Complex chemical and physical changes occurring during carbonization result in a heterogeneous system composed of gaseous, liquid, and solid phases, whose relative proportions and chemical compositions change constantly as temperature increases. Studies in which the participating variables are isolated and controlled should be useful in formulating the mechanism of coal carbonization. The most characteristic property of a coking coal is its ability to form a plastic mass at a certain stage of the carbonization process. During this period it is believed that fluidity of the coal influences the properties of the resultant coke. This report gives results of an investigation by the Federal Bureau of Mines of the influence of the maximum fluidity attained by the charge on the physical quality of the coke or char produced. As a first approach to the problem, researchers investigated high-melting-point pitches, which are relatively simple carbonaceous materials. The plastic properties of these pitches, prepared specially for this work, varied greatly; their fluidities, as measured by the Gieseler plastometer, covered most of the fluidity range characteristic of coking coals. Blending these pitches with increasing pro-portions of fine coke progressively reduced their fluidities. Coal-pitch and coal-coke blends also were treated; their fluidities were varied by changing their blending ratios. The various blends were carbonized in a small-scale carbonizer and the resistance of the carbonized residue (char) to abrasion was determined in a small-scale tumbler test, using the Roga drum.

Jan 1, 1960

By Andrew Allan

[This report describe the first experiment of the Anthracite Research Laboratory, Bureau of Miners, in attempting to reduce underground-mining costs and conserve anthracite as a natural r-source by introducing now minim methods. The work war, dons in cooperation with one of the large anthracite-producing companies. It applies to productive mining, characterized by comparatively low cost, per ton and high production per man, as differentiated from development mining, which is always necessary before the, productive or retreat phase can begin. The system d scribed in this report is believed to be generally applicable to beds pitching 70° to 90° and, under certain conditions, to beds pitching loss than 70°. After development hate been completed, an openings is made, extending the full width of the 9- to 10-foot coal bad and reaching from the haulageway to the vertical limits of the solid coal. Long drill holes (20 to 50 feet) charged with about one stick of permissible explosive riper foot of length are fused to break the coal. Once broken, the coal is loaded onto a shaker conveyor by gravity and thence into mine: cars. The coal is mined retreating in 15- to 20-foot sections that are broken and loaded onto the conveyor through a specially constructed chute. In the Bureau?s experimental work, the height of sections arse ranged from 35 to 60 fact, depending on the geologic extent of the coal bed.]

Jan 1, 1952

By Sidney Katell

Tonnage oxygen plants are or can be made available in sizes ranging from 150 to 1,000 tons per day. Capital requirements are estimated from $5,400 to $14,700 per daily ton, depending upon size of plant, cycle employed, and purity and discharge pressure of the product. Similarly, operating costs before return on investment will range from $4.80 to $10 per ton. INTRODUCTION Several processes4 5/ that can be used to convert coal to synthetic liquid fuels, synthetic pipeline gas, or hydrogen require high-purity oxygen as one of the basic raw materials. Depending on the and product and its specific use, the oxygen required will be of 95 or 99.5 percent purity. The quantity required, in turn, depends on the process for which the oxygen will be used and the size of the processing plant and will range from 150 to 4,000 tons per day.

Jan 1, 1960

By P. A. Bloom

Bureau of Mines research was conducted to develop effective separation methods that might be used in exploiting substantial tonnages of complex barite-fluorspar ores in Arizona. The exploitable reserves now may be increased as recent batch and continuous flotation tests demonstrated that a complex barite?-fluorspar ore from the Red Chief deposit, Yuma County, Ariz., could be selectively treated to concurrently produce (1) fluorspar and (2) a barite byproduct of marketable grade. The sample contained 24.8 percent CaF2 and 24.3 percent BaS04. Processing comprised production of a fluorspar product containing 97 percent CaF2 with an 82 percent recovery, using a sodium fluoride-lignin sulfonate-fatty acid reagent combination. Concurrent retreatment of the fluorspar tailing, using sodium cetyl sulfate as a collector, yielded a barite product of 94 percent BaS04 grade with a 71-percent recovery. The products met specifications for acid-grade fluorspar and drilling mud-type barite.

Jan 1, 1963

By S. M. Shelton

The widespread occurrence of domestic manganese deposits and the shortage of ferromanganese-grade ore have been sources of much speculation and investigative effort for many years. The present emergency has intensified the search by the Bureau of Mines for methods of producing ferromanganese-grade concentrates4/ from low-grade ores.

Jan 1, 1941

By D. P. Schlick

The German experience in dealing with the health hazard of respirable dust in underground mines is reported from first-hand observation in this Bureau of Mines paper. The report covers-- 1. The control of dust by water infusion, water spraying, and ventilation. 2. The sampling devices (tyndalloscope , konimeter , and BAT-I) and methods used to determine the dust concentrations in mines. 3. The systems of classifying hazardous and safe dust levels in mines. 4. The research facilities devoted to theoretical and applied work on mine dust and pneumoconiotic disease. Tile major research projects on dust and disease now underway in West Germany are outlined in an appendix.

Jan 1, 1970

By D. P. Schlick

As of June 30, 1970, Federal regulations required the operator of each underground coal mine to maintain the average concentration of respirable dust below legislative standards. As of March 1, 1971, over 152,000 respirable dust samples have been processed by the Bureau of Mines. Approximately 75 percent of underground working sections are being sampled in accordance with Federal regulations. Results indicate that 72 percent of the sections which have completed at least one basic sampling cycle are below 3.0 mg/m3, the standard in effect under the Federal Coal Mine Health and Safety Act of 1969 (P.L. 91-173). Notices of Violation were issued on 1,670 underground mines for failure to begin a sampling program; Withdrawal Orders were issued in 64 of these instances. Notices of Violation were issued on 1,121 sections where applicable dust levels were exceeded; Withdrawal Orders were issued in seven of these instances. There are 381 mining sections currently operating on permit; from the interim Compliance Panel.

Jan 1, 1971

By Blade O. C.

This report is one of a series made by the Bureau of Mines under a cooperative agreement with the Coordinating Fuel and Equipment Research Committee of the Coordinating Research Council, Inc., on the characteristics of commercial aviation gasolines. The series of surveys is a continuation of like work conducted from 1940 to 1946 by the National Bureau of Standards under a similar cooperative agreement. A list of reports of previous surveys is given at the end of this paper.

Jan 1, 1950