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By B. H. Eccleston, R. F. Kendall, D. E. Hirsch, Norman G. Foster

The mass spectra of 23 alkylthiophenes are presented , including 21 that have not been previously reported . Correlations between mass spectra and the structure of the thiophene homologs are discussed . Comparisons with , and corroboration of , earlier workers ' correlations and predictions are made . Several additional correlations are reported to enable the spectroscopist to identify the substituents on alkyl - substituted thiophenes , and the relationship of the mono - substituted and 2,5 - disubstituted alkylthiophenes is discussed in detail .

Jan 1, 1964

By W. N. Marchant

The Bureau of Mines performed chemical research to elaborate details of sulfur chemistry pertaining to the citrate flue gas desulfurization process in which sulfur dioxide (SO2), absorbed (as bisulfite ion) in a buffered sodium citrate solution, is reduced by hydrogen sulfide (H2S) according to the overall reaction 2H2S + HSO3 + H+ ? 3S + 3H20. The rate-limiting step in the process was shown to be the reduction by H2S of thiosulfate (S2031-) that is formed as an intermediate. Pseudo first-order kinetic measurements were made at room temperature to retard the reaction sufficiently that adequate analysis was possible. These measurements showed the rates of the following net processes to be -d [S02]/dt (pH 4.5) = (0.409±0.050)min-1 [S02]; d [S2032-]/dt (pH 4.5) = (0.199±0.017)min-1 [S02]; -d [S2032-]/dt (pH 4.0) = (0.0437±0.0265)min-1 [S2032-]~1; -dH2S/dt (pH 3.9) = (21.6±3.0) mmoles/min-atm [H2S]g1.4, where [H2S]g is the partial pressure of H2S in the gas phase, in atmospheres, and the rate describes the consumption of H2S, in millimoles per minute; d[S]/dt (pH 4.0) = (38.0±3.4)min-1 [H2S]1, where [H2S] is the concentration of H2S in solution. Hydrogen ion consumption during the slow phase of regeneration was shown to occur at (2.1±0.5) times he rate of thiosulfate consumption, which is interpreted as evidence for the following as the rate-limiting reaction: 2H2S + S2032- + 2H+ ? 4S + 3H20 A scheme consisting of five sequential general reactions is proposed to account for sulfur formation.

Jan 1, 1981

By F. R. Cattoir, T. A. Sullivan

Commercial uranium metal was electrore fined to a high- purity product using molten- salt electrolytes in an inert atmosphere cell . Electrorefined uranium that contained , after consolidation , less than 30 ppm of metallic impurities was prepared . A method of leaching the electrolyte crystals to remove the salts was developed . Cathode current efficiencies from 90 to 100 percent were obtained . Two molten- salt electrolytes were prepared and evaluated : (1 ) lithium chloride - potassium chloride - uranium trichloride and ( 2 ) sodium chloridepotassium chloride - uranium trichloride . Very little difference was found in the purity of the uranium metal produced in either system . The lithium chloride - potassium chloride - uranium tri - chloride electrolyte was preferable from an operational standpoint .

Jan 1, 1964

By H. W. Busch

In the course of examinations by representatives of the Bureau of Mines of several compressed-air systems in which explosions had occurred, samples were obtained of the carbon deposits that are formed normally in various parts of the systems by decomposition of the compressor lubricating oil. Experimentation with these carbon deposits has demonstrated that they contain a "carbon-oxygen complex" similar to that formed on coal and on other carbonaceous materials and generally recognized as being the cause of spontaneous heating of coal. The exothermic properties exhibited by such a complex are considered significant in relation to the possible initiation of combustion reactions that may lead to explosions or formation of carbon monoxide in compressed-air systems. This report discusses the occurrence of explosions and formation of carbon monoxide in the use of compressed air and presents results of experimentation conducted with carbon deposits from air compressors.

Jan 1, 1949

By S. R. Zimmerley, C. H. Schack

"INTRODUCTION The pilot-mill concentrator at Boulder City, which has a nominal capacity of 40 tons per day, was planned and built to investigate further the beneficiation of domestic manganese ores that have been concentrated successfully in the ore-dressing laboratory. As milling of manganese ores in general is a new field, it is necessary to prove the success of laboratory processes by means of large-scale operations employing standard milling equipment, and thus to obtain engineering and metallurgical data essential to designing and operation of full-scale concentrating mills.The first ore tested in the pilot plant was the Three Kids Annex manganese ore from the Las Vegas Wash area 15 miles southeast of Las Vegas, Nev. The deposit was worked for its high-grade ores during the First World War From 1930 to 1939, 4,500 feet of diamond drilling was completed by a private company. Diamond drilling started by the Bureau of Mines in November 1940 and completed in July 1941 aggregated 6,600 feet. Exploration by the private company and the Bureau outlined reserves of about 1,000,000 tons of ore assaying plus 28 percent manganese. A much larger tonnage of lower-grade ore also was outlined by the drilling.Because of its physical nature, the Three Kids Annex ore had long proved unamenable to concentration by ore-dressing methods. The ore is a mixture of manganese oxides (wad) filling the pores and to some extent replacing a silt composed of very fine grains of volcanic tuff, quartz, feldspars, other silicates, and clay. Some gypsum occurs as fillings along fracture planes. The ore is light and very porous. Upon wetting, it disintegrates into granular but friable particles and a large amount of slime. It is these characteristics that make the ore so difficult to concentrate."

Sep 1, 1947

By R. L. Montgomery

Heats of solution of cerium metal and cerium (III) chloride in hydrochloric acid were measured. The standard heat of formation of the aqueous cerium (III) ion at 25° C is -166.1 ± 0.3 kcal/mole. Heats of solution of cerium (III) chloride in hydrochloric acid are consistent with the existence of a complex CeC1++ having a stability constant of 1 and a heat of complexing of 5.4 kcal/mole.

Jan 1, 1962

By E. J. Murphy, A. P. Rowles, John C. Holtz

"INTRODUCTION The use of sheaths or hollow cylinders of flame-extinctive materials surrounding cartridges of permissible explosives has been developed during the last few years; the history of sheathed explosives in their salient development in Belgium was treated recently in a publication of the Bureau of Mines. 6/ This development is of great interest in explosives technology, for it holds possibilities of reducing further the ignition hazards that may cause many coal-mine disasters. The township interest in sheathed explosives in this country is attested by the passage of some State laws permitting the use of such explosives on shift 7/; inquiries are received in increasing numbers concerning the effects of sheaths on practical hazards as well as the general technology underlying their use."

May 1, 1943

By R. W. Michelson

The Bureau of Mines developed computerized mathematical models to estimate the economic availability of Mesabi Range taconite concentrates; these are a quality model, a cost model, and an economic availability model. The quality model evaluates metallurgical test data; the cost model determines iron unit cost from mining and processing cost data; and the economic availability model determines quantity from geologic and ore quality data. By correlating all of the physical resource quality factors and dimensional characteristics with the economic cost factors associated with producing iron ore pellets, these three models combine to establish a final relation between iron ore reserve quantities and iron unit cost.

Jan 1, 1970

By Michael Rieber

Among the principal gathering/distribution systems for coal is over-the-road trucking. Where alternative trunk line modes such as barge or rail links are weak or nonexistent, trucks may, particularly for relatively short line hauls, act as substitutes. Their major application, however, appears to be in connection with smaller mines or coal users particularly where terrain problems are significant. Truck use has increased as rail lines have been abandoned or suffered neglect. For example, in 1956 about 38 percent of the coal transported in eastern Kentucky and about 8 percent of the coal moved in western Kentucky went by truck. By 1975, the percentages were almost 77 percent and 26 percent, respectively [4,U-11]. While rail route .limitations and deterioration played a part in the change, increased emphasis on road building, particularly during the 1950's and 1960's, and improved truck load capacity and efficiency were also important.

Jan 1, 1977

By R. J. O'Dea

"The United States hat large reserves of titaniferous iron ores that are a potential future source of both iron and titanium. Although it is not now economically feasible to recover iron and titanium metals from these ores, they may become important in times of stress and, in some instances, already have served as a source of pigment-quality titania.The iron- and titanium-bearing constituents of the ores considered in this report are not completely separable from each other by ore-dressing methods, and chemical (or smelting) procedures must be employed. It is im¬portant, therefore, that information be available concerting their reactivities. The most important titanium-bearing constituent is ilmenite (FeTiO3), the thermodynamic properties of which were discussed in a previous publication.3/ The results of thermodynamic studies showed that both hydrogen and carbon monoxide are relatively ineffective reducing agents for the iron in limonite. On the other hand, carbon theoretically is effective at tempera¬tures above 8510C., at which. point the combined equilibrium pressures of CO and CO2 from the reactionsFeTiO3 + C = Fe+ TiO + COand200 = C+ CO2reach 1 atmosphere.This report gives results of small-scale tests of selective reduction by carbon of the iron in titaniferous iron ores, both with and without addition of sodium carbonate. It is shown that the bulk of the iron may be reduced and separated without serious reduction or loss of titanium. Three Wyoming ores, Iron Mountain, Shanton, and Taylor, wore studied. The principal factors investigated were temperature, time, carbon:ore ratio, particle size, and sodium carbon ore ratio.Two methods of investigation were employed. In the first, intimate mixtures of ore and carbon were roasted and the reduced iron and titanium evaluated by leaching with dilute sulfuric acid and analyzing the leach solution (and, in some instances, the dried residues).Twenty grams of ore were mixed thoroughly with carbon and tamped into an alundum thimble having a loosely fitting cover. The thimble and contents were placed in a test-tube end porcelain tube and heated to the desired temperature in a Globar tube furnace. The open end of the porcelain tube was connected to a bubbler containing sulfuric acid, in a manner that permitted complete shut-off of the tube when desired. This allowed removal of the tube from the furnace at the end of the roast period without exposure of the contents to the atmosphere."

Jun 1, 1946

By G. S. Scott, G. W. Jones

"INTRODUCTION An important phase of the accident-preventing program of the Bureau Mines is the determination of the explosion hazards of various combustible gases, vapors, and liquids encountered in mining and allied industries and the development of methods of eliminating or mitigating them.Recently, isobutane has become a commercially important raw material in the production of aviation gasoline by the alkylation process. 4/ in which isoparaffins are combined with olefins to give higher molecular weight compounds of branched-chain structure.Because of the anticipated commercial importance of isobutane in industry, it has been deemed necessary to study and determine its general explosion haz¬ards. This report gives its limits of inflammability, minimum ignition temper¬atures, and the amounts of nitrogen and carbon dioxide required to render isobutane-air mixtures noninflammable."

Jun 1, 1947

By M. A. Schellhardt

The Bureau of Mines has made periodic back-pressure tests on numerous gas wells in the Texas Panhandle field during the past several years to study the delivery capacities of the wells under different pressure and operating conditions and to determine the relationships between pressures and rates of delivery from gas wells.4/ However, information regarding the intake capacities of gas-well systems is meager, end in projects involving the flow of gas into porous-rock reservoirs it has been necessary to determine intake capacities of gas wells by trial. Accordingly the fundamental intake characteristics of natural-gas yells have been studied to develop a method for determining intake capacities under different wellhead pressures from data descriptive of the "output" or producing characteristic of the wells.

Jan 1, 1936

By L. C. IlsLey

"This paper is intended for State mining inspectors, safety engineers of mining companies, and others interested in electrical safety inspection in mines, It presents the important points that should be watched by inspectors, and briefly reviews the work of the Bureau of Mines in the testing of electrical apparatus or equipment to determine their permissibility for use in gaseous coal mines.Important Points in Inspecting Mine Electrical Installations or Equipment.The following questions are intended as suggestions to a safety inspector who may not have been specially trained in looking for defects in installations or in the maintenance of electrical equipment:1.,Is there someone in charge of electrical equipment who is fitted for this position by ability, training and experience?2.,Is a systematic recorded inspection of electrical equipment made at least once each month?3.,Is a plan map of the mine kept showing all permanently installed electrical machinery and apparatus, including cables, conductors light etc.?4.,Are there instructions for resuscitation from electric shock posted in each surface and underground electrical station, also at the entrance of the mine and in the first aid station and are employees working on electrical equipment trained to apply these instructions in case of accident?"

Nov 1, 1923

By J. L. Kohler

The final report for Phase II of Bureau of Hines Contract J0134025 concerns the research and development of sensitive ground-fault relays for dc utilization systems in mining. Sensitive relaying employs very low pickup levels such that, when used in conjunction with very high resistance grounding, the exposure of a human to ventricular fibrillation is significantly reduced. To delineate the desired relay characteristics, the report begins by reviewing previous research in this area. A theory for the saturable transformer used to sense the fault current is presented. The design of the ground fault relay is described in sufficient detail that it may be duplicated. Test procedures and results are given. Finally, conclusions and recommendations related to Phase II are presented.

Jan 1, 1986

By M. A. Schellhardt

In recent years development of instruments and equipment for determining subsurface pressures and temperatures in. gas and oil wells has made it feasible to obtain information that eras not available in the past on many gas-production problems. The material presented in this report illustrates particularly the value of subsurface-temperature data in the study of subsurface leakage from gas wells. An abnormal decline in the shut-in pressure of the Lone Star Gasoline Co. A. Jones No. 1 gas well in the southern part of the Buffalo (Tex.) field was observed during an interval when a negligible volume of gas bras being withdrawn from the reservoir. Wellhead-pressure readings indicated that the shut-in pressure of the well declined from 2,295 pounds per square inch gage on February 3, 1937, to. 1,445 on February 12, 1935. Tests conducted by engineers of the Lone Star Gas Co. suggested that the subnormal pressure gaged on February 12, 1938, probably was not caused by a head of liquid in the well.

Jan 1, 1940

By Donald E. Redmon

This Bureau of Mines report examines the injury experience in the quarrying industry for the years 1968-69. Twenty-eight tables for each year are presented in which disabling work injuries are summarized by department, source of injury, extent of disability, part of body injured, and nature of injury. Correlative information on employment, worktime, and operating activity is also presented.

Jan 1, 1973

By Gary W. Kramer

The Bureau of Mines has developed a rapid analytical method for the determination of anions by ion chromatography (IC) in phosphate rock mining materials and cement kiln dust (CKD). The procedure employs an Na2C03 fusion of the sample, followed by a water extraction that allows direct injection of the sample into an ion chromatograph without separator column poisoning by the transition metal ions. Fluoride (F-) and phosphate (P043-) were determined in 24 phosphate rock processing and waste material samples by the IC method. The results were compared with a pyrohydrolytic distillation-titration method for F-and a colorimetric procedure for P043-. Excellent analytical agreement was obtained for F-and p043-values determined by IC and the comparable wet chemical methods. Fluoride values ranged from 0.3 wt-pct in the filter cake to 3.6 wt-pct in phosphate rock concentrate. Phosphate values ranged from 1.2 wt-pct in the filter cake to 33.8 wt-pct in the rock concentrate. Fluoride, chloride, phosphate, nitrate, and sulfate in several CKD samples were determined by the IC method and standard wet chemical techniques. Excellent agreement was obtained between the two methods for all anions. A total of 113 CKD samples from all areas of the United States was analyzed by the IC method. Fluoride values ranged from <0.01 to 0.36 wt-pct. Chloride values ranged from <0.01 to 12.5 wt-pct. Sulfate values ranged from 0.41 to 31.6 wt-pct. Phosphate and nitrate were detected in only about 25 pct of the samples at >0.02 wt-pct. Maximum phosphate and nitrate values were 1.0 and 1.6 wt-pct, respectively.

Jan 1, 1982

By George S. Rice, J. W. Paull, R. R. Sayers

"Standard rock dust for use in the rock dusting of coal mines might be defined tentatively as powdered mineral, light colored and free of carbonaceous matter and free silica, all of which will pass a 20-mesh screen while 50% of it will pass-through a 200-mesh screen.Such dust may be prepared from limestone, gypsum, anhydrite, or shale free of sand and flint. For the initial rock dusting of the average nongaseous bituminous mines enough standard rock dust should be applied so that the combustible content of the resulting mixture of rook dust with mine dust shall not exceed 45%, a range somewhere between 35% end 45% being the practical objective sought.All entries, slopes or passageways and room necks should be rock dusted.Additional safeguards are:a.,Rockdusting roomsb.,Scattering of dust in vicinity of shots before firing.c.,Placing of barriers in the mouths of panels, cross-entries and other key positions.Redusting becomes necessary whenever the combustible content of the mine dust exceeds the permissible maximum. This should be determined by regular, systematic sampling, followed by a simple analysis of the samples for combustible content. A Bureau of Mines volumeter for measuring the density can be used for the determination of combustible content."

May 1, 1924

By K. K. Kershner

To meet an increasing demand for high-purity cobalt, the Bureau of Mines has conducted investigations for producing this metal. Cobalt having a purity of 99.95 percent or higher is needed to determine heats of formation, corrosion resistances, phase diagrams, and other basic properties of the element and its compounds. This grade of cobalt may be used for preparing radioactive metal. As a result of its investigations a detailed procedure, which is of practical significance to the production of high-purity cobalt, has been developed by the Bureau for purifying cobalt solutions and for electrolytic deposition of the metal. Cobalt metal, which had a purity of 99.99 percent with reference to metallic contaminations, was deposited electrolytically. Qualitative spectrographic analysis showed only traces of calcium, copper, iron, magnesium, nickel, and zinc.

Jan 1, 1956

By Agnes Y. Lee

The Bureau of Mines has developed an effective hydrometallurgical method to recover high-purity Pb metal and elemental S from concentrates. This low-temperature process eliminates S gases and Pb emissions, in contrast to the current high-temperature smelting technology. The method consists of (1) oxidative leaching with H202, Pb02, and waste fluosilicic acid at 95° C to produce a solution of PbSiF6 and a residue containing elemental S, (2) electrowinning the PbSiF6 solution at 35° C to produce 99.99 pct Pb metal and H2SiF6, and (3) solvent extraction to recover S, leaving a residue containing Cu, Ag, and other metal values. Spent electrolyte was recycled repeatedly, with impurity buildup controlled by controlling the leach parameters.

Jan 1, 1986