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By C. J. Wilhelm, John M. Devine, Ludwig Schmidt

"Steel tanks often corrode rapidly in oil fields where the Gas produced with crude contains an appreciable quantity of hydrogen sulphide. In many instances working tanks have been discarded after only six months of service because of failure induced by corrosion.Aluminum has been used for some time in the fabrication of certain equipment incidental to the handling of oils containing hydrogen sulphide gas in solution, and has exhibited no carious corrosive action. These uses indicated that aluminum tanks,be equally effective in counter- acting hydrogen sulphide corrosion. Consequently, in the spring of 1920, an all-aluminum stock tank of 500 barrels capacity and a ""composite"" tank of equal capacity, having a steel bottom and bottom ring and an aluminum top and top ring, were placed in service on the State-Lassiter lease of the Gulf Production Co, in Crane County, Tex. These tanks were under observation for one year, the toot being sponsored by the Gulf Production Co., the Aluminum Co. of America, and the Parkersburg Rig and Reel Co. The results of this preliminary test sustained the belief that aluminum is highly resistance to hydrogen sulphide gas and likewise indicated the type or grade of aluminum which could be most economically used for lease tankage. However, in this preliminary test the tanks were not subjected to contact with the quantities o highly concentrated brines such as often are associated and produced with crude oil. Therefore, it was suggested by representatives of the aluminum Co. that additional tests be made to include production conditions in large quantities of brine would be handled, for pact experience had shown that aluminum often is susceptible to the corrosive action of brines."

Apr 1, 1931

By Marvin L. Whisman

Several parameters controlling the reproducibility of tritium determina¬tion in organic compounds by liquid scintillation counting were evaluated by the Federal Bureau of Mines. These included optimum volume of scintillator solution for maximum counting efficiency, reproducibility of counting a sealed commercial standard and comparison with duplicate counts on laboratory-prepared samples. The error introduced by using microliter pipets, optical differences in counting vials, reproducibility of counting organic samples where quenching is a factor, reproducibility of counting laboratory-prepared samples with an added internal standard, optimum ratio of internal standard activity to sample activity, effect of sample volume upon counting efficiency, count rate at which coincidence losses become apparent, and reproducibility of organic compound radioassay by the standard addition technique are outlined. From the evaluation of these parameters, a technique that can be applied routinely to organic compounds containing tritium has been established, and details are included in this report.

Jan 1, 1961

By R. L. Benner

A compound stability diagram was constructed by the Bureau of Mines for the Zn-Fe-S-O system to show the phases that should be thermodynamically stable at various temperatures, oxygen pressures, and SO2 pressures. The diagram was demonstrated to have good qualitative value for predicting stable phases that may, in turn, be related to the recovery of zinc in the leaching phase of the electrolytic zinc process. The study showed that roasting temperature is the most Significant variable in preventing roaster formation of zinc ferrite, which is directly related to subsequent extraction of zinc in the leaching step.

Jan 1, 1966

By Henry E. Perlee

Air compressor explosions that are caused by the ignition of combustible vapor mixtures cannot be explained by a single reaction mechanism or sequence of events. Explosions have been caused by the sudden release of large quantities of lubricating oil, by the rapid vaporization of oil that had accumulated slowly in high-pressure piping, and by the production of decomposition products from carbonaceous deposits. Ignitions can be caused by the heat produced in a catalytic reaction, in a compression process, or when a shock wave is propagated through a combustible vapor-air mixture. The frequency of these ignitions can be minimized by establishing proper maintenance and cleaning schedules. Further study is needed to satisfactorily correlate the various factors involved in compressor explosions.

Jan 1, 1963

By L. L. Oden

The Bureau of Mines is conducting research to develop methanation catalysts for converting synthesis gas derived from coal to synthetic natural gas. This report describes a method to prepare supported Raney nickel coatings by dipping screen-covered nickel sheet in molten aluminum-nickel alloy. Coatings were formed at 1,050° C that were comparable in thickness, composition, microstructure, and catalytic properties to flame-sprayed commercially pre-pared Raney nickel. A molten salt comprising cryolite-8 wt-pct LiF was employed over the molten metal bath to clean and preheat the substrates, to protect the metal bath from oxidation, and to heattreat the coated specimens. Immediately following heat treatment, specimens were quenched to 700° C in a molten salt bath containing CaC12-34.5 wt-pct NaCl, which also functioned to remove the insoluble occluded fluoride salt.

Jan 1, 1976

By G. Richards Gwinn

The mineral graphite, a form of carbon, has been known for hundreds of years, and, was first used commercially as a coloring agent. Its true identity, however, was not recognized until the end of the eighteenth century, and its commercial development did not become extensive until near the close of the ninteenth century.

Jan 1, 1943

By Lulie H. Crump

Salient historical data on consumption of fuels and energy have been summarized by State and census district for the years 1960 through 1972. This Information Circular covers States east of the Mississippi, and Information Circular 8705 covers States west of the Mississippi. These data replace previously published compilations of energy consumption statistics by States and districts. Future annual studies are planned using the same Btu conversion factors applied in these two. Information Circulars.

Jan 1, 1976

By P. T. Brooks

Semipilot scale tests were made to demonstrate a newly developed electrorefining process which could be extrapolated to commercial scale in producing high-purity nickel and cobalt from crude nickel metal and high-grade ferronickel. The new process comprises application of solvent extraction techniques to remove and separate cobalt and iron from nickel and the electrodeposition in diaphragm cells of pure nickel and cobalt from chloride-based purified electrolyte. Using water insoluble organic amines, the solvent extraction operations enabled production of commercial-sized nickel and cobalt cathodes of higher purity than that of commercial electrolytic metals. The solvent extraction operation for separation of cobalt from nickel was made simpler than the conventional method. Furthermore, the solvent. extraction operation for iron removal made possible the electrorefining of ferronickel without the prohibitive loss of nickel resulting from the method ordinarily used for iron removal.

Jan 1, 1970

By P. J. McDonough

The Bureau of Mines designed and tested a hardware-software system for measuring on-line corrosion rates of materials in a rod mill in operation. Currents ranging from 10-6 to 10-3 A and potentials in I-mV increments were converted to a digital signal. The digitized data were frequency-modulated and transmitted from a rotating ball mill to an FM receiver, where they were decoded by computer and then processed in real time using assembly language software. This design approach would allow accurate measurement and control of systems where signals of small amplitude and large ranges are present.

Jan 1, 1988

By R. L. Rock

The Bureau of Mines conducted radiation-ventilation studies in six large underground uranium mines to investigate the extent of radon-daughter exposure experienced by the miners and to analyze the ventilation systems to set what changes were required to achieve recommended radiation standards. The studies entailed tracing and measuring the mines' ventilating air, quantitatively and qualitaitively, from its entrance into the mines, through production areas, and lack to the surface. Pressures consumed in creating airflow through mine circuits were determined by altimeter surveys. Air quantities were measured with anemometers or by chemical smoke cloud methods. Air quantities delivered through tubing were determined using U-tube water gages to magnahelic gages to measure velocity pressures. Radon-daughters were filtered from mine air to measure alpha activity; activity levels were converted to "working levels," the established unit for reporting miner exposure. Attention was given to locating unnecessary contamination influx sources and recirculating air. The radiation-ventilation surveys showed that where basic principles of food ventilation were not followed, high alpha radiation levels invariably resulted. Some mines required more primary air for controlling radiation levels throughout active areas, but more efficient use of available air was generally possible. Premature contamination of intake air was prevalent where development Openings intersected ore or passed by worked-out stopes. Several auxiliary systems were inefficient in secondary distribution, recirculating air already too highly contaminated for ventilation. Many got these common problems can be traced try the lack of dine planning with radiation control in mind.

Jan 1, 1969

By Mary S. Esfandiary

This is a revision of a directory of coal research organizations throughout the world that was first published in 1961 as Bureau of Mines Information Circular 8008. Because of the wide acceptance of the first edition, a revision which would supply up-to-date information on coal research and which would facilitate communication among organizations of similar interest seemed important. This compilation includes the names and activities of organizations of various types-government, university, private, and industry. The areas of investigation that each organization is engaged in are indicated in broad terms: Analysis and constitution, mining and geology, preparation, briquetting, combustion, high- and low-temperature carbonization, gasification, conversion to solid and liquid fuels, and health and safety. Publications issued by and describing the work of each organization are cited; almost all of the organizations also publish results of their investigations in the technical press. Selected technical and trade publications that publish information on the science and technology of coal and are not published directly by any of the organizations listed are cited in the pages following the list of organizations in each country.

Jan 1, 1966

By Mary S. Esfandiary

This is a revision of a directory of coal research organizations throughout the world that was first published in 1961 as Bureau of Mines Information Circular 8008. Because of the wide acceptance of the first edition, a revision which would supply up-to-date information on coal research and which would facilitate communication among organizations of similar interest seemed important. This compilation includes the names and activities of organizations of various types-government, university, private, and industry. The areas of investigation that each organization is engaged in are indicated in broad terms: Analysis and constitution, mining and geology, preparation, briquetting, combustion, high-and low-temperature carbonization, gasification, conversion to solid and liquid fuels, and health and safety. Publications issued by and describing the work of each organization are cited; almost all of the organizations also publish results of their investigations in the technical press. Selected technical and trade publications that publish information on the science and technology of coal and are not published directly by any of the organizations listed are cited in the pages following the list of organizations in each country. Information that would improve coverage and accuracy of the next revision of the publication will be welcomed by the Bureau of Mines.

Jan 1, 1966

By Lung Cheng

The Bureau of Mines conducted laboratory tests to investigate the ease of frictional ingition with frozen (nonrotating) conical bits cutting into sandstone. The number of strikes with a new bit to obtain ignition of a combustible methane-air environment was measured. Tests were made with bits tipped with both tungsten carbide and steel at several bit attack angles (angle between bit axis and sandstone surface) and initial tip angles (included angle at the tip of the new bit). Carbide-tipped bits required more strikes for ingition than steel-tipped bits, by a factor of 7 to 10. With a carbide-tipped bit, the number of strikes for ingition increased by a factor of about 3 if the bit attack angle increased by 10° or if the initial tip angle decreased by 10°. During use, abrasive wear of the frozen bit caused a flat surface to form at the tip of the bit, thereby decreasing the tip angle. As the attack angle increased, however, the new bit involved a smaller wear-flat area whereby, abrasive wear was decreased.

Jan 1, 1987

By M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

Jan 1, 1964

By Elizabeth A. Johnson

Minor-element behavior and interaction in the copper matte-iron silicate slag system have been studied by the Bureau of Mines. In the present work, the possibility of interactions among the minor elements As, Sb, Bi, Se, and Te was investigated. Equilibrations of matte, slag, and one of each of the five minor elements were performed at 1,250° C under typical matte smelting atmospheres of CO, CO2, and S02 for mattes containing 40, 50, and 60 pct Cu. Results are compared with those of a previous Bureau of Mines study in which all five minor elements were present simultaneously.

Jan 1, 1984

By Francis X. Cannaday

The Bureau of Mines developed equipment to measure the sonic velocity of pulses transmitted through rock samples varying in size from laboratory specimens to mine pillars in place. Pulses are produced by electronically excited piezoelectric ceramic transducers. Special equipment components were developed by Bureau facilities; other components are commercially available. The technique permits a nondestructive, repetitive, stable, shaped pulse to be used in place of explosive caps or hammer blows. Longitudinal wave travel time measurements were taken on an oscilloscope screen; transverse wave measurements were taken under special field conditions. Results were consistently repeatable within the accuracy of the oscilloscopes utilized.

Jan 1, 1966

By C. T. Baroch

This report summarizes cost data accumulated during 15 months of sustained operation of the Bureau of Mines Boulder City (Nev.) titanium plant, which had a capacity of about 1,350 pounds of titanium sponge per day. The plant was constructed during the 1952 fiscal year with funds supplied by the Ordnance Corps, Department of the Army. Its original purpose was to engage in process development work as a continuing phase of the Bureau of Mines policy to seek improvements in producing titanium metal. In early 1953 the Defense Materials Procurement Agency contracted with the Bureau of Mines for producing approximately one-half million pounds of usable ductile titanium sponge. Production began in May 1953, ended in September 1954, and yielded 492,503 pounds of acceptable metal. Operating costs covering this period of operation, with suggested depreciation and administrative costs, are given, as well as outlines of building and equipment capital costs. In addition, miscellaneous economic considerations are discussed, including labor and operating-time schedules.

Jan 1, 1956

By Gerald W. Elger

This report describes development of the fusion-leach crystallization precipitation process for producing a hafnium content feed material for hafnium-zirconium separation plants. Mixtures of zircon, potassium silicofluoride, and potassium carbonate (or potassium chloride) were fused to prepare soluble potassium zirconium hexafluoride-potassium hafnium hexafluoride salts. High extraction of these salts was obtained by countercurrent leaching the fused material in dilute hydrofluoric acid. About one-half of the hafnium was recovered in hafnium-enriched mother liquor by cooling clarified lead: liquor to crystallize most of the zirconium salt. Additional hafnium was recovered from the primary crystals in a multiple dissolution-recrystallization step. Hafnium-enriched oxides having a hafnium-zirconium ratio of more than three times that of zircon were precipitated from the combined mother liquors. The hafnium and zirconium recoveries in the precipitate were 83 and 24 percent, respectively. About 71 percent of the zirconium and the remainder of the hafnium were recovered in potassium zirconium hexafluoride crystals of low-hafnium content.

Jan 1, 1966

By L. A. Haas

The Bureau of Mines conducted bench-scale leaching tests with recycled spent copper electrolytes and copper-nickel mattes produced from the Minnesota Duluth Complex concentrates. This report describes the first stage of an overall two-stage leach operation. The objective of this research was to determine the matte-leach technology required to convert spent copper electrolyte into an enriched nickel liquor suitable for a nickel refinery and there-fore essentially free of copper, iron, and sulfuric acid. The experimental variables investigated were matte composition, particle size, spent electrolyte content, pulp concentration, oxygenation, temperature, and time. The time required to produce an enriched purified nickel liquor decreased with increasing pulp concentration, temperature, and oxygenation, but increased with increasing particle size and electrolyte copper and acid content. Nickel-rich (about 50 g/l) liquors at a pH of about 4 and containing less than 1 g/l of copper and iron were produced at 70° C by leaching minus 325-mesh low-iron (less than 5 pct) matte for 8 hours with spent electrolyte containing 22.4 g/l Cu, 28.9 g/l Ni, less than 0.1 g/l Fe, and 50 g/l H2S04 at a pulp concentration of 1 kg of matte per liter of spent electrolyteo Varying the nickel content of the spent electrolyte from 11 to 101 g/l appeared to have no appreciable influence on the matte leaching characteristics.

Jan 1, 1981

By N. A. Gokcen

This Bureau of Mines report reviews and summarizes recent studies of the rates of chlorination of aluminous resources with CO and C12 mixtures with and without COC12. No reaction mechanism could be obtained from the existing results; however, diffusional barriers in the gas and solid layers probably control the chlorination rate in thermogravimetric experiments. Fluidized beds of particles smaller than 0.1 mm appeared to show very little solid layer diffusional barrier. For optimum chlorination the particle size should probably be less than 8 mm, the calcination temperature approximately 700° C, and the chlorination temperature from 650° to 750° C. Relatively rapid chlorination with COC12 in thermogravimetric experiments was attributed partly to the simultaneous supply of reductant and chlorinator by one gas to the sample reaction site. Comparable results for chlorination of fluidized beds with COC12 are not available. Equimolar mixtures of CO and C12 produced the optimum rate of reaction. Addition to the calcine of 10 to 20 wt-pct NaCl accelerated the rate of chlorination, and addition of SiC14 to the gas mixture decreased the rate of chlorination of SiO2 drastically, but at the expense of chlorination of significant fractions of Al2O3. Further research in various areas is suggested.

Jan 1, 1983