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By E. C. Tarpley

An acid-extraction procedure developed in Germany for determining mineral matter in coal was investigated by the Bureau of Mines to determine its application to American coals. It was found to be suitable for all ranks of coal from anthracite to lignite if modified slightly for coals containing considerable quantities of calcium compounds, such as calcite or calcium humate. The precision of the method is satisfactory, and the results are probably closer to the true content of mineral matter than those obtained by empirical formulas. The method requires considerably more analytical data than the Parr or approximation formulas but is no more time consuming than obtaining the necessary data for the King, Maries, and Crossley formula (theoretically the most comprehensive empirical formula used). An appendix to this report includes a detailed description of a recommended procedure.

Jan 1, 1959

By J. F. Barkley

Field tests were made on the rate of corrosion of 30 materials used in air preheaters under regular operating conditions, and the buildup of deposits was observed. Twenty-three materials were tested with coal as the fuel on an underfeed stoker and seven with oil, including a short period with pulverized coal as fuel, The plant equipment is described, and pertinent plant operating data are tabulated. Figures 17 and 19 (pp. 24 and 27) give the results of corrosion tests on the uncoated metal test specimens. The information obtained from these tests follows the general pattern described in Bureau of Mines Report of Investigations 4996, Corrosion and Deposits in Regenerative Air Preheaters. The deposits were similar, and the corrosion rates of Cor-Ten and Mayari-R steel (previously found to be essentially the same at the Harding Street Station using coal) continued to show little difference at the Marion Generating Station using principally oil. The one high-alloy steel tested, type 321, showed a much higher corrosion rate than the low-alloy steel, Cor-Ten.

Jan 1, 1959

By Richard N. Appling

This report presents information obtained by examination and investigation of manganese deposits in northeastern Oregon during May and June 1954 and April 1957. Maps, assays, and other examination data are presented on 10 manganese deposits -9 in Baker County and 1 in Grant County. Included among these deposits are all those that have undergone substantial exploration or have a record of production. Seven of the Baker County deposits occur as characteristically small, irregular pods and lenses in argillite. The remaining Baker County prospects are [marily] narrow, vein-type occurrences in schist. The Grant County occurrence in greenstone and serpentine. All the deposits are composed of various manganese oxides, intermixed with abundant quartz and chert.

Jan 1, 1959

By T. M. Nasiatka

This report sterns from a study undertaken by the Federal Bureau of Mines to determine the possibility of reducing filter-cake moisture by applying radiant heat. Suitable laboratory equipment was set up to study the effect of heat, heating time, proximity of the heater to the filter cake, cake thickness, and other variables related to the final filter-cake moisture. A minus-48-mesh coal slurry and application of heat for 60 seconds resulted in filter-cake moistures 5.6 to 13.2 percentage points lower than could be accomplished by filtration alone at 24 inches of Hg for 1-1/4-and 1 1/2-inch cake thickness, respectively. The moisture reduction can be attributed to the combined effect of lower fluid viscosity and evaporation.

Jan 1, 1959

By H. S. Caldwell

A magnesium-base incendiary alloy, containing about 20 percent cadmium, 4 percent aluminum, and 0.5 percent zinc, was investigated in a series of vacuum-distillation experiments to determine the feasibility of recovering magnesium and cadmium as refined metals. Alloys prepared in the laboratory and actual bomb-casing alloy were studied at temperatures of 550° to 750° C. and pressures of 100 to 150 microns. Simple distillation and fractional distillation methods were only partly effective in separating the cadmium and magnesium. They were separated satisfactorily, however, with a special vapor baffle designed to condense the metals selectively. Magnesium and cadmium products were 99 percent pure and together comprised 82 percent of the total condensate. About 17 percent of the condensate was intermediate-grade alloy that could be recycled with new charge and contained about 70 percent magnesium and 30 percent cadmium.

Jan 1, 1959

By J. P. Coughlin

Gypsum plaster is calcium sulfate hemihydrate (CaS04-1/2H2O). There are two varieties, commonly designated as a and ß. The hydration setting) of this plaster involves the chemical reaction: CaS04?1/2H20(c) + 3/2H20(l) = CaSO4?2H20(c); that is, the hemihydrate combines with water to form the dihydrate. Many substances, when present as impurities, either in the hemihydrate or the water have influenced the rate of the hydration reaction. The objective of the Bureau of Mines work described in this report was to investigate the accelerating or retarding effects of small amounts of dissolved substances and to attempt to classify these effects upon a chemical basis. To eliminate competing effects, the work was conducted separately on the two varieties of hemihydrate; both were in highly pure form. (Commercial plasters usually are a mixture of the hemihydrates, with other substances present as impurities.) As the hydration reaction of each variety of hemihydrate evolves heat in amounts known from previous work, 5,6/ the authors decided to use calorimetric methods to follow the extent of the hydration reaction as a function of time. Two calorimetric methods were employed. One was designed to study the hydration reaction with a large water to plaster ratio and the other with a small water to plaster ratio (to simulate commercial practice in utilizing plaster).

Jan 1, 1959

By J. B. Gayle

The merits of the various methods for dry-quenching coke have been the subject of numerous publications and almost equally numerous controversies for the past 40 years.5/ Most investigators have concluded that dry quenching is advantageous. Some have based their arguments on the improved physical properties of the resultant cokes. Others have claimed little or no improvement and have based their arguments on the economies acquired from the recovery and utilization of sensible heat. The extent to which the method of quenching influences the properties of the resultant cokes is of importance in connection with the operation of both commercial and experimental ovens. On the other hand, the recovery and utilization of sensible heat are economic problems related solely to commercial oven operation and- depend on the method of dry quenching used and the demand for a low intensity energy source. The scope of the present Bureau of Mines investigation has been limited to a comparative study of the properties of wet- and dry-quenched cokes produced from six coals and blends carbonized at flue temperatures of 2, 000° and 2,400° F. in the Tuscaloosa oven.

Jan 1, 1959

By R. L. Grant

An investigation was undertaken by the Bureau of Mines to determine the relationship between freespace and ignition probability for borehole shots. A series of experiments was concluded which covered six freespace conditions for a pemissible explosive in a 3/4-inch borehole and encompassed some 700 shots. The results were analyzed statistically. From the analysis of variance, it was concluded that the freespace means were different and that this conclusion is not impaired by possible differences in the explosives used. Within the limitation of this experiment, a definite relationship was found between the freespace and the ignition probability. Specifically, the incendivity increases with increased freespace up to a maximum; beyond this maximum there is some indication of decreasing incendivity. Further investigations are in progress to establish whether the effects of freespace on ignition probability reported here are applicable to the large test gallery, INTRODUCTION A borehole loaded with an explosive charge is a common feature of the routine gallery tests for determining the permissibility of coal-mine explosives, of Experimental Coal-Mine shots, and of the small steel cannon shots used in connection with certain research programs on the ignition of firedamp (6, 10).6/ The question of the interrelationship of freespace, weight of charge, and ignition probability of the methane-air atmosphere has been raised

Jan 1, 1959

By Quintin A. Aune

This report presents the results of a field and laboratory study by the Federal Bureau of Mines, in cooperation with the California Division of Mines, of the swelling-type bentonite deposits in the Vallecitos area in San Benito County, Calif. The purpose of the study was to learn if these large deposits contain bentonite of sufficient quality and quantity to be of economic value as an oil-well drilling mud additive. Large amounts of bentonitic clays are used by the petroleum industry as well as the steel industry in California. Additional amounts may be required in the near future as a concrete or earth-fill admixture in constructing dams and canals in the California Central Valley. Depletion of some local clay deposits and loss of others to military installation areas have given new emphasis to the need for developing new bentonite deposits in California.

Jan 1, 1959

By K. K. Kelly

METALLURGICAL thermochemistry of titanium is a broad subject and (if data were available) could include a wide variety of topics. The present report is restricted to extractive metallurgy and to substances and reactions that bear upon the magnesium, sodium, and hydrogen-reduction processes employing titanium tetrachloride. The aim has been to present enough data so that the reader not only can check: the calculations for the reactions discussed but also can conduct related calculations if he so desires, without recourse to other compilations of data. The subject matter divides naturally into two parts-the selection of the data to be adopted and the application of these data to pertinent metallurgical reactions.

Jan 1, 1959

By P. G. Pigott

The lack of technical information regarding the physical characteristics of kaolins and bauxitic kaolins, rejected during the mining of bauxite near Eufaula, Ala., has retarded their commercial utilization. This investigation was undertaken to determine their behavior when used in refractories. Ores were evaluated as refractory raw materials by compounding dry-press mixtures and specialties following procedures common to the industry. Products now on the market were used for comparison in laboratory evaluation.

Jan 1, 1959

By O. Q. Leone

Excellent metal quality, with lower power requirement, is attained in electrorefining titanium by using internal heating of the fused-salt bath. An internal heater provides more effective heat utilization, simplifies structural components in cell design, and prolongs cell life by eliminating direct application of heat to the cell container. This Bureau of Mines report covers one phase of the research in progress at the Electrometallurgical Experiment Station at Boulder City, Nev., for improving the techniques and lowering the total power requirement for electro-refining titanium metal.

Jan 1, 1959

By H. G. Wolfhard

The mode of propagation of explosions through narrow passages is important for understanding flameproofed equipment employed in mines. Narrow channels have been used in this investigation that connected between a small explosion chamber and a large chamber containing fuel-air mixture. The oxygen index of the mixture in the small chamber was determined which caused an explosion in the outer chamber. Preliminary measurements have already been given in Bureau of Mines Report of Investigations 5457 and suggested that) flames do not pass through narrow channels. The hot, burned gases from the explosion in the small chamber, however, are able to ignite the mixture in the large chamber by a process of hot-gas ignition. Systematic measurements are reported in the present paper that cover the influence of channel length and diameter and the properties of the gas mixtures in the large chamber on the transmission of explosions. The influence of such properties as quenching diameter and flame temperature is also discussed. This paper concludes the work on this problem and presents a theory that describes in detail parameters that influence transmission of explosions through narrow channels. INTRODUCTION Flameproofed equipment in mines is usually provided with flanges. A gap between the opposing flanges allows ventilation and release of pressure. The safe gap width has been determined for a number of flange lengths by Smith4/

Jan 1, 1959

By R. B. Fisher

This report gives the results of mineralogical research on the Nicaro (Cuba) nickel ores and plant products. These studies were made under a cooperative agreement with the General Services Administration (GSA) of the U. S. Government. The purpose of the investigation was to obtain fundamental data that would be useful to other GSA contractors concerned with the Nicaro ores in their research on reduction roasting, leaching, and other phases of the project; and to the metallurgical staff of the Nicaro plant in Cuba. The overall objective of the combined research was to provide data to accomplish metallurgical improvement in the operations of the U.S. Government-owned plant at Nicaro, Oriente Province, Cuba. Particular emphasis is placed on improving the recovery of nickel from the ores and on the possibility of recovering other valuable constituents, especially cobalt. This study presents the physical and chemical characteristics, mineral associations, differential thermal analyses in controlled atmospheres, and X-ray studies of the ores and plant products. The nickel ores, serpentine and laterite, were from the Ramona-Lama Mulo and Ramona ore deposits. Serpentine ore consisted of serpentine-group minerals, basic iron oxide, magnetic iron oxides, chromite, olivine, enstatite, anthophyllite, cryptocrystalline quartz, wad, and a trace of calcite. This ore contained 1.6 percent nickel, 0.05 percent cobalt, 0.86 percent chromium, and 17.4 percent iron. Laterite are was composed principally of goethite with some altered serpentine, quartz, chromite, wad, magnetite, maghemite, and hematite. It carried 1.3 percent nickel, 0.11 percent cobalt, 1.9 percent chromium, and 48.4 percent iron.

Jan 1, 1959

By William J. Campbell

This report describes a Bureau of Mines study undertaken to determine the applications and limitations of solution techniques as a general method of fluorescent X-ray spectrographic analysis. Systematic errors due to variations in particle size, surface preparation, and sample inhomogeneity are eliminated by the use of solutions. The range of applicability of fluorescent X-ray spectrography is increased in two ways: (1) Samples in the form of wire, filings, turnings, etc., can be analyzed as solutions, and (2) samples submitted as solutions can be analyzed as received 0 The lower limit of detectability varies from 0.14 gram per liter for sulfur, atomic number 16, to 0.0015 gram per liter for strontium, atomic number 38. Most elements have limits of detectability between 0.02 and 0.002 gram per liter.

Jan 1, 1959

By William A. Stickney

The zirconium-hafnium separation plant at Albany, Oreg., was the result of a chain of events that started with studies by A. R. Kaufmann at the Massachusetts Institute of Technology. Variations in the listed neutron-absorption cross-section of zirconium caused him to suspect a misprint. As a result of these discrepancies and following his suggestions, Oak Ridge scientists made studies establishing a value of 0.4 barn or lower. This meant that the potential of zirconium for reactor application was greatly enhanced. Since hafnium is invariably associated with zirconium and has a high neutron cross-section, it was necessary that an efficient hafnium-separation method be developed before the superiority of zirconium as a structural material in nuclear reactors could be realized. The Albany plant was built and operated for the Atomic Energy Commission (AEC) under Letter Agreement AT-(11-1) -140, patterned after a plant operated by the Carbide and Carbon Chemicals Corp. at Oak Ridge, Tenn. Construction was begun in April 1951. Hafnium was to be extracted preferentially as hafnium thiocyanate from an aqueous mixture of zirconyl and hafnyl chlorides in hexone (methyl isobutyl ketone) by a liquid-liquid countercurrent system.

Jan 1, 1959

By Carl Rampacek

Recent research by the Bureau of Mines has demonstrated that the segregation process has merit for treating oxidized and mixed oxide-sulfide copper ores. The process comprises heating the crushed ore with salt and coke or other carbonaceous materials at about 700° C. to produce fine flake copper, which then is recovered by conventional copper-flotation methods. Bench-scale laboratory tests of a number of oxidized and mixed copper ores assaying 0.78 to 5 percent Cu gave copper recoveries of 73 to 96 percent. The flotation concentrates assayed 21 to 76 percent Cu, depending on the ore being treated.

Jan 1, 1959

By J. W. Chester

The rapid depletion of zinc-lead ore reserves and the rising costs of exploration have been major factors in the decline of mining activities and explorations for additional reserves in the Tri-State mining district. There is a need to develop new or adopt known, improved exploration techniques that will appreciably lower the costs of exploration. Demonstration of the practicability of using improved techniques to indicate, rapidly and cheaply, mineralized areas or geologic structures where more intensive explorations are justified could stimulate the search for and discovery of additional ore reserves. Various operators in the Tri-State district have used geophysical surveys to some extent since 1928 to guide exploratory drilling. Some geophysical investigations have also been made in the district by the State Geological Surveys of Kansas (11)3/ and Missouri (8, 13) and by Federal agencies (16), with the objective of directing exploratory drilling to areas where geologic conditions favored ore deposition. Many factual data obtained have not been published. The investigations generally have not been broad enough to permit conclusive evaluation of the usefulness of the geophysical techniques in all parts of the district.

Jan 1, 1959

By W. Beckering

IN CHARACTERIZING tars obtained by the low-temperature carbonization or North Dakota lignite, infrared spectra have been an invaluable aid in both qualitative and quantitative examination. Quite early it became evident in the tar-research program of the Bureau of Mines, U.S. Department of the Interior, that the small number of published spectra available for hydroxy aromatics would be inadequate for comparative purposes when dealing with the wide range of compounds present in coal tar; therefore, compiling a catalog of spectra was initiated as a continuing part of the tar program. As these spectra should be valuable to other investigators in this and related fields, they are being presented in this report. This group or spectra (figs. 1-98) represent 97 compounds, largely phenolic materials. The major problem of this project has been the availability of materials for examination. Samples have been obtained from commercial and private laboratories or synthesized at the Bureau of Mines Lignite Experiment Station, Grand Forks, N. Dak.

Jan 1, 1959

The complex organic chemicals in coal differ from those in petroleum mainly by the ratio of carbon atoms to hydrogen atoms; this ratio is about 2 for coal and 1 for petroleum. By changing the ratio, coal can be converted into compounds similar to those found in petroleum. In. very simplified form, omitting here the special conditions required, the paths by which this can be done are: [ ] Part or all of the coal is first gasified by reaction with steam and oxygen, either in a gasifier or while the coal is still in place underground. The resulting gas is mainly hydrogen and carbon monoxide, with impurities that .must be removed before further processing by one of the following routes.

Jan 1, 1959