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By N. E. Hanna

The effect of small percentages of sodium chloride on the incendivity of permissible explosives was studied by the Bruceton up-and-down technique in gallery tests. Both the reduction in incendivity achieved by addition of sodium chloride and application of the test method to explosives evaluation are discussed. It is demonstrated that the up-and-down technique in gallery testing is suitable for distinguishing differences in incendivity between different explosive compositions and between lots of the same composition. The study also shows that addition of relatively small quantities of sodium chloride tends to reduce the incendivity of explosives to firedamp, but addition of sodium chloride cannot insure reduced incendivity. Any improvement attributable to the salt can be counteracted by undefined variations in the explosive. The need for experimental investigations of a number of factors that may affect the safety of permissible explosives is emphasized. ACKNOWLEDGMENTS Grateful acknowledgment is made of the assistance of Roy L. Grant in analyzing for normality of distribution of the data obtained by the up-and-down methods and to Harold E. Tubbs for numerous calculations.

Jan 1, 1959

By J. B. Gayle

The Bureau of Mines sole-heated oven has been used for studying coal expansion for some 20 years. During the period before 1940 emphasis was placed on studies of the mechanism of coal expansion and the effects of variations in operating conditions on the results. Since 1940 emphasis has shifted to a survey of the expansion properties of various coking coals. Because additional information concerning a number of unsolved problems in connection with the earlier studies appeared highly desirable, this investigation of the use of sole-heated ovens for studying coal expansion was undertaken. The principal findings, in order of their discussion in the text, may be summarized as follows. 1. Expansion results for binary blends of coking coals exhibit nonadditive behavior, both positive and negative deviations from additive behavior being noted, depending on the particular coals tested. Additive behavior can be achieved, however, either by charging the blend components in separate layers (which indicates that the observed phenomena are not characteristic of the particular expansion oven used) or by testing relatively coarse sizes of coal (which suggests that the effects of crushing on the expansion properties of coking coals may be even more complex than is generally recognized).

Jan 1, 1959

By W. M. Mahan

This report describes work carried out by the Federal Bureau of Mines in cooperation with the General Services Administration (GSA). Tests on nickel oxide reduction were conducted at the Pyrometallurgical Laboratory at Pitts-burgh and Bruceton, Pa., and at a rented plant at Canonsburg, Pa. Nickel oxide was reduced to sponge nickel, which was then melted to produce specification-grade nickel ingots containing a minimum of 98.50 percent nickel plus cobalt and a maximum of 1.00 percent cobalt. One purpose of this study was to determine if specification-grade nickel could be made from nickel oxide produced at the United States-Government-owned plant at Nicaro, Cuba, in pilot-plant scale operations involving direct reduction and melting processes. A second and equally important purpose was to obtain cost data on the pilot-plant operation to estimate the cost of producing ingot nickel at an annual rate of 12 million pounds. Laboratory tests verified that nickel oxide, in saggers and in the presence of anthracite fines and dolomite in the ratio of approximately 20:5:1, could be converted to sponge nickel when heated to approximately 1,900° F. for about 2 to 4 hours, depending on the size and density of the oxide charge. The tests also determined the type of saggers suitable for pilot-plant operations.

Jan 1, 1959

By R. Barany

This paper reports determinations of heats of formation (from the oxides and elements) of crystalline cadmium metasilicate and crystalline lead meta-silicate by hydrofluoric acid solution calorimetry. The results, in conjunction with known entropy values, yield free energies of formation. There are no earlier data of this type for cadmium metasilicate. The results of this investigation for lead metasilicate deviate from the literature values (which are less reliable) in the direction of increased thermodynamic stability. Both cadmium and lead metasilicate are much less thermodynamically stable with respect to their constituent oxides than are the corresponding compounds of the alkaline earth metals.

Jan 1, 1959

By J. G. Walters

In a survey of the coking properties of United States coals, the Bureau of Mines has accumulated data on more than 500 coals and blends tested by the Bureau of Mines-American Gas Association (BM-AGA) method.4/ The importance of these tests depends upon the fact that a greater number of different coals has been tested in this apparatus than in any other of similar scale, thus permitting comparison of the carbonizing properties of many coals. Evaluation of BM-AGA results with respect to industrial data supplied by member firms of the American Gas Association was one of the first objectives in developing this test apparatus and procedure. Early data showed that, de-pendent upon BM-AGA carbonizing temperature, BM-AGA and commercial results agree closely.5/ Because of limited data, statistical relationships were not established at that time.

Jan 1, 1959

By R. L. Montgomery

The literature has been surveyed and values recalculated for the heats and free energies of formation of solid rare-earth compounds at 298° K. In most instances it was necessary to estimate the entropies. Thermodynamic properties of aqueous rare-earth ions have also been calculated. INTRODUCTION The accumulation of thermochemical data on rare-earth compounds in recent years makes it possible to review the subject and to obtain more consistent and more reliable information than was available previously.

Jan 1, 1959

By J. H. Field

Capital and operating costs have been estimated for removing sulfur dioxide from flue gases of a powerplant of 12,000-kw. capacity by liquid-purification processes, using limestone, ammonia, or sodium sulfite as the reactant. The annnonia and sodium sulfite processes yield end products that may be marketable. Coals containing about 1.5 and 5.0 percent sulfure have been considered. The sulfur dioxide content of the gases to be treated is 0.083 and 0.30 percent, respectively. Estimates have been made for 90-percent removal of the sulfur dioxide from both gases. A third instance has been considered in which 70 percent of the sulfur dioxide is removed from the flue gas of 0.30-percent concentration. The scrubbed gas would contain 0.09 percent sulfur dioxide, which might be within the permissible limit for discharge to the atmosphere in most areas. Although it is unlikely that flue gases with sulfur dioxide concentrations of less than 0.10 percent would require purification, a cost estimate for such a gas is included because an estimate is available for a British plant employing the limestone process at these conditions. Capital investment and operating costs, with no credit for products, are lowest for the limestone process for gases of both concentrations. Crediting the ammonium sulfate and sulfur produced in the ammonia process at their market prices at the end of 1956 of $32 and $28 per ton, respectively, the operating costs of the ammonia process become the lowest for purification of the gas containing 0.30 percent sulfur dioxide. The operating costs of the sodium sulfite process for purifying gas of high sulfur dioxide content approach those of the limestone process when the byproduct sulfur dioxide is credited at $14 per ton. Even if credit for products is allowed for the ammonia and sodium sulfite processes, the operating costs are higher than those of the limestone process for the gas of low sulfur dioxide content. Because of the large quantity of materials that would be produced by removing sulfur dioxide from a relatively small number of plants, credit for products should be allowed with extreme caution.

Jan 1, 1959

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 Van E. Shaw

Bastnaesite is a natural rare-earth fluorcarbonate of the cerium group that affords an abundant and high-grade source of the lighter rare-earth elements. A simple and efficient method has been developed by the Bureau of Mines for extracting rare-earth compounds from this mineral. Digesting of a flotation concentrate with sulfuric acid converts the rare-earth compounds from fluorcarbonates to sulfates. Action of the acid releases gaseous com-pounds of fluorine and silicon, leaving the sulfated material free of these elements; carbon dioxide from carbonate decomposition is eliminated at the same time. Calcining the sulfated material at 1,200° F. renders the gangue constituents insoluble, whereas the rare-earth sulfates are left in water-soluble form. Leaching with water yields a solution of pure rare-earth sulfates. Bastnaesite could become prominent as a source of cerium-group rare-earth elements. It is rich in the light rare-earth elements and comparatively easy to process; reserves of the mineral are extensive enough to supply a greatly expanded market for many years.

Jan 1, 1959

By T. E. Gray

This report describes the preparation characteristics of the more significant coal beds in Washington County, Pa. It is one of a series planned to determine coals suitable for producing metallurgical coke, either as mined or after beneficiation. More than 15 million tons of coal was produced in Washington County in 1956; 89.8 percent was cleaned mechanically in 10 cleaning plants. The Bureau of Mines has estimated that 2,280 million tons of recoverable coal remained in beds 28 inches thick or more as of January 1, 1954.

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 Alton B. Cook

Equipment has been designed and fabricated for study of the vaporization of oil during gas-cycling operations, A sand-packed steel tube, which can be rotated to minimize gravity drainage, is used as a model oil reservoir. A minute windowed cell at the discharge end of the tube through which the liquid-gas interface may be observed, makes possible the separate removal of produced free gas and gas-saturated oil. The operation of the model oil reservoir, and auxiliary equipment, are described by use of a schmatic flow diagram. Details of the specially designed equipment are illustrated by isometric and pictorial drawings, and a description of the experimental procedure is given.

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 Kenneth M. Earl

The purpose of this investigation was to obtain subsurface information on the John Burdette barite-fluorite deposit, Garrard County, Ky. The deposit was intersected in each of five inclined diamond-drill hales aggregating 1,163 feet. All holes were drilled from the hanging wall of the deposit; the inclinations varied from minus 41° to minus 75°. Disseminated metallic sulfides were noted in the drill cores from holes 1, 2, 4, and 5. The deepest drilling was hole 5, which intersected the deposit at approximately 490 feet down dip. Visual inspection of the cores did not indicate mineralization of economic importance; therefore, no chemical analyses were conducted. Condensed logs of diamond-drill cores are included in this report. All drill cores were shipped to the Bureau of Mines core library in Minneapolis, Minn., for future reference,

Jan 1, 1959

By D. H. Baker

This report, one of a series prepared by the Federal Bureau of Mines on the technology of titanium, describes the development of an electrorefining cell from which cathode deposits up to 30 inches long can be produced. Data show individual deposits to be homogeneous, comparable from top to bottom, and not varied in quantity or quality of metal over the entire length of the deposit. Investigations concerned with various diameter cathodes showed that cathode current efficiencies were materially reduced with cathodes less than 2 inches in diameter. Deposits produced on 1/2-inch-diameter cathodes showed cathode current efficiencies of 19 percent and on 1-inch cathodes, just over 22 percent, whereas deposits produced on 2- and 4-inch-diameter cathodes showed about 70-percent current efficiencies. A series of 20 deposits on 4-inch-diameter cathodes was produced under simulated production operation. The average current efficiency, based upon a divalent ion, was 72 percent with 11 1/2 pounds of metal produced per cycle of operation - 98.8 percent of which had a Brinell hardness number (B.h.n.) of 80 or less.

Jan 1, 1959

By T. T. Campbell

This report describes the development of new electroplating baths from which tin-nickel alloy plate was deposited. Although tin-nickel plate can be deposited from an aqueous ammonium bifluoride bath, the corrosive nature of this bath has served as a deterrent to its use. The Bureau of Mines felt that more general acceptance of this new alloy plate would follow if neutral or alkaline baths could be developed. Promising results were obtained from electrolytes containing both tin and nickel chlorides dissolved in triethanolamine-hydrochloric acid or in ethylene glycol hydrochloric acid baths. Current efficiencies close to 100 percent were obtained with these baths. Research revealed that tin-nickel plate could be produced from organic solvents or from mixed aqueous-organic electrolytes. The composition of the alloy deposit - 65 percent tin and 35 percent nickel - was found to exhibit the same single-phase structure that is obtained from the commercially accepted fluoride-type bath.

Jan 1, 1959