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By G. J. Slavens

The U.S. Bureau of Mines conducted research on preparing submicrometer titanium nitride (TiN) powder as a substitute for tungsten carbide (WC) in cutting tools and wear-resistant parts. Earlier research on a small scale was expanded to include a larger reactor. The TiN powder was produced by contacting titanium tetrachloride (TiCI4) with anhydrous ammonia (NH3) in the presence of Mg at 1,100° C. The powder was collected in an electrostatic precipitator (ESP) filled with ultra-high-purity (UHP) Ar. All collected powder was thermal vacuum distilled to remove Mg and magnesium chloride (MgCl2), leaving the purified TiN. Powder handling and purification procedures were conducted to assure low oxygen content in the powder product. Oxygen content in the distilled TiN powder product was as low as 0.40 wt pct. Nitrogen averaged near 22.0 wt pet with a high of 22.4 wt pct. The purified powder product had an average median particle diameter of 0.14 µm with a standard deviation of 0.09 µm.

Jan 1, 2010

By P. M. Sullivan

Galvanizers' sal skimmings have been treated by two methods of leaching in attempts to produce preflux solutions suitable for use in galvanizing operations. Both water-leaching and acid-leaching procedures are effective, except in severely exhausted skimmings when water-leaching becomes impractical. A preliminary analysis of the skimmings is not required. Solutions in the recommended concentration range can be produced conveniently by control of pH, specific gravity, and chlorine content. A technician would require only a short period of training to be able to perform the operations described.

Jan 1, 1958

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 Alton B. Cook

In the Scurry Reef field, Scurry County, Tex., a study was made to determine the physical properties of the oil in all parts of the reservoir by a new method developed for this study. The method involved correlation of data from a survey 1 of the gravity of the produced oil, from measurements of gas-oil ratios on key wells selected to give representative data for the entire reservoir, and from laboratory analyses of reservoir oil samples. A field survey was made of the API gravities of the produced oil by testing oil samples from 107 key wells. Precise gas-oil-ratio tests were made on 45 key wells that were producing under comparable separator-operating conditions. Subsurface-oil samples were obtained from seven wells, selected to provide reservoir oils ranging approximately from a minimum to a maximum in saturation pressure. The physical properties of the subsurface-oil samples were determined, and correlations were made of these laboratory data with the field gas-oil-ratio test data. These correlations were then used to estimate physical properties of the oil throughout the reservoir. A logical procedure of determining the variations in physical properties of reservoir oils in most fields is to obtain and analyze subsurface-oil samples from enough key wells to provide an ample coverage of the field. Under this procedure, data from a large number of samples would be needed to provide the desired information on the Scurry Reef field, as it is one of the largest known in the United States.

Jan 1, 1955

By Alla D. Mah

The energies of combustion of two carbides of tungsten and two carbides of molybdenum were measured , and the corresponding standard heats of combustion were derived . The results are as follows : WC : AH298.15 ( combustion ) = -285,940 ± 250 cal /mole , W₂ C: AH298.15 (combustion ) = -490,660 ± 400 cal /mole , Mo₂ C : AH298.15 ( combustion) = -439,350 ± 600 cal /mole , MoC : AH298.15 ( combustion ) = -269,800 ± 1,000 cal /mole . The combustion heats were combined with the heats of formation of the corresponding metal trioxides and carbon dioxide to obtain the following heats of formation : WC : AH298.15 ( formation ) = -9.6 ± 0.4 kcal /mole , WC: AH298.15 ( formation ) = -6.3 ± 0.6 kcal /mole , Mo₂ C : AH298.15 (formation) = -11.0 ± 0.7 kcal / mole , MoC : AH298.15 (formation ) = -2.4 ± 1.0 kcal /mole . The heats of combustion and formation of MoC are tentative .

Jan 1, 1963

By Curt D. Edgerton

This study was made to determine trends in fresh water usage by California petroleum refineries, to forecast fresh water requirements to 1975, and to evaluate water conservation practices. Statistical data used in the study were obtained largely from published sources and from records of selected companies. An adequate sampling of the State's refining capacity was obtained, and the data were extrapolated to the total California refining capacity. A breakdown of the data was then made on the basis of the following refining regions: (1) the Los Angeles Basin and Southern Coastal region, (2) the Southern San Joaquin Valley, and (3) the San Francisco Bay area. An unpublished forecast of crude oil input to refineries by a major oil company operating on the West Coast was used as a basis for predicting fresh-water usage. The 1963 fresh water intake by California petroleum refineries was 84 million gallons per day. This is expected to increase to 128 million gallons per day by 1975. The fresh-water to crude-oil ratio is increasing in all regions except the Southern San Joaquin Valley. At present, the supply of fresh water available to almost all of the State's petroleum refineries, mostly from surface sources and company-owned wells, is adequate, although shortages may develop within the foreseeable future. Present conservation methods are centered around the following four objectives: (1) minimum intake of fresh water of the lowest possible quality commensurate with sound technologic practice; (2) optimum recirculation; (3) proper treatment before discharge; and (4) substitution of air cooling for water cooling.

Jan 1, 1965

By Daniel T. Rogers

The Bureau of Mines, in its alumina miniplant project to investigate alumina recovery from domestic, non bauxitic ores, has conducted research on the use of a hydrochloric acid leaching, gas sparging crystallization technology. An important element of this research is the efficient separation of undissolved, siliceous residue from AICI3 -bearing leach liquors by continuous, horizontal, countercurrent vacuum belt filtration. In an effort to calculate material balances quickly and to predict material balances based on different belt filtration configurations, the perfect-mixing-cells-in-series model (PMCS) for calculating material balances around belt filters was used. Because of the porous nature of the solids, the model produced erroneous material balances. Therefore a reliable model, the shrinking voids model, was developed postulating the presence of an unwashable voids liquor volume that decreases with decreasing liquor AICI3 concentration. This volume decrease postulation is equivalent to assuming that dilute liquors flow more freely, causing more voids liquor volume to become washable. Least-squares based computer programs are provided, which are useful not only in producing material balances from plant data but also in predicting balances for untested configurations using the same feed materials.

Jan 1, 1982

By M. G. Zabetakis

The use of liquid hydrogen as a high-energy fuel introduces numerous hazards not ordinarily associated with the use of other more conventional fuels. These hazards are attributable to the unique properties of hydrogen in the liquid and gas states (table 1). Since little work has been conducted on explosion and related hazards of cryogenic fuels, a research program was undertaken to obtain basic data on such dangers for hydrogen and other combustibles under these conditions. These data were used to outline emergency procedures for protecting personnel and equipment when an accidental spillage of liquid hydrogen occurs and to establish a quantity-distance table for the storage of this fuel. The vaporization of liquid hydrogen from a surface is treated as a prob¬lem in heat transfer theory. Two extreme cases are briefly considered: (1) The transfer of heat occurs at constant temperature drop between, the boiling liquid and the hot surface, and (2) the transfer of heat is limited by the rate at which it can flow to the surface from a hot insulating medium. The available data indicate that the former case (1) is applicable when vaporizing from a conducting surface and, initially, when vaporizing from an insulating medium; the latter case (2) is applicable after initial flash vaporization has occurred from the insulating medium. The vaporization rate determines in part the rate at which flammable hydrogen vapor-air mixtures are formed above a spill area. However, the rates at which heat is transferred to the vapor, and air is brought in contact with it also are of importance. Accordingly, the distribution of flammable mixtures above a spill area was determined experimentally. In general, flammable mixtures were found to be both above and within the visible vapor cloud.

Jan 1, 1961

By Donald P. Schlick

This Information Circular presents a brief historical digest of the early attempts of the Bureau of Nines and the U.S. Public Health Service to establish coal mine dust exposure standards. It reviews current, accepted standards of the United States as well as available standards of other countries.

Jan 1, 1971

By R. H. Nafziger

Bureau of Mines research has shown that very low-sulfur pressure vessel steels with improved mechanical properties can be prepared by two melting processes. Four pressure vessel steels having sulfur contents ranging from 0.0008 to 0.0040 wt-pct, were produced by the electric-arc furnace or by the electroslag processes. Calcium carbide was used as a desulfurizer in the electricarc furnace. Fluxes containing at least 40 wt-pct CaO provided sufficient desulfurization during electroslag remelting. Element recoveries were higher for electroslag remelting than for metal melted in the electric-arc furnace. Bar rolled from electroslag-remelted ingots generally possessed higher tensile strengths and ductility than bar rolled from it t melted in the electric-arc furnace. Charpy V-Notch upper shelf energies were also improved as a result of electroslag remelting. The primary failure mode during impact testing was was microvoid coalescence. Sulfide inclusions were minimal, especially in the electroslag-remelted material.

Jan 1, 1979

By W. W. Agey

Past investigations on waterborne impurities in the flotation process have been concerned primarily with the treatment of specific ores with particular local waters. Although some anions and cations present in water are known to react with flotation reagents, a definitive study has not been made on the effect of such common ions upon the flotation process. This report describes the fundamental research undertaken to define and measure the adverse and/or beneficial effects of different concentrations and combinations of several common anions and cations when oleic acid is used to froth-float limestone from a pulp of quartz and limestone. Research on the effect of waterborne impurities upon the flotation process was composed of two equally important phases. The first phase comprised development of a procedure for floating limestone from quartz that would give the same results in test after test. Some difficulty was encountered, but once such a procedure was developed, the second phase, comprising study and measurement of the effect of various ions c on to natural water upon the flotation of limestone, was quickly completed.

Jan 1, 1963

By W. E. Robinson

Samples of raw oil shale and kerogen concentrates were oxidized by alkaline potassium permanganate, air, nitric acid, oxygen, and ozone to obtain information about the chemical structure of organic kerogen in oil shale. In one test, oil shale and oil-shale products were oxidized exhaustively with alkaline potassium permanganate, and the distribution of the organic carbon in the final oxidation products was determined. Comparing results of this oxidation with those obtained from other carbonaceous materials and known compounds gave information about the structure of kerogen. Alkaline potassium permanganate oxidation also was used partly to degrade kerogen into soluble products for characterization purposes. Structures present in these degradation products were indicative of type structures originally present in the kerogen. Nitric acid, oxygen, and ozone were used also for partly degrading kerogen to soluble oxidation products. Carbon-balance oxidation tests using alkaline potassium permanganate showed that Colorado oil-shale kerogen differs from many other carbonaceous materials such as coal and kerogens from other areas. Composition of the degradation products indicated that Colorado oil-shale kerogen is predominantly cycloparaffinic and saturated heterocyclic structures with some long-chain paraffinic and aromatic structures present. The ring systems may be connected through short carbon chains or bridges containing oxygen, nitrogen, and sulfur.

Jan 1, 1963

By Bruce F. Grant

This report discusses research being done by the Petroleum and Natural Gas Branch und the Applied Physics Branch of the Bureau of Mines to deter-mine the most effective uses of explosives in shooting oil and gas wells, as measured in terms of rates of production from the wells. An experimental investigation of the effects of detonating explosives in shallow holes drilled in rocks, chosen to be similar to those forming oil and gas reservoirs, forms the basis of this study. Records obtained from strain gages placed in the rock around the experimental shots permit determination of the generation and propagation characteristics of the strain wave. Water-injection tests made on the test holes before and after shooting allow the increase in fluid conductivity resulting from the shot to be determined. By rotating these data to the physical properties of the rock, and by conducting shooting experiments over the range of rock types common to oil and gas reservoirs, it is expected that relationships between the fluid conductivity and the properties of the explosive and rock can be developed and used for designing efficient shots for oil and gas wells. Four series of experiment.al tests were completed during the summer of 1949 and are described herein. The results of these tests confirmed the feasibility of the experimental approach and permitted outlining the plans for future research discussed in this report. This report is presented to acquaint industry with this research program and the progress to date, so that the Bureau may have the benefit of suggestions from interested readers.

Jan 1, 1950

By C. M. Mason

The methods currently used by the Bureau of Mines to evaluate the sensitivity, strength, incendivity, gaseous products, and physical properties of explosives and hazardous chemicals are described. Included are the tests used to evaluate explosives which arc certified as permissible for use in underground coal mines.

Jan 1, 1972

By L. R. Fisher

The purpose of this investigation was twofold: (1) To devise a rapid method for determining quantitatively the porphyrin-carboxylic acid content of a particular crude-oil porphyrin aggregate, and (2) to isolate porphyrins in the crystalline state from crude-oil porphyrin aggregates. The first purpose was accomplished by applying adsorption chromatography. In fulfillment of the second aim three different crystalline porphyries were isolated by methods which involved both adsorption chromatography and fractionation of benzene solutions with hydrochloric acid of varying strength. The three porphyrins had etio, rhodo-, and phyllo-type absorption spectra, respectively. INTRODUCTION Many samples of petroleum have, as interesting minor constituents, chemical compounds known as metalloporphyrins. Their presence in crude oil and other bituminous materials was first discovered by Treibs a quarter century ago. Much experimental work has been done on metalloporphyrins because of their importance to the petroleum industry. They have a deleterious effect on refining catalysts. The ash resulting from the burning of heavy fuel oil is very reactive, We to the presence of metallic constituents, particularly vanadium. In oil-fired gas turbines, the ash may build up on the blades, causing imbalance of the rotors and, in addition, severe corrosion. In industrial boilers, the ash residue is responsible for severe damage to boiler tubes and to the refractory brickwork (15).4 Through study of the chemical constitution of the various metalloporphyrins found in petroleum, much can be learned concerning the origin, migration, and history of crude oils.

Jan 1, 1961

By D. F. Hambley

This report documents the work carried out by Engineers International, Inc. and its subcontructor, W. G. Pariseau, in order to develop a design manual for ore passes for open pit mines. The work included an extensive information search, novel analyses in rock flow theory, cost and time estimation for shaft and raise construction methods, and development of design criteria for the are pass proper, dump point, and draw point.

Jan 1, 1983

By Mackenzie Burnett

The Brattice Window Method was used to measure the leakage rates of a total of 42 ventilation stoppings in 8 hardrock mines. Various types of stopping construction were evaluated. The following types are listed in order of decreasing effectiveness: 1) Cinder block, 2) Timber and mortar, 3) Timber and polyurethane foam, and 4) Timber and brattice material. There are slight differences in the effectiveness of the first three types, while the timber and brattice type is substantially inferior to the others. The repeatability of the Brattice Window Method was found to vary with physical conditions in the mine such as stopping location with respect to intersections, regularity of drift cross section, and the presence of hardware such as air and water pipes, timber sets and wire mesh. The Brattice Window Method is viewed primarily as a tool for estimating and comparing stopping leakages for the purpose of determining where repair efforts should be concentrated. A laboratory test program resulted in the derivation of several "rules of thumb" for employing the Brattice Window Method, which will aid in securing accurate and repeatable data.

Jan 1, 1979

By Thomas S. Jones

This Bureau of Mines publication reviews characteristics, manufacture, and uses of natural and synthetic iron oxide pigments. Supply and demand trends within the domestic industry and in foreign trade are presented for 1955 through 1976. Iron oxides are expected to continue in demand for traditional uses, and if anything, to be favorably affected by technological developments. Imports have been significant in relation to domestic production, most notably for synthetic oxides from West Germany and Canada.

Jan 1, 1978

By George Watkin Evans

The United States Geological Survey has estimated 1 that the State of Washington contains 11,412,000,000 tons of bituminous coal and 52,442,000,000 tons of subbituminous coal, in beds more than 14 inches thick. As the present rate of production is about 4,000,000 tons a year, Washington apparently contains coal enough to supply Pacific coast markets for many years. The character of the coal beds of Washington renders the production of clean coal very difficult, and a considerable proportion of the output is washed before it is marketed. In 1915 Washington ranked fifth among the States in the amount of coal washed, though only twentieth in total output. In that year 37.9 per cent of the coal produced in the State was treated in surface cleaning plants.

Jan 1, 1924

By David J. Kusler

This report describes a primary or direct, continuously sampling, and automatically averaging gravimetric method for analyzing gaseous mixtures of carbon dioxide, carbon monoxide) hydrogen, and (by volume measurement) nitrogen. The gaseous mixture is analyzed by passing it at a controlled and definite rate through a system that permits carbon dioxide and water retained by appropriate absorbents to be determined and the residual-gas volume (essentially nitrogen) to be measured. The accuracy and dependability have been established by comparison with very carefully conducted Orsat analyses. The method was developed for, and has been satisfactorily applied to, the analysis of blast-furnace top gas. It permits relatively attention free operation, using simple and low-cost materials usually found as basic equipment in the analytical laboratory. It provides, over a wide range of time or sampling intervals (from less than 1 to over 24 hours), the average composition, in terms of volume-percent, for those components usually determined in blast-furnace gas, if (as is usual) the flow rate of gas from the blast furnace is essentially constant over a selected analysis interval. Oxygen and methane are not determined; but, since these gases are normally absent or present only in traces, their analysis is seldom required.

Jan 1, 1959