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By R. L. Hopkins

Fifteen alkyl cycloalkyl sulfides and three dicycloalkyl sulfides were synthesized to provide reference compounds in the search for these classes of sulfur compounds in crude oils. In synthesizing sulfides by alkaline alkylation the order in which the reactants were added was shown to determine the yield and purity of the product.

Jan 1, 1966

By H. C. Fuller

Submerged combustion and inverse solubility methods were investigated as promising alternative means for crystallizing manganese sulfate from solutions produced by leaching manganese ores with either sulfuric acid or sulfur dioxide. Evaporation of water from typical manganese sulfate solutions by sub-merged combustion techniques enabled production of a slurry containing 32 to 39 pct MnSO4.H2O crystals suspended in a saturated solution of manganese sulfate. Such a slurry required further processing by thickening or filtration and drying to produce crystals of MnSO4.H2O. In a second approach, semicontinuous processing of manganese sulfate solu¬tions by thermal crystallization under pressure effected a recovery of 94.5 pct of the MnSO4.H2O as dry free-flowing crystals. Treatment of a solution containing about 100 grams manganese per liter at 189° C, produced a "barren" solution containing only 1.9 grams manganese per liter. Calculations made on comparable manganese sulfate solutions show that the heat requirement of the thermal crystallization method was about one-third to one-fourth that of the submerged combustion method.

Jan 1, 1966

By W. K. Coughlan

The Wabana deposit of Dosco Industries Limited is situated on the east coast of Newfoundland, at Bell Island in Conception Bay. It is a Clinton-type iron-formation of Lower Ordovician age. Five separate beds have been recognized, with others noted locally. Economic production has been obtained from the Lower, Middle and Upper beds, which are second, third and fifth in sequence, al-though at present only the Lower Bed is worked. The potential area of occurrence is about 70 square miles. It i;; bounded by major faults to the north, east and west and truncated by erosion at the south, where rocks of the de-posit crop out on the north side of the island. The iron is contained in oolitic hematite and chamosite, with minor siderite. As the deposit is submarine, conventional exploration methods are not applicable and much interpretation and projection from mined areas is necessary to guide exploration and development. With the interpretation of information from existing mined ores, it is possible, using a minimum of diamond drilling in advance of working faces, to maintain adequate ore reserves.

Jan 1, 1966

By J. A. Cavallaro

The heats of formation of anhydrous barium carbonate (witherite), strontium carbonate (strontianite), and lead carbonate (cerussite) were determined by solution calorimetry. The solution mediums were hydrochloric acid for barium and strontium carbonates and perchloric acid for lead carbonate. The heats of formation at 298.15° K are as follows: BaCO3 -297.5 ± 0.8 kcal/mole; SrCO3 -294.6 ± 0.5 kcal/mole; and PbCO3 -168.0 ± 0.3 kcal/mole.

Jan 1, 1966

By Harry R. Nicholls

Preliminary tests on presplitting rock in the presence of an in situ static stress field were undertaken to study the influence of a horizontal static stress field on the creation of a vertical presplit fracture plane. These tests indicated that it is easier to fracture the rock parallel to the in situ maximum compressive stress than in other directions. Instrumented shots indicate that the interaction of stress waves generated by the detonating charges is probably responsible for starting tensile fractures between shotholes and that expanding gases may propagate these initial cracks by a wedging action. The hole spacing for presplitting appears to be equal to the half wavelength of the stress wave. However, wider hole spacing appears feasible if the initial fracture is started by closer hole spacing.

Jan 1, 1966

By Donald W. Mitchell

Certification tests for urethane-foam systems and techniques for apply-ing foam safely in mines are described. Fire hazard from foam exists if flame propagates beyond the ignition source or penetrates the foam. Foam that passes the certification tests can be applied on stoppings, continuous sections of ribs of relatively wide passageways (with no foam on the roof), short sections of roof such as overcasts, roof cavities, and intersections (with no foam on the ribs), and between buntons on one wall of a shaft. Foam on the ribs and adjoining roof presents a fire hazard. Stoppings covered with foam passing the certification tests are resistant to penetration of heat, flame, and smoke than similar stopping without foam. Flame propagation can be arrested by water sprays. Spontaneous ignition of foam can be prevented.

Jan 1, 1966

By H. V. Fairbanks

It is estimated that millions of tons of coal fines are unsaleable each year due to difficulty of drying them economically with conventional mechanical dewatering and thermal drying equipment. The difficulty is due to the fact that coal of small particle size presents a large surface area with polar groups which have a great affinity for water. In order to remove this water thermally, a high temperature is necessary which oxidizes the surface of the coal. This substantially reduces the heating value of the coal. If drying could be satisfactorily carried out at a lower temperature, much more of the heating value of the coal fines could be retained. It was conjectured that acoustic energy applied during the drying process might prove to be of value since acoustic energy has the property of producing cavitation at a liquid-solid interface when the intensity is sufficiently great. This cavitation process produces water at room temperature which can be carried away from the solid surface by a flow of relatively cool air. Hence, moisture removal is made possible at a lower temperature.

Jan 1, 1966

By John Nagy

The Bureau of Mines adapted thermal theories explaining combustion of gases to correlate parameters affecting ignition of dust dispersions. The dust dispersions were ignited in a Godbert-Greenwald furnace at atmospheric pressure. Ignition temperature and the concentrations of fuel, admixed inert powder, and atmospheric oxygen were related mathematically. Values for these parameters obtained in laboratory experiments for cornstarch agreed with theory. The developed equation permits extrapolation; the predicted upper igni-tion limits correspond with limited experimental data from laboratory and large-scale tests. Explanation of the effect of fineness of dust on ignition parameters is attempted by introducing a surface-area constant to modify the activation energy. Arguments are presented to show that the ignition process is a solid-gas phase reaction rather than an ignition of prevolatilized gases.

Jan 1, 1966

By J. H. Elledge

Hydraulic Transportation of Phosphate Ore from, a 40,000 Cubic Yard per Day Strip Mine IMC is transporting 1500 yards per hour of phosphate ore in a water slurry a distance of approximately five miles from a strip mine to a flotation beneficiation plant at their Noralyn Operation. in Barrow, Florida. This ore, which consists of approximately 1/4 phosphate, 1/2 silica sand, and 1/4 clay slimes, is being pumped through a 20 inch O. D. pipeline using seven 20 and 18 inch GIW metal pumps direct connected to electric, motors. This paper details some of the problems involved and the specific methods used to accomplish this bulk material handling requirement.

Jan 1, 1966

By Constantine C. Popoff

This report reviews and analyzes, by a simple analytical and logical reasoning, the conventional methods of reserve computations of mineral deposits described in various domestic and foreign publications. It brings together, formulates, and evaluates the principles underlying interpretation of exploration data; and ties such principles to the proposed classification of methods. The material is discussed in sufficient detail to allow general application.

Jan 1, 1966

By W. G. Bearden, G. C. Howard, J. W. Spurlock

An investigation of the factors af-fec.ting the inter-zonal flow of fluids in the casing-wellbore annrc1rt.s of an oil or gas ivell is presented Laborntory tests revealed that failure of the caring-cement bond allows communi-cation of fluid at pressure differentials near 1.000 psi. Perforating with a 11011011: carrier gun does not shatter or crack the cement sufficiently to allow communication through these cracks and does not seriously affect the casing-cement bond failure pressure. The pressure to cause communication at the casing-cement bond can he increared to 3,000 psi by. limiting pipe deformation during cementing and subsequent operations. Communication can be prevented, however. up to pressures sufficient to cause the cement to fail or the casing to col-lapse, by attaching to the casing a seal ring of deformable ruhber molded between two steel flanges. When installed, one flange is attached rigidlv to the casing to serve as back-up for the gasket While tile other flange is movable. To date, these gasket seal rings have been field-tested in 27 Wells. Althotrgh communication has been noted in two wells, inter-zonal flow has been prevented in other wells in the same area by installing more seal rings between the communicaring zones. INTRODUCTION The inter-zonal flow of fluids behind casing cemented in oil wells during normal production or stimulation operations is a major operating problem. If it cccurs during production operations. it can seriously limit the pressure to which a reservoir may be depleted without harmful invasion of unwanted fluids. If it occurs during stimulation operations, it may preclude the possibility of stimulating the desired zone. This communication can be caused by failure of the bond between the casing and cement, failure of the bond between the cement and formation, or failure of the cement itself. This paper presents the results of an investigation of factors affecting com-munication at the casing-cement bond and methods which aid in preventing it. LABORATORY INVESTIGATIONS The laboratory tests performed in this study were divided into three phases. The first phase consisted of tests to determine if perforating would shatter and crack the cement sheath so severely that communication would occur through the cement itself. The second phase consisted of tests to determine more precisely the cause for the casing-cement bond failure. The third phase consisted of tests to evaluate the effectiveness of various de-formable seals attached to the casing in preventing communication. EFFECT OF PERFORATING, The effect of perforating was invest~gated in tests performed with apparatus shown on Fig. 1. Cement was poured into the annulur space hetween 5%-in. casing and 8%-in. casing and allowed to cure for 72 hours. The apparatus was then perforated with a hollow carrier gun containing eight duPont 26-A shaped charges. Bull plugs were placed over the perforations in the 8 5/8-in. casing and hydraulic pressure was applied inside the 5 1/2i-in. casing. The pressure to cause fluid communication past the cement sheath was observed and termed the "bond failure pressure". Several different cement compositions were included in these tests, the results of which are shown in Table 1. In Tests 1 through 4 of Table 1, bond failure occurred at- the inter- .

Jan 1, 1966

By J. C. Ingles

"A new technique is in the process of revolutionizing inorganic chemical analysis. Galled atomic absorption spectrophotometry, it combines the use of a special light source, a flame, and the equipment of conventional spectrophotometry, to provide a quick, reasonably accurate method for the determination of a large number of elements.This paper outlines the principles on which it is based, describes the commercial instrumentation"" available for exploiting it, and. summarizes current applications in process metallurgy."

Jan 1, 1966

By John M. Gomes

Two molten salt systems were evaluated as electrolytes for the repetitive recovery of tungsten from tungsten oxide (W03) made by calcining commercial-grade ammonium paratungstate. Using a sodium chloride-sodium fluoride-potassium aluminum tetrafluoride electrolyte at 800° C, 1 pound of 99.8 percent tungsten was recovered for each 2.7 kilowatt-hours of energy consumed. The metal contained 1,100 ppm carbon, was in dendritic masses of spherical grains, and had an apparent bulk density of 5.41 g/cm3. T ngsten of 99.9 percent purity was won from a sodium pyrophosphate-sodium tetraborate-sodium chloride electrolyte at 1,000° C; 6.0 kilowatt-hours of energy was consumed for each pound of metal recovered. The metal contained 120 ppm carbon, was in dendritic masses of hexagonal acicular crystals, and had an apparent bulk density of 7.25 g/cm . Each metallic impurity--aluminum, calcium, copper, iron, nickel, and silicon--in the two tungsten products was 16 ppm or less.

Jan 1, 1966

By Frank B. Fulkerson

A study was made of scrap iron and steel in the South Central States in order to determine trends in processing, shipment, and consumption if this important commodity. These data were derived in part from statistical sources and in part by visits to scrap yards and steel mills. Trends in the industry were reviewed. Dealers in 1963 supplied 1.8 million tons of iron and steel scrap to steel mills and foundries in the south-central area, compared with 2.1 mill ion tons in 1955. Most of the scrap was processed and shipped within 200 to 300 miles of consuming centers. Exports provide a principal outlet for dealers along the gulf coast. Most of the scrap that fills these orders is loaded onto freight cars at yards in Texas and Louisiana and is shipped to ports for direct transfer from railroad car to ship. The tonnage exported varies greatly from year to year. The largest scrap operations are in or near large cities which are heavy scrap generating areas, steel mill sites, or port cities for export of scrap. A tentative analysis indicates that the short-run supply of prepared scrap is inelastic to price changes; therefore, buyers probably are in a strong bargaining position at times of declining demand. One technological development in the iron and steel scrap industry is the use of large presses which can take complete automobiles with frames, wheels, springs, and other heavy parts still intact and reduce them to bundles. At Houston, Tex., and Kansas City, Mo., shredding plants are in operation that reduce car bodies and other light scrap into flat pieces 4 to 6 inches in size.

Jan 1, 1966

Jan 1, 1966

Essential features of the role of the fill material in mechanized cut and fill mining are discussed, with particular emphasis on its dewatering and strength development after emplacement. The fill material is regarded as a chemically-reactive porous medium, the most important property of which is permeability. Methods are described for measurement of permeability and other fill properties and results of such measurements applied to develop an orderly approach to the operation.

Jan 1, 1966

By J. M. Singer

Quenching distances for flames of methane-coal dust mixtures were determined with air and oxygen-enriched air. Coals used were Pittsburgh, Sewell, and Pocahontas No.3. Quenching distances were greater for flames of hybrid mixtures of coal dust and methane than for methane flames of corresponding stoichiometry. From the data of quenching distances and methane-coal dust concentrations was calculated the quenching equivalence, which is the increase in coal dust concentration required to maintain a given quenching distance value as the methane concentration decreases. These equivalences could be useful in identifying hazardous methane-coal dust mixtures in mines.

Jan 1, 1966

By Edward E. Johnson

The U.S. economy boomed in 1965, completing its fifth consecutive year of expansion. Although the advance was somewhat irregular, previous records for production, sales, employment, and income were topped. During the first few months of 1965, as the economy recovered from the depressing effects of the automobile strikes of late 1964, increases were unusually large. The gains moderated in early spring, but were stimulated at midyear by sharply rising capital outlays, excise tax cuts, in? creased Social Security payments, and accelerated Viet-Nam defense expenditures. Gross national product (GNP) in cur-rent dollars rose $49.5 billion or 7.8 percent, to a total of S681.2 billion. In constant dollars (effects of price changes eliminated), GNP increased 5.9 percent, a rate considerably higher than the historical postwar annual average growth of 3.5 per-cent. Demand increased in most final markets and was especially strong for business fixed investment and consumption expenditures. With the exception of construction, most of the increases in GNP were real, since prices increased less than 2 percent.

Jan 1, 1966

By Richard F. Link

A statistical technique, useful to analyze assay and other data characterized by location in three dimensions, is described in this Bureau of Mines report. If present, trends in the data are defined for the purposes of improving ore estimation, predicting ore beyond existing workings, and aiding geological interpretation. The technique is to fit linear and quadratic polynomial equations to the data through the statistical method of regression analysis. The fitted linear equations have the geometric form of hyperplanes; the fitted quadratic equations have the geometric form of ellipsoids or elliptic hyperboloids of one or two sheets. To visualize these three-dimensional forms, contour maps of a series of plane sections through the fitted surfaces are plotted. Both the fitting of the polynomial equations and the plotting of the con-tour maps are done by electronic computer to facilitate calculations and to obtain accurate results. Computer programs are described in appendixes. Methods employed are illustrated by an example analysis) based on data from a part of the Fresnillo mine) Zacatecas, Mexico.

Jan 1, 1966

By N. R. Morrow, C. C. Harris

The experimental points which describe capillary pressure curves are determined at apparent equilibria which are observed after bydrodynamic flow has ceased. For most systems, the time required to obtain equalization of pressure throughout the discontinuous part of a phase is prohibitive. To permit experimental points to be described as equilibria, a model of capillary behavior is proposed where mass transfer is restricted to bulk fluid flow. Model capillary pressure curves follow if the path described by such points is independent of the rate at which the saturation was changed to attain a capillary pressure point. Aemodified suction potential technique is used to study cyclic relationships between capillary pressure and moisture content for a porous mass. The time taken to complete an experiment was greatly reduced by using small samples. INTRODUCTION Capillary retention of liquid by porous materials has been investigated in the fields of hydrology,l soil science,2 oil reservoir engineering,3 chemical engineering," soil mechanics,5 textiles: paper making: and building materials In studies of the immiscible displacement of one fluid by another within a porous bed, drainage columnsl and suction potential techniques2 have been used to obtain relationships between pressure deficiency and saturation (Fig. 1). Except where there is no hysteresis of contact angle and the solid is of simple geometry, such as a tube of uniform cross section, there is hysteresis in the relationship between capillary pressure and saturation.2 The relationship which has received most attention is displacement of fluid from an initially saturated bed (Fig. 1, Curve R2), the final condition being an irreducible minimum fluid saturation Swr. Imbibition (Fig. 1, Curve A), further desaturation (Fig. 1, Curve R), and intermediate scanning curves have been studied to a lesser but increasing extent.2 ,3,9-12 This paper first considers the nature of the experimental points tracing the capillary pressure curves with respect to the modes and rates of mass transfer which are operative during the course of measurement. There are clear indications that the experimental points which describe these curves are obtained at apparent equilibria which are observed when viscous fluid flow has ceased; and any further changes in the fluid distribution are the result of much slower mass transfer processes, such as diffusion. Unless stated otherwise, this discussion applies to a stable packing of equal, smooth, hydrophilic spheres supported by a suction plate5 with water as the wetting phase and air as the nonwetting phase. The discussion can also be applied, in many

Jan 1, 1966