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By Alton B. Cook

A material balance equation was derived for calculating (1) the initial oil volume and (2) the relationship of average reservoir pressure to net gas in storage in reservoirs used for natural gas storage operations. The equation is also applicable to secondary-recovery operations where reservoirs are completely repressured and gas cycled. Using this equation minimized two probable sources of appreciable error in conventional material balance calculations: inaccurate measuring of and accounting for produced gas, and differences between true reservoir pressure and average reservoir pressures as derived from bottom-hole pressure measurements. A new procedure is presented for calculating water encroachment. By solving the conventional material balance equation and the derived equation for gas storage simultaneously, the values for initial oil in place and net water encroachment can both be determined.

Jan 1, 1966

By J. W. Stevenson

The Bureau of Mines investigated the influence that atmospheric pressure changes exert in a gassy coal mil on a ventilating air current with a system of bleeder entries. During the season when abnormal barometric fluctuations usually occur, recording instruments monitored the air current ventilating an active coal-producing area. It HL he rate of coal production caused a more significant change in methane concentration than did barometric change. The hazard that accompanies methane release due to expansion of the gob gases during atmospheric lows was minimized by the effective bleeder system.

Jan 1, 1966

By Ramon B. Santos

The Atlas Concentrator, reputedly the largest in the Far East today, is located on the island of Cebu in the Republic of the Philippines. It started operation on a 4000 TPD capacity in 1955. An expansion program, coupled with significant improvements both in the Crushing Plant and the Mil, made the Atlas Concentrator what it is today, treating about 14,000 tons of ore per day at a comparatively low cost of about $0.50 per ton treated. The Atlas Copper Mine is at present mainly an open pit operation, with ore supplied from two pits (Lutopan and Biga) north of the Concen¬trator. Development of an Underground Mine, situated on the main ore body at Lutopan, which will be a block caving operation, has been underway since 1963, and this underground mining operation is expected to b e in full production by the latter part of 1966.

Jan 1, 1966

By E. H. Dudgeon

In order to make increased use of automation in copper smelting, it is evident that a useful first step .world be the accurate determination of the copper end point in the converter operation. After laboratory tests, the copper end points in a copper converter at Gaspe Copper Mmes Ltd. were determined without reference to melt samples or other observations. The results indicated that the rapid measurement of the S02 level in the gas released from the converter has potential as a new and independent method of determining the copper end point in converter operation.

Jan 1, 1966

By M. M. Fine

This Bureau of Mines report describes the theory, experimental procedures, and the results obtained to date in the development of the Bureau's process for magnetically roasting iron ores using scrap iron as a means of reduction. Since magnetic separation is an operational step common to magnetic taconite plants, the preliminary research studies emphasized only the novel magnetic roasting step. The studies included the use of automobile scrap, ferrous reductants such as borings and turnings, and prereduced pellets. Technical feasibility of the process was demonstrated both on a bench- and pilot-scale. Quality magnetic concentrates with recoveries of over 90 percent were obtained from a direct shipping ore containing 59.5 percent Fe and from fine grained semitaconites with about 30 percent Fe.

Jan 1, 1966

By F. W. Jessen, C. C. Patton

Adsorbed films were formed on polished stainless steel specimens from dilute benzene solutions of two crude oil distillation residua. Although the two residua were extremely dissimilar in composition, contact angle measurements showed that the two films increased the wettability of the steel specimens to oil by equal amounts. Furthermore, the wettability of the films was essentially unaffected by the desorption techniques used. Paraffin deposits were formed from heptane-wax solutions on the same stainless steel specimens. These deposits definitely adhered to the surface. Presence of an adsorbed crude oil film on the metal surface increased its free surface energy and resulted in increased deposition of paraffin. The addition to the heptane - wax solution of small amounts of the same distillation residua that were used to form the adsorbed films resulted in decreased cohesive strength in the deposits formed, which resulted in decreased deposition. The presence of a crude oil fraction both in the solution and as a preadsorbed film eliminated the adherence of a deposit of any kind. A mechanism of deposition is proposed which explains the results obtained. INTRODUCTION The natural formation of any predominantly organic accumulation in oilwell tubing, surface flow lines or other production and storage facilities is called a paraffin deposit. These deposits restrict the production of crude oil, causing a substantial increase in production costs because of decreased flow capacity, expense for periodic deposit removal and unproductive downtime. The conditions under which such deposits form, their physical characteristics and the nature and severity of the problem created are extremely varied. Over the past several years, much progress has been made in developing and utilizing methods to remove accumulated paraffin deposition. However, like so many other problems, the basic stumbling block appears to be a lack of understanding of the fundamental mechanism involved in the formation of such deposits. Crude petroleum is known to contain considerable quantities of polar, surface active substances which Doddl has shown to be present at the oil-water interface. Denekas, Mattax and Davis2 observed that the wettability of reservoir rocks was drastically altered by exposure to crude oil fractions; and Zisman, et a1.3 showed that the nature of the compounds adsorbed on a surface would determine its wettability characteristics. Cole and Jessen4 and Ehrig5showed that surface wettability can have a profound effect on the magnitude of paraffin deposition, and Parks6 demonstrated chat the presence of certain adsorbed films on a metal surface would reduce the adherence of paraffin to that surface. Zisman7 has since advanced the theory that the conditions for adhesion are the same as for wetting. Therefore, it was felt that there was adequate evidence to support the supposition that adsorption of compounds from a crude oil might play an important part in paraffin deposition. ADSORPTION-WETTABILITY EXPERIMENTS Initial experiments were conducted to determine the effects of adsorption from solution of crude oil residua on the wettability of a polished stainless steel surface. Distillation residua with initial atmospheric boiling points of 700F were used in preference to the whole crudes in order to concentrate on the molecular weight range of interest, and to eliminate the possibility of composition change due to evaporation of the light ends. Also, these high boiling materials would be expected to be adsorbed from the whole oil in preference to similar compounds of lower molecular weight.

Jan 1, 1966

By J. A. Cavallaro

To determine whether magnetite consumption could be reduced and salable coal production increased by using froth flotation units in series with magnetic separators, the Bureau of Mines conducted laboratory froth flotation tests on primary magnetic separator effluents obtained from three coal preparation plants. Tests were performed in a standard 500-gram-capacity laboratory batch flotation cell. Oleic acid and methylisobutyl carbinol were used as the collector and frother, respectively. Magnetite recovery was comparable to that expected from secondary magnetic separation, and salable float coal recoveries of 0,8 to 7.6 tons per hour were obtainable. The economics of the proposed technique appear to be sound.

Jan 1, 1966

By C. I. Pierce

The Bureau of Mines used an electrolytic tank model to investigate the response of guard electrodes of different dimensions under different simulated reservoir conditions. Sandstone disks from the Berea and Connellsville Formations were used as resistive beds in the model, and agar gel or water was used as conductive beds. In the experiments, bed thickness, hole diameter, mud resistivity, and bed resistivity were varied. The guard electrode is an excellent tool for determining true bed resistivity in the thin-bedded oil reservoirs of the Appalachian area. Vertical resolution and resistivity values are good when there is little or no invasion. Resistivity values are near true bed resistivity in beds thicker than about six hole diameters when the electrode-to-hole-diameter ratio is close to 1. However, low-resistivity muds cause false peaks to appear on the logs near bed boundaries in thick beds, and for resistive beds having a thickness approximately three to five times the hole diameter, apparent resistivities tend to be excessively high when mud resistivity is low.

Jan 1, 1966

By R. W. Heins, N. Street

An investigation was made of the Rehbinder-Kuznetsov pendulum as an instrument to aid in the study of rock drillability and of the effect of surface active agents on rock drillability. The "critical weight", i.e., the pendulum weight at greatest sensitivity, was determined for several solids and it was shown that a change in surface environment changed the maximum value of the apparent hardness but not the critical weight, and the critical weight increased with increase of hardness of the solid used. Using silver halides as the solid material, and solutions of either silver nitrate or the appropriate alkali halide, it was shown that there is a hardness maximum at the zero point of charge of the particular silver halide. INTRODUCTION The development of relative hardness measurement by the method of damped oscillations, or what has been called the pendulum sclerometer, is due largely to the Russian workers P. A. Rehbinder and V. D. Kuznetsov and their co-workers.1,2 The apparent simplicity of the method has led to its use in a number of fields, particularly those where relative hardness has to be determined on a brittle solid. As will be shown, the simplicity of the method belies its complexities. THEORY OF THE PENDULUM SCLEROMETER The operation of the pendulum is quite simple. Make a sharp point such as a diamond, hardened steel or tungsten carbide, as the fulcrum of a pendulum, with the center of gravity of the system below the point of support. The attenuation of this pendulum is a function only of air friction, provided no fragmentation, breakage or other work is performed by the point. However, when the solid surface breaks or disintegrates under the point, and the latter penetrates the solid, part of the energy of oscillation is absorbed in the work of creating new surface, and the rate of attenuation increases. In the case of brittle solids, the point of the pendulum produces fragmentary particles, whereas the point produces plastic deformation in a plastic solid; but in both cases damping occurs. This pendulum damping is a function of the hardness or strength of the solid. Whereas a pendulum oscillating on a hard material attenuates primarily by air friction, in the case of a soft material, the points penetrate the surface of the solid, producing new surface, and the pendulum damps much faster. Thus the attenuation rate is a function of the hardness or strength of a material in both plastic and brittle substances. Russian workers initially used a single support for the pendulum, but this created many problems because of oscillation of the pendulum in more than one plane. A revised version used two points, or sometimes a prism as support, successfully confining oscillation to one plane. The version using two points was constructed and used throughout this investigation, making the recording of the attenuation as a function of time relatively easy. That both points should be in contact with the solid during the damping is implied. Rehbinder (c.f. Kuznetsov2) proposed that the hardness H as measured by this method could be expressed by a quantity which is inversely proportional to the relative initial rate of attenuation of amplitude. where H = hardness parameter (arbitrary units) a, = initial amplitude da/dt = rate of attenuation of amplitude with time. In the simplest case of damping with a constant logarithmic decrement, H can be regarded as a constant for the duration of the whole damped oscillation process. That is

Jan 1, 1966

By T. S. Chen

A study was made by the Bureau of Mines of the temperature and thermal stress distributions in thin circular disks subjected to peripheral thermal shock at various rates of heat transfer. The theoretical analysis is based on one-dimensional radial heat flow by conduction in the disk, and on heat exchange by convection between the disk and its surroundings. Preliminary experimental data obtained from shock tests on thin circular disks of basalt, quartzite, and taconite show reasonably good agreement with theory. The case of constant properties and plane stress is treated. Solutions of the stress distribution are presented for both cooling and heating shocks. The elastic energy stored at fracture is examined, and on this basis an average stress theory is formulated. Physical properties vital to the studies include thermal conductivity, thermal diffusivity, tensile strength, Young's modulus, and linear coefficient of thermal expansion. This work is of importance in predicting the thermal shock responses of a rock body of finite size.

Jan 1, 1966

By Paul M. Buttermore

As part of a national canvass of water use the Bureau of Mines compiled data on water requirements in the petroleum and natural gas industries for the calendar year 1962, specifically in well drilling, secondary-recovery operations, and natural gas processing plants. Total new water use in the petroleum industry of the United States, excluding refining, was 5.3 billion barrels. Secondary-recovery operations and natural gas processing plants required about 2.5 billion barrels of new water input; each of these requirements was about eight times greater than that for well drilling. Total use, including recirculated water, was 45.3 billion barrels of which 3.4 billion barrels was consumed. The greatest use of recirculated water was for natural gas processing, amounting to 38.2 billion barrels. Projections of total water use show that by 1975, 75.4 billion barrels will be used by the petroleum industry, of which 10.2 billion barrels will be new water. By 1985, the total use requirement will be 92.8 billion barrels, of which 13.1 billion barrels will be new water.

Jan 1, 1966

By D. C. Treilhard

After a brief history of the mining and smelting operations of Kilembe Mines Limited, this paper outlines the smelter layout and describes . the. daily operations at the Jinja plant. Particular attention 1s paid to the details of the furnace and converter operation. A subsequent section of the paper deals with the significant developments in plant metallurgical practice, covering both smelting and converting.

Jan 1, 1966

By d&apos, Kathleen J. Amico

This summary appears in Minerals Year-book volumes I and III, which cover mineral production in the United States, its island possessions, the Canal Zone, and the Commonwealth of Puerto Rico, as well as the principal minerals imported into and exported from the United States. The several commodity and area chapters contain further details on production. A summary table comparing world and U.S. mineral production also is included. Mineral production may be measured at any of several stages of extraction and processing. The stage of measurement used in the chapter is normally what is termed "mine output." It usually refers to minerals in the form in which they are first extracted from the ground, but customarily includes for some minerals the product of auxiliary processing operations at or near mines.

Jan 1, 1966

By A. W. Deurbrouck

This report describes the preparation characteristics of the significant coalbeds from which samples could be obtained in Webster County, W. Va. In 1964, approximately 825,000 tons of coal was produced in the county, of which 732,000 tons was mechanically cleaned in three preparation plants. The Sewell coal bed accounted for 94 percent of the coal produced. Twelve samples were collected from five coalbeds. Four of the samples would require upgrading to meet metallurgical requirements; two others of just over 8.0 percent ash would require some upgrading. In general the coalbed samples collected in the county were of medium-sulfur and medium-to low-ash content as received or after removal of the sink 1.58-specific-gravity material.

Jan 1, 1966

Rb-Sr measurements on total-rock samples of granitic rocks from the Mount Isa region have confirmed the existence of two periods of granite-forming activity. The Kalkadoon Granite, together with the Ewen Granite and possibly an older phase of the Sybella Granite, has been shown to belong to the earlier age-group at 1760 m.y.; the Wimberu Granite and a pegmatite associated with the Sybella Granite have been dated at 1540 m.y. The initial Sr ratio suggests that the Wimberu Granite may be new material of deep-seated origin.Further Rb-Sr measurements have confirmed previously-reported K-Ar results upon biotites from these rocks, whilst showing that, in this metamorphic terrain, biotites have lost varying amounts of radiogenic Sr and Ar, and therefore yield ages which are younger than the true age of the second event.

Jan 1, 1966

By Robert F. Shurtz

This paper discusses and compares methods of statistical analysis of the information relating to the evaluation of an asbestos deposit. From a study of 10-ft. lengths of drill core, the separate effects of visual evaluation errors were determined, as well as the deviations between evaluators and the deviations produced by a slight displacement in the center lines of the check drill holes. The importance of careful statistical analysis of such information is stressed.

Jan 1, 1966

By J. P. Hansen

Reducibility tests were run by the Bureau of Mines on an open hearth lump ore and four groups of pellets whose smelting characteristics had been deter-mined previously in the Bureau's experimental blast furnace. When reduction data from various tests were plotted on specially prepared paper l-(l-percent reduction/100)1/3 against time, the plots were linear. The iron-wustite inter-face therefore advances at a constant rate. The rate of the interface advance in mm/min was used as a reducibility index. The reducibility index measured at 900° C, using 0.45 cu ft hydrogen per minute varied inversely with the surface area of the sample. Even with carefully controlled surface areas, how-ever, duplicate reducibility indices varied considerably. When enough tests were run to give a stable mean, the mean reducibility index did correlate with blast furnace production for the four pellet groups. Results indicated that if the interface speed itself were to be used for correlation with blast furnace production, a sample size of about 180 grams of minus 0.742-plus 0.525-inch particles should be used with a test temperature of 900° C and a flow of 0.45 cu ft hydrogen per minute.

Jan 1, 1966

By W. W. Weller

Heat capacities of ferrous molybdate (FeMoO4) and ferrous tungstate (FeWO4) were measured over the temperature range 51° to 298.15° K. Ferrous tungstate has a lambda type heat capacity anomaly at 74° K. The 298.15° K entropies are FeMoO4) 30.9 cal/deg mole and FeW04) 31.5 cal/deg mole.

Jan 1, 1966

By R. E. Coleman

The molecular species occurring at the mineral-reagent interface of the galena-aqueous potassium ethyl xanthate system was studied by developing a technique for using an attenuated reflection method in conjunction with standard infrared spectroscopy procedures. Lead ethyl xanthate was detected from the infrared spectra of all galena surfaces treated in the pH range of 7 to 11. At pH 8.5, lead ethyl xanthate formed as a film chemically bonded to the galena surface. A solvent extraction sampling method was employed with infrared spectroscopy to obtain quantitative data on the lead ethyl xanthate removed from the galena surface. The data showed that between pH 7 and 11 thy quantity of lead ethyl xanthate physically adsorbed decreased as the pH was decreased; in the same pH range, the quantity of free lad ethyl xanthate in the aqueous medium remained constant, and the amount of unreacted xanthate varied.

Jan 1, 1966

By C. L. Klingman

The Bureau of Mines tested eight commercially available, activated charcoals experimentally to compare the following characteristics: capacity for adsorption of nitrogen at 77° K and 170 atmospheres' pressure, surface area, carbon tetrachloride adsorption capacity, hardness, and density. The nitrogen adsorption test was devised to simulate plant conditions occurring in the final step of purification in Bureau helium faciliti.es. The remaining tests were patterned after empirical acceptance tests that are widely used throughout the adsorbent industry. Surface area and carbon tetrachloride adsorption correlated well with nitrogen adsorption. The samples with low density generally had better adsorption qualities than those of higher density. The carbon tetrachloride test appeared to be the most practical for selecting a charcoal to be purchased, but an attrition, or hardness test should also be run to be sure the charcoal will not crumble in use.

Jan 1, 1966