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By Howard I. Smith

The mineral trona was discovered on Government land in 1938, about 18 miles west of the town of Green River, Wyo., in the core of the John Hay, Jr., well, a test well drilled for oil by the Mountain Fuel Supply Co. in sec. 2, T. 18 N., R. IIO W., sixth principal meridian. Although no oil or gas was reported, the drilling led to a discovery of great potential economic importance and exceptional scientific interest. Trona is a relatively rare mineral found at various places in playa deposits but not previously found at any great depth. It is composed of hydrous sodium carbonate and sodium bicarbonate (Na2CO3 NaHCo3.2H2O). Pure trona con-tains the equivalent of 70.35 per cent of sodium carbonate. Total sodium computed to carbonate times 1.42 equals the percentage of trona in the absence of other sodium carbonate minerals in the sample. Analyses Two short pieces of core sent to the author a few days after the completion of the Hay well were analyzed by R. C. Wells† and found to be exceptionally Pure trona. A brief article on this discovery has already been published.1 Arrangements were then made through W. T. Nighten-gale‡ for the author to inspect and sample the core. The company log of the well included notations of sodium salt crystals from a depth of 1190 to 1820 ft. Not being able to identify all the minerals present, the author selected several specimens of the core for petrographic examinations and sampled the sections of trona for analysis. J. J. Fahey, of the Geological Survey, examined the specimens and reported most of the crystals to be a new anhydrous sodium carbonate and calcium carbonate mineral (Na2CO 3.2 CaCO3), which he named shortite,² after Maxwell N. Short." He analyzed the samples of trona, with the results shown in Table I. In addition to the 10 ft. 1 in. of trona in the first section, it is reasonable to assume that the 9 ft. 8 in. for which no core was available for sampling is either i mostly trona or some other soluble salt, but it should not be included in calculating | reserves. In the part of the core between i 1590 ft. 3 in. and 1600 ft. 4 in. the material insoluble in cold water, amounting to about 5 per cent, was estimated petrographically I to contain 70 per cent clay, 25 per cent shortite, and 5 per cent pyrite. Accompanying Minerals Fahey later secured about 600 ft, of the core for a detailed examination and study

Jan 1, 1942

By Howard I. Smith

The mineral trona was discovered on Government land in 1938, about 18 miles west of the town of Green River, Wyo., in the core of the John Hay, Jr., well, a test well drilled for oil by the Mountain Fuel Supply Co. in sec. 2, T. 18 N., R. IIO W., sixth principal meridian. Although no oil or gas was reported, the drilling led to a discovery of great potential economic importance and exceptional scientific interest. Trona is a relatively rare mineral found at various places in playa deposits but not previously found at any great depth. It is composed of hydrous sodium carbonate and sodium bicarbonate (Na2CO3 NaHCo3.2H2O). Pure trona con-tains the equivalent of 70.35 per cent of sodium carbonate. Total sodium computed to carbonate times 1.42 equals the percentage of trona in the absence of other sodium carbonate minerals in the sample. Analyses Two short pieces of core sent to the author a few days after the completion of the Hay well were analyzed by R. C. Wells† and found to be exceptionally Pure trona. A brief article on this discovery has already been published.1 Arrangements were then made through W. T. Nighten-gale‡ for the author to inspect and sample the core. The company log of the well included notations of sodium salt crystals from a depth of 1190 to 1820 ft. Not being able to identify all the minerals present, the author selected several specimens of the core for petrographic examinations and sampled the sections of trona for analysis. J. J. Fahey, of the Geological Survey, examined the specimens and reported most of the crystals to be a new anhydrous sodium carbonate and calcium carbonate mineral (Na2CO 3.2 CaCO3), which he named shortite,² after Maxwell N. Short." He analyzed the samples of trona, with the results shown in Table I. In addition to the 10 ft. 1 in. of trona in the first section, it is reasonable to assume that the 9 ft. 8 in. for which no core was available for sampling is either i mostly trona or some other soluble salt, but it should not be included in calculating | reserves. In the part of the core between i 1590 ft. 3 in. and 1600 ft. 4 in. the material insoluble in cold water, amounting to about 5 per cent, was estimated petrographically I to contain 70 per cent clay, 25 per cent shortite, and 5 per cent pyrite. Accompanying Minerals Fahey later secured about 600 ft, of the core for a detailed examination and study

Jan 1, 1942

By Howard I. Smith

THE mineral trona was discovered on Government land in 1938, about 18 miles west of the town of Green River, Wyo., in the core of the John Hay, Jr., well, a test well drilled for oil by the Mountain Fuel Supply Co. in sec. 2, T. 18 N., R. 11o W., sixth principal meridian. Although no oil or gas was reported, the drilling led to a discovery of great potential economic importance and exceptional scientific interest. Trona is a relatively rare mineral found at various places in playa deposits but not previously found at any great depth. It is composed of hydrous sodium carbonate and sodium bicarbonate (Na2CO3.NaHCO3.2H2O). Pure trona contains the equivalent of 70.35 per cent of sodium carbonate. Total sodium computed to carbonate times 1.42 equals the percentage of trona in the absence of other sodium carbonate minerals in the sample. ANALYSES Two short pieces of core sent to the author a few days after the completion of the Hay well were analyzed by R. C. Wells† and found to be exceptionally pure trona. A brief article on this discovery has already been published.1 Arrangements were then made through W. T. Nightengale‡ for the author to inspect and sample the core. The company log of the well included notations of sodium salt crystals from a depth of 1190 to 1820 ft. Not being able to identify all the minerals present, the author selected several specimens of the core for petrographic examinations and sampled the sections of trona for analysis. J. J. Fahey, of the Geological Survey, examined the specimens and reported most of the crystals to be a new anhydrous sodium carbonate and calcium carbonate mineral (Na2CO3.2CaCO3), which he named shortite,2 after Maxwell N. Short.* He analyzed the samples of trona, with the results shown in Table i. [ ] In addition to the 10 ft. I in. of trona in the first section, it is reasonable to assume that the 9 ft. 8 in. for which no core was available for sampling is either mostly trona or some other soluble salt, but it should not be included in calculating reserves. In the part of the core between 1590 ft. 3 in. and 1600 ft. 4 in. the material insoluble in cold water, amounting to about 5 per cent, was estimated petrographically to contain 70 per cent clay, 25 per cent shortite, and 5 per cent pyrite. ACCOMPANYING MINERALS Fahey later secured about 600 ft. of the core for a detailed examination and study

Jan 1, 1942

By Howard I. Smith

THE mineral trona was discovered on Government land in 1938, about 18 miles west of the town of Green River, Wyo., in the core of the John Hay, Jr., well, a test well drilled for oil by the Mountain Fuel Supply Co. in sec. 2, T. 18 N., R. 110 W., sixth principal meridian. Although no oil or gas was reported, the drilling led to a discovery of great potential economic importance and exceptional scientific interest. Trona is a relatively rare mineral found at various places in playa deposits but not previously found at any great depth. It is composed of hydrous sodium carbonate and sodium bicarbonate (Na2CO3.NaHCO3.2H20). Pure trona contains the equivalent of 70.35 per cent of sodium carbonate. Total sodium computed to carbonate times 1.42 equals the percentage of trona in the absence of other sodium carbonate minerals in the sample. ANALYSES Two short pieces of core sent to the author a few days after the completion of the Hay well were analyzed by R. C. Wells[t] and found to be exceptionally pure trona. A brief article on this discovery has already been published.1 Arrangements were then made through W. T. Nightengale[$] for the author to inspect and sample the core. The company log of the well included notations of sodium salt crystals from a depth of 1190 to 1820 ft. Not being able to identify all the minerals present, the author selected several specimens of the core for petrographic examinations and sampled the sections of trona for analysis. J. J. Fahey, of the Geological Survey, examined the specimens and reported most of the crystals to be a new anhydrous sodium carbonate and calcium carbonate mineral (Na2CO3.2CaCO3), which he named shortite,2 after Maxwell N. Short.* He analyzed the samples of trona, with the results shown in Table I. [ ] In addition to the 10 ft. I in. of trona in the first section, it is reasonable to assume that the 9 ft. 8 in. for which no core was available for sampling is either mostly trona or some other soluble salt, but it should not be included in calculating reserves. In the part of the core between 1590 ft. 3 in. and I600 ft. 4 in. the material insoluble in cold water, amounting to about 5 per cent, was estimated petrographically to contain 70 per cent clay, 25 per cent shortite, and 5 per cent pyrite. ACCOMPANYING MINERALS Fahey later secured about 600 ft. of the core for a detailed examination and study

Jan 1, 1942

By Emby Kaye

IT is the purpose of this paper to outline briefly some of the considerations that enter into the economics of so-called recycling, the generic designation of the relatively recently developed process by which a condensate† is separated from gas-distillate gas at high pressure and the residual gas returned to the reservoir. This subject necessarily embraces not only a discussion of factors that should be considered in projecting a recycling operation, such as estimating reserves, investment and operating costs, but also a comparison of condensate with other types of petroleum. The place of condensate in its relation to the total supply of crude oil is pointed out as well as certain logical methods of product disposal. The cost of drilling wells and lease maintenance is not pertinent to this discussion because income and revenue are in this paper confined to that retained by the plant or plant operator for supplying processing facilities for the gas. Before the development of recycling a great many gas-distillate gas fields in Louisiana and. Texas provided no income to their owners. When gas was sold from these reservoirs it was accompanied by irretrievable losses of condensate in the formation. The understanding of the function of retrograde condensation resulted in the introduction of a new commercial petroleum recovery process for these hitherto unexploited fields and now permits the conditioning of this type of wet gas field for the sale of dry gas therefrom without waste. SOME ECONOMIC FACTORS The study of a gas-distillate field for possible exploitation necessarily involves the critical appraisal of a number of elements, chief of which will be discussed here: (I) estimate of distillate in place, (2) estimate of distillate that can be brought to the surface, (3) available market, (4) costs. The considerations affecting the estimating of distillate reserves. in place are in the main subject to the same errors as are involved in determining dry gas reserves. Determinable data including acreage, sand thickness, reservoir pressure, reservoir temperature, porosity and connate water provide the basis for calculating the volume of gas in place. Ample allowance must be made for connate water, which may occupy from 20 to 35 per cent of the pore space of the sand. The factor of supercompressibility is to a considerable extent nullified by the reservoir temperature. It has been considered well advised to allow this factor to serve as a cushion. With the gas reserves calculated, it remains only to assay the distillate content of the gas. Those familiar with the handling of "wet" gas at high pressure readily appreciate the variables in sampling gas from

Jan 1, 1941

By Emby Kaye

It is the purpose of this paper to outline briefly some of the considerations that enter into the economics of so-called recycling, the generic designation of the relatively recently developed process by which a condensate† is separated from gas-distillate gas at high pressure and the residual gas returned to the reservoir. This subject necessarily embraces not only a discussion of factors that should be considered in projecting a recycling operation, such as estimating reserves, investment and operating costs, but also a comparison of condensate with other types of petroleum. The place of condensate in its relation to the total supply of crude oil is pointed out as well as certain logical methods of product disposal. The cost of drilling wells and lease maintenance is not pertinent to this discussion because income and revenue are in this paper confined to that retained by the plant or plant operator for supplying processing facilities for the gas. Before the development of recycling a great many gas-distillate gas fields in Louisiana and Texas provided no income to their owners. When gas was sold from these reservoirs it was accompanied by irretrievable losses of condensate in the formation. The understanding of the func- tion of retrograde condensation resulted in the introduction of a new commercial petroleum recovery process for these hitherto unexploited fields and now permits the conditioning of this type of wet gas field for the sale of dry gas therefrom without waste. Some Economic Factors The study of a gas-distillate field for possible exploitation necessarily involves the critical appraisal of a number of elements, chief of which will be discussed here: (I) estimate of distillate in place, (2) estimate of distillate that can be brought to the surface, (3) available market, (4) costs. The considerations affecting the estimating of distillate reserves in place are in the main subject to the same errors as are involved in determining dry gas reserves. Determinable data including acreage, sand thickness, reservoir pressure, reservoir temperature, porosity and connate water provide the basis for calculating the volume of gas in place. Ample allowance must be made for connate water, which may occupy from 20 to 35 per cent of the pore space of the sand. The factor of supercom-pressibility is to a considerable extent nullified by the reservoir temperature. It has been considered well advised to allow this factor to serve as a cushion. With the gas reserves calculated, it remains only to assay the distillate content of the gas. Those familiar with the handling of "wet" gas at high pressure readily appreci-ate the variables in sampling gas from

Jan 1, 1942

By Emby Kaye

It is the purpose of this paper to outline briefly some of the considerations that enter into the economics of so-called recycling, the generic designation of the relatively recently developed process by which a condensate† is separated from gas-distillate gas at high pressure and the residual gas returned to the reservoir. This subject necessarily embraces not only a discussion of factors that should be considered in projecting a recycling operation, such as estimating reserves, investment and operating costs, but also a comparison of condensate with other types of petroleum. The place of condensate in its relation to the total supply of crude oil is pointed out as well as certain logical methods of product disposal. The cost of drilling wells and lease maintenance is not pertinent to this discussion because income and revenue are in this paper confined to that retained by the plant or plant operator for supplying processing facilities for the gas. Before the development of recycling a great many gas-distillate gas fields in Louisiana and Texas provided no income to their owners. When gas was sold from these reservoirs it was accompanied by irretrievable losses of condensate in the formation. The understanding of the func- tion of retrograde condensation resulted in the introduction of a new commercial petroleum recovery process for these hitherto unexploited fields and now permits the conditioning of this type of wet gas field for the sale of dry gas therefrom without waste. Some Economic Factors The study of a gas-distillate field for possible exploitation necessarily involves the critical appraisal of a number of elements, chief of which will be discussed here: (I) estimate of distillate in place, (2) estimate of distillate that can be brought to the surface, (3) available market, (4) costs. The considerations affecting the estimating of distillate reserves in place are in the main subject to the same errors as are involved in determining dry gas reserves. Determinable data including acreage, sand thickness, reservoir pressure, reservoir temperature, porosity and connate water provide the basis for calculating the volume of gas in place. Ample allowance must be made for connate water, which may occupy from 20 to 35 per cent of the pore space of the sand. The factor of supercom-pressibility is to a considerable extent nullified by the reservoir temperature. It has been considered well advised to allow this factor to serve as a cushion. With the gas reserves calculated, it remains only to assay the distillate content of the gas. Those familiar with the handling of "wet" gas at high pressure readily appreci-ate the variables in sampling gas from

Jan 1, 1942

By Hamilton Wingate

In view of the fact that the fineness of the resultant bullion varies with the particular treatment to which the zinc-precipitate is subjected, and since there are considerable losses attributed to both methods, the following notes on the results obtained at the Waitekauri Extended mine, Maratoto, N. Z., may be of interest. The ordinary method of roasting the vacuum-dried precipitate was adopted instead of the treatment with sulphuric acid, the necessary facilities for the latter method not being available. Moreover, provided the ordinary method is carried out with the necessary care, it is questionable if it is not the most satisfactory where large quantities of precipitate have to be handled, and where (as is generally the case in this district) a considerable amount of silver is present. All the precipitate was first washed through a 40-mesh sieve. If it was necessary to recover the bullion at once from the accumulated short zinc, it was oxidized and melted separately; but, as a general rule, being heavily charged with bullion, it was placed on the bottom of the trays at, the top end of the extractor-boxes, where it acted as an excellent precipitant, the bullion being recovered at the next clean-up. After drying on a filter with the aid of a vacuum-pump, the precipitate was weighed and removed to the oxidizing furnace, which is similar to that generally in use in New Zealand, consisting essentially of an ordinary square tray of cast-iron, with 6-in. sides, built over a brick furnace. Wood is used as fuel. The tray is hooded over with sheet-iron, fitted with a sliding-door, and the fumes pass through a flue at the top into a dust-chamber, then into the open air. Oxidation of the Precipitate.—The oxidation was conducted first at a low temperature, which was gradually raised, until

Jan 1, 1903

By W. R. Hudspeth

AS an outgrowth of its spodumene recovery operation at Kings Mountain, N. C., Foote Mineral Co. has been recovering a heavy mineral by-product. Foote leased this idle plant in 1951, reactivated it, using a new spodumene recovery process, and purchased plant and properties in October 1951. While the operation at Kings Mountain is primarily concerned with the production of spodumene concentrate, pilot plant work determined that the pegmatites also contained heavy minerals including cassiterite. Plans were made to recover the heavy minerals as a by-product and the flowsheet incorporated these facilities when the mill was modified for the new spodumene recovery process. The orebodies consist of spodumene, feldspar, quartz and mica. Apatite, tourmaline, and beryl are present in small quantities. The wall rock is pre- dominantly hornblende shist. The heavy minerals, including cassiterite, columbite, pyrrhotite, monazite, pyrite, and rutile represent about 0.2 pct of the ore. The fine-grained heavy minerals are disseminated throughout the dikes, apparently unassociated with the spodumene. The pegmatites are quarried and secondary breakage is by mud-capping and block-holing. Power shovels load into trucks transporting the ore to a coarse ore bin. A Telesmith 10x36-in. apron feeder delivers the ore to an 18x36 in. Traylor Jaw crusher adjusted to discharge -3 in. product to a primary conveyor. The conveyor delivers to a 4x5-ft Tyrock single deck vibrating screen using 3/4 in. cloth. The screen undersize is elevated to the crushed ore bin. Screen oversize goes to an Allis-Chalmers Hydrocone Crusher fitted with 4 in. concave and set to deliver approximately 66 pct minus 3/4 in. The crusher discharge returns to the primary conveyor. The crushing and screening installation has a capacity of about 60 tons per hour. Spirals The crushed ore is delivered at a rate of 350 tons per day to two 6x8-ft Hardinge Pebble Mills, equipped with 20 mesh Ton-Cap trommel screens. The screen oversize is pumped to a 12-in. hydroclone for primary desliming. The hydroclone underfl spirals. There is no heavy mineral loss in the hydro-clone overflow. The spirals bank consists of eight 5-turn Model 24-A Humphreys Spirals. The top port and the last four ports of each spiral are blanked, the remaining nine port splitters are adjusted to remove about 5 pct feed weight. The heavy mineral rougher concentrates are upgraded on a Deister Overstrom table. The spiral concentrates contain approximately 4 pct heavy mineral, and the spiral reject, which goes to another section of the plant for spodumene recovery, contains about 0.03 pct heavy mineral. There is an interesting feature in the spirals installation. An adjustable splitter mounted on the discharge boxes splits out a mica fines product containing very little heavy mineral. The mica product is cleaned by spiralling and screening. Thus the spirals recover two products; mica, and a heavy mineral rougher concentrate. Table Treatment The rougher spiral concentrate goes to a Deister Plato table, modified to receive a Deister-Overstrom No. 6 rubber cover with sand riffles. The table is operated with a 5/8 in. stroke, 270 strokes per minute, and a slope of 1/2 in. per ft from feed to tailings side. There is no slope adjustment from motion to concentrate end. Wash water consumption is relatively high, since the large spodumene grains tend to report with the fine heavy minerals. A middling band about 4 in. wide is maintained in order to produce clean concentrate. The middling, representing about 10 pct of table feed, is recirculated by air-lift. A band of concentrate grade coarse spodumene occurs just below the middling. This is removed and delivered to concentrate storage. The table tailing, containing approximately 0.7 pct heavy minerals, is returned to the spodumene feed preparation circuit. The heavy mineral table concentrates are approximately 45 pct cassiterite, 33 pct columbite, 14 pct pyrrhotite and 8 pct monazite, together, with some rutile, pyrite, and copper from blasting wire. Concentrate is collected at 24 hour intervals. and dried. If the concentrate remains in wet storage appreciably longer surface oxidation takes place which seriously interferes with the subsequent magnetic separation process. About 150 lb of heavy mineral concentrate is produced per 24 hours and shipped to the company's plant at Exton, Pa. for final separation into tin and columbium concentrates.

Jan 1, 1952

By Joseph W. Richards

(New York Meeting, February, 1912.) THE Ashio copper-mine of the Furukawa Mining Co. is situated 18 miles from Nikko, and 109 miles north of Tokyo, near the center of Japan. The mine-waters are run over scrap-iron, whereby most of the copper is precipitated as cement copper, leaving iron sulphate with some copper sulphate in solution. After using in the wet concentrating ore-dressing plant, the waste water contains clay and ore-slimes. The only avenue of disposal of this water is the Watarese river; but as this flows through valleys in which the water is used for irrigating the rice-crops, it is necessary to purify and clarify the water before discharge. The water amounts to from 600 to 700 cu. ft. (from 17 to 20 cu. m.) per minute, and averages about 0.00025 per cent. of copper, representing more than 18 tons of copper per month. The water carries H2SO4, FeSO4, Fe, (SO,),, CuSO4 and other metallic sulphates in solution, and clay, ore-fines, slimes and basic. iron sulphates as suspended matters. To purify and clarify the water, precipitation by milk of lime has been used, in three different ways, as follows: I. First Method, Copper not Recovered. Milk of lime was run into the water, and the mixture run through six settling-ponds, and then through a sand filter into the river. Fig. 1 is a view of the settling- and filtering-ponds. In the first pond, sand and metallic hydrates free from copper collected; in the next five ponds, slime, calcium sulphate, and metallic hydrates carrying copper settled out. The effluent carried from 0.1 to 0.05 mg. of copper per liter

Jun 1, 1912

By Walter Rose, W. A. Bruce

Improved apparatus, methods, and experimental techniques for determining the capillary pressure-saturation relation are described in detail. In this connection a new multi-core procedure has been developed which simplifies the experimental work in the study of relatively homogeneous reservoirs. The basic theory concerning the Leverett capillary pressure function has been extended and has been given some practical application. Some discussion is presented to indicate the relationship of relative permeability to capillary pressure, and to provide a new description of capillary pressure phenomena by introducing the concept of the psi function. INTRODUCTION For the purposes of this paper the capillary character of a porous medium will be defined to express the basic properties of the system, which produce observed results of fluid behavior. These basic properties may be classified in the following manner, according to their relationship to: (a) The geometrical configuration of the interstitial spaces. This involves consideration of the packing of the particles, producing points of grain contact, and variations in pore size distribution. The packing itself is often modified by the secondary processes of mineralization which introduces factors of cementation, and of solution action which causes alteration of pore structure. (b) The physical and chemical nature of the interstitial surfaces. This involves consideration of the presence of interstitial clay coatings, the existence of non-uniform wetting surfaces; or, more generally, a consideration of the tendency towards variable interaction between the interstitial surfaces and the fluid phases saturating the interstitial spaces. (c) The physical and chemical properties of the fluid phases in contact with the interstitial surfaces. This involves consideration of the factors of surface, interfacial and adhesion tensions; contact angles; viscosity; density difference between immiscible fluid phases; and other fluid properties. Fine grained, granular, porous materials such as found in petroleum reser~oir rock possess characteristics which are expressible by (1) permeability, (2) porosity, and (3) the capillary pressure-saturation behavior of immiscible fluids in this medium. These three measurable macroscopic properties depend upon the microscopic properties enumerated above in a manner which defines the capillary character. Systems of capillary tubes or regularly packed spheres may be thought of as ideal and numerous references can be cited in which exact mathematical formulations are developed to show the relationships governing the static distribution and dynamic motion of fluids in their interstitial spaces. The capillary character of non-ideal porous systems such as reservoir rock also is basic in determining the behavior of fluids contained therein; although, in general, the connection is not mathematically derivable but must be approached through indirect experimental measurement. This paper gives consideration to the evaluation of petroleum reservoir rock capillary character. The methods employed may be applied to the solution of problems in other fields, and the conclusions reached should contribute to the basic capillary theory of any porous system containing fluid phases. In this paper, a modification of the core analysis method of capillary pressure is employed and it is intended to show that the capillary character of reservoir rock can be expressed in terms of experimental quantities. A very general method of interpretation correlating the capillary pressure tests with fundamental characteristics such as rock texture, surface areas, permeability, occasionally clay content and cementation is introduced. Eventually an attempt is made for establishing a method of deriving relative permeability to the wetting phase from capillary pressure data. The experimental evaluation of capillary character must be approached in a statistical manner if reservoir properties are to be inferred from data on small cores. This is implied by the heterogeneous character of most petroleum reservoirs, and suggests that considerable intelligence should be applied in core sampling. Finally, this paper supports the view that once the capillary character of a given type of reservoir rock has been established by core analysis, fluid behavior can then be inferred in other similar rock. Although no great progress has been made in establishing what variation can be tolerated without altering the basic fluid behavior properties, evidence will be presented to indicate that certain reservoir formations are sufficiently homogenous with respect to capillary character that the data obtained on one core will be useful in predicting the properties of other cores of similar origin. Tests have shown that cores under consideration can vary widely with respect to porosity and permeability and still be considered similar in capillary character. EXPERIMENTAL METHODS AND TECHNIQUES Various types of displacement cell apparatus for capillary pressure experiments have been described in the literature. Bruce and Welge; Thornton and Marshall; McCullough, Albaugh and Jones3; Hassler and Brunner; Lever-

Jan 1, 1949

By N. Mungan

Formation damage, i.e.. reduclion in permeability, has been generally attribuled to clay minerals which expand or disperse upon contact with water that is less saline than the connate water. Luboratory, studies show that penneahility reduction can also occur in formalions containing only nonexpandable clays such as illite or kaolinite, and can be caused also by changes in pH. Furthermore, pH changes can damage even formations that are essentially free of clays. It is suggested that permeability reduction is due to the small passages being blocked by particles, which may be dispersed clays, cemenlion material or other fine parricles. These particles are dislodged by dispersion of clays due to changes in salinity or by dissolution of calcareous cement by acids, or of silicaceous cement by alkaline solutions. In working with reservoir cores, it was found that extracted cores damaged more easily and extensively than nonextracted cores. The extent of damage depended also on tenlperatltre. INTRODUCTION Permeability is an important property of porous media and has been the subject of many studies by engineers and geologists. Many of these studies are conccrned with formation damage, i.e., reduction in permeability, resulting from exposure of oil-producing formations to water substantially less saline than the connate water. This effect causes understandable concern since during drilling, completion and production phases formations are often exposed to fresh water. The damage resulting from contact with relatively fresh water has been attributed to expansion and dispersion oF clay minerals. During laboratory investigation of the use of NaOH as a wettability reversal agent to increase oil recovery from oil-wet reservoirs, several cores used in the displacement studies suffered loss in permeability. Despite the traditional usage of NaOH for conditioning aqueous mud systems, the role of the caustic filtrate in wellbore damage seems to have been overlooked. Browning2 as recently reported on the effects of NaOH in dispersing clay minerals but he was concerned only with complications that may arise in drilling massive shale beds. The following study was made to examine the role of pH and salinity changes in core damage. Where cores from reservoirs were used, tests were performed with extracted and nonextracted cores both at room and reser- voir temperatures, since it was felt that the test environment and core condition may affect the results. Because of its limited coverage and exploratory nature, this study is not intended to provide answers to field formation damage problems. It is hoped that it will encourage research into new aspects of the permeability reduction problems, particularly those allied to new recovery and production processes. PROCEDURE In all permeability tests, fluids were pumped through the cores at a constant volumetric rate. Only deaerated fluids and reagent grade chemicals were used. The fluids were passed through two ultrafine filters before injection to remove any entrained particles. The cores, with the exception of the unconsolidated cores, were mounted in Hassler holders. Water was used to transmit pressure to the sleeve. The inlet endpiece had two entry ports which permitted scavenging one fluid with another to avoid any mixing in the small holdup volume. The cores were flushed with CO2 gas, evacuated for 5 to 6 hours and saturated with the first liquid at a pressure of 1,000 psi for 24 hours to eliminate any free gas from the cores. Pressure differences up to 20 psi were measured by transducers, calibrated in inches of water and continuously recorded. For greater pressure drops, gauges were used. All reservoir cores were cleaned with a light refined mineral oil, then with heptane, and finally dried with CO2. Compatibility tests showed that no precipitates formed when mineral oil and the crudes were mixed. Some cores were extracted in Dean-Stark-type solvent extractors using xylene and trichloroethane and dried in a vacuum oven at 450F. Each test consisted of a sequence of water, test solution, and again water flow. RESULTS AND DISCUSSION STUDIES IN BEREA CORES Salinity Contrast Berea cores 2-in. in diameter and 12-in. long were cut from sandstone quarried in Cleveland, Ohio. The clay minerals were identified by X-ray diffraction to be chlorite, kaolinite, illite and incerlayered illite. Flow of fresh water or 30,000 ppm brinc does not cause any permeability reduction (Fig. 1). However, after injection of brine the core is readily damaged by fresh water. Damage starts almost instantly as the fresh water injection is begun, and at a cumulative injection of 1.2 PV fresh water, the permeability has dropped from 190 to 0.9 md. Upon continued injection, the effluent contains clay minerals dislodged from the core. The final core per-

Jan 1, 1966

By Walter Rose, W. A. Bruce

Improved apparatus, methods, and experimental techniques for determining the capillary pressure-saturation relation are described in detail. In this connection a new multi-core procedure has been developed which simplifies the experimental work in the study of relatively homogeneous reservoirs. The basic theory concerning the Leverett capillary pressure function has been extended and has been given some practical application. Some discussion is presented to indicate the relationship of relative permeability to capillary pressure, and to provide a new description of capillary pressure phenomena by introducing the concept of the psi function. INTRODUCTION For the purposes of this paper the capillary character of a porous medium will be defined to express the basic properties of the system, which produce observed results of fluid behavior. These basic properties may be classified in the following manner, according to their relationship to: (a) The geometrical configuration of the interstitial spaces. This involves consideration of the packing of the particles, producing points of grain contact, and variations in pore size distribution. The packing itself is often modified by the secondary processes of mineralization which introduces factors of cementation, and of solution action which causes alteration of pore structure. (b) The physical and chemical nature of the interstitial surfaces. This involves consideration of the presence of interstitial clay coatings, the existence of non-uniform wetting surfaces; or, more generally, a consideration of the tendency towards variable interaction between the interstitial surfaces and the fluid phases saturating the interstitial spaces. (c) The physical and chemical properties of the fluid phases in contact with the interstitial surfaces. This involves consideration of the factors of surface, interfacial and adhesion tensions; contact angles; viscosity; density difference between immiscible fluid phases; and other fluid properties. Fine grained, granular, porous materials such as found in petroleum reser~oir rock possess characteristics which are expressible by (1) permeability, (2) porosity, and (3) the capillary pressure-saturation behavior of immiscible fluids in this medium. These three measurable macroscopic properties depend upon the microscopic properties enumerated above in a manner which defines the capillary character. Systems of capillary tubes or regularly packed spheres may be thought of as ideal and numerous references can be cited in which exact mathematical formulations are developed to show the relationships governing the static distribution and dynamic motion of fluids in their interstitial spaces. The capillary character of non-ideal porous systems such as reservoir rock also is basic in determining the behavior of fluids contained therein; although, in general, the connection is not mathematically derivable but must be approached through indirect experimental measurement. This paper gives consideration to the evaluation of petroleum reservoir rock capillary character. The methods employed may be applied to the solution of problems in other fields, and the conclusions reached should contribute to the basic capillary theory of any porous system containing fluid phases. In this paper, a modification of the core analysis method of capillary pressure is employed and it is intended to show that the capillary character of reservoir rock can be expressed in terms of experimental quantities. A very general method of interpretation correlating the capillary pressure tests with fundamental characteristics such as rock texture, surface areas, permeability, occasionally clay content and cementation is introduced. Eventually an attempt is made for establishing a method of deriving relative permeability to the wetting phase from capillary pressure data. The experimental evaluation of capillary character must be approached in a statistical manner if reservoir properties are to be inferred from data on small cores. This is implied by the heterogeneous character of most petroleum reservoirs, and suggests that considerable intelligence should be applied in core sampling. Finally, this paper supports the view that once the capillary character of a given type of reservoir rock has been established by core analysis, fluid behavior can then be inferred in other similar rock. Although no great progress has been made in establishing what variation can be tolerated without altering the basic fluid behavior properties, evidence will be presented to indicate that certain reservoir formations are sufficiently homogenous with respect to capillary character that the data obtained on one core will be useful in predicting the properties of other cores of similar origin. Tests have shown that cores under consideration can vary widely with respect to porosity and permeability and still be considered similar in capillary character. EXPERIMENTAL METHODS AND TECHNIQUES Various types of displacement cell apparatus for capillary pressure experiments have been described in the literature. Bruce and Welge; Thornton and Marshall; McCullough, Albaugh and Jones3; Hassler and Brunner; Lever-

Jan 1, 1949

By Felix A. Vogel

I (New York Meeting, February, 1912.) FLUE-DUST, to most blast-furnace operators, means a troublesome by-product, the formation of which should be curtailed, if not prevented entirely. However, with the increasing use of fine ores, larger furnaces, and high-pressure blast, the production of flue-dust is constantly increasing, and amounts annually in the United States to from 3,000,000 to 3,500,000 tons, An exceedingly high tonnage, of which a large part has been discarded as valueless. As a result of greater economy in the iron industry, the attention of our furnace-men has been directed towards the utilization of this enormous amount of waste material, a problem which had also been given due consideration by metallurgists abroad. Flue-dust is generally a fine material containing considerable coke and iron-ore, with a small admixture of lime and silica, depending upon the burden. The iron-ore is partly reduced, which shows that the dust originates largely in the reducing-zone of the blast-furnace. In the United States this dust usually contains 20 per cent. of coke and more than 40 per cent. of iron. Estimating coke to be worth $3.25 per ton, and iron-ore 7 cents per unit, a ton of flue-dust, unless made available, represents a loss to the furnace-man of $3.50. This accounts for the first efforts to recharge the flue-dust into the furnace, either by moistening it clown with an excess of water, or mixing it with clay to form balls of pulp, or treating it with lime-water. These methods, however, have been practically discarded, as they failed to produce the desired economies. To recover, in the blast-furnace, all the values represented by the material contained in the flue-dust, the following con¬ditions should be complied with

May 1, 1912

By D. R. George, J. R. Ross, J. D. Prater

In the United States nearly 200,000 tons of copper per year are being produced, by leaching waste rock and oxidized copper ore with dilute sulfuric acid-ferric sulfate solutions and precipitating the copper on scrap iron. The flow of solutions is in excess of 80 million gpd. A survey conducted by the U.S. Bureau of Mines in late 1965 at 14 mines in Arizona, Utah and Nevada, showed that with a few exceptions, the solutions contain from two to a maximum of 15 ppm U3O8, and there is strong evidence that these represent equilibrium concentration and not merely an accumulated in-process inventory resulting from recycling the solutions for many years. Consequently, it is believed that uranium could be recovered at a constant rate as long as mining and leaching operations continue. Preliminary surveys and estimates by the USBM indicate a production potential of possibly 1000 tons of U3O8 per year at a cost of less than $8 per lb if the major process streams from most of the large copper mines in the western United States were to be treated. Laboratory research by the USBM showed that the uranium could be efficiently recovered as a specification-grade uranium concentrate by a combination of ion exchange resin and solvent extraction of liquid ion exchange techniques. A joint pilot plant investigation by Kennecott Copper Corp. and the USBM was conducted on solutions from the Bingham Canyon mine to evaluate a new system of countercurrent ion exchange developed during the laboratory studies. In subsequent small-scale continuous tests, recovery of uranium from the pregnant eluate by solvent extraction and chemical precipitation techniques was investigated.

Jan 1, 1968

By Harrison Souder

THE object of this paper is to bring to. the notice of engineers a safety detonating fuse by the use of which misfires in blasting may be eliminated and safety in blasting operations promoted. This new detonator is a French invention and is known as Cordeau detonant or detonating fuse and is sold under the name of Cordeau-Bickford. It consists of a lead tube 5 to 6 mm. in diameter, filled with trinitro-toluene. While applicable to all classes of mining it will appeal especially to those who have to do with deep-hole blasting in open-cut clines or quarries, or any operations where a large number of holes are to be shot at one time. Since the introduction of the deep-hole blasting in the Cornwall iron mines, much trouble has been experienced from misfires and many experiments were made to determine the best and safest method of blasting. Before the introduction of the detonating fuse it was found that to insure the best results, two or more high-power electric exploders, not less than No. 6, with specially insulated conductors, should be placed in each hole; the holes wired in parallel, and for a large number of holes the current to be supplied by a live wire to the bus or lead wires at about the middle of the bench. The voltage in general use is 110 to 220, but as our material is a magnetic iron ore and the holes are generally damp, we found it advisable to reduce this to about 30 volts to prevent short circuits. A No. 7 or No. 8 special insulated detonator was adopted. But with the best of care and attention to the minutest detail, we were not able to eliminate occasional misfires and the consequent ever present danger of accidents.

Jan 10, 1914

By W. R. Seyfried

The problem of extracting alumina from clay and low-grade bauxites has been the subject of considerable interest for some time. The basic reason, of course, lies in the fact that known reserves of high-grade bauxite are not inexhaustible and that the present commercial process cannot successfully cope with low-grade bauxites or clay. Ultimately it may be necessary to use these poorer raw materials for all commercial operations. An unprecedented demand for aluminum during the war emergency and the constantly threatened shortage of imported bauxite caused the United States Government to take an active role in this problem. Through the National Academy of Sciences, the War Production Board and the Defense Plant Corporation, it investigated processes and finally selected four to be used in the construction and operation of four experimental plants. Each plant was to be designed in such a way as to facilitate its incorporation into a larger commercial plant should the need arise. The Chemical Construction Corporation process, or "Chemico" ammonium sulphate process as it is better known, was one of the four selected. The extensive literature and patents on record before the war generally follow one of two process-types depending upon the extracting reagent used. One group uses an acid reagent, the other an alkali. The Chemico process uses an acid reagent. For those interested in other processes described in literature, there is a short bibliography at the end of this paper. The basic steps of all acid extraction processes are: (I) to make the aluminum silicates acid soluble, (2) to separate the released alumina from impurities and insoluble gangue, and (3) to recover the reagent for re-use. The Process as Planned In April 1941, a group of chemists and engineers of the Chemical Construction Corp. became interested in the problem of extracting alumina from clays and low-grade bauxites and, under the leadership of Mr. Blakeslee Barnes, Vice President and General Manager of the company, first drafted a process in July of that year—five months prior to Pearl Harbor. The work continued in our research laboratories and with a small pilot plant. By June 1943, the work had progressed to a point where it was possible to apply for a patent on the process which was U.S. patent 2,405,426, granted August 6, 1946. Immediately prior to the development of the Salem plant, the process was envisaged to be as follows: I. The first step was to make the aluminum silicates acid soluble. It was planned: (a) Clay or lour-grade bauxite would be roasted at 700 to 800°C (1292° to 1472°F). (b) The roasted ore would then be leached with hot aqueous ammonium bi-sulphate to form a slurry. In this way the

Jan 1, 1949

By N. J. Grant, B. C. Giessen, Paul Predecki

ALLOYS of gold, silver, and aluminum with elements of the groups BII, BIII, BIV, and BV were prepared by a rapid quenching technique (splat) and were examined by X-ray diffraction. Five new intermediate phases were found and will be described briefly herein. For the gold and silver systems, the concentration ranges having an electron/atom ratio e/a of 1.4 to 1.5 ("3/2 Hume-Rothery phases") were studied primarily. Master alloys were prepared from high-purity metals (99.9+ pct or better) by melting either in evacuated fused silica capsules or by nonconsum-able-electrode arc melting in an argon atmosphere. Small pieces, 20 to 50 mg, of each alloy were blast-atomized to form a splat, by a technique similar to that described by Duwez and Willens.1 The technique used for this study is described in detail in Ref. 2; it utilizes a resistance-heated graphite crucible with a small hole at the bottom, directed toward a metal substrate or quenching plate. The prepared alloy rests over the fine hole, through which it is expelled by an explosion shock wave in the form of fine droplets (1 to 50 µ) of molten metal onto a copper or silver substrate, which is maintained at about -190°C. The resulting very high cooling rates (see Ref. 2 for quantitative measurements) can prevent the process of nuclea-tion and growth in many instances, resulting in the formation of metastable phases. The splat particles were transferred to a GE-XRD5 diffractometer and maintained at -190°C, where they were examined with CuKa radiation. The samples were then allowed to warm to room temperature or were heated to higher temperatures until the equilibrium structures formed. Of fifteen alloy systems considered, nonequi-librium structures were encountered in six; these are described below and summarized in Table I. In the system Au-Sb a metastable £ phase (A3 type, hcp, a = 2.898 + 0.002A; c = 4.731 * 0.004A; c/a = 1.633) was found in the concentration range Au + 13 to 15 at. pct Sb. This phase is isomorphous with the stable phases in the systems Au-Cd, Au-In, and Au-Sn, all at an average e/a ratio of 1.4 to 1.5. The concentration range of one-phase metastable was deduced from the small amounts of supersaturated gold solid-solution phase present in the splat product. It was found that ? could also be retained by splatting onto a substrate held at room temperature: however, decomposed into the equilibrium phases Au + AuSb2 after heating to 200°C for 1/2 hr, or on holding the powdered splatted alloy at 20°C for several months. Calorimetric measurements will be made in an attempt to decide the question whether ? is metastable at all temperatures or whether it is a stable phase at low temperatures. There is evidence that another phase, possibly also close-packed but with a different stacking sequence, can be obtained by rapid quenching of alloys with a different antimony content. Klement, Willens, and Duwez3 reported the existence of an amorphous phase on quenching Au-Si alloys (25 at. pct Si) to - 196°C. They found that on heating to room temperature another phase of unknown crystal structure was formed. This was confirmed (see Table I); however, the new crystalline phase, designated as ?, could also be formed simply by rapid quenching to room temperature, and even was found to exist already in the as-cast Au + 20 at. pct Si alloy. It was found that ? decomposed into Au + Si on the specimen surface at room temperature. This behavior, and the question whether or not there is an equilibrium-temperature region for ?, have not yet been resolved. It is probable that ? (Au + 20 to 21 at. pct Si) is cubic of the -brass type (D81-3) with a = 9.60, + 0.01A and N = 52 atoms per cell [compare 6 (CU-Sn)4]. Except for two very weak lines, the powder pattern of about thirty lines could be indexed on this basis; however, a determination of the atom positions has not yet been attempted. For Au-Ge the C phase was observed at about 21 at. pct Ge as reported by Luo et at.5 Lattice parameters a = 2.876A, c = 4.73,A, c/a = 1.64 were found. In the Au-Pb system, formation of a ? phase was not observed, but in the lead-rich region at 75 at. pct Pb, broad peaks belonging to an amorphous phase were found. The maximum diffracted intensity occurred at 28 = 32.4 deg which is about 1 deg larger than the position of the (111) line of lead (Cuka). For Ag-Pb, an amorphous phase analogous to the one found in the Au-Pb system was observed; this metastable phase exists probably at about 75 at. pct Pb. Since no lead-rich alloys were tested, all alloys consisted of silver + amorphous phase at -190°C. In A1-Ge alloys, line-rich and complex powder patterns were obtained at about 30 at. pct Ge; they bear similarities to those of aluminum and germanium, but are of lower symmetry; the existence of more than one intermediate phase is possible. The authors are grateful to the Kennecott Copper Corp. for Fellowship support, and ARPA (Contract

Jan 1, 1965

By Franklin Bache

THERE seems to be in the public mind, and even in the minds of some coal-operators not experienced in mines subject to dust-explosions, a feeling that there has been something mysterious at the bottom of a number of recent American colliery-explosions. It has been declared in cases of accidents in mines regarded as particularly well equipped, in which every preventive precaution was said to have been taken, that the explosions were incomprehensible, and resulted from causes beyond the present knowledge of the practical coal-operator. But it is safe to say that no explosion has taken place which could not be explained by reasons well understood by most operators. The LT. S. Geological Survey Test Laboratory, recently inaugurated at Pittsburg for the reported purpose of investigating scientifically the matter of explosions in mines, will discover no new explanation of explosions. It call, however, co-ordinate the previous investigations of similar boards in England and on the Continent; and it may do a vast amount of good by promulgating widely, and in a form comprehensible by the most unlettered miner, certain facts and obvious deductions that cannot but have an effect in reducing the number and extent of the mine-disasters which, in the last few years, have been so terrible in frequency and magnitude. The only possible sources of explosions of any magnitude in coal-mines are : (1) explosives stored in quantity in the mine; (2) gases generated or liberated in the mine; and (3) coal-dust. Combinations of any of the three may, of course, take part in the result. The danger of any great loss of life from stored explosives alone is very remote. The simplest ordinary precaution forbids the presence, in one place underground, of any considerable quantity of explosives, and it would require an

Aug 1, 1909

By R. W. Carpenter, J. C. Ogle

It is possible, by using pack-rolling instead of conventional rolling, to reduce a number of metals to thicknesses of 2µm or less. Such thinfoils are generally made at room temperature without intermediate annealing. In addition, pack-rolled foils fail by developing pinholes at thicknesses near 2µm instead of developing the shear cracks usually observed in cold-rolled ductile metals. This paper presents the results of a general investigation of the deformation substructure and texture developed in copper and iron pack -rolled from 130 to about 2µm thickness. Electron microscopy showed that in both metals a fine (0.2 to 0.5?µ m) deformation subgrain structure formed during pack-rolling; in neither case was this substructure grossly different from substructures formed during conventional rolling. The deformation texture formed in pack-rolled iron was quite similar to usual bcc textures; however, in the case of copper, the cube texture was stable during pack-rolling and the normal copper deformation texture was unstable. It is shown analytically that the constraining pack induced a large hydrostatic pressure in the foils during pack-rolling. The pinhole failure mechanism is attributed to the presence of the large hydrostatic pressure during pack-rolling; this strongly suppressed the growth of shear cracks. The stability of the cube texture in copper is also probably due to the unusuul stress distribution developed during pack-rolling. EXPERIMENTS at several laboratories have shown that very thin foils of the common structural metals and many of the rare earths can be made by "pack-rolling". 1-3 The technique was originally developed to make specimens for nuclear scattering experiments and foils for X-ray filters. It is also useful for making experimental laminar metallic composite bodies and foils thin enough for direct examination by ultra-high voltage electron microscopy without the need for special thinning techniques. Pack-rolling in the present context means a three-layer pack, with the material to be rolled into foil comprising the center layer. The outer two layers, which constrain the foil during reduction, are ordinarily austenitic stainless steel. Typically, a 130 µm (0.005 in.) metal strip can be reduced to a final thickness of 2 µm or less by this process. This is accomplished at room temperature, without intermediate annealing. It has been observed that foils produced by this process do not exhibit at any stage of their reduction the severe work-hardening found in strip rolled by conventional cold-rolling methods. Neither is the failure characteristic the same."&apos; Conventionally cold-rolled ductile metal strip fails by developing shear cracks on planes whose normals nearly bisect the angle between the rolling direction and normal to the rolling plane; these are planes of maximum shear stress. In pack-rolling this mechanism has not been observed; failure occurs by the formation of pinholes on the foil surface (penetrating the foil). If pack-rolling is continued the hole density increases. These differences in behavior imply the existence of appreciably different substructure in pack-rolled foils compared to substructure in conventionally rolled material, or perhaps that the geometry of pack-rolling has an effect on the foil behavior. This paper describes an investigation of deformation substructure and texture in some specimens of pack-rolled copper and iron, and some considerations of the stress distribution in the foils during rolling that result from the geometry of pack-rolling. EXPERIMENTAL DETAILS Three different materials were used for pack-rolling in the present work: soft copper sheet (99.8 pct Cu, 0.03 pct 0, electrolytic tough pitch) and two types of iron, Ferrovac E* and Armco iron. Each was "Crucible Stccl Co. initially in the form of 130 µm annealed strip with grain size ranges of approximately 10 to 40 µm. The initial texture of the copper (determined as noted below) was the normally observed cube type (001)[100]; there was evidence of a small amount of material in the cube-twin orientation reported by Beck and Hu.4 The initial texture of the Ferrovac E was similar to that reported for recrystallized iron by Kurdjumov and sachs,5 who list the principal orientations as {111}<112>, {001}<110> 15degfrom RD and a weak component {112}(110) 15 deg from RD. The starting texture of the Armco iron was not determined. Pack-Rolling Procedure. A four-high mill was used for all specimens. The work roll and backing roll diameters were 1.625 and 5.25 in., respectively. The peripheral roll speed of the work rolls was about 2.5 in. per sec. All foils were initially reduced from 130 to 100 µm by conventional straight rolling and then inserted into a pack, without any intermediate annealing, for further reduction. The pack consisted of an 0.033 in. (838 µm) thick 3 by 6 in. polished sheet of austenitic stainless steel, folded to make a 3 by 3 in. jacket. After folding, the jacket was given a small reduction to close the fold tightly before insertion of the foil. During pack-rolling a constant change in roll spacing was made every third pass. The roll-spacing change corresponded to a 5 pct reduction in thickness for a new pack. This approached a 10 pct reduction when the pack had decreased to about half its original thickness. At this point the deformed pack was discarded and a new one

Jan 1, 1970