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By Walter Miller

Crude oil stocks were some 10,000,000 bbl higher on June I, 1947, than at any time during 1946 but the extremely heavy refinery runs the last half of 1947 cut crude inventories to approximately the 1946 closing level of 225,000,000 bbl. Many refiners were seriously short of crude oil during the year. This shortage was reflected in numerous advances in the posted price of crude, justified in part as an incentive for more production but more generally due to competitive bidding. Some purchasers of crude, endeavoring to keep their plants running, resorted to the payment, either directly or indirectly, of premiums above the posted price. Another common practice employed by some suppliers of crude oil was to demand refined products in exchange or trade for their raw material. The refined products picture has darkened in spite of record throughputs. Stocks of gasoline and light and heavy fuel oils were uncomfortably low at the beginning of the year and were in general still lower at the close. The rationing of some products, principally gasoline, to dealers and stations? initiated during the year, gained momentum as stocks continued to diminish. The emphasis placed by the manufacturers of oil-burning equipment on the convenience and economy of heating with oil, together with the tight situation in coal, has developed a tremendous demand for burning oils. Consumption of liquefied petroleum gas for domestic and household fuel had more than doubled in 1946 over 1943, and the demand seems to be limited only by the ability of the equipment builders to furnish necessary storage. transportation, and burning equipment. The supply situation is likely to become more acute in 1948. Demand for petroleum products is being pushed to new heights not only by the unprecedented domestic market but by a sudden and drastic upswing in estimates of military and governmental requirements. Additionally, oil exports are running far below the volume requested, amounting to less than forty percent in a recent quarter, and export licenses are reportedly being approved on the basis of urgent need *only. AX recent White House release sees little likelihood that estimated requirements of the sixteen nations participating in the proposed Marshall Plan can be met in full over its projected life—1948 to 1951. Present demand dictates maintenance of refinery operations at the highest possible level and the Bureau of Mines has forecast daily average crude runs in 1948 of 5,265,000 bbl. The Economics Advisory Committee of the Interstate Oil Compact Commission recently estimated the 1948 demand for petroleum products at nearly 6 pct above 1947. They further estimate daily average crude runs of 5,375,000 bbl in 1948, some 2 pct higher than forecast by the Bureau of Mines. Projected demand exceeds supply to the extent that Capitol Hill is reportedly investigating ways of enabling oil companies to act in concert without danger of antitrust prosecution, such as elimination of crosshauls, pooling of products, and lowering of octane.

Jan 1, 1948

By Nicholas J. Grant, H. C. Chang

EMPHASIS on the importance of grain boundary sliding as a mode of deformation at elevated temperatures has been presented elsewhere.' The extent to which boundary sliding occurs under certain creep conditions has been determined for high purity aluminum2,3 and aluminum alloys.' In general, boundary deformation extends quite far into the adjoining grains, resulting in a rather wide band of deformation along the grain boundaries. This has led some investigators to doubt that grain boundary sliding consists of shearing along the boundary surface; it has been contended instead that boundary sliding is a result of concentrated slip in the neighborhood of the deformed grain boundaries."' The purpose of this note is to present evidence that grain boundary sliding takes place by a bulk shear process. gh purity polycrystalline aluminum, wherever and whenever there is grain boundary sliding, boundary migration and concentrated deformation along both sides of the deformed boundary are associated with it. Therefore, it has been rather difficult to obtain unambiguous evidence of boundary sliding. On the other hand, it would be expected in certain alloys of aluminum, when tested under particular conditions. that the severity of the interfering effects of boundary migration and concentrated deformation along the deformed boundary might be reduced. Current research in this laboratory' shows that a 20 pct Zn-A1 solid solution alloy fractures in an intercrystalline manner during creep at 500°F with a small total elongation of not more than about 14 pct, and that it does so with extremely limited grain boundary migration. Accordingly, this alloy was chosen for the present study. The experimental procedure was similar to that used in previous work and has been presented elsewhere.' Two parallel flat surfaces were milled from a round specimen. The gage portion of the specimen was 1 in. x .09 in. x .17 in. The specimens, which were annealed at 1030°F for 24 hr, showed two to four grains across the width of the test bar. The specimens were subjected to creep at 500°F at stresses of 2000 to 5000 psi. The rupture times were from 10 sec to 3 hr. Appreciable boundary sliding occurred in all the tests. A typical example of boundary sliding is shown in Fig. 1. (The tension axis is vertical in the micrographs.) Sliding has taken place along the boundary between grains A and B unaccompanied by important boundary migration. The sharpness of the offset at the triple point can be clearly seen in grain C. As a result of sliding along the boundary between grains A and B, a new boundary surface between grains A and C was created. The offset at the triple point is about 0.07 mm. This boundary sliding is accompanied by the formation of rather sharp kinking bands and, of course, slip on several slip systems in grain C. This type of deformation has been referred to as fold formation' in previous work with high purity aluminum.

Jan 1, 1957

By John Wulff

IN a previous paper Burwell and Wulff1 have shown by electron diffraction studies that allotropic transformations can be induced in 18-8 stainless steel by polishing to a depth of about 5 X 10-5 cm. The development of a successful etching technique, which removes accountable amounts of metal from the surface without pitting and without changing the root-mean-square profile as measured with an Abbot profilometer, led to the application of the whole technique and material to an investigation of various mechanical methods of surface preparation, such as grinding, lapping, superfinishing and cold-rolling. Ideally suited to such a study is 18-8 of low carbon and nitrogen content. The material can be heat-treated to produce a coarse-grained single-phase structure. On cold deformation there occurs not only a reduction in grain size but, at regions of maximum stress, a change of face-centered material to body-centered material, provided the metal is worked below about 200°C. When worked between 200° and 415°C., diffraction studies evidence a reduction in grain size without the appearance of any new body-centered ferrite. Ferrite, which can be referred also to strains induced by carbide precipitation, is evident when the material is worked at temperatures between 415° and 800°C. Stainless steel is advantageous because the usual surface-finishing operations do not readily oxidize it to any appreciable depth. In order to produce detectable oxide films on the surface of austenitic 18-8 in a time equivalent to that required to produce, for example, a fine ground finish on ½ sq. in., the sample must be held in a furnace or oxygen stream above 600°C. By using longer heating times, it is possible to achieve measurable oxide films on samples whose surface temperatures exceed only about 250°C. EXPERIMENTAL PROCEDURE The apparatus, material, and technique described in the previous paper1 were employed in this investigation. Samples of 18-8, 1 by 1 cm. by 4 mm., were carefully annealed in the austenitic range to produce a coarse-grained structure. They were then quenched and pickled to remove scale. On a lapping machine of the Graton2 type, both sides of each sample were polished to a flatness of 1/6 a wave length of sodium D light. Thereafter they were electrolytically etched to remove at least 1 X 10-3 cm. of the surface, a depth that is well below that of any deformations induced by surface preparation. Samples of this material, carefully mounted in steel holders, were then sent to various industrial organizations known for special finishing techniques. In the instrument shops at the Massachusetts Institute of Technology check samples were finished by the same methods, as far as they were available. Abbot profilometer3 readings were made on all the samples, which were then carefully degreased in double distilled benzine and alcohol, dried in a hot-filtered air blast, and kept in a desiccator. Suc-

Jan 1, 1941

By A. N. Holden, J. H. Hollomon

Inhomogeneous yielding during the early stages of plastic flow has been observed in many metals and has long been a subject of controversy. Low carbon steel, when strained at room temperature, exhibits a distinct yield point at which the metal ceases to behave elastically and begins to flow plastically without further increase in stress,† often with an actual decrease in stress from that existing at the yield point. One manifestation of this behavior is the familiar Lüders lines. The extent of the yield point elongation (the plastic strain which results without raising the stress above that at the initial yield point) may be several percent. Several explanations of this type of yielding in steels have appeared in the literature:1-3}; 1. The segregation of carbides or other constituents at the grain boundaries of ferrite forms cell-like blocks which break down at a higher stress than that at which the ferrite alone will flow. 2. The precipitation of various constituents within the ferrite itself in some way blocks initial flow until a higher stress is reached, after which a great deal of flow occurs without further increase in stress. 3. The restraining influence of neighboring, less favorably oriented grains in a polycrystal results in a storing up of energy, which on yielding is sufficient to cause the continued propagation of slip bands on the multiplicity of slip systems available in adjacent iron crystals without increase in stress. 4. Local segregation of carbon atoms increases the stress required for the initial propagation of dislocations. The stress required for further deformation is lower.3 Such an explanation would require the presence of upper and lower yield points in single crystals. Low and Gensamer2 have shown that heterogeneous yielding can be eliminated by removal of carbon and nitrogen from polycrystalline steels by wet-hydrogen treatment. They also demonstrated that the re-introduction of minute amounts of carbon or nitrogen caused a return of the yield point. Observations of the initial flow of single crystals containing small amounts of carbon and nitrogen- should provide a clue to the explanation of inhomogeneous yielding. Previous tests of iron crystals4-6 can not be considered conclusive because it is uncertain whether the carbon and nitrogen were satisfactorily removed by the decarburization technique employed. The purpose of the experiments described herein was to determine whether single iron crystals containing either carbon or nitrogen would exhibit in-homogeneous yielding. Experimental Procedures THE PREPARATION OF SINGLE CRYSTALS All crvstals were formed in the following way. Aluminum killed sheet material 80 mils thick was machined into specimens of the outer contour shown in Fig 1. These mildly tapered specimens were decarburized at 730°C for 16 hr in hydrogen that had been bubbled rapidly through water maintained at 70°. The resultant grain size after decarburizing was approximately ASTM 5. Several stress-strain curves were made of the decarburized niate-

Jan 1, 1950

By A. B. Dyes

In the operation of a water-driven reservoir, a free gas saturation can he established by maintaining production rates fast enough to cause the reservoir pressure to decline below the bubble point. The benefit of such a procedure on the displacement efficiency of the oil by water is illustrated for two types of sandstone samples from one reservoir. Those rock samples showing the poorest recovery to water drive in the absence of a free gas saturation give the most improvement in the presence of a free gas saturation. Employing one type of reservoir fluid (low .shrinkage) the benefit of evolved gas on oil displacement is calculated at several reservoir pressures below the bubble point. This demonstrates the presence of air optimum pressure for water displace,rnent which is .several hundred pounds per .square inch below the bubble point. Displacement of oil at the optimum pressures results in the removal of 7 to I? per cent more oil than would be obtained by displacement at the bubble point pressure. In some instance. this magnitude of increase may be worthy of consideration in establishing the maximum efficient rate of production from many water-driven fields. INTRODUCTION For many years the belief that the use of gas could be combined with that of water to result in a better recovery operation than the use of either of these phases alone has been prevalent in the oil industry. This is evidenced by the several field trials which have employed the injection of gas and water in combination.1.2.v In most cases the small amount of any additional recovery, in combination with the limited knowledge available on the older reservoirs, has left uncertain the influence of gas on recovery in these earlier attempts to combine the use of gas with water. Research studies in recent years have demonstrated through laboratory. floods the magnitude of the benefit of the presence of gas on the displacement of oil from sandstones by water.5,6,7,8,9,10,11 In addition, studies of the distributions of the phases which are present during the displacement process have developed concepts concerning the mechanism by which this benefit is obtained."." It now remains for the engineer to incorporate these findings into the general technology of reservoir operations. It is the purpose of this paper to illustrate that the production of a water-driven reservoir at pressures below the bubble point is one such operation whereby improved oil displacement efficiency can be obtained as a result of gas evolution. The establishment of a gas saturation by evolution of dissolved gas was one of the techniques used by several investigators in the laboratory studies. The possibility of obtaining the benefit of gas evolution in water-driven reservoirs by producing at pressures less than the bubble point has 3150 been pointed out previously." The desirability of this operation has undoubtedly

Jan 1, 1955

By J. B. Chatelain, M. F. Dufour

FLUID jet mills, employing a compressible fluid to grind materials to the subsieve range, was developed in the early 1930's, and the subsequent acceptance of these units was the result of their ability to pulverize solids that, because of physical properties, could not be processed by other attrition methods, such as ball, pebble, and hammer mills. Also, the fluid energy pulverizer is the only grinding device that will discharge continuously a 5-micron or smaller product. Simultaneous ultra-fine grinding and classification is the widest application of this unit. Jet mills may be used to advantage to reduce particle size of solids suspended in liquids, for coating one material with another, and effecting chemical reactions and changes in physical characteristics other than a reduction in size. Materials that can be processed by this grinding method include nonmetallic and metallic minerals, ores, metals, pigments, insecticides, fungicides, pharmaceuticals, plastics, dyes, and numerous other organic and inorganic products. Grinding principles utilized in the fluid mills available on the market are basically the same, the major difference being in the shape of the, grinding and classification chamber. Grinding in fluid jet pulverizers is accomplished by collisions between particles of the material being ground with the energy being supplied by compressed fluids entering the grinding chamber at high velocities. The "Micronizer" is a fluid energy mill employing a relatively flat cylindrical grinding chamber. Fig. 1 shows general construction details. The mill shown is equipped with a venturi type feeder using a compressed fluid to inject the feed into the grinding chamber. The energy consumed in forcing the feed into the grinding chamber against the mill pressure is, in some cases, as much as 40 pct of the total required for processing. Recent improvements, using a compression screw feeder as shown in Fig. 2, can reduce this to 1 or 2 pct of the total energy requirements. Grinding Grinding, as carried out in the. Micronizer involves the action of gaseous jets emerging from nozzles located in the peripheral wall of the grinding chamber. The axes, of the jets are tangential to a circle of smaller diameter than the grinding chamber as is shown in Fig. 1, and the gases entering the chamber maintain a high rotational velocity. The feed introduced into the mill is accelerated by the rotating gases and is thrown to the outside where a portion, coming in the zone of action of a nozzle, is further accelerated tangentially and inward. Violent collisions occur between the particles so accelerated and other particles circulating at a slower rate in a thin band near the periphery. It is estimated over 90 pct of the reduction in Micronizers occur as a result of impact within a fraction of an inch of the orifice. Observations also indicate that size reduction is independent of any interaction with the walls of the

Jan 1, 1952

By Stuart E. Buckley, C. R. Hocott

The viscosity of the oil in the reservoir is one of the properties that influence its movement through the sand to producing wells. Measurements of viscosity, therefore, are pertinent to problems associated with well behavior and with the estimation of recoveries, and afford an indirect means for partial evaluation of various methods of controlling reservoir behavior. The effect of dissolved gases on the viscosity of crude oil has been determined,ls2 but no data have been published on the viscosity of representative samples of reservoir oils. This paper describes a simple instrument that has been used to determine the viscosities of a number of subsurface oil samples at the temperatures and pressures existing in the reservoirs, and presents the results of the determinations for typical fields. Construction oF the Apparatus The principal requirements of any instrument used for the examination of subsurface samples are that it be strong and simple both in design and in method of operation. Accuracy beyond that of the degree of reproducibility of subsurface Sam-~les from various wells in a reservoir or exceeding that of the common measure-merits of reservoir temperatures and Pressures is not required. Because of the expense of procuring subsurface samples, it is necessary also that the instrument operate on a relatively small fraction of a sample, leaving the remainder for other tests, and that there be few or no failures of the equipment to cause undue delay or loss of a sample. After preliminary experiments with a falling bullet, the results of which were not satisfactory, a simple viscosimeter was built of the rolling ball type first proposed by Flowers3 and later used by several investiga-tor. 5.8 The apparatus consists essentially of a removable, accurately bored cylindrical barrel of 1/4-in. nominal internal diameter, 8 in. long, in which a closely fitting steel ball rolls through the oil with the barrel inclined at a definite angle. The ball makes contact at one end of the barrel with ail insulated electrode, closing an electrical circuit, which actuates a buzzer. The meas-urements consist essentially in determining the time required for the ball to travel the length of the barrel. The details of the construction are shown in Fig. I. The barrel in which the ball rolls was made from a section of 25-caliber blank rifle barrel, specially bored to an exact uniform diameter and polished. The barrel slides snugly into a hole bored in a solid stainless-steel cylinder, an upper external shoulder of the barrel compressing a small spring, and is held in place by a hollow nut. The spring prevents the barrel from seating against the bottom of the bored hole in the cylinder, while narrow external longitudinal slots in the barrel permit fluid to flow around it and through the bottom. The upper part of the recess in the steel cylinder is enlarged to form a tapered chamber, which acts as a reservoir for the oil and affords space for agitation to ensure

Jan 1, 1941

By G. W. Healy, J. C. Schottmiller

Molten silicates were found to exist in the Cr-Si-0 system at temperatures above 1450°C. one atom of oxygen is readily removed from CrzOs in the presence of Si02 at 1700°C, forming a silicate melt. Steam-hydrogen ratio measurements made at this temperature indicate that the free energy of the reaction: Cr20s(c) + Hz = 2CrO (in Si02 -saturated melt) + H20 is approximately 5600 * 1500 cal. A deep-blue chromous silicate, probably Cr2Si04, forms from these melts at about 1400" to 1500°C, and is characterized by.its distinctive X-ray diffraction pattern and optical properties—distinct pleochroism and high refractive indices. THE question of the state of oxidation of chromium in slags has vexed metallurgists for many years The experiments of Koerber and Oelsenl suggested the probable presence of divalent chromium in silica-saturated slags equilibrated with high-chromium melts. Hilty and coworkers2 had also found chromium at lower valency, as Cr304, in inclusions formed from oxygen-saturated Fe-Cr melts with as little as 10 pct Cr. In both cases, disproportiona-tion of the lower oxide to CraO3 and chromium was found to occur to a greater or lesser extent, depending upon the rate of cooling from the high temperature. The work on Cr304 was sufficiently detailed for chipmans to derive its thermodynamic properties, but Oelsen's experiments in the silicate system were not extensive enough since most of his runs were made with slags containing large amounts of manganese oxide in addition to iron and chrome oxide and silica. The present study describes experiments carried out to map out an approximate liquidus diagram in the CrzOs, "CrO", SiOa portion of the Cr-Si-0 system, and to measure the partial free energy of solution of oxygen in the system. EXPERIMENTAL 1) Approximate Melting-Point Determinations. Preliminary trials showed that when an equimolar mixture of Cr20s and SiOa was treated with hydrogen in the temperature range 1500" to 1600°C, copious amounts of steam were evolved, and a low-melting liquid formed which could be quenched to a blue, crystalline, material having a distinctive X-ray diffraction pattern. It was found that the identical material could be produced by heating intimately mixed, finely divided Cra03, Cr, and SiOa, held in a tungsten crucible, under purified argon. Thus, it was possible to prepare mixtures containing any desired proportions of chromium, silicon, and oxygen, pel-letize them, heat to temperature in the furnace shown in Fig. 1, and observe, after cooling, whether the pellet remained unchanged or showed signs of incipient, partial, or complete melting. 2) Free Energy of Solution of Oxygen. This was studied by measurement of steam-hydrogen ratios for the reaction: H20 (gas) + O (dissolved in charge) + Ha (gas) The experimental method chosen was to prepare a

Jan 1, 1964

By R. S. Shoemaker, F. W. McQuiston

SOUTH AFRICAN MILLING PRACTICE All modern South African gold plants operate primarily on the principle of exposing the gold particles in the ore by fine grinding and then cyaniding the total pulp. Although there are minor variations and occasional depart- ures from established practices among the fifty gold mines in South Africa, the normal plant operations proceed as follows. After removal of waste rock by hand sorting (15Y0 on average) the ore is crushed in cone crushers to minus 1/2 inch and then ground to approximately 75% minus 200 mesh by milling with either rod, ball or pebble mills as primary units and pebble mills for the secondary grind. Classification in both circuits is almost invariably conducted with 20" cyclones of 30" or larger diameter. Gravity concentration in the milling circuit followed by barrel amalgamation of the concentrates is practiced in 70Y0 of the plants, particularly where the ore grade is high. A slightly better overall recovery is obtained than with direct cyanidation, but additional handling is involved. Johnson cylinder s , plane tables or belt concentrators, all lined with suitable types of molded rubber riffles, are used for this purpose. At all mines, cyanidation is the main process, usually conducted by continuous treatment in Pachuca tanks and pulp separation with rotary drum filters. Cyanide solutions contain about 0.0 1570 NaCN and require a protective alkalinity of 0.02070 CaO. Precipitation of the gold from cyanide solution is exclusively by zinc dust and lead nitrate using the Merrill-Crowe system in conjunction with Stellar pressure filters. The zinc precipitate is smelted, generally after a preliminary concentration by sulfuric acid, in electric furnaces, mostly submerged arc types, with a silica and borax flux, yield- ing a bullion of 8870 gold, 9% silver, and 370 base metals. The gold content of the ore varies between 0.20 and 1.0 oz Troy per short ton and extraction efficiency ranges from 9570 to 9870. In general, 4070 of the gold output is recovered by amalgamation and 6070 by cyanidation; but in some cases, it is entirely by cyanidation. Flotation has not been adopted for gold extraction as it has not proved as efficient as cyanidation. It is, however, often applied to ores containing higher than 1% sulfur for the recovery of pyrite for sulfuric acid production. On the eastern side of the Witwaters rand Basin, "run-of -mine milling” was introduced in 1960 and in three of the four mills in this area both sorting and crushing have been eliminated. The ore received from the shafts is conveyed to storage silos and then fed by Williamson automatic feed controllers to pebble mills ranging from 12 to 14 feet diameter, and 16 to 20 feet long. The pebble mills operate in closed circuit with 42 inch cyclones and the slime produced is thickened and cyanided in the conventional manner. No selective

Jan 1, 1975

By W. I. Duvall, L. D. Sadwin

Three explosives with different detonation characteristics were tested by studying their cratering ability in a granite-gneiss. The strain wave generating characteristics of these explosives were also studied in the same rock medium. Correlations between the relative performance of three explosives as evaluated by crater studies and other methods of evaluation are indicated. Numerous test methods have been employed to evaluate the output performance of explosives; for example, the underwater explosion method, the airblast method and the ballistic pendulum method.'*' For blasting applications, the study of explosion produced craters and explosion generated strain waves are the most meaningful. This laboratory has employed these techniques extensively for many years and has shown that the detonation properties of explosives and their ability to generate strain waves in rock are related and that the amplitude and shape of the strain wave is related to some of the crater parameters such as slab thickness and fly rock velocity.3'11 However, a good comparison between the relative performance of explosives as determined by the crater and strain wave methods had not been made. The purpose of this investigation was to determine if the relative performance of three explosives as determined by the crater method shows a correlation with the relative performance as determined by the strain wave method. If a good correlation exists between these two sets of relative performance, it should then be possible to relate the detonation properties of an explosive to its ability to break rock in a crater test. In most commercial blasting operations, the diameter of the blast hole remains constant even though the type of explosive may change. In general, it is the explosive volume rather than the weight which remains constant when two or more explosives of different density are compared. Therefore all tests in this investigation were conducted on a constant volume basis rather than on a constant weight basis. TEST SITE AND ROCK PROPERTIES The tests described in this paper were conducted at a granite quarry owned and operated by the Consolidated Quarries Div. of the Georgia Marble Co. at Lithonia, Ga. The tests were performed in an area where the exposed rock surface was nearly horizontal and where the general rock mass had few joints or faults. The rock has an apparent sp gr of 2.6 and a longitudinal propagation velocity of 18,000 fps. The characteristic impedance of Lithonia granite gneiss is 53(lb - sec/in3). EXPERIMENTAL PROCEDURE There are many parameters which must be considered in the study of explosion-produced craters. The role played by each variable in the explosive-rock-crater system can be determined by experimental techniques in which one parameter is varied while others are maintained constant. In this investigation, the crater geometry was studied as the depth was varied for each of three explosives. The explosive volume and rock-type were held constant for all crater tests. The experimental arrangement used in performing the crater tests is illustrated schematically in Fig. 1.

Jan 1, 1965

By C. R. Hocott, Stuart E. Buckley

The viscosity of the oil in the reservoir is one of the properties that influence its movement through the sand to producing wells. Measurements of viscosity, therefore, are pertinent to problems associated with well behavior and with the estimation of recoveries, and afford an indirect means for partial evaluation of various methods of controlling reservoir behavior. The effect of dissolved gases on the viscosity of crude oil has been determined,ls2 but no data have been published on the viscosity of representative samples of reservoir oils. This paper describes a simple instrument that has been used to determine the viscosities of a number of subsurface oil samples at the temperatures and pressures existing in the reservoirs, and presents the results of the determinations for typical fields. Construction oF the Apparatus The principal requirements of any instrument used for the examination of subsurface samples are that it be strong and simple both in design and in method of operation. Accuracy beyond that of the degree of reproducibility of subsurface Sam-~les from various wells in a reservoir or exceeding that of the common measure-merits of reservoir temperatures and Pressures is not required. Because of the expense of procuring subsurface samples, it is necessary also that the instrument operate on a relatively small fraction of a sample, leaving the remainder for other tests, and that there be few or no failures of the equipment to cause undue delay or loss of a sample. After preliminary experiments with a falling bullet, the results of which were not satisfactory, a simple viscosimeter was built of the rolling ball type first proposed by Flowers3 and later used by several investiga-tor. 5.8 The apparatus consists essentially of a removable, accurately bored cylindrical barrel of 1/4-in. nominal internal diameter, 8 in. long, in which a closely fitting steel ball rolls through the oil with the barrel inclined at a definite angle. The ball makes contact at one end of the barrel with ail insulated electrode, closing an electrical circuit, which actuates a buzzer. The meas-urements consist essentially in determining the time required for the ball to travel the length of the barrel. The details of the construction are shown in Fig. I. The barrel in which the ball rolls was made from a section of 25-caliber blank rifle barrel, specially bored to an exact uniform diameter and polished. The barrel slides snugly into a hole bored in a solid stainless-steel cylinder, an upper external shoulder of the barrel compressing a small spring, and is held in place by a hollow nut. The spring prevents the barrel from seating against the bottom of the bored hole in the cylinder, while narrow external longitudinal slots in the barrel permit fluid to flow around it and through the bottom. The upper part of the recess in the steel cylinder is enlarged to form a tapered chamber, which acts as a reservoir for the oil and affords space for agitation to ensure

Jan 1, 1941

By L. J. Boucher

The beneficiation process at Northampton is described and reasons are given for installing a flotation plant. The economics of running the plant, the difficulties of operation, and subsequent remedial action are discussed. CEMENT rock from a quarry operated by the Northampton plant1, 2 of the Universal Atlas Cement Co. has a relatively low average CaCO³ content. To meet specifications required for cement manufacture it was formerly necessary, over succeeding years, to add increasingly larger amounts of high-lime, low-alumina rock, which was obtained from a quarry operated by the company at a point along the New Jersey-New York state border, 79 miles from Northampton. Previous to 1940, 8 pct of total kiln feed consisted of high-lime rock. From 1940 to 1943, this figure jumped to 13 pct. Today it would be necessary to use 18 pct of this high-lime to meet current specifications. Increasing transportation costs made this an expensive operation. In addition, this high-lime rock quarry was contaminated with granite and high magnesia pockets. As there was no available high-lime rock in the Lehigh Valley, it was decided in 1936 to install a pilot plant where experimental work was done on processing local cement rock with flotation and burning the resulting product in a small kiln. This plant was in operation for six months and at the end of that period a suitable method of flotation had been established. From these studies it was also found that if the proportion of shipped-in rock rose slightly above 10 pct it became economically advisable to use the flotation process. It is the object of this paper to present briefly the operation of the flotation system at the Northampton plant. It seems advisable to comment on the raw material used in this process. The Northampton quarry lies geologically in what is known as the Jacksonburg formation of Trenton limestone.' In Pennsylvania this extends in a southwesterly direction from Portland, through Nazareth, Bath, and Northampton and across the Lehigh River to Ormrod. This argillaceous limestone was formed from marine deposits laid down during the early Ordivician period when a shallow sea covered most of Pennsylvania. Carbonaceous matter in the original deposit formed graphitic carbon under later metamorphic forces. From this graphite the cement rock of the Lehigh Valley derives its dark color. Most of the graphite must be removed before lime flotation can proceed. The quartz in this rock is desirable from the chemist's point of view, as it furnishes him with a form of silica necessary in the calcining process, but its abrasive properties damage pumps and piping. Aluminum silicates of potassium, sodium, iron, and magnesium are found in the form of sericite. Cal-cite averages from 69 to 76 pct. Iron in the form of iron pyrites is also present and has no deleterious effect. Talc is present in minute quantities. The

Jan 1, 1954

By P. A. Tucker, C. R. Hudgens, D. E. Etter, D. L. Roesch, D. B. Martin

The equilibrium phase diagram of the Pu-Cd system is presented based on data obtained by differential thermal analysis, metallography, and electron-microprobe X-ray analysis. Liquidus temperatures range from 320° to 934°C. The system contains one congruently melting compound, PuCd, (945°C), and three incongruently melting compounds, PuCd, (800°C), PuCd, (730°C), and PuCd11 (410°C). A liquid-miscibility gap extends from 2 to 60 at. pet Cd with the monotectic reaction isotherm at 910°C. INTEREST in the potential use of plutonium alloys as reactor-fuel materials has prompted investigation of the phase equilibria in plutonium binary systems. A cursory investigation of the phase equilibria in the Pu-Cd binary system was conducted by differential thermal analysis (DTA), metallography, and electron-microprobe X-ray analysis (EMX). Extensive solid solubility of cadmium in both e and 6 plutonium was predicted1 based on atomic radii and electronegativities. Liquid immiscibility between these two elements was also predicted based on Mott's extension of Hildebrand's method. In the only previous investigation of the Pu-Cd system,2 two intermetallic compounds, PuCd11 (incon-gruent melting point 406°C) and PuCd8, were identified. EXPERIMENTAL The plutonium metal used in this work had a total impurity content of 500 ppm; the major impurities were: carbon (215 pprn), silicon (75 ppm), iron (60 ppm), nickel (40 ppm), and aluminum (25 ppm). The cadmium was reagent grade with a purity of 99.99 pet. The DTA technique for the study of plutonium alloys was previously described in detail.3 The alloys to be studied were prepared in tantalum DTA specimen capsules which were sealed by inert-gas welding. The alloys were homogenized in the liquid state in these sealed capsules which prevented the loss of cadmium by vaporization. Only the thermal arrests in the DTA heating curves were used to define the transformation temperatures of the system since supercooling affected many of the results during cooling. After the alloys were analyzed by DTA, the same alloys were used for the metallographic studies. Metallographic examinations were conducted in the manner described for plutonium alloys., No reaction was detected between the alloys and the tantalum capsules. Alloys for EMX analysis were placed in metallographic mounts together with specimens of unalloyed plutonium and cadmium which served as standards. The samples were highly polished but unetched. No protective coatings were applied to the surfaces of these radioactive specimens. Such coatings are detrimental to the excitation conditions and have been found to be unnecessary for the control of radioactive contamination. RESULTS The results of the DTA studies are presented in Table I. The phase diagram, constructed from these data plus the metallographic and EMX results, is presented in Fig. 1. The congruently melting compound, PuCd2, was identified by the occurrence of a maximum melting point (945°C) at 33.3 at. pet Pu-66.7 at. pet Cd and by the presence of a single phase in this composition.

Jan 1, 1965

By J. S. McNeil, J. U. Messenger

In the drilling of oil wells the control and prevention of lost circulation of the drilling- fluid is a oroblem which is frequently encountered; in many cases existing materials and methods for alleviating this condition have not been adequate. For severe cases of lost circulation in which the simpler methods, such as application of various bridging materials to the mud system, have proven unsatisfactory. a new material and method for applying to the loss zones have been developed which appear to he superior to existing techniques in many respects. The material, called a clay cement, is capable of being handled as a drilling fluid after initial mixing of the solitl ingredients with water and may be pumped down the drill pipe and squeezed into loss zones. After a short period, the material develops a very high gel strength which seals off the zone against further losses of the drilling fluid. In field tests, the process has been demonstrated to be a very effective method for combatting lost circulation. INTRODUCTION Methods of treating lost circulation in rotary-drilled wells by the addition of special materials to drilling fluids have long been in the process of development and are continuing to improve.' However, the annual drilling costs which can be traced directly to lost circulation difficulties still run into the millions of dollars. The loss of mud materials into highly permeable zones may range up to $50,000 per well in some areas. In addition to mud costs, excessive requirements of casing, cement; rig time, and the attendant blowout hazards further emphasize the importance of the need for improved methods of combatting lost circulation. The shortcomings of presently-used materials and methods have led to the development of a new lost returns material in the form of a time-setting clay cement. In field tests this material has proven very successful in plugging off loss zones. which other more conventional materials had failed to do. REVIEW OF PRESENT CORRECTIVE MEASURES The proper control of such operating factors as pump pressure, clearance between pipe and hole, and speed of running pipe in a holez is of primary importance in preventing and minimizing lost circulation problems. These factors, however, concern matters of drilling technique and do not directly involve lost circulation materials. Aside from setting casing past loss zones, three principal methods are generally employed for the purpose of avoiding or combatting lost circulation: (1) adjustment in properties (principally density) of the drilling fluid, (2) addition of fibrous, flaky, granular or other types of bridging materials to the mud system, and (3) the application of cements to the loss zones. The latter method is usually employed only after the first two have proven unsuccessful. In Table I are listed some advantages and disadvantages of the common corrective measures. Frequently, a combination of bridging material and cementing material is used." This combination is based on the premise that a bridge will

Jan 1, 1952

By W. C. Ellis

Growth directions of tin, zinc, and cadmiun whisker crystals grown spontaneously fi-om the solid are summarized. In tin the edge and diagonal directions of the unit cell are jound with the exception oj- the [110] diagonal. In cadmiurn and zinc the usual dip-ections are a or a + c. The c direction has not been ohserwed. The gvouth directions from the solid are for the most part the same as those found for vapor-grozun crystals and are the ohserz:ed glide directions in plastic j-lou. Whisker crystals of these elements grown from the solid are not twinned. Specular lateral reflections are associated with planes of snall crystallographic indices. WHISKER crystals of tin, zinc, or cadmium grow spontaneously at room temperature in periods from months to years from thin electroplates and other prepared films of the respective metals.''2 It has been established that these crystals are single, but the question of twinning, such as occurs in whisker crystals of silicon,3'4 has not been resolved. Studies of morphology have been restricted to determinations of growth directions.5-' Whisker crystals are both straight and kinked. A few studies have been made on kinked whiskers including measurements of kink anglesa and determinations of growth directions,' but unfortunately not both on the same crystals. The kink angles, for the most part, for each species are grouped closely about a few unique values, but these values are not always those between observed growth directions in a single crystal. To supplement existing data, the growth directions, identification of lateral features, and presence or absence of twinning were determined with a Weissenberg goniometer by a method described elsewhereg on eight whisker crystals of tin, five of zinc, and five of cadmium. One kinked cadmium whisker was examined in detail. The specimens were needlelike, a few microns in cross section, and of the order of a millimeter in length. They were removed from electroplated substrates on laboratory specimens and commercial equipment after several years of growth as described in Table I. Since the specimens were less than 10 p in cross section they were ideally strong with no attendant risk of plastic deformation or damage in handling. Only deformation twinning has been reported for these elements. Therefore, twinning probably should not be expected in whisker crystals of these metals, particularly a twin plane containing the growth direction. A twin plane oriented in this direction was the one sought in this study. No examination was made for twinning at the boundary between kink segments except for one cadmium crystal. Well-defined reflections occur as a whisker crystal of tin, zinc, or cadmium is rotated about its growth direction when illuminated by a beam of light Although these reflections had been noted in earlier investigations, no study of them was made, probably because the earlier studies had disclosed also that

Jan 1, 1967

By J. D. Price, W. M. Bertholf

One of the chief difficulties with which the operator of a coal washing plant has been forced to contend is the handling of the very fine coal. First he has the problem of separating the fine coal from washery water. This is usually accomplished by the use of settling cones or Dorr thickeners: in either event the separated fine coal contains a high amount (40 to 80 pct) of water and, somewhat loosely, dependent upon the size of the coal particles present, may be known as sludge or slurry. His second problem is the satisfactory further dewatering of such separated sludge and/or slurry. At the coal washing plant of the Colorado Fuel and Iron Corp., washed coal from the Deister Plat-O tables is sluiced to a stationary inclined de-watering screen provided with 3/16 by 1-in. slots, and the coarse coal passing over this screen is conveyed by a Baum-type elevator and a flight-type distributing conveyor to a battery of Carpenter centrifugal driers. The fine coal and water passing through the openings of the primary dewatering screens, plus the fine coal passing through the screens of the centrifugal driers (and no small portion of which is the result of the disintegrating action of these driers) is pumped to two 30-ft Link Belt settling cones. The sludge recovered as underflow from these cones was formerly dewatered on stationary screens having 1/16 by 1-in. slots and discharged on top of the coarse washed coal in the Baum drainage conveyor; but after a relatively few hours of op eration the circulating load of fine coal on this conveyor built up to a point where it became necessary to reduce the quantity of feed to the washing tables. The original arrangement of our coal washing and dewatering equipment is shown in Fig 1. In order to regain the loss in active throughput which had been caused by this circulating load, an installation of six vibrating filters was made during the year of 1936. This resulted in an increase in normal tonnage of washed coal from 1430 to 1750 tons per 8-hr shift, a gain of slightly over 22 pct. This increase in throughput has made a very substantial decrease in the " conversion cost" per ton of washed coal. Since the vibrators were installed, we have gained about 2,000,000 tons in production, compared to what would have been produced in the same number of shifts at the former rate. Putting it in slightly different form, we have saved in the past 12 yr the cost of 1400 operating shifts in the washery. Fig 2 shows the location of the vibrating filters as applied to the original flowsheet. It will be noted that the sludge from the bottom of the settling cones is passed through a distributing box and thence to the filters. The de-watered coal from the filters is de-livered to the conveyor receiving the dried coal from the Carpenter driers.

Jan 1, 1950

By M. H. Mueller, P. A. Beck, W. P. Chernock

HARRIS introduced the term inverse pole figure for the diagrams previously used by Barrett' to represent the volume fraction p(a,ß) of material in various orientations with respect to the fiber axis in a specimen with fiber texture. The direction of the fiber axis with respect to the crystal lattice is specified by the two independent angle variables a and ß. In such a diagram p gives the fiber axis density distribution over the various crystallographic directions. The p(a,ß) may be given in a two-dimensional diagram by means of contour lines (p=con-stant) in a stereographic projection. The inverse pole figure incorporates in a single contour line diagram all the information given conventionally in pole charts for various (hkl) reflections and, therefore, it represents a considerable degree of condensation. Also, it gives this information directly in terms of the volume fraction of the specimen in various orientations, and it obviates the necessity of referring back and forth between the various pole charts in an attempt to interpret them in terms of orientations. Inverse pole figures undoubtedly represent the most adequate method for describing a texture in a quantitative manner and, at least in the case of fiber textures, this method is certainly a practicable one. Harris described1 a simple procedure for determining at least the rough outlines of a quantitative inverse pole figure. This method depends on the measurement of the intensity of X-ray reflections from various (hkl) planes lying parallel to the same specimen surface. In the case of a rod, reflections from a plane specimen surface perpendicular to the rod axis (fiber texture axis) are to be used. Harris has shown that the measured intensities I,,, reflected by crystal planes (hkl), aligned perpendicularly to the fiber axis of a specimen with unknown fiber texture, and the corresponding intensity Iu nkl from a random specimen are related to the p(a,ß) value for the unknown texture by the following equation IAkl/I°Aklw=c/c°.p(a, ß) [1] where C and C° re parameters depending on the crystal imperfections (extinction), surface preparation (e.g., thickness of oxide layer), the absorption coefficient in the specimen, effective line breadth, and instrumental factors. The values of the variables a and ß1 defining the crystal orientation, depend only on the indices hkl of the reflecting plane perpendicular to the fiber axis. Since p, as described by Harris1, is normalized in such a way that upon integration over the total orientation range its mean value is 1, the parameter C/C may be calculated approximately by the summation of Eq. l over all available X-ray reflections hkl, corresponding to a set of discrete orientations (rather than by integration over the complete range of orientations represented by the continuous variables a and ß). From the summation of Eq. 1 1/n SI AKL/I° Akl = C/C. SP(a,ß)/n is obtained where, as stated above 2p(a,ß) =1. n Therefore

Jan 1, 1959

By G. D. Gemmell

Effects of solid-sdutidn alloying with titanium, molybdenum, and tungsten at concentrations up to 10 pct on the strength of pure columbium at elevated temperatures (mainly 2000°F) have been investigated by means of creep-rupture, hot-tensile, and hot-hardness testing and recrystallization studies. ThIS paper presents some results from the initial part of a study of the effects of alloying on the high-temperature strength properties of columbium. The elevated-temperature strength characteristics of pure columbium were first studied. Binary alloys of columbium with titanium, molybdenum, and tungsten containing 1, 5, and 10 pct of the solute elements were chosen on the basis of their high melting points, their known solid solubility in columbium, and results of separate oxidation-resistance studies of columbium alloys. EXPERIMENTAL PROCEDURE All the materials used were of highest purity. A typical analysis of the columbium is shown in Table I. Compositions of the alloys are also given in Table I. To evaluate the strength properties of pure co-lumbium and the alloys at elevated temperatures, creep-rupture, hot-tensile, and hot-hardness testing was done on recrystallized material. To prepare the pure metal and the alloys for these tests, 1- 1b buttons were made in a water-cooled copper crucible, inert atmosphere, tungsten arc furnace. Tapered ingots, 3 in. long, were made from these buttons by a skull-casting technique and these were machined to 1/2 in. diam, swaged to 50 pct reduction (pure columbium at room temperature, alloys at lowest temperature possible without cracking, generally in range 1100" to 1800°F) and heated in vacuum (lo-' mm Hg) for 16 hr at 2550°F for re-crystallization and homogenization. The resulting grain diameter was 0.1 to 0.3 mm. The 10 pct Mo alloy casting was not successfully swaged at temperatures up to 1800°F without cracking and was not included in the test program. Creep-rupture testing was done at constant load in vacuum on cylindrical specimens of 0.16 in. diam, using Instron capsules. The pressure at test temperatures was less than 10-1 mm Hg. Hardneas readings taken on the test specimen before and after testing were used as a check on possible gaseous contamination. Hot tensile tests in vacuum on cylindrical specimens of 0.125 in. diam were also made with Instron equipment at a strain rate of 0.067 min.-l. Hot-hardness measurements were taken with a unit constructed at the Du Pont Experimental Station. The test piece, supported on an alumina anvil, and the molybdenum indenter shaft with sapphire tip is heated in a platinum-wound furnace. The load applied to the pyramid indenter is measured by strain gages attached to a proving ring located outside the hot zone. In the measurements reported here the load was I kg. The tester operates in a vacuum of about 10"5 mm Hg and is capable of temperatures up to 1400°C.

Jan 1, 1960

By Hugh H. Waesche

High quality quartz crystals weighing more than 50 grams are required in several important industrial applications.30,31 Primarily, they are the basic raw material for precision, electronic, frequency control components; this includes oscillators and filters in both radio and telephone services. Quartz crystals are also necessary for optical lenses and prisms in special applications requiring high ultraviolet light-transmission as in spectrographs. Quartz wedges are regular components for petrographic microscopes. The application of crystalline quartz as a transducer* in ultrasonic devices has increased in recent years despite strong competition from barium titanate and magnetostrictive [f] devices. Some quartz is fabricated into delay lines for radar. Man has valued quartz for fabrication of art objects since the dawn of history. The art forms were and are painstakingly carved and polished to form intricate figurines, bowls, statuettes, and the well-known crystal balls. The largest known ball, made of perfect quartz from Burma, is now in the National Museum in Washington. It is 12 7/8 in. in diameter and weighs 106 lb 12 oz. Clear, pure quartz chips and small crystals not meeting the electronic-grade dimensional requirements are known by the Brazilian term lasca. They are used to produce fused quartz having wide application in laboratory equipment, as special glasses, for torsion suspension in scientific instruments, and as a source material for growing large artificial quartz crystals 18,35 Electronic applications far exceed all other uses in importance so any discussion of high-quality quartz crystals must be concerned almost exclusively with those functions. Historical Background Because of their ubiquitous character and natural beauty, quartz crystals have long been of interest and known to man. They have been found among early Egyptian and Chinese art forms and the Sumerians are believed to have fashioned seals, beads, and other jewelry from quartz crystals, perhaps 5,000 years ago. Also, American Indians made arrow heads and fashioned some simple objects of different kinds. The origin of the name quartz, although of Greek derivation, is uncertain. The Greeks appropriately applied their word for frozen water or ice, krustallos, to quartz. The present-day, large-scale practical applications of quartz crystals began in 1880-1881 when Pierre and Jacques Curie reported discovery of the "piezoelectric" effect. They found this effect first in Rochelle salt, a common product of grape-wine refineries, while studying crystal symmetry. Piezoelectricity is that property found in certain crystals, including quartz, whereby electrical charges of equal and opposite sign appear on opposite parts of the crystals when they are stressed. If equal and opposite forces are applied to two opposing prism edges of a single untwinned quartz crystal a positive electrical charge will appear on one edge and a negative charge on the other. The amount of the charges will be directly proportional to the force applied. This property seems to be intimately related to pyroelectricity

Jan 1, 1960

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675' and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946