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By G. Richards Gwinn

Graphite is one .of the so-called minor nonmetals that have become of major importance during the present conflict. Requirements of the domestic industry for graphite are relatively small and uses have changed so greatly in the past 25 years that different types, with few exceptions, are more nearly interchangeable in use. However, the quality of the graphite required for crucibles is exacting and under present manufacturing practices only a small part of the world production can be utilized economically by this industry. Graphite, for the domestic crucible industry, was supplied almost entirely by imports from Madagascar and Ceylon before the present war. The quantity required has been increased by the war and the greatest demand is for Madagascar flake. The fall of France to Germany in 1941 and the Japanese expansion southward threatened our supply of crucible-grade graphite, therefore the domestic industry was revived to supplement imports and to act as insurance in the event of complete stoppage of imports. Two plants were constructed for the Government, one at Ashland, Alabama, called the Crucible Flake Graphite Co., operated by Haile Mines, Inc., and one near West Chester, Pennsylvania, operated by the Benjamin Franklin Flake Graphite Co. Loans were made by the Reconstruction Finance Corporation to the Alabama Flake Graphite Co. at Ashland, the Ceylon Graphite Co., at Goodwater, Ala., and the Southwestern Graphite Co., at Burnet, Texas. However, by the end of 1943 the import situation had improved and it was no longer necessary to continue Government assistance to mine and stock-pile the high-cost domestic material. Graphite is found in virtually every country of the world. Most occurrences are of no economic importance because of their poor quality, prohibitive mining and milling costs, inaccessibility, and poor location with reference to the industrial centers where graphite is used. The principal commercial deposits are found in Ceylon, Madagascar, Chosen (Korea), United States, U. S. S. R., Canada, Germany, and Mexico. Graphite is a typical international mineral in that it is utilized mainly in countries noted for industrial activities, whereas the two islands, Ceylon and Madagascar, which produce the major part of the world's high-grade graphite, are virtually devoid of any manufacturing establishments requiring its use. The industry thus is violently disturbed by wars. Types oF Graphite Used in Crucibles Graphite of various kinds and from many countries has been used for making crucibles. Passau (Bohemian) flake was first used in Europe, but by the middle of the seventeenth century crucible formulas were established largely on Ceylon graphite and German Klingenberg clay. Ceylon graphite is granular and the grains are subdivided into more or less

Jan 1, 1948

By W. C. Hauber

Techniques previously published to predict the production performance of a water flood when the mobility ratio is not unity have been primarily restricted to a five-spot well pattern. When other types of well patterns are considered, the prediction of performance has required either a model study or a complex numerical solution of a multiple-fluid system with a high-speed digital computer. Simple methods are developed in this report for predicting the areal sweep efficiency and injectivity history of a water flood for arbitrary well patterns and mobility ratios. The effect of an initial gas saturation can be incorporated into this method of prediction. With the layer superposition concepts published by Prats, et al.,1 these methods can be used to predict the production performance of a water flood in a reservoir having a wide range in permeability. A reasonably good agreement is shown by comparisons of the results calculated by this method with those obtained either by model studies or by complex numerical solution of multiple-fluid systems. Therefore, it has been concluded that a reasonably accurate method has been developed for predicting the production performance of a water flood employing an arbitrary type of well pattern for any given mobility ratio. A medium-speed digital computer can be used in applying this method. INTRODUCTION Production performance of multi-fluid five-spot water floods can be predicted by the techniques published by Prats, et al.1 This technique takes into account the effects of initial gas saturation, mobility ratio and vertical variations in horizontal permeability. A basic assumption in applying this technique is that unit displacement efficiency does not vary with time after the passage of the flood front. Prats, et al. demonstrated that this assumption is valid for normal waterflood applications with small mobility ratios. To extend Prats' technique to other types of well patterns has required either an experimental model study or a numerical solution of a multiple-fluid system to describe the performance of an individual homogeneous layer. Sheldon and Dougherty2 presented an exact numerical solution employing any arbitrary well pattern. This technique is complex to apply, requiring (1) numerical solution of the single-fluid system, (2) conformal mapping of the streamlines and iso-potential lines to form a new grid network, and (3) a numerical solution of the multi-fluid system on the new grid network. A method was developed in this paper to approximate areal sweep efficiency and injectivity as functions of time for an individual homogeneous layer for arbitrary well patterns and mobility ratios. Analytic expressions were derived to directly apply this method to five-spot and direct line drive well patterns. For other types of well patterns, this method is similar to the approach of Higgids and Leighton,6 in that it utilizes the stream tubes and iso-potential lines obtained by the solution of differential equations when the mobility ratio is unity. However, this method is easier to apply than the Higgins-Leighton method since it does not require knowledge of the variation between oil and water relative permeabilities and saturation. Using the relationship between areal sweep efficiency, injectivity and the volume of water injected into an individual homogeneous layer as obtained by the method presented in this paper, and Prats' technique for the superposition of individual layers, one can predict the production performance of any water flood. ASSUMPTIONS GENERAL Basic assumptions made in this report are that fluids are incompressible and the layers are horizontal, homogeneous and uniformly thick. It is assumed that as water is injected into the layer, three distinct regions are formed —a water bank, an oil bank, and an unflooded region. Each region is assumed to displace other regions in a pis-tonlike manner, with only one fluid flowing in each region, so that there is no change in unit displacement efficiency with time after the flood front has passed in the reservoir. Therefore, the residual oil saturation in the water bank and the oil saturations in the unflooded region are constant throughout the layer. The ratio (F) of the bulk volume of a layer occupied by the oil and water banks at any time before oil breakthrough, to the corresponding bulk volume of a layer occupied by the water bank, is given' by the equation BREAKTHROUGH AREAL SWEEP EFFICIENCY To predict the behavior of any type of waterflood pattern, one must know the breakthrough areal sweep efficiency Eb(Mc,o, F) for the pattern for any water:oil mo-

Jan 1, 1965

By H. B. Fuqua, B. E. Thompson

The area discussed herein, commonly known as the North Texas district, embraces the following 10 counties: Archer, Baylor, Clay, Cooke, Foard, Hardeman, Knox, Montague, Wichita and Wilbarger. It is underlain by two major structural features. The northernmost portion of the district, including Cooke, Montague, northern Clay, Wichita, Wilbarger, Foard and Hardeman counties, is underlain by the system of buried mountains known as the Red River uplift, which is parallel to and closely related to the Wichita-Amarillo uplift of Oklahoma and the Texas Panhandle. While the presence of a great majority of the numerous oil fields of the area is traceable to this feature, the production in Archer, southwestern Clay and southeastern Baylor counties is due to the influence of what is known as the Cisco Arch (so called because of its influence on Cisco deposition), the axis of which extends in a northwest-southeast direction across Archer County. It has been impossible for the authors to isolate the statistics for production for each of the many small pools of this district, as such statistics are not kept by the operators except for the district as a whole, therefore Tables 1 and 2 are comparatively short. The number of wells

Jan 1, 1935

BECAUSE it is necessary that the powders made for casting have a magistery of salt water, I wish now to teach you to prepare the salt that must form this magistery, for without it these powders would not have the toughness to hold themselves together when they are dry. In short, you take the quantity [119v] of salt that you need to prepare and put it in a rough pot, either baked or, if it suits you better, raw but well dried. This is completely covered with a lid or is luted with well- made moulding clay. Then it is encircled with brick ends at a distance of three dita, like a drying furnace. This space is filled with good charcoal; fire is applied and it is left to stand until all the charcoal is consumed by itself* Then you take that quantity of this burned or rather melted salt which you wish to use for moistening the clay and which you think can be dissolved in the water so that it wd remain very salty. It is boiled in a pot with water and then left to stand. After it has settled, your powder is moistened with it and used for moulding. When you see by testing it that the powder stands up as you wish, it is good. If not, give it some more of this water again and continue until you see that it holds enough. For without this magistery it would return to the dryness that it had before as a powder, and you could not use it without fear that it would fall from the Games. In this way this earth, either natural or artificial, is prepared and made ready, and it is used as the need occurs.

Jan 1, 1942

By Theodore Simons

During the last half century a great amount of ingenuity and energy has been devoted to the invention of appliances for the recovery of valuable minerals from very fine sands and slimes. The reason for this is that in almost every dressing plant the greatest losses of values, considered relatively as well as absolutely, occur in the treatment of slimes. The natural aim of mill operators to minimize these losses has in recent years received another impetus, from the fact that the gradually diminishing occurrence of high-grade ores makes a more intense recovery of values from existing resources absolutely necessary for profitable operation. The results of such attempts are found in the appearance of a great number of machines and appliances which make it profitable to-day to rework old clumps, containing the tailings of older processes. A constantly growing difficulty of obtaining skilled labor and the increase in wages made it prohibitory to employ those types of machines which required much attention, and in the middle of the ninieteenth century the various concentrating tables of the percussion type, which automatically discharge their products, began to take the place of the intermittent tables, on which, when the bed had reached a certain thickness, operation had to be stopped in order to allow the skimming by hand of the separate layers formed on the table. In the course of years, two general types of machines evolved for the treatment of fine sands arid slimes: The so-called concentrators and vanners, on the one hand, and the buddles and round tables on the other.' For the profitable treatment of the very finest slimes, round tables have as a last resort proved more satisfactory and econoillical than other machines. In recent years they have agaiu become the subject of close inves-

Jan 1, 1914

By D. J. Carney, J. Chipman, N. J. Grant

G. Derge—With the development of this last weapon, there is not much of a chance for hydrogen. It is certainly a very interesting paper, and it gives us more confidence in sampling liquid steel for hydrogen than we have ever had before. This satisfactory work gives considerable confidence to all of the chilled methods of sampling which should be more or less successful depending upon the degree of chilling obtained. J. T. MacKenzie—How do you handle a nonmagnetic specimen in that device? D. J. Carney (authors' reply)—I left that out in going over the analytical procedure. For the 18-8 steel, what was done was to get some iron wire which was degassed. One turn of wire was made around the sample; it was inserted into the analytical apparatus, and that was enough to allow the magnet to pull the sample and drop it in the furnace. Other methods could be devised for this apparatus to do the same thing. This was just a quick method. C. E. Sims—This method of sampling and analysis is very ingenious, and the results obtained attest to a satisfactory degree of accuracy. It was noted in the paper that the samples are satisfactory only when there is a complete absence of pipe. This should be empha- sized, particularly in view of the fact that they are cut off under water. Some reservations are held in regard to the adequacy of the method of sample storage prior to analysis. Cooling on dry ice undoubtedly slows down the rate of diffusion to a marked degree, and it obviously suffices when the analysis is made within a few hours. All of the samples, except some of high-nickel steels, were analyzed within 12 hr. It is still unknown how long this method would be safe. In the work at Battelle Institute, it was impracticable always to start analysis within 12 hr for various reasons. Some samples did not reach the laboratory for several days, and some were held as long as a month before analysis. During this period, they were held over mercury, and the gas evolved at room temperature was collected and analyzed. It should be mentioned that both the mercury and the container must be kept very clean.

Jan 1, 1951

By P. A. Beck

In the course of work on grain growth in high purity aluminum a simple optical method was developed for detecting the presence or absence of preferred orientation in annealed specimens. The specimens were prepared by grinding, polishing and "deep etching." The etching reagent used for high purity aluminum has been described.* The resulting etch pits produced selective

Jan 1, 1949

By D. V. Carter, D. C. Williams

Four oil discoveries were made in east and east central Texas during 1940, three of which represented new fields. In the Chapel Hill field, Smith County, oil was found where formerly only gas and distillate were produced. The three oil fields discovered are: Hawkins, Wood County; Pittsburg, Camp County; and Tehuacana, Limestone County. Important extensions were made to the following fields: Bazette, Navarro County; Long Lake, Anderson and Leon Counties; Cayuga, Anderson, Freestone and Henderson Counties; Opelika, Henderson County; and Talco, Titus and Franklin Counties. At the close of the year 54 oil and gas fields were producing in the district. There were 13 other fields, 11 oil and 2 gas, which have been abandoned. The East Texas field led the district in the number of completions for the year. During the year about 622 wells (oil and distillate wells included) were completed and 80 wildcats were drilled. Production and Proration During the year 170,424,685 bbl. of oil (distillate production included) were produced in the district—a decrease of 2.6 per cent from the 175,053,729 bbl. (distillate production included) during the preceding year. The district's production for the year 1938 was 182,369,484 bhl. As usual, most of the district's annual production was in the East Texas field, which produced 139,095,694 bbl. (distillate production in- cluded) during 1940, or 81.6 per cent of the total oil produced as compared with 141,333,317 bbl. (80.7 per cent) for 1939. The December estimated daily average production in the district was 424,565 bbl. The district accounted for 34.9 per cent of the state's annual production, compared to 36.7 pcr cent of the state's 1939 production. The decrease in production for 1940 may be attributed to changes made in proration schedules. Any material changes in the district's annual production may be considered for the most part as a reflection of proration-schedule changes affecting the East Texas field, since it is by far the most important field in the area. The entire state was subject to 71 shutdown days for the year; the East Texas field to 131; and the Rodessa field (Cass County, Texas, portion) to 5 days. No important changes were made in field rules and regulations during the year regarding the allocation of oil in individual fields in this district. Discoveries The Hawkins field is in southeastern Wood County in and principally north of the town of Hawkins. Development to date indicates that the field is somewhat of an elongated anticline trending slightly east of north and the proved oil area appears at this time to cover approximately 4000 acres. The oil production has been secured from the Woodbine sand, Upper Cretaceous; a considerable quantity of gas has been encountered in the Sub-Clarksville formation (Eagleford shale) in the higher part of the structure. It appears that a free gas

Jan 1, 1941

By D. C. Williams, D. V. Carter

Four oil discoveries were made in east and east central Texas during 1940, three of which represented new fields. In the Chapel Hill field, Smith County, oil was found where formerly only gas and distillate were produced. The three oil fields discovered are: Hawkins, Wood County; Pittsburg, Camp County; and Tehuacana, Limestone County. Important extensions were made to the following fields: Bazette, Navarro County; Long Lake, Anderson and Leon Counties; Cayuga, Anderson, Freestone and Henderson Counties; Opelika, Henderson County; and Talco, Titus and Franklin Counties. At the close of the year 54 oil and gas fields were producing in the district. There were 13 other fields, 11 oil and 2 gas, which have been abandoned. The East Texas field led the district in the number of completions for the year. During the year about 622 wells (oil and distillate wells included) were completed and 80 wildcats were drilled. Production and Proration During the year 170,424,685 bbl. of oil (distillate production included) were produced in the district—a decrease of 2.6 per cent from the 175,053,729 bbl. (distillate production included) during the preceding year. The district's production for the year 1938 was 182,369,484 bhl. As usual, most of the district's annual production was in the East Texas field, which produced 139,095,694 bbl. (distillate production in- cluded) during 1940, or 81.6 per cent of the total oil produced as compared with 141,333,317 bbl. (80.7 per cent) for 1939. The December estimated daily average production in the district was 424,565 bbl. The district accounted for 34.9 per cent of the state's annual production, compared to 36.7 pcr cent of the state's 1939 production. The decrease in production for 1940 may be attributed to changes made in proration schedules. Any material changes in the district's annual production may be considered for the most part as a reflection of proration-schedule changes affecting the East Texas field, since it is by far the most important field in the area. The entire state was subject to 71 shutdown days for the year; the East Texas field to 131; and the Rodessa field (Cass County, Texas, portion) to 5 days. No important changes were made in field rules and regulations during the year regarding the allocation of oil in individual fields in this district. Discoveries The Hawkins field is in southeastern Wood County in and principally north of the town of Hawkins. Development to date indicates that the field is somewhat of an elongated anticline trending slightly east of north and the proved oil area appears at this time to cover approximately 4000 acres. The oil production has been secured from the Woodbine sand, Upper Cretaceous; a considerable quantity of gas has been encountered in the Sub-Clarksville formation (Eagleford shale) in the higher part of the structure. It appears that a free gas

Jan 1, 1941

By G. Barbery

Since the original paper, two methods have been introduced to compute the parameters of the three parameter size distribution equation: [ ] Both of them are based on graphical means, which are time-consuming and of little statistical significance. A program has been developed, using the Gauss-Newton method to compute by nonlinear regression analysis the parameters of the equation. Although the method is quite general in curve-fitting applications, it does not appear to be used in the field of size analysis, and a brief description is given. As applied here, the Gauss-Newton method involves the minimization of the least squares: [ ] where n is the number of sieves used. The second member of Eq. 2 can be approximated by a multiple Taylor's series expansion of first order about a starting value [ ] The minimization of Q (r,s,Xo) means: [ ] Putting Eq. 3 into Eq. 2 and differentiating, we obtain a system of equations which can be represented in matrix symbolism (box) The system can be solved for: [ ] and the operations repeated with new values: [ ] The starting values for r and s are taken as 1, for Xo, a value higher than the maximum sieve opening value. Applied to the data given by Herbst 5,6 for batch grinding of 7 X 9 mesh dolomite, the parameters given in Table 1 were obtained. The discussion of the significance of the residual sum of squares is a difficult subject in multiple nonlinear

Jan 1, 1972

By Dwight K. Smith

A new pozzolanic composition has been developed for cementing oil wells where moderate to high temperatures prevail. This material is an entirely different concept to other oil well cementing materials, such as portland cements, cements containing additives, or liquid resins. Its characteristics are such that it is not, at present, recommended for use at temperatures less than 140º F. It can he either accelerated or retarded across a wide range of well conditions. This new cement is composed of a pozzolanic material, hydrated lime, and a chemical activator to give it early initial strength. This material can be used in wells from 6,000 to 18,000 or more feet where temperature conditions are similar to those along the Gulf Coast. This cement, when set, has no soluble portion subject to leaching or any compounds that should be attacked by sulfate waters or brines. For this reason, it should be permanent when placed adjacent to formations carrying any type of fluid. The compressive strengths in 24 hours are more than adequate for wells where temperatures are 140°F and higher. These values ore in excess of many other types of cementing composition presently in use in the field. This pozzolanic composition does not retrogress in strength at high temperatures as do some other types of cementing materials. The slurry weights of this material will vary slightly according to the specific gravity and water requirements of the pozzolnn itself. The materials covered herein will mix from 13.5 to 14.3 lb/gal, and will have a waiting-on-cement time comparable to other materials used under the same conditions. Economically speaking, this composition is less expensive than either portland cements or retarded cements presently being used under deep well conditions. INTRODUCTION Pozzolans are siliceous material which, though not cementitious in themselves, contain constituents which at ordinary temperatures will combine with lime in the presence of water to form compounds which have a low solubility and possess cementing properties. The use of pozzolanic materials dates back many hundreds of years and both the ancient Greeks and Romans were aware that certain volcanic deposits, if finely ground and mixed with lime and sand, yielded a mortar which possessed special properties. Generally, the early strengths of such materials were rather weak and were considered insufficient for modern commercial usages. Pozzolanic materials have been used extensively with portland cement in mass concrete to obtain special properties. In recent years, large quantities of certain pozzolanic materials have been used successfully admixed into portland cements for oil well cementing. Pozzolans, being reactive silicates, will combine with the free lime that is an inherent component of set portland cements and thereby. becomes cementitious themselves. POZZOLANS FOR OIL WELL CEMENTING There are many types of pozzolans, some of which are more reactive than others. The quality of the pozzoIan depends on the degree of reactivity, chemical composition, fineness, and other less well understood factors. Some of the more widely accepted pozzolans are those classified as fly ashes, while others are certain materials of volcanic origin. pozzolans which require large vol-

Jan 1, 1957

By K. A. Slagle, D. K. Smith

weight obtained. Additives used in conjunction with salt in these slurries have included silica flour, calcium ligno-sulfonate and cellulose retarders, granular lost-circulation materials, bentonite and selected low-water-loss additives that are not significantly deteriorated by the presence of the chloride ion. In some other areas of South Texas, the salt-saturated slurries have been used quite extensively for improvement of the flow properties of slurries and attainment of better circulation characteristics at lower displacement rates. Concurrently with this property, the protection of shales and shaly sands is also realized, as well as useful retardation of the slurry. Resultant superior cementing jobs have been indicated by both communication tests and acoustic logs for bonding to pipe and formation.' In one section of Louisiana, a major oil company has been using salt-saturated API Class A cement with calcium lignosulfonate retarder for cementing through the Miocene at 9,000 to 10,000 ft. This is another of the situations where interbedding of sands and shales exists, creating difficulty in maintaining formation competency when a fresh-water slurry contacts the clay minerals of the formation. Further work has also been done in the shaly Miocene formation at 13,000 to 15,000 ft where fairly close water or gas contacts are encountered. Indications thus far are that better segregation of these various fluids is obtained by use of the saturated salt slurries because of their improved formation bonding characteristics. In addition to the properties of salt in this situation, attainment of turbulent flow at minimum displacement rates has also been accomplished by use of an additive to help provide exceptional dispersion and viscosity reduction of the slurry. Another oil company was encountering considerable expense in completing wells in Southwestern Louisiana due to extensive block squeeze requirements for effective separation of zones. A very effective mud program was being used to minimize washout in the shale sections and, apparently, a nearly gauge-size hole was being obtained. However, primary cementing results with fresh-water slurries were generally poor. On a few occasions when slurry was actually circulated to the surface, large pieces of shale formation were brought out of the hole with the slurry, indicating a severely water-sensitive, sloughing formation. Inhibition of shale heaving was being accomvlished in the drilling program, and immediately indone ipon circulation of the fresh-water slurry even though it contained a low-fluid-loss additive to reduce filtrate damage in the sands. The subsequent change to salt-saturated slurry yielded 11 successful primary cement jobs out of 12, compared to the previous success ratio of practically zero. Since these were deep, high-temperature wells in the range of 13,000 ft with high-pressure zones necessitating 17.5-lb/gal fluid densities, the slurry used was API Class E cement, silica flour, weight material, retarder, salt saturation (which also reduced the amount of weight material) and maintenance of low fluid loss by use of a salt-compatible additive. Other salt slurries have been used to a limited extent in this same general area for similar problems at depths ranging from 5,000 to 17,000 ft. In the shallower wells, the cement has usually been API Class A where the salt functions as a retarder, and in the deeper wells API Class E cement is used with the additional salt advantage being its increased slurry weight and inability to dissolve salt stringers. A considerable number of squeeze jobs have also been done on older wells using the salt-saturated slurries with very good results. MID-CONTINENT In North Texas, salt-water slurries have been used for cementing the Woodbine sand, Strawn sand, KMA sand and Pettit lime. Shales surrounding these formations have created the same difficulty in obtaining separation of producing zones that has been the problem in other areas. Depths in this area range from 3,400 ft for the Strawn to 7,400 ft for the Woodbine, and concentration of salt has varied accordingly. In the deeper wells, where retardation is desired, saturated salt-water cement is used; for the shallower wells, in order to provide shorter waiting-on-cement times, the amount of salt has been 18 per cent by weight of the mixing water. Results have been excellent with no reported failures on any of the salt cement jobs; where acoustic bond logs have indicated indifferent bonds previously, they are indicating very good bonding for the salt slurries. In Oklahoma various shales of Pennsylvanian age exhibit a high degree of sloughing in the presence of fresh water, causing severe washouts above and below sand formations which it is desired to isolate. This situation exists to some degree in practically all parts of Oklahoma and includes formations of other ages such as the Wood-ford shale. For the past few years, salt-saturated cements and displacement rates as high as practical have been used as a remedy for this problem, with very good results. The Layton and Bartlesville formations are two examples of shaly sands where saturated slurries have been helpful. In one area where five wells were drilled through this type of problem shale without obtaining a satisfactory primary cement job, a change was made to salt-saturated cement preceded by a suitable chemical wash for the drilling mud involved. Acoustic bond logging indicated excellent bonding, and final completion bore out this result by being trouble-free. This type of slurry has also been used extensively on squeeze jobs where shales have been heaving around the producing formations. Predominantly, the basic slurry has been either API Class A cement or a pozzolan cement—although, as deeper wells are being drilled, the use of salt in Class E cement is also increasing. Salt cement in West Texas has been used primarily to help prevent channeling through the shales around the Delaware sand, Queens dolomite and Hope lime. Many of the shaly and dirty sands of this area are sensitive to the filtrate from a fresh-water cement. Salt at 16 to 18 per cent by weight of mixing water has been added to centent, and has been effective in controlling formation damage and communication between zones in these formations. Use of these lower salt concentrations is dictated in this area by the relatively low formation temperatures where retardation of the slurry would create unduly long waiting-on-cement times. Also, quite a bit of cementing has been done in this area using salt concentrations in the accelerating range— that is, 2 to 5 per cent by weight of water. Specifically, these concentrations have been used in coiljunction with high percentages of gel to overcome the retarding effect of the calcium lignosulfonate dispersant, although there are probably several shales where these concentrations could provide some degree of formation stability. On several occasions, the salt has also been used to lower the critical velocity or rate for turbulence with the slurry, particularly in the pozzolan cements. On wells in the Hope lime, it has usually been necessary to squeeze the shale above and below the lime to get a water-free completion. Use of salt-saturated slurries has largely eliminated this

By David A. Thomas, Eugene S. Meieran

MECHAMCAL, electrical, and other property measurements are often more easily made on wires than on sheets. In order to carry out transmission electron microscopy on the same material used for property determinations, we have developed a method for preparing thin foil specimens of wires. The technique was developed for 0.030 in. diam tungsten wires, and is a modification of the thinning techniques used by Wilsdorf, et al 1 A length of wire is first ground to about 0.010 in. thick by mounting the wire in low melting temperature wax, hand grinding a longitudinal flat, removing and reversing the wire in the mount, and then grinding a second parallel flat. The 0.030 in. wide and 0.010 in. thick strip is cut into 1/8 in. lengths to fit in the specimen holder of the electron microscope. Next the specimen is gripped in platinum-tipped tweezers (the anode) and placed 2 mm below a hol- low copper cathode with a 0.010 in. ID nozzle. Electrolyte, 10 pct NaOH, flows by gravity feed through the nozzle onto the specimen, as shown in Fig. l(a). Polishing is carried out until a shallow impression is made on one surface, and then the specimen is turned over and the opposite surface indented. The metal between the two impressions should be about half the specimen thickness, as is shown by the heavy line in the cross section in Fig. l(b). The entire specimen is then electropolishedin 2 pct NaOH until a hole appears at the location of the indentations. The apparatus is shown in Fig. 2, and is essentially the same as that used by Wilsdorf et al. at The Franklin Institute. Light is reflected by a mirror onto the bottom surface of the specimen! which is viewed by a stereoscopic microscope placed above it. Polishing is carried out until light is seen, indicating that a hole has formed, and then immediately stopped. The specimen is washed in water. alcohol, and ether, and is then ready for examination. The specimen should be reversed in its platinum clip during electropolishing to insure equal polishing on both sides of the impression. For tungsten, indenting at 120 v and 0.04 amp takes less than 1 min, and final polishing, at 10 v and 1 amp, less than 5 min. The portion of the specimen available for transmission microscopy surrounds the hole, as is seen by the dashed lines in Fig. l(b). Slight electroetch-ing accompanying electropolishing reveals the mi-crostructure, as seen in Fig. 3(a) by light microscopy. Low-magnification electron microscopy, as in Fig. 3(b), enables the same areas and grains to be viewed and identified when subsequently examined at high magnification. Fig. 4 is a typical structure of

Jan 1, 1963

By W. H. Herrnstein, J. B. Clark, E. C. Utley, A. J. McEvily

The ratio of the endurance limit (10' cycles) to tensile strength of age-hardened aluminum alloys is approximately 0.3, whereas the ratio for annealed alloys is about 0.5. The lower value for the age-hardened alloys has been associated with the instability of coherent precipitate during cyclic loading, but it has not been definitely established whether this instability is due to overaging or reversion during cyclic loading. The results of the present investigatzon support the reversion viewpoint. In this work specimem of 2024-T4 aluminum alloy were aged for 16 hr at 150°C after cycling for 10 pct of the life at 25.000 psi. These specimens were then tested to failure and exhibzted a marked increase in fatigue life. It is proposed that during the early stages of fatigue in this alloy dislocations cut through the coherent precipitate and bring about the reversion of the precipitate. Subsequent aging at 150ºC induces reprecipitation in the precipitate-free zones so that the weakened regions are strengthened and the fatigue life is extended. It Is recognized that the fatigue strengths of precipitation hardened aluminum alloys are unusually low relative to their tensile strength.'-= This feature is illustrated in Fig. 1 where it can be seen that age-hardened alloys have lower fatigue ratios (the ratio of the fatigue strength to the tensile strength) than those in the annealed or cold worked state. Further, as shown in Fig. 2, the more an alloy is dependent upon precipitation hardening for its total strength, the lower is the ratio of the fatigue strength to the tensile strength. This state of affairs has been associated with an instability of the metastable metallurgical structure of precipitation hardened aluminum alloys during cyclic loading. Evidence2 in support of this view is that the fatigue ratio increases in these alloys as the test temperature is lowered, thereby indicating that thermo-mechanical instability, rather than some other factor such as a non-uniform distribution of precipitate, is the factor responsible for the low fatigue ratio at room temperature. Two mutually exclusive proposals have been ad- vanced to account for this instability. Hanstock has proposed that overaging takes place during cyclic loading, and in support of this view, Broom et a1.2 have indicated that an overaging process might be promoted by the large numbers of vacancies which are created during cyclic loading. The creation of vacancies by radiation4 has been shown to lead to rapid overaging. Hanstockl obtained visual evidence of overaging in an aluminum alloy after cyclic loading, but in this instance it has been pointed ou? that because of the high frequency used (60,000 cpm) the observed effect may have been due to normal high temperature precipitation around energy dissipating cracks. Efforts to discern visual evidence of overaging in this alloy at lower test frequencies were not successful.3 The alternative postulate3 is that reversion takes place during cyclic loading and leads to localized soft spots at which fatigue cracks are readily initiated. Evidence for this process has recently been provided by Polmear and Bainbridge5 who demonstrated metallographically that regions depleted of precipitate were created during cyclic loading of an aluminum alloy. Inasmuch as precipitate particles bordering the depleted region had not grown in size, it was concluded that the solute atoms which had constituted the missing particles had gone back into solution. No mechanism for the reversion process was presented. The present study was undertaken to investigate further the conditions leading to instability during cyclic loading, and to determine whether reversion or overaging had taken place as a result of cyclic loading. BACKGROUND AND TEST PROCEDURE In order to differentiate between the processes of reversion and overaging, rest periods at an elevated temperature, which ordinarily would insure additional precipitation, were used in this investigation. It was expected that after a period of cyclic loading an elevated temperature rest period would result in a decrease in the remaining life of the specimen if overaging were occurring during cyclic loading, whereas in the case of reversion, reprecipitation would occur and the fatigue life would be extended. Such an expectation is based on the assumption that the crack-nucleation phase is a significant portion of the total fatigue life, and that such a treatment is of influence in the crack-nucleation stage and is relatively unimportant thereafter.

Jan 1, 1963

By J. A. Morgan, R. E. Lund, D. E. Warnes

The design, operation, and performance of an integrated pilot plant for recovering zinc and copper from a complex sulfide ore are described. Metallurqical processing comprised selective sulfate roasting in a fluid bed, leaching in a weak sulfuric acid solution, recovering copper by cementation with scrap iron, air oxidation to remove soluble iron, more-or-less conventional Purification for removal of impurities deleterious to zinc electrolysis, recovering zinc by electrolyzing solutions, and recycling spent electrolyte to the sulfating roaster. The effects of several feed preparation and roasting variables on the sulfation response of zinc, copper, and iron are set forth, together with the electrolyzing characteristics of the zinc solutions. SEVERAL years ago, St. Joseph Lead Co. undertook a research program to develop procedures for winning values from a complex ore. The deposit was a massive sulfide ore body containing upwards of 65 pct pyrite. Gangue, composed principally of quartz, calcite, dolomite, and alumina, comprised only 10 to 20 pct of the mineralized zones. Zinc, lead, and copper values were variable, but averaged about 6.7 pct Zn, 2.6 pct Pb, and 0.4 pct Cu. Early in the exploratory test work, it was established that the intimate physical association of the minerals in the ore made beneficiation by conventional flotation procedures difficult. Accordingly, in addition to a comprehensive program to investigate physical methods of ore beneficiation, a research program was established to develop a direct metallurgical method for processing the ore. After surveying a number of potential methods for recovery of both metal and sulfur values, effort was concentrated on the development of a sulfate roasting process. It is the pilot-plant development of the sulfate roasting-solution purification—electrolyzing procedures which forms the subject of the present paper. PREPILOT PLANT INVESTIGATIONS From a thermodynamic viewpoint, it is feasible to sulfate selectively a host of metals, including Zn, Cu, Pb, Cd, Ni, and Co, in an iron sulfide ore without sulfating iron. Of course, a number of conditions such as roasting temperature and gas composition must be controlled. In addition, as first disclosed by Hybinette,' an alkali metal salt is frequently beneficial in promoting the sulfation reactions. The application of fluid bed roasting to the sulfate roasting of nonferrous metals was pioneered by Stephens of Battelle Memorial Institute.' Subsequently, Falconbridge Nickel Mines, Ltd. developed an unique process for selectively sulfating and recovering nickel, copper, and cobalt from their nickeliferous pyrrhotite, which recently has been described in an excellent paper by Thornhill.3 One of the unique features of the Falconbridge process is that the feed is introduced into the fluidized roasting furnace in a manner such that the feed slurry is broken up into droplets and the droplets lose their moisture before contacting the surface of the fluidized bed. The dried droplets do not tend to cake or fuse, but rather remain as discrete agglomerates of concentrate particles and roast without significant degradation. St. Joseph, aware that Battelle Memorial Institute had participated in the development of the Falconbridge process, obtained permission from Falcon-

Jan 1, 1962

By Raymond S. Weimer

Of the several characteristics of a coal that influence its suitability for use in a given piece of burning equipment, the clinkering and slagging characteristics of the ash of the coal are highly important. They determine the maximum rate at which the coal may be burned on a stoker or in pulverized form without difficulty from damage to metal parts, from erosion of refractory walls, or from stoppage of gas passages by accumulation on the tubes. They also determine the minimum rate at which a slag-tap furnace may be operated without difficulty in removal of the ash in fluid form. Need for a Better Criterion In common with other producers and users of coal, the Northern Illinois Coal Corporation has long used the available methods for the measurement of the clinkering characteristics of coal ash, chemical composition and fusion temperature of the ash, as criteria for the selection of coal that would suit the particular requirements of its customers. These two available criteria have greatly helped in the problem of selection but it is unnecessary to dwell upon the fact that they are not completely adequate for the purpose. The composition of the ash and its clinkering tendency vary widely over the company's mining area. In a certain period, some years ago, an unusual amount of severe clinkering of the ash of coal shipped made extremely acute the need for a better criterion of the clinkering that might be expected. It was also desirable that the criterion result from a reasonably rapid method, so that the clinkering characteristics of the coal would be known before shipment. Complaints on the severe clinkering of the ash came from only a fraction of the output of the mine but the occurrence of the clinkering seemed quite unpredictable. Attempts to relate the chemical composition of the ash and the fusion temperatures to the clinkering were unsuccessful. Coal from the area of the mine in which the fusion temperature of the ash was the lowest gave the least trouble from clinker-ing. Chemical analysis of the ash from that section giving the most trouble showed high contents of iron and low contents of silica, but frequently these were not greatly different from those of coals that gave little trouble from clinker. Aside from the clinkering difficulty, the coal was quite satisfactory. The ash content was normal and high rates of burning could be obtained, but again and again such severe clinkering would occur that the furnace would be shut down because of the accumulation of clinker. Examination of the clinker from the customers' plants showed that the clinkers that adhered to the grates and fouled the fuel beds were hard, flat, dense, and usually dark in color. Coal that was satisfactory gave clinkers that were softer, bulky rather than flat, of low density, and usually lighter in color.

Jan 1, 1944

By Raymond S. Weimer

Of the several characteristics of a coal that influence its suitability for use in a given piece of burning equipment, the clinkering and slagging characteristics of the ash of the coal are highly important. They determine the maximum rate at which the coal may be burned on a stoker or in pulverized form without difficulty from damage to metal parts, from erosion of refractory walls, or from stoppage of gas passages by accumulation on the tubes. They also determine the minimum rate at which a slag-tap furnace may be operated without difficulty in removal of the ash in fluid form. Need for a Better Criterion In common with other producers and users of coal, the Northern Illinois Coal Corporation has long used the available methods for the measurement of the clinkering characteristics of coal ash, chemical composition and fusion temperature of the ash, as criteria for the selection of coal that would suit the particular requirements of its customers. These two available criteria have greatly helped in the problem of selection but it is unnecessary to dwell upon the fact that they are not completely adequate for the purpose. The composition of the ash and its clinkering tendency vary widely over the company's mining area. In a certain period, some years ago, an unusual amount of severe clinkering of the ash of coal shipped made extremely acute the need for a better criterion of the clinkering that might be expected. It was also desirable that the criterion result from a reasonably rapid method, so that the clinkering characteristics of the coal would be known before shipment. Complaints on the severe clinkering of the ash came from only a fraction of the output of the mine but the occurrence of the clinkering seemed quite unpredictable. Attempts to relate the chemical composition of the ash and the fusion temperatures to the clinkering were unsuccessful. Coal from the area of the mine in which the fusion temperature of the ash was the lowest gave the least trouble from clinker-ing. Chemical analysis of the ash from that section giving the most trouble showed high contents of iron and low contents of silica, but frequently these were not greatly different from those of coals that gave little trouble from clinker. Aside from the clinkering difficulty, the coal was quite satisfactory. The ash content was normal and high rates of burning could be obtained, but again and again such severe clinkering would occur that the furnace would be shut down because of the accumulation of clinker. Examination of the clinker from the customers' plants showed that the clinkers that adhered to the grates and fouled the fuel beds were hard, flat, dense, and usually dark in color. Coal that was satisfactory gave clinkers that were softer, bulky rather than flat, of low density, and usually lighter in color.

Jan 1, 1944

By L. P. Teas

The year 1931 has been one of unusual interest in Gulf Coast petroleum development, not so much because of the number of new prospects discovered, for apparently none of any present distinction have been found, but because of the discovery of so many new oil fields and the proving of so many old prospects. During the year 10 new oil fields have been found on the Coast; five in Louisiana and five in Texas. Two suspected salt domes were proven by the drill. Production dropped from a daily average of 192,000 to 162,670 bbl., or an average of 58 bbl. for each producing well, and active operations from 189 to 119. During 1931 the Coast produced approximately 48,600,000 bbl., or 44 per cent less than in 1930, when 86,500,000 bbl. were produced. The daily return at the beginning of the year was $192,000 and at the end only $126,780, the price having dropped from $1 for A grade and a range of $0.75 to $1.22 for B grade to a price range of 70 to 86c, or an average of 78c $ per barrel at the end of 1931. The average Coastal well produced 17,400 bbl. of oil during 1931. During the year development in the old fields has continued active at Barber's Hill only, although some work is in progress at Humble, Pierce Junction, Refugio and Pettus. Clear Lake is active but the large ownerships will prevent the "boom" type of field. Production is being held fairly steady at Barber's Hill and Pierce Junction, but has declined rapidly during the year at Refugio, Humble, and to a lesser degree at Pettus. The 6000-ft. production at Barber's Hill has shown a decided drop during the year and has not measured up to expectations.

Jan 1, 1932

By C. F. Frey, P. J. Ahern, J. F. Wallace

THE high affinity of molten titanium for oxygen and nitrogen has resulted in considerable difficulty in developing a satisfactory melting procedure. It has been found necessary to perform melting operations either in a vacuum or inert atmos-phere, and failure to obtain a satisfactory crucible material has necessitated the use of special melting techniques. These techniques have included cold-mold arc-melting utilizing both consumable and nonconsumable electrodes, skull-melting, drip-melting, and levitation melting.' It has been recognized generally that the melting of both titanium sponge and titanium scrap would be expedited by the use of induction-melting procedures but the lack of a crucible capable of containing molten titanium without objectionable contamination thus far has prevented the use of induction-melting procedures. An extensive investigation: which included the common refractory materials was not successful in developing a satisfactory crucible for induction-melting. Some success in induction-melting has been attained with the use of a graphite crucible material, but in all instances sufficient carbon contamination was encountered to cause an appreciable reduction in the optimum mechanical properties of the titanium or titanium alloys. These investigations"" report an increase in the carbon content from approximately 0.3 to 1.0 pct. A serious reduction in the tensile and forming properties has been observed as a result of this carbon contamination. The development of a satisfactory induction-melting procedure for titanium without undue contamination undoubtedly would have considerable economic significance. Such a process would be particularly useful in melting the large quantities of low-cost scrap now available that can only be reprocessed at considerable expense and difficulty by the more elaborate techniques referred to previously. In addition, the process could provide a satisfactory method of melting and alloying of bri-quetted sponge for forging ingots.

Jan 1, 1959

By K. A. Pauly

Compressed air has been and is still very extensively used in connection with mining-operations, but its application in the past has been almost entirely confined to supplying power to underground machinery. Its introduction was due to the difficulty of taking care of the steam which is exhausted underground, rather than to any advantage in efficiency to be gained by its use. The ease with which electric power may be carried to the remotest parts of the mine and the high efficiency of the electric motor have long been appreciated by mine-operators, and electric power is now extensively used underground in the more recent developments, while many of the compressed-air engines in the older workings are being rapidly replaced by electric motors. Recently, however, it has been suggested to use compressed air for driving the large shaft-hoists, the air for the engines being supplied by electrically-driven compressors, and an installation of this character is being erected at Butte, Mont. It is the object of this paper to compare the compressed-air system of hoisting with the various electrical systems, from the stand-points of first-cost and cost of operation. However, before entering into a discussion of the various systems, it will be well to consider briefly the conditions affecting the choice of a system of hoisting in which electricity is the ultimate source of power. The power required by a mine-hoist is extremely intermittent and fluctuates between very wide limits, the all-day average consumption of power not exceeding from 5 to 15 per cent. of the maximum demand during hoisting. The cost of supplying power for such a fluctuating load is necessarily higher than that for supplying an equal amount of

Jan 1, 1912