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By T. E. Tietz, J. E. Dorn

Activation energies for creep of copper at intermediate temperatures, where crystal recovery was negligible, were determined by the simple technique of rapidly alternating the test temperature between and T2 (T2 = TI + about 10°K) throughout a constant stress creep test. The activation energy for creep H was found to be 37,000± 3,000 cal per mol, independent of stress and strain. The same creep laws as have been previously established for high temperature creep were found to be valid for creep at intermediate temperatures. But the AH was found to be lower than that for self-diffusion in the intermediate temperature range whereas it is known to be equal to that for self-diffusion at high temperatures. IT is now well established that creep at high temperatures can be correlated by the functional relationship'-" e = f(?) s = constant [I] where E is the total plastic strain, f is the function that depends on the stress, ? = f e -- dt, t is the duration of test, e is the base of natural logarithms, AH is the activation energy for creep, R is the gas constant,T is the absolute temperature, and s is the stress. Thus, identical values of are achieved during creep under a given stress at two alternate temperatures at the same total strain. At the same strain therefore where subscripts refer to the two alternate temperature conditions of test. Consequently, the activation energy for high temperature creep is readily obtained with the aid of Eq. 2. Activation energies so obtained have been observed to be insensitive to the creep strain at which they are evaluated, the applied stress, grain size, minor alloying additions,'-' cold worked state, and the presence of thermally stable dispersions of intermetallic compounds in an a solid solution matrix Furthermore, the activation energy for high temperature creep is very nearly equal to that for self-diffusion in all cases where adequate data are available for comparison." " The apparent identity of the activation energies for high temperature creep and self-diffusion strongly suggest that high temperature creep arises from a dislocation climb process. This hypothesis is further strengthened by the fact that the energy of activation for high temperature creep is insensitive to the applied stress," and by the observations that the correlation suggested by Eq. 1 cannot be ex- tended to temperatures below those for rapid crystal recovery. When using the activation energy for self-diffusion, Eq. 1 fails to give the required correlations between creep curves at various intermediate temperatures.' This suggests that the dislocation climb mechanism for creep might be superseded by some alternate mechanism in the intermediate range of temperatures. This investigation was initiated in a preliminary attempt to ascertain the type of creep law that might be valid in the intermediate range of temperatures. Special consideration, however, was given to the determination of the activation energy for creep in this range because the Becker-Orowan', " and the Mott-Nabarro10 theories for transient creep suggest that the activation energy should increase

Jan 1, 1957

By Herbert J. French

Herbert 1. French (Member 1934), vice president of the International Nickel Co. Inc., assistant vice president of the International Nickel Co. of Canada Ltd., and AIME Howe Memorial Lecturer for 1956, died in Rochester, Minn. on Aug. 17, 1955, after a long illness. Before his death, Mr. French had laid the foundation of research on which the Howe Memorial Lecture (p. 770) was based. His associates at Inco, 0. 0. Miller and J. W. Sands, were able to complete the project, present the lecture, and prepare it for publication, following Mr. French's general outline. Born in New York on May 27, 1893, he graduated from the School of Mines, Columbia University, with a degree in metallurgical engineering in 1915. Mr. French gained his early engineering experience with the American Smelting and Refining Co., serving as a chemist and as-sayer at the company's Murray, Utah, installations. He later returned east and became a metallurgical engineer for the General Vehicle Co., Long Island City, IT. Y., a subsidiary of the General Electric Co. In 1917 Mr. French was appointed civilian inspector of materials for the U.S. Army Signal Corps, and continued this work when it was later absorbed into the Bureau of Aircraft Production. Subsequently he was appointed district inspector in Philadelphia for the Pittsburgh (Ordnance Metallurgical) office, later transferring to Pittsburgh. After World War I Mr. French became an assistant physicist on the metallurgical staff, U. S. Bureau of Standards, Washington, D. C. During his years with the Bureau, he was successively associate physicist, metallurgist, senior metallurgist, and assistant chief, division of metallurgy. In 1929 Mr. French joined International Nickel as a metallurgist at the company's Bay-onne, N. J., research laboratory. Transferring to the development and research division, New York, in 1931, he took charge of alloy steel and iron development, becoming assistant manager of this division in 1943. Mr. French's appointment as an Inco vice president came in March 1947. Previously, he was appointed assistant vice president of the International Nickel Co. of Canada Ltd. in January 1947. Mr. French served the War Production Board during World War II as senior technical consultant in charge of the metallurgical and specifications section of the iron and steel branch. When this section of the WPB was organized into the steel division, he was appointed chief of the metallurgical branch. From March 1944 to September 1945 Mr. French served as assistant director. Herbert French was well known not only for his prolific contribution to the metallurgical literature, for which he received numerous awards, but also for his prolonged service to the profession through its technical societies. He was a past president of ASM, and was the Campbell Memorial Lecturer for that group in 1933. Mr. French was honored by the American Society for Steel Treating in 1931 when he was awarded the Henry Marion Howe Medal. A series of lectures he gave in 1941 before the Fourth Western Metal Congress in Los Angeles was later published in book form under the title Alloy Constructional Steels.

Jan 1, 1957

By Jack Wright

The analysis of water produced with crude petroleum has interested oil producers since inception of the industry. Records of the first analysis of mineralized water produced from an oil-productive formation are obscure, and references to the first use of brine analyses to assist in solving problems of petroleum production are not available in the technical literature. However, many early reports of the Federal Bureau of Mines5-8 and Federal Geological Survey,9-11/ as well as articles in engineer and geological journals12-14/ placed special emphasis on the importance, interpretation, and application of water analyses. One of the earliest applications of water analyses, and still a major one today, is for identification of intrusive waters in oil wells. This may be done by comparing the chemical constituents of a sample of water indigenous to the oil-productive formation with those of samples from upper, water-bearing formations within the same general area. Some earlier investigators recognized the need for Analyzing samples of all waters encountered in drilling operations. Ambrose15/ stated, in part, "In wells being drilled, the engineer should grasp every opportunity to get a true sample of water from each sand. . .," and, "The waters of each oil field are chemically different from those of another field." The validity of the latter observation and the importance of the former one have been borne out by comparing the results of analyses of many samples and noting the differences in relative concentrations of like constituents of waters from the a geological formation in different localities or oil pools.

Jan 1, 1957

By A. J. Barry

Five makes of expansion-type shells and two types of bolts (mild-steel and high-strength) were used in 30 tests made in sandstone and shale roof, The results show that the anchorage obtained in both the sandstone and shale were stronger than either type of bolt. That is, the yield loads of both bolt types were exceeded before excessive anchor slip occurred. A relationship for evaluating the anchorage effectiveness of 3/8-inch-diameter, expansion-type bolts is presented. A comparison of test results indicates that the anchorage effectiveness of 5/8-inch- and 3/4-inch-diameter expansion-type bolts did not differ appreciably.

Jan 1, 1957

By A. J. Teplitz, T. Bardeen

In the course of an investigation of lost circulation, a new tool has been developed which gives a qualitative measure of the relative velocity between the fluid column in the borehole and the tool. The position of a diaphragm in the side wall of the instrument depends on the flow through the device. This position is established by using the conductive borehole fluid in a potentiometric circuit. The instrument has high sensitivity and can detect changes in velocity as low as. 5 ft/min. Lost circulation mud additives do not interfere with the satisfactory performance of the tool. In a number of circulation losses of the pressure induced type, the instrument has shown that the losses were confined to extremely narrow zones (less than I ft), indicating that such ruptures occur in a more or less horizontal rather than vertical plane as has often been assumed. This pinpointing of the zone of loss is important in remedial procedures since it allows the treatment to be applied directly to the point of loss rather than to the entire open hole. The device can also be employed for indicating points of entry of water in producing wells. INTRODUCTION The need for an improved means of locating the positions of lost returns zones became evident during an investigation of lost circulation difficulties in the Gulf Coast area.1 With instrumentation available at the time, it had been learned that, contrary to common belief, the position of the thief zone responsible for a given loss seldom coincided with the point of bit penetration at the time the loss was encountered. In the majority of cases, the losses were found to be occurring at some distance removed from the bottom of the hole —sometimes as much as a few thousand feet. This information, along with other observations made during the investigation, led to improved techniques' for dealing with lost circulation problems. Highlighted, however, among the results of this work and of similar studies subsequently conducted in drilling operations in other parts of the country, was the indication that a considerable portion of the difficulty and expense involved in treating prolonged circulation losses is due to the unsystematic application of remedial measures to one or more apertures of unknown position. Basis of Tests It is worth considering that if the troublesome formation could somehow be transported to the surface where it could be directly observed, there would likely be little difficulty in readily effecting a seal. Although this is a decided oversimplification of the situation, it does appear that the chief obstacles to similar ease of handling of a lost circulation zone in a well are lack of visibility and of ready accessibility. The latter handicap is overcome to a considerable extent by placement techniques already in use, and other procedures now in the process of development are expected to offer further improvement. But in the matter of visual observation, the technique to be presently described appears to afford a quite satisfactory substitute.

Jan 1, 1957

By G. A. Vissac, R. G. Minet, N. E. Sylvander

R. G. Minet—The authors' description of the remarkable progress made in the last few years in applying the fluidized solids technique to the problem of lignite drying and carbonization clearly demonstrates that engineering techniques available today may make many processes practical and profitable which a few years ago were considered otherwise. As pointed out in the article, the future of the carbonization step hinges on the value and utilization of low temperature tar. On paper, at any rate, this tar looks like a valuable raw material for the chemical industry to use. Some 50 to 60 pct may be converted to pitch for electrodes, roofing, road tars, and other valuable products; the 25 to 30 pct tar acids could conceivably form a basis for a new low cost resin or plastic of the phenolformalde-hyde type. Yet these materials are so new and dissimilar from available sources that much work must be undertaken by the chemical industry before they will be accepted. Now that the work of Dr. Perry and his colleagues has made a large supply of low temperature tar a real possibility, I would expect the chemical industry to accelerate its work in this field. On the basis of certain data available in the literature it appears possible to produce a more aromatic tar, although in smaller yield, by operating at temperatures in the range of 1300" to 1500°F. Operating a fluidized bed process for lignite at these conditions should be technically possible, at least, and could produce a tar having more familiar characteristics. I wonder if Dr. Parry would care to comment on such a possibility. Incidentally, in our own work on carbonizing coking coals in fluidized beds, using Ohio, Pennsylvania, and West Virginia high volatile bituminous coals, we have obtained yields which agree with the correlation given for tar yields vs moisture and ash-free volatile Btu. Our data are slightly under the line, but certainly in the range of the correlation. We have also obtained evidence in support of the authors' statement as to the effect of air on the process. In our pilot plant all the heat required for carbonizing is released by internal combustion of char in the fluidized bed in normal operation. We are also equipped to obtain all carbonization heat by external electric heaters on the shell of the carbonizer while introducing only an inert gas to the process. We note no difference in tar yield or characteristics between the two operations. In the case of the gas, however, it appears that some hydrogen is consumed by the air combustion. We would be interested in hearing in a little more detail about the hot dust and char handling problems at Sandow. Have the authors found char subject to spontaneous combustion? Have they ever tried a coking coal in their pilot plant? V. F. Parry (author's reply)—Production of a more aromatic tar by operation of the carbonizer at 1300" to 1500°F does not appear to be economical. 1) The capacity of a reactor operating at 1500°F would be 30 to 50 pct less than the capacity at 932 °F and the cost of processing would increase materially. 2) The cracking of tar vapors in a reactor requires appreciable time to complete the reactions and it is doubtful that considering the very short time of residence of tar vapors within the reactor (4 to 10 sec after evolution) the basic character of the tar would be changed significantly. This is indicated from the data reported in Table XIV. 3) General studies have shown that it is advisable to operate at the minimum temperature to produce the maximum tar and minimum gas. 4) Operating problems and the maintenance of vessels and reactors, and the hazards of handling hot char, increase with the temperature of carbonization. It is technically possible to operate at temperatures as high as 1500°F, but in my opinion it is not economical or desirable. We believe that the primary tar must be won in the simplest way and then processed alone to change its character for production of desired products. It is interesting to have confirmation of our observations on the reaction of air with the products of carbonization. The major reaction is with the char, fol-

Jan 1, 1957

By G. W. P. Rengstorff, L. E. Olds

High purity molybdenum ingots containing controlled amounts of a single impurity element (oxygen, nitrogen, or carbon) were prepared. These ingots were tested for ductility by bending test specimens at various temperatures. The relationship between the plastic behavior of the ingots and their chemical composition has been determined. MANY proposed applications for molybdenum require ductility at or near room temperature. At the present time, it is possible to obtain wrought molybdenum with considerable ductility only if special fabrication techniques are used to control the grain structure. Starting with are-cast or powder metallurgy ingots, the usual methods for obtaining ductility rely on fabrication procedures that result in fibered microstructures in the finished product. Recently, it has been found that the ductility of either powder metallurgy or are-cast molybdenum can be improved by uniform recrystallization of the metal to a very fine equiaxed grain structure.' The need for a fibered or a fine grained structure may limit the practical usefulness of molybdenum. For example, welding. which may be used in fabricating the metal, generally produces coarse grained structures that lead to brittleness. This applies, certainly, to currently available commercial molybdenum. Although commercial molybdenum is brittle when the grains are coarse, it has been shown experimentally that fine grained structures are not always essential for ductility. For instance, as-cast molybdenum with a coarse columnar grain structure is ductile if it is sufficiently pure.' Because high purity cast molybdenum has good ductility even when coarse grained, it is probable that the brittleness in coarse grained commercial molybdenum is caused by the impurity content of the metal. Although the general effects of impurities on the cold ductility of molybdenum have been known in a qualitative manner for some time, no quantitative evaluation of these effects has been available. The present investigation was made in order to determine more accurately the effects of oxygen, nitrogen, and carbon on the cold ductility of cast molybdenum. Oxygen has long been known to be detrimental to ductility, although the minimum amount which will embrittle molybdenum has been open to speculation. Parke and Ham" showed that ingots with oxygen contents above 0.003 pct could not be forged. Maringer and Schwope have described the embrittle-ment of molybdenum wire by oxygen. A discussion on the effects of heat treatment on the distribution of oxygen in molybdenum has been given by Perry, Spacil, and Wulff." Although nitrogen would also be expected to have harmful effects on ductility, no extensive work has been done previously to determine whether this is so. However, Tury and Krausz" found that wires presumably with less than 0.007 pct N were brittle. Carbon is added to commercial cast molybdenum for deoxidation. Parke and Ham" have shown that molybdenum containing as much as 0.06 pct C could be forged if the oxygen was kept below 0.003 pct. Also, Bruckart and others' found that the room temperature ductility of sintered molybdenum improved with carbon contents up to 0.84 pct. However, Rengstorff and Fischer' found that residual carbide particles in cast molybdenum apparently had an unfavorable effect on room temperature ductility.

Jan 1, 1957

By A. N. Holden, W. E. Seymour

DURING the last several years, the U-Zr system has been studied at many laboratories as one of the research programs sponsored by the Atomic Energy Commission. The equilibria in part of this system have been difficult to determine, although the phase diagram from 0 to 60 atomic pct Zr has been established with reasonable certainty. Existing diagrams of the system vary appreciably beyond 60 atomic pct Zr, particularly with regard to the existence of an intermediate phase. Most existing diagrams show a transformation or reaction horizontal near 600°C. In 1955, a collection of uranium phase diagrams' was prepared at the Battelle Memorial Institute and the U-Zr diagram in that collection contained a questionable region in the vicinity of 60 to 80 atomic pct Zr. Summer-Smith" has published a phase diagram of the system that shows no intermediate phase. Summer-Smith did his work with powders and found only the uranium and zirconium eutectoid mixture from X-ray patterns of material annealed below 600°C. Mueller3 at Argonne National Laboratory did similar work with filings, and he found that initially there was a pattern of an intermediate phase, but on long-time annealing

Jan 1, 1957

By J. H. Faulk

An examination is made of the various factors influencing drilling rate and drill bit life in various diameter holes. It is concluded that drill bits in the size range 4% to 6 1/4 in. can be used to attain substantially the some daily drilling progress as conventional size bits in soft rock drilling operations. An examination of the most important factors influencing "hazard of losing the hole" in the different hole size results in the conclusion that the smaller hole sizes can probably be drilled at reasonably low risk. However, this risk will be somewhat greater in the smaller diameter holes, requiring that special drilling and mud engineering practices be used to make small diameter holes practicable in soft rock drilling operations. An engineering analysia is made of the power and hydraulic requirements of several drill string-hole combinations to test the feasibility of drilling .small diameter holes in soft rock areas. Large econormies in rig power requirements appear possible by drilling .smaller .size holes in these operations. INTRODUCTION The industry now is re-examining the utility of small diameter holes in the light of substantial technical advances made in recent years. Faced with increasing cost of finding reserves and with proration after developing them, the industry must either develop methods of economizing or receive a lower rate of return on investments. Small diameter holes appear to involve an attractive method of economizing. Our objective is to determine if this is technically possible in soft rock operations. Soft rock, as used in this report, refers to those formations of a "drill-ability" corresponding to that of all Gulf Coast formations shallower than and frequently including much of the Eocene rock system. An important phase of technology which we shall examine is relative drilling rate and bit footage which may be obtained with various size bits. Rig operating efficiency, particularly as influenced by hazard, is also discussed in detail. The technical conclusions resulting from these examinations are used to develop sample drill string design and rig horsepower requirements for drilling holes as smaH as 4 3/4 in. and larger. The principal criterion used for the drill string design is that approximately the same daily drilling progress would be possible in all size holes in soft rock operations. This facilitates a comparison of rig size required for drilling the hole sizes in the range between 4 3/4 and 8 3/4 in. BROAD PROBLEM OF DRILLING RATE AND BIT FOOTAGE The three factors controlling daily drilling progress are: (1) drilling rate of bit while on bottom turning, (2) bit footage, and (3) rig operating efficiency. Let us look now at the first two of these factors. Drilling technology has progressed to the point that a semi-quantitative analysis of the effect of various operating variables upon these factors can be made. Those factors which apparently limit both drilling rate and bit footage for bits now in use are: (1) bit design, (2) weight on bit, (3) hydraulic cleaning capacity for bit cutting surfaces and hole bottom, and (4) rotary speed. (We neglect the effect of mud and formation properties because these factors arc the same for the various size bits.

Jan 1, 1957

By J. N. Butler, R. J. Morris

A series of organic collectors has been developed which successfully float synthetic secondary uranium minerals, such as autunite, carnotite, and torbernite. Recoveries up to 97 pct have been obtained. With cleaning of rougher concentrates, ratios of concentration as high as 15:1 are possible on head assays of 0.10 to 0.50 pct U 3 O 8. Additions of certain base metal salts aid in recovery and materially increase the rate of flotation and selectivity of the collectors for the synthetic minerals. Flotation tests on natural uranium minerals have not yet equaled results obtained on the synthetics, although these collectors do give better results than conventional collectors for nonsulfide minerals. RAPID increase in mining and milling uranium ores during the past seven years and the discovery of large tonnages of uranium-bearing material too low in grade to stand the cost of leaching have developed considerable interest in possible methods for beneficiating these marginal ores. Such ores are generally classed as those containing less than 0.10 pct U3O8. Development of a beneficiation method that would give both high recovery and high ratio of concentration would also make possible the beneficiation of higher grade ores and would provide higher grades of feed to existing leaching plants. Although considerable research and testing on physical or physico-chemical beneficiation of domestic uranium ores has been done in the past, to the best knowledge of the authors only a single application of physical beneficiation is now in operation on a commercial scale. Flotation has been attempted on the basis of mineral association rather than by direct concentration of the contained uranium minerals. Flotation studies conducted on this project on certain ores gave recoveries of 60 to 70 pct of the uranium by the use of conventional flotation agents such as oleic acid, but ratios of concentration were in the order of 1.5:1 to 2.5:1. Subsequent cleaning to upgrade the concentrates rapidly increased losses in the cleaner tailings, which were not later refloated in the rougher flotation. Selection of Collector: In selecting desirable organic collectors for these oxide systems, a thorough study was made of the relationship between structural characteristics and collector activity by an examination of the behavior of a number of different functional arrangements present in a variety of organic molecules, (see Fig. 1). It is generally accepted that a collector must have a relatively long-chain hydrocarbon radical and a chemically reactive elec-trophilic center. Such a requirement could be met by a large number of compounds, but steric effects at the uranium mineral surface, solubility, compat-ability with aqueous systems, air avidity, bond strength at the mineral surface, interfacial concentration of the collector, and diffusion rate of the formed complex from the air-water interface eliminated many as unsuitable for this purpose. Preliminary investigations were completed of possible collector designs consisting of aliphatic and aromatic hydrocarbon radicals attached to stable combinations of nitrogen, oxygen, sulfur, and halogen electrophilic centers, Fig. 1.Tests were made to determine melting point spans, solubility of mineral-collector combinations in various solvents, reactions with soluble uranium salts, contact angles, and floatability by semi-quantitative beaker methods.' Contact angle determinations were not too useful because of the fine particle sizes of available mineral samples. From the foregoing study it appeared that nitrogen-sulfur electrophilic centers coupled with straight-chain saturated alkyl hydrocarbon radicals would hold the most promise for floating secondary uranium minerals. As the dithiocarbamate compounds can be made to combine these attributes they were selected for further study. The dithiocarbamates form a parallel structure to the xanthates, with the fortuitous exchange of

Jan 1, 1957

By J. S. Crump, H. L. Stone

Laboratory studies have indicated that displacement of oil from a reservoir by means of a condensing gas drive results in extremely high oil recovery, approaching 100 per cent under the most favorable circumstances. A condensing gas drive is defined as a gas drive in which the gas utilized is appreciably soluble in the oil it is displacing. The laboratory studies consisted of a number of gas drive displacement experiments, all using a horizontal, sand-packed, steel tube as the laboratory reservoir. The experimental results indicate that the more soluble a gas is in the oil to he displaced, the more efficient that gar is as a displacing fluid. Experiments were conducted utilizing both a light, volatile crude and a heavy, asphalt crude as the in-place oil. In both cases, oil recovery was appreciably enhanced by solubility of the displacing gas. It is believed that the use of condensing gas drives would result in increased oil recovery from many reservoirs during either primary or secondary phases of production. INTRODUCTION Since the early days of the oil industry there has been an increasing awareness of the problems of oil recovery. During the last few decades particularly a growing recognition of the problems has led to widespread attempts on the part of the industry to increase oil recovery by improved technology. One method which has been used to increase recovery is the maintenance of reservoir pressure by injection of gas. Part of the beneficial effect resulting from this gas injection was to prevent evolution of the gas dissolved in the reservoir oil, since such evolution would cause the oil to shrink and become more viscous, thereby adversely affecting oil recovery. In most instances, the gas injected was predomillantly methane, and so the possibility of oil recovery by retrograde vaporization existed. Laboratory investigations of displacement of reservoir oils by methane, carried out at high pressure, have indicated that considerable additional recovery of light oils could be effected by vaporization, but only at the cost of a severe volumetric shrinkage of the residual oil which would cause a decrease in relative permeability to oil in the reservoir. Consequently, recovery of oil by physical displacement would be impaired. The study suggested, therefore, that recovery of oil might be enhanced by injecting into the reservoir a gas known to be appreciably soluble in the oil at reservoir conditions. Swelling of the oil due to solution of gas should result and yield a consequent increase in the relative permeability to oil. The work described in the following sections was, therefore, undertaken to investigate the possibility of increased recovery by this mechanism. Research similar to that reported in this paper has been conducted by The Atlantic Refining Co.1,2,3 In these studies, Whorton, et al, and Slobod, et al, used methane-rich gas to displace oil from model reservoirs. Solubility of the gas was achieved by keeping the reservoir pressure greater than the saturation pressure of the original oil, and the degree of this solubility was varied by operating at different reservoir pressures. Thus the Atlantic project was primarily a study of the effect of reservoir pressure upon oil recovery by gas drive. The objective of the work reported in this paper was to study the effect of gas composition upon oil recovery while holding the reservoir pressure constant. DESCRIPTION OF EXPERIMENTS The discussion of the preceding section suggests that

Jan 1, 1957

By Frank E. Hauser, Philip R. Landon, John E. Dorn

The flow and fracture strengths of polycrystalline aggregates of high purity magnesium and a solid solution of aluminum in magnesium were determined as functions of temperature and grain size. Magnesium was found to obey two distinct fracture laws. Over the high temperature range, the fracture stress decreased with increasing test temperatures in a manner that closely paralleled the flow stress-temperature relationship. However, over the low temperature range, the fracture stress was independent of the test temperature though highly dependent on grain size, following the trend that is typical for the low temperature brittle fracturing of polycrystalline aggregates of body-centered-cubic and close-packed-hexagonal metals. Even at 78°K, however, plastic strains of 1 to 7 pet were obtained preceding onset of brittle fracturing. Over the brittle fracture range of temperatures, the fracture stress increased linearly with the reciprocal of the square root of the mean grain diameter, while over the entire range of temperatures investigated, the flow strength was observed to increase linearly with the reciprocal of the square root of the mean grain diameter. PREVIOUS investigations', 'have shown that deformation of coarse grained aggregates of high purity magnesium is interrupted by fracturing at very small strains. Such tendency toward brittle fracturing increased with increasing grain size and decreasing test temperature. In several respects, however, low temperature fracturing of magnesium appeared to differ from the truly brittle type exhibited by zinc, molybdenum, tungsten, and iron, so often characterized as a cleavage mode of fracturing. The absence of a well-defined cleavage mechanism for fracturing and the fact that some plastic deformation precedes fracturing might suggest that magnesium does not exhibit the same kind of brittle fracturing that is common to body-centered-cubic metals and to other close-packed-hexagonal metals. But, as will be shown, the low temperature fracture laws for magnesium are analogous to those that apply to iron, molybdenum, tungsten, and zinc in spite of differences in mechanisms and in plastic strains to fracture. In view of these observations. the low temperature fracturing of magnesium will also be called brittle fracturing. This, of course, does not imply that the brittle fracturing of metals is synonymous with the brittle fracturing of glass or other nonmetallics. Whereas the brittle fracturing of glass probably obeys Griffith's law, the low temperature brittle fracturing of metals arises from stresses induced by a series of dislocations piled up at an opaque grain boundary. Experimental Results All tests were made on tensile bars having gage sections that were 2 in. long and 0.375 or 0.25 in. wide. In order to develop a series of grain sizes, the

Jan 1, 1957

By T. A. Evans

The Bureau of Mines conducted a Laboratory and pilot-plant investigation of the flotation of iron sulfides from zinc-lead mill tailings near Platteville, in south-western Wisconsin, at the North Central Experiment Station, Minneapolis, Minn. The procedures used and the results obtained in this investigation are described in this report. Samples for laboratory tests were obtained from each mill in the district, namely, Calumet & Hecla, Inc., Eagle-Picher Co., Vinegar Hill Zinc Co., and Tri-State Zinc, Inc. The sample fat pilot-plant work was obtained from the Davis Mining Enterprises mill.

Jan 1, 1957

By A. E. Powers

YEARS of experience and research have shown that molybdenum, tungsten, and vanadium are among the most useful and effective elements in augmenting the high-temperature strength of heat-treatable, ferritic steels. Grün, for example, in conducting an early survey of the strengthening effects of various elements in annealed, low-carbon steel at 750° and 930°F (400° and 500°C), found molybdenum and vanadium to be the most effective.' Holtmann comprehensively studied the strengthening effects of molybdenum and vanadium in quenched and tempered steels at 930°F as a function of microstructure and carbon content.' He found creep strength to be related to the saturation of the austenite at the austenitizing temperature, such that strength is increased by alloying until the y loop is reached—the terminus of complete austenitization. Beyond this degree of alloying, the inability to heat treat will result in lower strength, at least for low and moderate creep temperatures. Tungsten, owing to higher cost than molybdenum, has been little used in ferritic high-temperature steels. As a result, very few investigations have been made of its high-temperature strengthening ability, and reliable data on its effectiveness are not available. Grün rated tungsten far less effective than molybdenum at 930°F (500°C) on a weight-percentage basis.' However, Tammann has found that tungsten is as effective as molybdenum in raising the recrystallization temperature of iron. For this reason Smith, in a review of the subject, has advocated a re-examination of the influence of tungsten on the high-temperature strength of steel.' In any study of the effects of alloying additions on high-temperature properties, recognition must be made of the many variables involved, some of which can be controlled but have been ignored in innumerable investigations of the past, and some of which are difficult or even impossible to control. One cannot, for example, assign a definite strengthening index to any one alloying element, for this will be dependent upon the microstructure (heat treatment and mechanical treatment), testing con- ditions (temperature, time, and stress), and the complete composition of the steel (accompanying alloying elements, impurities, etc.). One ever-appear ing variable, hardness or tensile strength at room temperature, may be eliminated by heat treating all of the alloys to a single hardness level. An attempt may be made to control the variable of primary quenched structure by oil or water quenching the test specimen. The control of such variables may not be possible in cases of widely varying compositions, but at least such deviations should be recognized. Material and Procedure The alloys, made as 30-lb ingots in an induction furnace, all had the same base composition of about 0.18 pct C, 0.85 pct Mn, and 0.48 pct Si. They were grouped as follows: Mo Group—Containing up to 5.2 pct Mo. W Group-Containing up to 6.0 pct W. V Group—Containing up to 3.3 pct V. Mo-V Group—Containing up to 2.7 pct Mo and up to 1.4 pct V. Mo-W Group—Containing up to 2.5 pct Mo and up to 2.5 pct W. The steels, listed in Table I, were forged to ¾ in. sq bars and the material for the high-temperature, rupture-test specimens was further swaged to %-in. round bars.

Jan 1, 1957

By Miro Mihelich

The mines and prospects in the vicinity of Landlocked Bay, 25 miles southwest of Valdez, Alaska (fig. 1), were examined, mapped, and sampled in July and August 1955 as part of a comprehensive investigation by the Bureau of Mines of ore deposits adjacent to Prince William Sound. The purpose of the investigation is to establish and record the location, nature, extent, and metallurgical characteristics of copper and associated metallization in the Prince William Sound district and to indicate, if possible, those areas in which additional exploration and development may be justified. Of particular interest are the possibly numerous deposits of massive iron sulfides that were neglected during early mining operations. These deposits may constitute important reserves of sulfur and iron. At Landlocked Bay deposits of copper-bearing iron sulfide minerals have been mined or partly explored through mine workings, which are in a zone about 1 mile wide along the western side of a large overthrust fault known as the Landlock Overthrust. Eight of the principal mines along this zone were examined end sampled. Although only three of the mines have a recorded production of shipping-grade copper ore, all have deposits of copper-bearing iron sulfide minerals that are similar in occurrence. The deposits occur as lenticular masses and disseminations of chalcopyrite, pyrite, and pyrrhotite which replace crushed rock or fill cavities along shear zones in greenstones and in sedimentary rocks that are exposed between sea level and an altitude of 2,500 feet. These lenticular masses of sulfide minerals range in size from small pods to ore bodies that have been stoped to maximum widths of 9 feet, strike lengths up to 70 feet, and dip lengths as much as 350 feet. Where accessible for sampling,, the copper content of the deposits ranged from a few hundredths of a percent to over S percent; zinc, gold, and silver are present in negligible amounts. Flotation tests of a sample composited to represent typical mine-run ore indicate that 81 percent of the copper is recoverable in a product assaying 28 percent copper at a concentration ratio of 17.5 : 1. INTRODUCTION Statistical records indicate that approximately 110,000 tons of metallic copper (about 16 percent of total Alaskan production) was produced from mines adjacent to Prince William Sound during the 40-year period ended in 1938. Although the principal production was from a large-scale mining and milling operation on Latouche Island (Kennecott Copper Corp., Beatson mine), a substantial amount of the total copper was derived from direct-shipping ores selectively mined or hand-sorted from numerous other deposits in the district. No production has been made since 1938; many of the claims have long been abandoned, and mine workings are either caved or deteriorating rapidly.

Jan 1, 1957

By Paul A. Farrar, Louis P. Stone, Harold Margolin

The Ti-Mo-0 system was investigated in the region 0 to 45 wt pet Mo and 0 to 10 wt pet 0, from 600° to 1400°C. Solidus data are also presented. Isothermal sections at 700°, 900°, 1100°, and 1300°C, and vertical sections at 1 and 28 wt pet Mo, and 1 and 10 wt pet 0 are included. STUDY of the Ti-Mo-0 system has been carried out as part of a general study of titanium phase diagrams. The binary Ti-Mo system has been investigated in whole or in part by several investigators.1-8 It was found that molybdenum and ß-tita-nium form a complete series of solid solutions and that the ß/a + ß transus is depressed to below 600°C at approximately 30 pet Mo.* The Ti-O system has been investigated partially or fully in the range 0 to 30 pet 0 by several investigators." Extensive solubility of oxygen occurs in the field. While a is

Jan 1, 1957

By M. R. Geer

The widespread adoption during the past decade of the dense-medium process for cleaning coal increases the need for technologic studies of the process. Such studies provide information that will insure maximum usefulness of this process in its present form and may well lead to substantial improvements in design and opera¬tion. The Bureau of Mines has published the results of cleaning trials on a wide variety of coals in two dense-medium pilot plants5/ and reported the recovery of coal from waste by dense-medium treatment.6./ The present report deals with the viscosity of magnetite dense medium, an important subject about which virtually nothing has been published. Specifically, the report concerns methods for measuring viscosity, the influence of various medium contaminants on viscosity, the effect of viscosity on cleaning results, and the influence of viscosity on consumption of medium. Cleaning trials on four coals of varied density composition in a pilot plant, using mediums of different viscosities, showed a steady reduction in cleaning efficiency with increasing viscosity in every instance. However, the behavior of each coal in a viscous medium was distinctly individual. With one, an increase of only 1 centipoise in viscosity caused a reduction in recovery efficiency of 7.7 percent, whereas the same increase in viscosity with another reduced recovery efficiency only 2.7 percent.

Jan 1, 1957

By R. F. Dickerson, D. A. Vaughan, A. F. Gerds

ALTHOUGH the metallurgy of uranium has been under intensive study since the early 1940's, no systematic effort has been made to identify the non-metallic inclusions in uranium. Uranium carbide (UC), which is probably the most common inclusion found in graphite-melted metal, has been tentatively identified by previous investigators, but the other nonmetallic inclusions have received little attention. Since metallography is a valuable tool in metallurgical studies, the metallographic identification of the nonmetallic inclusions in uranium is important. Such an investigation has been completed and the identification of slag-type inclusions and of uranium monocarbide, uranium hydride, uranium dioxide, uranium monoxide, and uranium mononitride is described. Metallographic Preporation It is often possible to prepare specimens for metal-lographic examination equally well by several methods. The specimens which were examined in this work were prepared by one of two acceptable methods. For the convenience of the reader, both methods will be discussed in detail and will be referred to simply as Method I or Method II in the subsequent sections. For both Methods I and 11, specimens for microscopic examination usually were mounted either in bakelite or in Paraplex room temperature mounting plastic. Method I—Specimens were ground in a spray of water on a revolving disk covered successively with 120-, 240-, and 600-grit silicon carbide papers. It was necessary to perform the final grinding operation carefully on worn 600-grit paper to keep the scratches as fine as possible. After washing and drying, the specimens were polished for 3 to 4 min on a slow speed wheel (250 rpm) covered with a medium nap cloth. Diamet Hyprez Blue diamond polishing paste, Grade 00, 0 to 2 µ, was used as abrasive with kerosene as lubricant on the wheel. Specimens were washed thoroughly in alcohol and final polished electrolytically in an electrolyte composed of 1 part stock solution (118 g CrO, dissolved in 100 cm3 H2O) with 4 parts of glacial acetic acid. A stainless steel cathode was used. At an open circuit potential of 40 v dc, a polishing time of 2 sec retained inclusions well with the bath at room temperature. If additional etching was required to sharpen the interface between the metal and the inclusions, an electrolyte composed of 1 part stock solution (100 g CrO3 and 100 cm8 H20) and 18 parts glacial acetic acid was used at room temperature. Best results were obtained by etching for from 10 to 15 sec at 20 v dc in the open circuit. Surfaces obtained by this method are suitable for microscopic examination. However, if desired, they may be etched further with other chemicals. Method 11—Rough grinding was done on a wet 180- or 240-grit continuous grinding belt. The specimen was then ground by hand successively on 240-, 400-, and 600-grit silicon carbide papers in a stream of water. Final polishing was accomplished on a 4 in. high speed wheel (3400 rpm) covered with Forstmann's cloth. Linde B levigated alumina, suspended in a 1 volume pet chromic acid solution, was the abrasive. Specimens usually were polished in 5 min or less by this technique. Often the inclusions present in the metal were identified in the mechanically polished condition. When etching was required to outline inclusions more sharply, one of the two following methods was used. In the first method, the specimen is etched lightly while electropolishing in the chromic-acetic acid solution described above (1 part of stock solution to 4 parts of acetic acid). The electrolyte was refrigerated in a dry ice-ethyl alcohol bath and specimens were etched at 60 v dc on the open circuit for 2 or 3 cycles of 3 to 4 sec each. The second technique utilizes electrolytical etching at about 10 v dc (open circuit) in a 10 pet citric acid solution at room temperature. X-Ray Diffraction Technique The major problem in the identification of inclusions in metals by X-ray diffraction techniques is the extraction of a sufficient amount of each type of inclusion to obtain an X-ray diffraction pattern. In the present study, X-ray diffraction patterns were obtained from individual inclusions of the order of 10 µ diam. The polished and etched samples shown in the micrographs were examined at a magnification of X54 or XI00 with a binocular microscope. This allowed sufficient working distance to extract the inclusions with a needle probe for powder X-ray diffraction analysis. Friable inclusions such as MgF2, CaF2, UO2, and UH3 could be freed from the metal by probing the as-polished and etched surface. The fine particles then were picked up on the end of a Vistanex-coated glass rod (0.002 in. diam) which was held in a brass adapter made to fit the powder X-ray diffraction camera. The end of the glass rod was centered in the path of the X-ray beam. In the case of the UC, UO, and UN inclusions which are smaller in size, more metallic in appearance, and less friable than the other inclusions, it was necessary to etch the inclusion in relief before extraction. UN inclusions etched sufficiently in relief in the electrolytic polishing solution described in Methods I and II by increasing the polishing time. UN inclusions were relief etched by extending the

Jan 1, 1957

By J. R. Kyte, L. A. Rapoport, R. J. Stanclift, S. C. Stephan

Experimental studies covering a wide range of core materials and fluid properties have been conducted to determine the mechanism of oil displacement by water in a partially gas-saturated porous medium. In all instances, the presence of a gas phase was found to have a beneficial effect in reducing residual oil saturations. The practical significance of this benefit is discussed, and a simplified procedure is outlined for evaluating the effects of free gas on water flooding by means of short core tests. INTRODUCTION In addition to oil and water, reservoirs subjected to water flooding frequently contain, also, a gas phase. Common engineering procedures account for the presence of this "free gas" only from the viewpoint of volumetric balance, implying that the only role of the gas consists of providing "fill up" space. It is usually visualized that during the initial stages of the water invasion, the oil, moving ahead of the water, displaces part of the gas and that subsequently the remaining portion of the gas phase is totally compressed and dissolved in the advancing oil bank. Thus, consideration of a two-phase, water-oil flooding mechanism supplies an adequate basis for predictions of oil recovery if the pressure build-up caused by the flood is sufficiently great, so as to reduce the free gas saturation to a negligible value in any portion of the reservoir by the time that portion is reached by the advancing flood water. In many in- stances, however, waterflooding operations are carried out when the reservoir pressure is still relatively high SO that the pressure build-up associated with the water flood may not result in complete dissipation of the gas phase. Under such circumstances it is necessary to ascertain whether or not the presence of free gas has an effect on waterflood behavior and, if so, to account for any such effect in the evaluation of field operations. The difficulties encountered in attempting to arrive at a comprehensive picture of the displacement mechanism of oil by water in the presence of free gas stem from the fact that most of the published data on this subject were obtained under conditions that were either not clearly representative of those existing in a reservoir or not sufficiently controlled to permit evaluation of the effects specifically caused by the gas phase. Some of the most precise data found in the literature were obtained in tests using a "static" gas phase created prior to each water flood by circulating oil through partly gas-saturated cores until a "trapped," residual gas saturation was established throughout the system.' Other investigations were conducted under more representative conditions where the gas phase was free to move during the water flood: but in most cases the results of these tests were obscured by auxiliary phenomena which arise from the compressibility and solubility of the gas and preclude quantitative conclusions.2,3,4 Prior to water flooding, a reservoir usually contains oil and gas, distributed in a manner in which both are free to move. Thus, the principal objective of the present studies was to determine the type of displacement mechanism occurring when water invades a porous medium containing oil and a "mobile" gas phase. Further-

Jan 1, 1957

By Fred A. Webber

STEEL ROPE WIRE is one of the more specialized commodities among the many grades of highcarbon steel wires. In its production there are many metallurgical aspects of interest from the steelmaking on through the final stages of wire drawing. We produce rope wire in an integrated mill com prising all the operations from the blast furnaces to finished wire drawing in the wire mills. Steelmaking is carried out with close control on hot metal, selection of scrap, and fluxing materials. The basic open hearths are of 170 tons capacity. Steel is teemed into 19 1/2 in by 19 1/2 in big-end-down molds and is hot-topped with the use of clay refractory hot-tops. The weight of this ingot is 6,900 pounds. All high -carbon steel ingots are charged hot into the soaking pits and are then rolled through the blooming mill in 16 p asses to a bloom ax~ in. by 41/2 in. and approximately 65 feet long. Necessary bottom and top crops are taken on the bloom as it passes from the blooming? mill to the billet mill. The still hot bloom is continuously rolled through the billet mill in . 5 passes to a 2 3/8 in. square. Billets are cut to 32 feet in length by a flying shear and then allowed to cool on the hot bed.

Jan 1, 1957