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By George R. Elliott

Methods are presented for measuring and comparing "degree" of water drive, and for observing the control that rate of withdrawal exerts over decline of reservoir pressure. Degree of water drive is studied from pressure-production curves of 10 reservoirs; the method used to present these comparatively is to convert cumulative oil production from barrels to percentage of ultimate. Degree of water drive is also represented by a "water-encroachment factor," representing barrels of water influx per pound-month per acre-foot of oil reservoir. Pressure-production curves for the water-drive reservoirs after a period of declining pressure show a diminishing angle of slope, in some cases to the point where pressure ceases to decline or where it even increases; the shapes of these curves are in marked contrast to the dissolved-gas type of curve, which shows a general trend toward zero pressure at ultimate oil recovery. Yearly rate of oil production in percentage of ultimate oil recovery is correlated with pressure decline. The correct rate of production of oil with its associated gas and water sustains pressure in reservoirs having a high water-encroachment factor. For reservoirs having a low water-encroachment factor, it is necessary to inject the produced water and even inject large volumes of water from an outside source. The discussion of the actual reservoirs is preceded by a general review and is followed by a substantial bibliography. It is now generally accepted that water drive is capable of yielding 60 to 80 per cent of the original oil in place in most reservoirs, as compared with 20 to 40 per cent for dissolved-gas drive. There is no need to question the importance of controlling a reservoir in order to take advantage of such an efficient mechanism. What is a water-drive reservoir? Oil reservoirs usually combine two or more of the four basic mechanisms: dissolved-gas drive, gas-cap drive, water drive, gravity drainage. A water-drive reservoir is one in which water advances to take the place of the oil and gas produced. When the oil withdrawal rate is sufficiently low, the water will tend to maintain pressure. The maximum effectiveness is attained when the water follows the oil withdrawal so closely that little or no decline in pressure occurs. Oil in its underground reservoir is associated with water. This water is significant in the production of the oil according to the source of supply and the permeability of the surrounding formation. As oil is produced and the pressure is lowered, water can move in to replace the oil. With adequate supply and sufficient permeability, actual movement takes place on an extensive scale. The first movement of water takes place by expansion of the water and its associated fluids. While this expansion is of little importance in some fields, in others it is sufficient to supply all of the energy required for the production of oil. When a pressure differential has been established

Jan 1, 1946

By George R. Elliott

Methods are presented for measuring and comparing "degree" of water drive, and for observing the control that rate of withdrawal exerts over decline of reservoir pressure. Degree of water drive is studied from pressure-production curves of 10 reservoirs; the method used to present these comparatively is to convert cumulative oil production from barrels to percentage of ultimate. Degree of water drive is also represented by a "water-encroachment factor," representing barrels of water influx per pound-month per acre-foot of oil reservoir. Pressure-production curves for the water-drive reservoirs after a period of declining pressure show a diminishing angle of slope, in some cases to the point where pressure ceases to decline or where it even increases; the shapes of these curves are in marked contrast to the dissolved-gas type of curve, which shows a general trend toward zero pressure at ultimate oil recovery. Yearly rate of oil production in percentage of ultimate oil recovery is correlated with pressure decline. The correct rate of production of oil with its associated gas and water sustains pressure in reservoirs having a high water-encroachment factor. For reservoirs having a low water-encroachment factor, it is necessary to inject the produced water and even inject large volumes of water from an outside source. The discussion of the actual reservoirs is preceded by a general review and is followed by a substantial bibliography. It is now generally accepted that water drive is capable of yielding 60 to 80 per cent of the original oil in place in most reservoirs, as compared with 20 to 40 per cent for dissolved-gas drive. There is no need to question the importance of controlling a reservoir in order to take advantage of such an efficient mechanism. What is a water-drive reservoir? Oil reservoirs usually combine two or more of the four basic mechanisms: dissolved-gas drive, gas-cap drive, water drive, gravity drainage. A water-drive reservoir is one in which water advances to take the place of the oil and gas produced. When the oil withdrawal rate is sufficiently low, the water will tend to maintain pressure. The maximum effectiveness is attained when the water follows the oil withdrawal so closely that little or no decline in pressure occurs. Oil in its underground reservoir is associated with water. This water is significant in the production of the oil according to the source of supply and the permeability of the surrounding formation. As oil is produced and the pressure is lowered, water can move in to replace the oil. With adequate supply and sufficient permeability, actual movement takes place on an extensive scale. The first movement of water takes place by expansion of the water and its associated fluids. While this expansion is of little importance in some fields, in others it is sufficient to supply all of the energy required for the production of oil. When a pressure differential has been established

Jan 1, 1946

By D. O. Noel

IT is, of course, expected that manufacture of the various metal powders should involve numerous methods adapted to the specific characteristics of the metals themselves. Several methods for powdering a particular metal may be available, but the physical characteristics of the powder as produced by the several methods may be quite different. In the final analysis, the application of the metal powder dictates the physical properties that the metal powder must possess, and this, to a very large extent, will determine which of several possible methods of manufacture is adopted. Sometimes powder of the same metal is produced by more than one method, each powder having specific characteristics that make it particularly suitable for its application. For purposes of classification, the various methods of powdering metals can be grouped as follows: 1. Machining. 2. Milling (by ball mills, stamps, attrition mills, etc.). 3. Shotting (pouring molten metal into water, air, etc.). 4. Granulation (by stirring molten metal while solidifying). 5. Atomizing (disintegrating by steam, compressed air, etc.). 6. Condensation of metal vapor. 7. Reduction of oxide powders. 8. Chemical precipitation. 9. Electrolytic deposition. 10. Sintering (for producing alloy powders). 11. Formation of an alloy followed by dissolving or otherwise remov-ing one of the alloying constituents.

Jan 1, 1938

By H. B. Pulsifer

ABOUT 15 varieties, or modifications, of the best magnesium available were prepared and subjected to etching tests, then examined for microstructure. Of the 30-odd etching reagents that were tried, nearly half, mostly ammonium salts, etched the metal satisfactorily. The surfacing and etching of magnesium is shown to be a very simple and quick operation. The density and hardness of magnesium were determined. The most interesting new observations relate to the finding of the hexagonal etch figures, the crystal laminations, and the fact that the metal is plastic, cold, when restrained or quickly deformed. Under slowly applied pressure cold metal deforms slightly, then shears to fracture without plastic flow: The chief structural features of magnesium are presented in two reduced photographs and 30 photomicrographs.

Jan 1, 1927

By H. M. Ziesemer

PRIOR to 1909 that mountain of porphyry, known as. Sacramento Hill, had remained hardly touched but had always aroused suspicions as to the presence of ore within.. During that year, exploratory work was started by underground methods; drifting and raising continued until 1913. It was proved that a mineralized zone existed, the limits of which had not been determined; so, because of the lower costs of exploratory work and the greater desirability of vertical sections, it was decided to prove the extent of the ore zone by churn drills. Drilling continued until the year 1917, when it seemed almost certain that the horizontal limits of the orebodies had been determined. Ore continued in depth in one direction beyond a point where it was economical to explore by churn drilling; this extension is still being developed by underground methods. The irregularities of the boundaries of the ore zones, together with the variable grades of ore encountered, made it necessary to drill on the corners of 100-ft. squares. Two ore zones were proved, known as the East and West Orebodies. The Sacramento Hill porphyry stock intruded into the Dividend fault. The fault ran roughly east and west with a dip to the south, having pre-Cambrian schists on the north against Paleozoic limestone on, the south. This intrusion was accompanied by a silica breccia on the south periphery, along the limestone contact side. The ore lay in the silica breccia and in the porphyry, some distance from the breccia. No ore was found in the heart of the porphyry mass on the north side, along the schist contact. The West Orebody is elliptic in shape, having a major axis of 1200 ft. (366 m.) and a minor axis of 800 ft. (244 m.); these diminish with depth until, at 300. ft., the axes are 500 ft. and 300 ft., respectively. The ore consists of chalcocite, some bornite, chalcopyrite, and considerable pyrite in a silicious gangue. About 30 per cent. of the copper is caused by

Jan 2, 1922

By J. J. Kanter

There has been much research and commercial development in recent years in the use of chromium and nickel in steels of various types, including those intended for high-temperature service. By "high-temperature steels" are meant those specifically designed for service at elevated temperatures in steam plants, oil refineries and other industries where high-temperature operations are conducted. This paper is devoted to some preliminary data on the effect of silicon on certain of the most popular chromium-molybdenum steels now being used in quantity by the refining industry and includes a short statement on the influence of copper in steels intended for high-temperature service. Uses of Silicon Next to oxygen, silicon is the most widely distributed and abundant of the earth's substances. Although classed as a nonmetal, it is highly important in the metallurgy of all steels, having been used for years as an efficient and economical degasifier and deoxidizer. Silicon is added to various steels in the form of ferrosilicon, generally at the end of the heat so as to avoid oxidation losses. With acid steels it is added in the furnace (also in the ladle) and generally with basic steels is added in the ladle, so as to avoid reaction with the basic lining through high-temperature acidic reaction with silica, which may be formed by oxidation of the silicon alloy. Several grades of ferrosilicon are available, containing, respectively, 15, 50, 75 and 90 per cent Si. By far the largest tonnage produced is the 50 per cent grade although the 75 and 90 per cent ferro-silicons are used as ladle and furnace additions in the manufacture of steels of high silicon content. The introduction of silicon into steel as an alloying element is well known in connection with high-yield-strength constructional steel for bridges, ships, car construction, etc., and it is also well known as an alloy-

Jan 1, 1938

By J. J. Kanter

There has been much research and commercial development in recent years in the use of chromium and nickel in steels of various types, including those intended for high-temperature service. By "high-temperature steels" are meant those specifically designed for service at elevated temperatures in steam plants, oil refineries and other industries where high-temperature operations are conducted. This paper is devoted to some preliminary data on the effect of silicon on certain of the most popular chromium-molybdenum steels now being used in quantity by the refining industry and includes a short statement on the influence of copper in steels intended for high-temperature service. Uses of Silicon Next to oxygen, silicon is the most widely distributed and abundant of the earth's substances. Although classed as a nonmetal, it is highly important in the metallurgy of all steels, having been used for years as an efficient and economical degasifier and deoxidizer. Silicon is added to various steels in the form of ferrosilicon, generally at the end of the heat so as to avoid oxidation losses. With acid steels it is added in the furnace (also in the ladle) and generally with basic steels is added in the ladle, so as to avoid reaction with the basic lining through high-temperature acidic reaction with silica, which may be formed by oxidation of the silicon alloy. Several grades of ferrosilicon are available, containing, respectively, 15, 50, 75 and 90 per cent Si. By far the largest tonnage produced is the 50 per cent grade although the 75 and 90 per cent ferro-silicons are used as ladle and furnace additions in the manufacture of steels of high silicon content. The introduction of silicon into steel as an alloying element is well known in connection with high-yield-strength constructional steel for bridges, ships, car construction, etc., and it is also well known as an alloy-

Jan 1, 1938

By W. H. Coghill, A. M. Gow, M. Guggenheim, A. B. Campbell

The object of this paper is to discuss the fundamental principles of ball milling and to present some observations which have been made in laboratory and plant investigations. The discussion will be limited to wet grinding of ores in cylindrical mills, but doubtless many of the principles involved will be equally applicable in the other fields of fine grinding in which mills of the same type are used. In the concentrators of the United States there are about 650 ball, rod, or pebble mills, operating or ready to operate, and these have about 100,000 connected horsepower. For grinding in cement plants there is about three times this connected horsepower, and other industries have an unestimated amount, all used for the general type of grinding that is to be discussed here. It is true that these figures do not represent stupendous amounts of power, but when one considers that ball milling is often the ((bottle neck" in a concentrator and that it often accounts for the largest single item in the cost sheet, the importance of a comprehensive understanding of the principles of ball milling can be appreciated. Much of the past literature devoted to the subject has been concerned with the Kick-Rittinger dispute over evaluating grinding, or with dissertations on ball paths and the closely allied impact versus attrition hypotheses, or with the exclusive consideration of certain specific variables, such as mill speed or circulating load, irrespective of the other factors in operation. Such subjects may be dismissed with but little discussion in what may be called, by comparison, a new philosophy in the study of ball milling. Briefly, this '(new philosophy" consists of using power as an index of the mill operation, and investigating grinding from the standpoint of set and induced varisbles, with emphasis on the latter.

Jan 1, 1935

By R. E. Shinkosk

This paper outlines the development of a program for increasing the life of woolen bags used for filtering Dwight-Lloyd gases by treating the bags and gases with hydrated lime. Methods and apparatus are described for determining alkalinity of dusts, acidity and breaking strength of bag cloth. Procedure and results, based on several years of operation, are presented. DURING 1939, additional facilities were constructed in the Dwight-Lloyd Blast Furnace and Baghouse departments at the Selby, California, Plant of the American Smelting and Refining Co. In order to handle adequately the increased volume of gases from the resultant increase in production, it was necessary to increase gradually the amount of water used for cooling gases ahead of the sinter machine baghouse. As a result of this increased water cooling, the average bag life dropped from 27 months in 1939 to 14 months in 1941. (Table I). This drop in life meant an increased. bag cost, as well as lower recovery of dust and some curtailment of operation. During 1941, it was found new bags showed as high as 0.3 pct acidity* after two weeks of opera- tion and as much as 2.0 pct acidity after some months of operation. This high acidity was present in spite of the fact that free oxide or relative alkalinity of the unburned dust ran from 5 to 6 pct. In view of these circumstances, a twofold program was started in Nov. 1941.t Part one of this program consisted of vigorously dipping all new bags in a weak lime solution, containing 50 lb of hydrated lime per 50 gal of water. Part two consisted of feeding fine, dry, hydrated lime into the gas stream intake of the sinter baghouse fan. Apparatus for feeding this lime is shown in fig. 1. All baghouse chambers are shaken in rotation about once each hour. On alternate hours, the baghouse operator places 50 lb of hydrated lime (one sack) into the lime feeder, starts feeder and immediately starts the bag shaking machinery. The rate at which lime is fed is set to coincide with the approximate time necessary to shake all sinter bag-house chambers, or about 15 min. It is felt this method of lime addition is most effective for getting lime into the woolen bag fabric. The amount of lime so fed averages about 600 lb per day. The amount of lime fed per day is varied to keep a minimum relative alkalinity of 9 pct in the unburned sinter dust. A daily dust sample is taken for alkalinity by allowing dust to accumulate in a sample pipe over a 24-hr period. This sample pipe, placed in any chamber cellar, is 2 in. in diam, 4 ft long, is sealed on the inner end, and capped on the outer end. It has a 1/2 in. slot cut for 18 in. along the tip end. This slot faces upward and allows the pipe to fill gradually with dust as bags are shaken. Breaking strength of bags has, in most cases, been the deciding factor in bag replacement. Bags that normally test 100 psi breaking strength when new are replaced when they test under 35 lb. The method for determining breaking strength is shown in the description accompanying fig. 2. Since the start of the liming program in 1941, bag life has increased from 14 months to an average of over 23 months, with a consequent material decrease in bag cost per year. Acidity, as per cent sulphuric acid, may be determined by means of a Beckman pH meter as follows: From a piece of bag cloth. which has been thoroughly cleaned of dust, a 5 g sample is weighed on a balance. Cut the sample into fine pieces and place in a 400 cc beaker. Add 100 cc (measured) of distilled water and stir vigorously. Filter on suction funnel, holding cloth pulp in beaker with a stirring rod. Wash cloth sample and filter wash water four additional times, each time with 20 cc distilled water, the last time squeezing cloth pulp over funnel. Discard pulp and rinse funnel and filter paper. Pour wash solution jnto measuring graduate and make up to exactly 300 cc with distilled water. Place into clean 600 cc beaker and measure the pH on meter. The per cent acid in bag cloth is read from the following table:—

Jan 1, 1951

By D. K. Crampton

THE study of copper alloys of the age-hardening type has received considerable attention, and, among the alloys which the authors have considered, those containing small amounts of nickel and phosphorus as essential constituents seem especially interesting. Such alloys have attractively great capacity for being hardened and also have relatively high electrical and thermal conductivity in the hardened state. In addition, it has been found that the increase in hardness and strength imparted by aging can be greatly augmented by cold-working, so that axcellent combinations of conductivity and strength are obtainable. In view of the possible importance of the alloys, it was considered desirable to investigate the solubility relationships in the copper-rich portion of the copper-nickel-phosphorus system. This paper presents some of the results obtained in this investigation to date and also gives properties of typical alloys that appear to be of commercial interest.

Jan 1, 1940

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Jan 1, 1938

Schedule of Events

Jan 1, 1977

By Michael Tenenbaum

The importance of semikilled steel as a high tonnage grade has long been recognized. The increasing severity of the applications for which semikilled steel is used makes it desirable to obtain further information regarding the features of open hearth practice and ingot structure that can affect steel performance in subsequent rolling and fabricating operations. Accordingly, an investigation is being carried out studying the structure of various types of semikilled steel ingots. This paper reviews some of the observations made and information gathered in this investigation. By definition, semikilled steel may be considered to include all nonrimming steels in which the natural shrinkage occurring during ingot solidification is offset to an appreciable degree by gas formation. Accordingly, this type of steel includes the entire range intermediate between rimmed and fully killed steel. The resultant ingot structures range from those of steels that have been capped to suppress a weak rimming action to those steels that have been killed in the furnace or ladle to the extent that no mold deoxidizer is required. A survey reported to the 1946 -AIME Open Hearth Conference' reviewed the practices being used at 28 major plants for the deoxidation of semikilled steel. It was found that most plants divide the deoxidizing additions between the ladle and the mold—many of the plants adding only minor amounts of deoxidizer to the bath or none at all. Silicon, aluminum and titanium were the only elements used for ladle and mold deoxidation. Mold deoxidizers were added as capping additions or as uniformly fed additions. Several practices were reported in which the steel was deoxidized in the ladle to the extent that little or no mold deoxidation was needed. No reference was made to grades capped by using special mold designs or special closures over the top of molds. .Accordingly, specific examples of this type of practice will not be considered in this paper. It appeared from this survey of deoxidation practice that semikilled steel can be divided into three types, namely, capped semikilled, in which aluminum is added near the end of pour or after shut-off, intermediate semikilled steels, in which aluminum is fed uniformly throughout the pour, and semikilled steels requiring no mold deoxidation. In an attempt to cover the ingot structures obtained by the range of practices reported in the preceding survey, three series of experimental heats were made using increasing amounts of aluminum, silicon and titanium for ladle deoxidizers. The ladle deoxidizers were added as stick aluminum, 50 pct ferrosilicon and 20 pct ferrotitanium (4 pct carbon), respectively. Two methods of studying ingot structures were used. Ingots were removed from production, burned longitudinally and machined to allow observation of the central pipe and coarse blowholes. During the machining operation much of the finely porous subsurface structure was obliterated. Accordingly, observations were also made

Jan 1, 1949

By Michael Tenenbaum

The importance of semikilled steel as a high tonnage grade has long been recognized. The increasing severity of the applications for which semikilled steel is used makes it desirable to obtain further information regarding the features of open hearth practice and ingot structure that can affect steel performance in subsequent rolling and fabricating operations. Accordingly, an investigation is being carried out studying the structure of various types of semikilled steel ingots. This paper reviews some of the observations made and information gathered in this investigation. By definition, semikilled steel may be considered to include all nonrimming steels in which the natural shrinkage occurring during ingot solidification is offset to an appreciable degree by gas formation. Accordingly, this type of steel includes the entire range intermediate between rimmed and fully killed steel. The resultant ingot structures range from those of steels that have been capped to suppress a weak rimming action to those steels that have been killed in the furnace or ladle to the extent that no mold deoxidizer is required. A survey reported to the 1946 -AIME Open Hearth Conference' reviewed the practices being used at 28 major plants for the deoxidation of semikilled steel. It was found that most plants divide the deoxidizing additions between the ladle and the mold—many of the plants adding only minor amounts of deoxidizer to the bath or none at all. Silicon, aluminum and titanium were the only elements used for ladle and mold deoxidation. Mold deoxidizers were added as capping additions or as uniformly fed additions. Several practices were reported in which the steel was deoxidized in the ladle to the extent that little or no mold deoxidation was needed. No reference was made to grades capped by using special mold designs or special closures over the top of molds. .Accordingly, specific examples of this type of practice will not be considered in this paper. It appeared from this survey of deoxidation practice that semikilled steel can be divided into three types, namely, capped semikilled, in which aluminum is added near the end of pour or after shut-off, intermediate semikilled steels, in which aluminum is fed uniformly throughout the pour, and semikilled steels requiring no mold deoxidation. In an attempt to cover the ingot structures obtained by the range of practices reported in the preceding survey, three series of experimental heats were made using increasing amounts of aluminum, silicon and titanium for ladle deoxidizers. The ladle deoxidizers were added as stick aluminum, 50 pct ferrosilicon and 20 pct ferrotitanium (4 pct carbon), respectively. Two methods of studying ingot structures were used. Ingots were removed from production, burned longitudinally and machined to allow observation of the central pipe and coarse blowholes. During the machining operation much of the finely porous subsurface structure was obliterated. Accordingly, observations were also made

Jan 1, 1949

I. N. KNAPP, Ardmore, Pa. (written discussion*).-Captain Lucas has made an important contribution to our, knowledge of Belle Isle, especially as to the outline of the sulphur deposit, and the pronounced irregularity of the salt surface. I agree with his view, that the elevation or mound that constitutes Belle Isle may consist of several salt domes formed at different periods. It may be interesting to note the high gas pressure encountered in pockets in the salt by my No. 1 Belle-Isle well. While drilling a dry hole with cable tools, we sometimes struck. pockets of gas which would float the tools, so that drilling had to be suspended sometimes for several hours at a time, until the head of gas was exhausted, and this with a string of tools, 5-in. (127 mm.) stem 36 ft. (10.9 m.) long, that weighed complete about 3500 lb. (1587 kg.). At about 1800 ft. (548 m.), we struck the largest gas pocket and the string of tools was thrown up and nearly out of the hole. When it dropped back it made several loops

Jan 1, 1918

By Stephen Taber

A vein may be defined as an aggregation of mineral matter, more or less tabular or lenticular in form, which was deposited from solution and is of later origin than the inclosing rock. This definition differs from the one found in many text-books in that no assumption is made as to the origin of the space occupied by the vein or the manner in which the mineral matter was deposited. In the present paper the writer purposes to discuss the mechanics of vein formation, and does not wish to begin by begging the question. The origin of ore deposits has been diligently investigated in recent years, but, while much has been written concerning the chemistry of the process, the physical side of the question has received less attention. The source of the ore minerals; the chemical composition of ore-bearing solutions; the relative importance of magmatic and meteoric waters as agents of concentration; and the causes of mineral precipitation have all been discussed at length. On the other hand, little has been written concerning the mechanics of vein formation, and the theories given in text-books today are essentially the same as those developed by the early Cornish and Saxon miners. Early investigators often regarded both veins and dikes as igneous in origin, but today the theory that vein minerals have been deposited from solutions, either liquid or gaseous, is firmly established. The latter view is supported by the fact that many vein-forming minerals are not found in unaltered igneous rocks; by evidence obtained in the laboratory regarding the solubility of minerals; by the presence of many ore minerals in hot-spring waters; by the occurrence of some veins in regions consisting exclusively of unaltered sedimentary rocks; by evidence as to the temperature at which some minerals are formed; and by the absence of mineral segregation due to difference in specific gravity. There is still, however, much difference of opinion as to whether certain tabular-shaped masses should be classed as veins or as dikes. Some of the earlier investigators have also advocated the theory that veins are contemporaneous in origin with the inclosing rock, while others have believed the vein minerals to represent a recrystallization or transforma-

Jan 1, 1920

By J. W. Galpin, V. L. Minear, F. C. Sturges, B. H. Mott, R. H. Allen, W. W. Weigel, Wm. D. Owsley, R. E. Moeller

By definition the word "grout" means a thin mortar, or a kind of plaster or ce¬ment, and "grouting" means to fill up or finish with grout. The words "cement," "plaster" and "mortar" mean a substance that is used in a soft state which subsequently hardens. Thus, grouting is the filling of void space with a substance that hardens. Construction cements are the most common substances used, either by themselves or in mixtures, but the term grouting is applied quite correctly when other substances such as plastics and certain chemicals are used. Also, the use of the term grouting to cover the filling of voids with materials that do not actually become hard, such as the-flotation tailings used in grouting in the southeast Missouri lead district, should be considered correct, as some stiffening does take place and, anyway, it is a better descriptive term than any substitute. Engineers are interested in grouting because some of the materials with which they must work contain voids, and certain conditions can be improved if these voids can be filled with something solid and permanent. Grouting is done to accomplish several purposes: I. To stop the passage of fluids and gases, 2. To cement materials together to make them stronger, and 3. To prevent consolidation of materials by filling void space with something solid as a replacement for the air and water that could be forced out under load. The construction industry uses grouting extensively for all three purposes. Grouting is used to stop water percolation under and around dams. It is used to control water flow in tunnel driving and in shaft sinking. It is used to improve foundation conditions under civil engineering structures by permanently filling void space and thereby reducing settlement, or by cementing broken rock together and increasing its supporting strength. The oil and gas industry does a lot of grouting, primarily to stop the passage of gases and fluids. The search for oil at increasingly greater depths has meant greater investment per well, and the oil industry has spent large sums on development of improved drilling methods. This

Jan 1, 1948

By N. P. Goss

ASTERISM appearing in X-ray Laue dia-grams is an extremely sensitive index of changes in the internal structures of indi-vidual grains of polycrystalline metals. It indicates the existence of various forms of subboundary structure or subdivision within the grain. The present viewpoint is that the grain is made up of lattice blocks having substantially the same size and shape.1-4 When these blocks all assume exactly the same orientation, the crystal is perfect and asterism is absent. Cleaves and Thompson5 observed that the hardness of iron is virtually constant over a range of grain sizes. It is quite possible that the subboundary structure caused this, and that the latter is just as important as grain size itself. While the experiments reported here are not con-clusive, they do support this viewpoint. Metals can, under certain conditions, be prepared entirely free from asterism, but this preparation does not necessarily require long heating or slow cooling, as will be shown here. In this paper a distinction is made be-tween mosaic and distorted grain struc-tures but the difference is only a matter of degree. In a previous paper9 it was shown that the grains can become distorted even during heat-treatment. The block structure exists inherently, even in a perfect crystal; the size and shape of these crystallites, or lattice blocks, varies, depending upon a number of factors. Goetz, for example,7 has shown that a metal before crystallizing from the molten state must go through a paracrystalline phase with oriented groups of atoms about 10-14 to 10-15 c.c., or 10 5 cm. in size.

Jan 1, 1940

By M. van Swaay, C. E. Birchenall

A. S. lBrling (Johnson, Matthey & Co. Ltd., Laboratories)— Because of its initial emphasis upon the production of membranes by powder metallurgy and by normal casting and rolling techniques, this paper is of considerable interest to those concerned with the design and application of industrial diffusion units. As the subsequent performances of the three grades of palladium were not compared in detail, it can perhaps be concluded that specific permeabilities were very similar. A short table in which the absolute diffusion rates obtained by the Authors with their three grades of palladium were compared with those of other investigators18-25 would, however, have been of particular value in view of the very variable results obtained with this membrane material. The Authors state early in the paper that the permeability of the thoriated samples decreased in much the same way as that of the nonthoriated samples. Later, they emphasize that sintered palladium without thoria was very susceptible to poisoning and did not respond as well as the other materials to the decontamination treatment. These results, which suggest that sintered membranes are less effective than those produced by normal methods, have considerable industrial implications, and amplified experimental details would be very welcome. The results of the Authors differ in one important respect from those of other investigators. Thus, no "bleeding" was required to maintain a constant rate of diffusion, although Davis, Darling, and De Rosset found this to be necessary. Davisz3 found that "bleeding" was necessary even when the hydrogen had already been purified by diffusion through a palladium tube, and it would be of value to know the purity of the gas stream emerging from the purification train shown on Fig. 1 of the Authors' paper. The Authors show that diffusion rates varied according to the square root of the pressure difference providing that the palladium membrane was not contaminated in any way. This finding is in agreement with the results of those workers2,18,19,23,24 who diffused their hydrogen through the membrane into a partly or completely evacuated system.Those workers who did not find this square-root law dependence did not have a partial vacuum on the downstream-side of the membrane.'' The difference between the two experimental con- ditions appears to be significant, as the absolute diffusion rates per sq cm of diffusion area are lower when the square-root law dependence is not observed. While the effect could be attributable to poisoning of the membrane it is conceivable that a positive pressure on the downstream side of the membrane might influence the mechanism of diffusion. In view of the capricious behavior of palladium, factors of this type, which are likely to influence its industrial significance, should be carefully considered. M. van Swaay and C. E. Birchenall (authors' 9-eply) — Our Eq. 191 may be compared with several others for hydrogen diffusion in palladium: D = 5.95 x exp (-5770/1)' D = 3.55 x 10"3 exp (-5550/)' D = 4.3 x 10"3 exp (-5620/1')' Other values are given in the literature, but in many cases surface poisoning may have affected the results. No analysis was performed on the hydrogen gas stream after purification. It should be noted that the presence of liquid nitrogen traps near the heated membranes may have set up convection currents and provided the equivalent of "bleeding." The question of whether a partial vacuum existed on the downstream side of the membrane is not clear. Does it imply that there is something unique about the permeability measured near one atmosphere pressure? We do not believe that there is. When square root pressure dependence is not observed, diffusion rates are not measured. Is "absolute diffusion rate per sq. cm. of diffusion area" equivalent to permeability? The terminology is new to us. In any case we doubt very much that pressures of the order of several atmospheres can affect the mechanism of diffusion.

Jan 1, 1962

By R. Bakish, M. A. Badiali, N. W. Kirshenbaum

One pound of ultra pul-e molybdenum has been produced containing both metallic and nonmetallic impuvities close to or less than the limits of detection. various purification methods were investigated; althouglz the use of move than one purification step was consideved, it was found that a single, caefully-controlled sublimation of MoCl5 yielded a highly puvified product without prior treatment or recourse to repeated sublimation. Hydrogen reduction of MoC1, to metal was attempted at atmospheric pressure; however, reduced pressure was necessary to obtain substantial yields. The tubular deposits of metal were consolidated into bulk fovm by electron beam melting undev high vacuum yielding a very low gas content. Boblems involved in monitoring the puvity of these materials and analytical results obtained are also presented. THE pronounced effect of even trace amounts of impurities upon fundamental properties of materials is well known to metallurgists and solid-state physicists. Consequently, groups interested in basic studies of metals have in recent years immensely stimulated the preparation and production of numerous ultra-pure metals. Increased demand by scientists for these high purity materials has necessitated development of facilities to prepare them in significant quantities; the procedures reported here were devised to produce significant quantities of ultra-pure molybdenum. Previous work performed in the field of vapor phase purification and hydrogen reduction of several other refractory metal chlorides had demonstrated valuable techniques applicable to molybdenum.' Various purification and reduction steps were individually investigated. Those procedures which showed the most favorable results with respect both to attainment of high purity and to ease of operation were then incorporated in the process utilized to produce the metal.' STARTING MATERIALS It is well known that because of differences in volatility, chlorides may be separated by fractional distillation. It was presumed that distillation of molybdenum pentachloride offered a simple and straightforward method of purification due to its relatively low boiling point. Alternatively, sublimation of the solid chloride also appeared feasible since MoC15 has both a reasonably narrow temperature range in which it exists as a liquid (a property typical of refractory metal chlorides) and a low enthalpy of sublimation. Pertinent thermochemical data of MoC15 are given in Table I. It should be noted that this compound must be handled with care as it is extremely hygroscopic. Anhydrous MoC15 was obtained from the A Metal Climax Co. METHODS OF PURIFYING MOLYBDENUM PENTACHLORIDE Distillation. It was expected that distillation methods, while affording an efficient purification, would prove simple to control and would have a higher production rate than sublimation processes. Also considered was the possibility of effecting a high degree of purification by using both these volatilization methods in conjunction—possibly a distillation followed by sublimation of the solidified condensate. Distillation of MoC15 was investigated using a single stage distillation column packed with chemically resistant glass beads. Heating coils were wound around the column and collection tube (condenser). As-received MoCl5 was charged into a flask connected with the column using a side loading arm under an argon flow. After the column and condenser were brought to about 270" and 210°C, respectively, the apparatus was lowered until the flask was fully immersed in a constant temperature fused salt bath maintained at about 285 °C. Distillation was continued for about 10 or 15 min until 50 to 70 g of distillate had been collected. Analyses of these distillations indicated that several elements, e.g., Cu, Fe, Ni, Cr, and Mg, were lowered in quantity although not all were removed to the same extent. The occurrence of Na, B, Si, and A1 in the distillates appeared to be due to contamination, possibly from corrosion of the pyrex glass. An improved distillation system of larger capacity and longer distilling column was built. Improvements were effected in lowering the amounts of such impurities as B, Mn, Ni, Na, Mg, Cr, Cu, and Fe. These studies were pursued concomitantly with efforts to purify by sublimation; it was subsequently found that although improvements in purity were obtained by distillation, sublimation processes were simpler to control and effected a high degree of purity.

Jan 1, 1963