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By Paul L. Russell

THIS is a progress report of an experiment being undertaken in cooperation with the Bethlehem Steel Corp., the Crucible Steel Co., and the Rock Bit Sales and Service Co., involving heat treatment of the shank ends of drill steel. This experiment is being conducted by the U. S. Bureau of Mines in its experimental mine, Mining Research Branch, Bluemont, Va. The purpose of the experiment is to determine the effect of an increase in the time the steel soaks in the furnace during the hardening heat. It has been thought that increasing this time produces a soft zone below the lugs resulting in a metallurgical notch that causes early failure. Each of the steel companies furnished enough 11/4 - in. straight carbon, hollow, round steel to make up 10 sets of drill steel, in each instance the steel bars were from the same heat. These sets of drill steel, consisting of 2-ft, 4-ft, 6-ft, and 8-ft lengths were fabricated by the Rock Bit Sales and Service Co. Special attention was given to the forging of the steel to produce the best rods possible. The heat treatment of all thread ends was identical and followed the best practice. The heat treatment of the shank ends of five sets of steel from each company produced a soft zone 2 to 4 in. in front of the lugs. It was decided that possibly the best way to obtain this effect was not to overlap the hardening heat but to let the steel soak for an additional 30 min before quenching. Therefore the only variable in the test steels is the length of time the shank ends were in the furnace. The remaining drill steel shanks were treated as follows: Heat treatment in pyrometer-controlled furnace at 1550°F. Quenching oil at 105°F to 125°F temperature. Areas for heat treatment were; shanks, 11 in.; threads, 9 in. Time at heat, standard practice, 20 min for 11/4-in. steel. Actual drilling tests were made in greenstone, (a metamorphosed basaltic rock), and in epidosite. Greenstone has a specific gravity of 2.96 and a compressive strength of 44,200 psi. Epidosite has a specific gravity of 3.26 and a compressive strength of 63,100 psi. All drilling tests were made using a 31/2-in. column-mounted, automatic feed drifter, with a controlled air pressure of 90 psi at the throttle. Tungsten-carbide bits of 2 in. diameter were used for all drilling. Contrary to expectations the drill steels that were allowed to soak for the additional 30 min before quenching performed better than the steels that were heat treated according to standard practice. This performance, as shown in Table I, was especially noticeable in the drilling of epidosite. The "longheat" drill steels furnished by Company "A" drilled 154 pct more minutes than the "standard-heat" steel. Expressed in feet, the "long-heat" steel drilled 114.60 ft more before failure than the "standard-heat" steel. The "long-heat" steel furnished by Company "B" drilled 37 pet more minutes or 60.39 ft more before failure than the "standard-heat" drill steel. The effect of the long heat treatment was not as evident when the steels were drilling in greenstone (Table II). In greenstone, the increase in minutes drilled by the "long-heat" steel over the "standard-heat" steel was 47 pet and 1 pet, respectively, for Companies "A" and "B."

Jan 1, 1952

By J. Brian Eby

The Gulf Coast of southern Louisiana during the year of 1940 was subjected to an extensive exploration and development campaign, as a result of which 16 oil fields and about 38 new producing sands were found. Although this record of discovery appears in keeping with the rate of 1939 actually in amount of new proven reserves, it may fall short of that of the previous year. Only five or six of the discoveries rated as first-class or important fields at the close of the year. The most prominent new fields opened during the year were Neale field in Beaure-gard Parish, the West Cote Blanche field in St. Mary Parish, the Stella field and the West Bay field in Plaquemines Parish, and the Lake Salvador field in St. Charles Parish. There were many important oil-sand discoveries in proven fields, such as in the Bayou Perot field, the Golden Meadows field, the Iowa field, West Lake Verrett field, and the Venice field. During the year, 1047 weUs were drilled in southern Louisiana, of which 768 were completed as oil-producing wells, 17 as gas wells and 262 as dry holes. The Neale field in northwest Beauregard Parish is considered one of the most important discoveries of the year. The f~eld centers around the north half of sec. 26, 'Y.3 S., R.I I W., just north of the town of Neale. It was discovered by the Atlantic Refining Co., using reflection seismograph to locate the structure. Production was found in the second well drilled in the Wilcox sand on the downthrown side of a fault. The structure is known as the "Tepetate" type, being similar to that of the well-known Tepetate field. There were 12 oil wells and 3 dry holes drilled during the year. The Wilcox sand in this field occurs between 8350 and 8400 ft. and averages 30 ft. in thickness. The West Cote Blanche Bay field, in West Cote Blanche Bay, St. Mary Parish, is a 1940 discovery by the Texas Company, credited to reflection seismograph exploration. The oil is from two sands occurring at 3110 to 3140 ft. and from 4950 to 5020 it. Four wells were drilled during the year, three oil wells and one dry hole. The deepest hole drilled reached 9491 ft. without encountering salt or dome material. In Plaquemines Parish, south of New Orleans, the California company has a new field known as the Stella field. The sand was found at a depth of 7485 ft., and 5 ft. of perforations made a well capable of producing 486 bbl. of oil in 24 hr. through a 9.is-in. choke. The oil is 42" gravity. The discovery well was drilled to a total depth of 10,258 ft. and other producing sands were indicated. A good field appears assured, although only one well was completed within the year. The Lake Salvador field, in the center of Lake Salvador, St. Charles Parish, gives promise of being one of the most important discoveries of the year. The discovery well was perforated at 9775 to 9800 ft. making 850 bbl. of 33.7° gravity oil daily through a 1/4-in. choke. Three wells were completed in 1940 but few details have as yet been made available.he Gulf Oil Corporation apparently has a good field in its wildcat discovery in West Bay, Plaquemines Parish. This well found

Jan 1, 1941

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By E. E. Donath

Application of the coal hydrogenation process for the production of chemicals is described. It has been estimated that a plant to produce 31,090 bbl per day of chemicals and fuels would cost $326,- 000,000. These products would consist of 6.1 pct by weight tar acids, 50.8 pct aroma tics, 16.4 pct LPG, and 26.7 pct gasoline. THE coal hydrogenation process is well known as a means for the production of liquid fuels from coal. In this paper the possibilities of the coal hydrogenation process as a source of chemical raw materials will be discussed. The recovery of chemicals from coal hydrogenation products necessitates some modifications and additions to the equipment used for the production of fuels. The conversion of coal into liquid fuels such as gasoline requires two steps: liquid phase and vapor phase hydrogenation. Intermediate oils obtained in the liquid phase contain oxygen and nitrogen compounds, especially aromatic compounds, since the coal itself is composed mainly of cyclic compounds. These oils are the raw material for the separation of high molecular weight aro-matics and of tar acids and tar bases. The relative amounts of heavy and middle oil—boiling above and below, e.g., 325°C—can be influenced by temperature, residence time, and catalyst of the liquid phase hydrogenation. In the vapor phase hydrogenation a solid bed catalyst is used to convert the intermediate oil from the liquid phase operation into hydrocarbons of the gasoline boiling range. Essentially pure hydrocarbons with a low content of sulphur, oxygen, nitrogen, and olefines are obtained. Depending mainly on the catalyst, the high ring compound content of the liquid phase oil can be preserved and gasoline rich in aromatics obtained. However, with other catalysts, these ring compounds can be split into gasoline with a high content of isoparaffins.' Again, depending on the operating conditions, products of varying boiling range can be obtained. Selection of catalyst and operating conditions therefore makes possible the production of different grades of motor fuel and also variations in the relative amounts of benzene, toluene, and xylene when aromatic hydrocarbons are produced. The schematic flowsheet, Fig. 1, shows the main steps of the coal hydrogenation process, and the product streams used for the recovery of chemicals are indicated. In the liquid phase hydrogenation stage, coal is made into a paste with recycle heavy oil. The coal paste is mixed with hydrogen and preheated at a pressure of 300 to 700 atm in heat exchangers and preheaters. The coal paste and hydrogen enter high pressure converters where the liquefaction of coal, conversion of the high boiling liquid materials initially obtained, into intermediate oils is performed at a temperature around 470°C. The reaction products enter the hot catchpot in which lower boiling oil vapors are separated from the residue containing unreacted coal, ash, and heavy oil. This residue, usually called H.O.L.D. (heavy oil let down), is processed to separate solid and liquid material. By thermal treatment of the residue, e.g., a coking process, distillate oil is obtained, which can be recycled as part of the pasting oil. This stream is rich in polynuclear aromatics and can be, and has been, used for the recovery of such material. The oil vapors and hydrogen from the hot catchpot are cooled in heat exchangers and a cooler, and the condensed oil is separated from the recycle hy-

Jan 1, 1953

By H. L. Marcus, P. W. Palmberg

As can be seen from the phase diagram A1-W1 the equilibrium solubility of tungsten in aluminum is practically nil at room temperature. By quenching from the liquid state (50,000°C per sec), Varic, Burov, and Kolesnicenko2 obtained A1-W solid solutions up to 0.15 at. pct W. The quenched alloys were in the form of foils, 0.2 to 0.3 mm thick. Considering the results of Duwez and Willens,3 it is obvious that this thickness, which makes impossible a sufficiently rapid quenching, was the main reason for the relatively low content of tungsten dissolved in aluminum found by Varic.2 he present note shows that the metastable solubility of tungsten in aluminum can be appreciably extended in aluminum-rich A1-W alloys. The quenching technique and the procedure employed for the preparation of the alloys have been described previously.475 The resulting quenched flakes varied in thickness from 1 to 20 µm from experiment to experiment. However, the measurements of the lattice parameters were carried out only with flakes thinner than 5 µm. The areas of quenched flakes were between 0.1 and 15 mm2. The quenched flakes were placed into a 0.3-mm glass capillary tube which was then mounted in a 114.6-mm-diam Debye-Scherrer camera. Straumanis asymmetric film position and nickel-filtered CuKa radiation were used. The lattice spacings were computed taking X(CuKa1) = 1.54050A for resolved and ?(CuKa) = 1.54178A for unresolved doublets. All specimens were rotated at room temperature, 26" +2°C. The lattice parameters were estimated from extrapolation against the Nelson-Riley function. It was estimated that the error in the lattice parameter of the measurements on a single film lies within +0.0004A for lower and about +0.001A for higher concentrations of tungsten. The lattice parameters of the metastable solid solutions A1-W are plotted vs the concentration of tungsten in Fig. 1 together with the parameters measured by previous investigators.' Each point of the present measurements represents a determination of the lattice spacing on different quenched flakes, for a given concentration of tungsten. With experimental accuracy, the lattice parameters of the metastable solid solutions fall on the straight line passing through the already known data.' As estimated from the uncertainties in the lattice spacings of the solid solutions, the alloys were homogeneous within 0.1 at. pct W. The solubility of tungsten in aluminum-rich A1-W solid solutions obtained by a very rapid quenching technique is increased to about 0.95 at. pct W. This value is 6 times greater than the amount known up to now. -he lattice parameters of the resultant aluminum solid solutions with higher concentrations of tungsten than 0.95 at. pct W did not remain constant AUGER electron spectroscopy has been used to clarify the role of impurities in the embrittlement of AISI 3340 steel. Analysis of fracture surfaces has shown that the embrittled condition is correlated with appreciable antimony segregation at grain boundaries. The low temperature (400" to 600°C) temper embrittlement of low alloy steels containing various combinations of Cr, Ni, Sb, Mn, P, Sn, and As has been examined extensively for many years. General reviews of the area have been made by McMahon1 in 1968, LOW' in 1959, woodfine3 in 1953, and Holloman4 in 1946. Recent work by Low, Stein, Turkalo, and LaForce5 has done much in separating the alloy and

Jan 1, 1970

By J. Brian Eby

The Gulf Coast of southern Louisiana during the year of 1940 was subjected to an extensive exploration and development campaign, as a result of which 16 oil fields and about 38 new producing sands were found. Although this record of discovery appears in keeping with the rate of 1939 actually in amount of new proven reserves, it may fall short of that of the previous year. Only five or six of the discoveries rated as first-class or important fields at the close of the year. The most prominent new fields opened during the year were Neale field in Beaure-gard Parish, the West Cote Blanche field in St. Mary Parish, the Stella field and the West Bay field in Plaquemines Parish, and the Lake Salvador field in St. Charles Parish. There were many important oil-sand discoveries in proven fields, such as in the Bayou Perot field, the Golden Meadows field, the Iowa field, West Lake Verrett field, and the Venice field. During the year, 1047 weUs were drilled in southern Louisiana, of which 768 were completed as oil-producing wells, 17 as gas wells and 262 as dry holes. The Neale field in northwest Beauregard Parish is considered one of the most important discoveries of the year. The f~eld centers around the north half of sec. 26, 'Y.3 S., R.I I W., just north of the town of Neale. It was discovered by the Atlantic Refining Co., using reflection seismograph to locate the structure. Production was found in the second well drilled in the Wilcox sand on the downthrown side of a fault. The structure is known as the "Tepetate" type, being similar to that of the well-known Tepetate field. There were 12 oil wells and 3 dry holes drilled during the year. The Wilcox sand in this field occurs between 8350 and 8400 ft. and averages 30 ft. in thickness. The West Cote Blanche Bay field, in West Cote Blanche Bay, St. Mary Parish, is a 1940 discovery by the Texas Company, credited to reflection seismograph exploration. The oil is from two sands occurring at 3110 to 3140 ft. and from 4950 to 5020 it. Four wells were drilled during the year, three oil wells and one dry hole. The deepest hole drilled reached 9491 ft. without encountering salt or dome material. In Plaquemines Parish, south of New Orleans, the California company has a new field known as the Stella field. The sand was found at a depth of 7485 ft., and 5 ft. of perforations made a well capable of producing 486 bbl. of oil in 24 hr. through a 9.is-in. choke. The oil is 42" gravity. The discovery well was drilled to a total depth of 10,258 ft. and other producing sands were indicated. A good field appears assured, although only one well was completed within the year. The Lake Salvador field, in the center of Lake Salvador, St. Charles Parish, gives promise of being one of the most important discoveries of the year. The discovery well was perforated at 9775 to 9800 ft. making 850 bbl. of 33.7° gravity oil daily through a 1/4-in. choke. Three wells were completed in 1940 but few details have as yet been made available.he Gulf Oil Corporation apparently has a good field in its wildcat discovery in West Bay, Plaquemines Parish. This well found

Jan 1, 1941

By W. A. Ver Wiebe

Spurred on by the very high demands for new crude supplies resulting from World War 11, the oil men of Kansas strained every effort in 1943 to find as many new pools as possible. In all, 1761 test wells were drilled, ,of which 895 were successful in finding new oil supplies and 32 in finding new gas supplies. The total number of wildcat wells drilled in Kansas was 577, including the so-called "extension wildcats," which are located less than 2 miles from production. As a result of the very determined effort to find new oil reserves, 49 of the wildcat test wells found new oil pools in western Kansas and 7 found new oil pools in eastern Kansas. There were 289 rank wildcat tests, and among these 28 were successful ventures. They are responsible for 26 of the new oil pools recorded for the year and 2 of the new gas pools recorded. The ratio of dry holes to producing wells among such rank wildcats is thus approximately 10 to I (289 dry and 28 good). This compares with a ratio of II: I in 1942 and 6:1 in 1941; the same in 1940 and 5:Iin 1939. With nearly all wells flowing to their maximum economic capacity, the total production for Kansas during 1943 reached a new high; that is, 107,700,000 bbl., compared with 97,000,000 during the previous year. Similarly, the amount of gas sold during 1943 made a new high point on the production curve. The total amount was 122 billion cubic feet, compared with about 98 1/2 billion cubic feet for the year previous. As usual, the large Hugoton field of south- western Kansas accounted for approximately half of the total gas production. Highlights of the Year Despite the fact that 56 new pools were found in Kansas during 1943, it must be admitted that the future reserves of the state have not been increased greatly. Most of the new pools seem to be of minor value, although it is admittedly impossible to gauge the future production of any pool in Kansas with any exactitude. Judging by the later performance of some of the pools found in 1942 and in 1941, less than five of the new pools are likely to make any great contribution to the state's future oil reserves. Taking up the counties of Kansas in alphabetical order, the following statements summarize the highlights of the year. In Graham County, the Morel pool was extended to the southeast and this pool now promises to become one of the important pools of western Kansas. Several of the older wells have already contributed more than I000,000 bbl. of oil, and such a figure is considered very satisfactory in Kansas. In McPherson County, important new reserves were found by persistent drilling in township 17 S., R. I. W., the most northeastern township of the county. Many new wells in older pools and discovery wells in new pools make this region look promising. The Lindsborg pool, which had a sensational revival during 1942, was also extended in a number of directions and has now become a rather large producing area with a fairly high future potential capacity.

Jan 1, 1944

By W. A. Ver Wiebe

Spurred on by the very high demands for new crude supplies resulting from World War 11, the oil men of Kansas strained every effort in 1943 to find as many new pools as possible. In all, 1761 test wells were drilled, ,of which 895 were successful in finding new oil supplies and 32 in finding new gas supplies. The total number of wildcat wells drilled in Kansas was 577, including the so-called "extension wildcats," which are located less than 2 miles from production. As a result of the very determined effort to find new oil reserves, 49 of the wildcat test wells found new oil pools in western Kansas and 7 found new oil pools in eastern Kansas. There were 289 rank wildcat tests, and among these 28 were successful ventures. They are responsible for 26 of the new oil pools recorded for the year and 2 of the new gas pools recorded. The ratio of dry holes to producing wells among such rank wildcats is thus approximately 10 to I (289 dry and 28 good). This compares with a ratio of II: I in 1942 and 6:1 in 1941; the same in 1940 and 5:Iin 1939. With nearly all wells flowing to their maximum economic capacity, the total production for Kansas during 1943 reached a new high; that is, 107,700,000 bbl., compared with 97,000,000 during the previous year. Similarly, the amount of gas sold during 1943 made a new high point on the production curve. The total amount was 122 billion cubic feet, compared with about 98 1/2 billion cubic feet for the year previous. As usual, the large Hugoton field of south- western Kansas accounted for approximately half of the total gas production. Highlights of the Year Despite the fact that 56 new pools were found in Kansas during 1943, it must be admitted that the future reserves of the state have not been increased greatly. Most of the new pools seem to be of minor value, although it is admittedly impossible to gauge the future production of any pool in Kansas with any exactitude. Judging by the later performance of some of the pools found in 1942 and in 1941, less than five of the new pools are likely to make any great contribution to the state's future oil reserves. Taking up the counties of Kansas in alphabetical order, the following statements summarize the highlights of the year. In Graham County, the Morel pool was extended to the southeast and this pool now promises to become one of the important pools of western Kansas. Several of the older wells have already contributed more than I000,000 bbl. of oil, and such a figure is considered very satisfactory in Kansas. In McPherson County, important new reserves were found by persistent drilling in township 17 S., R. I. W., the most northeastern township of the county. Many new wells in older pools and discovery wells in new pools make this region look promising. The Lindsborg pool, which had a sensational revival during 1942, was also extended in a number of directions and has now become a rather large producing area with a fairly high future potential capacity.

Jan 1, 1944

By Robert T. MacMillan

Of all the mineral substances utilized by man, salt or sodium chloride has one of the longest and most varied histories. Because all animal life is descended from marine organisms, sodium and chlorine became necessary to life, and as sodium chloride meets requirements most readily, common salt has been essential to human and animal diets from earliest times. As civilization progressed, man learned to evaporate sea water and brines of saline lakes and springs to obtain salt, and gradually ceased to depend on the flesh of animals and the occasional salt outcrops or "salt licks" they frequented. He also learned that salt had a multitude of uses, particularly as a preservative of meat and other foods. The importance of salt in the minds of early men may be readily seen from many allusions in the Bible and other ancient writings. Expressions such as "not worth his salt," and "the salt of the earth" are deeply embedded in the English language. Salt has symbolized friendship, fidelity, purity, and hospitality. It has been used as currency; had religious significance; caused wars; and has been a favorite commodity for taxation. The English word "salary" stems from the Latin word for salt, in which Roman soldiers received part of their pay. Although salt today retains its dietary importance, it has thousands of other uses. Of each 100 pounds produced in the United States less than three pounds is for table use. The other 97 pounds goes for agricultural, industrial, and chemical uses. Fortunately, reserves of salt are enormous and reasonably well distributed on the face of the earth. The sea is an inexhaustible source of salt which may be had at prices which vary with climate and other factors. In addition, large underground salt deposits and many salt lakes, springs and playas are scattered throughout the world. Most countries have access to a salt supply, although some are more favored than others. Properties Crystallized sodium chloride or common salt is known as halite. Its molecular weight is 58.454 and it contains, by weight, 39.34 pct sodium and 60.66 pct chlorine. Alternate positions in the cubic lattice are occupied, respectively, by negative chloride and positive sodium ions; the crystal form is isometric. Crystallization from water produces concentric shells, and when broken, a crystal shows conchoidal fracture. Salt has a hardness of 2.5; its specific gravity ranges from 2.1 to 2.6 for rock salt and is 2.165 for the pure crystal. The refractive index is 1.554; it melts at 800.8 ± 0.5°C and boils at 1413°C. Its heat of fusion is 123.59 cal/ gram. Salt is transparent or translucent and highly diathermous. It is colorless when pure and has a vitreous luster. Salt containing traces of iron oxides has varying shades of yellow, orange, brown, pink, or red. The peculiar shade of red sometimes found in that produced by solar evaporation of sea water has been attributed to tiny organisms. Blue mottlings sometimes seen in halite crystals have been attributed to colloidal sodium. Salt is soluble in water to the extent of 35.7 parts per 100 parts of water at 0°C and 39.8 parts per 100 of water at 100°C. The small difference in solubility with increasing temperature is important in the economics of producing salt by evaporating brine. Salt has a negative heat of solution which is 1.281 kg-cal/ mole at 18°C in 200 moles of water.

Jan 1, 1960

By J. E. Harris

By elimination of other possible nucleation processes, it has been demonstrated, for commercially pure magnesium and a Mg-Al alloy, that at stresses less than that necessary for triple-point cracking creep cavities are most probably nucleated heterogeneously at second-phase particles. Evidence for the existence of such particles is presented and the role of grain boundary sliding in the nucleation process is examined quantitatively. DURING creep deformation of polycrystalline magnesium and its dilute alloys in the temperature range 0.45 to 0.7 Tm (Tm = absolute melting temperature) cavities form mainly along grain boundaries oriented normal to the stress axis and failure eventually occurs by their growth and impingement.' The possibility of low-ductility creep failure of magnesium-alloy reactor cans during service has prompted a number of studies of cavity formation in these materials.2-5 In this paper divergent theories of cavity nucleation6-10 are examined critically and conclusions drawn regarding the most probable mechanism of formation of cavities in magnesium. The paper is divided into two parts. The first section consists of the review and quantitative assessment of the possible role of grain boundary sliding in the nucleation process. In the second part an experimental program is described where an electron-microscope technique has been used to determine if second-phase particles exist in as-received commercially pure magnesium and in a magnesium alloy 1) THEORETICAL REVIEW Possible nucleation sites for creep cavities are: a) high-angle grain boundary triple points,11-14 b) subboundary/grain boundary intersections,15-18 c) ledges in the grain boundary, 19-25 d) second-phase particles. 9,26-30 Each of these possibilities is now considered with special reference to deformation of magnesium. 1.1) Triple-Point Cracking. The stroh31 condition to nucleate fracture is: " > vr [1] where ss = applied shear stress, ? = surface energy, C = shear modulus, L = length of sliding interface. This relationship is independent of the nature of the interface and it is possible to calculate the stress concentration at the end of a sliding high-angle grain boundary and thus deduce, approximately,* the minimum applied stress necessary to nucleate triple-point cracking. Such theoretical predictions for Nimonic alloys have been made by McLean13 and found to agree quite closely with the minimum stress determined by experiment. Stresses capable of nucleating triple-point cracking should also be sufficient to nucleate fracture at a grain boundary due to intragranular slip, for the lengths of sliding interface in the two cases are approximately equal. Thus the minimum stress for triple-point cracking should represent a demarcation between failure due to general "cracking" and that due to cavitation. Hauser, Landon, and Dorn32 have demonstrated that for polycrystalline magnesium in the temperature range 78° to 298°K the fracture stress is inversely proportional to the square root of the mean grain diameter. As pointed out by stroh31 this result indicates that Eq. [I] describes the fracture characteristics of magnesium at low temperatures. Heal3 has reported that for rapid deformation (112 pct hr-1) of polycrystalline magnesium the transition from cracking to cavitation occurs in the temperature range 175" to 275°C. He also presented the fracture-stress values for the same material tested under similar conditions. From Eq. [I] taking G = 1.3 x 10" dynes , ? = 600 ergs . cm-2,33 and L = 0.017 cm, a Stroh-McLean13,31 tensile stress of -266 kg. cm-2 is calculated, corresponding to a transition temperature of -190°C; this is in

Jan 1, 1965

By M. J. Blackburn

The ordering reaction and its effect on dislocation awangements in alloys based on Mg3Cd has been studied by transmission electron microscopy. Ordering occurs by the growth of ordered domains until they impinge, thus producing an antiphase domain boundary (APB) network. In the disordered alloy, slip is confined to the basal plane while in the ordered condition slip occurs on the basal, prism, and pyramidal planes. Superdislocations have been identuied on these planes and their origin and expected spacings are discussed and compared with the observations. The APBs between the dislocation pairs have been resolved and have proved useful in the identification of superdislocations. Observed slip structures are related to the changes in mechanical properties produced by ordering. At high temperatures magnesium and cadmium form a continuous series of disordered hexagonal solid solutions. At lower temperatures three ordering reactions occur; two based on the compositions Mg3Cd and MgCd3 are transformations to DO19-type superlattices while alloys based on the composition MgCd transform to a B19 lattice. The ordering process in alloys near the composition Mg3Cd has been studied by several workers'-4 and it has been shown to be a first-order type transformation. The variation of mechanical properties with the degree of order and temperature have been reported in some detail by Stoloff and Davies.5 It was shown that the disordered alloy was stronger and less ductile than the ordered alloy, the differences being attributed to changes in the number of active slip planes and to the presence of short-range order in the disordered alloy. In this investigation the ordering reaction has been qualitatively followed by transmission electron microscopy. The effect of this ordering transformation on the dislocation arrangements in deformed specimens has been studied in some detail. EXPERIMENTAL Alloys were melted in a stainless-steel crucible under a flux and chill cast; both melting and casting were performed in an argon atmosphere. The ingots were hot-rolled and tensile specimens cut from the resultant strips. Some large-grained specimens were grown by the strain-anneal method. Heat treatment was carried out in inert atmosphere furnaces and in oil baths at the lower temperatures. Thin foils for transmission electron microscopy were produced by electropolishing in a cooled solution (temp = -40°C) containing 50 cu cm of nitric acid and 180 cu cm of methanol at a potential of 10 v. The ordering reaction was followed by transmission electron microscopy, X-ray, and electrical resistivity measurements but this paper will be concerned chiefly with the electron-microscopy results. Much of the work described in this paper was performed on an alloy containing 26.10 at. pct Cd although two of the micrographs are taken from work on a 25.55 at. pct Cd alloy. RESULTS i) The Quenched Solid Solution. Specimens which were quenched from above the critical temperature showed diffuse superlattice reflections. sark-field analysis on these reflections failed to reveal the presence of ordered domains and thus the superlattice reflections were assumed to arise from regions of short-range order. Quenching from temperatures of 400" to 450°C results in the formation of dislocation loops and helical dislocations. Such defects have been observed and analyzed in detail in several hexagonal metals6-' and as the crystallography and interactions of such loops appear similar in this alloy they will not be reported in detail. Fig. 1 shows a high density of loops

Jan 1, 1968

Jan 1, 1985

By Robert D. Pehlke, Arden L. Bement

A mass transfer coefficient for the removal of hydrogen from liquid aluminum by inert flush degassing has been determined experimentally at 700°C. A mathematical model has been derived, assuming transport control, which adequately describes the experimental data. The removal of hydrogen is shown to increase with decreasing bubble size, and with increasing flow of flushing gas. The presence of hydrogen in liquid metals in amounts which exceed the solid solubility at one atmosphere hydrogen pressure is highly undesirable, causing unsound ingots or castings, or resulting in difficulties during further fabrication. The removal of hydrogen from liquid metals can be accomplished by several methods, the principal two being vacuum treating and inert flush degassing. The design of a process involving either of these techniques is based on the mass transfer coefficient for hydrogen between the liquid metal and a hydrogen-dilute gas phase. In an effort to extend our knowledge in this area, an investigation of the rate of removal of hydrogen from liquid metals by inert gas flushing was undertaken. In view of the difficulties encountered with gas porosity in the casting of aluminum and aluminum alloys, and because of certain experimental advantages, liquid aluminum was selected for the study. PREVIOUS INVESTIGATIONS The removal of gases from liquid metals, particularly steel, has received considerable attention in recent years, The first definitive work of a theoretical nature was presented by Geller1 who considered the case where equilibrium exists between purging gases and metal bath during flushing, and also deviations from this ideal case. Hulme2 has surveyed a number of experimental studies and discussed some of the practical limitations of removing dissolved gases from molten metals. More recently a number of studies have been reported on degassing of steel melts by flushing with an inert gas.3'4 Considerable work has also been reported on aqueous and organic liquid-gas systems, and an excellent summary prepared by Hovis.5 The treatment of liquid aluminum by a flushing gas to remove dissolved hydrogen has been known for several decades.6 A number of gases have been used for this purpose, including nitrogen, argon, and chlorine, or mixtures of these gases. Tikkanen and Erkko7 have studied the relative density changes of aluminum castings poured from melts degassed with chlorine, nitrogen, and mixtures of the two gases. Their

Jan 1, 1962

By Francis A. Thomson

IN reviewing mineral industry education a year ago, occasion was taken to congratulate the Institute in general and to felicitate the Education Di- vision in particular on "the most gratifying growth which is taking place in Institute consciousness in regard to its responsibility for the recruitment and adequate training of student personnel and for the successful bridging of the difficult gap between graduation and achievement of professional status." Continuation of this growth of interest throughout 1939 is a recognition of the validity of the splendid statement of George Otis Smith that the mining students of today are the ore reserve of the Institute for the future. In this connection one recalls the equally apt expression of another distinguished geologist, George M. Fowler, who, speaking of exploration for ore deposits, says, "The place to look for elephants is where elephants have been found."

Jan 1, 1940

By W. H. Bassett

ABOUT twenty-five years ago the copper industry had outgrown the Lake Superior production. The electrolytic copper producers had- their process well in hand and the industry was well started in the use of electrolytic copper, both for working into wire and sheet, and for the making of alloys. The trade knew that some brands of copper made good material and that other brands did not. There came together a group of men-a refiner, a rolling-mill man, and a manufacturer of electrical machinery-each of them desiring to know why there was a difference and what .it was. Much investigation was done with wire bars and cakes which involved ' chemical analysis, metallographic examination, physical tests and electrical tests. To find the influence of different kinds of copper in making brass 200 carloads of ingots were made into ,eyelet brass under careful observation; each carload was carefully analyzed and tested before used. The alloy was made and rolled under standard conditions and the results recorded.

Jan 1, 1924

By J. R. Dawson, J. A. Glunt

VESTA No. 4 and 5 mines supply most of the high volatile coal required for Jones & Laughlin's byproduct coke plants. Until 1944 all coal produced in these mines was loaded by hand. Pressure to mechanize at Vesta was brought on by the manpower shortage in World War 11, and in 1943 a decision was made to change to mechanical loading. It was the opinion of those concerned that by use of selective mining the coal would be clean enough to be processed by the existing preparation plants. At that time coal cleaning at Jones & Laughlin consisted of hand picking the larger sizes at the mine tipples and wet washing at plants located at the Pittsburgh and Aliquippa Works. A typical section of the Pittsburgh seam as it occurs at Vesta is shown in Fig. 1. The 14 to 16 in. of drawslate immediately over the coal is too soft to be used for roof and must be taken down, leaving the rooster coal just above for roof. In selective mining an attempt is made to mine the coal under the drawslate first and then load out the drawslate separately as refuse. In full seam mining slate and coal are shot down at the same time and loaded out. Mechanical loading at Vesta created new problems. It was found that selective mining, even when carefully applied, increased the refuse in the raw coal to such an extent that the washers at the mills were unable to handle it. Large tonnages of refuse were being transported, a reject disposal problem was created, and good metallurgical coal was being loaded out and lost. In addition, the selective method handicapped operation of the loading machines. Fig. 2 shows how the ash content of the raw coal increased as mechanization proceeded at No. 5 mine. New Preparation Plant: After an exhaustive study of this situation by J & L management, is was decided that a preparation plant should be constructed at the mines, capable of handling full seam mined coal and large enough to process full production of both No. 4 and No. 5 mines. It was decided that from the standpoint of inside operation and haulage the new plant should be located as near as possible to the old No. 5 tipple on the Monongahela River near Vestaburg. Full seam mining at Vesta could be expected to produce a tremendous volume of refuse along with the coal, since 14 to 16 in. of slate would be mined with an average 78 in. of coal. Disposal of this refuse required serious consideration in selecting a plant site. The only area near Vestaburg large enough for disposal of the plant refuse was across the Monongahela River at LaBelle. Ample space was available here, and construction at this location would not interfere with operation at the No. 5 tipple. It had been noted over the years that the sulfur content of the coal produced at Vesta was gradually increasing, and there was every indication that this increase could be expected to continue as the mines developed further from the river. It was decided to construct a three-part separation plant with complete blending facilities to produce both metallurgical and steam coal. In this system an attempt is made to reduce the sulfur in the metallurgical coal in a secondary cleaning process. Construction of the new preparation plant got under way early in 1947 and continued until the spring of 1950. The plant was designed to handle 2400 tph of raw coal containing 30 to 35 pct refuse. Cost of outside buildings and equipment was about $14 million. Total cost of the plant, together with improvements and changes made at this time, was approximately $21 million.

Jan 1, 1957

By E. C. W. Perryman

IN spite of the large amount of work which has been carried out on the recrystallization of aluminum and its alloys, there has been no complete investigation of the recrystallization characteristics of A1-Mg alloys. The most complete investigation is that reported by Bungardt and Osswald' who, working with commercial-purity materials, found that the temperature both of beginning and of complete recrystallization increased with magnesium content up to about 2 pct Mg, then decreased with a further increase in magnesium up to 5.0 pct, and thereafter increased again. Michaud and Segolz working with 99.93 pct A1 also found the temperature of beginning of recrystallization to decrease as the magnesium content increased from 2.13 pct to about 4.5 pct. Chossat3 using aluminum of 99.99 pct purity found that 0.12 pct Mg had no effect but that 0.4 pct Mg increased the recrystallization temperature by about 30°C. That no effect was found for 0.12 pct Mg does not agree with the later results reported by Demer and Beck4 who found that 0.025 pct Mg in 99.99 pct A1 increased the time for complete recrystallization and furthermore increased the activation energy for the recrystallization process. Kratz" using 99.997 pct A1 found that 0.5 pct Mg increased both the temperature of beginning and of complete recrystallization by 100°C. Chadwick and Hooper" working with commercial-purity material found that 1 pct Mg increased the temperature of complete recrystallization by about 40 °C for cold reductions in the range 17 to 72 pct. With smaller amounts of cold work produced by stretching (10 pct strain), they found no significant effect of magnesium. The latter result agrees with that obtained by Williams and Eborall' who found no effect of 2 pct Mg on the recrystallization temperature of commercial-purity aluminum strained 10 pct or less by stretching. Experimental Procedure Material Used: The chemical analyses of the materials used throughout this investigation are given in Table I. Fabrication: The alloys were cast in iron molds which had been washed thoroughly with alumina. After scalping, the ingots were annealed for 16 hr at 450°C, pressed, annealed at 450°C for 16 hr and hot rolled to 0.25 in. After hot rolling, the slabs were alternately annealed and cold rolled to 0.036 in. Cold-rolling reductions between intermediate anneals were kept at about 30 pct and a high intermediate annealing temperature of 450°C was used so as to obtain, as nearly as possible, similar starting grain sizes for the different materials. All intermediate anneals were done in a salt bath and were followed by cold-water quenching so as to retain all the magnesium in solid solution. The final cold reductions investigated were 20, 30, 40, 50, 60, and 80 pct. The initial grain sizes, that is, the grain size before the final cold reduction, were all very similar. Annealing Procedure: Specimens, 1 in. sq, were cut from the 0.036 in. sheet and annealed in a salt bath, the temperature of which was controlled to k2"C. Separate specimens were annealed for different times at 350°, 375", 400°, and in one or two cases at 415°C and after annealing were quenched in cold water. The time taken for a specimen to reach temperature was approximately 5 sec. Metal-lographic examination after annealing showed that no precipitation of Mg+413 occurred during cooling. Procedures Used for Determining Recrystallization Characteristics: All specimens were electrolyti-cally polished and etched by the method described previously1° and polishing was continued until about 0.002 in. had been removed from each side of the specimen. Using this technique, the smallest recrys-tallized grain which could be observed with cer-

Jan 1, 1956

By G. T. Pruitt, T. L. Irby, P. B. Crawford, H. Ferrell

In water flooding peripheral, center-to-edge, line-drive or water-encroachment patterns the question has arisen, "when should a producing well be converted to a water-injection well?". It is realized that, if the producing well is shut in when water breakthrough occurs, some oil could be left in an unswept area. Yet, operation to high water-oil ratios may require processing much additional water. If a well is shut in, "where should the allowable be transferred?". A review of the literature indicates that very few data are available to the engineer to assist him in answering these questions. It is the purpose of this paper to present information which may be of value in selecting the flooding technique and the injection and producing wells and in scheduling injection and production rates. Certain phases of these problems can be studied in the laboratory. The Potentiometric model is well suited for studying many waterflooding problems. This model assumes that steady-state flow exists, that the mobility ratio is equal to one and that gravitational effects are neglected.'-' The three-phase sand model also has been recognized as an effective means for studying certain reservoir problems. Both models were used in making the study reported here. This paper discusses seven cases utilizing various waterflooding techniques. Data for the first five cases were obtained on the potentiometric model. Data for Cases VI and VII were obtained by constructing and flooding an unconsolidated sand pack (a three-fluid-phase system) and by determining the swept area and cumulative oil recovery for various types of operations. APPARATUS AND PROCEDURE The potentiometric model reservoir was 30 in. long X 10 in. wide by about 1/2 in. deep. Four wells were equally spaced in a line array along the lateral center line. (See Fig. 1.) Well No. 1 initially was an injection well for each of the patterns reported. The cases studied with the potentiometric model and sand model are described herein. The laboratory sand model reservoir was a 30- 10-in. rectangular Lucite vessel packed with sand to a depth of about 0.65 in. Four wells were equally spaced in a line array along the lateral center line. The reservoir material was an unconsolidated sand into which the reservoir fluids were mixed to yield fluid saturations of 55 per cent oil, 25 per cent water and 20 per cent gas. The water was added to the sand and the material mixed, after which the oil was added. Kerosene and water, the fluids used, gave a viscosity ratio of 1.64:1. In packing the reservoir, care was taken to assure constant fluid saturations and constant porosities. A new mixture was prepared for each run. During water flooding, a colored water was injected by a constant rate pump. The injection rate was 1.1 B/D/ft of sand thickness. For this series of tests, each of the producing wells was open to the atmosphere and, as in the potentiometric model study, Well No. 1 initially was an injection well for each of the patterns. KESULTS OF POTENTIOMETKIC MODEL STUDlES Two cases (Cases I and 11) involving equal pressure injections were studied, with the following results. Case Water injection was initiated at Well No. 1; the producing wells (Nos. 2, 3 and 4) were operated at constant and equal bottom-hole pressures. When water broke through at Well No. 2 and achieved the selected water-oil ratio, Well 2 was converted to a water injection well, resulting in two injection and two producing wells. The injection pressures at Wells 1 and 2 were maintained equal and constant; pressures at the producing wells were held equal, but they were lower than those at the injecting wells. A similar process was repeated when water broke through at Well No. 3. The flood was terminated when

By A. R. Elsea, E. E. Fletcher

Cast X-40 alloy with the lowest nitrogen content studied had a 100-hr rupture stress at 1500°F about equal to the reported value for the commercial alloy. Increases in nitrogen content progressively decreased the rupture strength, and with about 0.1 to 0.2 pct N a minimum strength was reached, but there was no accompanying change in microstructure. Further increases in nitrogen resulted in the fomzation of progressively increasing amounts of a lamellar, pearlitic-type structure at the grain boundaries, with accompanying increases in rupture strength, and above about 0.25 to 0.33 pct N, the rupture strength exceeded the normally reported values. Two series of melts representing different melting stocks exhibited minimum rupture strengths at different nitrogen contents. This suggests that some unidentwed trace element not removed by vacuum melting has a strong influence on the response of this alloy to variations in nitrogen content. In a series of melts with manganese contents ranging from 0.6 to 3.2 pct, the material with the lowest manganese content had the highest 100-hr rupture strength at 1500°F. The manganese variations had no appreciable effect on the microstructure. CAST cobalt-base alloys such as X-40* exhibit high strengths at elevated temperatures (1500°F and above), but they also show considerable scatter in high-temperature properties. Since the design of parts for critical applications must be based on the minimum expected properties, this broad scatter appreciably lowers the design strength of the alloy. If the relatively poor properties exhibited by a few test parts from any given group could be improved, the spread in properties would be narrowed, and the design stress could more closely approach the average expected properties. The purpose of this research investigation was to learn what were the causes of these erratic properties and, if possible, to find methods for eliminating them. Earlier unpublished work showed that vacuum melting markedly influenced the high-temperature strength of cast X-40 alloy. There were indications that this behavior may have been the result of changes in the nitrogen or manganese content of the castings. Consequently, in the current investigation, the influence of variations in nitrogen and manganese content on the structure and high-temperature properties of cast X-40 alloy was studied. In this program, X-40 melting stock was vacuum melted to produce a base material that was very low in nitrogen content and in volatile trace elements. Additions were then made to this base material to produce alloys of the desired composition. The metal was cast into investment molds producing coupons which were machined into stress-rupture bars. These bars were subjected to stress-rupture tests and me-tallographic study to determine the influence of changes in analyses (nitrogen and manganese content) on the structure and properties. Material—The melting stock used for these experi-ments was in the form of shot from two master heats of commercial X-40 alloy. Only one master heat was used in a given series of melts. Thus, any differences in structure or properties that showed up in the specimens from a given series would be the result only of the intended variations in composition. The certified analyses of the master heats were as follows: C Mn Si Cr Ni Lot No. 2 0.50 0.71 0.66 25.44 10.53 Lot No. 3 0.54 0.73 0.70 25.95 10.00 W Fe Co P S Lot No. 2 7.45 1.34 Bal. 0.011 0.013 Lot No. 3 7.58 1.53 Bal. 0.005 0.016

Jan 1, 1960

By W. C. PAGE

AS the pioneer operation treating the mixed lead- zinc-iron ores from the district tributary to the Salt Lake Valley, the International Smelting Co.'s plant has offered an extremely interesting and instructive opportunity to study some phases of this problem. Basically, there were two main reason for our attempting to work out a successful operation for the separation and concentration of the values contained in the rather widespread deposits of these so- called lead-zinc ores. In the first place, the time was ripe and demanded some method of curtailing the economic waste resulting from the costs of past and present practice of smelting ores of this character, or rather, those ores which could stand the charges inherent with smelting them. Secondly, but rather primarily with us, we believe that such a solution would greatly in- crease in general the production of lead in the district tributary to the Salt Lake Valley. It is generally known that there were and are three relatively large lead smelting plants in the Salt Lake Valley and the decreasing production of correspondingly clean lead ores was not efficient to justify the existence of all three. We could not hope for better lead smelting metallurgy nor more efficient business management than was being practised, so the only prospect was to at- tempt to work out some way to increase the primary production and thus widen the scope of operations.

Jan 1, 1926