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In reply to inquiries and comments which have reached me since the publication of this paper, and in explanation of some seeming discrepancies between my statements in the text concerning the amount of displacement of the faults, on one hand, and certain figures in the plates on the other hand, I give here, with some additional remarks, my measurements of the displacements in the different sections, which it originally seemed unnecessary to print : By displacement, I mean neither the throw, i.e., the vertical distance apart of the two edges of a faulted bed (what Mr.

Jan 1, 1896

By Charles L. Elliot

Data on mining applications of geophysical activity in the Free World in 1964 have been made available to SME again this year by the Society of Exploration Geophysicists. Worldwide data were collected as part of an annual service to the mining industry by the Committee for Geophysical Activity of SEG. Data are taken from 245 voluntary responses (53%) to questionnaires circulated to 463 company, government and university organizations engaged in mining geophysical operations and research all over the world. WORLD ACTIVITY Worldwide manpower utilization totalled 9323 professional man-months and $14.5 million was reported spent in mining geophysical activity in 1964. This is up from 9078 man-months and $12.6 million in 1963 and 8065 man-months and $12.8 million in 1962. Worldwide geophysical activity in terms of manpower utilization and expenditures is presented in the accompanying table.

Jan 9, 1965

FRank FirmstoNe, Easton, Pa.: The effect of lead on brass seems to have been recognized by Berthier, and the facts published by him as early as 1818 (Ann. des Mines, 1st ser., iii., 1818, p. 347 et seq.). He there says expressly that copper containing lead makes " dry " (see) brass, and that, for the same reason, blast-furnace

Jan 1, 1898

By W. C. Leslie

The textures of cold-rolled and of annealed iron are compared with those of an iron-0.8 pct copper alloy in which the amount of precipitation after cold rolling was controlled. Previously published pole figures -for cold-rolled and for annealed iron are confirmed. The effects of precipztatiotz after cold rolling are to retain the cold-rolled texture after annealing, to inhibit the formation of the usual allnealing texture, and to produce elongated recrys-tallized ferrite grains. It is suggested that the inhibition of new textures by precipitation after cold rolling is a general phenomenon. A great deal of attention has been paid to the development of texture during the secondary or tertiary recrystallization of ferritic alloys, but very little work seems to have been done on the control of texture during primary recrystallization. If such control were attained, it might be possible to simplify the processing of oriented materials or to change the characteristics of current cold-rolled and an-nealed products. From previous experience, it seemed likely that texture could be controlled by recrystallizing a supersaturated solid solution. Green, Liebmann, and Yoshidal found that the formation of preferred orientation in aluminum (40 deg rotation about <111> relative to the deformed matrix) was inhibited when iron was retained in supersaturated solid solution in the strained aluminum. The authors attributed this inhibition to iron atoms in solid solution. There is, however, an alternative explanation. Green et al, took a highly supersaturated solution of iron in strained aluminum and heated it to an unspecified temperature for recrystallization. It is probable that precipitation occurred prior to and during recrystallization, and it is proposed that the inhibiting agent is this precipitate, rather than the iron atoms in solid solution. It is important to note that precipitation before cold work is ineffective; the effective precipitate is that formed after cold working and either before or during recrystallization. The location and distribution of the precipitate are critical. Precipitation in such a manner has been found to have profound effects upon kinetics of recrystallization and the microstruc-ture of the recrystallized alloys.2-4 It would be surprising, indeed, if this were accomplished with no change in texture. Because of the relative simplicity of the system, and because of previous experience,4-7 it was decided to determine the effect of precipitation on texture in an alloy of iron and copper. Bush and Lindsay5 found an unspecified change in texture in cold-rolled and annealed low-carbon rimmed steel sheets when the copper content exceeded 0.1 pct. MATERIALS In earlier work, the rate of recrystallization of a low-carbon steel was greatly decreased by 0.80 pct copper, and, after the proper treatment, the recrystallized ferrite grains were greatly elongated.4 Accordingly, it was decided to investigate the effect of precipitation on texture at this level of copper content. The iron and the iron-copper alloy were made from high-quality electrolytic iron and OFHC copper, vacuum-melted in MgO crucibles, cast, hot-rolled to 0.2 in., then machined to 0.150 in. The compositions are given in Table I. The plates were heated to 925°C and brine quenched, twice. This produced a ferrite grain size of ASTM 0 in the iron and ASTM 1 in the Fe-Cu alloy. Disk specimens were cut from the heat-treated plates, repeatedly polished and etched, then used to determine (110) and (200) pole figures by reflection. Despite the complication of large grain size, these pole figures strongly indicated a random texture. PROCEDURES The copper content in solid solution in ferrite before cold rolling and recrystallization, and hence, the amount that could precipitate during the recrys-tallization anneal, was controlled at three levels by heat treatment. The specimens as quenched from 925° C were presumed to have all the copper, 0.80 pct, in solid solution. Other samples of the quenched alloy were aged 5 hr at 700°C to retain about 0.5 pct Cu in solid solution.6 A third set of quenched specimens was reheated to 700°C, then slowly cooled in steps, to reduce the amount of copper in solid solution to a very low level. All specimens were cold-rolled 90 pct, from 0.150 to 0.015 in. thick. The rolling was done in one direction only, i.e., the strip was not reversed between passes, with a jig on the table of the mill to keep the short specimens at 90 deg to the rolls. The rolls were 5 in. in diameter and speed was 35 ft. per min. Machine oil was used as a lubricant. In a supersaturated alloy, the maximum effect of the copper precipitate on microstructure and on recrystallization can be developed by a treatment at 500°C, after cold rolling and before recrystallization.&apos;

Jan 1, 1962

By John C. Bilello

The brittle fracture behavior of cold-worked sintered tungsten was studied over the temperature range 4.2° to 298°K using a high-sensitivity strain measuring system and electronfractography. Similar observations were made on a swaged electron beam zone-refined monocrystal. In sintered tungsten irreversible plastic deformation was observed during cyclic load-unload tests at stress levels well below the fracture stress for all temperatures, but general microyielding could be detected only down to 202°K. For the zone-refined samples macroyielding occurred at all test temperatures with evidence for twinning below -202°K. The fracture stress of the sintered tmgsten was virtually independent of temperature, while the zone-refined crystal showed a 2.3 times increase over the same temperature range. Electronfractography confirmed the presence of numerous rod-shaped and spherical submicroscopic voids which ranged in diameter from 1400 to 4300A in the sintered tungsten; no voids could be found in the zone-refined tungsten. Contrast effects observed on the replicas in the vicinity of certain voids indicated that plastic deformation could be induced by the local stress concentration. It has been suggested that the presence of these voids may be responsible for the low-temperature brittle failure of sintered tungsten. Based m this suggestim und on the evidence obtained here, a dislocatim model is presented to account for the brittle behavior of sintered tungsten. In this model slip, which is induced by the local high stress concentration in the region at the edge of a favorably oriented void, could cause the void to grow to a microcrack of critical size. STUDIES of brittle fracture in bcc metals have led to the well-known experimental relationships between grain size, yield stress, fracture stress, and temperature which have formed the basis for the various dislocation pile-up1-3 or interaction4&apos;= models for slip-induced microcrack nucleation. While microcracks can be nucleated by deformation twins,6,7 there has been no direct evidence furnished by transmission electron microscopy to support conclusively either the Zener pile-up or Cottrell dislocation reaction models for producing micro-cracks in all "brittle" materials. In addition to the "inverse" grain size relationship for yield and fracture stresses the cottrel14 theory predicts that the fracture stress below the transition temperature should behave in a fashion similar to that of the yield stress above this temperature. Such behavior has been verified for several bcc metals.8-10 With reference to both grain size effects and the tem- perature dependence of the fracture stress below the transition temperature, the behavior of sintered tungsten appears anomalous. Early work by Bechtold and Shewrnon 11 showed no apparent temperature dependence of the fracture stress below the ductile-brittle transition temperature (DBTT). They attributed this result to the intergranular nature of the fractures observed. More recent work by Wronski and Four-deux12&apos;13 on considerably purer material did not show any systematic relationship between the fracture stress and temperature below DBTT. The dependence of flow and fracture stresses on grain size is also not clearly established for sintered tungsten. Koo, for example, has shown that the DBTT for sintered tungsten depended chiefly on the annealing temperature and was relatively insensitive to the actual grain size achieved. Using electrofractography and transmission electron microscopy, Wronski and Fourdeuxl3 showed that numerous spherical and rod-shaped submicroscopic voids could be found in sintered tungsten but not in melted tungsten of nominally the same purity. They suggested that these voids could be responsible for the temperature insensitivity of the fracture stress below the DBTT. In the present work the temperature dependence of the fracture stress for high-purity commercially sintered tungsten has been determined. The presence of submicroscopic voids in sintered materials was confirmed, and these were studied in detail to examine the role they could play in nucleating brittle fracture. A dislocation model is suggested which could cause an inherent spherical void to lengthen into a Griffith crack of critical size. EXPERIMENTAL PROCEDURE Commercially sintered tungsten rod was obtained in the as-swaged condition from Sylvania. A zone-refined crystal was obtained from the same source. This crystal was grown by giving three zone passes (at 25.4 cm per hr) to a sintered rod of high-purity tungsten. The rod axis prior to cold working was -15 deg from the [110] direction. Originally the zone-refined rod was -6 mm in diam; it was reduced to -3 mm by eight swaging passes, at high temperatures, with each step having about the same reduction of area. The final swaging step gave a 7.5 pct reduction of area at 1050°C. All swaging operations were performed in a hydrogen atmosphere. For the sintered rod a similar working schedule was employed. Metal-lographic examination of the sintered material revealed that the cold-worked structure had an apparent grain diameter of -25 u transverse to the swaging direction (obtained by the intercept method). In the longitudinal direction cold-worked grains were approximately 1.5 to 2 times their diameter. No distinct fiber structure could be observed optically for the zone-refined rod. The cold-worked structure in the

Jan 1, 1969

By Forrest K. Pence

Bentonite deposits are known to occur in Texas within the Jackson group of formations. This group represents the uppermost Eocene age sediments found in the coastal plain area of Texas. It outcrops across this area of the state in a narrow band of some 4 to 20 miles width. The outcrop pattern roughly parallels the present Gulf of Mexico shore line and is some 100 miles inland from the Texas shore, Fig 1. The principal bentonite deposits are found in the areas where this outcrop pattern cuts across the south-central Texas counties of Karnes, Gonzales, and Fayette. In these deposits, the better quality bentonite is found in the lower or bottom layers of the volcanic ash deposits in which they occur. Some of these better quality benton-ite~ develop very light colors upon firing and therefore justify their being classified as "white firing." The deposits in Karnes and Gonzales Counties apparently occur in commercial quantity, whereas the white firing strata so far uncovered in Fayette County have been too thin to be classified as yet as "commercial." A study of the ceramic properties of the weathered ash in Gonzales and Karnes Counties was reported in 1941.&apos; Commercial development of the deposit in Gonzales County, 7 miles east of Gonzales, Texas. was started earlier by the Max B. Miller Co. for the purpose of marketing the material as a bleaching clay, and this operation has developed to very sizable proportions. In recent years, this company has offered a specially selected grade of the Gonzales material as a suspending agent in glaze slips. The white firing property especially adapts the material to use in white cover coat enamels. The strata in the deposit are practically horizontal and consist from top to bottom of approximately 2 ft of soil overburden, 10 ft of brown bentonite, 2 ft of coarse white bentonite, and 4 ft of waxy white bentonite overlying a he grained sandstone. The & being made in the quarry is approximately one-half mile in length. Only the bottom 4 ft of waxy bentonite is being recovered, the upper layers being stripped and wasted, Fig 2. It may appear somewhat surprising that the very bottom strata appears to have been the one most completely altered. To confirm this, samples from top to bottom of the various strata were studied microscopically by R. F. Shurtz. Professor of Ceramic Engineering, University of Texas. His interpretation is to the effect that the lower part of the seam was deposited at a much earlier date than the top, and that the lower part was chemically altered to a considerable extent before the upper part of the seam was laid down. The conclusion to be derived from these examinations may be stated briefly to he that the alteration in these strata or parts of strata has proceeded independently of the alteration in other parts of the strata during a considerable geological period. The presence of gypsum and iron stain throughout all of the strata indicates that alteration is now proceeding more or less uniformly throughout. It is contended that the alteration of the original ash to montmorillonite is not a result of the presently operating processes. A deposit which occurs approximately 7 miles southeast of Falls City and just south of the village of Casta-howa, has been explored and leased by J. R. Martin, of San Antonio. Mr. Martin has conducted mining and marketing operations in bentonite for a period of many years and asserts that the white firing strata found in this deposit occurs in commercial quantities. His pit, which is shown in Fig 3, exposes 2 ft of soil overburden, approximately 5 ft of white bentonite having coarse texture, and approximately 5 ft of waxy white bentonite which in turn overlies a brown sandy clay. Here, as in the Gonzales deposit, the most completely altered portion is found at the bottom of the seam, as per following report of microscopic examination by Mr. Shurtz. Sample No. 1: This sample was taken from the top stratum which is one foot thick. It is grayish in color and it contains visible fossilized plants. The color is probably the result of fine carbonaceous material in the rock. Under the microscope the sample is seen to consist of glass and feldspar; the amount of glass predominating. Both these substances are slightly altered. No montmorillonite or other clay mineral can be identified definitely; however, the products of the slight alteration mentioned are probably montmorillonite or mineral gel. Sample No. 2: This sample was taken from the stratum second from the top. This stratum is fourteen inches thick. The sample is light gray. It shows numerous veinlets of greenish translucent material ranging from one-eighth inches wide down to the limit of visibility with the unaided eye. It has the smooth, sub-conchoidal fracture characteristic of some bentonites. Microscopically the sample consists mainly of aggregates of clay minerals. The birefringence of the aggregates is lower than would be expected if the

Jan 1, 1950

By J. A. Barr, R. B. Burt, I. S. Tillotson

THE pumping of solids in water suspension is an important part of many metallurgical and mining operations. In most cases, it is still in the rule of thumb category for which no universal formula has been developed, and much research is needed. Because of the limited and incomplete data available, this article may be classed as an experience paper, which is presented with the hope that some contribution will be made toward the development of the so-called universal formula. This formula, if and when developed, may be evolved from several factors, many of which are not now available for general application. The designing engineer is interested in obtaining accurate forecasts on: 1—the minimum velocities needed to prevent choke-ups in the pipeline, which in turn dictates pipe sizes, 2—power required for pumping, 3—pump selection. The basic factors for a given problem will include: 1—weight per unit of time of solids to be handled, 2—specific gravity of solids, for calculation of volume, friction and power, 3—screen analysis of solids with the colloidal acting, i.e., the slime fraction, a very important factor, 4— shape of particle or some means of determining a friction constant, 5—effects of percentage of solids, 6—development of a viscosity factor to be used in the overall calculations, 7—calculation of the lower limits of pipeline velocities permissible, 8—calculation of total head, pump horsepower, and 9—setting up of pump specifications. In certain limited cases horsepower and total heads and minimum velocities may be computed and a suitable pump selected from basic data, but in many cases, as in mining of Florida pebble phosphate, experience rather than a hydraulic formula still should be used as a basis of selection. Pumping Florida Pebble Matrix Pumping at the Noralyn mine of International Minerals and Chemical Corp. will be used as an example. Other areas will vary as to the characteristics of the matrix, especially the slime content. A typical screen analysis of this matrix is: +14 mesh, pebble size,* 2.1 pct; —14 +35 mesh, 11.4 pct; -35 +I50 mesh, 60.5 pct; -150 mesh, 25.0; total, 100 pct; moisture in bank, 20.0 pct; weight per cu ft in bank, 120 lb. The —150 mesh fraction may increase to as much as 35 pct in adjacent areas. When thoroughly elutriated, the matrix has a relatively slow settling rate, which is an important factor in permitting lower pipeline velocities without choke-ups. Exact data is not available to evaluate settling rates. For a factor of 100 a suspension of clean building sand in water is suggested. When pumping long distances, a quick settling matrix allows the coarser solids to settle out along the bottom of the pipeline, causing drag, turbulence, and increased friction. With a slow settling matrix as at Noralyn, turbulence acts to keep the solids in suspension at a lower friction head, regardless of the pumping distance. When the pebble content of the matrix, i.e., the + 14 mesh fraction, is in excess of 10 pct of the total solids, trouble may be expected from settling out even in normal pumping distances. To prevent choke-ups and maintain tonnage, an additional pump must be added in the long runs, where one pump would otherwise be satisfactory. A typical pulp handled is: total volume, 7800 gpm; water, 4500; solids pumped per hr, 4200 lb; sp gr pulp, 1.4; percent solids in pulp, 46.; pipe size, 16-in. ID; pulp velocity, 12.85 fps; probable critical velocity, 10 fps, as below this minimum velocity choke-ups would be numerous. In calculating friction heads the Armco handbook is used where a roughness factor based on 15-year-old pipe is set up. Because the pipe used in pumping matrix is smooth and polished because of the scouring action of the phosphate and its silica content, the head losses in the Armco table for water are practically the same as in pumping the Noralyn matrix through smooth pipe, plus the fact that conditions vary widely over short periods, making accurate determinations difficult to obtain. New pumps and pump changes are being tested continuously and a wealth of data built up. This has resulted in a substantial improvement and lower relative costs in pumping matrix. The Florida phosphate industry is constantly seeking to offset higher wage and material costs with improved technique. Until a few years ago a 12-in. discharge pump was commonly used, with heads as low as 80 ft. Sizes have gradually increased and heads more than doubled. For example, the following pump was placed under test at the Noralyn mine: make, Georgia Iron Works; size, suction 16 in., discharge 14 in.; impeller, 39-in. diam; motor, 600 hp, slip ring; full load speed, 514 rpm. The results were increased head, higher capacity than the older design, with fewer pumps in the line from mine to washer.

Jan 1, 1953

By J. A. Barr, R. B. Burt, I. S. Tillotson

THE pumping of solids in water suspension is an important part of many metallurgical and mining operations. In most cases, it is still in the rule of thumb category for which no universal formula has been developed, and much research is needed. Because of the limited and incomplete data available, this article may be classed as an experience paper, which is presented with the hope that some contribution will be made toward the development of the so-called universal formula. This formula, if and when developed, may be evolved from several factors, many of which are not now available for general application. The designing engineer is interested in obtaining accurate forecasts on: 1—the minimum velocities needed to prevent choke-ups in the pipeline, which in turn dictates pipe sizes, 2—power required for pumping, 3—pump selection. The basic factors for a given problem will include: 1—weight per unit of time of solids to be handled, 2—specific gravity of solids, for calculation of volume, friction and power, 3—screen analysis of solids with the colloidal acting, i.e., the slime fraction, a very important factor, 4— shape of particle or some means of determining a friction constant, 5—effects of percentage of solids, 6—development of a viscosity factor to be used in the overall calculations, 7—calculation of the lower limits of pipeline velocities permissible, 8—calculation of total head, pump horsepower, and 9—setting up of pump specifications. In certain limited cases horsepower and total heads and minimum velocities may be computed and a suitable pump selected from basic data, but in many cases, as in mining of Florida pebble phosphate, experience rather than a hydraulic formula still should be used as a basis of selection. Pumping Florida Pebble Matrix Pumping at the Noralyn mine of International Minerals and Chemical Corp. will be used as an example. Other areas will vary as to the characteristics of the matrix, especially the slime content. A typical screen analysis of this matrix is: +14 mesh, pebble size,* 2.1 pct; —14 +35 mesh, 11.4 pct; -35 +I50 mesh, 60.5 pct; -150 mesh, 25.0; total, 100 pct; moisture in bank, 20.0 pct; weight per cu ft in bank, 120 lb. The —150 mesh fraction may increase to as much as 35 pct in adjacent areas. When thoroughly elutriated, the matrix has a relatively slow settling rate, which is an important factor in permitting lower pipeline velocities without choke-ups. Exact data is not available to evaluate settling rates. For a factor of 100 a suspension of clean building sand in water is suggested. When pumping long * Pebble is a commercial designation for the coarser fraction of finished phosphate from a washer, usually +14 mesh. distances, a quick settling matrix allows the coarser solids to settle out along the bottom of the pipeline, causing drag, turbulence, and increased friction. With a slow settling matrix as at Noralyn, turbulence acts to keep the solids in suspension at a lower friction head, regardless of the pumping distance. When the pebble content of the matrix, i.e., the + 14 mesh fraction, is in excess of 10 pct of the total solids, trouble may be expected from settling out even in normal pumping distances. To prevent choke-ups and maintain tonnage, an additional pump must be added in the long runs, where one pump would otherwise be satisfactory. A typical pulp handled is: total volume, 7800 gpm; water, 4500; solids pumped per hr, 4200 lb; sp gr pulp, 1.4; percent solids in pulp, 46.; pipe size, 16-in. ID; pulp velocity, 12.85 fps; probable critical velocity, 10 fps, as below this minimum velocity choke-ups would be numerous. In calculating friction heads the Armco handbook is used where a roughness factor based on 15-year-old pipe is set up. Because the pipe used in pumping matrix is smooth and polished because of the scouring action of the phosphate and its silica content, the head losses in the Armco table for water are practically the same as in pumping the Noralyn matrix through smooth pipe, plus the fact that conditions vary widely over short periods, making accurate determinations difficult to obtain. New pumps and pump changes are being tested continuously and a wealth of data built up. This has resulted in a substantial improvement and lower relative costs in pumping matrix. The Florida phosphate industry is constantly seeking to offset higher wage and material costs with improved technique. Until a few years ago a 12-in. discharge pump was commonly used, with heads as low as 80 ft. Sizes have gradually increased and heads more than doubled. For example, the following pump was placed under test at the Noralyn mine: make, Georgia Iron Works; size, suction 16 in., discharge 14 in.; impeller, 39-in. diam; motor, 600 hp, slip ring; full load speed, 514 rpm. The results were increased head, higher capacity than the older design, with fewer pumps in the line from mine to washer.

Jan 1, 1953

By R. B. Burt, J. A. Barr, I. S. Tillotson

THE pumping of solids in water suspension is an important part of many metallurgical and mining operations. In most cases, it is still in the rule of thumb category for which no universal formula has been developed, and much research is needed. Because of the limited and incomplete data available, this article may be classed as an experience paper, which is presented with the hope that some contribution will be made toward the development of the so-called universal formula. This formula, if and when developed, may be evolved from several factors, many of which are not now available for general application. The designing engineer is interested in obtaining accurate forecasts on: 1—the minimum velocities needed to prevent choke-ups in the pipeline, which in turn dictates pipe sizes, 2—power required for pumping, 3—pump selection. The basic factors for a given problem will include: 1—weight per unit of time of solids to be handled, 2—specific gravity of solids, for calculation of volume, friction and power, 3—screen analysis of solids with the colloidal acting, i.e., the slime fraction, a very important factor, 4— shape of particle or some means of determining a friction constant, 5—effects of percentage of solids, 6—development of a viscosity factor to be used in the overall calculations, 7—calculation of the lower limits of pipeline velocities permissible, 8—calculation of total head, pump horsepower, and 9—setting up of pump specifications. In certain limited cases horsepower and total heads and minimum velocities may be computed and a suitable pump selected from basic data, but in many cases, as in mining of Florida pebble phosphate, experience rather than a hydraulic formula still should be used as a basis of selection. Pumping Florida Pebble Matrix Pumping at the Noralyn mine of International Minerals and Chemical Corp. will be used as an example. Other areas will vary as to the characteristics of the matrix, especially the slime content. A typical screen analysis of this matrix is: +14 mesh, pebble size,* 2.1 pct; —14 +35 mesh, 11.4 pct; -35 +I50 mesh, 60.5 pct; -150 mesh, 25.0; total, 100 pct; moisture in bank, 20.0 pct; weight per cu ft in bank, 120 lb. The —150 mesh fraction may increase to as much as 35 pct in adjacent areas. When thoroughly elutriated, the matrix has a relatively slow settling rate, which is an important factor in permitting lower pipeline velocities without choke-ups. Exact data is not available to evaluate settling rates. For a factor of 100 a suspension of clean building sand in water is suggested. When pumping long * Pebble is a commercial designation for the coarser fraction of finished phosphate from a washer, usually +14 mesh. distances, a quick settling matrix allows the coarser solids to settle out along the bottom of the pipeline, causing drag, turbulence, and increased friction. With a slow settling matrix as at Noralyn, turbulence acts to keep the solids in suspension at a lower friction head, regardless of the pumping distance. When the pebble content of the matrix, i.e., the + 14 mesh fraction, is in excess of 10 pct of the total solids, trouble may be expected from settling out even in normal pumping distances. To prevent choke-ups and maintain tonnage, an additional pump must be added in the long runs, where one pump would otherwise be satisfactory. A typical pulp handled is: total volume, 7800 gpm; water, 4500; solids pumped per hr, 4200 lb; sp gr pulp, 1.4; percent solids in pulp, 46.; pipe size, 16-in. ID; pulp velocity, 12.85 fps; probable critical velocity, 10 fps, as below this minimum velocity choke-ups would be numerous. In calculating friction heads the Armco handbook is used where a roughness factor based on 15-year-old pipe is set up. Because the pipe used in pumping matrix is smooth and polished because of the scouring action of the phosphate and its silica content, the head losses in the Armco table for water are practically the same as in pumping the Noralyn matrix through smooth pipe, plus the fact that conditions vary widely over short periods, making accurate determinations difficult to obtain. New pumps and pump changes are being tested continuously and a wealth of data built up. This has resulted in a substantial improvement and lower relative costs in pumping matrix. The Florida phosphate industry is constantly seeking to offset higher wage and material costs with improved technique. Until a few years ago a 12-in. discharge pump was commonly used, with heads as low as 80 ft. Sizes have gradually increased and heads more than doubled. For example, the following pump was placed under test at the Noralyn mine: make, Georgia Iron Works; size, suction 16 in., discharge 14 in.; impeller, 39-in. diam; motor, 600 hp, slip ring; full load speed, 514 rpm. The results were increased head, higher capacity than the older design, with fewer pumps in the line from mine to washer.

Jan 1, 1953

By R. B. Burt, J. A. Barr, I. S. Tillotson

THE pumping of solids in water suspension is an important part of many metallurgical and mining operations. In most cases, it is still in the rule of thumb category for which no universal formula has been developed, and much research is needed. Because of the limited and incomplete data available, this article may be classed as an experience paper, which is presented with the hope that some contribution will be made toward the development of the so-called universal formula. This formula, if and when developed, may be evolved from several factors, many of which are not now available for general application. The designing engineer is interested in obtaining accurate forecasts on: 1—the minimum velocities needed to prevent choke-ups in the pipeline, which in turn dictates pipe sizes, 2—power required for pumping, 3—pump selection. The basic factors for a given problem will include: 1—weight per unit of time of solids to be handled, 2—specific gravity of solids, for calculation of volume, friction and power, 3—screen analysis of solids with the colloidal acting, i.e., the slime fraction, a very important factor, 4— shape of particle or some means of determining a friction constant, 5—effects of percentage of solids, 6—development of a viscosity factor to be used in the overall calculations, 7—calculation of the lower limits of pipeline velocities permissible, 8—calculation of total head, pump horsepower, and 9—setting up of pump specifications. In certain limited cases horsepower and total heads and minimum velocities may be computed and a suitable pump selected from basic data, but in many cases, as in mining of Florida pebble phosphate, experience rather than a hydraulic formula still should be used as a basis of selection. Pumping Florida Pebble Matrix Pumping at the Noralyn mine of International Minerals and Chemical Corp. will be used as an example. Other areas will vary as to the characteristics of the matrix, especially the slime content. A typical screen analysis of this matrix is: +14 mesh, pebble size,* 2.1 pct; —14 +35 mesh, 11.4 pct; -35 +I50 mesh, 60.5 pct; -150 mesh, 25.0; total, 100 pct; moisture in bank, 20.0 pct; weight per cu ft in bank, 120 lb. The —150 mesh fraction may increase to as much as 35 pct in adjacent areas. When thoroughly elutriated, the matrix has a relatively slow settling rate, which is an important factor in permitting lower pipeline velocities without choke-ups. Exact data is not available to evaluate settling rates. For a factor of 100 a suspension of clean building sand in water is suggested. When pumping long distances, a quick settling matrix allows the coarser solids to settle out along the bottom of the pipeline, causing drag, turbulence, and increased friction. With a slow settling matrix as at Noralyn, turbulence acts to keep the solids in suspension at a lower friction head, regardless of the pumping distance. When the pebble content of the matrix, i.e., the + 14 mesh fraction, is in excess of 10 pct of the total solids, trouble may be expected from settling out even in normal pumping distances. To prevent choke-ups and maintain tonnage, an additional pump must be added in the long runs, where one pump would otherwise be satisfactory. A typical pulp handled is: total volume, 7800 gpm; water, 4500; solids pumped per hr, 4200 lb; sp gr pulp, 1.4; percent solids in pulp, 46.; pipe size, 16-in. ID; pulp velocity, 12.85 fps; probable critical velocity, 10 fps, as below this minimum velocity choke-ups would be numerous. In calculating friction heads the Armco handbook is used where a roughness factor based on 15-year-old pipe is set up. Because the pipe used in pumping matrix is smooth and polished because of the scouring action of the phosphate and its silica content, the head losses in the Armco table for water are practically the same as in pumping the Noralyn matrix through smooth pipe, plus the fact that conditions vary widely over short periods, making accurate determinations difficult to obtain. New pumps and pump changes are being tested continuously and a wealth of data built up. This has resulted in a substantial improvement and lower relative costs in pumping matrix. The Florida phosphate industry is constantly seeking to offset higher wage and material costs with improved technique. Until a few years ago a 12-in. discharge pump was commonly used, with heads as low as 80 ft. Sizes have gradually increased and heads more than doubled. For example, the following pump was placed under test at the Noralyn mine: make, Georgia Iron Works; size, suction 16 in., discharge 14 in.; impeller, 39-in. diam; motor, 600 hp, slip ring; full load speed, 514 rpm. The results were increased head, higher capacity than the older design, with fewer pumps in the line from mine to washer.

Jan 1, 1953

By K. E. Brown, A. R. Hagedorn

Continuous, two phase flow tests have been conducted during which four liquids of widely differing viscosities were produced by means of air-lift through 1%-in. tubing in a 1,500-ft. experimental well. The purpose of these tests was to determine the effect of liquid viscosity on two-phase flowing pressure gradients. The experimental test well was equipped with two gas-lift valves and four Maihak electronic pressure transmitters as well as instruments to accurately measure the liquid production, air injection rate, temperatures, and surface pressures. The tests were conducted for liquid flow rates ranging from 30 to 1,680 BID at gas-liquid ratios from 0 to 3,-270 scf/bbl. From these data, accurate pressure-depth traverses have been constructed for a wide range of test conditions. As a result of these tests, it is concluded that viscous effects are negligible for liquid viscosities less than 12 cp, but must be taken into account when the liquid viscosity is greater than this value. A correlation based on the method proposed by Poettmann and Carpenter and extended by Fan-cher and Brown has been developed for 1¼-in. tubing, which accounts for the effects of liquid viscosity where these effects are important. INTRODUCTION Numerous attempts have been made to determine the effect of viscosity in two-phase vertical flow. Previous attempts have all utilized laboratory experimeneal models of relatively short length. One of the initial investigators of viscous effects was Uren1 with later work being done by Moore et al.2,3 and more recently by Ros.4 However, the present investigation represents the fist attempt to study the influence of liquid viscosity on the pressure gradients occurring in two-phase vertical flow through a 1¼-in., 1,500 ft vertical tube. The approach of some authors has been to assume that all vertical two-phase flow occurs in a highly turbulent manner with the result that viscous effects are negligible. This has been a logical approach since most practical oil-well flow problems have liquid flow rates and gas-liquid ratios of such magnitudes that both phases will be in turbulent flow. It has also been noted, however, that in cases where this assumption has been made, serious discrepancies occur when the resulting correlation is applied to low production wells or wells producing very viscous crudes. Both conditions suggest that perhaps viscous effects may be the cause of these discrepancies. In the first case, the increased energy losses may be due to increased slippage between the gas and liquid phases as the liquid viscosity increases. This is contrary to what one might expect from Stokes law of friction,&apos; but the same observations were made by ROS4 who attributed this behavior to the velocity distribution in the liquid as affected by the presence of the pipe wall. In the second case, the increased energy losses may be due to increased friction within the liquid itself as a result of the higher viscosities. The problem of determining the li- quid viscosity at which viscous effects becomes significant is a difficult one. Ros4 has indicated that liquid viscosity has no noticeable effect on the pressure gradient so long as it remains less than 6 cstk. Our tests have shown that viscous effects are practically negligible for liquid viscosities less than approximately 12 cp. Actually there is no single viscosity at which these effects become important. These effects are not only a function of the viscosities of the liquids and of the gas but are also a function of the velocities of the two phases. The velocities in turn are a function of the in situ gas-liquid ratio and liquid flow rate. Furthermore, the role of fluid viscosities in either slippage or friction losses will depend on the mechanism of flow of the gas and liquid, i.e., whether the flow is annular. as a mist, or as bubbles of gas through the liquid. These mechanisms are also a function of the in situ gas-liquid ratios and the flow rates. It would thus seem that the best one could hope for is to determine a transition region wherein the viscous effects may become significant for gas-liquid ratios and liquid production rates normally encountered in the field. The viscous effects might then be neglected for liquid viscosities less than those in the transition region but would have to be taken into account when higher viscosities are encountered. There are numerous instances where crude oils of high viscosity must be produced. The purpose of this study has been to evaluate the effects of liquid viscosities on twephase vertical flow by producing four liquids of widely differing viscosities through a 1 % -in. tube by means of air-lift. The approach used in this study was as follows:

Jan 1, 1965

By K. Brack, G. H. Schwuttke

Annealing properties of subszerface amorphous lavers produced through high-energy ion implantation in silicon are studied. The buried layers are produced through the implantation of ions (nitrogen), ranging in energy from 1.5 to 2 mev. X-ray interference patterns, transmission electron microscopy, and resistivity profiling are used to study the annealing characteristics of the ion damage. The annealing experiments indicate a low temperature (below 700°C) and a high temperature (above 700°C) region. Significant changes occur in the amorphous layer during the high-temperature anneal. Such changes are corre-lated with the re crystallization of the amorphous silicon and the formation of subsurface (buried) silicon-nitride films. TODAY&apos;S main problems in the field of ion implantation are related to the accurate determination and prediction of 1) the distribution profiles of implanted ions, 2) the lattice sites occupied by the implanted ions, 3) the lattice damage produced through ion implantation, and 4) the annealing characteristics of damage centers in the lattice. This paper reports investigations concerned with the problems listed under 3) and 4). EXPERIMENTAL Our investigations cover the energy range of incident ions from 100 to 300 mev and from 1 to 2.5 mev. The emphasis of this study is on the energy range from 1.5 to 2 mev. The experiments are conducted with single charged nitrogen ions. To implant the ions a van de Graaff generator is used as described by Roosild et al.1 Accordingly, a gas containing the desired ion specie is passed through a thermome-chanical leak into a radio frequency activated source. The positive ions are driven into the van de Graaff with the help of a variable voltage probe. Emerging from the accelerator the ions drift into a magnetic analyzing system and here the desired ion specie is bent 90 deg into the exit port. The ion beam leaving the analyzer is defocused and drifts down a 4-ft long tube to hit the silicon target. At this position the 20 pamp ion beam has a circular cross-section of 2.1 cm. N2 is used as a source gas for nitrogen ions. The implantation target is silicon with zero dislocation density, 2 ohm-cm resistivity, (111) orientation, mechanically-chemically polished, and 1 mm thick. The target is mounted on a water-cooled heat sink and kept at room temperature. A fluence of 1015 to 1016 ions per sq cm is used. RESULTS 1) Silicon Perfection after Bombardment. High-energy ion bombardment of silicon has some striking effects on lattice perfection. Some results were reported in detail previously at the Santa Fe conference2 and are here briefly summarized for the benefit of the experiments described in the following. 1.1) Identification of Surface Films on Silicon. After bombardment all samples are found to be coated with surface films. The films on the silicon surface vary in thickness and color; they can be transparent, slightly brown, or opaque. The films are thicker and darker in the high-intensity area of the beam and they delineate the bombarded surface area of the crystal. The films produce electron diffraction patterns characteristic of carbon and of SiO2. Carbon is predominant. The presence of carbon in these films was confirmed by use of the electron microprobe. Formation of the films occurs independently of the ions used and is attributed to a contaminated vacuum of the high-voltage machine. The carbon is most likely the product of the pump oil which is cracked and polymerized under ion impact. The films stick tenaciously to the silicon surface and burn off in a low-temperature Bunsen flame. 1.2) Mechanical Perfection of the Silicon Surface. The mechanical perfection of the bombarded silicon surface was investigated through optical microscopy, electron microscopy in which the replica technique is used, and optical interferometry. No mechanical damage of the surface was visible after bombardment. However, if a bombarded sample is soaked for several minutes in hydrofluoric acid (HF), gas bubbles may develop in certain spots of the silicon surface. It is also noted that in these areas the surface film starts to peel off. Relatively large patches of film come off if the sample is soaked in HF during ultrasonic agitation. After HF treatment, pits may be present on the silicon surface. The pit dimensions are estimated to be as large as 50 µ. The pits appear in the region of most intense irradiation. 1.3) Lattice Perfection After Bombardment. No lattice damage is found on the silicon surface. Electron transmission micrographs and selected area diffraction patterns of the surface show no difference before and after bombardment. Measured approximately 2 µm down from the surface, the silicon lattice throughout this depth is of good perfection. Well-defined Laue spots and Kikuchi lines are obtained from the surface as well as from the indicated area below the surface. However, some radiation damage is dispersed in this top layer. A sharp boundary line separates this surface layer from a highly damaged layer which extends further downward into the silicon. Typical of this

Jan 1, 1970

By T. L. MacKay

Oxidation rates of single-crystal and poly crystalline zirconium in oxygen at temperatures from 307° to 815°C obey the parabolic rate law for short ex-posure time, 4 to 6 hr. The activation energy for the oxidation of single-crystal zirconium between 420° and 790°C is 42.6 ± 0.7 kcal per mole, and in the temperature range 307" to 600°C the activation energy for oxidation of poly crystalline zirconium is approximately the same. The high-activation energy is indicative that diffusion through the bulk oxide film is the primary mode of mass transport for both types of metal. The higher oxidation rates for poly -crystalline zirconium in this temperature range were attributed to differences in the orientation of the grains in the metal with respect to the oxidizing surfaces. Above 600°C, vain growth was observed in polycrystalline zirconium, and the oxidation rates approached those of single-crystal zirconium. ThE kinetic data of previous oxidation studies1-&apos; of zirconium in oxygen have been interpreted by both parabolic and cubic rate laws. There is some evidence that there is a transition from the parabolic to the cubic rate law at prolonged exposures, but the question is still controversial. For the parabolic rate law activation energies are reported in the range 18.6 to 35 kcal per mole, and for the cubic rate law in the range 38 to 47 kcal per mole. So far as the mechanism of zirconium oxidation is concerned, inert marker studies10,11 have indicated that the oxidation proceeds by oxygen (anion) diffusion through the oxide film toward the metal-metal oxide interface. Pemslerl2 observed that the orientation of the grains in the zirconium metal substrate affected the rate of formation of the oxide film on the surfaces of the grains and that the orientation dependence of the corrosion rate persisted beyond the initial stages of reaction. The rate of oxidation was a minimum when the c axis of the grain was parallel to the surface of the sample, and rose to a maximum when the c axis was inclined at about 20 deg to the plane of sample surface, and decreased again at higher inclinations. cox13 observed that in 300°C steam a thin oxide film was formed initially on zirconium and that this oxide film, which exhibited interference colors, became dark first along the grain boundaries and then over the whole surface in an inhomogeneous manner as the film thickened. Cox proposed a mechanism in which oxygen diffused along preferred paths created by grain boundaries in the metal and formed a much thicker film at or near the grain boundary than on the central zone of the grain. In the present study, the oxidation rates of single crystals of zirconium were measured in oxygen and compared with the oxidation rates of polycrystalline zirconium of the same bar stock. It was felt that such a comparison would elucidate the role of grain boundaries in the metal substrate. SAMPLE PREPARATION Single crystals of zirconium were prepared by following the procedure of I3apperport,14 starting with 1/4-in. rod purchased as crystal-bar zirconium. Zirconium rods 2 in. long were wrapped in tungsten foil and sealed in quartz tubes at pressures of less than 10-6 mm of mercury. Large single crystals were grown by thermal cycling above and below the a-/3 transformation temperature, 862°C. Several specimens were simultaneously subjected to the same cycling procedure, heating to 1200°C, holding for 4 hr, then cooling in the furnace and holding at a temperature of 840°C for 5 to 10 days. This cycle was repeated five or six times for each set of specimens. The grain size of the crystal-bar zirconium before thermal cycling was between 10 and 30 p. Fig. 1 shows the microstructure of an end section of as-received crystal-bar zirconium. A longitudinal section of each zirconium rod after thermal cycling was polished and examined under polarized light, see Fig. 2, and the largest single crystals were selected for this study. Zirconium rods 1/8 in. in diameter and 1/2 in. long with spherical ends were machined from the single crystals and from the as-received bar stock. An X-ray examination showed that the c axis of the single crystals made either a 34-deg or an 89-deg angle with the rod axis. The specimens were chemically etched for 2 min in solution consisting of 15 parts hydrofluoric acid (48 pct), 80 parts nitric acid, and 80 parts water. The chemical polish removed 1 to 2 mils from the surface. EXPERIMENTAL The Sartorius vacuum microbalance used in this study has a sensitivity of 0.5 pg and a capacity of

Jan 1, 1963

By T. S. Lundy, R. E. Pawel, F. R. Winslow, C. J. McHargue

The volume-diffusion coefficients of Nb-95 and Ta-182 in niobium have been measured over the temperature range 878° to 2400°C. High-temperature specimens (T 21500°C) were sectioned by conventional lathe and grinding techniques while low-temperature specimens were sectioned by an anodizing and stripping technique previously described. Over a range of more than ten orders of magnitude in diffusivity, the self-diffusion data is well-represented by the equation: D = (1.1+ 0.2) exp [- (96,000 * 900)/RT ] cm2/sec Upward deviations from this line are explained by short-circuit diffusion in combination with the loss of resolution of the sectioning techniques. Oxygen contamination within the range 100 to 450 ppm was found to have little or no effect on the self-diffusivitj 01 niobium. In a limited number of measurements, the diffusivity of Ta-182 in niobium was found to be about half that of Nb-95 in niobium. These data may be described by D = (I.0+0.90.5)exp [- (99,300 * 2400) /RT ] PREVIOUSLY reported studies of self-diffusion in niobium were by Resnick and Castleman1 and Peart, Graham, and Tomlin.2 The data of Resnick and Castleman over a temperature range 1585" to 2120°C show considerable scatter but. can be represented by D = (12.4 *0.8) exp [-(105,000+3OOO)/RT] cm2/sec The limited data of Peart, Graham, and Tomlin follow the equation D = 1.3 exp (-95,00O/RT) cm2/sec In view of recent diffusion data for ß zirconium3 and 0 titanium4 in which Arrhenius-type plots do not yield straight lines and of the potential high- temperature uses of niobium and its alloys, we thought it important to investigate the diffusion behavior of this bcc refractory metal over a large temperature range. This has recently been done for molybdenum,5 chromium,6 vanadium,"" and tantalum.9 Niobium was a particularly suitable material for this study largely because of the development of an anodizing and stripping sectioning technique which enables diffusivities as small as l0-19&apos; sq cm per sec to be determined accurately.10 In addition to self-diffusion data, data were obtained for the diffusion of Ta-182 in niobium and for the effect of varying oxygen content on self-diffusion. I) EXPERIMENTAL PROCEDURE Materials. The niobium was obtained from three sources: 1) melting stock from Shieldalloy Corp., 2) electron-beam melted single crystals, 1/2 in. diameter, from Semi-Elements, Inc., and 3) oxygen-doped, electron-beam melted single crystals from Materials Research Corp. The melting stock was electron-beam melted and specimens 5/8 in. diameter by 1/2 in. long were machined from the center of the bar. The analysis supplied by the vendor and an interstitial analysis of one of the specimens are given in Table I. The single crystals (type 2 above) were cut with a jeweler&apos;s saw to specimens about 3/8 in. long. The interstitial analysis of this material is given in Table 11. This material was used

Jan 1, 1965

By Michael Hoch, Seong Kwan Rhee

The ternary system Zr-Cr-0 was investigated at 1200°, 1500°, and 1700°C. The isotherms at these temperatures were determined by metallographic and X-ray diffraction analysis of carefully selected alloys. AS a part of a series of investigations1-4 of the ternary and quaternary phase diagrams on refractory metals and their compounds, the ternary system Zr-Cr-O was investigated at 1200°, 1500°, and 1&apos;700°C. The binary diagrams Zr-Cr, Zr-O, and Cr-0 as reported by Hansen5 and Levin et a1.&apos; and the existence of a ternary coompound ZrsCrsO (q-carbide structure a. = 11.96A) provided a good base for this investigation of the Zr-Cr-O phase diagram. MATERIALS The materials used and their suppliers were: Zirconium powder, 99.4 pct pure, Charles Hardy, New York; Zirconium dioxide, Fairmount Chemical Co., Newark, N.J.; Chromium powder, 99.85 pct pure, Fairmount Chemical Co., Newark, N.J.; Chromium sesquioxide, 99.86 pct pure, J. T. Baker Chemical Co., Pillipsburg, N.J. Though the materials used were not "hyperpure", the impurities present do not affect the results (lattice parameters, phase boundaries) within the experimental accuracy. EQUIPMENT AND PROCEDURE The detailed procedures and equipment used for this investigation were similar to those described elsewherel&apos; "ith the exception that in this study an induction-heated argon-atmosphere furnace was used. The latter furnace was used to prevent the vaporization of chromium metal in samples in the higher temperature range (above 1200°C). The tungsten crucible was induct ion-heated in a vertical quartz tube filled with argon gas. The quartz tube was 1-1/2 in. in diameter and 10 in. long; it was connected at the top and bottom to water-cooled copper plates. The argon gas of a purity 99.995 pct was further purified by being passed through zirconium metal chips which were maintained at 800°C in a silica tube 1 in. in diameter and 30 in. in length. The furnace was flushed with argon gas for an hour before starting heating; during heating, a slight (3 cm oil) overpressure of argon was maintained in the system. Power was supplied by a 20-kw Ther-Monic Induction Generator. The samples rested on a tungsten-wire basket; the wire basket was connected to a tungsten wire which passed through the tungsten crucible lid, and entered the system on top through a Wilson-type seal. By pulling on the wire, the sample was removed from the crucible and dropped to the water-cooled copper base of the furnace. Because of the presence of argon gas, the cooling of the sample was even more rapid than in the vacuum furnace.&apos; EXPERIMENTAL RESULTS AND DISCUSSION 1) Isothermal Section at 1200°C. The compositions investigated have been numbered within the phase diagram, Fig. 1, and all the pertinent information about the samples can be found in Table I. This table lists the composition of the samples, the phases present in the room-temperature diffraction patterns, the phases detectable in the microstruc-ture, and calculated lattice parameters of the a-zirconium phase. The shapes of the various phase

Jan 1, 1964

SEC. 1. The membership of the Institute shall comprise seven classes, namely: 1. Members; 2. Honorary Members; 3. Senior Members; 4. Associates; 5. Junior Members; 6. Rocky Mountain Members; 7. Junior Foreign Affiliates. All shall be equally entitled to the privileges of membership, excepting that no member of any class whose residence shall be outside of the United States of America, except those residing in Mexico and Canada, shall be entitled to vote. SEC. 2. Members: A person to be eligible for election or transfer into the. class of Member must be at least 27 years of age and must have had at least six years&apos; employment in the practice of engineering, mining, geology, metallurgy, or chemistry, during at least three years of which he must have held positions of responsibility in one or more of these fields. This shall not apply to Rocky Mountain members. SEC. 3. Honorary Members: Each candidate for Honorary Membership must be recommended by at least ten Members and must be elected by ballot at a meeting of the Board of Directors by the unanimous vote of the Directors present; provided, however, that the number of Honorary Members shall at no time exceed twenty. Such election shall automatically act as a transfer of such member from any other class of membership to which he may belong. SEC. 4. Senior Members: The Directors may, at the special request of any Member or Associate who has reached the age of seventy years and who has paid dues for thirty years, transfer such Member or Associate to the class of Senior Member; and in special cases may waive either the requirement as to age or as to the number of years for which dues have been paid. SEC. 5. Junior Members: A person to be eligible for election to the class of Junior Member must be qualified -through education or experience to hold a subordinate position in engineering, mining, metallurgical, geological or chemical work. He shall be not more than 33 years of age at the time of election. .SEC. 8. Associates: A person eligible for election or transfer into the class of Associate shall be one, who, in the opinion of the Committee on Admissions and the Board of Directors, is suitable for such election or transfer by reason of his interest in or connection with mining, geology, metallurgy, or chemistry. SEC. 7. Rocky Mountain Members: Membership in a special class of life memberships without annual or other dues and without right to receive the printed literature distributed to other members or the right and privilege of wearing the official badge of technical members, is given to all members of the Rocky Mountain Club at the time of consolidation. These special Rocky Mountain memberships shall be claimable by any member of the Rocky Mountain Club, not already a member of the Institute, availing himself of the privilege within ninety days after mailing of notice to him, by the Secretary of the Institute. SEC. 8. Junior Foreign Affiliate: Upon appropriate action by the Board of Directors and with its approval, members in good standing of any technical society having its headquarters outside of the United States of America, Canada, or Mexico,

Jan 1, 1940

By A. M. Gaudin, C. S. Chang

IN general, fatty acids or their alkali salts do not cause clean quartz to float. However, the presence of multivalent ions, such as the alkaline-earth metal ions and heavy-metal ions, can activate quartz and thus make it respond to soap flotation. The mechanism of activation and soap flotation of quartz has been studied.1-4 The problem was attacked by making flotation tests rather than by careful adsorption measurements on suspensions of ground quartz in solutions containing the activator and the collector. Attempts have been made to determine the adsorption of barium ion and calcium ion on quartz. The results have only qualitative value as the analytical methods were not adequately precise. Artificial radioactivity and progress in radioactivity detection have introduced a new analytical tool, which can have a sensitivity several orders of magnitude greater than that of other methods.5-6 In the experimental work described in this paper the radioactive tracers, barium 140 and carbon 14, were employed. Lauric acid was synthesized, having a radioactive carbon atom and was used with Ba140 to study the adsorption of barium and laurate ions from aqueous solution on ground quartz. Flotation tests, using the vacuum flotation technique,4 were run in conjunction with the adsorption experiments. The object of this investigation was to understand better the reaction mechanism of barium activation and soap flotation of quartz. Methods and Materials Quartz Sample Preparation: Lumps of hand picked quartz, washed free of stains, were reduced in size to -20 mesh in laboratory crushers. The product was boiled in concentrated hydrochloric acid to remove the abraded iron. The cleaned product then was ground dry in a laboratory porcelain mill, using siliceous pebbles, to pass through a 200 mesh screen. The ground product was deslimed by sedimentation at 37 microns. This -200 mesh +400 mesh material was subjected again to boiling with concentrated hydrochloric acid, followed by washing with distilled water and further desliming. The cycle was repeated until no trace of iron could be detected in the wash liquor. During the final washing, the pH of the wash water was checked to insure the complete removal of the acid from the mineral. The quartz then&apos; was rinsed with conductivity water. The resulting product was dried in a drying oven and stored in mason jars. The impurities (spectrographic) were as follows: Al, 0.01 to 0.001 pct; Li, Mg, Mn,, Na, each less than 0.001 pct; Fe and Cu not detected. The specific surface of the quartz sample was determined by the krypton gas adsorption method.7 The average of two measurements was 881 sq cm per g. The calculated specific surface for 37/74 micron quartz particles, using a surface factor of 1.96,8 is 900 sq cm per g. This is in good agreement with the measured value of 881 sq cm per g. Beta-Counting Method: The radioactive isotope of barium used in the experimental work was barium 140. It has a sufficiently long half-life, 12.8 days, emits high-energy beta particles (up to 1.0

Jan 1, 1952

By P. F. Gnirk, J. B. Cheatham

An experimental investigation has been made to study the effects of tooth angle and confining pressure on the force required for indentation of dry rock samples under confining pressure. In these experiments static single-tooth indentations were made on two standstones, a limestone, a schist and a slate under confining pressures of 5,000 to 15,000 psi. Sharp wedge-shaped teeth with included angles ranging from 30°to 105°were used. In all cases the force-displarenzent curves are approxinlately linear for rocks tested under confining pressure, as contrmted with the discontinuous curves obtained for silnilar rocks at atmospheric conditions. Photonzicrographs of thin sections through the craters indicate very little evidence of chip formation during indentation. In general the experimental data lie between calculated values for perfectly rough and perfectly smooth tooth-rock interfaces. INTRODUCTION The variables associated with ctrilling at depth are numerous and, in many instances, are not easity isolated and controlled. Also, many of these variables are interdependent; however, if the variables which are sufficiently independent of each other are held constant and are appropriately introduced, the dependent variables can be more easily studied and evaluated. It is the purpose of the present investigation to study experimentally the simplest case of bit tooth-rock interaction. In essence, the experiments have involved the static loading of sharp wedge-shaped tools on the surfaces of effectively semi-infinite dry rock samples subjected to confining pressures. During this investigation the following quantities have been maintained constant: 1. Pore pressure: atmospheric (i.e., the rock is dry). 2. permeability: although the rocks may be permeable, they are "jacketed" in such a manner that the fluid is not permitted to flow through them. 3. Temperature: 75F. 4. Rate of loading: essentially static (approximately 0.002 in./second). 5. Bit tooth: a sharp wedge-shaped tooth loaded normal to the rock surface. 6. Rock surface: smooth and flat. 7. Drilling fluid: hydraulic oil. In addition to the above conditions, the rock surface was free of a layer of cuttings. There was no indexing to previously indented surfaces, and the influence of corners of the borehole was neglected because the rock samples were effectively semi-infinite. The following quantities have been varied, and the resulting effects have been studied: 1. Rock a) Type (e.g., limestone, sandstone, etc.). b) Mechanical properties ) Necessarily dependent c) Porosity on type of rock. 2. Bit tooth (included angle of wedge-shaped tooth). 3. Depth of penetration. 4. cobfining pressure. On the basis of laboratory experiments which have shown that many rocks exhibit ductile behavior at confining pressures corresponding to depths usually reached during drilling,&apos;.&apos; a theory has previously been advanced which predicts the force required for penetration by a single sharp wedge tooth into a ductile* material.&apos; The material is assumed to be isotropic, homogeneous and rigidly plastic (no elastic deformation) and to obey the Coubomb yield criterion (Figs. 1 and 2). Equations governing the force required for penelration are given for two extreme cases:** 1. A smooth, perfectly lubricated tooth-rock interface (fridionless boundary), in which the solution gives a minimum value for the penetrating force: in which F = force of the tooth, b = length of tooth edge,

By J. L. Foster, G. R. Gray, T. S. Chapman

The wall-building properties of salt-water drilling muds can be improved markedly by the addition of: (I) natural gums, such as traga-canth, karaya, and ghatti; (2) seaweeds, such as Irish moss; or (3) gelatinized starch. Results of laboratory tests have been confirmed by field trials. For drilling operations in which the mud becomes contaminated by salt, either through penetrating salt-bearing rocks or by addition of sea water to the mud, the added cost resulting from the use of one of the substances listed above is more than offset by freedom from stuck drill pipe and ease in running casing. Introduction It has been recognized for many years that oil production might be seriously hampered by infiltration of water from the drilling mud.l-4 As knowledge of the mechanism of the wall-building process advanced, methods were developed for evaluating the filtration characteristics of muds.5-ll The wall-building properties of freshwater muds are commonly regulated by the addition of bentonitic clays, or of agents to promote the dispersion of the natural mud solids. When strata bearing soluble salts are encountered in the course of drilling, the salts are incorporated in the mud; the clay solids are flocculated and water loss is increased tremendously. Methods gen-crally used in controlling filtration of freshwater muds are no longer applicable. The problem of reducing water loss from salt-water muds is not confined to any particular area, but is acute in parts of West Texas. Salt beds several hundred feet thick must be penetrated before the oil-bearing formation is reached. Since the formation drilled does not provide mud-making material, it is necessary to use large quantities of commercial clays, and even the best commercial clay does not afford relief from the problem of high filtration. A laboratory study has been made of methods of improving the filtration characteristics of salt-water muds, and some of the methods have been used in field practice. Laboratory Investigations Procedure Inasmuch as the immediate object of the investigation was the development of means of improving the wall-building properties of muds used in West Texas, an attempt was made to employ muds in the laboratory study comparable to those in field use. Samples of muds used in drilling the producing formations in six wells were secured. The properties of these samples are summarized in Table I, which lists the densities, viscosities, filtrations, and analyses of the filtrates for calcium, chloride, and sulphate. Viscosity was measured in the Stormer viscosimeter at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester8 at a pressure of 100 lb. per sq. in. Filtration rates are considerably higher than those of usual fresh-water muds, which amount to about 20 C.C. in 30 min. Water loss was so rapid in samples 4, 5 and 6 that filtration was complete in less than 10 min. and the values for 30 min. were extrapolated from the rates at shorter

Jan 1, 1942

By G. R. Gray, T. S. Chapman, J. L. Foster

The wall-building properties of salt-water drilling muds can be improved markedly by the addition of: (I) natural gums, such as traga-canth, karaya, and ghatti; (2) seaweeds, such as Irish moss; or (3) gelatinized starch. Results of laboratory tests have been confirmed by field trials. For drilling operations in which the mud becomes contaminated by salt, either through penetrating salt-bearing rocks or by addition of sea water to the mud, the added cost resulting from the use of one of the substances listed above is more than offset by freedom from stuck drill pipe and ease in running casing. Introduction It has been recognized for many years that oil production might be seriously hampered by infiltration of water from the drilling mud.l-4 As knowledge of the mechanism of the wall-building process advanced, methods were developed for evaluating the filtration characteristics of muds.5-ll The wall-building properties of freshwater muds are commonly regulated by the addition of bentonitic clays, or of agents to promote the dispersion of the natural mud solids. When strata bearing soluble salts are encountered in the course of drilling, the salts are incorporated in the mud; the clay solids are flocculated and water loss is increased tremendously. Methods gen-crally used in controlling filtration of freshwater muds are no longer applicable. The problem of reducing water loss from salt-water muds is not confined to any particular area, but is acute in parts of West Texas. Salt beds several hundred feet thick must be penetrated before the oil-bearing formation is reached. Since the formation drilled does not provide mud-making material, it is necessary to use large quantities of commercial clays, and even the best commercial clay does not afford relief from the problem of high filtration. A laboratory study has been made of methods of improving the filtration characteristics of salt-water muds, and some of the methods have been used in field practice. Laboratory Investigations Procedure Inasmuch as the immediate object of the investigation was the development of means of improving the wall-building properties of muds used in West Texas, an attempt was made to employ muds in the laboratory study comparable to those in field use. Samples of muds used in drilling the producing formations in six wells were secured. The properties of these samples are summarized in Table I, which lists the densities, viscosities, filtrations, and analyses of the filtrates for calcium, chloride, and sulphate. Viscosity was measured in the Stormer viscosimeter at 600 r.p.m. Water loss was determined at 80°F. with the Baroid low-pressure wall-building tester8 at a pressure of 100 lb. per sq. in. Filtration rates are considerably higher than those of usual fresh-water muds, which amount to about 20 C.C. in 30 min. Water loss was so rapid in samples 4, 5 and 6 that filtration was complete in less than 10 min. and the values for 30 min. were extrapolated from the rates at shorter

Jan 1, 1942