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By Khosrow Bakhtar

A series of nineteen shear tests were performed on fractures 1 m2 in area, generated in blocks of sandstone, granite, tuff, hydro- stone and concrete. The tests were conducted under quasi-static and dynamic loading conditions. A vertical stress assisted fracturing technique was developed to create the fractures through the large test blocks. Prior to testing, the fractured surface of each block was characterized using the Barton JRC-JCS concept. The results of characterization were used to generate the peak strength envelope for each fractured surface. Attempts were made to model the stress path based on the classical transformation equations which assumes a theoretical plane, elastic isotropic properties, and therefore no slip. However, this approach gave rise to a stress path passing above the strength envelope which is clearly unacceptable. The results of the experimental investigations indicated that actual stress path is affected by the dilatancy due to fracture roughness, as well as by the side friction imposed by the boundary conditions. By introducing the corrections due to the dilation and boundary conditions into the stress transformation equation, the fully corrected stress paths for predicting the strength of fractured blocks were obtained.

Jan 1, 1984

By J. C. Bradley

THE relation of annealing temperature to conductivity of copper wire has been determined. Conductivity hard was 98.26 per cent. After a 10-min. heating at 200°C. it was 98.69. By annealing 10 min. at 300° C. a large increase, to 100.93, occurred. Maximum conductivity, 101.15, was attained after a 500° C. anneal; thereafter it decreased to 100.53 after a 950° C. anneal. If copper is gassed the decrease is much more than this. Materials and Methods The work was done on high grade electrolytic copper, 99.942 per cent. copper plus silver, silver 0.0008 per cent. It was hot-rolled to >/4 in., then cold drawn to 0.080 in. The wire was cut into 25 5-ft. lengths and numbered 1 to 25 as cut. Four samples were tested hard. The others were wound into 5-in. diameter coils. For the 100° C. heating a coil was put into water, the water brought to boiling, and the wire kept at this temperature for 10 min. For the higher temperatures the coils were placed in envelopes of sheet copper, a little water added, and the envelopes sealed by folding over the edges twice, and hammering them together. This kept the air out very well. The envelope and wire 'were brought to the desired temperature; this was maintained for 10 min., then the whole was water-quenched.

Jan 1, 1927

By E. Douglas, D. N. Collins, J. R. Stevens

E. Douglas (Dept. of Scientific and lndustrial Re-search, Warren Spring Laboratory, Hertfordshire, England) — The authors are to be congratulated on the considerable improvements they have made in tailoring efficiency and selectivity terms which are generally superior to the alternative forms in current use. However, I feel that their efficiency expression is limited to lower-grade feeds; its accuracy reduces as the feed grade increases. For example, its application to such processes as the beneficiation of glass sands, refractories and clays will invoIve considerable inaccuracies. The reason for this lies in the direct use of recovery, which, with high-grade feeds, biases their empirical expression, R(1 - c/h). With a 90% grade feed, the recovery weighting for the slightest degree of beneficiation, over a zero efficiency sampling operation, will be 90+%+ I disagree with their second basic requirement which states that there can be no fundamental basis for any single quantifying expression. A formula giving a comprehensive representation of concentra- tion efficiency can be derived fundamentally accord-to the procedure outlined in the literature. '' This formula, called the Basic Efficiency formula, is

Jan 1, 1963

The following officers and committee chairmen were elected: Honorary Chairman, Herbert Hoover; Chairman, Elmer A. Sperry, New York; Vice-Chairman and Chair-man of the Executive Committee, John W. Lieb, New York; Vice-Chairman, C. E. Grunsky (Pacific Coast), San Francisco; C. F. Kettering (Middle West), Detroit; Execu-tive Secretary, Maurice Holland; Executive Committee: Gano Dunn, George W. Fuller, Maurice Holland, Frank B. Jewett, John W. Lieb, H. J. McGraw, Calvin W. Rice, W. E. Wickenden, all of New York; Dugald C. Jackson, Cambridge, Mass.; 0. C. Merrill, Washington, D. C.; Charles F. Scott, New Haven, Conn.; Elmer A. Sperry, Brooklyn, N. Y.; Finance Committee. John W. Lieb; Technical Program Committee: D. C. Jackson; Transporta-tion Committee: F. B. Jewett; Entertainment Committee: 0. C. Merrill; Publicity: J. H. McGraw; Promotion and Attendance: George W. Fuller.

Jan 5, 1928

Mining and oil industry representatives are scheduled to testify May 15 at hearings on the Simpson bill to extend the Reciprocal Trade Agreements Act, Several Congressmen have introduced bills to extend present trade agreements without modification. Price of copper appears to be stabilizing at 30[] per lb, after a period where market price ranged from 27 to 34[]. Copper offerings from abroad were finding no takers at 30.24[] per lb late in April.

Jan 5, 1953

Abbey, Robert Graham, District Mgr.. The W. W. Sly Mfg. Co., 50 Church St.. New York, N. Y. '21 Abbott, A. N., Mines Supt., Mazapil Copper Co., LtdConcepcion del Oro, Zac., Mexico. '28 *Abbott, Argyle Campbell, Dev. Dept., E. I. du Pont de Nemours & Co., Wilmington, Del. '29 Abbott, Clarence E., V.P., Charge of Raw Materials, Tenn. Coal, Iron & R. R. Co., 1242 Brown-Marx Bldg.. Birmingham, Ala. '04 Abbott, Louis Benjamin, Chief Engr., Elkhorn Div., Consolidation Coal Co., Jenkins, Ky. '16 Abeel, George H., Jr., Cons. Min. Engr Box 427, Santa Monica, Cal. '18 Abel, Albert E., Asst. to Pres., Valley Mould & Iron Corp Hubbard, Ohio. '19 Abel, Raymond L., Asst. Prof., Dept. of Pet. Refin., Univ. of Pittsburgh Pittsburgh. Pa. '28 Abeel, Leo M., Research Engr., Sullivan Concentrator Chapman Camp, B. C., Canada. '31

Jan 1, 1929

By J. C. Bradley

THE relation of annealing temperature to conductivity of copper wire has been determined.1 Conductivity hard was 98.26 per cent. After a 10-min. heating at 200° C. it was 98.69. By annealing 10 min. at 300° C. a large increase, to 100.93, occurred. Maximum conductivity, 101.15, was attained after a 500° C. anneal; thereafter it decreased to 100.53 after a 950° C. anneal. If copper is gassed the decrease is much more than this. MATERIAL AND METHOD The work was done on high grade electrolytic copper, 99.942 per cent. copper-plus silver, silver 0.0008 per cent. It was hot-rolled to 3 in., then cold drawn to 0.080 in. The wire was cut into 25 5-ft. lengths and numbered 1 to 25 as cut. Four samples were tested hard. The others were wound into 5-in. diameter coils. For the 100° C. heating a coil was put into water, the water brought to boiling, and the wire kept at this temperature for 10 min. For the higher temperatures the coils were placed in envelopes of sheet copper, a little water added, and the envelopes sealed by folding over the edges twice, and hammering them together. This kept the air out very well. The envelope and wire were brought to the desired temperature; this was maintained for 10 min., then the whole was water-quenched.

Jan 1, 1927

In 1973, US Borax & Chemical Corp. began investing three days wages and about $20 in training materials in every new employee before having him report to his first job. The result? Accidents involving new employees in the past two years have dropped by more than half from the 1972 level. What made this success possible was safety training done with programmed instruction materials-which, incidentally, US Borax also uses for vocational training.

Jan 4, 1976

Jan 1, 1967

By Charles S. Larkey

Numerous papers have been published on the use of graphic methods for determining the best curve for estimating the production decline of oil wells but, as far as the writer has been able to ascertain, nothing has been published showing how curves may be worked out mathematically that will conform most closely to the production data under consideration in any given instance; hence the writer has endeavored to show just how such application can be made. Among the valuation engineers, two types of curves are in current use for the representation of the decline in production of oil wells. One may be represented by the equation, y = krx; this is sometimes known as a percentage curve, for the production for any period is multiplied by a constant rate or percentage to obtain the production for the succeeding period. It appears as a straight line on semilogarithmic cross-section paper. The other curve may be represented by the equation, y = kxn, and is shown as a straight line on logarithmic cross-section paper. In each equation, y represents the number of barrels produced in a given period of time, and x the successive periods of time. The other letters are constants to be determined for each well, or group of wells considered in arriving at the most probable curve to represent the rate of production for a given property. From this the underground reserves may be estimated by extrapolation, or by extending the curve beyond the last known period of production to show the most probable production values for the future. Application to the Burbank Pool Fig. 1 relates to a property in the Burbank Pool, Osage County, Okla. The production is shown as an average per well per month, is plotted to the vertical scale of barrels on the left-hand margin and to the horizontal scale of months at the bottom of the chart. In column y, the number of barrels is listed beginning with May, 1922, as the first month on which to base a decline curve. The type of curve used is of the form, y = krx, or, expressed in logarithms, log y = log k + x log r, in which log k and log r are constants to be determined so that the curve will most closely approximate the production data given.

Jan 1, 1925

By F. A. Olson, S. L. Pohlman

A unique method of measuring weight loss as a function 3 of time, with a sensitivity of 10-5 grams, while leaching copper minerals with a flowing acid leach solution has been developed. Kinetic results obtained coupled with visual and microprobe analyses show topochemical reaction for the leaching of chrysocolla with sulfuric acid. The kinetics follow a shrinking core model and show ion diffusion through a product layer, chemical reaction at the unreacted core interface and mass transfer through the boundary layer as being important.

Jan 1, 1974

By James J. Halbouty, Michel T. Halbouty

Drilling activity in the South Texas area, which includes the South Corpus Christi and Laredo districts, showed a marked decline during 1941 from that of the preceding year. The rate of new discoveries, however, 'compared favorably with exploratory results of 1940 because of the many new productive sands opened in existing fields. South Texas completions for 1941 were about 12.3 per cent below the 1940 figure, compared with an increase of approximately 5.5 per cent in the total number of completions in the United States during 1941 over the 1940 total. During the year, 1452 wells were drilled in this area; of these, 1205 were drilled in or as extensions to the proven fields, and 247 were rank wildcats drilled in search of new producing pools. The comparable 1940 figures were: 1320 field or extension wells and 336 rank wildcats, a total of 1656 completions. This represents a decline in 1941 of approximately 8.7 per cent in proven-area wells, and of about 26.5 per cent in rank wildcats. It must be stressed that wells that were considered rank wildcats at the beginning of operations, but which opened production later classified as additions to existing fields, are not regarded as rank wildcats in this and previous annual reports on this same area. These wells are classified as semiwildcats (Table 2). There were 13 new oil or distillate fields and 4 new gas areas opened during the year, as listed in the next column. This listing represents a decline of 32 per cent from the 25 new areas found during the previous year, and to a great extent can be attributed to the 26.5 per cent decline in wildcatting. The rate of new discoveries based on the 247 wildcats was 14.5 to I, which compares somewhat unfavorably with the 13.4 to I ratio obtained in 1940 (Table 5). Dry wildcats totaled 230. The proof of the prolific character of the South Texas area as a source of petroleum reservoirs is to be found in the fact that of the 1205 field or extension (semiwildcat) wells completed during the past year 61 opened production from new sands or found crude in formerly distillate-producing sands. The 1940 total of 1320 such wells accounted for 50 horizons that provided either new production or crude in distillate sands, and in this respect the 1941 rate of discovery shows to greater advantage, the ratios for new sands being 19.7 to I for 1941 and 26.4 to I for 1940. The 1205 field or semiwildcat wells completed in 1941 resulted in 926 oil or dis-

Jan 1, 1942

By James J. Halbouty, Michel T. Halbouty

Drilling activity in the South Texas area, which includes the South Corpus Christi and Laredo districts, showed a marked decline during 1941 from that of the preceding year. The rate of new discoveries, however, 'compared favorably with exploratory results of 1940 because of the many new productive sands opened in existing fields. South Texas completions for 1941 were about 12.3 per cent below the 1940 figure, compared with an increase of approximately 5.5 per cent in the total number of completions in the United States during 1941 over the 1940 total. During the year, 1452 wells were drilled in this area; of these, 1205 were drilled in or as extensions to the proven fields, and 247 were rank wildcats drilled in search of new producing pools. The comparable 1940 figures were: 1320 field or extension wells and 336 rank wildcats, a total of 1656 completions. This represents a decline in 1941 of approximately 8.7 per cent in proven-area wells, and of about 26.5 per cent in rank wildcats. It must be stressed that wells that were considered rank wildcats at the beginning of operations, but which opened production later classified as additions to existing fields, are not regarded as rank wildcats in this and previous annual reports on this same area. These wells are classified as semiwildcats (Table 2). There were 13 new oil or distillate fields and 4 new gas areas opened during the year, as listed in the next column. This listing represents a decline of 32 per cent from the 25 new areas found during the previous year, and to a great extent can be attributed to the 26.5 per cent decline in wildcatting. The rate of new discoveries based on the 247 wildcats was 14.5 to I, which compares somewhat unfavorably with the 13.4 to I ratio obtained in 1940 (Table 5). Dry wildcats totaled 230. The proof of the prolific character of the South Texas area as a source of petroleum reservoirs is to be found in the fact that of the 1205 field or extension (semiwildcat) wells completed during the past year 61 opened production from new sands or found crude in formerly distillate-producing sands. The 1940 total of 1320 such wells accounted for 50 horizons that provided either new production or crude in distillate sands, and in this respect the 1941 rate of discovery shows to greater advantage, the ratios for new sands being 19.7 to I for 1941 and 26.4 to I for 1940. The 1205 field or semiwildcat wells completed in 1941 resulted in 926 oil or dis-

Jan 1, 1942

By W. H. Hough, P. B. Leavenworth

Development during 1942 led to the discovery of 26 new fields in the Texas Gulf Coast, as compared with 27 during 1941. Of these, 19 are classed as oil fields, 4 distillate fields, and 3 gas fields. Production from the new fields amounted to 614,467 bbl. to October 1942. Producing Sections.—Discoveries in I942, compared with the previous two years, classified by producing formations, are shown in the following table: It is interesting to note the increase in Wilcox discoveries due to the extensive geophysical campaign that has been con. ducted since 1940. Drilling.—During the year 688 wells were drilled, of which 574 produced oil or gas and 114 were dry. This represents a considerable decline in activity over the previous year, when 1405 wells were drilled in the area, of which 1081 were producers and 324 failures. Jackson County continued to hold the lead, with 222 wells completed. Production.—-Despite curtailed drilling, production amounted to 118,009,451 bbl. for 1942, indicating a slight increase over the 113,726,893 bbl. produced during 1941. The statistics in Tables I and 2 include condensate and distillate as oil production, because many Gulf Coast fields produce oils with a wide variation of specific gravities, all of which are commingled in pipe lines. Table 3 shows by counties most of the activities referred to. The number of wells drilled includes only field wells; not wildcats. Outstanding Fields of 1942 The Texas Gulf Coast covered in this report has 270 more or less active oil and gas fields, including the new discoveries of 1942. Of these the most outstanding from the standpoint of production are listed in Table 4. Each of these fields produced one million barrels or more during 1942. Some of the fields where new extensions are occasionally referred to as separate fields, such as West Columbia and New West Columbia, or Thompson and South Thompson, are combined to give a more accurate outline. Two interesting facts may be noted from this list of some 26 oil fields: (I) that the Lolita field, Jackson County, is the only discovery since 1938 to produce more than one million barrels annually, although there have been 79 discoveries since Jan. I, 1940; (2) that 20 of these 26 fields produce from the Frio. New Fields ALief, Harris County.—Pure Oil Company's No. I Mike Albanese was drilled to 8637 ft. in Cook Mountain shale. After numerous tests the well was completed on Apr. 20, 1942, in a Yegua sand at 7919 to 7924 ft. for 54 bbl. of 52' gravity oil and 3,335,000 cu. ft. of gas through

Jan 1, 1943

By W. H. Hough, P. B. Leavenworth

Development during 1942 led to the discovery of 26 new fields in the Texas Gulf Coast, as compared with 27 during 1941. Of these, 19 are classed as oil fields, 4 distillate fields, and 3 gas fields. Production from the new fields amounted to 614,467 bbl. to October 1942. Producing Sections.—Discoveries in I942, compared with the previous two years, classified by producing formations, are shown in the following table: It is interesting to note the increase in Wilcox discoveries due to the extensive geophysical campaign that has been con. ducted since 1940. Drilling.—During the year 688 wells were drilled, of which 574 produced oil or gas and 114 were dry. This represents a considerable decline in activity over the previous year, when 1405 wells were drilled in the area, of which 1081 were producers and 324 failures. Jackson County continued to hold the lead, with 222 wells completed. Production.—-Despite curtailed drilling, production amounted to 118,009,451 bbl. for 1942, indicating a slight increase over the 113,726,893 bbl. produced during 1941. The statistics in Tables I and 2 include condensate and distillate as oil production, because many Gulf Coast fields produce oils with a wide variation of specific gravities, all of which are commingled in pipe lines. Table 3 shows by counties most of the activities referred to. The number of wells drilled includes only field wells; not wildcats. Outstanding Fields of 1942 The Texas Gulf Coast covered in this report has 270 more or less active oil and gas fields, including the new discoveries of 1942. Of these the most outstanding from the standpoint of production are listed in Table 4. Each of these fields produced one million barrels or more during 1942. Some of the fields where new extensions are occasionally referred to as separate fields, such as West Columbia and New West Columbia, or Thompson and South Thompson, are combined to give a more accurate outline. Two interesting facts may be noted from this list of some 26 oil fields: (I) that the Lolita field, Jackson County, is the only discovery since 1938 to produce more than one million barrels annually, although there have been 79 discoveries since Jan. I, 1940; (2) that 20 of these 26 fields produce from the Frio. New Fields ALief, Harris County.—Pure Oil Company's No. I Mike Albanese was drilled to 8637 ft. in Cook Mountain shale. After numerous tests the well was completed on Apr. 20, 1942, in a Yegua sand at 7919 to 7924 ft. for 54 bbl. of 52' gravity oil and 3,335,000 cu. ft. of gas through

Jan 1, 1943

By G. Thodos, W. F. Stevens

The point-source function introduced by Horner' us a solution to the general unsteady-state equation for the flow of fluids through porous media has been utilized to calculate pressure profiles for adjacent wells as a function of time. By trial and error, the time at which the pressure waves meet to cause interference can then be calculated. For this calculation, the time of interference is arbitrarily defined as that time when both pressure waves exhibit a pressure decrease of 25 psi ar the same point within the formation. To illustrate the method, an example involving two adjacent wells producing at different rates has been worked out and is presented in detail. INTRODUCTION The initiation of production of a new well is usually accompanied by pressure drawdown measurements in order to establish the extent and characteristics of the formation. The interpretation of such pressure drawdown data is based on mathematical developments involving a single well in an infinite reservoir. If more than one well is present in a reservoir, the possibility of interaction between wells exists. Therefore, care must be taken in interpreting the pressure drawdown data. It becomes important to be able to determine when this interaction, or interference, becomes significant. This paper presents a method for the prediction of the approximate time of interference between two such adjacent wells. The basic differential equation describing the pressure distribution existing during unsteady-state flow of a slightly compressible fluid has been solved by Hor-ner.' for a constant production rate from a circular homogeneous reservoir of infinite extent. The solution utilizes the point-source function to define the pressure at various points within the formation as a function of time. The resulting expression is: q = production rate, STB/D ,;= formation volume factor, dimension-less µ = fluid viscosity, cp k = formation permeability. md H = formation thickness, ft C - fluid compressibility, psi' F = formation porosity, dimensionless R = distance from centerline of well, ft T = production time, hours Ei(—u) = Ei-function of U Eq. 1 may be used to calculate the pressure profiles generated during production from a single well in an infinite reservoir.

By S. E. Bretherton

This title introduces the subject I wish to describe to my fellow members, very few of whom, I 'hope, have ever had as much trouble with the smelting of ore containing much zinc, either in the lead blast furnace or the matting furnace, as circumstances have forced upon me: First, for several years in Leadville, Colo., after the sulphide ores containing zinc had been developed with greater depth and were sold to the intereats with which I was connected for smelt-ing in the blast furnace for the recovery of the lead, silver, and gold; then, in New Mexico and Arizona, where the principal source of ore supply for our custom smelter was from miners who sent most of their product in the form of concentrates, which we briquetted and smelted in the blast furnace, producing a matte containing copper, silver, and gold, for which we were paid; together with some zinc and lead, which was penalized if in excess of a maximum base set by the refinery to which we sold our copper matte; last, but not least, my experience in Shasta county, Gal., where for the sake of recovering $13 per ton value in copper, silver, and gold, I have smelted ore containing as high as 40 per cent. zinc (the last 18,951 tons smelted averaged 15 3/10 per cent. zinc) which we not only lost, but which it cost us money to lose. After such an experience, and knowing that, instead of being worth only $13 per ton, such 15 per cent. zinc ore should be worth about $30, including zinc at the present market value, the question of recovering the zinc in a profitable manner from such ore became very interesting to me. During several years' time I sent samples, of from 5 to 1,200 lb. each, to be tested by the different best-known zinc-recovery plants, and experimented with several processes proposed by others for the treatment of such ore, with but little encouragement, until I

Jan 1, 1914

By R. Schuhmann, J. Th. Overbeek, P. L. De Bruyn

THE technique of concentrating valuable minerals from lean ores by flotation depends upon the creation of a finite contact angle at the three-phase contact, mineral-water-air. If the mineral is completely wetted by the water phase, contact angle zero, there is no tendency for air bubbles to attach themselves to the mineral. However, when the contact angle is finite, the surface free energy of the system, water-air bubble-mineral particle, can be diminished by contact between the bubble and the particle, and if not too heavy the mineral will be levitated in the froth. With a few exceptions, all clean minerals are completely wetted by pure water. Thus the art of flotation consists in adding substances to the water to make a finite contact angle with the mineral to be floated, but to leave the other minerals with a zero contact angle. The contact angle concept and experimental measurements of contact angles have played important roles in flotation research for several decades.'-" Nevertheless, there remain unanswered some basic questions as to the scientific significance of the contact angle and the nature of the processes by which flotation reagents affect contact angles. The contact angle is a complex quantity because the properties of three different phases, or rather of three different interfaces, control its magnitude. Considering the interfaces close to the region of ternary contact to be plane, the relation among the contact angle and the three binary interfacial tensions is easily derived. The condition for equilibrium among the three surface tensions, Fig. 1, or the requirement of minimum total surface free energy leads to Young's equation, Eq. I: ysa — ysl = yLA cos 0 [1] According to this equation, the contact angle has one well-defined value. Actually it is found in many experiments that the value of the contact angle depends on whether the air is replacing liquid over the solid (receding angle) or the liquid is replacing air (advancing angle). The receding angle is always the smaller of the two.4 Two explanations have been offered for this experimental fact. According to some investigators,5-8 roughness of the surface causes apparent contact angles that are different for the receding and the advancing cases although the actual local contact angle may be completely determined by Eq. 1. The other explanation involves the hypothesis that the solid-air interface after the liquid has just receded is different from the same interface when no liquid has previously covered it.1,4 Adsorption of constituents of the air or liquid might play a role here. In this discussion the difference between advancing and receding contact angle will be neglected and plane surfaces where Eq. 1 describes the situation will be considered. But there is still a fundamental obstacle to the application of Young's equation. The surface tension of the liquid (rla) can easily be determined, but the two surface tensions of the solid (rsa and ySL) cannot be measured directly. Eq. 1, however, is not without value. By contact angle measurements it is possible to establish how ysl — ysl varies with the addition of solutes to the liquid phase. Also, Eq. 1 affords a convenient starting point for calculating net forces and energy changes involved in the process of bubble-particle attachment.1,2 . If for the moment surface tension of the liquid (yLa) is considered a constant, an increase in ysa — ysL, will tend to decrease the contact angle. A decrease in ySA — ysl, corresponds to an increase of the contact angle. In cases where ySA — ySL > yLa the contact angle is zero; it will only reach finite values when ysa — ysa has been decreased below YLA. Thus on the basis of Young's equation and contact angle measurements alone, it can be learned how flotation reagents affect the difference Ysa — ysl, but no conclusions can be drawn as to the effects of reagents on the individual surface tensions ysa, and ysL, not even as to signs or directions of the surface tension changes resulting from reagent additions. A quantitative relationship between the surface tension or interfacial tension and the adsorption occurring at a surface or an interface is given by the Gibbs equation, which for constant temperature and pressure reads dy = — 2 T, du, [2] where dy is the infinitesimal change in surface tension accompanying a change in chemical potential

Jan 1, 1955

By Charles E. Lundin

Pressure-temperature-composition data were obtainedfor the Er-H system. Measurements werecar-ried out in the temperature range of 473° to 1223°K, the composition range of erbium to ErH,, and the pressure range of 10-5 to 760 Torr. Solubility relationships were established from these data throughout the system. Three solid-solution phases were delineated: metal solid solution, dihydride phase, and trihydride phase. The trihydride Phase decomposes at about 656°K and 1 atm pressure. The dihydride phase is stable to about 1023°K, but becomes more deficient in hydrogen above this temperature. The equilibrium decomposition pressure-temperature relationships in the two-phase regions, erbium solid solution plus dihydride and dihydride plus trihydride, were deter- The differential heats of reaction in these two regions are AH = - 52.6 * 0.3 and - 19.8 i 0.2 kcal per mole of Hz, respectively. The differential entropies of reaction are AS = - 35.2 * 0.3 and - 30.1 * 0.4 cal per mole HZ.deg, respectively. Relative partial molal and integral thermodynamic quuntities were calculated in the system to the dihydride phase. RARE earth metal-hydrogen systems have been the subject of general survey,1"4 and all have been found to form hydride phases. The heavy rare earths, of which erbium is a member, form dihydride and trihydride phases with different crystal structures, whereas the light rare earths form only a single-phase dihydride which expands without structure change, as hydrogen is added, to the trihydride composition. These materials are of interest primarily because of their theoretical properties, such as bonding, defect structure, and thermodynamic and electronic characteristics. Erbium has been studied in several previous investigations.5, 6 It was deemed desirable to more thoroughly and accurately define the system, both for the phase equilibria and the thermodynamic properties. I) EXPERIMENTAL PROCEDURE A Sieverts&apos; apparatus was employed to conduct the experimental measurements. Briefly, it consisted of a source of pure hydrogen, a precision gas-measuring buret, a heated reaction chamber, a mercury manometer, and two McLeod gages (a CVC, GM 100A and CVC, GM 110). Pure hydrogen was obtained by passing hydrogen through a heated Pd-Ag thimble. The hydrogen was analyzed and found to have only a trace of oxygen and nitrogen. A 100-ml precision gas buret graduated to 0.1-ml divisions was used to measure and admit hydrogen to the reaction chamber. The reaction unit consisted of a quartz tube surrounded by a nichrome-wound furnace. The furnace temperature was controlled by a recorder-controller to ±1°K. An independent measurement of the sample temperature in the quartz tube was made by means of a chromel-alumel thermocouple situated outside, but adjacent to, the quartz tube near the specimen. Pressure in the manometer range was measured to ±0.5 Torr and in the McLeod range (10-4 to 10 Torr) to ±3 pct. The hydrogen compositions in erbium were calculated in terms of hydrogen-to-erbium atomic ratio. These compositions were estimated to be ±0.01 H/Er. The erbium metal was obtained from the Lunex Co. in the form of sponge. The metal was nuclear grade with a purity of 99.9 pct +. The oxygen content was reported to be 340 ppm and the nitrogen not detectable. Metallographically the structure was almost free of second phase (<1 vol pct). A quantity of sponge was arc-melted for use as charge material. The solid material was compared with the sponge in the pressure-temperature-composition relationships. They were found to be identical. Therefore, sponge material was used henceforth, so that equilibrium could be attained more rapidly. The specimen size was about 0.2 grain for each loading of the reaction chamber. The procedure employed to obtain the pressure-temperature-composition data was to develop experimentally a family of isothermal curves of composition vs pressure. First, a specimen of erbium was wrapped in a tungsten foil capsule to prevent contact with the quartz tube. After loading the specimen, the system was evacuated to less than l0-6 Torr, flushed several times with high-purity hydrogen, and evacuated again ready for the start of the experiment. The furnace was then brought to the desired temperature. A measured amount of hydrogen was admitted into the chamber. Equilibrium was allowed to be attained, the pressure read, and the process then repeated many times until 1 atm of gas pressure was finally reached. Other isotherms were then developed in the same manner. The partial pressure plateaus were determined by another manner. In the solid solution-dihydride region a composition of approximately 1.0 H/Er was selected on the plateau. The temperature was varied throughout the range of interest. At each temperature level, equilibrium was achieved, the pressure read, and the next temperature attained. The temperature was cycled both up and down. In the dihydride-trihy-dride region, the plateaus were determined in the 473" to 651°K range only by heating to the desired temperature and not by both heating and cooling. The data were much more reproducible in this manner. Equilibrium required long periods of time. Specimens were initially hydrided to 2.8 H/Er, so that at the higher

Jan 1, 1969

Jan 1, 1967