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By S. C. Miller, R. D. Carter, H. G. Riley

A merhod based on theoretical considerations is presented for estimating srabilized performance of gas wells from data obtained from short-term flow tests. Calculated results are presented for II gas wells evaluated with four-to five-hour flow tests. For seven wells on which comparison war available, satisfactory agreement between measured and calculated performance was obfained. Although the final results are favorable, diflerences in flow capacity k,h obtained from flow tests conducted at different rates were observed. This inconsistency did not seriously affect the calculated results in the test wells. INTRODUCTION In order to negotiate the sale of gas from newly drilled gas wells and to plan otherwise for the orderly exploitation of gas reserves, it is necessary to predict the long-term withdrawal rates physically possible for each well. Since low permeability gas wells do not stabilize except after a lengthy period of flow, the operator is unable, without wasting large amounts of gas, to measure directly the stabilized performance prior to contracting for sale of the gas and connecting the well to a pipeline. This problem is not new, but is one which has recently received considerable attention because of the rising importance of natural gas in the economy and new emphasis on the development of gas reserves. Thus, a method is needed for estimating stabilized performance from information obtained from short-flow tests in which stabilized flow is not attained. Such short tests would be suitable for wells not connected to a pipeline since the tests require only small amounts of time, labor and production of gas. Other requirements of such a method are short calculation time and use of a model of the gas well and its reservoir drainage area which is as consistent as possible with present theoretical, experimental and field knowledge. The method presented herein was developed in an effort to meet these requirements. It has been named the "two-Row method". In addition to the section on the evelopment and description of the method, a description of field application of the method and a discussion of well test results are in- cluded. Finally, there is a section on an additional consideration prompted by some of the test results. The Appendix contains certain details of the derivation of the two-flow method and a sample calculation for Test Well 1. MATHEMATICAL DEVELOPMENT AND DESCRIPTION OF THE METHOD The method is based upon the following assumptions: (1) The system can be described as a finite cylindrical gas reservoir produced by a single cylindrical well located at the center of the reservoir. Flow is strictly radial. (2) Flow obeys Darcy's law except very near the well where a quadratic flow law is assumed. (3) The system is also characterized by a laminar flow skin factor. The use of a quadratic or turbulent flow term is more fully justified in Refs. 1 and 2. When such a system is opened at the wellbore to constant rate flow from an initial condition of uniform pressure distribution, the radius or drainage quickly passes through the non-Darcy flow and "skin effect" region imrnediately surrounding the well. After the drainage radius or "transient" has passed beyond this region and before it reaches the external boundary, drawdown can be expressed by'." After the drainage radius reaches the external boundary, stabilized flow exists and drawdown is given by'," Eqs. 1 and 2 form the basis for the method. The validity of these equations will now be examined in the light of some well test data previously available. It has been found by actual measurements on gas wells that the relationship between drawdown and flow rate, that is the performance curve, is closely approximated by' Eq. 3 is a straight line on log-log graph paper. Eq. 2 and, for any lixed value of time, Eq. 1 plot as a curve which is slightly concave upward on log-log graph

By N. J. Themelis, A. W. Last

Autogenous grinding, broadly defined as the self-comminution of ore in a cylindrical tumbling mill without using auxiliary grinding media, was first applied in the early 1930s in the so-called Hadsel mills (Hardinge, 1955) as seen in [Fig. 1], mainly used in gold mines on the US West Coast. A number of these mills were built in sizes of 6.1 to 7.3 m (20 to 24 ft) in diameter and 1.5 to 1.8 m (5 to 6 ft) in length but were later abandoned because of operating and maintenance problems. Further development of autogenous grinding led to the Hardinge wet grinding mill, the Aerofall dry grinding mill, and others. A tabulation of all known autogenous and semiautogenous installations around the world was sent recently to the authors by G. J. Kushner of Koppers Metal Processing Division. In the size range of 7.3 to 9.8 m (24 to 32 ft) in diameter, it lists a total of thirty mills used in the processing of copper ores. An additional 120 units are listed in the same size range for the processing of iron ores and other minerals. The largest mills in existence are 11.1-m-diam X 4.6-m-long (36-ft-diam X 15-ft-long) mills in Minnesota, powered by 8950 kW (12,000 hp) motors and used in taconite beneficiation. It is indicative of the phenomenal growth of this technology that none of the above 150 mills was in operation prior to 1964. Grinding rates in autogenous mills are very sensitive to variations in ore breakage characteristics and even with fairly constant ore type can exhibit large fluctuations in throughput. Autogenous grinding also depends on availability of a fraction of the ore to be ground in the form of "competent" rock which can withstand to a certain degree the tumbling and impact action within the mill. If the ore is uniformly "soft", it will soon be crushed into small size particles and further grinding, which depends on the existence of large size rocks in the mill, becomes impossible. This apparently is the case with most copper ores, as discussed by Bachman, Last and Nabbs (1970) who described pilot testing of a large number of ore samples from Kennecott 's Chino Mines. Under circumstances where autogenous grinding is impractical, it is possible to realize most of its benefits by utilizing large grinding balls in place of the "competent" rock and practice what has become known in the mining industry as semiautogenous grinding. In semiautogenous grinding (SAG), a grate discharge tumbling mill is fed the product of a primary crusher or run-of-mine rock. Forged steel or alloy grinding balls, in proportions ranging from 3.10% of the total volume in the mill, are used to complement the self-grinding ability of the ore. Semiautogenous circuits can be either designed for single-stage closed-circuit grinding which produces a final product for recovery processes, or for two-stage operation in which the SAG mill product is fed to a second stage of grinding in a conventional ball mill.

Jan 1, 1981

LIST OF THE MEETINGS OF THE INSTITUTE AND THEIR LOCALITIES FROM ITS ORGANIZATION Transactions Number Place Date Vol Page 1 Wilkes-Barre, Pa May, 1871 1 3 2 Bethlehem, Pa August, 1871 1 10 3 Troy, N Y November, 1871 1 13 4 Philadelphia, Pa February, 1872 1 17 5 New York, N Y May, 1872 1 20 6 Pittsburg, Pa October, 1872 1 25 7 Boston, Mass February, 1873 1 28 8 Philadelphia, Pa May, 1873 2 3 9 Easton, Pa October, 1873 2 7 10 New York, N Y February, 1874 211 11 St Louis, Mo May, 1874 3 3 12 Hazleton, Pa October, 1874 3 8 13 New Haven, Conn February, 1875 3 15 14 Dover, N J May, 1875 4 3 15 Cleveland, 0 October, 1875 4 9 16 Washington, D C February, 1876 4 18 17 Philadelphia, Pat June, 1876, 5 3 18 Philadelphia, Pa October, 1876 5 9 19 New York, N Y February, 1877 5 27 20 Wilkes-Barre, Pa May, 1877 6 3 21 Amenia, N Y October, 1877 6 10

Jan 1, 1917

By F. V. Tideswell

THE suggestion, which appears to find increasing favor, that the elementary composition of coals should be used as the basis of their classification, makes it important that our methods of expressing this elementary composition should be refined. It is doubtful whether many published ultimate analyses of coals are accurate within 1 per cent. carbon. Many are probably as much as 3 or 2 per cent. in error in carbon. It is, perhaps, not always realized that the extreme variation in carbon content over the range of bituminous coals is but 16 per cent. An error of 1 per cent. in carbon on analysis corresponds therefore with one-sixteenth of the whole range, an amount which is unjustifiable even for the application to commercial needs of a system of classification based on ultimate analysis. For the purposes of scientific research such limited accuracy is of little value. The object of this paper is to examine one important source of error in ultimate analysis, that due to the occurrence in coal of inorganic material, and to emphasize the need for the quantitative measurements (of carbon more particularly) on coals to be rendered independent of their contents of such material.

Jan 1, 1928

By Otto H. Henry, Edward L. Badwick

Up to the present time, according to Hansen1 and Haughton,2 the constitution of the bismuth-indium system has not yet been published. The generally accepted value for the melting point of indium, as listed in most scientific journals and textbooks, is 155°C. Recently, however, H. M. Davis3 has determined a new melting point for indium of 257.3°C ± 0.1°C. Since bismuth has been used in preponderance as an alloying element in the majority of low-melting alloys, and indium has been used with considerable success in lowering the melting points of low-melting alloys,4,5 an interest has been developed in the application of these two metals, making a complete knowledge of the constitution of its alloys desirable. In this investigation, the melting point of indium reported by H. M. Davis has been found to be substantially correct. A value of 157.2°C ± 0.5°C was determined. The two eutectic compositions have been placed at 34 and 50 pct bismuth with their respective eutectic temperatures as 72.4'C ± 0.5°C and 90°C ± 0.5°C. The bismuth-indium phase diagram has been determined by thermal and microscopic analysis and is shown in Fig I. THERMAL ANALYSIS Granulated bismuth and indium shot, having a guaranteed purity of 99.99 and 99.95 pct, respectively, were melted in a carbon crucible by means of a laboratory heater. To minimize oxidation of the alloys, a heavy mineral oil (Nujol) having a high flash point was used. A platinum-platinum rhodium thermocouple 0f fine wire encased in a thin-walled Pyrex glass tube, about 1/8 in. in diameter, was connected to a type K potentiometer for temperature measurements. The thermo-couple was calibrated against the melting points of tin, bismuth, and the silver-copper eutectic and the boiling point of water. Since the temperature readings could be reproduced to 0.2°C, and the accuracy of the temperature standards in this range is slightly better than 0.5°C, it seems reasonable to assume that the temperature readings are reliable to approximately 0.5°C. The cooling rate could be controlled by varying the amount of insulation surrounding the crucible. Three or four layers of asbestos paper, 1/16r, in. thick, sufficed to give a cooling rate of from 1° to 2°C per minute. Undercooling was slightly noticeable. This condition was minimized by vigorous stirring, since the advantage of using slower rates was too small to justify the greater expenditure

Jan 1, 1947

The following additional notes about prices of coal in the early days were collected from the sources shown. Several data about canal tolls and labor conditions are also included. 1796, November: "The inhabitants lay it (coal) in at about 3;d. (83¢) sterling per bushel." (Ref. 73: p. 147.) 1804, March: "In March, 1804, I sent a person accustomed to mining to open the vein of coal, and to load the ark, which was accomplished, and early in the month of April the ark, with the first cargo of bituminous coal passed safely the Conewago falls, and landed her coal at Columbia, Lancaster County. The coal was sold at 31¢ per bushel at Columbia." ($7.75 per ton). This was the first coal from Clearfield County near the town of that name. (Letter from William Boyd: Pa. Senate Jour., 1833-1834, vol. 2, p. 561.) 1807: The following notice appeared in the Bedford Gazette: "Huntingdon, June 4. "Stone Coal.-Such of the farmers as wish to make experiment with stone coal as a substitute for plaster, in manuring their Indian corn, may be supplied with coal gratis upon application to Peter Hughes, at Mr. Riddle's mines, on the Raystown Branch. The proprietor of the mines offers not only to refund the carriage, but to pay the expenses of applying the coal, if upon a fair experiment it is found to be inferior to plaster, which now sells at two dollars per bushel." (Ref. 735: p. 708.) 1809: Coal was delivered in Pittsburgh at 5¢ per bushel or $1.25 per net ton. (Ref. 444: p. 50.) Coal was delivered in Connellsville at 4¢ per bushel or $1.00 per net ton. (Ibid.: p. 185.) 1810: Pittsburgh.-"Coal may be obtained of a good quality, ready delivered at 5¢ a bushel." ($1.25 per net ton.) (Ref. 315: vol. 2.) 1811: "It (coal) costs 6¢ a bushel at your door." ($1.50 per net ton.) (In Pittsburgh.) (Ref. 277: 1811, p. 68.) 1814: At Columbia, now part of Donors, Washington County, Pa., an original sale of lots in 1814 gave the purchaser of each lot the right to mine stone coal gratis from a bank on the property. (Ref. 410: vol. 1, p. 547.) "A laborer is able to dig upwards of 100 bushels per day." (4 tons.) (Ref. 277: 1814, p. 109.) A paper about the early newspapers in West Virginia says: "Collier Wanting. From 10 to 20 steady and industrious men, who understand digging coal, may obtain high wages in Kenhawa for that business, if immediate application is

Jan 1, 1942

By Paul B. Crawford, Bobby L. Landrum

Electrical model studies have been made of the effect of unsymmetrical vertical fractures on production cnpacity. The study war restricted to the case of two vertical fractures originating at the well and extending out into the reservoir for various distances and orientations. The ratio of the short fracture length to the long fracture length was varied from 0.1 to 1.0 in successive studies. The angle separating the two fractures was varied from 0 to 180 degrees. The most effective fractured patterns were obtained when the fractures were oriented 180 degrees. It was found that when the total fracture length was equal to 0.2 of the drainage radius, the increase in production capacity may vary from approximately 1.55 to 1.95. depending upon the ratio of the short fracture length to the long fracture length and the angle separating the two fractures. If the total fracture length were 0.5 of the drainape- radius. poroduction cavacitv., increases varving 1.95 to 2.65 were observed, depending on the angle between the fractures and the ratio of the .short fracture length to the long fracture length. The fractured well production capacity decreased aPproxin?ately I to 10 per cent as the angle separating the fractures was varied from 180 to 90 degrees. It was dependent on the particular fracture. The commercial application of reservoir fracturing techniques has caused an interest to be expressed in the effect of vertical and horizontal fractures on production capacities. Some data have indicated that substantially vertical fractures may be created in some reservoirs. It is believed that the fractures are possibly unsymmetrical, that is, one fracture may extend due north 100 ft and a second fracture on the opposite side of the well may extend south or southeast only 50 ft. The total fracture length, ratios of the lengths and angles of separation may vary considerably. For this reason variations in these factors were considered. The study was restricted to the case of two vertical fractures originating at the well and extending out into the reservoir. It is not known that such will occur in a reservoir, but the results may be of value in interpreting or studying fracturing applications. PROCEDURE An electrical model was used in this study of the effect of unsymmetrical vertical fractures on production capacity, A wooden tank 30 in. in diameter and approximately 2 in deep was coated with paraffin wax. A copper band was situated at the periphery and a single wire electrode was positioned at the center of the tank. The ratio of the reservoir radius divided by the

Jan 1, 1956

By G. Thodos, E. M. Phillips

A reduced density correlation for the gaseous and liquid regions of ethane has been developed from all the experimental PVT data available in the literature for this substance. Saturated vapor and liquid densities reported for methane, propane and n-butane were utilized to establish the rectilinear-diameter line for ethane. This line was then used with the saturated-vapor data for ethane to produce the saturated envelope for this substance. Most of the saturated liquid data reported for ethane were found to be inconsistent with the saturated-liquid curve resulting from this study. The correlation covers the regions 0.65 < TR <6.0 and 0 < PR < 15. For regions for which no experimental data have been reported, the isobars of the correlation were extended by the use of the theorem of corresponding states. This correlation is presented both on rectilinear and log-log coordinates. INTRODUCTION At the present time, there is considerable interest in the exact PVT behavior of pure hydrocarbons. Matschke and Thodos12 recently have developed a comprehensive compilation of experimental vapor and liquid density data for methane. Similar studies have been conducted for other pure substances.4, 7 In the present study the density data available in the literature for gaseous and liquid ethane have been critically reviewed and utilized to develop a reduced density correlation for this substance. SATURATED LIQUID AND VAPOR DENSITIES The rectilinear-diameter rule proposed by Cailletet and Mathias5 states that the sum of the saturated liquid and vapor densities of a pure substance is a linear function of temperature which passes through the critical point. This law, although empirical, has been well established by continued verification since its conception in 1886. This rule has been applied to the saturated density data of methane,6 propane 17 and n-butane8 to produce the straight lines presented in Fig. 1 which pass through the critical point TR = 1.00, Pr = 2.00. The rectilinear-diameter relationship for ethane was established from the lines for the other substances in Fig. 1 by plotting the quantity p~, + PR against zc for different reduced temperatures. A critical analysis of the saturated vapor and liquid densities reported for ethane by Kuenen,10 Maass and McIntosh,11 and Sage, Webster and Lacey18 revealed that the values of PR1 + pr resulting from these studies were inconsistent with the rectilinear-diameter line obtained from the reliable density data of the other substances, as shown in Fig. 1. In the analysis of these data, reduced quantities were calculated using the critical con-

By Park Wright

THE fact that granite has been encountered by the drill by those in search of oil and gas in Kansas is becoming more and more a matter of interest, not only to the oil producer but to everyone directly and- indirectly connected with the oil business. It is, therefore, time that someone should offer an explanation for its presence and form a definite opinion based on all the data available in regard to the effect it will have on the future prospects of the area affected as probable oil- and gas-producing territory. At present there seems to be no consensus of opinion. To the writer&apos;s knowledge, only one attempt has been made to explain; by Erasmus Haworth, State Geologist of Kansas, in a paper entitled Bulletin, Number Two on Crystalline Rocks in Kansas. The purpose of the present paper is to offer a theory for the presence of the granite and to draw conclusions which will aid in determining the prospective oil and gas value of the area in question. In taking up this question it will be well to consider first the tests in which granite has been reported, with a general history of each. The accompanying map (Fig. 1) shows the location of all wells described. The first well in which granite was reported was that drilled just south of Zeandale in section 27, township 10 south, range 9 east, by a local company which had taken up a block of leases in that vicinity. At a depth of 958 ft. (291.99 m.) granite was encountered. Drilling was continued to a depth of 1,093 ft. (333 m.) in the same formation, at which depth the hole was abandoned. Another well was started 1 mile east of the first well and the same rock was found at a depth of 945 ft. (288 m.). Drilling was continued to a depth of 1,200 ft. (365.76 m.) with the bit in the sane formation. Samples of the drill cuttings have been examined and they are undoubtedly crushed granite. The next well in which granite was found was that drilled by DeLaat and Shepard, independent wildcat operators, in section 34, township 19 south,. range 7 east, near the town of Elmdale. Granite was struck at 1,707 ft. (520 m.) and the hole was abandoned in the same formation at 2,525 ft. (769 m.). Mr. DeLaat watched the drilling of this well very closely and he has described to me in some detail the formation immedi-

Jan 8, 1917

By J. B. Cohen, S. L. Sass

The nucleation process for y&apos;, Ni3Ti, is shou&apos;n to change from heterogeneous to uniform as the undercooling within the phase boundary increases. As unifornz nucleation beconres copious, (100) alignment is observed in the early stages of aging; howecer. whether or not the alignment is due to spinodal decomposition could not be determined. The presence oi a large-scale reversible segregation of titanium and not the intermediate precipitate y&apos; may be the cause of the initial strengthening in this alloy system and the discrete regions detected magnetically by Ben-Israel and Fine. Evidence is presented for the role of dislocations in the formation at long aging tines oJ the equilibrium precipitate . ThE nickel-rich portion of the Ni-Ti phase diagram consists of a terminal fcc solid solution of titanium in nickel called y.&apos; For temperatures below 1290°C if the solubility limit is exceeded and the temperature is high enough, the excess titanium will combine with nickel to form q, Ni3Ti, a four-layer hcp ordered structure with stacking sequence ABAC."~ Since a change in structure is involved, formation of q is slow and a metastable precipitate referred to as y&apos; forms. This metastable precipitate is an ordered cubic phase in the unconstrained state having a structure similar to Cu3Au (LIZ) with the composition Ni,Ti."&apos;5 From X-ray studies,8, 7 the following sequence is indicated for the precipitation reaction at low temperatures: 1) The appearance of satellites around low-index diffraction spots and splitting of high-index spots, indicating the formation of a slightly tetragonal phase in an imperfectly periodic arrangement. The tetragonal phase is y&apos; or the depleted matrix, depending on the volume fractions of matrix and precipitate (and hence, the alloy composition); tetragonality apparently arises from coherency strains. 2) The appearance of diffraction spots from the equilibrium second phase, q. Ben-Israel and Fine&apos;" used magnetic methods to measure the changes in matrix composition during aging, and to estimate the precipitate composition in a Ni-10.1 at. pct Ti alloy. They observed that the alloy, solution-treated at 1270°C and quenched, contained heterogeneities with discrete compositions which gradually vanished upon aging. It was suggested that y&apos; may initially form as a defect structure with several possible compositions deficient in titanium as compared to Ni3Ti; the composition Ni3Ti develops with prolonged aging. The initial composition was Ni6Ti which would require a very large deviation in stoichiometry for y&apos;. It was noted that at 700°C the precipitation reaction was 80 pct complete after 2 hr and that the volume fraction of second phase was 0.2 after 1 hr. Mihalisin and Decker&apos; suggested that the equilibrium precipitate, besides being nucleated at grain boundaries, could also form at stacking faults. ~errick" examined the formation of in Ni-Cr-Ti, and suggested that a collapsed vacancy cluster within y&apos; acted as a nucleus for intragranular q at high temperatures, 820" and 900°C. After long aging times at lower temperatures, 650" and 750°C, diffraction patterns taken from regions containing ribbons of stacking faults showed spots associated with q. Aging greatly enhances the mechanical properties of these alloys, even at high temperatures, and the metastable precipitate y&apos; is thought to be responsible.&apos; At 600°C the hardness of a Ni-10.1 at. pct Ti alloy increases rapidly during the first 20 hr of aging and continues to increase slowly thereafter.&apos;" At 700°C the hardness reaches a maximum at 1 to 2 hr and then decreases.l1 In this paper the kinetics of formation of y&apos; and the mechanism of transformation to in a Ni-Ti alloy are described. Evidence is presented that suggests that large-scale regions of titanium segregation are present initially and these may have an important influence on the initial strengthening of the alloy: these regions may be the heterogeneities detected by Ben-Israel and Fine. I) EXPERIMENTAL TECHNIQUES The Ni-10.3 at. pct Ti-0.6 at. pct A1 alloy was prepared by vacuum melting. Its chemical analysis is given in Table I. A 0.007-in.-thick strip was sandwiched between foils of the alloy and placed in an open Vycor tube with titanium chips (to get oxygen) and solution-treated for ; hr at 1150°C in a Globar Furnace under a flowing argon atmosphere. Following a quench into an ice-brine mixture at -5" to -2"C, a sample to be aged at temperatures up to and including 700°C was sealed in an evacuated Vycor capsule before being put into a fused salt bath. Aging above 700°C was carried out on bare samples in a salt bath. When removed from this bath and quenched into an ice-water mixture, the sample was normally coated with a thin layer of oxide easily removed with emery

Jan 1, 1970

By T. Cantwell, N. C. Rasmussen, H. E. Hawkes

Beryl is a mineral that may be difficult to distinguish from quartz by casual field inspection. The easily recognized green color and hexagonal crystal form of coarse-grained beryl are by no means universal, even in beryl from pegmatitic deposits. If it occurred as a fine-grained accessory mineral in an igneous rock, it would almost certainly escape detection unless samples were submitted for petrographic or chemical analysis. There may be substantial deposits of some beryllium mineral, other than beryl, that has been overlooked because that mineral also closely resembles the common rock-forming minerals. A reliable and simple method of identifying beryllium minerals and determining the beryllium content of a rock would be helpful in exploration. This article describes preliminary experiments in applying nuclear reaction to the qualitative identification of beryl and to the semiquantitative determination of the beryllium content of rock samples. Gaudin,1,2 the first to apply a nuclear reaction in detecting beryllium minerals, developed a method that irradiates the sample with gamma rays, which react with beryllium nuclei to produce neutrons. The neutrons are then measured with standard equipment. The cross section for this reaction is about 1 millibarn. The cross section is a measure of the probability that a reaction will take place, for example, between a beryllium nucleus and an incident gamma ray or alpha particles.3-5 At 1-millibarn cross section for the reaction, satisfactory performance required a source strength of the order of 1 curie (3.7 x 10"&apos; disintegrations per sec, where each disintegration releases one or more gamma rays). The reactions will not take place if the gamma radiation is below a minimum energy, in this case 1.63 mev. The size of the source and the energy of the radiation made heavy shielding necessary for these experiments, both to reduce the background count of the neutron counter and to safeguard personnel. The original discovery of the neutron by Chad-wick in 1932 resulted from experiments with another nuclear reaction, induced by bombarding beryllium with alpha particles in which the products are carbon-12 and neutrons. The equation for this reaction is as follows:&apos; " ,Be" + ,He&apos;? 6C12 + 8,n&apos; [1] re-particle neutron In the above nuclear equation (Eq. 1), the sub- script number indicates the number of protons in the nucleus (the atomic number) and the superscript the total number of neutrons and protons (approximately the atomic mass). For the alpha-neutron reaction the cross section is about 250 milli-barns, or 250 times that of the gamma-neutron reaction used by Gaudin. The positively charged alpha particle is repelled by the positive charge of the beryllium nucleus; it must, therefore, have a certain minimum energy in order to approach close enough to the beryllium nucleus to react. For reaction with the beryllium nucleus, the lower limit of the alpha-particle energy is 3.7 mev. The alpha-neutron reaction, with polonium-210 as an alpha source, was selected for the present experiments. Alpha particles are emitted by polonium-210 at 5.30 mev, which is adequate for the reaction with beryllium. Furthermore, this isotope of polonium emits alpha particles with negligible associated gamma radiation, thus eliminating the necessity of shielding. The half-life of polonium-210 is 138 days. Inasmuch as alpha particles carry a possible charge and are large compared with most nuclear particles, their energy is rapidly dissipated in passing through matter. Their range in standard air is 3.66 cm,3 and they penetrate only a few tens of microns into a mineral sample. The short range in air can be minimized by preparation of a flat sample surface that can be brought very close to the alpha source during analysis. On the other hand, short range of alpha particles in air lessens the radiological health hazard and makes it possible to use this method without shielding. It must be emphasized, however, that the alpha emitters are potentially very dangerous if they enter the human body. Polonium must be handled with extreme caution. The literature has reported experiments on the yield of neutrons from reaction of alpha particles with beryllium nuclei. Feld" reports that in intimate mixtures of polonium and beryllium, 3 x 106 eutrons per sec are produced per curie of polonium. Elsewhere in the same reference it is stated that a sandwich-type source yields about one third as many neutrons as an intimate mixture. A table of neutron yields for full energy polonium alpha-particles on thick targets as reported by Anderson7 is the basis of Table I. From Table I it can be deduced that the elements most likely to interfere, i.e., those that also produce neutrons when bombarded by alpha particles, are boron and fluorine. These data also show that it will probably not be possible to determine very small quantities of beryllium in rocks because of the masking effects of the major elements, sodium, magnesium, and aluminum. The neutrons emitted in the alpha reaction are detected by another nuclear reaction. Either of the

Jan 1, 1960

By B. J. Harlan

The trying times experienced by the steel industry during the past four years have emphasized the necessity of producing pig iron at the lowest possible cost. The trend in both design and operation of blast furnaces has been toward this end rather than toward securing maximum production from a unit or group of units. In the following discussion the trend in design of stacks and auxiliary equipment will be taken up before operation is considered. Although few furnaces have been constructed in the past few years, the trend is definitely toward larger furnaces with a hearth diameter of 24 or 25 ft. Such a furnace is very flexible, being able to produce efficiently any desired daily tonnage between 500 and-1000 or more. The detail of the design of furnace stacks, with the exception of the top, has changed little in recent years. To decrease the velocity of gas through the throat of the furnaces, thereby reducing flue-dust losses, the stock-line areas are constantly being made larger. The top dimensions of the larger furnaces are usually as follows: Stock-line diameter, 19 to 20 ft.; large bell diameter, 14 to 15 ft.; straight section of throat, 5 to 10 ft. high; inwall batter, 1 to 11/4 in. Pe ft. The ratio between the area of the stock line and the area of the large. bell is usually about 1.85 to 1. The stock-line diameter of some smaller furnaces has been increased to that of the hearth diameter of the stack at the expense of the stack batter. Remarkable decreases in flue-dust production are claimed for the so-called " Venturi top," which is achieved by flaring the stock line, in the form of an inverted cone, from a diameter of 17 ft. at 10 ft. below the large bell closed to a diameter of 19 ft. 6 in. at 3 ft. below the large bell closed. Time alone will tell which of the two designs is the better. Because of differences in raw materials, one top may be better for some plants and the other top for other plants. In the search for lower costs and higher efficiencies all operators are, adopting stoves that will maintain maximum hot-blast temperatures with a minimum gas consumption. To meet these requirements, stove capacity of approximately 7 sq. ft. of heating surface and 1.8 cu. ft. of brick volume is required per cubic foot of wind blown per minute.

Jan 1, 1934

By Shiro Ban-ya, John Chipman

Using the same experimental method previously described, the activity of sulfur in a number of quaternary and more complex liquid iron alloys at 1550oC is determined. A "cross-product term zj.zk is determined for each of the quaternary alloys to take account of the mutual effects of the combinalion on the indi-vidual contributions to In 5 The interactiotl coefjicienls delermined for ternary solutions and cross-pvoducl coefficierlts from the quaternary systems are used to estimate the activity coefficient of sulfur in more complex alloys. OUR recent papers 1,2 have described new determinations of the activity of sulfur in Fe-S binary and Fe-S-j ternary solutions, but the practical applications of these data require the estimation of activity of sulfur in more complex systems. Previously, Sherman and chipman3 devised an approximate method for calculating the activity of sulfur in complex systems by summing the contributions to the logarithm of the activity coefficient of each element in the alloy. This procedure is more successful, as one of us has pointed out,4 when the concentration variable is taken as zs = ns/(nFe — nS t CLJ~ nj) rather than the conventional atom fraction x~ = nS/(nF, + nS + Enj). In the former definition, which is based on analogy to interstitial solutions, the value assigned to uj is normally +1 for metallic and -1 for nonmetallic elements." In addition, however, the effects of mutual interaction between alloying elements must be considered for the accurate estimation of the activity of sulfur in more complex systems. The purpose of this investigation has been to devise a more reliable method for estimating the activity coefficient of sulfur in nmIticomponent iron alloys. The measurements were carried out on some quaternary systems Fe-S-j-k for combinations of silicon, chromium, nickel, cobalt, molybdenum, and tungsten. Manganese was not included since the experimental method has been found unsatisfactory for volatile, sulfide-forming elements. The experimental method was the same in every detail as described previously. 1,2 The concentrations of sulfur, silicon, chromium, and copper in the quenched metals were determined by chemical analysis but those of nickel, cobalt, molybdenum, and tungsten were calculated from charged amounts. Iron sulfide was included in the charges in amounts estimated to furnish approximately the final sulfur content. CALCULATION W2 have shown2 that when zs and zj are the concentration variables in a ternary Fe-S-j solution the logarithm of the activity coefficient S = a~/zg is a linear function of the variables as and aj defined as follows:

Jan 1, 1970

Asarco&apos;s Sacaton unit, located near Casa Grande 45 miles southeast of Phoenix, Arizona, was brought into production in February 1974. Ore reserves are estimated at about 48 million tons at 0. 95% copper. Mineralization of the orebody comprises both sulfides and oxides, with minor amounts of gold and silver. Preproduction stripping of 40 million tons of overburden was accomplished in less than two years. Mining is done at the rate of 9,000 stpd ore with a waste-to-ore ratio of 4.6 to 1. 0. The mine is developed on 40 ft benches, and by 1979 underground block caving methods will be phased into the operation at a depth of 1900 ft. Ore is mined in the pit two shifts per day, seven days per week, and is hauled with 85 ton trucks to the primary crushing plant. Trucks dump their loads into a 165 st capacity pocket equipped with a chain curtain which controls the ore flow to the 6 ft 6 in. wide by 24 ft long (2. 0 m by 7.3 m) vibrating feeder grizzly. Grizzly bars are inclined at a 5º slope on the first half of the 0 feeder and 10 on the last half. Grizzly bars have 6 in. (13 mm) spacings which pass 60 to 70% of the mine-run ore. Grizzly oversize drops into a 48 in. by 60 in. (1. 22 m by 1.52 m) primary jaw crusher. Both the grizzly undersize and crusher discharge are collected on a 42 in. (1.07 m) conveyor belt operating 398 fpm (121 mpm) for transport to the 4,750 live st intermediate storage area ahead of the fine crushing plant. Capacity of the Sacaton primary crushing plant is a nominal 1150 stph (1043 mtph). It operates fourteen shifts per week with an effective crushing time of four hours per shift. An economical open-air design was used, but an enclosed operator control room is located on the upper level where the dump truck, feeder, and crusher can be observed. Oversize rocks are removed from the feeder or crusher by the 10-ton bridge crane. Direct operating costs for this well-designed primary crushing plant, including labor, power, supplies, and maintenance, are only 3.5 cents per short ton. An interesting feature of the Sacaton orebody is that the non-sulfide copper minerals, which are less prevalent than the sulfides, occur intimately with the sulfide minerals; for this reason, all ores as mined are treated in a flotation circuit using sulfidizing methods for oxide recovery.

Jan 1, 1978

By A. Boltax

The effect of cold work on the electrical and magnetic properties of solution-treated and aged Cu-Fe alloys was studied. The electrical resistivity of solution-treated and of aged Cu-1.7 wt pct Fe samples increased by up to 25 and 140 pct, respectively, follozcing a 55 pct reduction of area. The principle contributions to the increase of resistivity of the solution-treated and aged samfiles are examined. Measurements of the .saturation induction, coercive force, and stacking fault Probability are also reported. 1 HIS paper is the second in a series which examine the behavior of the electrical and magnetic prop- erties of Cu-Fe alloys. The first paper1 was primarily concerned with the effects of thermal treatment whereas the present paper examines the effects of cold work on solution-treated and aged Cu-Fe alloys. The effects of cold work on the transformation of the coherent fcc iron precipitate to the ferromagnetic form2 and the coercive force and remanence3 have already been described, but the unusually large increases in resistivity (up to 220 pct) which occlir with cold work have not been reported previously. EXPERIMENTAL METHOD The methods used for alloy preparation, heat treatment, and electrical and magnetic measurements are described elsewhere.1 The specimens, initially 4-in. lengths of 0.0625-in. diam wire, were cold worked by swaging in hardened steel dies. Following each reduction, the samples were etched lightly in hydrochloric acid to remove surface con-

Jan 1, 1962

By D. Mills, G. B. Craig

ZIRCONIUM has been float-zone-refined in an electron-beam furnace and the redistribution of oxygen, iron, and tungsten has been measured. The iodide zirconium used in the present experiments initially contained both oxygen and iron in the range 100 to 200 ppm by weight, and tungsten in amounts less than 10 ppm. Float-zone refining of zirconium, using induction heating, has previously been attempted by Kneip and Betterton1 and Langeron.2 Kneip and Betterton were primarily interested in the removal of iron and nickel. They achieved some purification, with respect to both these elements, in material given up to six passes at 150 mm per hr under an argon atmosphere. Langeron reported purification for a large number of elements after four completed passes in a static vacuum system operating at pressures less than 10-6 mm of Hg and with rates of zone travel between 30 and 40 mm per hr. He did not report oxygen concentrations, but stated that there was inverse segregation of this element. westlake5 has also used a minimum of four zone passes to remove iron from zirconium. No rates or conditions were given. Belk6 has shown that tungsten contamination can occur during electron-beam melting. He reported an increase from 0.01 to 0.05 pct by weight tungsten in molybdenum after four complete zone passes. The vacuum system for the electron-beam unit used in the present investigation consisted of a single-stage rotary pump backing a liquid-air-trapped oil-diffusion pump. A pressure of less than 10-8 mm of Hg was obtained with Dow-Corning 705 fluid in the diffusion pump. In order to avoid contamination of the zirconium by evaporation from the tungsten filament, a special focusing cage4 was employed. Three rates of zone travel, 114, 38, and 4 mm per hr, were investigated, with the liquid zone moving from the bottom to the top of the bar. The bars used were 3 mm diam and the total melted length was 130 mm. Oxygen was analyzed by neutron-activation analysis using a neutron flux of 10&apos; neutrons per sq cm per sec to form the isotope N16 by the 016 (n,p) N16 reaction. The standard deviation is quoted for each oxygen determination. The iron and tungsten analyses were performed spectrographically, and the precision is estimated to be ±6 pct. Analyses for tungsten were all below the detectable limit of 10 ppm, confirming the protection given by the focusing cage. No significant redistribution of oxygen was found at the two higher rates of zone travel. The redistribution of oxygen and iron obtained after five passes at a rate of zone travel of 4 mm per hr (1.1 x 10-4 cm per sec) is recorded in Tables I and 11. Burris, Stockman, and Dillon3 have estimated the distribution of solutes during multipass zone refining. Using their curves for an effective distribution coefficient of Keff = 1.5 and 2 for oxygen and Keff = 0.3 for iron, the expected concentrations were estimated for the present material. These are shown in Tables I and 11, along with the experimentally measured values. The calculated concentrations are based on a molten-zone length of 10 pct of the total melted length, whereas in the present experiments the molten zone was approximately 5 pct of the total melted length. The effect of zone length on solute redistribution is most pronounced after a large number of zone passes. Comparison with Pfann&apos;s published data8 for solute redistribution for various Keff&apos;s and zone lengths indicates only small differences at low numbers of completed zone passes. It is evident that the expected distribution has not been realized in the case of iron. Scrapings of material deposited on the inner surfaces of the electron-focusing cage were found to be magnetic. It is, therefore, concluded that redistribution of iron is masked by evaporation. Deposition of iron inside the focusing cage was observed at all rates of zone travel. The results of the investigation may be summarized as follows: 1) Segregation of oxygen is typical for a solute with a distribution coefficient, Keff > 1. 2) No redistribution of oxygen takes place at high rates of zone travel. 3) The distribution coefficient for oxygen lies between 1.5 and 2.0. 4) Purification with respect to iron occurs mainly by evaporation. 5) The focusing cage is effective in preventing tungsten contamination.

Jan 1, 1967

By Chester T. Sims

RECENTLY, a new type of superalloy material called TD Nickel* has been marketed.&apos; It is a sim- ple, two-phased alloy, consisting of thoria particles dispersed in nickel of rather high purity (Ni-2 pct Thoz). Its mechanical properties appear relatively superior to previous experimental material attempting to use the oxide nonmetallic dispersion concept (except SAP), and superior to conventional nickel-base alloys at high homologous temperatures. This is derived from an interesting method of creating the dispersion, arising during chemical processing of the nickel and thorium salts in solution while reducing the nickel to metal. An evaluation of the thoria phase was conducted at this laboratory. Material and Procedure. TD Nickel was made available, consisting of several inches of 0.470-in. rod, extruded at a ratio of 64: 1, straightened, and centerless ground. Property determinations on this rod by the supplier at 1800°F showed an ultimate tensile strength of 11,400 psi, yield strength of 9600 psi, and 6 pct elongation. Specimens were removed from the rod for as-extruded metallography, and two 1/2-in. lengths supported on high-purity Al2O9 bricks were placed in a laboratory muffle furnace for exposure at 2000° F. The furnace door was left cracked to allow a slight amount of circulation. One specimen was removed at 200 hr for examination; the other was left for 2000 hr. Metallography. The micro structures obtained for the three conditions of exposure are shown in Fig. 1. Elongation of the grain structure in the extrusion direction is readily evident. The grains appear to be up to 0.001 in. (0.003 cm) long, with a length/width ratio of about 10: 1. Allowing for modest local in-homogeneities in structure, no significant change in thoria particle size or nickel alloy grain size occurred during the 2000°F exposure. However, etching depth varies slightly from one specimen to another, changing the number of particles visible. The thoria dispersion appears to be in the order of 0.01 (min) to 0.5 (max) p diam. The minimum diameter is difficult to estimate at X10,000, and may be less. Interparticle spacing appears to be about 0.1 p. Etching effects can be seen, depending upon grain orientation. A cubic etch-pit pattern appears in certain grains, apparently when etching is started by an anodic particle of thoria, Fig. l(c). The cubic pattern appears related to crystallographic orientation, and is prominent when the [ l00 ] direction is perpendicular to the plane of polish. The grains which present a ridged appearance in the photograph appear to be oriented with the [110} direction perpendicular to the plane of polish. Analysis. The thoria particle size was measured by a line intercept method perpendicular to the extrusion direction. Only particle sizes measuring 0.001 in. at X10,000 or larger could be extimated. Within limits of experimental error, particle size distribution appears to be unaffected by exposure, Fig. 2. To check structural stability further, a grain-growth evaluation was made. The number of grain-boundary intersections was counted at X500 on each of several traces normal to the extrusion direction for each condition. It can be seen from Table I that grain diameter appears unchanged by the 2000°F exposure. The slightly finer grain diameter after 200 hr may be attributed to variations in grain size from area to area in the original extrusion. From the present rather limited study of Ni-2 Th on, it appears that: 1) for time-temperature exposure up to 2000 hr at 2000°F (Larsen-Miller parameter = 57, homologous temperature = 0.8) thoria particles of the size studied are highly thermally stable; they do not significantly react, agglomerate, or diffuse; and

Jan 1, 1963

By A. J. Griest, A. P. Young, P. D. Frost

A study was made of the effect of ß grain size on the tensile ductility of a-ß titanium alloys haet treated to strengths in the range 165,000 to 180,000 psi. It was concluded that the primary cause of $ embrittlement is the large grain size which is obtained so rapidly in many a-ß titanium alloys when heated into the ß field. It was also found that grain-boundary a and acicular intragranular a in the microstructure are not necessarily detrimental to the tensile ductility if the prior ß grain size is sufficientlv fine. BETA embrittlement occurs in a-ß alloys when the finish hot-working or stages of the subsequent heat treatment have been done at temperatures in the ß field. In order to avoid this embrittlement, for-gings must be finished at temperatures under the ß transus. For better workability, it would be desirable to forge at temperatures in the ß field. For this reason, research has been conducted to determine the cause of ß embrittlement. Although ß grain size has been considered as a possible contributing factor to ß embrittlement, only limited research has been done to evaluate its effect. The effect of addition elements on ß grain growth in unalloyed titanium has been studied by Liu.&apos; Complete mechanical property data, however, were not obtained for correlation with grain size. Ogden and coworkers2 have investigated the effect of both a and ß grain size and grain shape in Ti-Cr-Mo alloys. Their data indicated that tensile ductility was relatively insensitive to ß grain size at annealed strength levels (140,000 psi ultimate). No study has apparently been made to determine the relationship between ß grain size and ß embrittlement in a-ß alloys heat treated to high strength (180,000 psi ultimate). The high-strength condition is that in which ß embrittlement is particularly severe. Beta grain size is not easily varied through the use of a range of annealing times and temperatures in the ß field, because of the rapidity with which ß grain growth occurs. Short-time heating techniques are needed to obtain the smallest ß grains. EXPERIMENTAL PROCEDURE In this research, the experimental procedure was as follows: 1) Tensile and microimpact specimen blanks were resistance heated to produce a range of ß grain sizes. 2) The tensile and microimpact blanks were then solution-treated in the a-ß field and aged to produce predetermined ultimate tensile strengths in the range 165,000 to 180,000 psi. Tensile and impact ductility were then correlated with a grain size for constant strength levels. Materials—The alloys Ti-6A1-4V, Ti-4A1-4Mn, and Ti-16V-2.5Al are representative of the heat-treatable a-ß types in which ß embrittlement can be severe. The compositions and ß transi of the heats studied are given in Table I. The Ti-16V-2.5Al heat was melted and fabricated to 1/4 in. round at Battelle; the other alloys were obtained as 1/4 in. round rolled from commercial heats. The micro-structures of the as-rolled alloys were fine a-ß mixtures. This structure is typical of titanium alloys hot-worked extensively in the a-ß field. Resistance-Heating Treatments to Establish ß Grain Size—For direit resistance heating, a 1/4-in.-diam s~ecimen was heated with a 3000-watt transformer rated for 1000 amp with adjustable secondary voltage. The apparatus included a spray quench fixture. Both heating and quenching periods could be automatically controlled. For temperature measurements, 28-gage Chromel-Alumel wires were tack-welded to the specimen at its midpoint. A high-speed recorder-controller was used to control the heating cycle.

Jan 1, 1960

By W. Mitchell, B. H. Bergstorm, C. L. Sollenberger

A unique compression testing machine was constructed to load individual 1/8 to I-in. spheres of glass, etc., at rates from 100 to 100,000 lb per min. During loading the applied load was continuously plotted us the deformation of the sphere-platen system. The load-deformation curve conforms to the theory of elasticity. The spheres were surrounded by steel retaining rings or by gelatin (to prevent secondary fracture). The product size modulus was determined from screen analyses. The data shows: 1) Energy input per unit mass is inversely proportional to the product size modulus (or directly proportional to the surface area per unit mass). 2) Increased loading rates slightly increase the energy input per unit mass required for fracture without affecting the preceding relationship. Theory and experiments show that much of the input strain energy is transformed into kinetic energy of fragments at fracture, this being a reason efficiencies based on "surface energies" are exceedingly small. This large kinetic energy component is usually dissipated as heat but may be partially reclaimed because impact of fragments against the surface of steel retaining rings causes additional comminution. There are currently several theories of crushing, all of which can be derived from the general energy equation of Gillilandl as was pointed out by Mitchellet al in 1954&apos;and more recently by Rose and Sullivan. If the exponent of the equation dE-x-"dx is assigned values of 2,1, or 3/2, one obtains by intergration between suitable limits, the equations of Rittinger, kick,&apos; and Bond,&apos; respectively. Other investigators prefer to let the exponent be a variable parameter. To help resolve the controversy, the Allis-Chal-mers Research Laboratories set up a series of carefully controlled experiments in which the level of energy input required to induce the comminution of a single particle by slow compression loading was very accurately measured. The energy input requirement, in conjunction with the size analysis of the fragments produced at fracture, yielded an accurate energy-product size relationship for the conditions studied. APPARATUS The experimental apparatus was designed to apply a compressive load on opposite sides of an "ideal particle." Spherical shapes were chosen, because point contact loading is typical of the mechanics of conventional crushers. The bulk of the experimental data was obtained with glass spheres because glass is a fairly homogeneous, brittle material for which the properties follow definite statistical distributions. The spheres ranged from 1/8 to 1-in. diam. The compressive load was applied to the specimen at a uniform rate by a loading mechanism (Fig. 1) which acted through a system of levers. The uniform rates, ranging from 100 to 100,000 lb per min, were obtained by metering water into a bucket suspended at the end of the secondary level. Point contact was made with the sphere through tungsten-carbide platens. This latter material is extremely hard and has a high modulus of elasticity, thereby having a minimum of distortion when loaded. The actual load on the sphere was measured independently of the lever system by a load cell, Fig. 2, which was designed so that the voltage output of the load cell would be proportional to load. The deformation of the specimen was indirectly measured by a pair of transformers which were attached to opposite edges of the upper platen. The cores of the transformers, which were attached to the lower platen, moved relative to the transformer so that the voltage output was proportional to the deformation of the sphere-platen system. The load was plotted against the deformation on an X-Y recorder. The area under the curve, as shown on Fig. 3, was proportional to the energy input of the

Jan 1, 1961

By G. A. Chadwick, D. Jaffrey

The morpho1ogies and orientation relationships of the phases in the Sn-Zn and A1-A13Ni eutectic systems were examined by electron microscopy and X-ray diffraction techniques. In each alloy the "transition" from the lamellar to the fibrous morphology was found to be one of scale, not of type. The minor phase in both systems exhibited certain well developed facets which were not affected by changes in the ingot solidification rate. The crystallographic relationships displayed by the pairs of phases in both systems were also insensitive to the growth rate. In the Sn-Zn alloy, the unique relationship of: growth direction - II [1201 Sn - II [01101 Zn and ribbon interface plane 11 (101) Sn 11 (7012) Zn was determined. The Al-Al3Ni alloy phases did not possess any particular orientation relationship, though the Al3Ni phase invariably grew in the [010] direction and exhibited the same set of facet planes. These results are discussed in relation to current eutectic growth theories and explanations of the "lamellar to fibrous transition". THE lamellar to fibrous transition that occurs in many eutectic alloys has been the subject of considerable speculation and experimental study. In some alloys it can be induced solely by an increase in the solidification rate,&apos;-3 whereas in others the transition supposedly occurs only if the lamellae are forced to grow out of the overall ingot growth direction.4-6 he cause of this latter type of transition has been attributed to deviations of the lamellae from their low energy habit planes;4&apos;5&apos;7 fibers are produced because the sustaining force for lamellar growth (a low energy boundary) is destroyed. Implicit in these explanations is the assumption that fibers are circular in cross-section and completely lacking in low energy inter-phase interfaces. The "natural" growth rate dependent transition has been studied less thoroughly although Tiller8 has attempted a theoretical explanation of it. Tiller&apos;s arguments are not completely satisfactory9 but his suggestion that the relative undercoolings of the solid/liquid interface for lamellar and fibrous morphologies are growth rate dependent cannot be totally discounted; it is possible, for instance, that the relative interfacial undercoolings could alter and produce the observed morphology change if the orientation relationships between the phases and the associated interphase bound- ary energies were sensitive to growth rate. Salkind et al." have reported finding a change in the orientation relationships in the A1-A13Ni system accompanying the lamellar to fibrous transition, but contradictory evidence has also been reported for this3&apos;" and another system,12 so the position remains unclear. In an attempt to clarify matters a study was made of the "lamellar to fibrous" transition in the Sn-Zn and A1-A13Ni eutectic systems; the morphologies of these two selected systems are quite similar when viewed by optical microscopy. In the present research the morphologies and morphology changes were investigated by electron microscopy. The orientation relationships existing between the eutectic phases were also determined for both morphologies in both eutectic systems. EXPERIMENTAL PROCEDURE The materials and method of alloy preparation and ingot solidification for the Sn-Zn system have been reported previously.2 In this investigation nine horizontally grown ingots of the highest purity (99.9997 pct) were used. The temperature gradient in the melt was not intentionally varied and was approximately 10°C per cm. Seven growth rates between 1.3 cm per hr and 20 cm per hr were imposed. The A1-A13Ni alloys were prepared from "Spec. Pure" nickel and 99.995 pct aluminum by melting the components in an open alumina crucible and casting the melt into the cold graphite mold. Six ingots of the Al-Al3Ni alloy were unidirectionally solidified at growth rates from 1 cm per hr to 12 cm per hr under high purity argon. A typical ingot was 20 cm long, 1 cm wide, and 0.75 cm to 1.5 cm thick. Samples taken from the bars at positions 12 cm from the nucleation end were examined by conventional orthogonal-section metallo-graphic techniques. When required, samples were mounted for X-ray diffraction analysis using the Laue back-reflection technique with a finely focussed X-ray source. The surfaces of the A1-A13Ni specimens were prepared by mechanically polishing them down to the 1 µ diamond pad stage followed by an electropolish in 80/20 methanol/perchloric acid solution at 0°C and 20 to 30 v. The Sn-Zn specimens were repeatedly polished on an alumina pad and etched in hot dilute (2 pct) nitric acid until the diffraction spots were found to be sharp. Thin films of the alloys were prepared for observation in an electron microscope by spark machining thin discs (0.03 to 0.04 in. thick) from longitudinal and lateral sections of the bars and elec-trolytically thinning them via a jet polishing technique. For the A1-A13Ni eutectic alloy, an 80/20 mixture of ethanol/perchloric acid at 40 v and 20°C was found to be satisfactory. A solution of 70/20/10 methanol/perchloric acid/butylcellosolve at 25 v and 20°C was used on the Sn-Zn alloy. For the former alloy the jet nozzles (cathodes) and the disc clamps were of aluminum;

Jan 1, 1970