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The Midvale Plant of the United States Smelting, Refining and Mining Company, situated twelve miles south of Salt Lake City, consists of mills for concentrating lead-zinc ores and a custom lead smelter. The milling department includes a 475-ton gravity mill for ores from the United States Mines at Bingham, a 100-ton Huff electrostatic zinc plant and a 60-ton pilot flotation mill for differential separation of lead and zinc. The gravity mill and electro- static plant are being replaced by a 600-ton differential flotation plant, now under construction, for differential separation of lead, zinc and iron. This new mill will have capacity for treating custom ores in addition to ores from the company's mines at Bingham.

Jan 1, 1925

By Yoichi Ishida, Ching-Yao Cheng, John E. Dorn

Tile creep behavior of a iron was investigated over the range of temperatures from 375° to 1150°K. Apparent activation energies for creep, obtained by the effect of sudden changes in temperature on the creep rate, revealed the presence of- four distinguishable regions. The creep behavior of a iron in Regions II (480° to 774°K) and 111 (775° to 1045°K) was found to correlate well with a model where the creep rate is controlled by the nonconsevualive motion. of jogged screw dislocations. An anomalous increase in the apparent activation energy fur creep in Region III was found to be in harmony with the known decrease in the free activation energy for self-diffusion over the Curie transformation range. Furthermore, the creep rates in Regions II and III were found to increase with stress due not only to the effect of stress on the activation energy but also to an increase in density of mobile dislocations. The evidence suggests that pipe diffusion along moving dislocations could be a significant factor over the lower temperatures of Region II. ALTHOUGH the creep properties of iron and steel have been of interest to metallurgists for some time and an extensive literature is now available, most of the published information has not produced much toward understanding the fundamental dislocation processes controlling the creep behavior of these materials. Whereas the activation energy for high-temperature creep of metals usually agrees well with that for self-diffusion, Sherby, Orr, and Dorn1 deduced from the data of Tapsell -and c1enshaw2 that the activation energy for creep of Armco iron is about 78,000 cal per mole and more recently Lytton and sherby3 reviewed the data of Jenkins and Mellor4 and found an activation energy for creep of a iron of 80,000 cal per mole. Both values are substantially greater than the activation energy for self-diffusion in a iron. Because of the limited data suitable for purposes of identifying the controlling dislocation mechanisms of creep and the unusually high activation energies for creep quoted above, it was considered desirable to reinvestigate in detail the creep of a iron by more reliable techniques which would provide sufficient data for determination of the creep mechanisms. EXPERIMENTAL TECHNIQUE Creep specimens were prepared from 3/8 by 4 in. iron bar stock of the following composition by weight percent: 0.001 C, 0.0120 0, 0.001 N, 0.004 S, and 0.003 P. The as-received bars were cold-rolled to a thickness of 0.100 in., annealed under argon for 30 min at 1113°K, cold-rolled to a final thickness of 0.063 in., and machined into tensile specimens having gage section 0.250 in. wide and 1.70 in. long. Finally they were recrystallized under argon at 1113°K. Specimens to be crept above 1060°K were recrystallized at 1173°K. Both recrystallization treatments gave the same reproducible equiaxed ASTM No. 4 grain size. Creep testing was conducted in machines fitted with Andrade-Chalmers arms that maintained a constant stress to within ±0.2 pct of the reported values. Deformation over the specimen gage section was sensed with a linear differential transformer and recorded auto-graphically as a function of time. The strains deduced from these measurements were sensitive to ±5 x 10-5. During creep the specimens were contained in an argon-filled chamber which was immersed in a temperature-controlled molten tin bath. Creep temperatures, as measured by thermocouples attached to the specimen, were maintained to within ±10.25°K of the reported values. For activation-energy determinations rapid changes in temperature of about 12°K were obtained within 30 sec by direct resistance heating of the creep specimen, and maintained to ±1°K of the reported values. Observations of structural details of specimens before and after creep tests were made by electrolytic polishing and etching in acqueous ammonium persulfate. EXPERIMENTAL RESULTS A typical example of the determination of apparent activation energies, Q, by the effect of small changes in temperature is illustrated in Fig. 1. Q is defined by

Jan 1, 1967

By F. E. Rizzo, L. R. Bidwell, D. F. Frank

THE poor high-temperature oxidation resistance of the refractory metals becomes an important problem as higher operating temperatures are sought. A meaningful analysis of their oxidation behavior requires a knowledge of the phases that can appear during oxidation as well as their relative stability. Although several extensive investigations have been carried out to obtain this information for the W-0 system,1-10 serious inconsistencies still remain. First, the standard free energies of formation (AG°) determined in recent studies which used the solid electrolyte galvanic cell technique6,7,9 differ significantly from those obtained primarily from gas equilibration measurements.1,3,4,10 The disagreement is especially large for the highest oxides. These data have been used to predict the decomposition temperatures of WO2. 72 and WO2.90.1 A considerable extrapolation is required, resulting in a large uncertainty in the decomposition temperatures. Second, Bousquet and perachon3 have presented convincing evidence, ob- tained by gas equilibration measurements, in support of the long-contested existence of W30. Phillips and chang,ll on the other hand, were not able to observe this phase under similar experimental conditions. The purposes of this work, which is part of a continuing investigation of the W-Mo system, were to resolve the discrepancies between the AGO measured by gas equilibration and solid electrolyte galvanic cell techniques, to extend the latter measurements to lower temperatures, to redetermine the WO2.72 and WO2.90 decomposition temperatures, and to apply the more sensitive electromotive-force method to the question of the existence of W3O. I) EXPERIMENTAL PROCEDURE The measurement of ?G° of reaction by the use of calcia-stabilized zirconia solid electrolyte galvanic cells has been described previously.12 The method is based on the measurement of the difference in chemical potential of oxygen between an electrode containing the two oxides of interest and a reference electrode of known oxygen activity. Two different types of cell holders were used in this study. The first type of apparatus has been described earlier." It consisted of two solid electrodes separated by a disc of electrolyte. Both electrodes were exposed to the same stream of purified helium. With this design a gaseous transport of oxygen between the two electrodes is possible. The second type of apparatus, which has also been described earlier,14 effectively separated the two electrode atmospheres. It utilized a closed-end impervious, calcia-stabilized zirconia tube that was open to the atmosphere. The tube served as an electrolyte for the cell and provided a means for separating the anode compartment, which was held under a static vacuum, from an air reference cathode. The cells and reactions of interest are described in Table I. High-purity tungsten metal was obtained from the Fansteel Metallurgical Corp. and the Allied Chemical Corp. Table II contains an analysis of each material. WO3 was prepared by oxidizing the metal in air at approximately 600°C in high-purity recrystallized alumina boats and by the dehydration of reagent-grade tungstic acid in alundum boats. The two methods of preparing WO3 resulted in slightly different purities.

Jan 1, 1968

By Earl S. Bardwell

The determination of suitable and safe annealing temperatures is one of the most important problems arising in the operation of a copper rolling mill. Certain of the larger mills have worked this problem out for themselves and in these mills the operation has become more or less standardized. In some of the mills pyrometers are used to measure the temperature of the annealing furnaces and careful watch is kept to see that overheating does not take place. In a considerable number of the mills, however, dependence is placed entirely on the judgment of the operator. The almost total lack of literature bearing on this subject seems sufficient warrant for the publication of this paper. ' The discussion of this subject naturally divides itself into two parts: (1) The effect of annealing temperature on physical properties; and (2) changes in the microstructure of refined copper due to cold rolling and annealing. I. The Effect of Annealing Temperature on Physical Properties For the purpose of investigating this phase of the subject six test bars were selected, varying in oxygen content between the limits of 0.036 and 0.070 per cent. The chemical composition of each of these test bars was as follows: Bar Number 1 2 3 4 5 6 Copper + silver...... 99.95 99.92 99.945 99.94 99.95 99.93 Oxygen.............. 0.041 0.070 0.046 0.050 0.036 0.058 As + Sb............. 0.0038 0.0038 0.0038 0.0038 0.0031 0.0031 The bars were heated in an electric muffle to about 1,650" F. and rolled into rods. The rods were annealed, pickled, and drawn to No. 12 B. & S. gauge wire. The wire which was to be used for the annealing test was cut into 38-in. lengths and each length made into a coil 6 in. in diameter. The separate coils were marked so that they might readily be identified

Jan 1, 1915

By Alexander Gakner

Since the end of World War II the Soviet Union has made great strides toward economic development of the country. Today it is firmly established as the world's second largest industrial power after the United States and it has committed itself before the people on both sides of the Iron Curtain to catch up with and to overtake us within a few decades. No nation could achieve such a degree of industrialization or aspire to become the world's industrial leader without a large supply of many basic mineral raw materials or at least easy access to such resources. In addition, it requires technical competence, a large skilled labor force, and a high rate of capital investment. Why should we concern ourselves with these Soviet aspirations? The Free World's yardstick of measuring a nation's well-being is the standard of living of the people in that country. Presumably even Communist governments are committed to some, however gradual, improvement in the standard of living of their people. The population of the USSR is 20 pct greater than that of the United States. Hence, if they ever achieve a standard of living equal to ours, they must by all logic reach a greater overall industrial output. However, in the U.S.S.R. the standard of living of the masses has not kept pace with the expanding industrial production and is still far behind that of the United States. Our concern, therefore, is with what the USSR intends to accomplish with its expanding industrial power: Will they produce large mineral raw-material surpluses and manufacture products to compete with us for world markets and attempt to put us out of business if not use it directly to wage war; or will they use their resources merely to produce more consumer goods for the Soviet people; or will they, along with other Communist nations in the not-too-distant future, compete with us for the world's sources of mineral raw-materials to maintain a high level of mass consumption?

Jan 6, 1960

By Gealy W. Wallwork

INTRODUCTION The administrative processes of coal mines are becoming increasingly complex. As society evolves into a more complicated structure with greater emphasis on individuality, government regulations reach deeply into every activity in an effort to force individuals into a standardized mold. These contradictory pressures add an extra burden to the administration of a mining operation. Recent years have brought a substantial change in the skills needed by mine supervisors and managers. As a result, a better understanding of the administrative functions is necessary. The mine superintendent has the overall responsibility for the mine; for effective operation he must be sufficiently knowledgeable to oversee all the complex functions that make up the mine. This chapter does not cover all the administrative requirements because of the variation in mine operation and in company policies and organizational structure. It does attempt to identify the administrative functions that would be required at a large mine with a preparation plant. It is assumed that the mine operation is decentralized with very little duplication of functions at the organizational levels above the mine. Thus each function is assumed to be relatively complete at the mine and under the general supervision of the mine superintendent. EMPLOYMENT PROCEDURES Throughout the mining industry, in deep or surface mining, in union or nonunion companies, the success or failure of an organization is directly related to the caliber of employees who make up the organization. A company is nothing more than a group of people working together with

Jan 1, 1981

By Alfonso W. Ovalle

INTRODUCTION The block-caving mining method is one of the most economical ways existing today to extract ore from nature. It is undoubtedly the least costly of the underground systems and moreover it compares favorably to open-pit mining. In addition to its low cost characteristic, the block-caving mining method permits a great extraction volume as can be exemplified by El Teniente's output capacity of over 22 million tons of ore per year. These characteristics of block-caving give assurance that, even though it is a very old mining system, it will be a good answer to the many future large massive low ore grade deposits to come and a1 so to rep1 ace open-pi t mining as such operations get deeper with higher stripping ratios. These are the reasons that induce further study of block-caving. In this paper block-caving at El Teniente is analyzed with due consideration to the major problems that this mine will encounter. Emphasis is given to the factors influencing the mining of soft ore which accounts for most of the ore to be extracted in the next ten years. A separate paper is devoted to a major modification introduced to block-caving hard primary ore at El Teniente by means of LHD equipment extraction. DESCRIPTION OF THE PRESENT MINING Ore Production and Flow Over 62.000 tons per day of ore are extracted 359 days per year at the El Teniente Mine. The Teniente 8 train haulage level at 1.983 m takes 29.000 tons daily to the Col6n Concentrator. Two trains make the 8 km haul with 16 cars per train. Car capacity is 90 tons. The Teniente 5 train haulage level 298 m above takes 33.000 t per day to the old Sewell Concentrator. Ore is produced from three production areas in two different levels. The so called North Mine produces 42.000 tons daily from the Teniente 4 level 65 m above the Teniente 5 haulage level. The Central Mine produces 1.000 tons from the first hard rock block caved at the Te- niente 4 level. The combined 43.000 tons per day production is sent through inclined 2 m dia- meter raises to the Teniente 5 haul age level , where 33.000 tons are taken 2.5 km to the Sewell Concentrator and 9.000 tons are hauled 0.5 km to a 5 m diameter vertical ore pass which sends ore to Teniente 8. The haulage is by 7 trains, 15 gabble-bottom cars per train. Car capacity is 20 tons. The so called South Mine produces 19.000 tons per day from the Teniente 1 level 645 m above the Teniente 8 haulage level. Ore is transferred by 2 m diameter inclined raises to the Ten 1 Retram level 22 m below, where 5 trains with 20 Sandfor Day cars per train, 8 tons capacity per car, haul the ore 1.5 km to two vertical 5 m diameter ore passes which connect to Ten 8. Starting in 1982 the Central Mine will in- crease production to 6.000 tons per day. An in- dependent loop haulage system will start operat- ing at the Teniente 5 level to feed a new under- ground 1.372 mm (54 in.) gyratory crusher which will send minus 152 mm ore (9 in.) to Teniente 8. In two or three years time the North Mine will only feed the 33.000 tons to the Sewel 1 Concentrator with its old Teniente 5 haulage system. The Col6n Concentrator will be fed from the Central and South Mines. Figure 1 shows the transfer systems and ore flows. The Ore Body In plan view at the Teniente 4 level the ore body has a kidney shape 1.800 m long and between 400 to 700 m wide. The north-eastern section of the ore body was washed away by the Teniente River. At the Sub 5 Level, 125 m below Teniente 4, the mineralization completely surrounds the circular 1.000 m diameter steep-sided barren breccia pipe (Braden pipe) . The ore body rock is 73% andesite, 14% diori te, 13% dacite and 6% mineralized breccia. Most of this ore is secondary enrichment sulfides which apart from the dacite is strongly fractured being chal cocite, cove1ine , bornite and

Jan 1, 1981

By W. A. Eardley

FIFTEEN years ago the world's deepest oil well penetrated the earth about 7300 ft. That depth has now been more than doubled. Why has such deep drilling become necessary and how has it become possible? Three factors have had an important bearing: (1) Depletion of shallow zones, making it necessary to search for deeper producing measures. (2) The perfection of prospecting methods, which have been success- fully used to locate favorable buried structures, many at great depth. (3) Improvement in the quality of steels used for drilling.

Jan 1, 1940

By Joseph Mac Donald

Stripped of its romantic possibilities, mining is a commercial business, carried on for the profit there is in it; and the business of the manager, in its ultimate analysis, is to make the profit as large as possible. The general manager of a mining company should keep himself personally familiar with all the details of its operations. If he fails to do so, chaos results, labor becomes inefficient, costs go up, and profits go down. Nowhere is this emphasized more than in Mexico. If the mining operations are extensive and complex, involving, besides the work of mining the ore, its transportation and treatment by various milling operations, and the marketing of the products, the business, to be carried on properly, must be

Jan 1, 1909

WILLIAM H. KOBBÉ (communication to the Secretary*).-I have read with much interest the discussion of my paper by Arthur Knapp and I. N. Knapp published in the March Bulletin. These discussions apparently assume that my paper advances a. number of ideas that are not intended: 1. That the total sandbody or pay is to be removed. 2. That upon bringing this sand and oil to the surface 100 per cent., or perfect separation, can take place. 3. That this tremendous quantity of sand is then hauled away in wagons and distributed as road material. The paper raider discussion is not a theoretical treatment of the subject but is the result of actual experience in oil production under the conditions mentioned.. That wells that produce sand produce in ore oil, and the best operating methods to bring this about are fully treated. It is, of course, impossible to remove all the oil sand underlying a property, but the greater the amount removed the greater becomes the production of oil. As stated in my paper, the surface disposal of this large volume of sand is a problem and the only use to which it can be put is road surfacing; but I did not intend to convey the idea that all this sand was thus used. Only a very small quantity was required on the company's roads, and two wagons only were employed for this purpose. The remaining sand accumulated in the numerous "washes" and sumps. Although this sand contained sufficient oil to stain the hands, it was, surprisingly dry and could be easily shoveled. As stated in the paper, "the piles of sand are gradually freed of their oil content and a crust forms on their surface which will bear the weight of a man." I consider this a high degree of separation. A small amount of oil necessarily remains in the sand and is held there by capillarity. Otherwise it would be useless as a road binder, and, furthermore, to recover such oil special processes of treating are required. Arthur Knapp says, "of the total volume produced by pumping, not more than 4 or 5 per cent. can possibly be sand." I cannot agree with this statement as I have managed many properties where the wells were so operated that the amount of sand produced was five times this figure.

Jan 6, 1917

By Donald L. Katz

FIFTEEN years ago Dr. Manning published a paper in "Petroleum Development and Technology" on '.Fundamental Research Relating to Petroleum." He tabulated for several industries "the proportion of their present success which can be fairly attributed to the application of information and processes obtained by scientific research," giving petroleum a score of 7 compared to 100 for the electrical and coal-tar industries. Today the petroleum industry as a whole and the producing groups both have raised their score beyond the majority and are climbing toward the top. Present practices are being developed both by fundamental research and the application of the research method in field operation.

Jan 1, 1941

By Oliver Bowles, Carl A. Gnam

THE construction industry normally contributes extensively to the general economic welfare of all sections of the country. Billions of dollars are spent for materials and labor, and the success or failure of many business enterprises depends upon the volume of construction. The steel, aluminum, copper, cement, brick and tile, lime, gypsum, stone, sand and gravel, and several of the less prominent mineral industries are vitally concerned. Of great interest, therefore, is the accumulation of needed construction following the relative inactivity of the past five years, the recent moderate revival in building, and the prospect of a broader and more definite upturn. One may judge the magnitude of possible expenditure for construction by what has occurred in the past. The peak years were 1925 to 1928, inclusive, when the annual values of con- tracts awarded amounted to over six billion dollars. In marked contrast was the 1933 total of about 1% billion, the lowest level shown in the Federal Reserve Board Index, which goes back to 1919, and the more favorable 1935 figure of about 1.7 billion. An increase of nearly four billion over the 1935 volume would be necessary to equal the peak year 1928.

Jan 1, 1936

By S. S. Clarke

ABOUT two years ago some of my friends were discussing the amount of drill-steel breakage that was permissible or not excessive, per month, per rock ton, per ton of steel or any unit of measure or output that would give a comparison between different kinds of drill steel. No one seemed to know what life to expect of steel, or what percentage of breakage might be termed excessive. In fact there were no operating data available to guide one in selecting the best steel for our mines, nor could any ideas or information be secured from the steel manufacturers. One was merely told that so and so used their steel and it was very satisfactory; or else one was given a highly technical lecture on their specific heat-treatment. Any estimates on expected breakage were just guesses, ranging from a fraction of a per cent to as high as ten per cent per month.

Jan 1, 1933

By G. W. Brownell, H. T. F. Lundberg, R. W. Pringle, K. I. Roulston

The rapid improvement of the airborne scintillometer and the perfection of its efficiency for counting low energy gamma radiation has made it possible to work out a technique to map in great detail the radiation pattern at the earth's surface. On such maps low radiation over certain areas appears to indicate the existence of oil accumulations, forming a pattern similar to that obtained by the geo-chemists. RADIOACTIVE analyses of samples from the surface of oil fields were carried out more than 10 years ago in Alberta by the alpha particle ioniza-tion chamber technique,' but large enough tracts could not be covered in these investigations to make possible any evaluation of the method as a means of oil exploration. Considerable interest has recently been revived, however, as a result of certain striking advances which have been made in the instrumentation available -for the measurement of radioactivity. It is the object of this paper to indicate the nature of these improvements in radiation technology and then to describe the attempts that have been made to interpret the radioactive patterns obtained in the course of airborne recordings with the new instruments. Since the survey can be carried out from the air and records can be accumulated over vast areas in a short time, the result may easily lend itself to statistical treatment. Areas have been surveyed in Alberta, British Columbia, Saskatchewan, Quebec, Texas, New Mexico, Nebraska, Colorado, Utah, and Montana. Producing fields in Alberta and West Texas have been flown over several times in different directions, Fig. 1. The operations were then extended into unknown territory and drill holes were put down on the anomalies which looked promising. The results from these drillings were encouraging and have given hopes for the development of an entirely new method of oil exploration. Any large scale method for the survey of radioactive anomalies must be based on the measurement of gamma rays, as beta and alpha rays have much too short a range to be of any significance. Thus the essential improvement which has made the present stage of this work attainable is the development of new highly sensitive detectors for gamma radiation. In the past the only detectors of any consequence that were available were the ionization chamber and the geiger counter, but both of these suffer from the defect that only a small proportion of the gamma rays passing through the counter are detected, possibly 0.1 to 0.2 pct. The recent development of the scintillation counter2,3 has completely transformed the situation and has had a considerable impact on many branches of nuclear technology. The detection of alpha particles in zinc sulphide screens by visual observation of the individual scintillations which these particles produce dates back to the early spinthariscope of Rutherford and Crookes, but the combined use of an appropriate scintillating phosphor and photomultiplier tube had to await the technical development of the latter many years later. With this development came the modern era of the scintillation counter and a knowledge of phosphors which have a large light output under the bombarding action of gamma radiation. Some of these phosphors are relatively dense and are capable of stopping a large proportion of the incident gamma radiation. As the sensitive region is the whole volume of the crystal, a very high detection efficiency, 50 pct or more, can be obtained for medium energy gamma rays. Scintillation counters for geological purposes were first developed in 19494-6 in an attempt to utilize this remarkable improvement in efficiency, which has the attractive consequence that only a small portion of the normal background of the counter is due to cosmic radiation. In 1949 tests were made in northern Saskatchewan by Lundberg Explorations Ltd. with portable scintillation counters which gave excellent results in the search for uranium and served to indicate unknown uranium deposits in areas previously closely surveyed with geiger counters. Portable scintillometers (registered in Canada) are now commercially available and in regular use,' and the adaptation of the instrument to radioactivity oil well logging has also been very successful.8 Initial attempts to measure radioactivity from aircraft with scintillation counters were made during this period in the same area and yielded most encouraging results. It would be appropriate to consider some specific requirements for airborne investigations. The essential problem to be met in the detection of any radioactive source is the necessity of obtaining a signal greater than the statistical fluctuations of the background counting rate for the instrument. It is possible to show that Nt>2k2 is the condition for detectability of a signal where N = average background counting rate for the detection. t = time constant of the counting rate meter, used to determine the average number of counts arriving in a certain predetermined time interval. N' = average source counting rate at the detector. k = N/N', and N>>N'. Sample values are given in Table I. Assume that the aircraft carrying the equipment is travelling at 120 mph, in which case it will cover 176 ft in 1 sec. Assume also, as a first approximation, that a point source target is in range when the air-

Jan 1, 1954

By Arthur S. Wright

THE accuracy of the silver-assay depends in great measure upon a careful regulation of the heat of the muffle during the process of cupellation. At the beginning of the operation, a relatively high temperature is required to " open " the lead buttons, that is, to clear off the black film of oxide that covers the surface of the metal button immediately after fusion has taken place. The muffle is usually closed up until the buttons are uncovered. As soon as a clear, free surface of molten metal is exposed to the oxidizing action of the air, the temperature should immediately be lowered to the minimum temperature at which the formation and absorption of litharge can progress freely, and the buttons still be kept from " freezing." The process, under satisfactory conditions, will be characterized by the formation of rings of litharge crystals (" feathers," as they are styled), on the cupel, about the oxidizing globule; and the nearer these rings of litharge crystals call be made to approach the central oxidizing globule without interfering with the freedom of oxidation and absorption, the smaller will be the volatilization of silver, and consequeiltly the greater the degree of accuracy attained. This minimum heat must be maintained uniformly during the oxidation of the lead; and just as the last of the lead is disappearing, and the button is preparing to l blick," the temperature of the muffle should be allowed to rise so that the last traces of lead will be driven off. This regulation of the heat calls into play all the skill of the assayer, and requires a vigilant eye, able to distirlguish between the slightest variations of temperature of the muffle, assisted by a nice adjustment of fuel and draft. With a few cupels in the muffle at one time, the proper heat for each cupel can be maintained by roughly approximating the proper temperature, and then moving the cupels backward and forward in the muffle; but this is gene-

Jan 1, 1897

By R. Wang, N. J. Grant, B. C. Giessen

By crystallographic and X-ray methods, the existence and isonzorphism of Ti3Rh5 and Hf3Rhs were confirmed. Both phases are of the orthorhombic Ge3Rh5 type; lattice parameters and refined positional parameters are given. The structure is related both to the filled-up NiAs-B8 and Cu-AI types. An analogous phase with zirconium does not exist; the effect of ternary substitutions for titanium ad hafnium suggests a size factor limit to be active. A recent survey of phase diagrams of the T4 metals titanium, zirconium, and hafnium with the T, noble metals rhodium and iridium indicated the existence of the A3B5 phases Ti3Rhs, ZrsRhs, and HfsRhs. Ti3Rhs and Hf3Rh5 were found to be isostructural, based on the line-rich powder patterns which had not been analyzed. Zr3Rh5 was considered to have a substructure of the NbRu type (orthorhombically distorted B2-CsCl type).&apos; Because, in combinations with other transition metals, hafnium and zirconium are generally more likely to form isostructural phases than hafnium and titanium (with the significant exception of the Ti2Ni-"E93" type phases based on T4 metals2), the reversal of this relation for the A3B5 phases was of interest. As shown in the following, the nonexistence of Zr3Rhs has been established, the structures of Ti3Rh5 and Hf3Rh5 have been worked out, and crystal chemical relationships and stability criteria are reported. EXPERIMENTAL METHODS AND RESULTS Alloy Preparation and Phase Diagram Work. Alloys were prepared from high-purity (99.99+ pct) elements by arc-meltin3,4.Heat-treated alloys were annealed in a vacuum of 3 x X torr for 24 hr at 1300DC. Metal-lographic samples were etched electrolytically in concentrated HCl with 5 v ac for 5 min.3 X-ray diffraction powder patterns were taken on a GE XRD-5 dif-fractometer with Cum radiation at low scanning rates (0.2 deg per min for 28). It was confirmed that Ti3Rhs and Hf3Rh5 have similar diffraction patterns, and that an alloy with the composition Zr3Rhs has a different pattern. Six Zr-Fh alloys with 59 to 69 at. pct Rh were therefore prepared and investigated in the as-cast state by X-ray diffraction and metallography. Alloys at 59 and 61 at. pct Rh were found to be a single phase, with the distorted B2-CsC1 type structure typical for the off-stoichio- metric region of the phase (Zr,-,Rh,)Rh. This phase forms a eutectic with ZrRhs at about 66 at. pct Rh: accordingly, alloys between 61 and 69 pct at. pct Rh consisted of two phases. There is no evidence for the existence of Zr3Rh5. Based on the results in Rafs. 1 and 5, on the present work on Zr-Rh, and on several additional alloys investigated, the portions between the AB and AB3 stoi-chiometry for Ti-Rh, Zr-Rh, and Hf-Rh are as follows: Further, several ternary alloys near Ti3Rhs and Hf,Rhs were prepared in which it was attempted to replace titanium and hafnium partly by zirconium, niobium, tantalum, and germanium. The results will be discussed in a later section. Structure Determination of Ti3Rh5. Since Ti3Rh5 and Hf3Rh5 are isostructural, the following discussion will largely deal with the former. Although the powder pattern of TisRhs is complex, as found previously,1 it could be indexed by comparison with other structures of A3Bs stoichiometry. Ti3Rh5 was found to be isostructural with Ge3Rh5, whose orthorhombic structure had been elucidated by Geller.9 As both the sizes and atomic numbers of germanium and titanium are comparable, the unit cell volume and the peak intensities could be expected to be similar; however, significant differences exist in the atomic positions, as will be shown. All lines in the powder patterns of Ti3Rh5 and Hf3Rhj could be indexed with primitive orthorhombic unit cells with the lattice constants: The fractional errors are 10 The low-angle portion of the indexed powder pattern of Ti3Rh with sin2 8 < 0.30 is listed in Table I. The extinction laws Okl only with k = 2n and hOl only with h - 2n are compatible with the space group Pbo2 and the more symmetrical space group Phnm of Ge3Rh5. Finally, the positional parameters of Ti3Rh5 and HfsRhs were refined under the assumption that titanium and hafnium occupy the germanium positions in Ge3Rh5. Integrated intensities were obtained from the diffraction patterns by planimetry. Intensities of overlapping reflections were separated by an iteration process incorporated into the least-squares positional refinement program according to a method described previously. The intensities of Ge3Rh5 were used in the first separation cycle, while the atomic parameters of Ge3Rh5 were used as starting values in the first refinement cycle. Absorption due to specimen

Jan 1, 1970

By W. M. Fox, D. P. Detwiler

IN the course of research on semiconducting inter-metallic compounds, it became necessary to obtain gallium metal of greater purity that that available commercially. Several methods were considered for further purification, including acid leaching,&apos; fractional crystallization,&apos; and zone-refining.3-5 The method of fractional crystallization was discarded as being equivalent to zone-refining in purification but inefficient in material and time. Both acid leaching and zone-refining were tried, and the method finally adopted is a combination of the two. The acid leaching technique has been reported&apos; to produce gallium in which no impurities are detectable spectroscopically. Although this method is very effective in removing oxides and surface contaminants, semiconducting material made of gallium subjected only to leaching indicated little reduction in the concentration of metallic impurities. Zone-refining, however, appears very effective in removing trace metallic impurities, but comparatively ineffective in removing the surface oxide film. Consequently, the method evolved consists of acid leaching to thoroughly clean the surface, followed by zone-refining to remove metallic impurities. The low melting point and relatively high thermal conductivity of gallium introduce some difficulty in maintaining frozen and molten zones in zone-refining. To accomplish this, it is found necessary to reduce the effective ambient temperature by circulating ice water in coils about the regions that are to be kept frozen, while heat is supplied to the molten regions by resistance coils. The power supplied to the heating coils is regulated by a constant-voltage transformer and a variable autotransformer. Both heating and cooling coils are mounted on a transite base. The gallium ingot is held in a closed pyrex tube sliding inside the heating and cooling coils, the reciprocating method of Tanenbaum et al. being employed to move the molten zones through the ingot at a rate of 2 in. per hr. This apparatus is shown in Fig. 1. The results of a spectroscopic analysis f a zone-refined ingot, as well as of the material as-received and after acid leaching, are shown in Table I. The ingot was 32 cm in length, and received 37 molten-zone passes, the molten zone being about 4 cm long. The only impurity found was lead, the following elements being reported also as checked but not found in the pure material: Al, Sb, As, Ba, Be, Bi, B, Cd, Ca, Cr, Co, Cb, Cu, Ge, Au, Fe, Mg, Mn, Mo, Ni, Pt, Si, Ag, Na, Sr, Sn, Te, Ti, W, V, Zn, and Zr. There thus appears no indication of pickup of Al, Mg, or Si from the pyrex boat as reported by Zimmerman&apos; in his fractional crystallization. Thus it appears that definite removal of lead from gallium occurs during the zone-refining process. It also may be concluded that a more sensitive analytical procedure than spectroscopy is required to evaluate quantitatively the purity of zone-refined metals. One such procedure which is proposed for use in the near future is the measurement of very low temperature resistivity. Although this will not identify the impurities present, it offers a very sensitive check of total impurity. Acknowledgment This work was supported by the Air Research and Development Command, United States Air Force.

Jan 1, 1956

By AIME AIME

THE Petroleum Division will hold two meetings this fall, one on the Coast at Los Angeles, Sept. 29, with the technical sessions in the assembly room of the California Oil and Gas Association and a banquet Friday evening at the Richfield Cafe atop the Richfield building; the other in the Southwest, at Dallas, Texas, Oct. 6 and 7, with the Baker Hotel as headquarters. Dr. Frederick M. Becket, President of the Institute, and A. B. Parsons, Secretary, will attend both meetings. Arrangements for the meetings are not yet complete but the respective local committees, working in close touch with the officials of the Division are rapidly shaping up the programs and other detail.

Jan 1, 1933

By E. H. Dix

All commercial aluminum contains small percentages of copper, iron, and silicon as unavoidable impurities. The purest metal obtainable commercially, special grade high purity ingot, contains a maximum of 0.50 per cent. impurities of which the usual minimum amount of copper is 0.01 per cent.; silicon, 0.12 per cent.; and iron, 0.20 per cent. This grade is too costly for most purposes. The two standard grades, Nos. 1 and 2, containing a minimum of 99.0 and 98.0 per cent. aluminum, respectively, are more generally used. Other grades of secondary aluminum often contain as high as 3 or 4 per cent. of impurities, which include 1 per cent., or more, of zinc. Specifications for high-grade aluminum-casting alloys generally allow a maximum of 1.7 per cent. for total impurities. The S. A. E. Specification No. 33, which is intended to cover alloys made from secondary aluminum ingot, gives the iron maximum as 1.5 per cent. and the maximum for silicon (including manganese and tin) as 0.75 per cent. The effect of even relatively small amounts of impurities on the physical properties of ingot aluminum is shown by the following cornparison of two lots of aluminum, which may be taken as representative of special grade and grade No. 2 ingot, respectively. AnalysEs Special Grade, Gbade No. 2, Per Cent. PeR CBnt. Copper................................. 0.01 0.32 Silicon................................. 0.12 0.32 Iron................................... 0.42 0.82 Aluminum.............................. 99.45 98.54

Jan 1, 1923

By E. H. Dix

All commercial aluminum contains small percentages of copper, iron, and silicon as unavoidable impurities. The purest metal obtainable commercially, special grade high purity ingot, contains a maximum of 0.50 per cent. impurities of which the usual minimum amount of copper is 0.01 per cent.; silicon, 0.12 per cent.; and iron, 0.20 per cent. This grade is too costly for most purposes. The two standard grades, Nos. 1 and 2, containing a minimum of 99.0 and 98.0 per cent. aluminum, respectively, are more generally used. Other grades of secondary aluminum often contain as high as 3 or 4 per cent. of impurities, which include 1 per cent., or more, of zinc. Specifications for high-grade aluminum-casting alloys generally allow a maximum of 1.7 per cent. for total impurities. The S. A. E. Specification No. 33, which is intended to cover alloys made from secondary aluminum ingot, gives the iron maximum as 1.5 per cent. and the maximum for silicon (including manganese and tin) as 0.75 per cent. The effect of even relatively small amounts of impurities on the physical properties of ingot aluminum is shown by the following cornparison of two lots of aluminum, which may be taken as representative of special grade and grade No. 2 ingot, respectively. AnalysEs Special Grade, Gbade No. 2, Per Cent. PeR CBnt. Copper................................. 0.01 0.32 Silicon................................. 0.12 0.32 Iron................................... 0.42 0.82 Aluminum.............................. 99.45 98.54

Jan 1, 1923