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(There are 82 Local Sections in the United States, 10 Foreign) ADIRONDACK Established June 18, 1952 Official year begins in January Meets next to last Saturday monthly April through October Local Section Dues AIME Mbrs $2 Affiliate Mbrs $3 Severn P Brown, Chairman George E Erdman, Vice-Chairman Patrick F Farrell, Secretary-Treasurer Republic Steel Corp Mineville, N Y

Jan 1, 1960

Year of Election 1959 Andrew Fletcher, New York, N Y "For his outstanding leadership in the lead and zinc mining industries, and for his able and devoted services to the Institute as its Treasurer and President, and as a Director for many years " 1917 Herbert Hoover, New York, N Y 1955 George M Humphrey, Cleveland, Ohio 1950 Zay Jeffries, Ptttsfield, Mass 1942 Essington Lewis, Melbourne, Vic, Australia 1959 John M Lovejoy, New York, N Y "For his distinguished service to the Institute, for his outstanding contributions in furthering the professional status of petroleum engineers, for his pioneering in application of engineering to petroleum production, and for his outstanding record of public service on behalf of the petroleum industry " 1957 Donald H McLaughlin, San Francisco, California 1957 C H Mathewson, New Haven, Connecticut 1938 Albert M Portevin, Parts, France 1957 Fred Searls, Jr, New York, N Y

Jan 1, 1960

By T. D. Murphy

This chapter deals with those types of silica raw materials that have been segregated and refined by natural processes into nearly monomineralic deposits and hence, by virtue of their high degree of purity, have become the sources of commodities having special and somewhat restricted commercial uses. In some instances, these raw materials occur in nature as unconsolidated quartzose sand or gravel and can be exploited and used with very little preparation and expense. More often, they occur as sandstone, conglomerate, quartzite, quartz mica schist, or massive igneous quartz which must be crushed, washed, screened, and sometimes chemically treated before commodities of suitable compositional and textural characteristics can be successfully prepared. The occurrence and distribution of silica raw materials is summarized and an effort has been made to bring commodity definitions, critical properties, and specifications up to date. Presentation of mining and processing methods is considered beyond the scope of this article; they are, for the most part, conventional and well known. New production techniques are currently reported in the trade journals and are later adequately described in technical publications as promptly as competitive restrictions allow. Discussion on Basis of Use ABRASIVE USES Industrial silica used for abrasive purposes falls into three main categories: (a) blasting sand; (b) glass-grinding sand; and (c) stone-sawing and rubbing sand. Blasting sand is a sound closely-sized quartz sand which, when propelled at high velocity by air, water, or controlled centrifugal force, is effective for such uses as cleaning metal castings, removing paint and rust, or renovating stone veneer. It is commonly referred to as Sand Blast sand. Multicycle quartz sand is an efficient blasting agent by merit of its survival characteristics which are soundness, toughness, and hardness. Steel grit and shot have supplanted it to a large extent but owing to their higher cost and tendency toward deterioration in storage, are still not universally used. It is conceded that angularity promotes faster cutting but this is offset by a higher loss in fines. The peening action of a rounded grain is a desirable feature in achieving a satin finish for certain light metal castings but a subangular grain is unsurpassed for fast heavy cutting. Specifications are chiefly based on size frequency distribution but it is mandatory that the grain be free of adhering clay or irony coatings. Material that dusts upon handling will not be tolerated. There is no uniform trade designation for the many blasting sand grades. Most producers sell on the basis of numbered grades; that is, No. 1, No. 2 and so on, this generally connoting fine to coarser grades. Designation of grade by the two sieve sizes between which most of the material lies, is practiced in some areas. Thus, in a No. 1220 grade, 98 pct of the material passes a 12 mesh sieve and is retained on a 20 mesh sieve. Blasting sand specifications vary according to use. Coarse grades range from 4 mesh to 12 mesh, medium grades range from 12 mesh to 30 mesh, finer grades may range from 20 mesh to 100 mesh or finer. Specifications generally call for narrow limits of gradation, requiring precise sizing methods. The fact that most blasting sands are retained

Jan 1, 1960

By W. V. Green

The creep-rupture behavior of commercial powder-metallurgy tungsten rod is reported for temperatures of 2250°, 2500°, 2700°, and 2800°C, stresses up to 7000 psi, and times up to 4 hr. The temperature dependence and the stress dependence of creep rates are evaluated. Rupture time is fitted to the Larson-Miller parameter and compared to lower-temperature and higher stress results reported by pugh.4 THE tensile strength of single-crystal wire1 and of polycrystalline wire2 have been measured by Goucher. More recently Bechtold3 and pugh4 have studied the mechanical properties of tungsten rod between room temperature and 1200°C. Since tungsten has the highest melting point of all metals, it should retain useful strength to very high temperatures, and should find many applications in missiles, rockets, and so forth. Therefore, the mechanical usefulness of polycrystalline tungsten rod was investigated in the 2250" to 2800°C temperature range by short-time creep-rupture tests. MATERIALS TESTED Creep specimens were machined from 1/2-in. round commercial tungsten rod which was manufactured from powder by cold pressing, sintering, and hot swaging. Purity reported by the vendor was 99.95 pct W. Spectrochemical analyses showed "traces" (less than 0.01 pct) of silicon, iron, and titanium, and "faint traces" (less than 0.001 pct) of calcium and manganese. Carbon content was 30 ppm and nitrogen content was 70 to 110 ppm. No oxygen analysis was obtained. Room-temperature stress-strain tests on the as-received tungsten gave badly scattered results. Threaded end specimens broke at the threads. When these specimens were retested using shoulder grips, the specimens broke at the shoulders. No fractures occurred in the gage lengths. The fracture stresses were: 127,000; 137,000; and 154,000 psi for three specimens which fractured at the shoulders. The microstructure of the as-received tungsten rod is shown in Fig. 1. SPECIMENS USED Fig. 2 shows the two types of creep specimens tested. The threaded-end type specimen, which was used in most tests, had a 3/4-in. gage length and 1/4-in. gage diam. The cone-end specimen, which was used primarily to investigate the effects of a smaller gage diameter and the practicability of the modified grips and specimen, had a 3/4-in. gage length and a 1/8-in. gage diam. In both cases, the gage length terminated at 0.005-in. high shoulders which served as fiducial marks for optical strain measurements. Surface finish on the gage length was 16 µ-in. rms. Creep rates and rupture times were not significantly different for the two types of specimens and were not affected by electropolishing the specimens before testing. TESTING PROCEDURE The constant-load creep-testing machine used has been described by Smith, Olson, and Brown.5 In it the specimen is held vertically by grips of similar material and on the axis of a cylindrical tungsten or tantalum heater-tube. The specimen is loaded by means of the specimen grips, a pull rod (which is sealed to the chamber lid by a vacuum-tight bellows), a mechanical lever system, and hanging dead weights. Both specimen and grips are heated by radiation from the heater-tube, which is heated by its own electrical resistance. An optical system views the incandescent specimen through slits in the radiation shielding and heater-tube. The optical system projects an enlarged image of the specimen gage length on a ground-glass screen. Periodic gage-length measurements are made on this image with two cathetometers. Thorium oxide coatings on the specimen threads or conical end surfaces completely prevented diffusion-welding of specimens to grips, and were used

Jan 1, 1960

A revolutionary development in blasting materials has occurred in the past 5 years. Ammonium nitrate, sensitized by the addition of a few percent of No. (class) 2 diesel fuel or other suitable petroleum product, has been adopted as a low-cost, efficient blasting agent2/ by a wide variety of mining and heavy construction operations. Moreover, ready availability of the component supplies throughout the Nation and ease of their formulation into effective blasting agents have made it possible for the blaster himself to pre-pare the mixes at the site of use. Although these field-mixed products have partly or wholly displaced explosives such as dynamites in some applications, there are other blasting operations where the fuel-sensitized ammonium nitrate agents do not appear to be well adapted. Important safety characteristics are inherent in ammonium nitrate-based blasting agents prepared under competent factory control, or when field mixed under equivalent close control--as long as the hazards they present are clearly understood and respected. This publication attempts to summarize knowledge of those hazards and to incorporate practical ways to cope with them. A series of safety recommendations thus is presented. These recommendations cover the preparation, storage, transportation, and use of field-mixed ammonium nitrate blasting agents.

Jan 1, 1960

By R. F. Sheldon

Largest uranium deposit in the Northwest is Dawn Mining Co.'s Midnite mine on the Spokane Indian Reservation. The orebodies lie along the contact of granite and metamorphosed sedimentary rock and are controlled by faults and shear zones near the granite contact. In the oxidized zone the deposits consist mainly of the secondary uranium mineral meta-autunite; sooty uraninite and primary uranium minerals are known to occur at greater depths. Elevations in the mine area range from 2500 to 3500 ft. The rolling hills and low, rounded mountains are covered with grass and evergreen trees. HISTORY AND DEVELOPMENT Original showings were discovered with a geiger counter in the spring of 1954 by prospectors Jim and John LeBret. High radioactivity in several schist outcrops was found due to scaly coatings of a greenish-yellow, fluorescent mineral, later identified as meta-autunite. Prior to this time autunite was not known to occur in the state of Washington, and no significant uranium deposits had been found in the Pacific Northwest. Outcrops in the area were few, and most of the ground was mantled with 2 to 10 ft of overburden, but three other radioactive zones were discovered by prospecting the ridge southward along the strike of the schist near its contact with granite for three quarters of a mile. Midnite Mines Inc. was formed

Jan 1, 1960

Established as Mining, Geology and Geophysics Division, Sept. 27, 1949 Name changed February 19, 1958 Robert J Lacy, Chairman John G Hall, Assistant Chairman Vice-Chairmen Peter Joralemon, Membership J M Ehrhorn, Program John C Wangaard, Publications A W Ness, Secretary American Smelting & Refining Co 600 Crandall Building Salt Lake City 1, Utah

Jan 1, 1960

By Sidney Katell

Tonnage oxygen plants are or can be made available in sizes ranging from 150 to 1,000 tons per day. Capital requirements are estimated from $5,400 to $14,700 per daily ton, depending upon size of plant, cycle employed, and purity and discharge pressure of the product. Similarly, operating costs before return on investment will range from $4.80 to $10 per ton. INTRODUCTION Several processes4 5/ that can be used to convert coal to synthetic liquid fuels, synthetic pipeline gas, or hydrogen require high-purity oxygen as one of the basic raw materials. Depending on the and product and its specific use, the oxygen required will be of 95 or 99.5 percent purity. The quantity required, in turn, depends on the process for which the oxygen will be used and the size of the processing plant and will range from 150 to 4,000 tons per day.

Jan 1, 1960

By R. H. W. Chadwick

We in Kennecott are well aware that Alaskans are interested in the progress of our project at Ruby Creek. We would very much like to be able to present you with a final report at this time and tell you about a new mine. I'm afraid, however, that it will be several years at best before such a report can be made. This, then, is an interim report to describe briefly some of our findings to date, and to acquaint you with some of the problems, both geologic and economic, which must 5e resolved favorably before we can talk about a mine. There are several things about this project which make it unusual and interesting to those of us who have been connected with it. Firstly, there is the fundamental importance to Alaska, in the present stage of its economic history, of any undertaking which offers promise of turning a natural resource into a competitive export product. I am sure all of us would get a lot more satisfaction out of having a part in bringing in a new mine in Alaska than we would out of adding another one to the long list in, say, Arizona.

Jan 1, 1960

By Sanford J. Douglas

This publication describes a study by the Federal Bureau of Mines of devices and methods used for testing and splicing 4,160-volt and 440-volt cables and for providing ground-fault protection for 440-volt circuits, as developed and used by the electrical staff of the Tecumseh coal mine, an open-pit operation at Boonville, Ind. The testing and ground-fault devices described should find ready application in other open-pit mines, and, with suitable modifications for voltages involved, in underground mining. The devices and testing methods are based on sound engineering principles and are time-tested and economically feasible, Four devices are used: A high-voltage tester, and a low-voltage high- current tester, both for testing 4,160-volt cables; a tester for 440-volt cables; and, electronic ground-fault protective device for 440-volt cable circuits. All the cable testers and the grounding device were designed and built at the mine from standard parts. They are inexpensive, dependable, and job tested, An attempt has been made here to describe them in enough detail so that interested persons can assemble duplicate units.

Jan 1, 1960

By John C. Machisak

THE INJURY data and experience at quarries and related plants of the United States are presented in this publication under the following general sections (A) General injury experience: Tables 1-3: Current data on number of injuries, injury-frequency rates, location, accident agency, degree of injury, and related employment data. (B) Injury experience at different kinds of quarries: Tables 4-5: Current data on number of injuries, injury-frequency rates, location, accident agency, degree of injury, and related employment, data. (C) Injury experience by States: Tables 6-20: Current data on the number of injuries, injury-frequency rates, accident agency, degree of injury, and related employment data. (D) Selected injury data: Tables 21-30: Current data on various selected factors of operating conditions at different kinds of quarries, including employment size-groups, length of shifts, comparative severity of injuries, and injury data and related employment experience at dimension-stone and nondimension-stone quarries and at underground quarries. (E) Historical injury experience: Table 31: Injury and employment data on the quarrying industry for 1911 through 1957. Statistical data on injuries and related employment in the quarrying industries have been collected annually from the operating companies since 1911. Reporting to the Bureau of Mines is voluntary; there is no Federal law compelling operators of quarries and related plants to supply such data. Data presented herein may not be complete for the entire industry. They are however, believed to be representative of the hazards common to all quarry and related workers. Moreover, the figures are comparable as between States-a significant fact in view of the lack of uniformity among the States with regard to the classes of injuries covered by State reports and other factors that tend to make it impracticable or impossible when using State records to

Jan 1, 1960

By W. A. Tiller, J. P. McHugh

HE majority of liquidus and solidus surfaces in phase diagrams have been determined by the conventional cooling- and heating-curve techniques.' These techniques have two main shortcomings: 1) the solidus may be in considerable error due to the difficulty involved in completely homogenizing the solid and 2) the determination of liquidus and solidus in more than a two-component system does not enable one to determine tie-lines connecting the specific equilibrium solid and liquid compositions. However, in a recent paper by one of the authors,' a method was suggested whereby the liquidus and solidus surfaces plus tie-lines in an n-component system may be determined. This method utilizes a controlled solidification technique and assumes that interface equilibrium exists during freezing. The present work was undertaken with a twofold purpose; first, to determine the liquidus and solidus lines in the pseudo-binary system Bi2Te3-Bi2Se3 by heating- and cooling-curve techniques and, second, to determine the partition coefficients of Te and Se in the BizTe3-,Sex system by controlled solidifica- tion techniques. The two sets of results can be compared to test the accuracy of the controlled solidification method. EXPERIMENTAL I—The starting materials for this study were 997999 pct Bi, Te, and Se, obtained from the American Smelting and Refining Co. The compounds BizTe, and Bi2Se3 were each prepared by melting together stoichiometric amounts of the elements, followed by twelve zone-refining passes. This produced homogeneous bars of the compounds for use in the phase-diagram studies. The apparatus used to obtain heating and cooling curves is illustrated schematically in Fig. 1. The alloy samples were located in a graphite crucible placed in a stainless steel canister. The canister was supported in a heavily lagged pit furnace by a device which oscillated the canister about its vertical axis at a frequency of about 3 cycles per sec during heating and cooling-curve runs. The graphite crucible was designed to minimize the thermal coupling of the sample to the furnace. A thin graphite sleeve separated the alloy sample from the stainless steel tube that housed the thermo-

Jan 1, 1960

By D. Kramer

HASEN1 has published a phase diagram for the zirconium-nickel system. This phase diagram has been redetermined by Hayes, Roberson, and paasche2 in the range 0 to 50 at. pct Ni. Recently, Smith and Guard3 have published a tentative diagram for the

Jan 1, 1960

By Raymond B. Ladoo

Wollastonite is a calcium metasilicate, with the formula CaSiO3; containing theoretically 48.3 pct CaO and 51.7 pct Si02. It is one of many natural and synthetic silicates with varying CaO/SiO2 ratios, with and without water of crystallization. While it is a very common mineral, deposits of sufficient size and purity to be of commercial interest are unusual. There is only one producer (1958) of wollastonite for industrial use in the United States, Godfrey L. Cabot, Inc. at Willsboro, New York. There has been a small production of surface material for ornamental use from near Blythe, California. Carload tests have been made on California wollastonite for making mineral wool and a commercial plant for this purpose was projected in 1957. Properties Wollastonite is monoclinic and commonly occurs in masses or aggregates of bladed or needle-like crystals. It has a perfect cleavage parallel to the long prismatic axis. It is rather brittle and some types grind easily to a very finely fibrous product, but other types, due to interlacing of fibers, are tough and difficult to grind. Mobs hardness is 4.5 to 5; specific gravity 2.8-2.9; index of refraction 1.616 to 1.631; melting point 1,512°C. Color when pure is a brilliant white, but when less pure it may be gray or brown. Luster is vitreous, transparent to translucent. Common mineral associates are garnet (several varieties), diopside, calcite and quartz. The nature of the mineral impurities determines to a large degree the commercial value of a deposit. At Willsboro, New York, the impurities consist chiefly of iron garnet and iron diopside which are both magnetic and so are easily removable by magnetic separation, yielding a nearly theoretically pure product. Some deposits in California contain calcite and quartz which cannot be removed cheaply, thus limiting market possibilities. Occurrence Wollastonite is a contact metamorphic mineral occurring in most places within or associated with impure limestones. The deposits at Willsboro, New York1,2,3,5 consist of two or more beds dipping 15-50°E and striking NW-SE. The main bed, 30 to 70 ft thick, may be traced on the surface for at least 2 ½ miles. In this belt, the Pre-Cambrian Grenville limestone has been injected and partially replaced by the more liquid portions of an anorthositic magma. Buddington and Whitcomb3 have described the rock as "Mixed gneisses, pyroxenite and garnetiferous gneisses and skarns." Prospecting revealed the wollastonite at ten different places in the belt, overlain in most places by a garnet rock. Diamond drilling has proven several million tons with probable reserves around 15 million tons. Interbedded with the wollastonite are beds of garnet from a few inches to several feet in thickness. In the wollastonite ore itself the chief and almost only associated minerals are garnet (mostly almandite but some andradite and grossularite) with small amounts of green hedenbergite. Inasmuch as the almandite and diopside are magnetic they are easily separated from the wollastonite in high intensity magnetic separators. If grossularite should occur in quantity other means of separation would be needed. Wollastonite has been reported at 35 localities in California12 but only those in the Big Maria and Little Maria Mountains, 16 to 20 miles north of Blythe, Riverside County, are

Jan 1, 1960

By A. A. Bauer, M. S. Farkas, F. A. Rough

An investigation of the d-phase relationships between the uranium-zirconium and uranium-molybdenum systems was conducted. A ternary cut joining U-31.5 at. pct Mo to U-74 at. pct Zr is presented on the basis of differential thermal analysis, metallographic and X-ray diffraction data. HyDothetical isothermal ternary sections, inferred from the determined d-phase relationships, are presented for the uraniztm-zirconium-molybdenum system. A ternary eutectoid, at 454ºC, was found in zirconium-rich alloys. Its composition, based on metallography and electron-beam micro-analysis, is estimated as U-61.7 at. pct Zr-7.1 at. pct Mo. URANIUM binary systems have been studied extensively in the past to supply basic information needed in reactor-fuel development. Alloys of uranium with zirconium, molybdenum, and titanium are of particular interest because, in these binaries, extensive or complete solid solubility between the body-centered-cubic forms of these elements and y uranium exists. In addition, an intermediate phase of limited solid solubility forms in each of these systems by transformation of the high-temperature ?-uranium phase. Previous investigation of the phase relationships existing between the intermediate 6 phases in the uranium-zirconium-titanium and the uranium-molyb- denum-titanium ternaries have already been reported.1,2 The results of an investigation of the phase relationships existing between the 6 phases in the uranium-zirconium-molybdenum system is reported here. The phase equilibria that occur in the solid-state portions of the pertinent binary systems are shown in Fig. 1. Phase nomenclature appearing throughout the report is as shown in these diagrams. The crystal structure of the phases in this system are given in Table I. EXPERIMENTAL PROCEDURES Alloys were cast and fabricated to 1/4-in.-diam rod. Specimens were heat treated and examined by metallographic and X-ray techniques. Thermal-analysis data were obtained.

Jan 1, 1960

By D. Gupta, S. Weinig

This investigation comprises the study of dislocation-oxygen interactions in a! titanium and its effect on the ductile to brittle transition in titanium. Internal friction techniques using a low-frequency lorsion pendulum were used to study the oxygen atom interactions with dislocations in "superpurity" titanium. A calculation of the interaction energy between an oxygen atom and a dislocation, based on the "breakaway" strain resulted in a value of 0.015 ev as compared to theoretical values of 0.022 and 0.035 ev for edge and screw dislocations, respectively. Both the saturation of the room temperature decrement and the transition from ductile to brittle behavior occurred at 1.5 at. pct 0. It was proposed that the embrittlement was due to oxygen atoms immobilizing the dislocations. It was possible to increase the ductility of the Ti-0 binary alloys by decreasing the oxygen pinning. The increase in uniform elongation was 30 pct for an increase in the preanneal temperature of 300°C. ThE room-temperature ductility of a titanium is significantly affected by interstitial solutes. Although oxygen has a solid solubility of 15.5 pct by weight, the room-temperature ductility extends only to 0.6 pct.' The ductility precipitously falls at this concentration and the fracture characteristics change from ductile to brittle.2 The small effective bulk composition of solute required to destroy the room-temperature ductility of the titanium must be indicative of an in-homogeneous distribution of solute atoms. Internal friction techniques were used in this investigation to

Jan 1, 1960

Jan 1, 1960

By H. J. McQueen, G. C. Kuczynski

ThE useful properties of k6-Alfenol and the thermenol alloys (summarized by J. E. Nachman and W. J. Buehler') have encouraged research into those alloys which, having compositions near 25 at. pct Al, 75 at. pct Fe, undergo an ordering transformation between 500° and 550°C. The equilibrium diagram of the iron-rich iron-aluminum alloys was first determined by Bradley and Jay.2,3 They distinguished three structures: the disordered, which is bcc; FeAl, which is simple cubic with one Fe atom and one Al atom per lattice site; and Fe3Al, which is fcc with three Fe atoms and one Al atom per lattice site. This last structure may be conceived as eight body-centered cubes with Al atoms at the centers of alternate ones, so that Al atoms have only Fe as first and second nearest neighbors. Later, Osawa and Murata4 determined the boundaries of the different superlattice regions in the iron-rich Fe-Al solid solution by dilatometric and X-ray methods. Two of the six phases, which they found between 0 and 50 at. pct Al, were never identified by other workers. A. Taylor and R. M. ones,' concurrently with and independently of this research, redetermined this diagram by measuring lattice parameters at temperature. Further reference will be made to their results. EQUILIBRIUM DIAGRAM A) Experimental Procedure—The alloys were prepared from NRC gas-free iron (99.9 pct Fe) and 99.99 pct Al. They were melted in alumina' crucubles under vacuum in an induction furnace. If the ingots were unsound or showed more than a 3 pct weight loss, they were rejected. The ingots were homogenized at 1100°C for 24 hr before hot-rolling at 700" to 900°C from 1 in. to 0.25 in. thick. It is interesting to note that alloys containing more than 28 at. pct Al were able to take an 80 pct reduction of area in the ordered FeAl region. The dilatometer specimens and specimens for chemical analysis were cut from these plates. A Leitz dilatometer was used to measure the coefficient of linear expansion as a function of temperature. The specimens were slowly cooled from 900" to 300°C where they were annealed for 10 hr before slowly cooling to room temperature. The expansion was recorded photographically as the alloys were heated and cooled at 1.5oC per min between 100" and 1000°C. The magnetic measurements determining the Curie points were performed on the dilatometer specimens in the dilatometer, by using direct current in the furnace windings both to heat the specimen at 1.5°C per min and to serve as the primary coil. The regular specimen holder was replaced by a thin alundum tube on which was wound, as a secondary, a closely spaced coil of fine copper wire. A reversal of current in the furnace windings produced, in the secondary, an emf which was proportional to the induction in the specimen, and which could be detected on a galvanometer. In this way, it was possible to determine the Curie points of alloys to within * 5°C. B) Results and Discussion—The coefficients of linear expansion, as obtained from the dilatometer curves, are plotted as a function of temperature and composition in Fig. 1. Since in many cases the heating and cooling curves were superimposed, it was decided to measure slopes of heating curves only. Definite high peaks, due to the transformations, were observed on each curve between 400" and 520°C, and, for alloys containing more than 23 at. pct Al, a second set of smaller peaks at temperatures above 660°C. The sharpness of the peaks indicates that ordering to Fe3Al is a first-order reaction. The compositions and the temperatures of these peaks are listed in Table I. When these temperatures are plotted as a function of the composition, the result is the constitution diagram presented in

Jan 1, 1960

By C. G. Kirkland

An apparatus for determining trace impurities in Grade-A helium by mass spectrometer methods was designed and built by the Federal Bureau of Mines. Grade-A is the designation for helium commercially produced by the Bureau. Its nominal purity is 99.995 percent. The device, following a suggestion by Deaton, concentrates the impurities in the helium by freezing them out in a coil-and-trap assembly cooled by liquid helium. A known volume of helium is passed through the trap, the concentration ratio determined, and samples of the concentrated impurities are analyzed by mass spectrometer methods. The apparatus has been in service for approximately 20 months and has satisfactorily met all requirements. Over 200 analyses were made of helium contained in conventional cylinders, obtained from the Amarillo, Exell, Otis, and Navajo Helium Plants, during the 6-month period ending March I, 1959. Total impurity concentrations, in parts per million, were as follows: Amarillo, 19.1; Exell, 17.1; Otis, 11.3; and Navajo, 6.6. Neon and nitrogen were the major impurities. Complete data are shown in table 4 in the body of this report.

Jan 1, 1960

By C. Land, R. Hultgren

Heat contents of four Cr-Ni alloys were determined in a diphenyl ethev calorimeter. Aside from ferromagnetic effects, Kopp's law of additivity of heat capacities is approximately fol-lowed, in disagreement with earlier results of A. W. Foster. In 1934 Foster1 reported heat-capacity measurements of dilute solutions of chromium in nickel, primarily as a study of the effect of alloying on the ferromagnetic Curie temperature. He found that, apart from the Curie temperature effect, the general level of heat capacities was reduced 10 pct by the addition of 1 pct Cr; 20 pct by the addition of 2 pct Cr. His measurements of pure nickel essentially agreed with accepted values. These results indicate that small amounts of dissolved chromium cause an increase in the Debye temperature of nickel, presupposing a change of frequency of interatomic bonding vibrations which is much larger than should be expected. If Foster's results were verified, therefore, they would have important implications for bonding theory. The only other heat-capacity measurements in this system seem to be those of Taylor and Hinton,' who studied anomalies which they attributed to super-lattice formation at 25 at. pct Cr. At temperatures above the anomaly, Taylor and Hinton found heat capacities at this composition were quite normal, approximately obeying Kopp's law of additivity. EXPERIMENTAL WORK In order to verify or disprove the remarkable results of Foster, the heat contents of four dilute solid solutions of chromiunn in nickel were measured in a diphenyl ether calorimeter. This instrument, described elsewhere,, operates on the principle of the Bunsen ice calorimeter, but uses diphenyl ether as the working substance. Diphenyl ether melts at the convenient temperature of 26.S°C and supplies a more sensitive measure of heat than ice. The hot sample, in an atmosphere of argon, is dropped from a furnace at a measured temperature into a chamber which is surrounded by a mixture of solid and liquid diphenyl ether. The heat from the hot specimen melts some of the solid without chang- ing the temperature of the calorimeter. The amount of solid melted, and therefore the number of calories released by the specimen, is measured from the increase of volume of the mixture, which pushes mercury down a graduated capillary tube. The apparatus has been standardized against the known heat content of pure platinum. Heat loss during the dropping of the specimen was estimated by comparing the heat content of an empty platinum capsule with a solid platinum ball of the same radius and degree of polish of the surface. Repeated tests demonstrate the precision of measurement to be closer than *0.3 pct. Smoothed experimental results are listed in Table I. The tabulated values for pure nickel are taken from kelley, several measurements were made which agreed closely with this tabulation. For chromium, however, no similar agreement was found. The values tabulated were taken from a thorough study of chromium with the diphenyl ether calorimeter which will be published elsewhere.= Suitable plots of the data showed the expected ferromagnetic anomalies in the low-chromium alloys, while the 11 pct alloy shows no ferromagnetic anomaly, but a different, small anomaly below 900°K. This is perhaps the same anomaly found in CrNi, which was once attributed to superlattice formation,' but is probably due to some other cause, such as antifer-

Jan 1, 1960