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By Paul Pietrokowsky

THE formation of intermediate phases in the solid state reaction of titanium with silicon, germanium. and tin (of subgroup 4B in the periodic table) was the subject of a recent paper.' Further investigation of the system Ti-Sn revealed the presence of a new compound on the titanium-rich side of this phase diagram. Metallographic evidence indicated that this new phase was situated very close to 75 atomic pct Ti. The present work is concerned with the crystal structure of the intermediate phase Ti3Sn. Iodide-process titanium metal, furnished by the New Jersey Zinc Co., was used in this investigation. The metallic tin was received in powder form from Charles Hardy Inc., New York; its purity was 99.80 pct. The titanium rod was machined into small cups 1 cm in diam and about 1.5 cm in height. The tin powder was compacted, melted, and then placed in the titanium cups and alloyed by electric arc melting in a helium atmosphere. The alloys, weighing approximately 8 g, were sealed in evacuated quartz tubes and homogenized at 1030°C for 5 days. This isothermal heat treatment was terminated by a water quench from the soaking temperature. Filings of the alloyed pellets were sealed in evacuated quartz bulbs and quenched from 1030°C into liquid argon. A 14.32 cm Debye Scherrer X-ray camera was used for the powder diffraction study. The copper radiation was filtered. X-ray diffraction data for the compound Ti3Sn are given in Table I. The data were indexed on the basis of a hexagonal lattice. Good agreement between observed and calculated values of the square of the reciprocal interplanar spacings was obtained with the following expression: (1/d)2 = 0.03810 (h2 + hk + k2) + 0.04410 (l2) Unit cell parameters were calculated by the method of least squares from the reflections (20.3), (22.2), (40.1), and (42.1); ao = 5.916 & 0.004A, co = 4.764 ± 0.004A, and co/ao = 0.805. The relatively small size of the unit cell allowed the unambiguous indexing of most of the reflections from planes of large spacing. An inspection of the assigned indices (Table I) reveals the absence of (hk.l) reflections when 1 2n. A systematic absence of this type leads to the space group C 6/mmc or one of its subgroups. Assuming, for a first approximation, a linear increase in the density of titanium with the addition of tin, it follows that there are two stoichiometric molecules of Ti3Sn per unit cell. The density calculated from X-ray measurements is 5.194 g cm-'. At this point it became clear that Ti3Sn might be isomorphous with Mg3Cd. The 6 Ti and 2 Sn atoms were placed in the following positions of space group D4 6h, C 6/mmc: 6Tiin (h): X 2X 1/4; 22;; 1/4;Xx 1/4;x2x3/4; 2x x 3/4; x x 4; with x = 516 2 Sn in (c): 1/3 2/3 1/4; 2/3 1/3 3/4.

Jan 1, 1953

By W. C. Ellis, E. S. Greiner

METALLIC titanium has been prepared in small quantities since the beginning of the century. Hunter1 reported in 1910 that he obtained a malleable product of 99.9 pct purity by the reduction of the tetrachloride by sodium in a closed container. Later Van Arkel2 and Fast3 prepared small quantities of malleable titanium by thermal decomposition of titanium iodide. Another method for producing malleable titanium from tetrachloride was reported by Kroll4 who used magnesium as the reducing agent. More recently Dean, Long, Wartman, and Anderson5 working at the U.S. Bureau of Mines have reported the preparation of the metal on a pilot plant scale by the reduction of titanium tetrachloride by magnesium in an atmosphere of helium. Their product, which is malleable, was used in the present investigation. Early in 1948 after the work of this paper: was completed Campbell, Jaffee, Blocher, Gurland, and Gonser6 described the strength and working characteristics of pure titanium which was prepared by the iodide method on a scale producing 300 to 600 g per run, in the form of 0.3- to 0.4-in. diam rods. Their product is characterized by low hardness and large capacity for cold work which they attribute to a high degree of purity with respect to oxygen, nitrogen, and carbon. Titanium has a melting point of about 1725°C5 it may be classed as a light metal since the specific gravity is 4.5 g per cc-1. The crystal structure is close-packed hexagonal from room temperature t0 885°C. Above this temperature the structure is reported7 as body-centered cubic. The change in crystal structure has been associated with discontinuities in specific heat8 electric resistance9 and thermoelectric force10 at temperatures near 890°C. It is reported11 that annealed titanium has a tensile strength 0f 78,700 psi which can be increased by cold-work to 123,000 psi. In the present investigation, the lattice constants at room temperature, the thermal expansivity between 30 and 800°C, as well as the electrical resistivity and thermoelectric force against platinum between - 200 and 1000°C have been determined. MATERIALS For the measurements, two series of specimens were prepared from titanium furnished by the U. S. Bureau of Mines. The first was lade from an annealed sintered compact, 0.38 in. thick. Sections of the compact were cold-swaged with intermediate anneals in vacuum to the sizes used. Sizes over 0.25-in. diam were annealed at 1000°C and smaller sizes at 800°C. Specimens originating from the sintered compact are designated in this paper as A. The second series of specimens was lade from a rod of titanium, 0.19 in. in dial, which was cold-swaged with the necessary intermediate anneals to the required sizes. This series of specimens is designated B. The impurities in the specimens of titanium, determined by chemical analysis, are given in Table I. Oxygen and nitrogen which were not determined by analysis, are probably present although in small quantities in view of the ductility of the material.

Jan 1, 1948

By S. F. Reiter, W. R. Hibbard

A survey of the effect of heat treatment on the room temperature hardness of Fe-Mo alloys has been made. Constant strain rate tensile tests were performed between room temperature and 1800°F. These data were analyzed to determine the effect of temperature and composition on the strain hardening coefficient and strain rate sensitivity. Constant load creep-rupture tests were made on these alloys and the results related to composition and structure. A relation between the high temperature strength of the precipitation hardened alloys and the volume of precipitate has been observed. IN view of the extensive use of ferritic materials at elevated temperatures, it is surprising to note the limited amount of information relating the variables of plastic deformation, i.e., composition, structure, temperature, stress, strain, and strain rate. Hollomon and Lubahn' showed how the several variables of plastic flow might be treated analytically. No data were available on carbon-free iron and its alloys in a form suitable for this analysis. Several German investigations2-" constitute most of the experimental work relating high temperature properties to the constitution of these types of materials. In order to obtain new data, the iron-rich alloys of the Fe-Mo system were selected for detailed investigation for the following reasons: 1—Some of the important effects of molybdenum on the mechanical properties of iron have already been studied.' , 821 2—By suitable heat treatment of selected alloys, it is possible to study strengthening effects of four types: AT -a transformation, B—substitutional, C—precipitation, and D—dispersion of hard inter-metallic compound. Materials and Treatment Four-pound ingots were vacuum cast, employing the same melting schedule previously used.? The raw materials were electrolytic iron and lamp-grade molybdenum. The ingots were forged to l/z in. sq. rod and one portion swaged to 0.350 in. diam rod for the production of 1 15/16 in. long button-head specimens. The button-head specimen blanks were solution treated for 16 hr at 2100°F in hydrogen of —70°C dewpoint and then water quenched. They were subsequently plunge ground to the standard 0.160 in. diam test bar. Micrographs of the solution treated alloys are given in Figs. la through Id. The higher molybdenum alloys contained large equiaxed ferrite crystals similar to those in Fig. Id. A portion of the % in. rod was hot rolled to 0.100 in., sandblasted, and cold rolled to 0.020 in. Strip tensile specimens having a 0.020x0.200 in. cross-section and a 2.25 in. gage length were machined from the sheet. The alloys containing molybdenum were subsequently annealed 1 hr at 1560°F. The iron strip was annealed 4 hr at 1300°F in wet hydrogen. The resultant structures are shown in Fig. 2a through h. The ASTM grain sizes were 1 to 3 as solution heat treated or 3 to 4 as annealed. The chemical analyses of the alloys are given in Table I. Carbon contents were obtained after the heat treatments in hydrogen. Alloy 15.9 pct Mo was tested as a cast alloy.'

Jan 1, 1956

By Edward E. Hicke, Charles A. Stickels

The dihedral angle of liquid-lead inclusions in solid nickel has been measured as a function of temperature from 371 to 816 C at zero pressure. and as a function of pressure up to 50,000 psi at 317 and 593 C. Thermodynamic expressions are derived for the temperature and pressure coefficients of interfacial tensions in this system. A method is presented for obtaining relative tempmature and pressure coefficients from dihedral-angle data, and the resulting values are used in conjunction with the thermodynamic relations to calculate excess properties of the solid-liquid interface. Defining the position of the solid-liquid interface by the condition that the excess concentration of lead is zero, the excess concentration of nickel and the excess entropy at the solid-liquid interface are: where y(593) is the interfacial tension of the nickel grain boundary saturated with lead at 593C and zero pressure. These values are considered reliable to within a factor of two. While similar calculations are not possible for the nickel grain boundary, it is shown that the expwimental results imply that the excess concentration of nickel at the boundary and the excess entropy of the boundary are negative. THE temperature and composition dependencies of interfacial tensions in metal systems have been reported by several authors in the last 15 years.'-' No measurements of the effect of pressure on inter- facial tensions in metals have been reported, although measurements made on nonmetallic gas/liquid and liquid/liquid systems suggest that a measurable effect should exist.6-l2 The purpose of these experiments was to determine the influence of temperature and hydrostatic pressure on dihedral angles in the Pb-Ni system. The equilibrium dihedral angle is expressed as a ratio of interfacial tensions by2: where 8 is the dihedral angle, yGB is the Ni-Ni grain boundary tension, and SL is the solid Ni-liquid Pb interfacial tension. Three sets of ex- periments were run to determine: a) the effect of temperature from 371" to 816°C on the dihedral angle at zero pressure; b) the effect of pressure up to 50,000 psi on the dihedral angle at 371° and 593°C. THERMODYNAMICS The properties of interfaces of most direct concern are the interfacial tension, excess concentrations of various components at the interface and the excess entropy of the interface, S°. These quantities are defined following Gibbs. Consider an interface separating phases a and 0. Construct two surfaces C, and C such that all properties of phase a remain uniform up to C, and all properties of phase 0 remain uniform up to C. The region between C, and Cp is the interfacial region. Let a "dividing surface", D, be constructed in the interfacial region such that it passes through all points "similarly situated with respect to the condition of the adjacent matter."l3 Surface D divides the interfacial region into a portion a' adjacent to phase adjacent to phase . Let a closed curve, C, enclose an area A in D. Erect normal lines to D along C; these lines and the surfaces C,, Cp, and D then enclose volumes V and V' in the two halves of the portion of the

Jan 1, 1964

By C. D. Rubert, W. J. Parton

A flotation plant was placed in operation in 1945 at the Tamaqua colliery of the Lehigh Navigation Coal Co. Inc., to recover fine anthracite which is discharged from the cleaning plant with the washery water.‡ In addition to the recovery plant, facilities were provided for the complete clarification of the washery water, recirculation of this clarified water for breaker use, and disposal of the refuse solids in a waste impounding dam. Fig I shows a view of the settling tanks and the flotation plant. Flow Diagram The flow diagram for the complete recovery project is given in Fig 2. All the waste water from the cleaning plant is collected in a sump A outside the breaker structure, from which a 7000 gpm pump B delivers it through a 16 in. line to a 75-ft diam hydroseparator C. The hydroseparator, acting as a classifier, is set to give a separation at approximately 200-mesh. The minus 200-mesh overflow is discharged by gravity into the 180-ft thickener D for final settling of the solids. The classifier underflow sludge is pumped to the flotation plant by a 6-in. quadruplex diaphragm pump E. A 10-ft diam hydroseparator F is used to make a second classification on the sludge solids at approximately 28-mesh. The underflow from this classifier containing the coarse particles is elevated by a 6-in. diaphragm pump G and is discharged on two 4- by 6-ft vibrating screens II. These screens are dressed with approximately 28-mesh cloth. Screen oversize product flows directly to the centrifuge that dewaters the cleaned froth. The screen underflow and the overflow from the 10-ft classifier flow to the flotation circuit. The flotation feed is conditioned in a 12 by 12-ft agitator tank J at a pulp density of I:2.33 (30 pct solids). Reagents are fed to the circuit by reagent feeder I. The conditioned pulp is then diluted to a pulp density of approximately I: 5 (18 pct solids) and is fed to two banks of four 100-cu ft froth flotation cells K for primary coal recovery and cleaning. Additional reagents from reagent distributor L are added to the feed weir-box of Nos. 2, 3, and 4 cells of each bank of flotation machines. Clean coal removed from these cells flows directly to the clean-coal sump. Dilute tailings from the primary cells is re-thickened in a 30-ft diam thickener M and is then retreated in a scavenger circuit for final recovery of coal. The scavenger circuit consists of a 6- by 6-ft agitator tank N and two banks of four 24-cu ft froth flotation cells 0. Coal froth from these cells flows to the dewatering equipment and the tailings flows to a vertical refuse pump which delivers it to the 180-ft diam waste thickener D. Dewatering of the coal products is accomplished in a 54- by 72-in Bird centrifugal filter P. The cake product is dropped onto a conveyor and is loaded

Jan 1, 1949

By Michael Bradbury

INTRODUCTION A major change in financing exports in recent years has been the decreased importance of subsidized export credits, following the commitment of the OECD countries to eliminate the subsidy element. Subsidized export credit rates are now often more expensive than market rates as the financing for exporters has decreased in volume and importance. The forfait market, in recognition of this decreasing importance, provides a rapidly expanding source of nonrecource finance for exporters. The following is a step by step guide to what it is, how it works, its benefits and problems. WHAT IS FORFAITING? Forfaiting is not new. It has been used in Europe for about 25 years to provide export finance for both capital goods and commodities without recourse to the exporter. Although long the preserve of exporters in Germany, and more lately Italy, forfaiting is now used increasingly by exporters in Great Britain, the United States, Canada and Scandinavia. It is a fairly simple operation with easy straight-forward documentation. The transaction involves the purchase by the forfaiting bank of a bill of exchange or a series of bills without recourse to the exporter. These bills will have been drawn by the exporter, accepted by the importer, and will usually bear the unconditional guarantee of the importer's bank. They are normally drawn payable at intervals during the credit period agreed between importer and exporter and are purchased at a discount by the forfaiter. The exporter thus obtains his cash payment and the importer receives his credit period. The forfaiter collects the amount of the bills as they mature directly from the importer. Credit periods vary, depending upon the type of goods and the country and commercial risk of the importer. The period is generally between one and five years with six monthly maturities. The usual forfait currencies are US dollars. Deutschmarks and Swiss francs and others, such as sterling, French francs, and the Scandinavian currencies are being used more frequently. CHOOSING FORFAITING Most types of financing require the continued involvement of the exporter in the financial side of the transaction during the credit period. Forfaiting has certain comparative advantages. In particular, it is possible to forfait 100 percent of the risk without recourse to the exporter, unlike government sponsored export finance schemes, where some retention of the risk by the exporter is required. In addition, exports from country sources do not present problems and forfaiting can also cover trade within the EEC. Other benefits for the exporter are: (a) The exporter's balance sheet is improved; debts are turned into cash thus improving the liquidity of the company and enhancing its cash flow. And there are no contingent liabilities for bills of exchange. (b) If the sales contract is in a foreign currency forfaiting removes the risk to the exporter of adverse movements in foreign exchange during the credit period. (c) Fluctuations in interest rates during the credit period can be ignored since in forfaiting the transaction is usually done on fixed interest rate terms on a discount basis. (d) The political and transfer risks are taken by the forfaiter. (e) The commercial risk is taken by the forfaiter. (f) The costs of administration and collection etc. during the credit period are removed.

Jan 1, 1985

By F. W. Glaser, W. Ivanick

A pressure-sintering method was used to produce binder-free and very dense TiC specimens. Some physical properties of these TIC bodies were determined and found to compare favorably with those of certain cemented Tic grades. It was also observed that the hot transverse rupture strength of TiC bodies remained substantially the same regardless of the amount or type of binder material used. STUDIES of the structure and physical properties of refractory materials have been intensified recently because of the urgent need for nonstrategic materials that retain their strength at high temperatures. Research aimed at determining and improving the physical properties of cemented carbides and borides has been accelerated with a view toward possible use of such materials in connection with turbine blades, rocket nozzles, and other high temperature applications. On the hypothesis that the strength requirements in connection with some of the above applications could be met only by proper choice of cementing agents for such refractory materials, the literature describing the physical properties of borides or carbides was reviewed. However, with a few exceptions,'-" references were found only to compositions containing at least one or more auxiliary binder metals. Cobalt and nickel are among the most frequently employed cementing agents. The melting point of Tic (approximately 3250°C) and therefore the sintering temperature, at which notable densification of a cold pressed Tic powder compact could be expected in the absence of a liquid binder phase, is relatively high. The present study makes use of a high temperature, pressure-sintering procedure, recently described by one of the authors in connection with the sintering of binder-free ZrB,," to produce dense bodies of sintered Tic—free of any cementing agent. During the course of this sintering study, some physical properties of dense Tic bodies produced by this method will be discussed. Materials, Preparation of Samples, Testing Methods The procedure for the forming of Tic powder consisted of mixing graphite and TiH, powders in stoi-chiometric proportions, and heating this mixture in a H, atmosphere and carbon crucible by high frequency, to temperatures ranging between 1900° and 2100°C (3452" and 3812°F). The powdered carbide was then comminuted and screened to the desired particle size. Table I shows the chemical analysis of the two grades that were employed for the production of samples during this work. Bodies of Tic, approximately 2.5xlx0.5 cm were produced in graphite molds that were heated by direct conduction. Sintering was carried out at temperatures for time intervals ranging from approximately 0 to 30 sec under a constant pressure of about 1.3 tons per sq in. An alternate method for the production of samples consisted in cold pressing the individual Tic grades at pressures ranging from 4 to 10 tons per sq in. and sintering in a hydrogen atmosphere in graphite crucibles heated by high frequency induction. Sintering temperatures ranged from 2600° to 2900°C (4715° to 5255°F). Electrical testing was done by measuring potentiometrically the voltage drop over a length of 1.5 cm for a current of 10 amp at room temperature. Cross-sectional areas as well as densi-

Jan 1, 1953

By S. S. Solomons, V. H. Tillmann, L. Smaniotto

INTRODUCTION The Zinc Corporation, Limited and New Broken Hill Consolidated Limited (ZC/NBHC) mines are situated at Broken Hill, New South Wales, Australia (refer Fig. 1). Both companies are wholly owned subsidiaries of Australian Mining and Smelting Limited (AM&S). Annual production from both mines is 2.3 million tonnes of lead, silver and zinc ore mined by a variety of underground methods. From 1911 to 1968, conventional overhand cut and fill stoping (both open and square set timber) was used almost exclusively, though some trials with shrinkage and sublevel stoping were undertaken. The trial stopes used short holes in conparison with today's sublevel open stopes. Mechanised cut and fill methods with regular rockbolt support were introduced in the early 1960's and undercut and fill stoping replaced square set timber stoping for pillar extraction in the late 1960's. Since 1968, increasing emphasis has been placed on longhole open stoping (LHOS) although some areas of the orebodies are comrnrnitted to the abovemehtioned methods since existing stope development makes it impracticable to change. In 1979, approximately half the total production was mined by LHDS and it is expected that the LHOS proportion will increase in the future. A vertical crater retreat method of longhole mining has also been successfully introduced to replace the undercut and fill stoping of some pillars and it is expected that this stoping method will be used in some future primary ore extraction. This paper reviews the progress of LHOS technology at ZC/NBHC with emphasis on the stope planning and design process and the importance of rock mechanics applications. The objective has been to maximise the primary extraction of the orebody giving due consideration to stability and safety. This has led to the design of a novel sloped wall longhole stoping method which should eliminate the formation of pillars by mining the orebody in a "continuous" manner incorporating a sloped sand interface between the blocks of ore being mined and the previously mined sandfilled stope. The expected results include the complete extract of the orebody without the formation of pillars and with minimal dilution of ore with sandfill. The evolution of the method can be best illustrated by following the mining progress of the relatively new Southern 'B1 Lode orebody at the NBHC mine. GEOLOGY Southern '8' Lode is the southern extension of the 'Bt Lode orebody, which is currently being mined further to the north in ZC/NBHC (refer Fig. 2). The ore block being developed and stoped extends for a vertical height of 90 metres from No. 17 level down to approximately ten metres above No. 19 level. The ore minerals are sphalerite and galena with the zinc:lead ratio averaging approximately 3:l with a minor amount of silver associated with the galena. There is a sharp contact between the ore and the country rock on the footwall and keel, while the hanging wall gradates into medium and low grade material. The gangue is primarily quartz together with garnet, biotite, feldspar, gahnite, sericite and minor apatite. In various horizons within the orebody, grey feldspar, quartz and garnet pegmatites occur as stratiform layers. The ore and country rock are competent with some inconpetent boundaries.

Jan 1, 1981

By W. C. Ellis, E. S. Greiner

Metallic titanium has been prepared in small quantities since the beginning of the century. Hunter1 reported in 1910 that he obtained a malleable product of 99.9 pct purity by the reduction of the tetrachloride by sodium in a closed container. Later Van Arke12 and Fast prepared small quantities of malleable titanium by thermal decomposition of titanium iodide. Another method for producing malleable titanium from tetrachloride was reported by Kr0ll4 who used magnesium as the reducing agent. More recently Dean, Long, Wartman, and Anderson5 working at the U.S. Bureau of Mines have reported the preparation of the metal on a pilot plant scale by the reduction of titanium tetrachloride by magnesium in an atmosphere of helium. Their product, which is malleable, was used in the present investigation. Early in 1948 after the work of this paper was completed Campbell, Jaffee, Blocher, Gurland, and Gonser6 described the strength and working characteristics of pure titanium which was prepared by the iodide method on a scale producing 300 to 600 g per run, in the form of 0.3- to 0.4-in. diam rods. Their product is characterized by low hardness and large capacity for cold work which they attribute to a high degree of purity with respect to oxygen, nitrogen, and carbon. Titanium has a melting point of about 1725 C," it may be classed as a light metal since the specific gravity is 4.5 g per cc-I. The crystal structure is close-packed hexagonal from room temperature to 885°C. Above this temperature the structure is reported7 as body-centered cubic. The change in crystal structure has been associated with discontinuities in specific heat,8 electric resistanceg and theimoelec-tric force10 at temperatures near 890°C. It is reportedll that annealed titanium has a tensile strength of 78,700 psi which can be increased by cold-work to 123,000 psi. In the present investigation, the lattice constants at room temperature, the thermal expansivity between 30 and 800°C, as well as the electrical resistivity and thermoelectric force against platinum between — zoo and I000 C have been determined. Materials For the measurements, two series of specimens were prepared from titanium furnished by the U. S. Bureau of Mines. The first was made from an annealed sintered compact, 0.38 in. thick. Sections of the compact were cold-swaged with intermediate anneals in vacuum to the sizes used. Sizes over 0.25-in. diam were annealed at I000°C and smaller sizes at 800°C. Specimens originating from the sintered compact are designated in this paper as A. The second series of specimens was made from a rod of titanium, 0.19 in. in diam, which was cold-swaged with the necessary intermediate anneals to the required sizes. This series of specimens is designated B. The impurities in the specimens of titanium, determined by chemical analysis, are given in Table 1. Oxygen and nitrogen which Were not determined by analysis, are probably present although in small quantities in view of the ductility of the material.

Jan 1, 1949

By W. A. Backofen, G. Mayer

Single crystals of iron, copper, and a Cu-7 wt pct A1 alloy were pulled through conical dies to simulate the constraint in a polycrystalline aggregate undergoing axisymmetric reduction. With Taylor-type hardening, dependence of the drawing stress, od, on the Taylor orientation factor, M, is predictable from the polycrystal stress-strain curve; in particular, for a power-law relationship, it should follow that d log od/d log M = (1 + n). A first-order agreement with analysis was found in the data from iron. For copper, the implied n from the observed d log od/d l°g M was -0, while for Cu-7Al it was negative. The trend was in the direction of random polycrystal behavior. Thus the idea of hardening only in response to the amount of prior slip loses validity as stacking fault energy (SFE) is lowered. Two possible explanations have been suggested: as stacking fault ribbons are widened, barriers from dislocation reactions become increasingly effective in dispersing slip and reducing the orientation dependence of the total glide strain dm that appears in alternatively, or conjointly, the polyslip shear stress, 7, acquires an orientation dependence of a kind which has the same leveling effect on M. The problem of relating the strain hardening of polycrystalline material to that of an isolated single crystal is still largely unsolved. In a new experimental approach from recent work, single crystals of different orientations have been deformed under the constraints found in an aggregate while measuring their deformation resistance. Procedures have involved drawing cylindrical crystals through conical dies1 and compressing slab-shaped crystals in plane strain.2'3 Predictions for the outcome of such experiments were made first by Taylor~ and later, in more general form, by Bishop and Hill.5'6 Taylor's example was the axisymmetric extension of an fcc crystal slipping on the usual {111}(110) systems or, equivalently, a bcc crystal undergoing 'kestricted" slip on {110}(111). In his solution, the deformation work supplied was equated to that dissipated internally in slip on all active systems. With o the single applied tensile stress, dc the resulting axial strain, and dyT the total glide strain on systems operating at resolved shear stress, 7: The orientation dependence of M was found by minimizing dyT for each orientation while activating five independent systems, Fig. l(a).? The Bishop and Hill analysis, based on a principle of maximum work, leads to essentially the same conclusion; the need for at least five active systems is recognized in the finding that either six or eight are actually brought into operation. The mean value from the entire stereo-graphic triangle in either case is M - 3.06. More recently, Hutchinson8 made a Taylor-type analysis for pencil glide in a bcc structure, from which piehlerg prepared Fig. l(b) as the counterpart in Fig. l(a); here M = 2.75. The obvious weakness in such analyses is the indifference to slip-system interactions. A condition of what might be termed "independent"

Jan 1, 1969

By John J. Curzon

The existence of mineralized ground in the area near Lake Chelan has been known since 1887, when Major A. B. Rogers, a locating engineer for the Great Northern Railway, came up Lake Chelan to Railroad Creek in search of a pass over the Cascade Mountains. The steep mountainsides near the crest of the Cascades proved too difficult for railroad construction, and the project was abandoned. Upon his return to Seattle, Major Rogers apparently told his friends, the Denny family, about the large, red, oxidized patches he had seen on the valley walls along Railroad Creek. The Dennys, being true pioneers in spirit, grubstaked J. H. Holden to explore the area and to stake any promising mining ground, and thus began the chain of events that culminated in the construction of the plant that is now known as the Chelan Division of the Howe Sound Company. Holden staked the first group of claims in 1892. Soon afterward, A. H. Murdock, who was then a storekeeper in Chelan, and who is still living at Waterville, and his partner, W. P. Robinson, staked adjacent ground. These two groups of claims formed a substantial part of the mining property being worked today. During the period from the original staking in 1892 up to 1928, when the Britannia Mining and Smelting Co. optioned the property, many attempts were made to bring the property into production, through the formation of several stock companies and by examination and testing by engineers from several well-known mining companies. Although the Britannia organization optioned the property in 1928, not much was done until 1930, when a subsidiary was formed—the Chelan Copper Mining Co.—to explore further the possibilities of the ground. Some work was done during the next few years, but it was not until March 1937 that the Chelan Division of the Howe Sound Co. took over with a program of "full speed ahead," and active development of the mine and construction of the complete plant was begun, including docks, tug and barges, 54 miles of power line, 11 miles of road, mill, shop buildings and complete camp. Production began in April 1938, and has continued without interruption, except for regular change days and holidays and a six-weeks strike in 1939. This interval of time has seen the gradual evolution of a mine and mill originally planned for a rate of 1000 tons per day into a compact operation that last year averaged 2264 tons per operating day. This operation, although rather small when compared with the large copper producers of the Southwest, is important to the state of Washington for several reasons: It has provided employment for several hundred people continuously since construction days in 1937; it has helped materially in the war effort, through production of vital copper and zinc, without which no war can be won; and last, but not least, it has conclusively refuted the old pessimistic arguments that a successful mine would never be found in the Cascade Mountains of Washington. The Holden mine has been producing

Jan 1, 1946

By John C. Calhoun, Alfred Chatenever

An exploratory study wap made to examine the possibilities of a visual approach in investigations into microscopic mechanisms of fluid behavior in porous media. Appropriate apparatus and techniques were developed so that microscopic phenomena could be recorded on color movie film as well as be observed visually. The observation flow cells in which tlie fluid behavior studies were made were essentially single-layered matrices of spheres between plates. sometimes all-glass, sometimes all-Lucite and sometimes a combination of the two. The fluids were limited to water and a filtered crude oil. Two flow regimes were observed during the flow of the immiscible liquids: channel flow and slug flow. In the former, transport was effected through stable networks of interconnecting channels; and in the latter, part of the movement took place in the form of slugs. Under certain conditions, flood-front patterns were found to be different depending upon which liquids were the displacing and displaced phases and not depending upon whether the matrix was water-wet glass or oil-wet Lucite. Residual formations of oil and water were observed and are described. Some of the ramifications and significance of the ohservetl phenomena are discussed. INTRODUCTION In recent years considerations of microscopic mechanisms of fluid flow in porous media have taken on greater significance. Much needs to be learned before the fundamentals of petroleum technology are completely established. For example, many unanswered questions exist in connection with relative permeability, displacement phenomena, residua! fluid formations. flow structure, etc.; and further analytical mathematical formulations are seriously indicated. It is hoped that systematic investigations into the microscopic mechanisms connected with the behavior of fluids in porous media will shed some light on some of the problems extant. Until recently microscopic mechanisms have been considered almost exclusively as speculative hypotheses. Within the past few years, however, the problem has been submitted to a limited number of experimental investigations. Nuss and Whiting' made some studies on the pore-space geometry of sandstones and limestones by impregnating cores with an inert plastic and leaching the solid matrices to leave behind plastic models of the pore spaces. SchaeferZ traced pore spaces microscopically through lengths of limestone cores by cutting away thin sections from the exposed faces normal to the line of view. In 1949 two projects were organized in which dynamic flow phenomena were examined microscopically to uncover microscopic mechanisms. One was set up at the Pennsylvania State College where Lowmanb bserved heterogeneous fluid flow phenomena in capillaries. The second was the American Petroleum Institute Research Project 47B at the University of Oklahoma where microscopic studies of dynamic fluid phenomena in synthetic porous matrices have been made by visual observation and cinephotomicrography.' It is with the latter that this paper is concerned. treating the techniques involved and the observations made. TECHNIQUES Observation Flow Cells The observation flow cells formed a focal point in the techniques employed. Essentially, these were matrices composed of a single layer of spheres sandwiched between two flat plates. This design was arrived at after a series of pre-

Jan 1, 1952

By J. Serra, M. Turpin, R. Alberny

A new method is proposed to obtain automatically an unbiased estimate of the interdendritic spacing A. It is shown that the structure can be built by a random distribution of a rectangular basic unit. The usual definition of the interdendritic spacing yields a value 1 which, coupled with A, gives the shape of the basic rectangular unit. A study of the relationship between dendrite arm spacing and solidification rate was conducted as a part of a research program on dendritic solidification. For any comparison between theory and experiments to be meaningful, it is necessary to measure reproducible and clearly defined spacings. Fig. 1 shows clearly that even in a fairly simple structure such measurements are difficult. if we compare photos (a) and (b), we can hardly assess which one shows the larger spacing. Moreover, the quantity to be measured can be defined in several ways. On a small scale, dendrites seem to be distributed in a very regular and ordered way. However, on a larger scale, this regularity no longer exists. The usual way to measure spacings is to pick up some rows of dendrite stalks; such measurements are obviously biased since less orderly regions are not taken into account. A more objective method is to section the picture with randomly oriented straight lines and average the measured interdendritic spacings. The purpose of this paper is to show that such measurements, which can be conducted automatically, yield objective and reproducible results which are directly related to characteristic features of the dendritic structure. I) THEORETICAL ANALYSIS 1-1) Mathematical Morphology and Function of Co-variance. Matheronl and Serra2 enlarced- the definition and geometrical meaning of the notion of covariance to encompass problems in mathematical morphology. A brief review of part of their theory can be stated as follows. Let A' be an isolated particle, and let us consider a group of two scanning points h is the vector joinlng these points, h its modulus, and a its direction. Let us also define a boolean function, k(x), whose value is 1 if x lies inside the particle and 0 if it 1s outside. The total number of events in which both points are inside A' IS the covariance Ii',(h): is the measure of the intersection of A' with the particle ALh obtained by translating A' of -h Obviously K,(O) is the volume of the particle A', or its area if A' is a two-dimensional body. The average value of K,(h), when the direction of a vector h of constant modulus is rotated, is: An important property of the covariance is illustrated on Fig. 2: if the shape of a particle shows some regularity along a direction a, K,(h) generally presents a maximum. We now consider a group A, made of many particles A' distributed in space; then k(x) is taken as the realization of a stationary random f~nction.~ The volume fraction (or fraction of area if the problem is two-dimensional) occupied by A equals the average value q of k(x): meaning "average value of"). We also replace

Jan 1, 1970

By K. A. Johnson, F. H. Ellinger, C. C. Land

The Pu-In phase diagram has been determined by thevmal, filtvation, micrographic, and X-ray diffraction methods. This alloy system is characterized by 1) limited solubility of indium (-2 at. pet) in 6 and e plutonium, 2) one eutectic, and 3) fizte intermediate phases. Of the latter, PuIn and PuIn3 melt con-gruently, and Pu31n, Pu31n5, and the high-temperatuve 7 solid solution are formed peritectically. The n phase decomposes eutectoidally into Pu3In and PuIn at 865°C. Although the 6 phase can readily be retained to room temperature, it is not thermo-dynamically stable below 300°C. The Pu-In system has been investigated at Los Alamos as part of a study of the alloys of plutonium with the group 111-B elements. Constitutional studies of the Pu-A1 and Pu-Ga systems have been reported earlier.'9' To date, published information on the constitution of Pu-In alloys covers only the identification of the intermediate phases Pu3In and PuIn3.3,4 EXPERIMENTAL The alloys were prepared from five different lots of plutonium and three different lots of indium. The principal impurities in the plutonium differed from lot to lot within the following limits (in ppm): iron, 30 to 80; nickel, 30 to 60; aluminum, 15 to 30; silicon, 20 to 145: thorium, 50 to 300; carbon, 75 to 335; and oxygen, 20 to 135. Spectroanalysis of the indium showed that two of the lots were 99.9 wt pct pure, and the third was 99.98 wt pct pure. The alloys, in the form of about 5-g buttons, were prepared by arc melting in conventional equipment. The components for each alloy were weighed to the nearest 0.1 mg. In most instances the weight losses during melting were negligible; therefore confirmatory chemical analyses were usually not made. A few results are given in Table I. Density measurements of the arc-cast buttons were made by the liquid displacement of bromoben-zene. Heat treating was done in muffle furnaces controlled to +2°C. The alloy buttons were wrapped in tantalum foil before being enclosed in evacuated clear silica capsules. As a precaution against breakage, each capsule was in turn placed in a silica tube closed with a refractory wool plug prior to being charged into the furnace. For a moderately fast quench of the alloys, the outer protection tubes containing the capsules were plunged into cold water. Differential thermal analyses (DTA) in racuo were performed at heating and cooling rates of about 1.5°C per min. Tantalum crucibles having inverted thermocouple wells were used for most of the analyses. It was found micrographically, however, that the liquid alloys containing more than about 35 at. pct In reacted with the tantalum, resulting in contamination of the surface of the alloy. A search for a more satisfactory crucible material was not successful: tungsten and yttria behaved comparably to tantalum; thoria, vitrified magnesia, and vitrified alumina severely contaminated the alloys. So as to minimize the contamination by the crucible mater-

Jan 1, 1965

By G. B. Craig, H. E. Rosinger, W. J. Bratina

NUMEROUS studies have been reported on how the mechanical properties of a bcc metal are affected by interstitial solute atoms in the temperature range where appreciable diffusion occurs in finite time. Only recently, though, has work on an "interstitial-free" iron been reported, this by Leslie and sober,' on an Fe-0.15 pct Ti alloy. The data was limited to a maximum temperature of 296°K. This work presents a systematic study of the flow stress and the activation volume of a similar material as a function of plastic deformation over the temperature range 253" to 473°K. The material studied was Ferrovac E iron containing 0.01 wt pct C and 0.0002 wt pct N annealed at 870°C for 1 hr, and the same iron with an addition of 0.15 wt pct Ti annealed at 870°C for 80 hr; cooling rates being 75°C per hr. In the latter alloy depletion of interstitials in the a-iron matrix associated with the second phase formation was expected. The temperature dependence of the flow stress was measured at 6 = 3.33 x 10-5 sec-1 from 253" to 473°K as a function of the deformation in 0.01 intervals from 0.03 to 0.12 strain. Results for two strains, 0.03 and 0.09 are shown in Fig. 1. The flow stress increased and reached a maximum in the Ferrovac E iron with increasing temperature, but showed a consistent gradual decrease in the Ferrovac E-0.15 pct Ti alloy. A yield point and Luders region, observed in Ferrovac E, was absent in the Ferrovac E-0.15 pct Ti alloy. Also, the Ferrovac E exhibited a serrated stress-strain behavior in the temperature range 330" to 400°K; dynamic strain-aging characteristics were absent for the titanium alloy. The activation volume was determined over the same temperature range by the method of stress relaxation at constant strain. Results are shown in Fig. 2. At the temperatures of serrated stress-strain behavior in Ferrovac E the activation volume was found to increase toward infinity and, as the temperature rose, to decrease, to about 100 to 200 v/b3. By contrast, the activation volume for the Ferrovac E-0.15 pct Ti alloy tended to increase continuously from the initial value of approximately 300 at 300°K to more than 800 at 473°K. Above 400°K, then, the corresponding activation volume values of Ferrovac E were less than that of the Ferrovac E-0.15 pct Ti alloy. The activation volumes, Fig. 2, appear to depend on dislocation-interstitial interaction in Ferrovac E and on dislocation-dislocation interaction in Ferrovac E-0.15 pct Ti alloy. The gradual increase in the latter metal is associated with thermally activated motion of dislocation segments.' The decrease of the activation volume in Ferrovac E above 400°K is probably related to the diminishing effect of interstitials on dislocations. Here, the interstitials can be moved along with a dislocation without appreciable drag. As indicated in Fig. 1, removal of interstitials

Jan 1, 1970

• One effect of the British devaluation of the Pound Sterling, with its resultant lowering of the pay limit, was the addition of considerable tonnages of previously marginal ore in gold mining. Crown Mines, Ltd., reported that 1,245,000 tons of such ore had been added to available reserves. But for devaluation, a steady decline in ore reserves had been a feature of operations during the previous ten years, and would have continued. •Loree Colliery of the Hudson Coal Co. is using a Humphrey spiral cleaning plant to meet requirements of the state in the matter of stream pollution. However, the process is producing a salable product. •Noranda is considering plans for constructing a commercial sized unit designed to produce elemental sulphuric acid and sintered iron oxide from pyrite. Test plant results have indicated the No. 5 ore zone can be treated by the new process economically. •A magnetic fluid clutch, and magnetic amplifiers for motor and generator control, have been developed under Navy contract by Vickers' Electric Division, in St. Louis, Mo. This constitutes the first commercial production of the clutch recently developed by the Bureau of Standards. •Fuel experts estimate coal production will run up to 500 million tons this year based on the expectation that business conditions will continue to be good. They also expect that in the future the use of coal will increase by 50 pct over today's level. These expectations are based on the fact that it provides the bulk of the heat, light, and power for making steel, for manufacturing, and for generating electricity as well as the development of the coal burning gas turbine and processes for making gas, gasoline, and oil from coal. •Entombed miners may benefit from a two-way communication system which utilizes the earth's strata as a network for electric signals. The use of FM radio waves makes this possible. The invention includes a portable transmitter-receiver unit kept near the face, and a more powerful portable equipment of the same sort above ground. In use, two probes on wires from the apparatus are driven into the earth. • The Union of South Africa has launched a uranium production project which government leaders think will help the West maintain world atomic supremacy. Experiments under way in the pilot plants are expected to lead to the establishment of a chain of processing factories along the Witwatersrand in which uranium will be reclaimed from gold tailing. •Recent developments in mechanized mining at the Bureau of Mines oil-shale mine near Rifle, Colo., have lowered mining costs to 29 cents per ton of shale. The cost of producing crude shale oil from 30-gal-per-ton-shale, using the new mining and processing techniques, would be about $1.50 per barrel. This is 500 lower than any previously stated price. • COMINCO is planning to open the old Bluebell lead-zinc mine near Nelson, B. C., on a 500-ton-per-day basis. The old workings will be pumped and a 970-ft incline sunk. A mill will be constructed at the property.

Jan 7, 1950

By Robert M. Dreyer

Although lateritic ore deposits are relatively flat-lying, surficial ore bodies, the evaluation of lateritic bauxite and nickel deposits is among the most difficult problems confronting an economic geologist. Laterite is a soil formed under tropical conditions resulting in the concentration, within the soil zone, of certain trivalent metals - principally iron and aluminum, but also, locally, nickel and manganese. The soil zone is divided into two parts: (a) the true soil or lateritic zone and (b) the zone of partially altered bed rock or saprolite. Whereas bauxite generally is confined to the lateritic zone, some nickel deposits occur in both the laterite and saprolite zones. The evaluation of bauxite and lateritic nickel deposits thus has both similarities and differences. These ores have been formed by supergene, soil-forming solutions moving downward through zones of widely varying permeability within the weathering rock. Because the permeability varies widely, both vertically and laterally. the extent of weathering may vary greatly within short distances. Because the weathering process varies widely, the degree of metal concentration may also vary widely. It is not at all uncommon for a laterite to change, within a few centimeters, from a virtually valueless rock to a high grade ore. Moreover, the depth of weathering, and hence the depth and form of the ore profile, vary greatly. Obviously, for this type of deposit, a few grab samples or a few drill holes are virtually worthless. The evaluation of such a deposit requires a sophisticated statistical study based on thousands of carefully selected samples. As a rule of thumb, the cost of evaluating a large bauxite or lateritic nickel deposit will be about one cent per ton of ore in the ground. Thus, the cost of evaluating a several hundred million ton deposit may be considerable. The following factors must be considered during the evaluation: Type of Sampling: The best and most reliable samples for the evaluation of lateritic ores are taken along large, vertical channels in hand-dug pits. Where labor costs are high, some form of drilling may be used in place of pitting, but it is always wise to choose a drilling procedure after checking drilling results against a series of pit channel samples. The drilling may not reproduce exactly the results from pit channel samples, but it may be possible to derive a constant correction factor. If the physical character of the laterite varies within the deposit, it may, of course, be necessary to change the type of drilling, the correction factor or both. In some areas, it has been found empirically that augers, chum drills, vacuum drills, rotary drills, or core drills yield satisfactory results. The problem is to find which drilling technique gives results most similar to channel samples through the heterogeneous sequence characterizing the laterite in a given area. In lateritic nickel deposits, the drilling characteristics of the lateritic and saprolitic portions of the deposit are very different. Within the saprolite, the major nickel values are commonly found in weathered zones within less altered boulders - a type of occurrence which makes sampling very difficult.

Jan 1, 1979

By J. D. Meakin

J. D. Meakin (The Franklin Institute Laboratories)— In a recent paper Garofalo12 has shown that a number of experimental creep results can be represented by the empirical relation In this expression ? is the steady creep rate, s is the applied stress, and A is a constant at a given temperature; a and n are adjustable parameters. Garofalo has shown that Expression [6] approximates to a power function at low stresses and a simple exponential function at high stresses. Among the data used by Garofalo are the results we published for creep of copper." For these results we found that the best correlation was an exponential law with different parameters in the low-and high-stress region, respectively. That is, i = A exp qs where A and q have different values above and below a critical stress a,. In Ref. 13 are listed a variety of observations which support the proposal that different mechanisms are operative at stresses above and below a,, and it is not felt appropriate to repeat those observations here. The purpose of this note is to demonstrate that, although the representation used by Garofalo does fit the experimental data very well, this fit cannot be used to conclude that only one mechanism is rate-controlling. The argument is best made graphically and is illustrated in Fig. 9. The continuous curves 2 and 3 represent pairs of simple exponential functions which intersect at i = 10-5. The curve 2 closely resembles the copper results in that a change of slope of 2:1 occurs at i = 10-5; the two functions shown are in fact: e = 10-7 exp (1.150) and ? = 10-6&apos; exp (0.576s) For purposes of comparison, curve 3 represents two exponential functions with a change of exponent of 3:1 and curve 1 has the exponent 1.150 throughout. It is quite clear that a satisfactory straight-line fit is obtained on a Garofalo plot for all three curves. The curves represent processes which have either a single stress exponent or two ex- ponents in a ratio as high as 3:l. It must, therefore, be concluded that the ability to obtain a linear dependence between log i and log (sinh cyo) cannot be taken as evidence for a single activated process. In fact, to some extent the way the experimental points quoted by Garofalo lie about a best fit straight line on the log (sinh as) plot indicates that two processes are indeed occurring. This is seen in Figs. 7(c) and 8(c) of Ref. 12 where it is particularly evident that the experimental points deviate from the straight line in a manner similar to curves 2 and 3 of Fig. 9. It is, of course, recognized that the generally used exponential form is an approximation to the hyperbolic sine function which is not valid for exponents of less than 1.2, e.g., qs < 1.2. The only curve in Ref. 12 which is affected by this restriction is Fig. 6(b) where the deviation from a In ? vs s

Jan 1, 1964

By R. D. Longyear

[Some Problems Involved in the Interpretation of Diamond-drill-hole Sampling and Surve ing (paper by J. J. Collins, Mining Tech., Jan. 1946). ............... I Geologic Interpretation of Magnetic Exploration on the Mesabi Range, Minnesota (paper by R. H. B. Jones, Mining Tech., July 1946) ................... 2] DISCUSSION R. D. LONGYEAR.*-Mr. Collins is to be commended very highly for the brief summary he has made of the currently used methods of taking diamond-drill sludge samples and the principles involved in evaluating the results. This paper should stimulate further discussion and research on this vitally important problem. It is particularly imperative that geologists and engineers know when assay results on sludge recovery can be accepted quantitatively and when they must be considered only qualitatively. In most cases where the sludge recovery is less than 95 per cent or more than 125 per cent, it is safest to consider the assays as of qualitative value only. Certain cases, however, are known where a relatively small proportion of the sludge sampling will give a reasonably accurate measure of the value of the total sample. One such case is ore in which the valuable mineral is of approximately the same specific gravity as the waste mineral, such as chalcopyrite in a massive pyrite body. The essential point is to determine the degree of accuracy of sludge sampling in any given drilling project and to weigh the results accordingly. It should be emphasized, however, that sludge sampling can be made reliable in many localities where careless practice produces unreliable results. In many instances, it is desirable to empty the core barrel in the core shack instead of at the drill, so that the engineer can examine the core as it first comes from the core barrel. It should be pointed out, however, that the drill * E. J. Longyear Co., Minneapolis, Minnesota. runner should be permitted to study the core to guide his future drilling. It is hoped that with the return of more normal conditions after the war geologists, engineers, contractors, and manufacturers will be able to carry on more research along the lines of improved core-barrel design and drilling technique with the objective of increasing core recovery so as to eliminate as far as possible the necessity of relying upon sludge samples. H. M. ROBERTS.*-Whoever in the future will have to do with the search for ore bodies and their exploration will have frequent occasion to refer to the clear and comprehensive summary on diamond-drilling methods by John Collins. His review of the experience of the last 40 years in this technique is invaluable. As Dr. L. D. Ricketts wrote in 1932, "The principles on which an art is founded are usually few and necessarily basic in nature, but he who wishes to achieve the power to select his aides and give success to important undertakings that may be intrusted to him in the future must ordinarily undergo years of drudgery in order to gain the experience that will enable him to distinguish such fundamentals through the haze of reinforcing detail that clothes and tends to disguise them."[t] Ricketts went on to say that since the beginning of the century there has been much

Jan 1, 1946

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