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US 4,201,749-In the Bayer process production of alumina wherein aluminum hydroxide is precipitated from a sodium aluminate solution for use as seed, sodium oxalate and caustic components are removed from the precipitate by washing it first with a washing liquor which is saturated with sodium oxalate but has little content of caustic, and secondly with hot water. Substantially no sodium oxalate is recycled, yet loss of sodium aluminate is minimal. K. Yamada, T Harato, and H Kato, assigned to Sumitomo Aluminum Smelting Co Ltd May 6, 1980 8 pp. (423-127). Filed. 5-8-79 (37,145) Priority. Japan, 5-8-78 (53/54,803). Same¬British 2,020,642, dated Nov. 21, 1979.

Jan 1, 1982

Discussion of the paper of G. P. Hulst, presented at the Salt Lake meeting, August, 1914, and printed in Bulletin No. 92, August, 1914, pp. 1865 to 1871. L. S. AUSTIN, Salt Lake City, Utah.-One question that I would like to ask is in regard to the sampling kettle which stands beside the softening furnace. How is the sample taken or melted? G. P. HULST.-The sampling kettles in question are of 45 tons capacity and are fired with coal. The lead bullion comes in on a high line in car-load lots of 30 to 40 tons. The entire lot is trucked from car, weighed over scales and thrown into the sampling kettle, which has been previously cleaned. The kettle is fired and the bullion melted, then heated up until no frozen bullion' remains in the .bottom or adheres to the sides of the kettle. The kettle is scraped clean, sides and bottom, and the wet dross is skimmed Doff clean into molds. The kettle is stirred thoroughly during the period in which 24 to 30 samples of approximately ½ assay ton are taken. These samples are taken in a long-hand loci iron mold, providing for taking six to eight "gumdrops." The mold is inserted and heated to the same temperature as the molten metal, and gumdrops are clipped out and cooled in the mold by dipping 'the bottom of. the mold into Water. The samples should be free from fins. The gumdrops represent the contents of the kettle, and in assaying, they should not be clipped, but weighed up and the result computed. The dross bars are weighed and sawed according to old hammer and punch sample template. The sawdust represents a sample of the dross. In eases of high gold in the bullion there is a slight correction in the assay. This method of sampling was developed at the Omaha plant of the American Smelting & Refining Co., W. T.. Page, Manager, in 1903 or 1904, for adjusting differences in checking smelter sampling. L. S. AUSTIN.-The base bullion which you treat is very clean. It has been remelted, and skimmed before shipment. How rapidly can you get it through the softening furnace, and how does it compare with ordinary base bullion? G. P. HULST.-Twenty-four hours is the softening limit on these charges. In other words, it is charged into the furnace, heated up, and the first and second skimmings are taken off, and it goes into the kettle the next day; that is, 24 hr. elapse from the time the bullion is charged to the time it is in the kettle. L. S. AUSTIN.-It seems to be a long time to hold such a pure bullion. I suppose, though, it comes around conveniently so that you have a time for all the other operations of refining. Isn't that the case? MR. HULST.-Every refinery is based on those principles.

Jan 11, 1914

By K. L. Young

The general energy equation, including change in kinetic energy, was solved by numerical integration and used to evaluate simplifying assumptions and application practices over a wide range of conditions. When extreme conditions were encountered, sizable errors were caused by large integration intervals, application of Simpson's rule and neglecting change in kinetic energy. A maximum error of only 1.31 percent was caused by assuming temperature and compressibility constants at their average value. It was discovered that a discontinuity can develop in the integral for the injection case. This discontinuity indicates a point of zero pressure change and is an inflection point in the pressure traverse. INTRODUCTION When a pressure in a gas well is to be calculated, one of the first decisions is to select a method of calculation. In many instances, this selection becomes a problem because the literature, at best, provides an evaluation of any method for only a limited range of conditions. Once a method has been selected, a question often arises as to the size of the calculation interval which should be used. The question regarding calculation interval arises because an analytic solution is not obtainable and approximate solutions must be used. This paper presents an evaluation of major assumptions and application practices of probably the two most widely used methods for calculating steady-state single-phase gas well pressures. The two methods are Cullender and Smith1-" (numerical integration), and average temperature and com-pressibility. The Cullender-Smith method assumes that change in kinetic energy is negligible and is normally applied in two steps with a Simpson's rule correcton. The average temperature and compressibility method, in addition to neglecting kinetic energy change, asumes that temperature and compressibility are constant at their average values. This method is normally applied for wellhead shut-in pressures of less than 2,000 psi, and in one step. Computer programs were written to compute bottom-hole pressure with and without the assumptions, using various approaches. Values of input parameters investigated are shown in Table 1. Flow rate was limited to a maximum of 5,000 and 10,000 Mcf/D for tubing sizes of 1.610 and 1.995 in. ID, respectively. Flow rate was also limited to 10,000 Mcf/D for a tubing size of 2.441 in. ID when wellhead flowing pressure was 100 psia. These limitations were imposed on flow rate so as not to exceed sonic velocity. The z factor routine available necessitated limiting bottom-hole temperature to 240F and wellhead pressure to 3,000 psia. Pressures were compared on the basis of percent deviation from the trapezoidal integration of Eq. l or 2 at 100-ft intervals. A preliminary investigation indicated that a 1,000-ft interval solution would differ from a 50-ft interval solution by less than 0.25 percent; therefore, the 100-ft interval was chosen for a base. For the purpose of comparison, deviations less than 1 percent were considered insignificant. where 111.1 qeC2/d p = kinetic energy term. Eqs. 1 and 2 can be evaluated numerically at specific depths using the trapezoidal rule as shown by Cullender and Smith. If change in kinetic energy is neglected and temperature and compressibility are assumed constant at their average values, Eq. 1 can be integrated to give the average temperature and compressibility equation,

By Y. C. Liu

THE existence of mechanical twins in bcc metals has long been known. With recent intensive interest in the mechanism of twin formation and its role in plasticity and crack initiation, a study of the general Characteristics of twin intersection appears pertinent. The scope of the present note will be limited to the crystallography of the twin intersections of (112) twins, without consideration of its mechanism, movement of atoms, crystal structure, or the strain energy involved at such an intersection. The twinning elements of (112) twins are considered to be K1 = {112}, n1 = (111) and K2 = {112}, n2 = (111) with a twin shear of 0.707. The crystallographic features of twin intersections have been worked out in detail by Cahn.1 The present work applies the general principles postulated by Cahn to the intersections of (112) twins. The basic conditions for the twin intersection are: 1) The trace of crossing (A) and the secondary (C) twins in the planes of the crossed twin (B) must be parallel. 2) The direction (n1) and magnitude (s) of shear must be identical in the crossing and secondary twins. Also the sense of shear must be the same. These two conditions have to be fulfilled in order to maintain geometrical continuity at the twin interfaces. Fig. 1 shows the perspective representation of how these two conditions are fulfilled at the intersection. This type of intersection will be named Type-I. It is the purpose of this note to point out the existence of another type of intersection, Type-II, as shown in Fig. 2. In this type of intersection, the crossing twin A remains straight and the crossed twin B has been bent. The two conditions laid down by Cahn must also be met. This leads to the following corollary conditions: 1) The interface between twins B and C must be parallel to the twin habit of crossing twin A. 2) n1c must be parallel to n1A. 3) The twin shear (s) of twin C must be exactly equal to and in the same sense as that of crossing twin A. Thus, in order for the Type-II intersection to take place, the twining elements of secondary twin C must fulfill the above three conditions with respect to crossing twin A. Let K1 of crossed twin B be (112). All indices of the matrix can therefore be converted into new in-

Jan 1, 1963

By S. E. Maddigan, B. R. Zimmerman

Most metallurgists are well acquainted with the contributions already made to the study of metals by the use of X-rays. On the one hand, the radiographic method is constantly becoming of increasing importance as a nondestructive testing procedure, while on the other hand the techniques of X-ray diffraction have made important contributions to the fundamental knowledge in studies of phase diagrams, stress conditions, and so forth. A new, and as yet insufficiently appreciated, tool exists in the application of microradiography to alloy structures. This new procedure in many respects bears the same relation to microscopic investigations as does macroradiography to the gross inspection of metal surfaces. However, where macroradiography is used ordinarily to determine the soundness of the metal structure, this new method can be used not only to investigate micro-un-soundness but also to examine the distribution of the constituent elements within the body of the alloy. When combined with the normal procedures of microscopy, this offers a technique of great potential power. It is intended in this paper to present a few examples of copper-base alloys demonstrating the additional knowledge obtained from the microradiographic method. The detection of micro-unsoundness is demonstrated in Fig. I for a sample of cartridge brass as cast. The sample ap- peared quite sound when viewed under the microscope, but in reality was thickly populated with minute voids. This application of the method conforms in every way to conventional large-scale radiography and has been used to facilitate production of metal for vacuum devices.' The true potentialities of the technique are revealed by comparison of Figs, 2a and 2b, which are respectively a photomicrograph and a microradiograph of a cast alloy of 80 per cent Cu, 10 per cent Sn, 10 per cent Pb. The remarkable difference in appearance provides some concept of the additional information this method may yield when used as an auxiliary to microscopic studies. Fig. 2a shows two phases of the copper-tin system plus segregated_ lumps of lead. Fig. 2b, on the other hand, shows with exceptional clarity the actual dendritic growth of the metal crystals during solidification. The practice of microradiography depends upon the laws of absorption of X-rays. This subject has been reviewed thoroughly in recent papers,l,2,3 but for clarity a brief resume will be given here. As is well known, when a beam of X-rays is transmitted through a, layer of homogeneous material, the intensity is reduced according to the relation: where Il is the transmitted intensity, I0 is the incident intensity, µ1 is the linear absorption coefficient of the material, t1 is the thickness of the material.

Jan 1, 1944

By S. E. Maddigan, B. R. Zimmerman

Most metallurgists are well acquainted with the contributions already made to the study of metals by the use of X-rays. On the one hand, the radiographic method is constantly becoming of increasing importance as a nondestructive testing procedure, while on the other hand the techniques of X-ray diffraction have made important contributions to the fundamental knowledge in studies of phase diagrams, stress conditions, and so forth. A new, and as yet insufficiently appreciated, tool exists in the application of microradiography to alloy structures. This new procedure in many respects bears the same relation to microscopic investigations as does macroradiography to the gross inspection of metal surfaces. However, where macroradiography is used ordinarily to determine the soundness of the metal structure, this new method can be used not only to investigate micro-un-soundness but also to examine the distribution of the constituent elements within the body of the alloy. When combined with the normal procedures of microscopy, this offers a technique of great potential power. It is intended in this paper to present a few examples of copper-base alloys demonstrating the additional knowledge obtained from the microradiographic method. The detection of micro-unsoundness is demonstrated in Fig. I for a sample of cartridge brass as cast. The sample ap- peared quite sound when viewed under the microscope, but in reality was thickly populated with minute voids. This application of the method conforms in every way to conventional large-scale radiography and has been used to facilitate production of metal for vacuum devices.' The true potentialities of the technique are revealed by comparison of Figs, 2a and 2b, which are respectively a photomicrograph and a microradiograph of a cast alloy of 80 per cent Cu, 10 per cent Sn, 10 per cent Pb. The remarkable difference in appearance provides some concept of the additional information this method may yield when used as an auxiliary to microscopic studies. Fig. 2a shows two phases of the copper-tin system plus segregated_ lumps of lead. Fig. 2b, on the other hand, shows with exceptional clarity the actual dendritic growth of the metal crystals during solidification. The practice of microradiography depends upon the laws of absorption of X-rays. This subject has been reviewed thoroughly in recent papers,l,2,3 but for clarity a brief resume will be given here. As is well known, when a beam of X-rays is transmitted through a, layer of homogeneous material, the intensity is reduced according to the relation: where Il is the transmitted intensity, I0 is the incident intensity, µ1 is the linear absorption coefficient of the material, t1 is the thickness of the material.

Jan 1, 1944

By George W. Lower, William A. Hockings, Donald A. Kaczynski

The rate of dissolution of polycrystalline metallic copper in aqueous cupric ammonium nitrate solutions in the non-film-forming region was investigated by the rotating disc method. The investigation was performed in solution concentration ranges applicable to hydrometallurgical processes. This investigation was an extension of a study on the cupric ammonium carbonate system previously reported by Smith, Lower and Hockings, in which the following kinetic model was proposed: (1) Diffusion of cupric ammine ions to the copper surface; (2) Forward reaction - first order reaction of cupric ammine ions with metallic copper; (3) Reverse reaction - disproportionation of cuprous ammine ions to metallic copper and cupric ammine ions ; and (4) Diffusion of cuprous ammine ions from the copper surface. The nitrate system was selected for this study because it simplified the determination of the ionic composition of the solutions. The variables studied were stirring speed and cupric, ammonia, and nitrate concentrations. The dissolution rate increased linearly with at low values of but exhibited increasingly negative deviations from linearity at higher values of m. The rate also increased with increasing cupric concentration but decreased with increasing ammonia and nitrate concentration. Good agreement was obtained between the experimental rate data and the proposed model. Further verification of the model was indicated by the close agreement of the diffusion coefficient calculated from the data and comparable literature values.

Jan 1, 1974

By H. Biloni, G. F. Bolling

The microsegregation in tin specimens containing 0.2, 0.5. or 1 wt pct Pb has been studied m detail. The specimens were grown from the melt in a controlled fashion and exhibited a well-developed cellular substructure. In general, a severe microsegre-gation can be observed in all the photomicrographs presented. Some observations of special interest are: the distribution of a second phase, the presence of a eutectic in several forms, the evidence for dif- THE Smialowski or cellular substructure which forms during solidification has been extensively studied during the past decade.'* Many of the im- *Most references to the cellular substructure except for the last 2 years are reviewed by Winegard.' portant characteristics of this substructure, such as its occurrence and variability with growth conditions, its association with the phenomenon of constitutional supercooling, and its effect on dislocation production and mobility, have received quantitative fusion of solute in the solid, and the enhancement of segregation at a dislocation subboundary network ("striations"). On the basis of the metallographic observations, it can be deduced that the segregation observed is representative of the solute segregation produced during crystal growth. Some deductions are also made about the interplay of the two substructures, cells and striations, and about the mode of cellular growth. investigation both experimentally and theoretically. However, the concentration profile of the solute segregated during crystal growth has not been examined in detail. Tin crystals grown from melts containing various concentrations of lead have been most extensively studied. In a recent investigation of Sn-Pb alloys, Kramer et a1.2 were able to measure the effective solute distribution coefficient, k,, at the most advanced points of the solid-liquid interface, over a large range of growth conditions, finding it to approach the value of k,, the equilibrium distribution coefficient. As will be shown, this must lead to drastic segregation. Another recent study of several Sn-Pb alloys was made by Plaskett and winegard3 who investigated the variation of growth conditions

Jan 1, 1963

By AIME AIME

FOR the purpose of subsequent discussion let me reiterate certain points in my paper. The things we are certain of are that individuals differ in their accident liability, and that the bulk of accidents in any industrial group is sustained by comparatively few individuals; further, that this difference in liability cannot be wholly accounted for by differences of exposure, since some of the personal factors involving a high accident rate have already been measured in certain industrial groups.

Jan 1, 1929

By Nicholas J. Grant, Robert H. Kane, Bill C. Geissen

The platinum-rich section of the Ta-Pt Phase diagram was worked out by metallographic and X-ray techniques, using twenty alloys; solidus temperatures and solid solubilities were determined. Besides s phase, four intermediate stoi-chiometric phases were found: TaPt (high-temperatzrre phase, structure unknown); TaPt2 (ortho-rhomhic, new type); a TaPt3 (orthorhombic, TiCu3 type); ß TaPf3 (monoclinic, new type). TaPt2 and TaPt3 melt congmentlv; two eutectic, two beritec-tic, and one eutectoid reactions occur in the inuestigated range. THE Ta-Pt system was examined as part of a study of the phase diagrams and the intermediate phases of niobium and tantalum with Group VIII transition metals. Since the main scope of this work was the relation among the ordered close-packed phases occurring in the concentration range from AB to AB3 (A = Nb, Ta; B = Pd, Pt, and so forth), only the platinum-rich side of the diagram was worked out thoroughly, while spot checks were made to determine the approximate outline of the tantalum-rich portion. The system has not been thoroughly treated in the literature; Greenfield and Beck1 in their survey of refractory metal intermediate phases found a o phase between -18 and 37 at. pct Pt which coexists at higher platinum concentrations with an unidentified intermediate phase. Browning2 worked on the range between 55 and 100 at. pct Pt; however, this preliminary study did not cover temperatures >1500°C, and included no conclusive crystallo-graphic data. More recently, a study of the platinum-rich section of the Ta-Pt system has been carried out by Ray,3 while Hartley, Parsons, and steedly4 have studied the tantalum-rich section. The crystal structures of TaPt2, a TaPt3, ß TaPt3, and others have been reported in abstracted form by Giessen and Grant.5 EXPERIMENTAL METHODS The methods of alloy preparation and processing and of the metallographic and X-ray procedures follow very closely those described by Ritter, Giessen, and rant' for other refractory metal-noble metal systems, and will not be repeated except where significant differences exist. Starting materials were: tantalum rod of 99.95 pct purity, supplied by National Research Corp., and platinum sponge 99.9 pct, supplied by The International Nickel Co. An oxygen analysis of the tantalum rod showed 30 ppm O; other impurities were C, N, Si, Nb, Mo, none of these exceeding 50 ppm, and 100 ppm W. Homogeneous buttons were readily prepared as follows: ingots of 5 g were weighed and arc-melted under welding grade argon, followed by two remelts after inverting the button. Between 40 and 100 at. pct Pt, weight losses during the first melt rarely exceeded 0.1 pct, in which case the alloy was rejected, and were nil on subsequent remelts. Since the vapor pressure of platinum far exceeds that of tantalum, the small evaporation loss could be assumed to consist of platinum; therefore, a corresponding amount of platinum was added on the second melt. Since it was confirmed on pure tantalum samples that no weight gain through oxygen or impurity pickup occurs (see Ref. 71, it could be assumed that the uncertainty in the composition did not exceed ±0.1 at. pct for the range 40 to 100 at. pct Pt. For the four control melts from 0 to 40 at. pct Pt, an error of ±0.5 at. pct was calculated. Microscopic examination of the whole buttons after melting showed no inhomogeneity other than local coring. This was eliminated by a homogenization heat treatment. A total of twenty-three alloys were prepared. Heat treatments were carried out in a tantalum

Jan 1, 1965

By A. M. Gaudin, T. P. Meloy

This paper presents the theoretical derivation of the distribution equation for single fracture. The equation is shown to accord with experiment. Several empirical size-distribution equations have been proposed to describe the size of broken materials. Among them are the Gaudin-Schuhmann equation and the Rosin-Rammler equation.3*4 The Gaudin-Schuhmann equation relates the relative fraction of undersize to relative size —. In this relationship Mo is the total weight of crushed sample, M(x) the weight of undersize contained, x the size considered, K a quantity called the size modulus, which together with the slope parameter, m, characterizes the product. The slope parameter is usually close to unity. The Rosin-Rammler equation relates the same relative fraction of undersize to the relative size modulus by an equation of different form In this relationship, e is the base of natural logarithms. In the fine size-range when m is unity both equations give Gilvarry and Berstrom have sought a size distribution equation having a sound theoretical basis. They have come to an equation taking into account the effect of volume, surface and edge flaws in fragmentation. If the effect of the volume and surface flaws is neglected, the equation taking only edge flaws into account has the form of the Rosin-Rammler equation. In the present paper, a theoretical size-distribution

Jan 1, 1962

By Fred R. Harris

INTRODUCTION MacMillan Tungsten is located in northwestern Canada on the border of Yukon and Northwest Territories at a latitude of 63º17' and altitude of 1800 m above sea level. The deposit lies within the Selwyn Mountains 10 km from the Canol Road. It is 660 km by road from Whitehorse, Yukon, and 1325 km by air from Vancouver, British Columbia. MacMil lan Tungsten is a contact metasomatic deposit in gently dipping Lower Paleozoic limestone and limestone breccia adjacent to a Cretaceous quartz monzonite stock. Four tabular tungsten skarn horizons contain total geological reserves of 30 million tons grading 0.9% WO3. DISCOVERY AND HISTORY J.F. Allan, a former AMAX geologist, located mineral claims in September, 1962, to cover the source of scheelite-bearing skarn float found in the headwaters of Cirque Lake Valley. Exploration work on the property conducted mainly between 1968 and 1973, includes geological mapping, 10,500 m of diamond drilling in 73 holes, and 735 m of underground exploration. Mil 1 tests were carried out on a 300 ton bulk sample obtained underground. Preliminary feasibility studies, collection of weather data and a variety of environment studies have been carried out since 1973. Although no production date has been set MacMillan Tungsten will undoubtedly be a major tungsten producer.

Jan 1, 1976

By John V. Beall

As recently as 1964, the situation in the Australian iron ore industry was chiefly one of potential. The only producer was the Broken Hill Pty. (BHP). That company mined about 5 million tpy from deposits in the Middleback Range in South Australia and at Yampi Sound in Western Australia. No ore was exported from Australia. Now, just five years later, and after expenditures amounting to approximately one half billion dollars, BHP and seven new companies exported about 15 million tons (long tons) of iron ore and pellets as well as meeting Australia's own annual requirements of approximately 8.5 million tons of ore. Early this year, the volume of iron ore on order stood at 328 mil- lion tons to be delivered over a period of 15 years, but Cliffs Western negotiations for sale of Robe River iron ore have boosted the volume to the new high of 466 million tons. All of this has meant a great deal to Australia in terms of new income. In fiscal year 1967 (ending June 30, 1967) exports of iron ore amounted to $52 million; in 1968, $128 million and by 1'972 the Bureau of Mineral Resources expects the value of exports from iron ore to reach $242 million. In achieving the position of major- supplier of iron ore to the Japanese steelmakers, it was necessary to build a great many new facilities, mostly in Western Australia. Three railroads, 70 miles long, 182 miles and 265 miles were constructed. A new port was created at Dampier; Port Hedland was deepened and otherwise improved; both of these ports are in Western Australia. In Tasmania, Savage River developers built an offshore shiploading station that has received the recognition of engineers internationally. At least a half dozen new communities have been founded. The narrow gage railroad from Kalgoorlie to Perth and Freemantle was replaced with a standard gage line.

Jan 6, 1969

By G. U. Greene

The various lead producers have given the subject of lead drosses much attention in recent years but the problem of their economical treatment is yet to be solved. Formerly the copper in the furnace feed was removed from the furnace in the form of matte. The speiss at that time consisted principally of the iron arsenide. The practice today is to roast off most of the sulphur and the copper in the feed forms a dross in the furnace, which is removed from the furnace with the lead. This material is poured into the drossing kettles and allowed to cool down to but slightly above the freezing point of lead. The copper dross, containing almost all of the arsenic and part of the antimony, is skimmed off and treated in a small reverberatory furnace at most plants. This is essentially a liquation process. The skimmed dross contains from 70 to 80 per cent lead, and much of this lead is liquated out. The products from this treatment are: (1) impure lead, (2) speiss and (3) matte. The speiss from the reverberatory furnace was studied in this research. The literature on the subject is of very little assistance, as almost no work has been done on the problem of establishing the exact identity of the various phases present. One author(1)† states that speiss consists of a series of isomorphous compounds of the general formula FexAsy in which the Fe may be replaced by Ni, Co, Cu, Pb, Ag, Au, Pt, Zn, Cd and the As replaced by Sb, S and Bi. Hofman(2) states that the iron arsenide present is Fe5As. Experimental Work In the present research, the author used for methods in an attempt to determine the composition of the various phases: (1) chemical, (2) microscopic, (3) roentgenographic and (4) thermal. Previous to this research, considerable time had been spent making analyses of different speisses, but unfortunately no very definite conclusions could be made as a result of these analyses.

Jan 1, 1937

By R. McEwen, G. W. Hansen, G. F. Lee

The effect of using an anionic collector, Reagent 308, a sodium petroleum sulfonate, with a cationic collector, Armac T, a tallow, fatty acid amine acetate, was studied in a series of monomineralic flotation trials with the alkali feldspars and heavy minerals, ilmenite, rutile, garnet, and monazite. This combination of cationic and anionic collectors is employed to float feldspar and heavy minerals from quartz in the beneficiation of sand in Normanville, South Australia, to produce a suitable quartz sand for glassmaking. In the alkali feldspar trials, Armac T additions were held constant, while the 308 additions were varied. In the heavy mineral trials, the 308 was held constant while the Armac T was varied. Peak enhancement of the feldspar recovery was noted when the 308 additions were between 25% and 150% that of the Armac T additions. At higher 308 addition, depression of feldspar flotation occurred. This appears to be due to a neutralizing effect in the combined collector system and to the formation of a nondissociating complex of both collectors. This variability in flotation response when Armac T is used with 308 suggests that the two collectors do not act independently of each other.

Jan 1, 1977

By H. L. Talbot, A. J. Hall, R. S. Young

A method for the chemical differentiation of oxidized cobalt from sulphide cobalt in complex mine and concentrator products is of considerable interest to a number of mining companies throughout the world. At Rhokana Corporation, in Northern Rhodesia, for instance, cobalt is found chiefly in the sulphide form, as carrollite, but a cobalt oxide mineral also occurs irregularly underground, and relatively small quantities in the mill feed from time to time are difficult to detect visually at the concentrator. The oxide cobalt is not amenable to the sulphide flotation process used at Rhokana and nearly all of it passes into the tailing. The occasional period when high tailing losses occur with no appreciable change in the cobalt content of the mill feed has naturally been disturbing to the concentrator staff, who had no means of determining whether an influx of cobalt oxide ore or laxity on the part of the mill flotation operators as responsible for these results. A procedure for determining oxidized copper minerals, based on their solubility in dilute sulphuric acid saturated with SO2, has been used for many years in the copper industry. In the presence of cuprite the procedure fails, but otherwise it gives results quite satisfactory for control pur- poses. Empirical methods for determining oxidized forms of zinc and lead have been proposed, but they are generally unsatisfactory except in isolated cases of a very simple ore. No published procedure for determining oxidized forms of cobalt or siinilar elements has come to the authors'notice. Experimental Procedure There are obviously two alternatives in attacking a problem of this nature. One is to employ a solvent for oxide cobalt that will not dissolve cobalt sulphide. The other is to find a substance capable of oxidizing the cobalt sulphide to sulphate, which of course is water-soluble and can then be leached from the water-insoluble oxide cobalt. A representative sample of Rhokana cobalt oxide ore was secured, ground to minus 200-mesh, and carefully rolled to furnish a standard sample for this work. The analysis of this material gave the following percentages: Co, 0.55; Cu, 1.64; Fe, 2.98; S, 0.08; SiO2, 41.42; Al2o3, 11.20; CaO, 13.82; MgO, 3.80. As a source of cobalt sulphide a similar large sample of carrollite was prepared, analyzing Co, 23.36 per cent; Cu, 27.32; and S, 31.13. This sample of course was not pure carrollite, but was the best obtainable in quantities sufficient for a standard intended for considerable work. It was a pure sulphide sample, microscopic examination showing only carrollite, a little bornite, and gangue, with no visible sign of oxidized ore present. A wide variety of reagents as used in an effort to selectively dissolve oxide cobalt or to oxidize sulphide cobalt to

Jan 1, 1949

"Power is transmitted to Butte, a distance of 130 miles, over two separate lines running parallel on the same right of way.The transmission line embodies the most approved ideas in construction. The conductors are No. O. B. & S. gauge, hard drawn copper strand. The insulators are of the suspension type, each insulator consisting of six units, 10 inches in diameter. The insulators will stand a wet test of over 300,000 volts, and were selected after long and careful tests by the company's engineers. The wires are carried on steel towers of four-legged, single crossarm type, manufactured by Milliken Bros. The three conductors are suspended in a horizontal row from the crossarm, and there are no transpositions in either line. Above the power wires and symmetrically located are two galvanized steel strands, Vs-inch in diameter, grounded at each tower, which serve as a protection against lightning.The distance between towers in level country is 600 feet. In mountainous country, however, the spans are irregular in length and spans of 1,500 or 2,000 feet are common. The longest one in the line is that crossing- the Missouri River and is equal to 3,034 feet. The length of this span is such that a person standing at one end of it can sec the wires go off and vanish into space, while the tower at the other end is barely visible to the naked eye on a clear day. The towers at one end of this span arc shown in the accompanying photograph. The line starts at an elevation of 3,200 feet, rises to an elevation of 8,200 feet as it crosses the Continental Divide, and again descends to 6,100 feet, the elevation at Butte.Quantity of coppc1· in transmission line, 1,330,000 pounds.Number of towers, 2,-1-00.Steel used in construction, approximately, 2,-1-00 tons."

Jan 1, 1913

By Raymond C. Boettner

The present work had for its purpose: 1) the identification of crack nucleation sites in AISI 4340, quenched to martensite and tempered over a range of 'temperatures; and 2) the comparison of fatigue processes in AISI 4340 with processes observed previously in pure metals From constant def1ection-bending fatigue tests, martensite boundaries were identified as the favored crack nucleation sites in quenched and tempered AISI 4340. It, also, was concluded that the fatigue processes operating- in this lous-alloy steel were similar to Processes observed in pure tnetals. ALTHOUGH much engineering data has been accumulated on the fatigue properties of quenched and tempered martensitic steels,' fatigue as a process is not as well understood in martensite as it is in pure metals.' Important features of the fatigue process, such as the identity of the nucleation sites, have not been determined in the commercially important high-strength low-alloy structural steels. The present work had for its purpose: 1) the identification of crack nucleation sites in a low-alloy steel, i.e., AISI 4340, which had been quenched to martensite and tempered over a range of temperatures; and 2) the comparison of fatigue processes in the AISI 4340 with processes observed previously in pure metals. This comparison of the fatigue processes in the different tempers was restricted to the high-strain low-cycle part of the S-N curve. Under these test conditions, previous work on a number of metals has shown that a large number of cracks are nucleated in less than 30 pct of the fatigue life.3 Furthermore, crack nucleation sites are not restricted to inclusions but are also associated with intrinsic structural characteristics of the metal. MATERIAL A 20-lb ingot of vacuum-melted AISI 4340 (for composition see Table I) was hot-rolled to 1-in.-diam rod and then cold-rolled to a 1-in.-wide strip, 0.08 in. thick. Fatigue specimens, see insert of Fig. 1, were machined from the strip with the long dimension parallel to the rolling direction. m this orientation, the stringers of 1 to 2 p inclusions present in the sheet lay parallel to the stress axis in the specimens. The specimens were austenitited at 2050°F in order to obtain a large prior austenite grain size, i.e., 2 mm, which facilitated the subsequent identification of the prior austenite boundaries. A helium atmosphere was used to minimize decarburization. After austenitiza-tion at 2050°F, the specimens were transferred to a 1450°F furnace so that specimen distortion was held to a minimum in the subsequent oil quench. Previous work4 indicated that refrigeration in liquid nitrogen prior to tempering reduced the percentage of retained austenite in the quenched specimens to less than 5 pct. Tempering was carried out in air over the temperature interval of 200°to 800°F to produce a range of mechanical properties, Table I. The preparation of the fatigue specimen was completed by grinding about 0.005 in. from each surface and electropolishing in a chrome trioxide-acetic acid solution for 30 min. Examination of etched cross sections of specimens prepared in this fashion showed the foregoing specimen preparation to be adequate for the removal of the decarburized layer present after the heat treatment. Transmission electron microscopy showed that the as-quenched microstructure of this alloy consisted of a mixture of martensite plates containing either a high density of dislocations or microtwins. Previous work5'6 indicated that in the course of oil quenching autotem-pering resulted in the formation of E carbide on the martensite and microtwin boundaries. Tempering for 2 hr at temperatures up to about 400°F resulted in further precipitation of the E carbide. Finally, at about 400°F, cementite began to replace the E carbide on the martensite and microtwin boundaries in addition to forming a Widmanstatten structure within the plate matrix. EXPERIMENTAL S-N curves were obtained using electropolished specimens cycled at 1800 cpm as cantilever beams in fully reversed bending at selected constant deflections. The deflections were translated into surface strains by means of a calibration curve obtained through the use of strain gages. An argon atmosphere was used to minimize environmental effects. To investigate the development of fatigue slip bands, the specimens of the different tempers were unidirec-tionally bent to a surface strain of 0.005 to 0.007, photographed to record the location and appearance of slip bands so introduced, and then cycled to failure

Jan 1, 1968

By N. N. Breyer

A specially built "hard" tensile machine with characteristics permitting the precise detertnination of the drop of the load at the yield point has been used to study the magnitude of the yield-point phenotnenon in prestrained martensitic 4340 steel. A new phenonzenon, the appearance of a secondary yield point, has been observed by holding the specimen at constant strain in the plastic region. Furthermore, it has been found that a series of yield-point drops could be introduced by successive constant strain holds in the plastic region. The isothermal kinetics of the development of the secondary yielding point lave been studied at four temperatures: 24° 0° -18°, and -79°C. From the results of the kinetic investigation, equations for the In a previous investigation1 it was shown that, contrary to generally held opinion, steels of medium carbon content, such as 4340, 4140, and 86B30, in the as-quenched martensitic condition, can be cold-drawn through a die with reductions in area of up to 10 pct without cracking. Tensile specimens of 4340 machined from bars quenched and prestrained in this manner exhibited tensile strengths of about 400,000 psi coupled with 30 pct reductions in area. In addition, it was found that each sample of such steels exhibited a yield point in the quenched, cold-drawn condition. Since these studies were conducted on a commercial hydraulic testing machine of a type which is not well-suited to detailed study of yield-point behavior, it was decided to study this phenomenon more thoroughly on a rigid straining machine. In this new investigation, use of such a "hard" machine not only allowed study of the magnitude of the yield-point drop but also revealed a new phenomenon—secondary yielding of the martensite introduced by stopping crosshead motion after plastic deformation of the sample had begun. The present paper is a report of these findings. MATERIALS AND PROCESSING The material used was a commercial 4340 steel of the composition shown below: 0.41 0.80 0.013 0.019 0.31 0.85 1.76 0.28 1 0.42 0.77 0.015 0.024 0.30 0.84 1.69 0.28 0.08 2 1 = Ladle analysis. 2 = Laboratory analysis. Bars of this steel were processed in the following way: 1) machined to predetermined diameters; 2) austenitized at 870°C for 1 1/2 hr; 3) oil-quenched; 4) cooled to -115°C for 1/2 hr; onset and increase in magnitude of the secondary yielding in this temperature region have been found to fit the relationship ?Ys = Atn where ?Ys is the magnitude of the secondary yield Point in psi, t is the time in seconds, and A and n are parameter characteris-tics of the material. Although the occurrence of the primary and secondary yield points could be rationalized qualitatively on the basis of stress-induced ordering of carbon atoms in the stress fields of dislocations, as postulated in an earlier paper, the kinetics of the secondary-yield-point development were interpreted to indicate that the ordering involves more than just single jumps of carbon atoms from high-energy to neighboring low-energy sites. 5) pickled and lime-coated; 6) drawn through a carbide die. The predetermined diameters were chosen so that drawing through the same die gave the various reductions desired. Tensile specimens of 0.252 in. diam with a 1 1/4 in. gage length were then prepared from the drawn bars and tested. In order to study the stress-strain behavior at the yield point in detail, a rigid tensile machine with a high spring constant was constructed. Columns of large cross section (relative to the specimen cross section) constituted the machine frame. A dc motor was used to drive a screw via a gear reducing train and a "crane" thrust bearing. In this relatively simple device small deformations could be observed un-blurred by the slow response and lower spring constant inherent in hydraulic machines.' A strain-gage dynamometer permitted load changes as small as 8 lb to be read. RESULTS Tensile test samples machined from bars in the as-quenched condition with no subsequent drawing and samples from bars with 3.8 pct reduction after quenching gave stress-strain curves typified by those shown in Figs. I and 2. The time lapse between predrawing and tensile testing varied but usually ranged between 3 to 6 days at room temperature. The strain rate during testing was 0.003 in. per in. per min. The as-quenched curve is seen to have a broad serrated maximum whereas the stress on the specimen prestrained 3.8 pct rose linearly to point A, Fig. 2, fell abruptly to B, and then gradually to C. The abrupt drop to B was accompanied by evidence of incipient necking. The drop of the stress at the yield point in the prestrained samples (A to B in Fig. 2) changed with the percent prestrain, as illustrated on Fig. 3. Although the tensile strength increased continuously with the amount of previous cold drawing, the magnitude of the yield point drop first increased—up to about 6 pct prior reduction—and then decreased. Specimens from bars predrawn more than 8 pct broke in a brittle fashion in the elastic portion of the stress-strain curve.

Jan 1, 1967

By J. Chipman, N. J. Grant, H. L. Bishop, H. N. Lander

Data of several studies on the equilibrium between molten iron and open hearth-type slags have been combined to determine some of the chemical reactions involved in steel-making. Effects of slag composition and temperature on the iron oxide activity, distribution of sulfur between slag and metal, and the carbon content of the metal are discussed. Also, an overall reaction for the equilibrium between sulfur and oxygen is presented. DURING the past 15 years, a number of significant equilibrium studies have been carried out between liquid iron and simple basic and acid slags in an effort to throw light on the chemical reactions involved in steelmaking. This paper is a summary of the experimental reports on investigations which have been conducted at the Massachusetts Institute of Technology, and of related work in other laboratories. The investigations summarized in this paper include the works of Fetters and Chipman1 and Taylor and Chipman,' which dealt with simple slags that are similar to those found in the open hearth. The sulfur determinations of the slag-metal tests of Fetters and Chipman as reported by Grant and Chip-man" are included. Also, the investigations by Win-kler and Chipman' and Grant and ChipmanQ f more complex slag systems are included in this summary. The experimental procedure is described in detail in each of these papers and will not be discussed. Since the previous reports have been somewhat independent, it is desirable to review and combine the data of the various investigations to determine, as accurately as possible, the reactions in the slag-metal systems of the open hearth. It is the object of this report to present the combined data in such a way as to enhance their utility and applicability. Oxidizing Power of Slags of the System (CaO+MgO)-Si0,-FeO in Equilibrium with Carbon-Free lron The slags selected to determine the iron oxide activity in equilibrium with pure liquid iron were those containing less than 2 pct each of P,O,, MnO, or A1,0, on a weight percentage basis. The method used to calculate activities of iron oxide in liquid slags was that developed by Taylor and Chipman.' The solubility of oxygen in molten carbon-free iron under pure iron oxide slags can be expressed by the following eauation —6320 log (pctO)-------------— + 2.734 [1] where T is the absolute temperature. The oxygen solubility values as determined from Eq. 1 were used throughout this study to calculate the iron oxide activity. The iron oxide activities of slags of various iron oxide contents are plotted in Fig. 1 as a function of the basicity, which is defined as the ratio (pct CaO + pct MgO)/pct SiO,, and are based on molecular percentage values of the components. The percent (FeO), is the total iron content in the slag calculated to FeO. Fig. 1 shows that as the basicity increases at constant mol pct (FeO),, the iron oxide activity increases rapidly and reaches a plateau which extends on the basicity scale from about 1.3 to 2.3; the iron oxide activity then decreases rapidly until a basicity of about 3.0 is reached, where it tends to level off. The solid portions of the curves represent the experimental data of Fetters and Chipman and Win-kler and Chipman. Their experimental heats were made in magnesia crucibles, and hence the slags were saturated with magnesia. The broken lines on the left represent the experimental data of Taylor and Chipman, who used a rotating crucible. In general, these slags contained less than 3 pct MgO. The absence of data for slags containing less than about 40 mol pct (FeO), and basicity ratios greater than about 2.5 made it necessary to calculate curves using ionic concepts of slags. The broken lines on the right, which disregard the solubility limits of di and tricalcium silicate and lime, were obtained by following the treatment of Flood and Grjotheim,"

Jan 1, 1957