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United Engineering Trustees, Inc. GEORGE D. BARRON ARTHUR S. DWIGHT R. M. ROOSEVELT The Engineering Foundation H. C. BELLINGER E. DEGOLYER J. V. N. DORR

Jan 1, 1932

By Ellsworth Daggett

In the first paper on the Russell process presented by Mr. Stetefeldt, in May, 1884 (Transactions, xiii.), the process was treated from a purely theoretical standpoint.. 111 his second paper of October, 1886 (Transactions, xv,), the details of the plant, the chemicals used, and the manipulation in both mill and laboratory were treated. The aim of the present paper is to present economical results recently attained, new data affecting the preparation and manipulation of ore in the mill, and a more complete and systematic scheme of laboratory work. This paper is compiled mainly from Mr. Russell's notes of his own experience. Many of these notes, particularly those relating to work at Cusihuiriachic,* Mexico, have been upon work directly under the personal observation of the compiler, who takes pleasure in thus presenting to the Institute, data and considerations of much interest and value pot only to users of the Russell process, but to mill men generally. The description of the chemicals used and of the preparation of the mill-solutions being' in part the same now as when Mr. Stetefeldt's second paper was published, some use is here made of portions of that paper. No theoretical matter is here given. For a treatise containing also the theory of the process the reader is referred to Mr. Stetefeldt's complete work on " Lixiviation of Silver Ores by Hyposulphite Solutions," now in preparation. To facilitate the consultation of this paper, the following synopsis and index is prefixed. The figures in parenthesis indicate the page of this paper on which the subject is treated.

Jan 1, 1888

By A. T. Yu

The energy crisis and the resurgence of mining activities highlighted 1972-73. Added to the impetus for more effective materials handling systems has been the continued upward trend of inflation and labor costs. The need for addressing the fundamentals has led to the trend toward an overall systems approach to materials handling problems.1 The decision to move forward with large mining ventures such as the $150 million Hibbing taconite comple2 and the immense Carajas iron project must base themselves on indepth studies of a host of factors viewed in the context of an integral mine-transport-market system. What's important is that each ton of pellet or ore must be an economical commodity at the end users' furnace. The project can still be viaable even if certain components in the entire network appear to be individually costly.

Jan 2, 1974

Jan 1, 1888

By H. E. Mussey

WHEN the American Institute of Mining Engineers visited the Birmingham district in May, 1888, the four Ensley furnaces (Fig. 1) then FIG. 1.-BLAST-FURNACE DEVELOPMENT IN ALABAMA. completed were referred to as monumental.1 Their dimensions are given in Table 1. Mr. Gordon stated, with considerable satisfaction, that on the preceding day one furnace had produced 165 tons. The blast was

Jan 10, 1924

By Robert H. Richards

During tile summer of 1870, I had an opportunity to visit the laboratory of the late David Forbes, Esq., in London, and was much interested in a labor-saving device which he had attached to his agate mortar. The mortar was placed in the centre of a small table, and about ten inches to the right of the mortar, a post, perhaps two

Jan 1, 1879

By W. A. Hooker

This portion of Mexico is quite beyond the ordinary routes .of travel, and is seldom visited. Its mines have not the record of enormous wealth which has recently attracted foreign capital to other parts of the republic; but for many centuries it has been a mining country, and at some periods evidently a productive one. In 1881 the writer visited the State and spent some time in the inspection of the mines. The absence of published information regarding its mining industry is his apology for presenting to the Institute these notes on the subject. Oaxaca is, with one exception (Chiapas), the most southerly of the Mexican States. It extends from latitude 18o 20' to 15' 45' N.— about 180 miles, by some 300 miles, in an east and west direction, and embraces a large part of the Isthmus of Tehuantepec. The coast-line is wholly on the Pacific. The State has an area of 27,470 square miles, nearly that of the State of Maine, and a population estimated at one million, or thirty-six to the square mile. The great continental Cordillera which farther north and west expands into broad table-lands, is here converged into narrower limits and occupies the greater portion of the country; the main

Jan 1, 1887

I. C. WHITE, Morgantown, W. Va. (written discussion *).-The writer's conclusions with reference to the possibility of finding commercial deposits of petroleum in Brazil were published in 1908 in the Final Report of the Coal Commission of Brazil.1 Since this volume is not generally accessible, and the author has nothing to acid thereto, the following quotation found on pages 243-7 may prove of interest: The Possibility of Petroleum Deposits in Brazil "The writer has often been asked to express an opinion as to the possibility of finding petroleum in commercial quantity in Brazil. "The question is one that does not admit of an adequate answer except for the regions visited by the writer, which as already stated, include only, a portion of that great territory, and only the southern portion of Brazil; namely, the states of Rio Grande do Sul, Santa Catharina, Paraná, and a few rapid excursions across São Paulo, and Minas Geraes, as well as the brief visit to Marahú in Bahia. "That the sedimentary beds of the Brazilian Permian once held some petroleum is attested by the evidence of the Iraty black shale which gives off the characteristic odor of this substance from São Paulo to Rio Grande do Sul.

Jan 1, 1918

Since the comprehensive review of the Persian fields presented by Sir John Cadman last year, operations have proceeded normally. No developments of especial importance fall to be recorded and it remains only to bring up to date the full information given at the beginning of 1933. Controlled production from the Masjid-i-Sulaiman and Haft Kel fields has been maintained at slightly higher rates than during 1932. The figures for the past five years are as follows: These represent crude oil and products piped to the coast but exclude products reinjected into the reservoir, a process that has been in continuous operation at Masjid-i-Sulaiman during the period under review. The systematic delimitation of the Haft Kel field has been continued during the past year and results have been sufficiently encouraging to justify the inception of a wider scheme for distribution of production. Drilling has been resumed recently in the Persian sector of the Naft Khaneh field, and preliminary survey work is in progress for the selection of a site for a refinery at Kermanshah arid the construction of a connecting pipe line. Investigations in connection with the scientific control of reservoir were dealt with in considerable detail in last year's review. This work has been steadily pursued during 1933 and certain of the investigations have been the subject of papers presented to the World Petroleum Congress held in London in July of last year.

Jan 1, 1934

A new departure of unusual importance in Institute annals was in-augurated by the trip of President Philip N. Moore to the Local Sections at Nevada, Southern California, San Francisco, Seattle, Spokane, Montana, Utah, and Colorado. Everywhere the visit of the President was the occasion of an enthusiastic and successful meeting, which is reflected in the account, published under the different Sections in this and other Bulletins. The President also joined the members of the Columbia Section in their visit to Nelson, British Columbia, at the International Mining Convention, which was attended by mining engineers of Canada and the United States. The President of the Canadian Mining Institute, as well as the officers and members of the Western Section also attended this convention. For full particulars we recommend to our readers the ac- count of this very interesting meeting, which is given on another page of this. Bulletin. It is believed that this is the first meeting between the mining engineers of America and any other country since America joined the Allies. The Secretary of the Institute accompanied the President at the first four meetings and was expecting to attend the others also, but was called home by a death in his family.

Jan 7, 1917

By Robert Glass Cleland

IN gathering material for this book, I have made extensive use of the archives of Phelps Dodge, contemporary news- papers, and a wide range of secondary sources. Two manuscripts-one on the history of Phelps Dodge by Arthur Train, Jr., and John L. Lawler, the other a biography of William E. Dodge by Richard Lowitt-have been of the greatest value. I owe a particular debt to the authors whose names I have just mentioned. I have also gathered important information and obtained revealing points of view from conversations with many people. Personal visits to the company's mines and plants added knowledge and understanding that nothing else was able to supply. I am greatly obligated to the officers of the company, especially to Mr. Louis S. Cates, chairman of the board of directors, Mr. Robert G. Page, president, Mr. George R. Drysdale, vice-president of Phelps Dodge Corporation, and Mr. Walter C. Bennett, president of Phelps Dodge Refining Corporation, for their co-operation and assistance. Mr. Wylie Brown, former president of Phelps Dodge Copper Products Corporation, also supplied valuable data and deeply appreciated hospitality. In my visits to the Phelps Dodge properties, company representatives extended every hospitality and placed at

Jan 1, 1952

The Arizona Committee, consisting of GERALD F. G. SHERMAN, Chairman, ARTHUR NOTMAN, Secretary, NORMAN CARMICHAEL, B. BRITTON GOTTSBERGER, W. L. CLARK, J. C. GREENWAY, W. G. MCBRIDE, FOREST RUTHERFORD, has arranged the following program for the Arizona Meeting, which has been approved by the President of the 'Institute and by the Executive Committee. It is printed herewith for the information of members, and probably will not be changed in any material respect. Monday, September 18, 1916.-Arrive at El Paso, Texas,, 6.30 A.M. Arrive at Deming, N. Mex., 9.30 A.M. Arrive at Chino, Ariz., 11.30 A.M., where luncheon will be served, after which there will be a visit to the Chino mines. From there the train will proceed to Hurley, N. Mex., where a visit will be made to the mill of the Chino Copper Co. Tuesday, September 19, 1916.-Arrive at Douglas, Ariz., at 8.00 A.M. The morning will be spent at the reduction works of the Copper Queen Consolidated Mining Co. "and of the Calumet & Arizona Mining Co. After luncheon a technical session will be held, with "Smelting" as a special subject for discussion. There will be a banquet in the evening, followed by another technical session or-a business meeting.

Jan 6, 1916

Jan 1, 1884

By Robert M. Grogan, James C. Bradbury

The Illinois-Kentucky mining district has, since 1880, accounted for 80 per cent of all U.S. production of fluorspar. The ore deposits are of two types: vein deposits formed by fissure fillings along faults and bedding-replacement deposits formed by the replacement of strata at certain favored stratigraphic positions along minor faults and fractures. Fluorite is the chief valuable mineral in the deposits. Sphalerite and galena commonly are present in small amounts but, in some ore bodies, may form a substantial part of the valuable constituents of the ore. Calcite is the chief gangue mineral; quartz and barite Exposed strata range from Devonian are present in various amounts. through Pennsylvanian in age. Igneous intrusive rocks occur as mafic dikes and sills and intrusive breccia dikes and plugs. Structurally, the district is situated on a generally northwest- trending arch that has been sliced into a series of long, narrow blocks by normal faults that trend northeastward. The structural The localization of the ore deposits by faults and fractures, the association of fluorite mineralization with intrusive breccias, and various lines of petrographic and geochemical evidence indicate that the fluorite-zinc-lead deposits were epigenetic and deposited by solutions emanating from a deep alkalic magma.

Jan 1, 1968

Page The Cobaltchromium Binary System (paper by A. R. Elsea, A. B. \Yesterman, and G. K. Manning, Met. Tech. June, 1948, Mechanism of Precipitation in a Permanent Magnet Alloy (paper by A. H. Geisler and J. B. Newkirk, Met. Tech. Aug. 1948, Tp 2444)................................................................................................. 300 Some Effects of Applied Stresses on Precipitation Phenomena (~aper by W. L. Finlay and W. R. Hibbard, Jr., Met. Tech. Sept. 1948, Tp 2470)....................................................................................... 301 Diffusion of Carbon in Austenite with a Discontinuity in Composition (paper by L. S. Darken, Met. Tech. Sept. 1948, TP 2443) 304 An Electron Diffraction Study of Oxide Films Formed on Nickelchromium Alloys (paper by J. W. Hickman and E. A. Gul- bramen, Met. Tech. June 1948, Tp 2372)..................................................................... 305 An Electron Diffraction Study of Oxide Films Formed on Copper-nickel Alloys at Elevated Temperatures (paper by J. W. Hickman and E. A. Gulbransen, Met. Tech. June 1948, TP 2391)................................................ 307 Decarburization of Chrome Nickel Alloys by Their Surface Oxides in High Vacua and at Elevated Temperatures (paper by E. A. Gulbransen, W. S. Wysong, and K. Andrew, Met. Tech. Sept. 1948, TP 2438)................................ 307 Fractographic Study of Cast Molybdenum (paper by C. A. Zapffe, F. K. Landgraf and C. 0. Worden, Met. Tech. Aug. 1948, TP 2421)................................................................................................. 308 Effect of Composition on Grain Growth in Aluminum-magnesium Solid Solutions (paper by L. J. Demer and P. A. Beck. Met. Tech. June 1948, TP 2374)............................................................................. 309 Effect of a Dispersed Phase on Grain Growth in Al-Mn Alloys (paper by P. A. Beck, M. L. Holzworth and P. Sperry, Met. Tech. Sept. 1948, TP 2475)................................................................................. 310 Statistical Rate Theory of Metals—Mechanism of Flow and Application to Tensile Properties (paper by J. W. Fredrickson and H. Eyring, Met. Tech. Aug. 1948, TP 2423)............................................................... 315 Nucleation of Slip Bands (paper by J. G. Leschen, R. P. Carreker, and J. H. Hollomon, Met. Tech. Sept. 1948, TP 2476) and.. 318 Transient Plastic Deformation (paper by R. P. Carreker, J. G. Leschen, and J. D. Lubahn, Met. Tech. Sept. 1948, TP 2477).. 318 Plastic Deformation of Large Grained Copper Specimens (paper by W. R. Hibbard, Jr., Met. Tech. Sept. 1948, TP 2469). ... 323 Plastic Flow in Anisotropic Sheet Steel (paper by L. R. Jackson, K. F. Smith, and W. T. Lankford, Met. Tech. Aug. 1948, TP 2440)................................................................................................. 323 The Effect of Thermal-mechanical History on the Strain Hardening of Metals (paper by J. E. Dorn, A. Goldberg, and T. E. Tietz, Met. Tech. Sept. l948, TP 2445)....................................................................... 325 The Room and Elevated Temperature Properties of Some Sand Cast Magnesium-base Alloys Containing Zinc (paper by T. E. Leontis, Met. Tech. June 1948, TP 2371)..............................................................., 327 The Low Temperature Properties of Tin and Tin-lead Alloys (paper by H. S. Kalish and F. J. Dunkerley, Met. Tech. Sept. 1948, TP 2442)............................................................................................335 Thermal and Electrical Properties of Ductile Titanium (paper by E. S. Greiner and W. C. Ellis, Met. Tech. Sept. 1948, TP 2466).................................................................................................... 335 Property Changes during Aging (paper by A. H. Geisler, Met. Tech. Aug. 1948, TP 2436)............................... 337 Factors Affecting the Tensile Notch Sensitivity of Magnesium Alloy Extrusions (paper by I. Cornet, Met. Tech. Aug. 1948, TP 2419)................................................................................................. 338 Effect of Grain Size on Tensile Strength, Elongation and Endurance Limit of Deep Drawing Brass (paper by H. L. Walker and W. J. Craig, Met. Tech. Sept. 1948, TP 2478)............................................................. 339 A Copper-base Alloy Containing Iron as a High-strength, Highconductivity Wire Material (paper by W. Hodge, R. I. Jaffee, J. G. Dunleavy, and H. R. Ogden, Met. Tech. Aug. 1948, TP 2422).............................................. 340 A High Strength-High Conductivity Copper-silver Alloy Wire (paper by W. Hodge, R. I. Jaffee, J. G. Dunleavy, and H. R. Ogden, Mel. Tech. June 1948, TP 2366)...................................................................... 340 The Effect of Chronlium on the Ma Point (paper by J. B. Bassett and E. S. Rowland, Met. Tech. Aug. 1948, TP 2417.... 341 The Kappa Eutectoid Transformation in the Copper-silicon System (paper by W. R. Hibbard, Jr., G. H. Eichelman, Jr., and W. P. Saunders, Met. Tech. Sept. 1948, TP 2441).............................................................. 343 Stabilization of the Ausknite-martensite Transformation (paper by W. R. Harris, Jr. and M. Cohen, Met. Tech. Sept. 1948, TP 2446)................................................................................................ 344 Secondary Hardening of Tempered Martensitic Alloy Steel (paper by W. Crafts and J. L. Lamont. Mel. Tech. Sept. 194,8, TP 2439)................................................................................................. 345

Jan 1, 1950

By T. Watanabe, S. Karashima, H. Oikawa

Creep tests of a! iron and its solid-solution Fe-Mo, Fe-Co, and Fe-Si alloys with bcc structure were conducted under constant stresses in ferromagnetic and paramagnetic temperature regions above 0.5T,(T, is the absolute melting temperature). It was found their high-temperature creep behavior changed in the vicinity of the magnetic transformation temperature, that is Curie temperature, TC. In the ferromagnetic region below the steady-state creep rates were lower than those expected from the extrapolation of the data in the paramagnetic region, the amount of decrease being affected by solute addition. Also, activation energies for steady-state creep were different in the two temperature regions. The observed changes were concluded to be due to the effect of ferromagnetism on diffusion. It is well-known that plastic deformation of metals and alloys in the temperature region where mobility of atoms becomes high enough is controlled by atomic diffusion." Many experimental results394 on fcc and hcp materials have been reported to confirm this view. In bcc metals and alloys, not much basic investigation of creep deformation has been performed. In particular, experimental work on iron5-&apos; and its alloys, covering a quite wide temperature range is extremely scarce. On the other hand, the effect of ferromagnetism on diffusion has recently been demonstrated in a iron and its alloys;&apos; it has been made clear that diffusion rates in ferromagnetic temperatur~e region are significantly lower than those expected from diffusion measurement in the paramagnetic region. Therefore, it is concluded that the magnetic effect influences the high-temperature creep behavior in a! iron and in its alloys. The present authors have conducted creep experiments on a iron and its solid-solution alloys over a very wide temperature range, and have demonstrated the magnetic effect. A part of the result has already been reported elsewhere.26 In this paper, the experimental results will be described in detail. While the manuscript was in preparation, a similar magnetic effect on creep deformation of a iron was reported by Ishida . Though their experiments covered an extremely wide temperature range, the creep stresses varied from several thousand psi to several ten thousand psi with decreasing temperature. Consequently, it may be said that there remain some questions concerning their results. I) EXPERIMENTAL PROCEDURE The materials used in the experiments were pure iron and its alloys; they were prepared by vacuum melting (10"" mm Hg) electrolytic iron (99.9 pct), molybdenum powder (99.9 pct), ultrapure silicon, and cobalt pellet (99.5 pct) in alumina crucibles. The ingots were hot-forged to plates 10 mm thick and 50 mm wide, and then were hot-rolled at about 700°C into sheets 1 mm thick. Creep specimens, 5 mm in width and 15 mm in gage length, were machined from the sheets. They were annealed at temperatures which were well above their respective recrystallization temperatures. The chemical compositions of the metal and alloys are shown in Table I together with their heat treatments. High-temperature creep tests by the use of a lever-type creep testing machine were carried out in argon atmosphere under constant tensile stress. In order to keep &eep stress constant within about *0.5 pct, stress change due to specimen elongation was compensated by tensile force of a stainless-steel bellows which was inserted between the loading lever and lower specimen grip with the assumptions of a linear relationship between change in cross section and strain and uniform strain along the section. Beyond the limit of compensation by the bellows, small amounts of load were removed after appropriate strains. The testing temperatures were maintained to within i2"C of the reported values. Creep deformation was auto-graphically recorded at the upper (moving) specimen grip using a linear differential transformer which was held by a stainless-steel rod mechanically connected to the lower specimen grip. It was also directly measured with a dial-gage reading to -& mm. 11) EXPERIMENTAL RESULTS AND DISCUSSION 1) Creep Curves of a Iron and Its Alloys. Creep curves of a! iron, Fe-Si, Fe-Co, and Fe-Mo (<2 at. pct Mo) alloys usually consisted of three stages, that is transient (primary), steady-state (secondary), and accelerating (tertiary) stages. An example is illustrated in Fig. 1 for a! iron. However, in Fe-Mo alloys with more than 2 at. pct Mo, an inverse transient creepZ8 was observed as indicated in Fig. 2. The inverse behavior, which varied with the amount of molybdenum, may be due to the substructure* in the annealed specimen as was sug-

Jan 1, 1969

By B. C. Allen, R. I. Jaffee, D. J. Maykuth

Wrought unalloyed iodide chromium, containing 39 to 95 ppm total interstitials, has a tensile transition temperature of —15°C. Re crystallizing at 1100°C causes the transition to rise to 90° to 390°C, depending on the purity, grain size, and cooling rate after annealing. At about the 100 ppm level, individual additions of carbon or nitrogen raise the transition of both wrought and recrystallized chromium by as much as 210°C, while oxygen has a lesser effect, and sulfur essentially no effect. High transitzon temperatures are exhibited by recrystallized and quenched chromium, and appear to be associated with the amount and distribution of inter-stitials. The latter cm be either in solid solution or in the form of precipitates within the grains or at the grain boundaries. Quench hardening in chromium is primarily caused by nitrogen. The hardness, re crystallization, and grain growth behavior of chromium with and without impurity additions were also investigated. BECAUSE of low density and good oxidation resistance, chromium-base alloys are potentially useful for elevated-temperature applications. The main deterrent to the use of chromium in structural applications is its lack of low-temperature ductility, especially in the recrystallized condition. Accumulated evidence has shown that the ductility of chromium is sensitive to purity. The objective of the current study was to determine the effect of common nonmetallic impurities on the tensile properties of high purity chromium. The separate effects of carbon, oxygen, nitrogen, and sulfur additions on the ductile-to-brittle transition were evaluated for wrought and recrystallized material after various cooling rates. EXPERIMENTAL WORK Unalloyed iodide chromium and seven impurity alloys containing individual carbon, oxygen, nitrogen, or sulfur additions were prepared in rod form. Nominal additions were 100 ppm C, N, and S, and 100 to 500 ppm O. The additions were about a factor of ten greater than the residual amounts in the unalloyed material. The seven alloys and two unalloyed compositions were consolidated into four-pound ingots by conventional consumable arc melting of pressed and welded electrodes under 0.5 atm of helium. Impurity additions were made to the electrode in the form of crushed master alloys. The impurity alloys were double melted to improve homogeneity. The ingots were broken down by extrusion at 1200°C in evacuated steel cans at a reduction ratio of 18 :1, using a molten borosilicate glass lubricant and a ram speed of 80 in. per min. The cans were removed by acid pickling, and the chromium core ground free of surface undulations. Cut lengths were sheathed in mild steel and swaged at 900°C until the core was about 1/4 in. in diam. Two additional 15-lb ingots of unalloyed chromium (ICr-3, ICr-4) were prepared by arc melting and broken down by 26:1 extrusion at 1250°C without a steel can. The billet was lubricated and protected from contamination by a coating of molten glass. The resulting extrusion was then sheath swaged as described previously. Representative chemical analyses of each of the materials, after removal of a 10-mil surface layer

Jan 1, 1963

By P. D. Rao, H. B. Charmbury, D. R. Mitchell

As a result of a changing market pattern for anthracite, there is now an increasing demand for steam size and a decreasing demand for domestic sizes. To help the producer meet this new demand, the authors present the technical aspects of the problem of crushing domestic sizes to steam fineness and size. The market pattern for anthracite coal has changed considerably in recent years. The demand for domestic sizes has been gradually decreasing and the demand for the steam sizes has been increasing. The companies however aim for a maximum production of domestic sizes, since these sizes command premium prices. To meet the market demands, particularly in certain periods of the year, further size reduction of the coarse clean coal is necessary. The present practice of multistage crushing in toothed rolls leads to complicated flow arrangements and is high in cost. Data presented herein indicate that crushers with high reduction ratios could be used with a resulting simplification of crushing flows and an appreciable reduction of capital and operating costs. The different types of crushing equipment investigated included the rotary-type breaker, the jaw crusher, the impactor-type crusher, and the Aerofall mill. CURRENT PRACTICE The standard sizes of anthracite are presented in Table I and market specifications require that any given size be maintained with only a limited amount of oversize and undersize material. The 1958 prices of the various sizes also are presented, so it may be seen that size reduction is only performed when dictated by market demands. At the present time the general practice of crushing anthracite consists of removing the top size and crushing it in a toothed double roll crusher to the next largest size. Consequently, to reduce the domestic egg, stove, and nut sizes to steam sizes of pea, buck, rice, and barley, the original material must be screened to produce the three top sizes and each size must be crushed in three separate rolls to the next largest size. Each crushed product must then be rescreened to remove the oversize for re crush ing. Thus a typical operation would consist of scalping the egg size from a mixture, crushing it to stove size, and rescreening the product. This same cycle would be repeated for the stove and nut sizes requiring three screens and three crushers as well as conveying equipment to handle the crushed products. This results in an expensive series of operations to make a product which sells for a lower price. If the three top sizes are crushed in one operation to the smaller sizes then the yield of steam sizes is low and the production of Nos. 4 and 5 sizes is large. These sizes sell for lower prices than the steam sizes. A typical operation is presented in Fig. 1. From the figure it may be seen that the original cleaned anthracite contains 67.4 pet domestic sizes, 26.4 pct steam sizes, and 6.2 pct fines. After multistage crushing of the domestic to steam sizes the composition of the product is 0.6 pct domestic sizes, 89.6 pct steam sizes, and 9.8 pct fines. From a technical standpoint these results are reasonable but the handling and crushing costs are

Jan 1, 1961

By R. W. Kewish

The preparation of massive uranium metal containing very low concentrations of a number of light elements by bomb reduction of UF4, with calcium is described. Details of procedures are given for preparing high-purity ingredients for the bomb reduction. The as-reduced uranium metal contained, on the average, less than the following amounts of light element impurities, in ppm: Li, 0.1; Be, 0.1; B, 0.1; C, 25; 0, 70; Na, 1; Mg, 3; Al, 2; and Si, 7. Other impurities for which the metal was examined averaged, in ppm: Ca, < 10; V, < 10; Cr, 2; Mn, 6; Fe, 50; Co, < 5; Ni, 8; and Cu, 1. THE preparation of very high-purity uranium metal in massive form for research purposes is of great importance. Recently the kilogram-scale preparation of uranium metal containing less than 70 ppm of detected impurities was accomplished by Blumen-thal and coworkers by vacuum remelting of high-purity crystals of uranium obtained by fused salt electrolysis.1"3 Albert and coworkers4 have reported successful experiments in lowering the concentrations of certain impurity elements in uranium, notably iron, to a few ppm by the zone-melting method. The present paper describes the preparation of high-purity massive uranium metal by the bomb reduction of UF4, with calcium. Early in 1951 a program was undertaken at the Los Alamos Scientific Laboratory to prepare uranium metal of very high purity with respect to a number of the light elements. The methods considered for this purpose were 1) bomb reduction of a uranium halide with calcium, 2) electrolysis of fused salts, and 3) hot wire decomposition of UI4, The first of these processes had been used extensively at Los Alamos since 1943 (and still is used) for the production of uranium metal.5 In considering the three processes it was evident that either of the last two would require an extensive development program with no certainty of success. On the other hand, a study of available data showed that uranium metal of very high purity with respect to some light elements had occasionally been made in routine processing by the first method. It was therefore decided that an intensive study of the bomb-reduction process would be made to see if it could be improved to yield uranium metal with very low concentrations of light elements. DEVELOPMENT OF PROCEDURES The bomb-reduction process used at Los Alamos consists of reducing UF4 with calcium, using iodine as a booster. The reaction is carried out in a magnesium-oxide crucible enclosed in a steel bomb. Argon is used in the bomb to avoid objectionable side reactions which would occur in the presence of air. All ingredients for this bomb-reduction process were examined as possible sources of light elements. It was known that high-purity UF4 was required. The calcium used in the reductions was a source of carbon and magnesium. The magnesium-oxide crucibles were sources of boron, silicon, and magnesium. The iodine did not appear to be a source of any impurities. Pure UF4- The UF4 for bomb reduction is prepared from U3O3 , by successive reduction to UO2, with hydrogen and hydrofluorination of the UO2, with anhydrous HF. Since it was known that no impurities were normally introduced during the gas-solid reactions, effort was directed toward the preparation of high-purity U3O3. Of the many possible procedures for the purification of uranium solutions the following were investigated: 1) Precipitation of uranium peroxide. (Two procedures were tried. The first consisted of simultaneously adding hydrogen-peroxide and ammonium-hydroxide solutions to a uranyl-nitrate solution, containing citric and malonic acids, at such relative rates that precipitation was carried out at a constant pH of 1.5 The second consisted of simultaneously adding uranyl-nitrate, ammonium-hydroxide, and hydrogen-peroxide solutions to an aqueous solution

Jan 1, 1960