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By S. E. Bronisz, Dana L. Douglass

a Uranium was deformed by cold rolling, and the effects of this plustic deformation on the microstruc-ture of the metal were observed by the technique of transmission elecbon microscopy. The recrystalli-zation of selected cold-wmked samples was also studied by this method. The samples were prepared for examination by electrolytic thinning in a standard metallographic electrolyte which has not been previously reported as being used in producing thin foils of uranium. The microstructural changes observed in the a uranium were generally similar to those seen by optical microscopy. The changes in the microstructure of a uranium following cold work and recrystallization treatments have been the subjects of several studies employing optical and X-ray techniques.12-19 These studies indicated that twinning was the redominant mode of deformation at room temperature20 and that the regions of high energy associated with the deformation twins were preferred sites for the initiation of recrystallization.15,18, Recently several workers have prepared thin foils of uranium suitable for examination by transmission electron microscopy.'-lo The foils thus prepared have been used to study fission fragment damage; a particular dislocation reaction,' and gas precipitation." At this laboratory the microstructural changes occurring during the cold working and recrystallizing of a uranium samples have been studied by using transmission electron-microscopy techniques. The foils used in this work were electrolytically thinned in a polishing bath not reported previously in the literature as being used for this purpose. EXPERIMENTAL PROCEDURE The uranium used in this investigation was depleted a uranium sheet 4 mils thick. The results of a spectrochemical analysis of this material are shown in Table I. The as-received uranium was cut into strips, 1 in. wide by 5 in. long, and annealed in vacuo at 600°C for 2-1/2 hr. The resulting microstructure consisted of relatively uniform, equiaxed grains having diameters of 10 to 50 p. Cold Working. The cold-worked samples were prepared by rolling several of the annealed uranium strips to various thicknesses. The strips were reduced 3.5 ± 0.5, 6.0 ± 0.6, 10.0 ± 0.5, 19.5 ± 1.0, and 28.5 ± 2.0 pct in thickness. It was not possible to achieve these reductions with a single pass through the rolling mill, so the strips were turned end for end during the rolling procedure. The cold-rolled strips were stored in dry ice until samples from them could be thinned and examined (within 24 hr after rolling). Annealing. The samples used in studying the re-crystallization behavior of a uranium were obtained by annealing sections of the strips which had been reduced 10.0 and 28.5 pct. These samples were sealed in evacuated Pyrex capsules and were annealed in a tube furnace at temperatures from 200" to 600°C and for times from 1/2 to 2 hr, see Table l. Thinning: The samples from the rolling and heat treatments were prepared for examination in the electron microscope by electropolishing in a bath composed of 25 g chromic acid, 133 ml glacial acetic acid, and 25 ml water. This electrolyte has been used and recommended for preparing specimens for optical metallography It was necessary to mask the edges of the sample with a stop-off paint in order to prevent preferential attack in these areas. The paint used was made by dissolving polystyrene in benzene. The electrolytic cell consisted of a cylindrical stainless-steel cathode placed in a beaker containing the electrolyte, with the sample as the anode positioned at the cell axis. The temperature of the electrolyte was held below 15°C by cooling with liquid

Jan 1, 1963

By H. H. Kellogg, T. R. Ingraham

Three anhydrous zinc sulfates have been identified. They are: ZnSO,(a), stable below 1007°K; ZnS04(/3), stable above 1007OK; and ZnO.ZZnSO,. The decomposition pressure of each sulfate has been measured and the following relations calculated from the results: The measured data have been combined with the known themzodynamic properties of ZnS, ZnO, Zn, SO,, and SO, to yield univariant and bivariant phase diagrams for the system Zn-S-0. The application of these diagrams to problems of roasting zinc concentrates is discussed. PRESENT knowledge of the equilibrium chemistry of the system Zn-S:O, so essential to scientific control of zinc-blende roasting, is deficient in several respects. A basic sulfate of zinc has been reported by many investigators, but its composition is in doubt and its thermodynamic properties have not been measured. Our scanty knowledge of the properties of the normal sulfate at roasting temperatures is based on old and inexact studies. A crystal transformation in the normal sulfate, involving a sizable heat effect, has been noted by several investigators but has never been quantified. The studies reported herein were designed to fill these gaps in knowledge and to make possible a reasonably complete thermodynamic description of the system Zn-S-0 at roasting temperatures. The results make possible a far more exact understanding of zinc roasting chemistry than was hitherto possible. EXPERIMENTAL The principal experimental technique employed was the measurement of the total gas pressure developed from decomposition of either ZnSO, or ZnO2ZnS0, in a closed system. The apparatus employed was essentially the same as that described by Warner and lngrahaml and Flengas and tngraham.' The unusual feature is a flexible Pyrex bellows used to separate the reaction gas mixture (S03, SOz, and 02) from the mercury in the manometer and thus prevent corrosion of the mercury by SO3. The bellows operates without evidence of hysteresis and, barring accidents, may be used for several months. The response of the bellows varies from manometer to manometer, but is generally of the order of 0.6-cm displacement for a l-cm change in pressure. The response for all manometers has been linear over the range 0 to 1 atm. To prevent condensation and polymerization of sulfur trioxide, the bellows-manometer was maintained at 100.0" * 0.5" by a circulating bath of silicone oil. The connecting tubing between the manometer and the furnace was maintained at 100.0" * 0.2"* also, with a stirred air bath. The open end of the manometer was connected with a chamber which was maintained at a known pressure. The pressure could be varied so that readings of the height of the mercury column, measured with a cathetometer, could be made with both rising and falling mercury column. By using the average of the readings, any error due to sticking of the mercury column was minimized. The sample was placed in a 2-in.-long platinum boat formed into the shape of a half-cylinder. The sample was prepared as a fine powder and pressed against the inner wall of the platinum boat. A silica thermocouple well, covered with a platinum sleeve, was placed lengthwise along the center of the boat. The temperature of the sample was read on a calibrated Pt-10 pct Rh theirnocouple. The temperature profile of the furnace was constant within ± 0.2 C over the length of furnace occupied by the sample. The horizontal furnace used to contain the sample and the quartz reaction tube was electrically heated, with the control thermocouple placed 1/4 in. from the windings. A Brown Pyro-O-Vane temperature controller with a 3-sec response time was used to maintain the furnace temperature. Before beginning a run, the apparatus, including the bellows manometer, was thoroughly washed in sib with acid and distilled water to remove any

Jan 1, 1963

From time to time the Bureau of Mines has interpreted and applied certain provisions of the Federal Coal Mine Safety Act and Federal Mine Safety Codes, primarily for the guidance of Federal Coal Mine Inspectors. Although interpretations of the Act have appeared in the Federal Register, the Code interpretations and practical applications have not been published. In response to many requests from representatives of the coal-mining industry, the Bureau is publishing this information to promote better understanding of those provisions that may be misinterpreted or misapplied. INTERPRETATIONS AND APPLICATIONS Two Federal Mine Safety Codes are discussed in this report, namely the Federal Mine Safety Code for Bituminous-Coal and Lignite Mines of the United States, Part 1, and the Federal Mine Safety Code, Anthracite Mines of the United States, Part 1. In this circular the word Codes refers to both directives; Code* refers to the code for bituminous-coal and lignite mines; Code? refers to the one for anthracite mines. Act* refers only to bituminous-coal and lignite mines.

Jan 1, 1963

By Moskovits E. E

Spodumene was recovered from pegmatite by flotation in laboratory and pilot-plant tests using an anionic collector emulsion. A similar process applied to beryl pegmatite gave encouraging results.INTRODUCTIONOver the past two decades lithium and beryllium have aroused increasing interest in the metallurgical world. Both these light metals have potential uses in nuclear shielding and cooling and in lightweight alloys, and there is a growing demand for lithium chemicals for ceramics, air conditioning and lubricants. The use, technology and history of lithium has been surveyed by Schreck (1961).For many years, the only commercial production of lithium and beryllium was from pegmatite deposits amenable to hand cobbing. The most important minerals of these ores are spodumene and beryl, which are respectively lithium aluminium silicate and beryllium aluminium silicate. Norman and Gieseke (1940) investigated the treatment of lithium ores by froth flotation. The process of flotation of the pegmatite constituents away from the spodumene was applied commercially in 1951, and the operation has been described by Goter, Rainey and Hudspeth (1953). Subsequently, the flotation of the spodumene from the pegmatite was studied by Munson and Clark (1955) and Browning and McVay (1961), and this method has superceded the reverse flotation process commercially. Muskett, Tasker and Hobson (1962), in applying the method of Browning and McVay in pilot-scale tests, reported difficulty because of activation of quartz and felspar by iron salts introduced during milling of the ore.The flotation of beryl, reported by Ashton and Weir...

Jan 1, 1963

By Laurence Pellier

Electron microscopical studies were made of the effect of sensitization at 1200oF on a Type-.104 stainless steel with high carbon and low nitrogen and oxygen contents, after solution annealing and after cold working. The loci of the carbide precipitates in the early stages of sensitization were followed in dry stripped plastic replicas. Some observations were made by direct electron transmission on thinned films. Intragranular dislocations showed a high degree of stability through the annealing necessary to produce sensitization. I HE present work was undertaken to determine the effect of sensitization, at 1200°F, for 1/2 hr, on the electron microstructure of a Type-304 stainless steel with high carbon, and low nitrogen and oxygen contents, after solution annealing and after cold working. Many electron microscopical studies of sensitization of 18-8 stainless steels have already been made. Most of them utilized extraction replicas, from which the morphology and composition of the precipitated carbides could be established.'-" ry stripped replicas were seldom used for such studies, although it was demonstrated that they are applicable, in general, to EurveYs of the general microstructure of many alloys' and, in particular, to the observation of precipitated carbides in austenitic stainless steels.3

Jan 1, 1963

By D. Bienstock

To develop a rugged catalyst capable of withstanding hydraulic attrition resulting from the oil-circulation process for synthesizing liquid fuels, use of an iron catalyst containing an active coating surrounding an inert solid core of metal was investigated. This massive-iron catalyst in the form of steel shot and lathe turnings was activated by partial oxidation with steam at 600° C, impregnated with alkali, and reduced with hydrogen at 450° 6. The massive-iron catalysts were resistant to oxidation and spalling, and a 6-month catalyst life was attained. Higher operating temperatures could be employed than with fused iron oxide catalysts, resulting in greater gasoline yields. Because the lathe turnings pack with void volumes of 70 to 90 percent, it has become possible to employ a fixed bed without the danger of cementation that occurs with fused iron oxides.

Jan 1, 1963

By James J. Scott

Three dimensional photoelastic techniques have been developed which provide information on the state of stress at any point in a model investigated. This investigation utilizes these techniques to determine the stress distributions in the pillars and the roof of a room and pillar mine model. Castolite plastic was used for the construction of the model in which a stress pattern was developed by the stress freezing process. Analysis of the stress pattern was accomplished by use of data obtained by observing points in slices from the model with a polariscope and solving data obtained by' the shear-difference method. Slices through the centerline, edge of pillar and centerline of span were investigated. Results of this work provide information on the overall stress distribution on points of stress concentration in compression, shear and tension, show relative magnitude of stress throughout the model and indicate directions of the most important stress values. A generalized roof bolt pattern is developed for room and pillar mines based on the stress distribution. A digital computer was used in the reduction of data and proved to be extremely useful for investigation of this type.

Jan 1, 1963

By C. J. Thompson

Two sulfur compounds--the 2,2,5-trimethyl- and the 2,2,5,5-tetramethyl derivatives of thiacyclopentane--were identified in Wilmington, Calif., crude oil, using microdesulfurization and gas-liquid chromtography techniques.

Jan 1, 1963

By Oliver Bowles

Sandstone, a widely distributed siliceous sedimentary rock, is the third most popular building stone in the United States. It is formed by the breaking down of preexisting rocks by weathering, subsequent segregation of the detrital quartz grains into discrete deposits by the sorting action of water or wind, and finally cementation of the quartz sand into a coherent rock. The homogeneity and resistance to weathering of the resultant sandstone make it suitable for exterior construction. Its excellent wearing properties explain its popularity for flagging and stair treads. However, quarrying and dressing methods and costs are adversely affected by the abrasiveness and hardness of sandstone especially as compared to limestone.

Jan 1, 1963

By Merwin H. Howes

Gnome shaft, situated about 24 miles southeast of Carlsbad, N. Mex., was designed and sunk by the U.S. Atomic Energy Commission for conducting a peace-time experimental nuclear explosion in the thick salt beds of the Permian Salado formation. Excavation was started July 1, 1960, and completed July 26, 1961. The 10-foot diameter shaft, lined with concrete through the rock section, was sunk 1,216 feet. A drift was driven approximately 1,140 feet on the 1,200-foot level terminating in a shot chamber. On completion of 100 feet of shaft, by means of a truck-mounted crane, facilities were installed for conventional sinking. About 709 feet of rock and 506 feet of salt were encountered in the shaft. Salt beds at this place are reported to be over 1,200 feet thick. The overlying rock section varies greatly in composition and thickness of beds and contains a 28-foot bed of water-bearing dolomite. The aquifer was sealed to facilitate shaft sinking and to prevent water-seepage damage in the salt section of the shaft. Sealing was accomplished by grout injection through holes drilled into the aquifer and by grouting behind the concrete liner.

Jan 1, 1963

By S. J. Hussey

This Bureau of Mines report presents a discussion of the statistical approach to the design of experiments and indicates, by concrete examples, how and when statistical design is essential for obtaining meaningful data with a minimum number of experiments. Every research worker plans his work and designs his experiments in a manner which, based on his experience, seems most rational to him and which he believes will produce the information essential for resolving the problems. If the results obtained are open to multiple interpretations and are not of definitive reliability, the failure of the experiment design to produce the desired information may be due to several causes, These include faulty judgment in selecting the factors to be tested, ignoring the importance of interaction between factors, failure to adequately control test variables, and assuming that meaningful trends in the results can be identified without comparison to a predetermined experimental error. An experienced researcher probably will deduce from the nature of the data obtained that the design is faulty and may by trial and error ultimately arrive at the correct solution to the problem. Statistical methods of planning research minimize the chance of faulty experiment design, embody concrete procedures for testing the validity and reliability of the test data and for indicating mandatory changes in the design, and enable the researcher to obtain meaningful information with the least number of tests.

Jan 1, 1963

Solid. dense, air-cooled slag can fulfil most, if not all, the functions of natural stone for civil engineering purposes. The value of pumice, also, has long been appreciated, and processes for the manufacture of similar synthetic material for light-weight concretes and insulating fills have been developed in past years.Foamed slag is, in effect, blast furnace pumice and is often referred to on the European continent as metallurgical pumice. It is made by the treatment of molten blast furnace slags with a critical quantity of water during which process the slag cools and expands into a sponge-like mass. The connection between foamed slag and air-cooled slag is also considered and a basis for density control given.All blast furnace slag cannot be foamed to give a product which would comply with B.S.S.877; 1939 Foamed Blast Furnace Slag. A large proportion of the total output of molten slag lacks the necessary inherent properties. This investigation attempts to discover the conditions necessary for the production of foamed slag capable of meeting the British specification.EARLIER WORKIt was generally accepted (Parker, 1951; Gallai-Hatchard, 1955) that the spongy structure of foamed slag was caused mechanically by steam trapped in the slag when it was poured into water. It was assumed that slags which would not foam would not trap steam, because their viscosities and surface tensions were unsatisfactory, on account of temperature and/or composition. The earliest systematic investigation was made by Frisak (1923) who attempted to establish a limiting chemical composition for foamable slags. He decided that foamable slags covered most blast furnace slag compositions on the basis of silica, alumina, and lime, and further "that the replacement of lime by magnesia up to 15 per cent has no noteworthy effect on foamability, that moderate quantities of alkalis are not deleterious, that sulphur raises the foamability and that MnO is only deleterious in the presence of 1...

Jan 1, 1963

By J. L. Green

Virginia-Carolina Chemical Corp., in its Florida Operations, uses both roller mills and ball mills in dry grinding of phosphate rock. The roller mills have been in operation since 1954 in the Mining Department. The ball mills were installed and put in operation in 1960 in the Harding Concentrate Superphosphate Plant. The roller mills in the Mining Department are used to grind phosphate rock for outside customers. This involves short notice orders of varying grinds, grades and types of rock. The ball mills grind phosphate rock for use in V-C's own phosphoric acid and concentrated superphosphate plant. These mills grind generally two types of rock for one grind. In 1959, a 10% speed-up was made in the operating speed of the roller mills. This paper deals with the operational gains and resulting cost savings which evolved from this speed-up, and compares the present operations of the roller mills and of the ball mills in grinding phosphate rock. In January 1959 it was decided to determine the feasibility of reducing the grinding cost on the roller mills, per ton of rock ground, by speeding up the mill 10%. At this time, one mill was completely reconditioned so it would be in top condition. Extensive tests were then run both before and after the mill speed-up to determine the resultant cost savings. These tests showed that, due to this 10% speed-up, the mill capacity was increased approximately 20% and grinding power costs per ton were reduced approximately 10%. Table I shows the results of these tests. Each test run actually represents several of the same type rock and grind, averaged together. Each test run lasted approximately three hours. The validity of these runs has been confirmed by subsequent operation in grinding over 1,000,000 tons of phosphate rock. Accurate records have been kept on power consumption and repairs as well as tons produced. Two types of feed rock were used for the tests — pebble phosphate rock and flotation phosphate concentrate rock. The pebble phosphate rock size is approximately 80-90% plus 20 mesh. The flotation concentrate phosphate rock size is approximately 15% plus 20 mesh and 95% plus 100 mesh. The same two types of rock feed were used for all the test runs. Test Nos. 1, 2, and 3 were run at the original mill speed of 85.5 rpm on the vertical shaft. Test No. 1 was run with a feed of high grade flotation concentrates; the desired fineness attempted was 70% passing 200 mesh. Tests No. 2 and No. 3 were run with a feed of low grade pebble. Test No. 2 was run for a desired fineness of 70% passing 200 mesh. Test No. 3 was run for desired fineness of 50% passing 200 mesh.

Jan 1, 1963

By Taylor G. H

The Triassic Ipswich (SE. Queensland) coals are of bituminous rank. The more exact rank of individual samples was determined by measuring the reflectance of the vitrinite. While in general the rank of the coals increases with stratigraphic depth, minor reversals, probably related to igneous intrusions, occur.The Ipswich coals form a coherent group so far as petrographic type is concerned. All are comparatively rich in vitrite and clarite, cutinite being the common maceral of the exinite group. The mineral contents of all the coals are comparatively high, clay and quartz being most abundant. The coals appear to be of essentially autochthonous origin, and to have been formed under conditions of fairly rapid subsidence.While the use of the coals is at present restricted to combustion, most have pronounced coking properties, as would be predicted from their petrographic composition and reflectance. However, the high mineral content of the coals would be a limiting factor in their use for coke-making.INTRODUCTIONDuring the last ten years, the Division of Coal Research, Commonwealth Scientific and Industrial Research Organization has carried out an extensive investigation of Australian coals, providing a wide range of analyses of most of the important of them. Special attention has been given in recent years to Queensland coals.Most seams were sampled as a number of subsections, enabling the internal variations, as well as the overall properties, to be assessed. The lenticularity of many of the mineralrich layers may tend to limit the significance of the samples, particularly in respect of ash yield, but although the vertical distribution of mineral matter may vary considerably from one sampling position to another, the lateral variation of the total mineral matter in the whole seam may not be great.Apart from extensive chemical analyses and utilization...

Jan 1, 1963

By David J. Kusler

A gravimetric method for the determination of carbon dioxide, carbon monoxide, hydrogen, methane, and oxygen in blast furnace top gas is described. Nitrogen may be determined directly by volume measurement or by difference. The method is direct, permits continuous as sampling, and provides an averaged analysis over a selected range of sampling intervals from 1/2 to 24 hr or more. Neither expensive equipment nor specialized personnel are required. The method is suitable for routine analysis, and the results compare favorably with those obtained by established methods.

Jan 1, 1963

By Innes J. A

The structural variations occurring in pellets of finely divided mixtures of iron ore and coke breeze, metallized by firing at elevated temperatures, have been examined microscopically. For any given pellet composition, time and temperature are the two most important factors in determining the development of the bonding processes.INTRODUCTIONThe success of sintering and pelletizing processes in the agglomeration of fine iron ores for blast furnace use has brought about rapid changes in thinking relative to methods of preparing furnace burdens. Increases in productivity with the use of sinter emphasize the advantages of a stable, uniformly sized furnace feed. Current practice is to produce a self-fluxing sinter containing most of the lime requirements of the furnace incorporated as a stable medium (Figgis and Charker, 1962). The elimination of fine material from the burden allows greater stack permeability and smoother operation.Sintering and pelletizing of iron ores with or without the incorporation of fluxing compounds has conditioned operators to the extent that it is now considered possible that all components of the burden may eventually be beneficiated in one form or another. Investigations are in hand to improve the quality and sizing of coke, which occupies the major part of the burden volume (Callcott, Innes and Brown, 1961; Innes, Gregory and Worner, 1963). Interest is also being revived in methods of pre-reducing iron ores prior to charging to the furnace (Hansen, Melcher and Fine, 1961). Recent experiments in a small experimental blast furnace (Melcher, 1963) show that charging of semi-metallized pellets can give rise to a production increase of 55 per cent...

Jan 1, 1963

By E. T. Turkdogan, P. Grieveson, J. F. Beisler

Jan 1, 1963

By Earl L. Hastings

Although the principal market for diatomite in the United States is in the East,4 production of the material is presently restricted to the West, because the deposits are larger, mining costs are cheaper, and the quality of product is better than that obtained from other domestic deposits. However, Tallahatta diatomite, occurring in Choctaw and Clarke Counties, Ala., has a freight rate advantage, which should encourage competition for those market that are now being supplied with the purer diatomites from the western deposits. For this reason, diatomite occurrences in the Tallahatta formation were examined by the Bureau of Mines and physical properties of samples from the deposit were determined to obtain additional data for use by any potential producer who wished to evaluate the material for its commercial possibilities. In 1894 K. M. Cunningham5 found that the buhrstone formation (now known as the Tallahatta formation) contained "siliceous shells of marine diatoms, radiolaria and foraminifera, thus being rather of the nature of tripoli or diatomaceous earth than of a true clay." Cooke6 and Semmes7 also reported the Tallahatta formation to be composed principally of diatomaceous earth with accompanying beds of sand, clay, and sandstone.

Jan 1, 1963

President Zakotnik opened the final session of the Institute at 9:30 a.m. Kenneth R. Herrmann of the Resolutions Committee presented the following resolutions to the group for their approval: RESOLVED: That the members of the Rocky Mountain Coal Mining Institute, in convention assembled, hereby ratify and confirm all official actions of the officers, the executive committee and other committees of the Institute between July 4, 1962, and the present time.

Jan 1, 1963

By Ruth F. Brinkley

Principle activities of the Bureau of Mines Explosives Research Laboratory from July 1, 1960 to June 30, 1961 are reviewed briefly in Part 1. Part 1 also includes data obtained in connection with several minor investigations which are not sufficient to warrant separate publications. Part 2 gives brief abstracts of publications that appeared during fiscal year 1961; in general, the research reported in these publications antedates this period.

Jan 1, 1963