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By C. H. Li, R. D. Carnahan, R. J. Stokes, T. L. Johnston

When silver chloride deforms by pencil glide at temperatures of 26ºand 72°C, grain size has no effect upon the proportional limit and the material necks down to a knife edge under tension. At -196ºC, deformation takes place on fewer slip systems to produce straight slip traces, the flow stress becomes sensitive to grain size and fracture occurs by cleavage from an intergranular source without any reduction in area. THERE are significant differences between the appearance of the slip bands formed in silver chloride and in the alkali halides at room temperature. The bands in sodium chloride, e.g., are fine and geometrically straight, whereas in silver chloride they are coarse and wavy.' Such differences in the slip behavior prompted us to inquire what the effects of grain boundaries might be on the mechanical properties of these solids. As an introduction to a general study of ionic poly-crystal behavior, we have investigated the effect of grain size on the stress-strain relationships in silver chloride at different temperatures. We have chosen silver chloride chiefly because polycrystals can be easily prepared free from cracks and macroscopic voids by conventional techniques. Moreover, as we shall see, the slip behavior can be readily modified by changing the temperature. It will be shown that the effect of grain size on the yield stress of silver chloride is strikingly dependent upon the temperature of deformation and that this temperature effect comes about through a change in the number of slip systems which operate at the onset of plastic flow. EXPERIMENTAL PROCEDURES Polycrystalline tensile specimens were made by recrystallizing cold-rolled AgCl sheet. Thirty-gram quantities of AR grade silver chloride powder were melted in a low heat capacity furnace, cast into cylindrical forms 3/4 in. in dim and approximately 1 in. in length and then extruded with a 16:l reduction ratio into rods 3/16 in. in dim. Extrusion temperatures were varied from room temperature to 350°C. In order to impart various degrees of cold'work to the extruded rod. All extrusions were then cross rolled to sheet 0.040 in. in thickness at room temperature and machined to form tensile specimens having a gage length of 0.750 in. with a width of either 0.250 or 0.145 in.* Annealing was carried out in an air oven at 200°C for periods up to 20 hr. specimens having average grain diameters ranging from 0.024 to 0.40 mm were prepared by varying the extrusion temperature and annealing time in the conventional manner. To obtain specimens with grain sizes larger than 0.40mm, lightly deformed thin prisims of silver chloride single crystals (supplied by Harshaw Chemical Co.) were recrystallized. Grain size determinations were made by an intercept method and revealed that the grains were equi-axed. Laue back-reflection X-ray patterns showed little tendency to form a preferred orientation texture. Specimens which were to be used for the slip band studies were polished by immersion in fresh boiling concentrated NH,OH for 60 sec. They were then etch polished for 10 sec on each side by hand lapping on a stationary velveteen lap wetted with a dilute Hypo solution (5 g of Kodak Acid Fixer in 100 cc H20). Finally the specimens were rinsed in warm water and alcohol, blown dry and carefully mounted in the tensile machine for testing. Tensile tests were performed at three temperatures, namely, 26º, -72º, and -196°C. A screw-driven hard tensile machine was used at a constant strain rate of 0.006 in. per in. per min. Loads were determined with a light- proof ring fitted with A-18 strain gages and extensions were measured with a 0.0001 in. dial gage. Constant level baths of alcohol with dry ice and liquid nitrogen were used to maintain the two lower test temperatures. EXPERIMENTAL RESULTS Reproducibility—In view of the light sensitivity and reactive nature of silver chloride, it was necessary to determine whether reproducibility depended upon either exposure to light or to the condition of the surface. However, during the course of the work it became clear that variation of laboratory lighting

Jan 1, 1962

By Roy L. Wilfong

The thermal decomposition of the ammonium sulfate, carbonate, nitrate, oxalate, and sulfate salts of praseodymium, neodymium, and samarium was investigated thermogravimetrically in the temperature range 25° to 1,500° C. Each salt was decomposed at a heating rate of 2.5° C, per minute. The pyrolytic sequences have been identified and the temperatures of formation of inter-mediates, the minimum oxide formation temperatures, and values for loss on ignition have been determined. The nonstoichiometric ranges between Pr6011 and Pr203 and the extent of these ranges have been determined for oxides derived from the carbonate, nitrate, and oxalate salts of praseodymium. The alum and sulfate salts of praseodymium produced the sesquioxide without forming the intermediate non-stoichiometric oxides. The temperature limits of formation and regions of stability for the alums and sulfates were better defined than were those for the carbonates, nitrates, and oxalates. The minimum oxide formation temperature increased in the order of samarium, neodymium, and praseodymium irrespective of the anion.

Jan 1, 1962

By G. P. Contractor

Many factors affect the forge ability of steels. One of the major factors is chemical composition.' This article discusses the individual effects of alloying elements and the effect of the resultant modification of microstructure onforgeability. INTRODUCTION T HE use of alloy steels is expanding considerably and the fabrication procedures for such alloys are becoming more complex. An attempt is made in this article to describe the effect of alloying elements on the hot-workability of steels. Most of the data reported here are taken from the studies of Ihrig, Clark and others (Refs. 1-4). Chemical composition is not the only controlling factor. Grain size and surface condition of the material, forging temperature, and speed of deformation are also important. Certain conclusions can be drawn regarding the effect of various alloying elements on the hot-work-ability of forging stock. The results of hot-twist tests are considered useful in this connection as the number of twists to failure has been taken as the level of forgeability at a particular temperature. The peak in the "Number of Twists -Tem--

Jan 1, 1962

By J. J. Laffin

In the pursuit of comfort and safety, the wonders of science have given us controlled heating and cooling, thus enabling us to enjoy all the aspects of present-day living to an extreme never previously •envisaged. Man's attempt to conquer the elements largely involves con-trolling the temperature around him. Without having conquered this aspect, his body energy would be consumed in trying to maintain physical comfort, rather than being invested in the explorations which have resulted in man's control over the forces of nature. The indirect methods used to obtain the most agreeable temperature environment were developed because of the natural tendency to strive for increased safety, convenience and comfort. Until the twentieth century, when heat generated by atomic fission became a reality, man's only source of heat, except for that of the sun, came from his discovery of fire.

Jan 1, 1962

By Alvin J. F

Tin in ores containing 0·025 to 1·5 per cent tin can be determined polarographically by the reduction of the chlorostannite ion at the dropping mercury electrode in 2M hydrochloric acid solution containing 15 per cent ammonium chloride. The tin is separated from interfering elements by distillation as the tetrabromide and collected from the distillate by co-precipitation with aluminium hydroxide. The method can detect 0·01 per cent tin in ore.INTRODUCTIONAn iodimetric method, suitable for routine analysis of titrating tin in concentrations down to 1 per cent, has been available for some years (Low, Weinig, and Schoder, 1939).As concentrations fall below 1 per cent tin, there is increasing difficulty in obtaining a distinct end point due to large amounts of iron and silica normally present after fusion of the ore. Since concentrations of tin down to 0·02 per cent are significant in ore dressing products it was necessary to examine methods to determine such low concentrations, and to adapt these to tin ores containing a wide variety of other minerals.EXPERIMENTALDigestion and separationCassiterite, the principal tin mineral, is refractory but readily attacked by a sodium peroxide flux to yield soluble sodium stannate. In a recognized procedure, a sample of ore is mixed with up to 15 g of sodium peroxide in an iron crucible and swirled over the full heat of a Meker burner for 7 min. The fusion is leached with water and acidified.This solution then contains tin, silica, and other soluble...

Jan 1, 1962

By D. H. Gurinsky, D. G. Schweitzer

The empirical equilibrium constantsd the heat of reaction for the reduction have been determined from 300° to 500°C. The mechanisms of the oxidation of uranium and magnesium from dilute bismuth solutions have been investigated. The kinetics of some of the reactions were affected by air adsorbed on the uranium oxides. THE Liquid Metal Fuel Reactor studied at Brook-haven National Laboratory uses a solution of uranium in bismuth as the fuel. Corrosion and stability problems require that the fuel solution contain corrosion inhibitors and deoxidants. Of the additives tested, magnesium has been found to be the best deoxidant and zirconium the best corrosion inhibitor in bismuth. Some experiments1 indicate that magnesium may play a secondary role in increasing the effectiveness of zirconium in inhibiting corrosion. The work reported here was intended to determine the relative concentrations of Mg and U required to prevent oxidation of the uranium fuel in the event of an air leak. In addition, an attempt was made to identify some of the mechanisms of the oxidation and reduction reactions occurring in the liquid bismuth solutions. EXPERIMENTAL Apparatus and Procedure—The equipment shown in Fig. 1 was designed so that the reaction kinetics could be studied as functions of temperature, melt composition, pressure, and flow rate. At the start of a run, the 10-liter bell jar (F) is removed by opening the bottom Dresser fitting (L), and the bismuth and additives are placed in a pyrex crystallizing dish (I). The bell jar is replaced, the system is evacuated to 10-5 to 10-6 mm Hg and then the heater (J) is turned on. When the selected temperature is reached, the oxidizing gas is admitted to the system to the desired pressure as read on the manometer (D). Gas is introduced through the slide tube (Q) which has a pyrex frit (R) sealed to its bottom. Stirring is accomplished by immersing the end of the tube in the melt. To maintain a constant pressure under flow the input and evacuation rates must be equalized. To obtain this condition stopcock (C) is closed and flowmeters (B) are matched. The reaction is "stopped" by closing the inlet flowmeter and quickly evacuating the system. To obtain a liquid metal sample, the system is evacuated with the sampler positioned near the surface of the liquid. The sampler, Fig. 2, is then immersed until its thermocouple reading matches thermocouple (G) Fig. 1. The system is then pressurized with helium which forces the solution through the frit. Twenty to 30 min elapsed between the time the system was evacuated and sampled. During evacuation and pressurization of the system, the temperature variations did not exceed ± 5°C. While bubbling occurred the temperature remained constant to within 1/2 oC. The volume of the equipment was determined by adding a known volume of air at atmospheric pressure to the evacuated system and noting the resulting pressure.

Jan 1, 1962

By J. A. Morgan, R. E. Lund, D. E. Warnes

The design, operation, and performance of an integrated pilot plant for recovering zinc and copper from a complex sulfide ore are described. Metallurqical processing comprised selective sulfate roasting in a fluid bed, leaching in a weak sulfuric acid solution, recovering copper by cementation with scrap iron, air oxidation to remove soluble iron, more-or-less conventional Purification for removal of impurities deleterious to zinc electrolysis, recovering zinc by electrolyzing solutions, and recycling spent electrolyte to the sulfating roaster. The effects of several feed preparation and roasting variables on the sulfation response of zinc, copper, and iron are set forth, together with the electrolyzing characteristics of the zinc solutions. SEVERAL years ago, St. Joseph Lead Co. undertook a research program to develop procedures for winning values from a complex ore. The deposit was a massive sulfide ore body containing upwards of 65 pct pyrite. Gangue, composed principally of quartz, calcite, dolomite, and alumina, comprised only 10 to 20 pct of the mineralized zones. Zinc, lead, and copper values were variable, but averaged about 6.7 pct Zn, 2.6 pct Pb, and 0.4 pct Cu. Early in the exploratory test work, it was established that the intimate physical association of the minerals in the ore made beneficiation by conventional flotation procedures difficult. Accordingly, in addition to a comprehensive program to investigate physical methods of ore beneficiation, a research program was established to develop a direct metallurgical method for processing the ore. After surveying a number of potential methods for recovery of both metal and sulfur values, effort was concentrated on the development of a sulfate roasting process. It is the pilot-plant development of the sulfate roasting-solution purification—electrolyzing procedures which forms the subject of the present paper. PREPILOT PLANT INVESTIGATIONS From a thermodynamic viewpoint, it is feasible to sulfate selectively a host of metals, including Zn, Cu, Pb, Cd, Ni, and Co, in an iron sulfide ore without sulfating iron. Of course, a number of conditions such as roasting temperature and gas composition must be controlled. In addition, as first disclosed by Hybinette,' an alkali metal salt is frequently beneficial in promoting the sulfation reactions. The application of fluid bed roasting to the sulfate roasting of nonferrous metals was pioneered by Stephens of Battelle Memorial Institute.' Subsequently, Falconbridge Nickel Mines, Ltd. developed an unique process for selectively sulfating and recovering nickel, copper, and cobalt from their nickeliferous pyrrhotite, which recently has been described in an excellent paper by Thornhill.3 One of the unique features of the Falconbridge process is that the feed is introduced into the fluidized roasting furnace in a manner such that the feed slurry is broken up into droplets and the droplets lose their moisture before contacting the surface of the fluidized bed. The dried droplets do not tend to cake or fuse, but rather remain as discrete agglomerates of concentrate particles and roast without significant degradation. St. Joseph, aware that Battelle Memorial Institute had participated in the development of the Falconbridge process, obtained permission from Falcon-

Jan 1, 1962

By O. Herstad, J. M. Toguri, K. Grjotheim

DURING the last three years, investigations on the aluminum reduction of magnesium-bearing compounds have been initiated at the Institute of Inorganic Chemistry, The Technical University of Norway. The results of these investigations are reported in this paper. Very little information exists in the literature on the reaction between magnesium compounds and metallic aluminum. The available information itself is conflicting, and, to clarify the existing discrepancy, the reactions between aluminum and magnesium oxide (MgO), caJcined dolomite (CaO . MgO) and olivine (Mg2SiO.) were studied. The logical approach for the study of these reactions between condensed states with the formation of a gaseous phase is, ( 1) the measurement of the equilibrium vapour pressure of the gas, in this case magnesium, associated with the respective reactions and, (2) the identification of the end products of the reaction in order to establish the re-action scheme.

Jan 1, 1962

By Ralph C. Flow

In Cleveland County, North Carolina, one and one-half miles south of Kings Mountain, Foote Mineral Company operates an open pit for the production of spodumene, feldspar, mica, and commercial stone. Spodumene concentrate is sent to Footers Sunbright, Virginia plant and to other customers. Exton, Pennsylvania and New Johnsonville, Tennessee plants produce lithium compounds sold to the oil industry for multipurpose lithium-base greases, to the metal industry as welding flux, to the air conditioning market, and to the glass industry. Ceramic grade spodumene, feldspar, and mica concentrates go to other processing companies from the Kings Mountain plant. Waste amphibolite is delivered to a neighboring quarry operation.

Jan 1, 1962

Differentiation of a basaltic (?) magma occurred in an active volcanic area during the late Miocene and Pliocene, and a change in the general mode of extrusion from fissure flow for the basalt to explosion for the andesite reflects an accompanying increasing magmatic viscosity. A caldera formed after the flow phase was completed and was filled with coarse agglomerate, much of which has a fused appearance. After an erosion interval its shape was modified and it became gradually deeper as repeated explosions from growing andesitic volcanoes caused large quantities of pyroclastic material to be deposited. At the close of this phase the floor abruptly collapsed when a, large block of the underlying crust was engulfed. The incompetent pyroclastics filling the caldera steepened in dip and the ensuing fractures were filled by the rising magma as dykes and sills and a chonolith formed below the caldera at a shallow depth. The ensuing activity reveals a further stage in differentiation and biotite is an important new ferromagnesian to be observed in the new rocks.Fracturing of the surrounding basalts was most intense in the rocks forming the periphery of the caldera where steeply and flatly dipping faults resulted from increasing horizontal pressure directed towards the caldera.Further differentiation resulted in the increased crystallization of orthoclase felspar, as evidenced by the numerous intrusives of trachy andesitic composition. Magmatic freezing caused mineralizers to accumulate at the top of the chonolith. These eventually escaped and auriferous pyrites, tellurides, quartz, and calcite were deposited in the surrounding rocks.The flatly dipping fractures are the most important and can be expected at various depths in a zone about 4,000 ft wide surrounding the caldera. Latest movement along these was controlled by magmatic consolidation rather than the shape of the caldera. Some flat faults were able to remain open during mineralization and acted as a feeder for the shallower fractures, thus limiting the depths to which the steeper dipping fractures were mineralized with the possible exception of one particular Nw.-striking lode (the Crown-Crescent).INTRODUCTIONThe gold deposits of the Tavua district were discovered in 1932 and from 1935 to June, 1961, 1,985,041 fine ounces of gold were produced from 4,202,504 tons of ore. Of the original three producers, only the Emperor remains active in the...

Jan 1, 1962

By L. W. Rowe, S. S. Cole

A laboratory bench scale unit is described whereby finely divided chlorinatable residues are held for a short period by a restraining bed of a coarse-grained ore of comparable composition to permit 'flash' chlorination of the high surface area powder. Results on chlorinating a finely divicled titania residue using rutile sand as the restraining bed showed that 92 pct utilization of chlorine and equivalent conversion of TiO2 in the fine residue to Ticl4 were attained with a dust loss of about 3 to 4 pct and an equivalent amount of ch1om'nation of the titanium values in the restraining bed. THE chlorination of coarse grain titaniferous ores; i.e., 20 to 150 mesh sizes in fluidized beds is practiced commercially.' One effective method found for the chlorination of a very fine material in a fluidized bed is the "flash" chlorination technique.' By charging the finely divided charge material into the bottom of an established bed of optimum sized rutile, ilmenite, titanium beneficiate, or even an inert material such as sand, chlorination occurs before the dust can pass through the bed. The major requirement is that the bed be less chlorinatable than the charge. In this process, the charge consists of a finely divided (between one and 50 µ) titania residue obtained from a titaniferous ore beneficiation process. The charge is blended with a 20 pct wt basis addition of 20 to 60 .mesh size low volatile coke (to minimize hydrogen chloride formation) and fed to the bottom of the bed with the chlorine gas stream. A ball check device is used to permit entry of the charge and prevent the bed from discharging when the gas flow is cut off. The coarse pieces of coke serve to reduce compaction in the charge mixture and permit sat]sfactory feeding without plugging or jamming. Feed and gas rates are adjusted to provide for complete reaction of the charge material, with 90 to 95 pct chlorine efficiency, and maintain a gas flow in the range of 0.4 to 0.6 ft per sec. The equipment consisted of a 3-in. diam mullite tube enclosed in an electric furnace. A bow-shaped 3/4 in. Saran tube fed the charge from an air lock type of feed hopper (to prevent the escape of the chlorine gas into feed bin) to the bottom of the bed. The charge rate was set by providing a small awiliary hopper below the feed hopper where a weighed portion of the charge could be discharged in a specified time interval into the main chlorine stream. The chlorine rate was measured by a flowmeter. The reaction tube was filled with a bed of Australian rutile ore, this restraining bed serving two purposes; i.e., it rapidly heated the fresh charge to the reaction temperature and retained the particles in the bed for a sufficient time for selective chlorination to proceed. Due to the fine particle size and open, porous structure of the charge, this reaction was almost instantaneous, and, with proper adjustment of feed and gas rates, very little fine material passed through the bed without reacting and only a very small fraction of the restraining bed was chlorinated. A typical reaction procedure was to fill the bench scale fluidized bed unit with a 1 kg charge of Australian rutile ore analyzing 95.5 pct TiO2, 0.6 pct FeO, a beach sand deposit 40 to 150 mesh size. When fluidized, the bed was approximately 2 ft in depth. The ore was fluidized with a 1:l mixture of chlorine and nitrogen at a rate of 0.40 ft per sec. This gas mixture was necessitated by the comparatively short bed depth; a larger unit, with a deeper bed, could be fluidized with chlorine alone without significant free chlorine loss. Feed rate was 8.0 g per min of beneficiated ilmenite analyzing 85.0 pct TiO2, 2.6 pct FeO plus 1.6 g per min of 20 to 60 mesh petroleum coke. The

Jan 1, 1962

By B. Bernstrom

A 22-ft diam, 7-ft long, wet autogenous grinding mill was installed in the new Cretaceous plant of the Jones & Laughlin Steel Corp. to prepare crude iron ore for concentration in spirals and flotation cells. The paper describes the flowsheet and gives a description of the operating and metallurgical results that have been obtained. These results include capacity, horsepower, operating problems and a comparison of pilot plant results with those obtained in commercial operation. The Cretaceous plant at the Hill Annex mine of the Jones & Laughlin Steel Corp. was designed with a wet autogenous mill for grinding low grade iron ore so that it could be concentrated by spirals and flotation cells. The plant, on the west end of the Minnesota's Mesabi Range, went into operation in June 1961, and preliminary operating and metallurgical information describing the performance of this mill can now be given. The crude is lean ore from the Cretaceous iron foundation. This formation is a beach deposit of Cretaceous age that overlies the Precambrian direct shipping and concentrating ores. This rock in nature is not extremely hard but is quite resilient, resisting blasting in mining and size reduction in milling. It contains hematite as water-rounded particles and other fragments of the underlying iron formation and adjacent rocks cemented together by a high alumina-silica ferruginous matrix. It is interspersed with hard dense hematite agglomerates and also contains granite pebbles and boulders that were not cleaned off during removal of the surface. It has a 3.48 sp gr and in the stockpile the material consists of frag-

Jan 1, 1962

By C. G. Rhodes, D. Kramer

The kinetics of precipitation of transient a phase during the transformation in U-16 wt pct Mo between 400° and 550°C were studied using quantitative metallography and electrica1 resistiuity measurements. The volume percent of a phase goes through a maximum in time, corresponding to a critical degree of progress of y' formation. prior to its re-solution after prolonged annealing. The fastest rate of a precipitation oc-cuvs at 500°C with a concomittant lowest peak of 9.5 vol pct a. At 450°C, 14 vol pct a, greatest fov any temperature, was observed after 24 hr witlz an associated slowest rate of formation. a precipitation at 400°C ceases after approximately 160 hr and the amount of a present remains unchanged after long times at temperature; no y' was observed metallographically at this temperature. IN the U-Mo system at 16 wt pct Mo, an ordering reaction takes place below 600°C, see Fig. 1, whereupon the random bcc solid solution, y, transforms to the ordered bct phase, y'."2 The new unit cell is constructed of three old unit cells somewhat distorted. While attempting to study the kinetics of this transformation it was observed that an unexpected phase was precipitating out early during the transformation anneal reaching appreciable amounts before disappearing after long times. The y' appeared in the presence of this new phase and after long times constituted the whole sample. Owing to the high optical activity of this unexpected phase under polarized light, it was suspected to be the a phase. Subsequent X-ray powder pictures confirmed this belief. The kinetics of a phase formation and disappearance is the subject of this paper. EXPERIMENTAL PROCEDURE A) Alloy Preparation. Alloys for this study were prepared by vacuum induction melting normal reactor grade uranium and 99.5 wt pct Mo pellets in thoria crucibles. Two ingots were prepared, and sections of the top and bottom of each ingot were chemically analyzed for uranium and molybdenum content. The results of the analyses appear in Table I. B) Metallography. Samples of 16M were wrapped in tantalum foil, sealed in evacuated (5 X 10"6 mm of Hg) quartz capisules, and annealed at 1110"C prior to being transferred directly to the transformation temperature. They were examined metallographically after increasing times to determine the progress of the transformation at 400°, 450°, 500°, and 550°C. The samples were prepared for metallographic examination by mechanical polishing with diamond paste and electrolytic polishing with a solution of glacial acetic acid and chromic acid. Since the y' phase is tetragonal, its presence can be detected by viewing the sample in polarized light. To increase the contrast between y' plates, the samples were electro-etched in a 10 pct oxalic acid solution. To reveal a phase in bright field (it can be seen in polarized light in the "as-polished" state), the samples were electro-etched in a solution of citric acid and nitric acid. To determine the vol pct a phase, a variation of the one dimensional systematic point count method as described by Hilliard and cahn3 was used. The

Jan 1, 1962

By J. H. Holden

Operations involving the processing of coal, oxygen, and steam into synthesis gas by means of two pressure-type gasifiers have demonstrated the effect of heat loss and operating variables on carbon gasified and oxygen and coal requirements. Carbon gasified is the fraction of carbon in the coal that is converted to gas. Oxygen and coal requirement is the quantity of each that is needed to produce a unit volume (M std. c.f.) of carbon monoxide and hydrogen. Operating pressure of the gasifiers ranged from 150 to 300 p.s.i.g. and coal was fed at 200 to 500 lb./hr./cu.ft. of reaction-zone space. Oxygen-to-coal ratios were 8.5 to 10.5 std. c.f./lb. Heat loss and residence time have opposite effects on carbon gasified; increasing the heat loss decreases the carbon gasified, but increasing the residence time (by raising the operating pressure or reducing the coal-feed rate) increases the carbon gasified. The effects of these two factors are difficult to separate because they usually change simultaneously. A comparison of the results obtained from the operation of two gasifiers with different levels of heat loss, however, permitted the effect of heat loss to be separated from that of pressure and coal-feed rate. When the results were deter- mined on the basis of constant heat loss, increase of the residence time increased the carbon gasified until the reaction virtually had come to completion. For example, at 150 p.s.i.g., decreasing the coal-feed ratio from 500 lb./hr./cu.ft. to 200 lb./hr./cu.ft. substantially increased the carbon gasified. At 300 p.s.i.g., however, changing the coal-feed rate had little effect on the carbon gasified because the reaction had almost reached completion and further increase in residence time resulted only in a negligible change.

Jan 1, 1962

By J. G. Haymes

This report by the Bureau of Mines is the first of two proposed papers on evaluation of spectrophotometric, spectrographic, polarographic, and other analytical methods for quantitatively determining impurities in high-purity tungsten. Some of the methods described are standard methods that have been successfully applied to determine low-level impurities, several are modifications of known methods, and some procedures are entirely original. The Bureau of Mines is actively engaged in tungsten research because tungsten has an extremely high melting point, in fact the highest of any known metal. The metallurgist must know the content of impurities in tungsten because of the marked effects even micro amounts of impurity elements have on its physical properties. The Bureau procured a number of analyzed samples of above-average purity from research laboratories of companies engaged in production and fabrication of tungsten. These samples were investigated by the analytical procedures of those companies for several metallic impurities. Subsequent analytical laboratory determination of impurities in these samples agreed with the analyses as reported. With this assurance that analytical methods were basically accurate for metallic impurities, procedures for the determination of several of these elements were modified to lower the limits of detection and increase the sensitivity of methods. Carbon and the gases hydrogen, nitrogen, and oxygen were determined by standard instrumental methods, modified to provide greater sensitivity for reliable determinations when content of these elements was low. After the reliability of the modified procedures was affirmed, they were used as a product evaluation guide in the development of a vapor-plating technique for the production of high-purity tungsten. The following list of elements can be determined by one or more of these methods: AI, B, Be, Ca, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, S1, Sn, Ti, V, and Zn. In addition, a vacuum-fusion method for the determination of H, N, and 0, and a conductometric method for carbon are described. Lower limits of determination and detection for each element listed are given.

Jan 1, 1962

By H. Warlimont

In recent investigations of the microstructure and crystallographic features of martensite by electgon microscopy,', '9 thin films (about 50 to l000A in thickness) have been used as specimens. It was found by W. Pitschl ,2 that the lattice relationships between the supefiaturated fcc matrix and the martensite formed in thin films were different from those observed after transformation in bulk material. Corresponding differences are to be expected in nucleation and in reaction kinetics in the formation of martensite in thin films, but have not yet been reported. In the course of the preparation of thin films of iron-base alloys for investigation by electron microscopy it was observed that films of alloys, whose martensite formation temperature (Ms) was below room temperature, formed martensite during the electrochemical thinning process conducted at or above room temperature. The chemical compositions and approximate bulkM,-temperatures of the three materials on which this observation was made are listed in Table I. The alloys were vacuum-melted from high-purity metals. It can be seen that the effect occurred in alloys that contain only sub-stitutional components as well as in alloys that contain carbon as an interstitial solute. The appearance of martensite formed in this manner is illustrated in Fig. 1, which represents a polished film of alloy No. 1 at XI0 magnification. The martensite plates can be recognized by their surface relief effects. In addition, heavily strained (owrinkledo) austenite can be seen near the edges of the film where it is thinnest and transformation stresses or strains can be accommodated by plastic deformation most easily. The nonuniform distribution of transformed regions is probably due to the varying thickness of the film. These observations were common to all materials listed in Table I. Because effects of supercooling or straining can

Jan 1, 1962

By R. W. Stahl

An emergency is defined as an unforeseen combination of circumstances that calls for immediate action. When applied to a coal mine, an emergency may call for prompt removal of the men to the surface through travelways other than the haulageway or intake airways, which are generally contaminated with irrespirable air as a result of an explosion or fire. Therefore, maintenance of adequate and travelable escapeways from all working areas of a mine is vitally important insurance against disaster. Several mine disasters could have been avoided if well-defined escape routes had been provided and made known to all mine employees. Such occurrences, unnecessary as they generally are, unfairly indict the industry when only a small segment thereof is involved. As a result of a rather recent disaster, which might not have happened if good escape routes had been provided, the Bureau of Mines decided to delve into the escape procedure to determine (1) what is being done in the industry and (2) what might be done at reasonable cost.

Jan 1, 1962

By G. V. Sullivan

This report summarizes the results of a preliminary study concerning manganese extraction from low-grade dolomitic materials from the Philipsburg district in Montana by the Dean-Leute ammonium carbamate process. Studies were made to determine the relationship between the variables involved in treating these materials by a roast-leach process and the amount of manganese extracted. The variables studied were the roast temperature, the roast particle size, the molar ratio of NH3 to CO2 in the leach solution, the liquid-solid ratio in leaching, the leach time, and the size of the particles being leached. The roast-leach studies were statistically designed, and the experimental results were evaluated by an analysis of variance.

Jan 1, 1962

By John D. Bardill

Data from extensive tests was obtained on friction-head losses of various sand slurries, composed of materials of different specific gravities and under varying transport conditions, to provide useful information for designing hydraulic transport systems. The tests were run in a pilot plant through 2-, 3-, and 4-inch lines with slurries composed of relatively pure barite and limestone solids. Available grinding and classification equipment did not permit attaining a comparable size distribution in the two materials tested, thus preventing direct correlation of friction-head loss values to physical properties or mineral composition. A total of 495 measurements were made of limestone slurries in the 2-, 3-, and 4-inch pipe test sections at flow velocities from 6 to 14 feet per second and pulp densities from 40 to 70 percent solids. A total of 640 measurements of barite slurries were made in the 3-and 4-inch pipe test sections at flow velocities between 7 and 14 f.p.s. and pulp densities ranging from 40 to 80 percent solids.

Jan 1, 1962

By V. F. Swanson

As part of the Bureau of Mines titanium resources examination program, samples of altered rock (saprolite) and unaltered rock from the Roseland anorthosite near Roseland, Nelson County, Va., were tested for amenability to beneficiation by flotation. A flotation technique was developed to produce bulk concentrates of ilmenite, rutile, sphene, and leucoxene. It was necessary to first float apatite using oleic acid as the collector, in an alkaline pulp with dextrine as a titanium mineral depressant. The titanium minerals could then be floated from the apatite tailing, using fluosilicic acid to depress the remaining apatite, morin to depress ferromagnesian minerals (when present), and oleic acid as the collector. A bulk titanium mineral concentrate, analyzing 66.0 percent Ti02 and 0.08 percent P205, was obtained from a sample of the unaltered rock which contained 5.45 percent TiO2 and 2.81 percent P205. Overall recovery in the concentrate was 47.1 percent of the total TiO2 in the ore. About 55 to 65 percent of the saprolite sample was clay and was removed by attrition scrubbing and decantation. The apatite prefloat procedure was applied to the saprolite sands; subsequent titanium mine: 1 flotation recovered 72.2 percent of the Ti02 in a bulk concentrate containing 65.1 percent TiO2 and 0.20 percent P205.

Jan 1, 1962