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By R. C. Annear

This report describes open, sublevel, and shrinkage stoping at the Greenwood mine, operated by Inland Steel-Co. The iron ore mine is in Marquette County, Mich., about 6 miles southwest of Ishpeming (fig. 1). The Greenwood is one of three active underground hard-ore mines on the Marquette range, the others being the Cliffs-Shaft and the Champion mines. The operation reflects an achievement in exploiting small, difficult-to-mine hard-ore bodies lying beneath a 200-foot overburden of glacial drift, which is partly water bearing. This report can indicate only briefly the efforts of personnel in overcoming adverse conditions in mining more than 2 million tons of ore, 80 percent of which was in lump form, for open-hearth production of steel. Significant data presented include descriptions of the principal mining methods employed, sublevel and shrinkage stoping; percent aged mining costs for the entire year 1957, covering both direct mining costs and general expenses; and performance records in units of labor, power, and supplies.

Jan 1, 1960

By Frank W. Cole, Sharanjit S. Dhillonn

A new method has been developed for calculating flowing bottom hole pressure in a gas well, using as a basis the general energy equation. Fundamentally, the method shows that a plot of flowing pressure versus depth for a gas well can be represented as a series of incremental .straight lines, with the accuracy in-creasing as the number of increments increase. It is shown mathematically that for most cases the slope of the flowing pressure versus depth curve is essentially constant, in which case a single calculation based on surface conditions will yield acceptable results. In all cases studied no more than two iterations were required for very good accuracy, and in most cases only one iteration was necessary. Several example calculations are shown and the results are compared to other commonly used methods of calculating bottom hole pressures These examples show that the method provides answers which are at least as accurate as other methods usually used, and results in a considerable reduction in computation time.

Jan 1, 1960

By J. H. Field

Results of studies by the Federal Bureau of Mines on a pilot-plant scale for removing hydrogen sulfide and carbonyl sulfide from gas mixtures by the hot carbonate system are given in this publication. Gases containing up to 10 pet. hydrogen sulfide and 48 grains carbonyl sulfide per 100 cu.ft. were treated. In most tests carbon dioxide also was present and was removed simultaneously with the sulfur compounds. Because the rate of absorption of hydrogen sulfide is much more rapid than that of carbon dioxide over a wide temperature range, selective removal of hydrogen sulfide occurred in the bottom section of the absorber near the point of gas entry. Hydrogen sulfide was removed to pipeline specifications with carbonate solutions by using split-stream flows in the absorber and regenerator.

Jan 1, 1960

By Byron E. Blair

This report describes procedures for using a high-speed camera to study blasting phenomena. Both quantitative and qualitative information can be obtained, provided that proper interpretations of the projected two-dimensional images are made. Geometrical relationships between object and image displacements are given in terms of horizontal and vertical angles of the camera optic axis with respect to the quarry face. Correction factors are given for obtaining true object displacements from image displacements in the camera film plane. The time of initial rock movement also is considered, and the control-ling factors of camera speed, scale factor, minimum increment of projection measurement, etc., are evaluated in terms of minimum time intervals. The high-speed camera and associated equipment are described, and field measurements and laboratory data analysis techniques are outlined. An analysis of a typical high-speed motion picture is made, and the application of the necessary correction factors is illustrated.

Jan 1, 1960

By A. G. Metcalfe, A. Siede

The hardening of annealed copper during fatigue testing appears to be independent of the applied stress and to occur largely within the first 4000 cycles. Copper hardened by fatigue is more resistant to annealing than copper hardened by static means, and softens by a multistage process. Creep studies at 300°C show that copper hardened by fatigue also has greater resistance to creep than statically hardened copper. Some theoretical explanations are discussed. RECENT interest in the behavior of metals subjected to fatigue stems from observations of phenomena which could not be explained by current theories of the structure of metals. In 1953 Bullen et al.l showed that the hardening caused by fatigue at low stresses did not cause severe bending of the lattice as did hardening by static methods. This was later confirmed by Wood, 'and Broom and Ham.3 Clarebrough et al4 showed that as the stress level used in fatigue hardening was increased, bending of the lattice was introduced, eventually approaching that of metals deformed by conventional cold-working methods. The type of hardening introduced by fatigue has other interesting characteristics. Kemsley5 showed that copper fractured by fatigue at low stresses resisted annealing as compared to copper hardened an equal amount by static means. The work of Clarebrough etal, shows that the manner of energy release during annealing differs for fatigue-hardened and statically hardened metal in both magnitude and temperature range of release. In addition to hardening of the lattice, fatigue has been shown to cause softening in materials previously hardened by static methods,5 and also in age-hardened alloys.7 The superposition of a small fatigue stress on the static loading of high-temperature alloys has been shown to increase their resistance to creep.' The present work was an attempt to determine the relationship between fatigue hardening, resistance to annealing, and the creep properties of pure copper. EXPERIMENTAL PROGRAM The program described here was designed to answer three questions: 1) Can stress-cycle combinations well below the failure values give significant increases in hardness? 2) Does hardening, under different stress-cycle combinations, give increase resistance to annealing? And if so— 3) Does superior resistance to annealing confer superior creep properties over statically hardened material? Three-quarter hard OFHC copper was annealed in vacuo at 550°C for 1 hr to produce a strain-free material having a fine grain size and uniform hardness. (The standard deviation of the mean hardness of the annealed samples was less than + 1.9 Dpn). Annealing was performed after machining the fatigue specimens so as to avoid work-hardened surfaces. Jigs were used to avoid distortion. The fatigue properties of the annealed copper were determined using an accurately aligned Baldwin-Sonntag SF1-U machine operating at 1800 cycles per min. This limited the minimum number of cycles which could be examined to about 4000 stress reversals. Since failure resulted in specimen damage, hardness increase with number of cycles was measured by testing specimens fatigued to different fractions of the failure values. The results are shown in Fig. 1, and are superimposed on the S-N curve of the copper in Fig. 2. The resistance to annealing of fatigue-hardened material was compared to that of material hardened by uniaxial tensile straining. Specimens hardened to equal values by both methods were progressively annealed for 1 hr at temperature in vacuo. After each annealing treatment the hardness was measured using a Leitz Durimet hardness tester with a 500-g load. At least five tests were made for each hardness determination. The standard deviation for individual specimens varied from 0.26 to 1.48 hardness points. The results are shown in Figs. 3 to 5. The discontinuous nature of the annealing process has been brought out by drawing idealized curves through the data points. This can be justified by the consistency of the results as well as by general agreement with results of Kemsley.5 The creep resistance of fatigue-hardened and

Jan 1, 1960

By C. O. Swanson

"OUR INTEREST in estimates of world reserves of lead and zinc is focussed mainly on the information they give about the sufficiency of metal supplies for the future. However, we soon realize that the estimates can be interpreted in several different ways. Accordingly, it is necessary to have some under-standing of the elements represented by a compilation of world re-serves, and we will start by examining the accuracy of the estimates and what they attempt to measure.Variations in Estimates of the ReservesIf we study the estimates of world reserves that have been published in recent years, we note immenediately that they vary over a considerable range. For example, an article by Shea in 1947 gave world reserves as about 36 million tons of lead and 60 million tons of zinc. Shea did not in elude the United States but I have added to his totals the estimates made by the Bureau of Mines for that country in arriving at the foregoing figures. For approximately the same date, the American Zinc Institute and the Lead Industries Association reported world reserves as about 50 million tons of lead and 77 million tons of zinc. A comparison of the two sets of figures shows a mean variation of 30 per cent. For individual countries the difference between estimates can be even larger. A few years ago the estimate of Canada's reserves made by the United States Bureau of Mines was 7.4 million tons of lead and 14.0 million tons of zinc, while the Gordon Commission reported 1 O. 7 million tons of lead and 26.0 mil-lion tons of zinc. In this case the mean variation was 55 per cent."

Jan 1, 1960

By J. R. J. Edwards

Jaspilite, a mineral consisting of silica and iron oxide in varying proportions, is one of the host rocks of the high grade ore deposits situated in the Middleback Range of South Australia. As a result of laboratory investigations, a flowsheet was postulated for the beneficiation of jaspilite to produce an acceptable grade product for feeding to blast furnaces, The flowsheet involved the reduction of the hematite in the haspilite to magnetite, the grinding of the reduced product to 95 pct minus 325 mesh Tyler followed by wet magnetic separation, hydroseparation and filtration to yield a magnetite concentrate. Agglomeration of the fine concentrate would then be necessary to meet the physical requirements of blast furnace feed. To prove the postulated flowsheet, to obtain a more accurate estimate of costs and to obtain design data for a commercial installation, a pilot plant was constructed at Whyalla, South Australia.

Jan 1, 1960

By C. M. Frost

Two Federal Bureau of Mines recycle hydrogenation experiments to prepare catalytic cracking feed stock were made at 3,000 pounds pressure with crude shale oil retorted from Green River (Colo.) shale in the gas-combustion retort. The hydrogenated product from the first experiment, made at 784° F., was used for investigating the effects of nitrogen content on catalytic cracking yields and for determining the quality of the catalytically cracked gasoline. Hydrogenated product containing 0.14 percent or more of nitrogen produced less gasoline when cracked in a CAT "A" unit than was obtained from East Texas light gas oil cracked at the same conditions; product containing 0.10 percent or less nitrogen produced a quantity of cracked gasoline equal to that obtained from the East Texas light gas oil. The catalytically cracked gasoline had research octane numbers calculated to be approximately 95 clear and 103 with 3 ml. of tetraethyl lead. The principal product from the second experiment, made at 828° F., was a low nitrogen content gas oil which was used for investigating the yields of cracked products obtained when it was catalytically cracked to different degrees of conversion. Yields of cracked products, when plotted as functions of conversion, were essentially the same, within the experimental range of the data, as published yields from catalytic cracking of East Texas heavy gas oil; however, yields from cracking the shale-oil product did not display the sensitivity to change of cracking temperature that has been found for East Texas gas oil.

Jan 1, 1960

By S. Saito, P. A. Beck

The crystal structure of MoNi3 was determined by means of X-ray diffraction. This structure is isotype with that of ovgered TiCu3. The lattice parameters are: a. = 5.064A, bo = 4.224A, co = 4.448A, and zf 0.157. If the orthorhombic distortion (slight relative to the corresponding orthohexagonal unit cell) is disregarded, the structure may be described in terms of a close-packed ordered atomic layer, stacked in the sequence: abab. The structztres of ordered TiCu3 and TiAl3 are homotectic. The three types of ordered hexagonal phases, iso-structural with TiNi3, MgCd3, and VCo3, are known to occur in AB3 alloys of transition elements of the first, second, ad third long periods. It was noted1 that phases with the TiNi3 structure occur selectively in alloys of Ti-group elements with Ni-group elements. In AB3 alloys of Ti-group and V-group elements with Co-group elements the AuCu3-type structure predominates.' The vCO3 structure, which was determined very recently,' has hexagonal symmetry, but the actual atomic arrangement here, too, is rather closely related to the ordered cubic structure of AuCu3-type. However, an ordered hexagonal close-packed structure of the MgCd3-type occurs in MOCO33 and WCO3.4 Consequently, the question arises as to whether or not the crystal structure of MoNi3 is also of the MgCd3-type. Grube and winkler5 found that MoNi3 has a hexagonal close-packed structure with a = 2.54A and c/a = 1.65. They pointed out that some additional weak diffraction lines could be observed in the powder pattern, which may have been due to an ordered atomic arrangement in this phase. However, no detailed information was obtained by them and the structure was apparently not further investigated by others. The present work was, therefore, undertaken in an attempt to determine in detail the structure of MoNi3, and to investigate the possibility of ordering. EXPERIMENTAL METHODS Alloys used in the present work were arc-melted in a water-cooled copper crucible under helium atmosphere. Electrolytic nickel and molybdenum, both 99.9 pct pure, were used. Chemical analyses were not made, but the melting loss was not higher than 2 pct for any alloy. Ingots were first homogenized at 1200°C for 48hr, quenched, heavily cold worked, and then annealed at 820" or 860°C for 1 week, followed by quenching in cold water. Powder specimens for X-ray work were prepared by crushing the heat-treated solid specimens. In order to remove strains, the powders were reannealed in evacuated scaled fused silica capsules for 6 hr at the same temperature at which the corresponding solid specimens were annealed. X-ray photographs were taken with an asymmetric focussing camera, using unfiltered CrK or CuK radiation. EXPERIMENTAL RESULTS The X-ray diffraction patterns of alloys containing 20.8, 25, and 26.4 at. pct Mo, homogenized at 1200°C, showed the face-centered-cubic structure of the Ni-base a-solid solution. It was revealed, however, by micrographic examination that the 26.4 at. pct Mo alloy contained in addition very small amounts of a second phase, in accordance with the phase diagram.6 On the other hand, the 20.8 at. pct Mo alloy after annealing at 820°C gave the X-ray diffraction pattern of the ordered face-centered-tetragonal MONi4.7 In this pattern several additional weak diffraction lines were also observed, corresponding to the strongest diffraction lines of MoNi3. The alloys containing 25 and 26.4 at. pct Mo after annealing at 820" or 860°C gave X-ray diffraction patterns, as shown in Tables I and 11, corresponding to MoNi3. Each one of the reflections which could be tentatively indexed on the hexagonal close-packed cell of Grube and Winkler,5 with the exception of the basal plane reflections, was split into a doublet, as seen in Table I. Since microscopically the alloy consisted of a single phase, it seemed probable that the lattice of MoNi3 is actually slightly deformed, as compared with the tentative hexagonal unit cell. In addition to these diffraction lines, several weak lines were also present, as shown in Table 11, which could not be indexed at all on the hexagonal close-packed cell considered. Satisfactory indexing of all diffraction lines observed was found to be possible by using an orthorhombic unit cell with ao = 5.064A, ft = 4.224A, and c = 4.448A. These values, whose accuracy is estimated to approximately ± 0.008A, correspond to 95.14A3 for the volume of the unit cell, and to an X-ray density of 9.50 g per cm3. If no attention were paid to the weak reflections listed in Table II, a reduced -unit cell of half the volume (a = 2.532A, b = 4.448A, and c = 4.224A), closely related to the orthohexagonal cell, might be used. The dimensions of the orthohexagonal cell of the same volume as the reduced cell are: a = 2.562A, b = 4.437 A, and c = 4.183A. It may be seen that in the reduced cell the a axis is slightly shorter, while the b and c axes are slightly longer than those corresponding to the orthohexagonal cell of the same volume. This slight orthorhombic distortion is re-

Jan 1, 1960

By B. C. Allen, W. D. Kingery

Surface tension and its temperature dependence have been determined for pure liquid Fe, Cu, Co, Ni, and Sn and for Fe-C, Co-C, and Ni-C alloys. The temperature coefficient of surface tension is negative for all these liquids. The surface tension and wetting behavior of tin and tin-titanium alloys on A120,, Si,N,, MoSi,, and Sic, as well as the behavior of titanium-containing nickel alloys on A1 20, have been determined over a wide temperature range. For all the solids investigated titanium additims markedly lower the contact angle. Some limits for the solid-surface energies have been calculated from liquid surface tension and wetting behavior. SURFACE tension and interface energy are important variables in a number of metallurgical and ceramic phenomena, and have been discussed at some length in connection with determining micro-structure of polyphase systems,' solid-state sintering,' thermal etching of grain boundaries, heats of solution and fine powders,'1 grain-growth phenomena,' the mechanical behavior of fine foils and fibers, nucleation, soldering and brazing,' and other phenomenz of academic or practical interest However, until recently few quantitative data have been available for high-temperature systems. Among available data are some indicating positive temperature coefficients for the surface tension of liquid copper,*,11,'2 cast iron,l3 and iron-carbon14 alloys. Although carbon was found to be not surface active in iron at 1570" some preliminary studies had indicated the possibility of a positive temperature coefficient for the eutectic composition at lower temperatures.16 One part of the present study has been largely concerned with determining the temperature coefficient of surface tension for several metals at elevated temperatures, In addition to surface-tension studies, the wetting behavior of alloys containing titanium has been investigated over a wide temperature range. Previous measurements indicated that titanium was selectively adsorbed from nickel at a liquid nickel-solid alumina interface,17 and the use of titanium hydride or titanium-alloy techniques for metal-ceramic soldering is well known. In the present study, previous data have been extended to new alloy systems, and measurements have been carried out with other oxidation-resistant ceramics. EXPERIMENTAL The sessile-drop method was employed to measure liquid surface tension and contact angle between liquid and solid, utilizing apparatus and techniques which have been described previously.'g The shape of a sessile drop depends on equilibrium between forces of surface tension tending to form a spherical surface of minimum area and forces of gravity tending to flatten the drop. Typical sessile drops are shown in Fig. 1. From precise measurements of maximum drop diameter and drop height the surface tension and drop volume were calculated. Four solid materials were employed as supporting plaques for the liquid-metal drops. Aluminum oxide (99.9 pct, J, T. Baker, reagent grade) was pressed and sintered at 1800°C. Molybdenum-disilicide powder (99.0 pct, Electro Metallurgical Co.) was pressed and sintered at 1650°C. Plaques were cut from silicon carbide (99.4 pct, hot-pressed at Alfred University) and silicon nitride (95.1 pct, with Al, Fe, 0 as major impurities, Norton Co.) rods. All plaques were polished, cleaned, and dried prior to use. A number of metals and alloys were employed. Chemical analyses of vacuum-melted ingots of iron, nickel, cobalt (National Research Corp.), commercial nickel-base alloys, electrolytic copper (International Smelting and Refining Co.), and tin (Mal-linckrodt Chemical Works) are given in Table I. Alloys were prepared in the laboratory by vacuum melting the base metal with either titanium hydride (Metal Hydrides, Xnc.) or spectroscopic-grade carbon (National Carbon Corp.). Nickel-titanium alloys contained between 0.001 and 0.005 pct oxygen and the ferromagnetic metal-carbon alloys contained 0.001 pct. Cylindrical metal specimens (1 to 2.5 g) were machined and bevelled at the bottom to insure a uniform advancing contact angle on melting. Before use the samples were acid-etched, cleaned with acetone, and rinsed in petrol ether.

Jan 1, 1960

Flue dust from the sintering of base metal sulphides was leached to remove cadmium and arsenic. Leach liquor contained cadmium, zinc and small amounts of other base metals as chlorides. Results are reported of the use of a cation exchange resin Zeocarb 225 to separate the base metals from the arsenic. The resin was eluted with sodium chloride or sulphate to give a solution of relatively concentrated cadmium suitable for recovery by zinc cementation. The limited solubility of sodium sulphate presented some practical problems which were investigated. Another problem was the precipitation of lead sulphate in the resin during elution.INTRODUCTIONWhen lead-zinc sulphides are sintered prior to smelting, the gases passing to the flue are mainly uncondensable but contain a certain proportion of sublimates and dust particles which deposit in the flue or are carried, after condensation in the gas stream, to some form of dust extraction equipment.The recovered dust is a complex mixture of base metal sulphates, sulphites, sulphides, chlorides and oxides, the composition depending on the original concentrates. A large proportion of the cadmium and some of the arsenic originally in the concentrates finds its way to this flue dust, the treatment of which can be a convenient means of removing these elements and controlling their concentrations in the main lead-zinc smelter circuit. However, disposing of this material represents an appreciable waste of base metals as well as a serious toxicity hazard.Sulphide Corporation Pty. Ltd. was faced with this problem in planning the flow sheet of the new lead-zinc smelter at Cockle Creek, N.S.W. From a test run carried out on a pilot plant at Avonmouth, U.K., using a mixture of lead and zinc concentrates, a sample of dust was obtained for...

Jan 1, 1960

By A. N. May

"This paper describes the present approach of the Mines Branch to the problem of measuring the stress condition in the interior of rocks surrounding underground openings. An instrument, which will be referred to as a stressmeter, has been developed at the Mines Branch to measure un-directional stress changes in absolute units. There are two modes of operation of this stressmeter. It can be regarded as a fixed instrument, in which case it is installed at the end of a diamond drill hole and left in position to record any subsequent stress changes taking place. Alternatively, three of the stressmeters can be used in conjunction with a trepanning opera-tion to allow the existing stress condition to be determined. The initial laboratory work and subsequent experiences in the field with the stressmeter are described. All the field development work on the stressmeter was made possible through the co-operation of Canadian Refractories Limited, Kilmar, Quebec."

Jan 1, 1960

By R. W. Coburn

The results of field experiments on wells which required stimulation indicated that engineered well-completions will cause an increase in ultimate recovery at reduced costs. Techniques and tools have been developed which can be used to establish well conditions most conducive to successful stimulation. Cementing, perforating and treating are bound together so completely that the success of one phase is completely dependent on the .effectiveness of the preceding phase. A method of determining the efficiency or effectiveness of any given well-stimulation treatment has been derived. Pressure behaviour during a treatment can be analyzed to yield the total percentage of the formation which has been treated.

Jan 1, 1960

By M. Smutz, C. J. Baroch, E. H. Olson

IN 1949 an orebody containing some 10 billion lb of recoverable rare earth metals was discovered in the Mountain Pass district of San Bernardino County, California.' The following year Molybdenum Corp. of America purchased a number of claims at the deposit and a mill on the property which had been constructed to process the district's gold ores. Average composition of ore from the San Bernardino deposit is less than 0.1 pct Tho2, 25 to 35 pct calcite, 10 pct rare earth oxides, 15 to 20 pct silica, and 30 to 40 pct barite.' Rare earth content of the ore analyzes 50.7 pct CeO2, 4.2 pct Pr6O11, 11.7 pct Nd2O3;, 1.3 pct Sm2O3,, and 34.3 pct La2O3 and others.' By floating the barite and depressing the bastna-site, Molybdenum Corp. of America produced a concentrate that contained 60 to 70 pct rare earth oxides. More than 25 pct of the rare earths, however, was lost in flotation. It seemed likely that a more economical method could be found. At the present time most of the rare earths in the concentrates are converted to rare earth chlorides, which are either fed to ion exchange columns for separation of the individual rare earths or reduced to misch metal. Current investigation shows that solvent extraction may achieve this separation more economically than ion exchange. The study reported here was undertaken to develop an economical method of preparing a pure rare earth nitrate mixture from California bastnasite ore. Results indicated that more than 98 pct of the rare earths could be recovered. Several possibilities were considered for processing bastnasite ore, but only the method outlined in Fig. 1 was investigated. This involved leaching the calcined ore with nitric acid. The nitric acid process is discussed under the following headings: 1) calcination of the ore, 2) leaching of calcine, 3) filtration studies, 4) solvent extraction, and 5) nitric acid recovery. Calcination: Since California bastnasite ore contains 25 to 35 pct calcite and about 10 pct bastnasite, calcination was needed to reduce the violence of reaction with nitric acid. Weight losses of 26 to 30 pct were obtained by calcining the ore at 900°C for I hr or at 800°C for 4 hr. Longer periods resulted in no further weight loss. Leaching the Calcine: When the bastnasite calcine was leached with 30 pct nitric acid for 8 to 10 days, rare earth recoveries of only 45 to 50 pct were

Jan 1, 1960

By J. P. McGee

As part of a joint U.S. Atomic Energy Commission-Federal Bureau of Mines program for using nuclear energy to supply process heat, a simulated nuclear loop has been constructed to test components. This loop has been operated for more than 1,800 hours at 100 p.s.i.g. Of this period, 23 hours were at 2,500° F. and higher; 540 at 2,000° to 2,500° F.; 840 at 1,500° to 2,000° F.; 200 at 1,000° to 1,500° F.; and 260 below 1,000° F. Leakage at flanges and welds was not a serious problem. A helium-recycle system with gas temperatures of 2,300° to 2,500° F. and a static pressure of 250 p.s.i.g. appears feasible. Difficulties were encountered with the recycle compressor due to thermal distortion of the impeller and shaft. The use of sealed bearings limits compressor operation to the life of the bearings.

Jan 1, 1960

By W. M. Nabors

As part of a program to promote conservation and efficient utilization of petroleum resources, Bureau of Mines engineers at the Morgantown (W. Va.) Petroleum Research Laboratory are studying secondary oil-recovery projects in the Appalachian region. The increasing demand for petroleum and its products and the increasing cost of exploratory drilling tend to emphasize the importance of improving the recovery of oil from known petroleum reserves. Published reports setting forth the pertinent facts of these operations may help others to profit by the experience. This report presents the results of a study of secondary-recovery methods used in West Virginia by the Piedmont Oil and Gas Co., the Ryan Oil Co., and Water floods , Inc., on their Roane County leases in the Walton and Clover Rush Run pools. The principal oil-producing horizon underlying the area studied is the Big Injun sand, at approximately 2,000 feet. The sand is often referred to as blanket sand because it underlies much of the State and is oil-productive in many localities. Most of the pools in the area were discovered during 1907 to 1910 and were similarly developed and operated.

Jan 1, 1960

By V. A. Nieberlein

This paper presents the results of research undertaken to recover titanium and columbium by low-temperature chlorination of low-grade columbium-bearing ilmenite concentrates, and to simultaneously remove chlorinated impurities from the volatile chlorides without resort to distillation. Coke-reduced ilmenite was chlorinated at 400° to 500° C., and the resulting TiC14 was free of most impurities before condensation. A heated purification column was used wherein various packing materials reacted chemically or physically with the impurities which passed through them in the vapor phase. A nearly water-white TiC14 product was obtained directly. The principal impurities in the titanium tetrachloride were: 0.02 percent Fe, 0.01 percent V, 0.05 percent A1, 0.04 percent Si, and 0.07 percent Cb. This is a less pure product than commercial TiC14. Most of the columbium was recovered as crude CbC15, requiring further refining.

Jan 1, 1960

By Charles T. Baroch

RESEARCH strengthened the position of cesium as the preferred material (commonly but erroneously called "fuel") for ionic propulsion engines. Its use as an element of the plasma thermocouple for generating electricity also seemed more likely. Domestic Production.-No domestic ore of cesium and rubidium was produced. San Antonio Chemicals, Inc., San Antonio, Tex., and Maywood Chemical Works, Maywood, N.J., continued to produce cesium and rubidium compounds including carbonate, chromate, hydroxide, nitrate, sulfate, and all four halides. Rocky Mountain Research, Inc., Denver, Colo., began producing various cesium and rubidium salts. American Potash & Chemical Corp., Los Angeles, Calif., offered cesium and rubidium for sale.

Jan 1, 1960

By N. P. Titkov

This paper presents the results of laboratory and pilot plant investigations for the development of efficient methods of beneficiating hematite ores from the Krivoi Rog, Kursk Magnetic Anomoly, Olenogorsk, and other localities. The tests included gravity, magnetic (in a high intensity field), flota¬tion, and magnetizing roasting methods. It was possible to develop efficient beneficiation methods depending on the mineral composition of the ore and degree of dissemination of ore and gangue minerals. The paper shows the relationship between the iron silicate and quartz content of the ore and the technologic indices of the various beneficiation methods. Some of the conclusions based on these investigations and the technical and economic computations related to the cost of one ton of pig iron produced from concentrates obtained by the various beneficiation methods are: 1. If the hematite ore is not disseminated uniformly, it is expedient to use a combined gravity and flotation process. Ore particles up to 50 am. in size are beneficiated by gravity (heavy suspension, jigging, and others) and yield a lump concentrate. The middlings from this process are recrushed and floated; 2. Finely disseminated hematite ores, containing small quantities (less than 5 percent) of iron silicates, are most effectively beneficiated by flotation. Anionic (sulphate soap, tall oil emulsion with various foam depressors) as well as cationic collectors may be used. Depending on the mineral and chemical composition of the ore, it is possible to obtain concentrates containing up to 65 percent iron with an extraction up to 94 percent; 3. Finely disseminated, mixed hematite-magnetite ores may be beneficiated by flotation or a magnetic separation-flotation process; 4. Finely disseminated hematite ores, containing large quantities of iron silicates and earthy hematite ores are most efficiently beneficiated by the magnetizing roasting method. This method will yield concentrates containing up to 68 percent iron with extractions up to 90 percent. Although beneficiation by the magnetizing roasting process is costly, it will nonetheless, when employed on this type of ore, yield the least expensive pig iron.

Jan 1, 1960

By Alla D. Mah

THERMODYNAMIC data for manganese and its inorganic compounds have not been critically surveyed since the work of Maier (31) 3 in 1934. At that time data were lacking or inadequate for many of the important metallurgical compounds. Experimental work, conducted during the intervening years, has supplied so many new thermodynamic values that it is again desirable to examine the available data and compile them into a single publication for handy reference. This paper consists of three main sections. The first summarizes the basic metallurgical thermodynamic data for manganese and its compounds, including heat capacities, entropies, heat contents, temperatures and heats of phase changes, vapor pressures, and heats and free energies of formation. All data available to May 1959 have been considered. The second section contains heats, free energies, equilibrium pressures, and equilibrium constants of reactions of manganese compounds, with special emphasis on metallurgical reactions. The third section supplies basic thermodynamic data for other elements and compounds encountered in metallurgical reactions of manganese, thus making it possible for the reader to conduct thermodynamic calculations without recourse to other literature.

Jan 1, 1960