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By A. A. Cochran

Methods of preparing small heats of steel containing radioisotopes were developed, and the techniques of stripping film autoradiography were used to detect and study the carbide and sulfide phases in titanium-bearing steels. Metallography had revealed areas of titanium sulfide and ferrite or pearlite adjacent to areas of titanium carbide and ferrite, and unidentified, irregular phases at the boundaries between these two areas. Sulfur 35 was used to deter-mine the extent of the titanium sulfide inclusions, and carbon 14 was used to delineate the titanium carbide phase. Individual radioactive areas were located with a resolution of approximately 10 microns. A general background exposure that was not correlated with microscopically visible phases was observed in the carbon 14 autoradiographs. The evidence from both sulfur 35 autoradiographs and carbon 14 autoradiographs indicated that the unidentified inclusions were sulfides rather than carbides. INTRODUCTION The use of radioisotopes to facilitate the work at the Rolla Metallurgy Research Center was expanded in fiscal year 1959 when the Bureau of Mines authorized the installation of an intermediate-level radioactivity laboratory. Before this time, sealed cobalt 60 sources had been employed for radiography, but no tracer work was done. The primary objective of the first experiments conducted in the new laboratory was to supplement physical metallurgy investigations of selected problems in steel research.

Jan 1, 1962

By R. E. Perry

To develop new or improved flotation methods for beneficiating low-grade red iron ores, the Bureau made many bench scale and continuous anionic flotation tests on ferruginous sandstones and calcareous iron ores from the north-eastern part of the Birmingham, Ala., iron district. The ores contained about 21 to 36 percent iron, a to 11 percent lime, and 22 to 64 percent silica. Production of iron concentrates containing 48 to 52 percent iron was technically feasible in batch tests, and the iron recoveries ranged from 85 to 92 percent. In continuous tests 49 to 51 percent iron products were obtained with 80 to 90 percent recovery.

Jan 1, 1962

By Richard D. Graves

Pitch from low-temperature carbonization of bituminous coal was hydrogenated at cracking conditions in a continuous bench-scale unit to produce low-molecular-weight oils and tar acids. The pitch contained 15.6 pct benzene-insoluble material, 4.0 pct hexane-soluble oil, and 80.4 pct asphaltene by weight. At 475° C, 7,500 psig, and 1.5 hours residence time, hydrogenation products, based on the weight of pitch, were about 36 pct oil boiling below 325° C, 24 pct hexane-soluble heavy oil, 17 pct asphaltene, 1 pct benzene insolubles, and 12 pct hydrocarbon gases. The yield of tar acids boiling below 250° C was 4.3 pct, and the yields of C6 to C8 paraffins, naphthenes, and aromatics were each less than 1.0 pct. The yield of tar acids was within the range of yields obtained by hydrogenation or high-temperature carbonization of bituminous coal (2 to 5 wt pct). Yields of oil boiling below 325° C increased with increased residence time or temperature. There was little or no effect of residence time on yields of alkali- soluble material which contained tar acids. Yields of hydro-carbon gases increased markedly with an increase in temperature from 475° to 500° C. Lowering the hydrogen pressure to 4,500 psig resulted in yields similar to those obtained at 7,500 psig.

Jan 1, 1962

By Raymond W. Hiteshue

To aid in designing a continuous system for evaluating processes for converting coal to high-Btu gas] the Bureau of Mines determined the amenability of various coals and a char to hydrogasification at 800° C and 6,000 psig using a molybdenum catalyst. A lignite from Rockdale, Tex., an hvCb coal from Rock Springs, Wyo., a char from the low-temperature carbonization of the latter, an hvAb coal from Pittsburgh, Pa., and an anthracite from Luzerne County, Pa., were selected. Highest yields of gaseous hydrocarbons, 94 pet, based on maf feed, were produced from char, and lowest yields, 67 pct, were obtained from lignite. Hydrocarbon gases contained 82 to 92 pct methane, 8 to 15 pct ethane; and 1 to 3 pct propane.

Jan 1, 1962

By A. J. Forney

The hot-gas-recycle process, for the hydrogenation of carbon monoxide, was investigated in a 12-inch-diameter reactor. Initially because the distribution of gas was poor, hotspots developed in the catalyst bed. After the velocity profile of the gas flowing through the bed was studied, the method of packing the catalyst was altered. Because this change improved the distribution of gas, temperature control was excellent. The l2-inch-diameter reactor was operated successfully in the synthesis of gaseous and liquid fuels. When high-Btu gas was synthesized in two stages, parallel-plate assemblies of Raney nickel were almost as active as granular Raney nickel in the second reactor. The pressure drop through the second reactor, however, was reduced 90 percent by the use of these assemblies.

Jan 1, 1962

By Michael G. Zabetakis

Investigation of gas explosions usually reveals that the combustible gases have come from transmission and storage facilities or from natural gas or oil wells. However, combustible gases such as methane and hydrogen can derive from biological processes. Hazardous situations have been created in the past by the use of abandoned mines for the disposal of sewage and rainwater, by the interconnection of storm and sanitary sewers, by sealing the openings in manhole covers when repaving the roadway over a sanitary sewer, and by the construction of buildings over or near garbage fill areas without adequately providing for the release of combustible gases.

Jan 1, 1962

By John Fitzpatrick

In this Bureau of Mines investigation a device was developed that permits the determination of the modulus of elasticity of the stress-relief cores obtained in the process of making in situ stress measurements. This determination is made by hydraulically loading the external surface of the stress-relief cores and by measuring the corresponding borehole deformation. The theoretical relationship between the borehole deformation, the applied pressure, and the modulus of elasticity is presented. Also, experimental results obtained from measurements on a simulated stress-relief core made of aluminum and on a limestone stress-relief core are given. Because of the symmetrical loading obtained with this device, the isotropy of the core material can be evaluated. With this device it is also possible to study the effect of eccentricity, that is, the effect within cores in which the inner hole is not coincident with the long axis of the specimen.

Jan 1, 1962

By James A. Whelan

The Bureau of Mines sponsored research studies of variables in rotary drilling, done in the Department of Mineral Engineering, University of Minnesota. By studying carefully controlled drilling with good instrumentation, it was hoped to obtain a better understanding of rock failure during drilling and of the stresses in drill bits during drilling. Experimental procedures and equipment are described. From these studies it was concluded that 1. Thrust requirements, other things being equal, are proportional to the total length of cutting edge in the bit. 2. Data from penetrating a wedge into rock under thrust only are not directly applicable to rotary drilling. 3, In rotary drilling the initial wear on a bit greatly decreases penetration rate under any given set of conditions; however, after initial wear the effect of wear on penetration rate is reduced. 4. An increase in rotary speed increases the overall penetration rate but decreases the penetration per revolution. 5. An increase in thrust increases the overall penetration rate and the penetration per revolution. 6, Torque on a drill bit is proportional to both penetration rate and bit diameter. 7. For small-diameter holes full-hole drilling will save both drilling time and energy compared with pilot drilling followed by reaming; for large-diameter holes pilot drilling-reaming is advantageous in both respects,

Jan 1, 1962

By W. W. Weller

This report provides low-temperature heat-capacity data and entropies at 298.15° K. for magnesium metavanadate (MgV206) and magnesium pyrovanadate (Mg2V207). The work completes low-temperature measurements planned for alkaline-earth vanadates; an earlier report dealt with calcium vanadates.4 No similar data for these compounds have been published previously. Free energy of formation values at 298.15° K. were derived by combination of the present entropy values with heat of formation data. MATERIALS The materials used in the measurements were portions of the samples described in a previous Bureau of Mines publication by King, Koehler and Adami.5 Methods of preparation, chemical analyses, and X-ray examinations are covered in this paper. The indicated purity of the samples was 99.9 pct.

Jan 1, 1962

By R. E. Lindstrom

Effective separation of rare-earth mixtures is obtained using hydrogen as a retaining ion at 200° F with ethylenediaminetetraacetic acid (EDTA) eluant. Results obtained in Bureau of Mines bench-scale apparatus and large columns with hydrogen as a retaining ion closely parallel those obtained with copper as a retaining ion. The use of hydrogen as a retaining ion permits EDTA and water, collected before rare-earth breakthrough, to be recovered in a form that allows the material to be recycled without extensive processing. With the exception of yttrium and dysprosium, separation of rare-earth mixtures is improved and throughput is increased by elevated temperatures. Separation with 1,2-diaminocyclohexanetetraacetic acid (DCTA) eluant increases markedly on increasing temperature from ambient to 250° F; however, on the basis of separation efficiency, DCTA does not compare favorably with EDTA.

Jan 1, 1962

Spectrochemical methods were developed to determine beryllium in the concentration range 0.0015 to 4.0 percent in siliceous mineral beneficiation products. Two methods are described. They are (1) a fusion-pellet-spark procedure (spark method) and (2) a sustaining alternating-current arc procedure (arc method). In the spark method the sample is fused with lithium tetra-borate and vanadium pentoxide. The resulting bead is crushed, mixed with powdered graphite, and briquetted. This is analyzed spectrographically using controlled high-voltage spark excitation. In the arc method the sample is diluted with germanium metal, graphite, and vanadium pentoxide. Weighed charges are packed into cupped graphite electrodes and subjected to excitation with a sustaining alternating-current arc. Vanadium serves as internal standard for both methods. Effects due to matrix variations in samples and standards are eliminated either by fusion with lithium tetraborate in the spark method or by dilution with germanium and graphite in the arc method. Beryllium determinations show deviations from accepted chemical values of approximately 5 and 8 percent for the spark and arc methods, respectively. Analyses can be made more rapidly by the arc procedure with a sacrifice in precision and accuracy. Either method can be applied to the determination of beryllium in silicate rocks.

Jan 1, 1962

By Frank A. Peters

This Bureau of Mines report is the second of a series of process evaluations planned to determine the relative processing costs of producing metallurgical-grade alumina from low-grade aluminous materials. Included in these evaluations are recommendations for additional research and development to improve the processes and to lower their costs. The design for each process is based on published work. The processes considered in this report are designed to extract alumina as aluminum chloride from calcined clay with 20 percent hydrochloric acid and to remove the silica residue by filtration. Iron is removed by one of the following processes: Isopropyl ether extraction, in which iron chloride is extracted before decomposing the aluminum chloride; gas precipitation, in which the aluminum chloride is precipitated with hydrogen chloride while leaving the iron chloride in solution; gas precipitation-isopropyl ether extraction, in which the aluminum chloride from precipitation is extracted with isopropyl ether, if necessary; caustic purification, in which a crude alumina is produced and then purified by a modified Bayer operation; or sinter purification, in which a crude alumina is produced and then purified by a lime-soda sinter operation. For plants producing 1,000 tons of alumina a day the estimated operating costs per ton of alumina are: [Isopropyl ether extraction process $ 65.09 Gas precipitation process 89.04 Gas precipitation-isopropyl ether extraction process 119.65 Caustic purification process 73.79 Sinter purification process 80.47] The estimated fixed capital costs per annual ton for these plants on a Marshall and Stevens chemical equipment basis of 240.0 are: [Isopropyl ether extraction process $229.03 Gas precipitation process 287.16 Gas precipitation-isopropyl ether extraction process 356.59 Caustic purification process 266.48 Sinter purification process 279.13]

Jan 1, 1962

By C. H. Riggs

This report describes the development, oil recovery, and potentialities of productive formations in the Hall-Gurney field, Russell County, Kans. It is presented as part of a general program to aid and promote increased recovery from petroleum reservoirs. The report is based on studies of well logs, drill cuttings, and oil-and water-production histories of individual wells and leases. The geological interpretations follow closely those in published literature with only slight local modifications. Oil and water analyses, made at a Bureau of Mines research center, were supplemented by many analyses obtained from oil-producing and service companies. The Hall-Gurney field, in south central Russell County, Kans., (fig. 1) was discovered in 1931 but was not developed extensively until 1941. By 1960 the rate of oil production from the field had declined to the extent that many wells were abandoned. In some areas natural productive forces have effected good recovery. However, in other areas inefficient waterflooding, both natural and accidental, has adversely affected recovery potentialities.

Jan 1, 1963

By J. T. Schimmel

The purpose of this investigation was to obtain complete information on some of the uses of a 24-inch-diameter auger in the underground mining of pitching anthracite beds. The auger was placed in operation early in 1958 to drive ventilation connections between coal gangways driven by a continuous miner. Although designed to drill rise holes only, it was used also to drill dip holes. The latter holes were drill id from an adjacent gangway to avoid interference between the auger and the continuous miner. These holes established immediate ventilation returns when intersected by the continuous miner. Bureau participation in the project covered 361 working days. The auger was used on 288 shifts, usually one 7-hour shift per day, and drilled 3,246 feet, of which 493 feet were reamed. The longest hole was 87 feet; hence the maximum drilling depth of the machine (rated at 100 feet) was not required. Holes drilled normal to the strike of the bed ranged from 30 to 66 feet deep, averaging 45 feet. The continuous miner drove gangways on 575 shifts. Thus, the auger worked one shift for each two worked by the continuous miner and was used on less than 80 percent of the workdays. The auger drove 24-inch holes 10 times faster than the larger, conventional openings could have been driven by usual mining methods and exceeded the workload for which it was purchased. Augering eliminates exposure to the hazards encountered in driving chute-work by conventional methods and provides adequate circular ventilation openings, which are strong in self support and are adaptable to reaming when required. With alterations, the auger may have limited use as a production machine in thin-bed pitch mining but cannot compete with established methods of thick-bed pitch mining.

Jan 1, 1962

By T. E. Gray

This report describes the preparation characteristics of the significant coalbeds in Nicholas County, W. Va. It is one in a series describing coals suitable for producing metallurgical coke, either as mined or after beneficiation. Almost 5 million tons of coal were produced in Nicholas County, W. Va., in 1960, of which over 2.6 million tons were cleaned in eight preparation plants. It has been estimated that over 6 billion tons remained in the county as of December 31, 1960, in beds 12 inches and more thick.

Jan 1, 1962

By Stephen Utter

This report summarizes the procedure and results of an investigation to determine the stresses in the rock around an underground opening in the Climax molybdenum mine, Climax, Colo. This study is part of an overall investigation conducted by the Bureau of Mines to determine the stresses induced by block-caving mining. The purpose of this study is to obtain estimates of the magnitudes and directions of the principal stresses, the location of the maximum stress concentrations, and the effect of topography on the stresses.

Jan 1, 1962

By Louis A. Panek

Tests of mine-roof models in a centrifuge show that the suspension effect due to bolting a horizontally bedded mine roof with frictionless surfaces of contact between beds depends principally on the number of bolted beds and their relative flexural rigidities, provided that sufficient bolt tension is exerted to prevent strata separations at the bolt locations. Strata separations tend to occur in the unbolted roof mainly because the beds have unequal thicknesses. "Suspension effect" refers to the transfer of part of the weight of weaker or thinner beds to the flexurally more rigid beds by roof bolts or by any other means. The factors investigated were number of beds in the bolted unit, bed thickness, modulus of elasticity of beds, length of bolts, spacing of bolts across and along the opening, bolt load, and intensity of roof load. The general principles of behavior of the bolted roof beds are explained by an approximate theory. Model test data are used to validate the theory and to obtain an expression for the "suspension efficiency". As the suspension effect actually observed in the models is smaller than that predicted by the approximate theory, the suspension efficiency in general is less than unity. Mathematical expressions are obtained for (1) the change in roof bending stress due to the suspension effect, which is needed for design of a roof-bolting system, (2) the change of roof deflection due to the suspension effect, which may be useful for evaluating the effectiveness of a roof-bolting system, and (3) the bolt load or pre-load that is required to achieve the desired reinforcing effect.

Jan 1, 1962

By Louis A. Panek

This report deals with the combined friction and suspension effects in the reinforcement of horizontally bedded mine roof by bolting. Other reports have treated these two effects separately. Friction effect refers to the reduction of bending in a laminated roof due to the clamping action of tensioned bolts. If the beds tend to have unequal deflections, the bolts oppose this tendency, thus creating a suspension effect, which consists of a transfer of part of the weight of weaker or thinner beds to the flexurally more rigid beds within the bolted unit. The combined effects of friction and suspension on the bending of the beds, whether an increase or a decrease, are difficult to generalize because they depend on the bedding sequence and the bolt pre-tension. Some analysis of the bedding sequence usually is required to determine the critical bed within a set of bolted beds. However, if the suspension effect is substantial and if the bolts are pre-tensioned, then the greatest bending stress is likely to occur in the thickest bed. Findings are based partly on theory and partly on tests of mine-roof models in a centrifuge, which were found to verify the theory. Mathematical formulas are obtained for the change in maximum roof bending stress and for the change of roof deflection due to the combined friction and suspension effects. The maximum bending stress is needed for designing a roof-bolting system and the deflection for evaluating its effectiveness.

Jan 1, 1962

By Webster S. Anderson

Two series of tests were run with planer model 'BB": one at the Arickaree mine of the San Francisco Chemical Co., Rich County, Utah, and one at the Roslyn No. 9 mine of the Northern Pacific Railway Co., Roslyn, Wash. The tests at the Arickaree mine were started on June 25, 1958, and continued until September 30, 1958. Prior to these tests, an electrically activated remote-control system was installed, and other modifications were made on the planer. The tests showed that the planer in general and the remote-control system worked very well; however, the various cutting tools used would not consistently penetrate and cut the phosphate rock. This indicated that the cutterhead design had to be changed before the planer would operate efficiently in phosphate beds similar to the "A" bed in the Arickaree mine.

Jan 1, 1962

By Raymond P. Maloney

The Rhyolite mercury prospect is on the south flank of Juninggulra Mountain--a large rhyolite intrusive in the Kuskokwim River region about 36 airline miles northwest of Red Devil, Alaska. Bulldozer trenching by the Bureau of Mines exposed bedrock at intervals in a 2,000-by 3,000-foot area where previous prospecting by the owners had disclosed abundant float and several in-place stringers containing cinnabar in widely varying amounts. The additional trenching indicated that the mercury mineralization in the limited area investigated was confined to erratically distributed short stringers and to small lenses, occurring in discontinuous zones in numerous silica-carbonate dikes and sills or along their altered contacts with sedimentary rocks. The geologic relationship of the mercury-bearing silica-carbonate dikes and the nearby rhyolite intrusive is similar to that existing at several other mercury mines and prospects in the. Kuskokwim region. The depth of over-burden and the presence of permafrost were serious obstacles to bulldozer trenching, and only a comparatively small part of the mineralized area was thus investigated.

Jan 1, 1962