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By H. J. Heinen

A technique offering promise as a metallurgical processing sequence the recovery of molybdenum (Mo) from the sulfide mineral--molybdenite?was investigated. The method consists of two steps: (1) electrosynthesis of pure dimolybdenum carbide (Mo2C) from molybdenite (MoS2) and (2) interaction of Mo2C and molybdic oxide (MoO3) to produce pure molybdenum metal. Two molten salt systems were satisfactory for electrosynthesizing Mo2C. The first was a mixture of potassium chloride (KCl), potassium fluoride (KY), and sodium metasilicate (Na2SiO3), and the second consisted of sodium fluoride (NaF), KF, sodium tetraborate (Na2B4O7), and sodium carbonate (Na2CO3). Yields up to 0.42 gram of Mo2C per ampere-hour were obtained. The carbide, mixed with monitored amounts of MoO3, was converted to molybdenum metal of 99.9 percent purity by sintering at 1,500° C.

Jan 1, 1965

By Tilman M. M.

The effects of substituting cobalt for nickel on the acid corrosion resistance of two types of austenitic stainless steel were determined. Cobalt substitutions to a maximum 2.2 weight-percent were made in types 302 and 309 stainless steels. Total immersion corrosion tests were made in 10 volume-percent hydrochloric acid, and boiling-acid tests were conducted in 65 weight-percent nitric acid and in undiluted glacial acetic acid. For modified type 309 in acetic acid, corrosion rates decreased for additions greater than 0.57 weight-percent cobalt. Corrosion rates increased as cobalt was increased up to about 1 weight percent for modified type 302 in nitric and hydrochloric acids and for modified type 309 in nitric acid, but these rates decreased with a further increase in cobalt content. A gradual increase in corrosion rates with increasing cobalt content was shown for type 302 in acetic acid and for type 309 in hydrochloric acid. Cobalt substitutions in larger amounts (above a ratio of 8 Ni to 1 Co) may increase the corrosion resistance of the austenitic stainless steels.

Jan 1, 1965

By L. B. Pankratz

Heat content measurements were conducted for GaPo.996 and InPo.986 over the temperature range from 298° to 1,100° K, and for In2S2.897 over the range from 298° to 1,200° K. Both the actual experimental data and values adjusted to conform with the stoichiometric compositions (GaP, InP, and In2S3) were reported. Entropy increments above 298.15° K were calculated for the stoichiometric compounds, and heat content and heat capacity equations were derived.

Jan 1, 1965

By R. V. Lundquist

The compound 2Na2O?3CaO?5Al2O3 occurs as a minor phase in lime-soda sinters prepared for extracting aluminum from siliceous aluminum-bearing materials. About 99 percent extraction of sodium and aluminum from synthesized 2Na2O.3CaO.5Al2O3 was obtained in solutions of NaOH-Na2CO3 at leaching temperatures of 50° C and above. Extractions in water were low because insufficient NaOH was generated by hydrolysis. Extractions in NaOH solutions were limited to about 80 percent owing to the precipitation of hydrated calcium aluminates. Rapid extractions of 100 percent were obtainable in NaaC03 solutions, but the subsequent rapid precipitation of alumina trihydrate caused losses in alumina recovery.

Jan 1, 1965

By D. K. Deardorff

The hafnium-vanadium phase diagram was constructed within an estimated accuracy of ± 10° C and ± 2 wt pct composition. Alloys for investigation were melted under an atmosphere of purified helium by nonconsumable tungsten-electrode arc melting on a water-cooled copper hearth. Melting points were determined by optical pyrometer, and the remaining phase relationships were investigated by metallography, thermal analysis, and X-ray diffraction. The existence of a face-centered cubic intermetallic compound HfV2 (a = 7.38 A) was confirmed. A eutectic reaction occurred at 20 wt pct vanadium and 1,395° C to yield HfV2 and 8 solid solution. HfV2 melted incongruently by a peritectic reaction at 1,480° C, and the 3 solid solution decomposed eutectoidally at 1,165° C and 6 wt pct vanadium to yield HfV2 and a solid solution. The eutectoid, the eutectic, and the peritectic isotherms extended from 1 to 36.3 wt pct vanadium, from 8 to 36.3 wt pct vanadium, and from 26 to 89.5 wt pct vanadium, respectively. Terminal solid solubilities of hafnium in vanadium at 1,300° C and of vanadium in hafnium at 1,100° C determined to be about 3 and 1 wt pct, respectively.

Jan 1, 1965

By Edward W. Parsons

The explosive-anchored rockbolt was field tested in six mines where rock conditions varied from incompetent shale or mudstone through fairly soft sand-stone to firm sandy shales. The purpose of the testing was to document, under a wide variety of conditions and in comparison to other rockbolt anchors, the quality of the anchorage produced by the explosive-anchored bolt. In addition, the length, strength, and design of the explosive charge necessary to produce positive anchorage up to the yield strength of the weakest component of the bolt were determined. A l4-inch length beaded explosive charge was found to be suitable, in general, in relatively weak strata, and the length can be reduced in more competent strata. Of the 127 explosive?-anchored bolts tested, 118 bolts produced an evaluated anchorage in excess of 17,000 pounds. Only 4 of 43 expansion-shell bolts and 4 of 14 wedge bolts produced anchorage this good. In preliminary tests, properly coupled explosive-anchored bolts did not ignite an explosive gas mixture. Some minor phases included in the investigation were as follows: (1) effect of explosive-anchored rockbolt on surrounding rock; (2) effect of time on anchored bolts based on torque tests; (3) effect of submersion in water on rockbolt anchorage; (4) pull tests to higher loads; and (5) ignition tests.

Jan 1, 1965

By R. C. Buehl

A pyrometallurgical process for recovering manganese from open-hearth furnace slags or low-grade manganiferous iron ores is described. The slag or ore is smelted in a blast furnace to produce spiegeleisen; the speigeleisen is then blown with air in a basic converter to give an oxide slag. This slag product contains 60 to 75 percent manganous oxide and may be considered a synthetic manganese ore. In the smelting operations coke rates for five test periods ranged from 3,255 to 4,130 lb per ton of spiegeleisen. The recovery of manganese in the spiegeleisen varied from 60 to 76 percent. Recovery increased to 83 percent when the open-hearth slag feed to the blast furnace was diluted with a high-? grade iron ore sinter to facilitate smelting. In blowing the spiegeleisen a cyclic procedure was developed that gave nearly 90 percent recovery of manganese in the slag product (synthetic ore) yet prevented excessive contamination of the slag by phosphorus and iron. The overall recovery of manganese was about 75 percent when iron ore sinter was used with the open-hearth slag in the smelting step. The metal remaining after oxidizing the manganese from the spiegeleisen contained approximately 3.5 percent phosphorus. It was refined in a basic converter by blowing with air in the presence of lime" A high--grade iron and a basic phosphate slag were produced.

Jan 1, 1965

By John Nagy

Dust explosion data obtained in laboratory studies by the Bureau of Mines are presented for activated carbon, asphalt, charcoal, carbon black, coal, coke, gilsonite, graphite, lignite, miscellaneous carbons, pitch, tunnel dust, and mixtures of these materials with other ingredients. The explosion hazard is shown to increase as the volatile content of the dusts increases.

Jan 1, 1965

By Robert M. Becker

This report (part 3 of a five-part series) presents computer programs for evaluating moments and moment relationships of the generalized probability distributions extended or developed in parts I and 2. The principal program is for evaluating the first three moments and moment relationships of the compound-multinomial distribution for finite as well as for infinite populations. This is the generalized distribution for sampling to some amount of items per sample. Another program is for evaluating the first four moments, the moments of the mean, and the moment relationships of the multinomial and generalized hypergeometric distributions. This is a general moment program in sampling to some number of items per sample or for sampling to some number of samples. This program will accept either ungrouped data, frequency data, or probability data.

Jan 1, 1965

By H. Dolezal

An investigation was made on the use of magnesium for the direct reduction of rutile to make low-cost, offgrade titanium which could be upgraded to an acceptable grade of metal by electrorefining. Reductions made with charges containing magnesium chloride under hydrogen yielded products with oxygen con-tests close to the theoretical equilibrium composition. Two reduction products were made from rutile for use in electrorefining amenability tests: (1) a product from reduction in an inert atmosphere which contained 88.9 percent titanium and 4.42 percent oxygen, and (2) a product from reduction in a hydro-gen atmosphere which contained 92.5 percent titanium and 2.40 percent oxygen. Reduction products obtained under both of these conditions were amenable to electrorefining.

Jan 1, 1965

By A. A. Sonnek

A simple, portable helium analyzer was developed primarily for field use. Its utility lies in making preliminary surveys before exact analyses are required. The analyzer is based upon chromatographic principles; that is, separation of gas mixtures resulting from variable retention times of the components with respect to a separation medium (column-packing material). It uses thermistors for sensing detectors, a dry battery as source of power, and a micro-ammeter for indicating helium concentration. The absolute accuracy of the instrument depends upon the recency and care with which the instrument is calibrated with a standard gas. The unknown gas should be analyzed immediately after calibration, and another calibration should be made before another unknown sample is analyzed. The instrument is simple to operate, requiring approximately 15 minutes, after calibration, to determine the helium content of a natural gas sample. Although developed primarily for helium determination, the analyzer possibly can be used for other analyses that can be performed at ambient temperatures.

Jan 1, 1965

By J. G. Eisele

Solvent-extraction characteristics of dodecyl phosphoric acid (DDPA) were investigated to determine its potential as a fractional or selective extract-ant for individual elements in a rare-earth-yttrium mixture. The DDPA is an effective extractant for splitting rare-earth mixtures into light and heavy subgroups. Yttrium normally extracts with the heavy rare-earth elements but may be shifted toward an extraction sequence with the light rare-earth elements by increasing the pH. Elements in the light and heavy ends of the rare-earth series can be separated from middle-group rare-earth elements by using diethylenetriaminepentaacetic acid (DTPA) as an aqueous phase counter-extractant. Hydrogen-ion dependency of the distribution coefficients differs from that reported for similar systems at tracer-level concentration.

Jan 1, 1965

By George L. Gates

The Bureau of Mines developed a rapid instrumental method of analyzing oil well scales containing primarily barium sulfate. After removal of oil and water by carbon disulfide) the scale was dissolved in strong hydrochloric acid. The cations, barium, calcium, strontium, magnesium, and iron, were determined with the flame photometer using the method of additions. Sulfate was deter-mined colorimetrically after separation by selective adsorption on an alumina column. Phosphate was determined colorimetrically and carbonate titrimetrically. The method was reasonably accurate, although iron and magnesium were found to have mutual interference.

Jan 1, 1965

By Jr. Frank Parrish

This report describes the performance of 17 selected water-injection projects producing from Pennsylvanian-and Permian-age reservoirs. Illustrations depict reservoir structure and thickness, and production and injection history. A selected bibliography of publications pertaining to area oil recovery and geology is included. Tabulations of field and reservoir data reveal marked differences in the projects. Increased oil recovery resulted from injecting water in most cases; however, seven projects recovered less oil than the operators anticipated. Oil recovery by water injection ranged from 0.2 to 262 bbl per acre ft, or 0.1 to 22.5 pct of the initial stock-tank oil in place. Major reasons suggested for poor performance include: (1) Adverse directional horizontal permeability, (2) channeling of injected water through fractures or zones of high permeability, and (3) lack of containment of injected water. One 330-foot-deep project is among the first successful shallow water-floods in north Texas. Another project is the first successful Canyon sand-stone waterflood reported in the area. Previous gas injection in two Cisco sandstone projects did not prevent the reservoirs from responding favorably to waterflooding.

Jan 1, 1965

By Robert L. Marovelli

The thermal conductivities of six rocks were measured by the transient line source method over the temperature range of -850 to 1,500° F. Close-fitting ceramic probes were used in 0.065-inch-diameter holes drilled through 5-to 6-inch-thick rock specimens. Taconite, granite, quartzite, and basalt were used in the tests. The method yields absolute data and is applicable to both laboratory and in situ measurements.

Jan 1, 1965

By S. J. Gasior

A method for destroying the caking properties of bituminous coal was developed by the Bureau of Mines. Coal is treated in a fixed bed by heating through its plastic range under controlled temperatures in mildly oxidative atmospheres composed of inert gas and/or steam containing about 1 volume-percent oxygen. High-volatile A (hvab) and high-volatile B (hvbb) and low-volatile bituminous (lvb) coals in the size range 1/8 to 1-1/2 inches were successfully treated at 0 (atmospheric pressure) to 300 psig in static beds 6 to 18 inches deep. Conditions of treatment depended on the coal and ranged from 80 to 200 minutes at 350° to 510° C. Char produced in this manner from hvab coal was gasified with steam at 800° C and 100 psig in a fixed bed in one series of tests and in other tests was exposed to hydrogen in a dilute co current free-falling-bed system at 750° C and 3,000 psig without agglomerating.

Jan 1, 1965

By Albert W. Deurbrouck

The performance of four sand cones was evaluated by the Bureau of Mines in three preparation plants that utilized cones in various flow schemes. The cone at plant A was a simple two-product one that provided clean coal and refuse. Plant B had two cones; one cone made a primary separation and the other a secondary separation. The primary cone separated salable coal from heavy rejects. The secondary cone separated a low-ash metallurgical coal and an intermediate-ash product suitable for plant fuel or steam markets. In plant C the sand cone was equipped with a middlings draw Which continually removed an intermediate specific-gravity product below the surface of the cone. The three primary separations of raw coal effected between floats and sinks were excellent. The recovery efficiencies for the plus 1/4-inch material ranged from 99.8 to 97.6 percent, the error areas ranged from 19 to 23 square centimeters, and the probable errors in specific gravity ranged from 0.033 to 0.024. The performance data of the two secondary separations varied from excellent in plant B, where the separation was on a par with the primary separations, to somewhat inferior in plant C, where the secondary separation was effected at the middlings draw.

Jan 1, 1965

By Manuel Gomez

The heat contents of thermally dried lignite, subbituminous B coal, and their corresponding low-temperature chars were determined at various temperatures below the highest temperature to which these materials had been exposed before testing. Similar studies were made on high-temperature char and coke, spent shale, and ash prepared from both coal and spent shale. Heat content of the carbonaceous materials tested correlated well with temperature. Heat con-tent results for spent shale compared well with the published results. Statistical analysis of experimental data together with published information showed moisture, volatile matter, carbon content, and temperature to be the principal variables influencing the specific heat of coal. The specific heat of devolatilized carbonaceous substances, char and coke, approached that of graphite as the carbonization temperature was increased. The elemental specific heats of coal constituents, estimated from the ultimate analysis and the specific heat of coal, compared favorably with published elemental specific heats.

Jan 1, 1965

By W. S. Landers

This report presents a detailed study of low temperature, entrained-bed carbonization of an Australian coking coal. The coal studied was high-volatile B bituminous from the Foybrook mine, an open-cut operation in the Liddell seam, New South Wales, Australia. Carbonization was conducted in an 8-inch diameter, continuous vertical reactor at several temperatures from 960° to 1,300° F. It was demonstrated that this bituminous coal can be carbonized within this temperature range to produce tar and a nonagglomerated char, without prior oxidation or char recirculation. Carbonization rates from 138 to 287 lb/hr (as-carbonized basis) were investigated. It was found that the carbonization temperature and the air-to-coal ratio must exceed minimum values to insure continuous operation. At the higher air-to-coal ratios employed, all or most of the carbonization heat was provided by internal combustion with air in the reactor. At the lower air-to-coa1 ratios, part of the heat for carbonization was supplied externally. On the moisture-and ash-free basis, the yield of tar plus light oil ranged from about 26 to 44 gallons per ton, and the char yield ranged from approximately 1,160 to 1,370 pounds per ton. The heat in the gas ranged from about 900 to 3,000 Btu/lb of moisture-and ash-free coal. Carbonization product yields correlated well with air-to-coal ratio and carbonization temperatures. The volatile matter in the char was found to be temperature dependent. At 1,300° F carbonization, the volatile matter in the char was 8.7 percent (dry basis), whereas at 9600 F carbonization, the residual volatile matter was about 16 to 18 percent (dry basis).

Jan 1, 1965

By A. J. Forney

Recent experiments used catalysts of plate assemblies in synthesizing high-Btu gas and gasoline indirectly from coal. A gas with a heating value of 925 to 943 Bt-: per cubic foot has been prod u la the hot-gas-recycle pilot plant from synthesis gas (3H2+100) with lathe turnings used as catalyst in the first reactor, and assemblies of parallel sprayed plats of nickel in the second. Solid plates made of Raney nickel, and steel and aluminum plates sprayed with Raney nickel or nickel oxide were tested. Those catalysts had very low resistance to gas flow; 90 percent lower than nickel granules used in previous experiments. In a single stage of synthesis thee nickel plates were only partially successful. Although the heating values of the product gas ranged from 856 to 941 Btu per cubic foot, the carbon monoxide content of he gas was above 0.1 percent. Both steel and wrought turnings were tested in single-stage synthesis, but the conversion of hydrogen and carbon monoxide was too low to attain the desired heating value of 900 Btu per cubic foot in the product gas. Assemblies of plates thermally sprayed with fusel iron were tried in an experiment to make gasoline. A gasoline yield of 52 percent (of the hydro¬carbons produced) was obtained using a 1H2-10O feed These sprayed assemblies were in service for 1,500 hours, the longest that this type of catalyst has been used. When a second reactor containing Raney nickel catalyst was added in series with the first reactor, complete utilization of the feed gas was obtained because in addition to the liquid product, a high-Btu gas with a heating value of 800 Btu per cubic foot was made.

Jan 1, 1965