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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 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 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

By John W. Buch

Hydraulic cutting tests made on samples of Pennsylvania anthracite (3,700 psi and 260 gpm) were promising enough for the Bureau to establish a full scale experiment in an anthracite mine. Water pressure and quantity for mining anthracite were arbitrarily established at 5,000 psi and 300 gpm (1,000 hp). For full-volume flow, hydraulic pressure is controlled by orifice size with the displacement pump. The hydraulic jumbo was designed for maneuvering on pitches from 0° to 20° in any direction and for a coalbed ranging in thickness from 10 feet 6 inches to 15 feet. All motions of the jumbo are by oil hydraulics. Jet flow is controlled (start-stop) at the face, through an interlocked pushbutton system. One button is in the operator's cab; one, at the pump station; and one (a safety shutoff), near the mining face. To December 1962, 7,400 tons of bed material had been mined at an average rate of 0.800 ton per minute, with an average power requirement of 14.125 kilowatt-hours per ton. In January 1963, the objective was changed from an engineering-development basis to a research basis--to determine, ultimately, the most efficient level of operating characteristics for maximum response, as measured by mining-out rate. This research phase of the project is not yet complete, but conclusions, and the method of arriving at them, will be made the subject of another Bureau publication. It should be noted that as of December 1963 nearly 13,000 tons of bed material had been mined, at rates as high as 1. 3 tons per minute for a complete face advance.

Jan 1, 1965

By C. C. Popoff

This report reviews the phosphate deposits, mines, and industry, and prospects in 10 districts covering most of the Montana phosphate field. These districts are discussed individually, and an evaluation of the resources and potential of each is presented. Phosphate rock produced from underground mines in the Garrison district is shipped to Canada for processing to fertilizers, utilized locally for production of animal feed supplement, and pulverized and sold for direct application to the soil. Production from the Melrose district is shipped to Silver Bow and processed to elemental phosphorus. The Maxville-Philipsburg district is destined to become a major producer with the development of the Douglas Creek mine and beneficiation plant by Montana Phosphate Products Co. Montana ranks fourth after Florida, Tennessee, and Idaho in total annual production in the United States. Production him increased from about 60,000 long tons of acid-grade phosphate rock in 1940 to more than 660,000 tons of acid-, beneficiation-, and furnace-grade ore in 1961. Montana has the second largest potential resources in the Western field; in the area south of Butte there are approximately 1.2 billion tons of phosphate rock (+18 to +31 pct P2O5) available above and within 100 feet below entry level; and in the northern part of the field there are about 67.6 million tons available above entry level. In contrast to Idaho, most of the phosphate deposits in Montana are best suited to underground mining.

Jan 1, 1965

By Clark F. Grain

The monoclinic to tetragonal inversion of zirconium dioxide was studied by single-crystal X-ray methods, high-temperature X-ray diffractometry, and differential thermal analysis. The unusual features of the inversion, such as no definite transition Lperature, hysteresis, and athermal kinetics, were confirmed for powders who mean crystallite size was greater than 1,000 A. Samples of mean crystallite size below 1,000 A displayed classical kinetics, obeying a logarithmic rate law. A detailed mechanism based on Ubbelohde's theory of continuous phase transformations was proposed which is consistent with all the experimental facts.

Jan 1, 1965

By J. B. Gayle

The Bureau of Mines studied the effects of air oxidation on the recovery of float coal. Both batch-and continuous-type tests were made on six bituminous coals, representing the range in rank of coals now commercially used for carbonization, and on one anthracite coal. The effects on flotation recovery of oxidation at 1000 C for periods up to 50 days were investigated using an alcohol-type frother and a kerosine-pine oil reagent. Two series of release analysis tests were made, using one medium-volatile bituminous coal. Float coal recovery was adversely affected by oxidation in all tests where the alcohol-type frother was used. Conversely, a small degree of oxidation improved recovery with kerosine-pine oil frother for some of the coals in continuous tests. Prolonged oxidation (beyond about 14 days) adversely affected float coal recovery for all coals, the effect being more pronounced for batch-type tests and for tests using alcohol-type frother. Reagent selectivity for the rejection of both ash forming and sulfur bearing minerals was reduced by oxidation. Severe reduction of reagent selectivity required only about 3 days' oxidation for alcohol-type frother but more than 10 days' oxidation when the kerosene-pine oil reagent was used.

Jan 1, 1965

By T. E. Sterner

The Bureau of Mines investigated the use of a chromatographic gas analyzer in determining the concentration of combustion products in gas produced during field and laboratory thermal oil-recovery tests. Several parameters (carrier-gas flow, cell current, sample size, and temperature) known to affect quantitative analyses were studied using a commercially available dual-column, dual-detector chromatographic gas analyzer which had been modified to provide close control of these variables. The apparatus made possible a much closer control of air-and gas-injection rates and provided adequate data for performing material-balance calculations and for determining oxygen utilization during the laboratory and field combustion tests. The chromatographic analysis also aided materially in evaluating and measuring bypassing and gas travel times and in detecting high-permeability zones that were present in the reservoir.

Jan 1, 1965

By M. R. Geer

Samples of coal from six beds in the Roslyn-Cle Elum field of Washington were subjected to float-and-sink tests to determine their amenability to the production of high-ash boiler fuel for on-site power generation. Grindability tests and analyses of ash were made. All of the coals would require some degree of cleaning to insure a product of 25 percent ash. With two of the coals the entire size range would have to be washed. With the other four, it would suffice to clean only the coarse coal and bypass the raw fines.

Jan 1, 1965

By R. E. Campbell

Uranium metal of improved purity was prepared by electrorefining commercial magnesium-reduced uranium in a molten sodium chloride-uranium trichloride electrolyte. The best operating conditions for the preparation of refined metal were established as follows: an electrolyte containing 8.7 to 13.3 weight-percent uranium; initial cathode current densities from 300 to 1,500 amp/sq ft; and a molten salt temperature of 860° C. Ingots produced from electrorefined uranium crystals prepared with these operating conditions were substantially free of metallic impurities. The only impurities in the refined and consolidated metal were present in low or undetectable amounts.

Jan 1, 1965

By Jr. Oitto

A polyester-type resin and deformed-steel reinforcing bars (rebars) were used in to strengthen and to stabilize bolted, fractured wall rock along pas 1:'y. in a western gold mine. Reinforcing bars were placed in boreholes drilled into fractured rock and then were surrounded by resin pumped under pressure into the holes and intersecting fractures until the wall rock was thoroughly impregnated. Pumping and injection equipment and infusion procedures are described. Visual examinations for movement in bonded and adjacent unbonded rock were made for 3 years. Fractured walls containing resin-rebar installations were strengthened. The results suggest that resin-rebar support can be used advantageously and economically in repairing fractured or broken rock when compared with rock bolting or timbering.

Jan 1, 1965

By Robert M. Becker

Particle mixtures were sampled in the laboratory, using ordinary sampling procedures, to determine whether or not the compound-multinomial probability distribution and other developments of part 2 agreed with experimental results. The objective was accomplished by the Bureau of Mines by comparing the moments and moment relationships of the appropriate probability models with their corresponding experimental values over a fairly wide range. The overall agreement between the corresponding theoretical and experimental values is both good and complete. The results demonstrate that sampling to a constant amount, such as weight, of items per sample is not the same, in general, as sampling to some constant number of items per sample. The results seem to confirm all the developments of part 2 and the application of the compound-multinomial function to bulk sampling.

Jan 1, 1965

By T. A. Sullivan

High-purity vanadium metal was prepared by electrorefining commercial vanadium in a molten sodium bromide, potassium bromide, and vanadium dibromide electrolyte. Variables investigated were operating temperature, current densities, electrolyte composition, and condition of the anode. The purity of the refined metal was in the range of 99.95 percent vana-dium. Iron and oxygen in the 50- to 250-ppm range were the only major impurities. Metal with hardness numbers of 50 to 60 in the Rockwell F scale was prepared from feed material with a Rockwell B hardness of 90. The arc-melted metal was highly ductile and could be cold-worked into sheet or foil.

Jan 1, 1965

By Jr. Gabler

Methods for the direct spectrochemical determination of impurities at the parts-per-million level in tungsten metal and oxide are presented. Several published procedures were investigated and numerous modifications were made in establishing procedures with improved precision and extended lower levels of determinability. Details of standards preparation are presented, experimental work is described, and three preferred methods are described in detail. A germanium carrier-distillation procedure is applicable to the determination of 13 elements in tungsten powder; a silver chloride carrier-distillation procedure provides for the determination of 24 elements in tungstic oxide, and a sustaining ac arc method is applicable to 26 elements in tungstic oxide. The choice of methods to be used depends upon sample form, elements and concentrations to be determined, and the precision and accuracy required. The investigations reported here were undertaken to develop direct spec-trochemical methods with increased accuracy and precision to determine impurities in high-purity tungsten and tungstic oxide, to define the lower concentration levels of detectability and measurement for the common impurities in tungsten by direct spectrographic means, and to present the details of the developed or modified methods that have proved applicable.

Jan 1, 1965

By Richard F. Hewlett

This report describes how a limited number of preliminary exploration drill-hole assays from a mineral deposit can be used to design grid spacing that is both economic and efficient for subsequent evaluation drilling of that deposit. Relationships between desired precision of the estimate of grade of ore and drilling cost are used to determine the economic drill-hole spacing. The statistical concept of precision in estimating grade of ore is used to determine the efficient drill-hole spacing. Assay data from approximately 50 known copper deposits were studied, and the relationships of the statistical parameters of these deposits were computed. Drilling requirements for various precisions of the estimates of grade of ore were computed for some of these known deposits to serve as guides for drilling future copper deposits. The effect of various geologic factors on the trend in grade of ore and, therefore, on the drilling requirements is shown for certain deposits.

Jan 1, 1965

By M. Copeland

Phase relations of gadolinium alloyed, up to 40 weight-percent (wt pct), with AISI 304-type stainless steel were established. Body-and face-centered cubic iron-rich solid solution phases and several intermetallic gadolinium-containing compounds of variable composition that approximated the formulas Fe9Gd, Ni7Gd2, Ni3Gd, Fe2Gd, NiGd, and NiGd3 were identified. The intermetallic phases Fe9Gd and Ni7Gd2 were noted to melt at about 1,080° C at about 0 to 2 wt pct gadolinium. The melting temperature of Fe9Gd increased with increas-ing gadolinium content to a plateau at about 1,230°C and 30 wt pct gadolinium, and the melting point of Ni7Gd2 decreased to a plateau at 900° C and 30 wt pct gadolinium where Ni3Gd, NiGd, and Fe2Gd coexist. Body-centered cubic iron solid solution was stable from 1 to 2 wt pct gadolinium to higher contents, 30 wt pct gadolinium or possibly more, and face-centered cubic iron up to 12 wt pct gadolinium below 1,200° C. The stability of these phases above 1,200° C was not resolved except for the mel points. A limited number of fabrication variables as well as mechanical and corrosion properties of alloys containing up to 5 wt pct gadolinium were studied. Equilibrating and forming operations were best conducted at about 940° to 1,080° C. Some variability in the yield and tensile strengths of alloys was noted; however, there was a continual decrease in ductility and impact resistance with increasing gadolinium contents. The resistance of gadolinium alloys to corrosion in water at 354° C was about the same as stainless steel.

Jan 1, 1965

By Jr. Norman

Thermoelectric properties of depleted uranium selenides and tellurides were investigated from room temperature to 700 C. Several depleted uranium monoselenides and monotellurides were doped with selected cationic and anionic materials to determine the effect of impurity additions on the thermoelectric properties. The undoped uranium selenides and tellurides were semimetallic conductors exhibiting low Seebeck coefficients and electrical resistivities. Partial or complete degeneracy was in evidence, indicating a charge carrier energy distribution similar to that in a metal. Doping increased the Seebeck coefficients of the uranium monoselenides and monotellurides; however, the corresponding change in the power factor in the figure of merit was small because of the increase in electrical resistivity.

Jan 1, 1965