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By D. J. Bauer

A primary amine extraction system was investigated for fractionating a cerium-group, lanthanide sulfate mixture. Addition of diethylenetriaminepenta-acetic acid (DTPA) to the amine extraction system resulted in separation factors as high as 5.4 for lanthanum-cerium, 8.0 for cerium-praseodymium, 3.7 for praseodymium-neodymium, and 7.0 for neodymium-samarium. In multistage studies on a cerium-free lanthanide mixture, 96 percent of the lanthanum was recovered with a purity of 95 percent.

Jan 1, 1968

By J. Hudy

An investigation has been made to determine the applicability of the Cendrex3 X-ray instrument for the measurement of the ash content of washed bituminous coal products. The results obtained for selected products from six preparation plants in the Appalachian region and one preparation plant in the mid-western region are described. Emphasis of the study was placed on low-ash bituminous coal products suitable for utility or metallurgical markets. There was good agreement between the results obtained by conventional ash determination methods and by ash determination using the Cendrex for all products tested.

Jan 1, 1968

By Kenneth J. Miller

To determine the effectiveness of the many new flocculants available to the coal industry 20 of these reagents were evaluated treating slurry feeds to four refuse thickeners. Settling rates and supernatant liquid clarities were determined for each of the flocculants on the four slurries, and zeta potential measurements of the slurry solids were made. The test results showed that the flocculants provided comparable results when judged categorically as anionic, nonionic, or cattonic. It was also apparent that control of zeta potential insures maximum benefit from a flocculant.

Jan 1, 1968

By J. M. Singer

Flame propagation of lower limit hybrid coal dust-methane-air mixtures in vertical and horizontal flame ducts of 15.2 cm id and 1.8 m length has been investigated to provide information bearing on safety in mines. Fuel concentrations at lower limits of flame propagation and equivalences of coal dust and methane are much higher for continuing flame propagation than for short-span flame propagation in the vicinity of an "overdriving" ignition source. As the energy of the ignition source was increased, the flame speed and the distance of flame propagation from the ignition source increased, whereas the total fuel concentration at the lower limit decreased.

Jan 1, 1968

By S. J. Aresco

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal, expressed in British thermal units, and the composition as shown by proximate analyses. To these, when required, are added the ash-softening temperature, the free-swelling index, and the Hardgrove grindability index. Under most of these specification contracts the bidders guarantee the quality of the coal, and that guaranteed by the successful bidder becomes the standard of his contract. The deliveries are sampled in accordance with instructions3 issued by the Bureau of Mines; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor; if it is not, a price adjustment is made. Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks) provide valuable data for use in evaluating future bids. In addition, the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal.

Jan 1, 1968

By Floyd G. Anderson

Bureau of Mines studies show than an electronic counter can be used for determining just concentrations from midget impinger samples collected in bituminous coal mines. A sample correlation coefficient of 0.91 for data obtained using the electronic counter and the Bureau of Mines microprojector procedures indicates a significant linear relationship between the methods. The electronic counter provides better counting precision and reduces analytical time.

Jan 1, 1968

By John M. Gomes

A two-phase molten halide-silicate technique for extracting tungstic oxide (WO3) from scheelite (CaW04) and wolframite [(Fe, Mn)W04] was investigated. The halide phase extracted over 99 percent of the was, whereas the lower silicate phase retained about 90 percent of the calcium, iron, or manganese oxides. The most efficient extraction and separation of tungsten from scheelite was accomplished at 1,080° C in a molten system containing, in mole-percent, 9 calcium tungstate (CaW04), 42 sodium chloride (NaCl), 28 sodium fluoride (NaF), 17 sodium metasilicate (Na2SiO3), and 4 alumina (Al2O3). Wolframite was also treated at 1,0800°C; the molten system contained, in mole-percent, 11 (Fe, Mn)W04, 74 NaCl, and 15 Na2 SiO3.

Jan 1, 1968

By M. M. Tilman

The objectives of this research were to determine the practicability of using cobalt as a means of controlling the amount of ferrite in the micro-structures of semiaustenitic stainless steels, and to determine the effects of reduced ferrite content on mechanical properties of these steels. Cobalt additions of up to 3 weight-percent were made to type 17-7 PH2 (AISI 631) stainless steel. Ferrite contents were determined for alloys in the aged condition, and for alloys quenched from the hot working temperature. Ferrite can be completely eliminated from the microstructure of 17-7 PH stainless steel by additions of cobalt, but complete elimination of the ferrite phase results in lower tensile strength, yield strength, and hardness. Tensile properties, hardness, and impact strength were determined for aged material. A subzero temperature treatment before heattreating was necessary to obtain maximum strength in the alloys containing cobalt. Addition of 2 weight-percent cobalt enhances mechanical properties of 17-7 PH stainless steel.

Jan 1, 1968

By J. F. Smith

A series of studies of emissions from large coal-fired steam generators have included measurements of the concentrations of oxides of sulfur and oxides of notrogen. The sampling equipment, method of sampling, and analytical techniques used for processing of these samples are detailed. A method based on the precipitation of benzidine sulfate was developed for determining both SO3 and total oxides of sulfur in the presence of interfering acidic components in the stack gases. In addition, difficulties encountered with sampling and analytical techniques are also described.

Jan 1, 1968

By Raymond L. Lowrie

For many years it has been considered that an average of 50 percent of the coal in the deposits exploited has been recovered. Owing to many changes in mining methods during the past two decades, this study was initiated to obtain an up-to-date measurement of recovery percentage and thus establish part of the basis from which presently recoverable reserves may be estimated. Recovery percentages were determined within mined areas of 200 underground coal mines. These comprised a statistical sample selected to be representative of operating mines in relation to their significance to depletion of reserves. The results ranged from 29 to 91 percent and averaged 57.0 ± 1.7 percent (95-percent confidence limit). Six factors were identified mathematically as significantly affecting recovery percentages: (1) Pillaring system, (2) top rock and conditions, (3) bottom rock and conditions, (4) marketability, (5) coalbed thickness, and (6) productivity. Skill and attitude of mine operators toward recovery, although not measured, were probable factors. Five other variables that were tested did not show any significant relationship with recovery percentages. Also, five mining equipment features were identified, through discussions with mine officials, as affecting adversely recovery percentage at some mines.

Jan 1, 1968

By M. R. Geer

The ever-increasing need to guard against stream pollution has intensified interest in the problems of handling and disposing of flotation tailing. Therefore, the Bureau of Mines investigated the possibility of using crushed washery refuse to adsorb the free water in thickened flotation tailings on a bench scale and then in a pilot plant because the conventional methods of disposing of coal flotation tailings--impounding them or filtering them so they are dry enough to be conveyed to the refuse dump--are sometimes either impractical because of space limitations or costly because of low filter capacity. Most of the refuse samples tested were of similar mineralogical composition and exhibited similar water retention capability. The amount of crushed refuse required to adsorb the water in a particular tailing was influenced greatly by the fineness of the solids in the tailing and hence the percentage of solids to which it could be thickened. The ratio of crushed refuse to tailing solids required to provide a mixture dry enough to be carried on an inclined conveyor belt varied from 2.4 to 6.4. Several chemical agents that were tested were very effective in turning the free water in tailings into a stable gel. Fly ash also was very effective in adsorbing water.

Jan 1, 1968

By R. V. Higgins

This paper describes a method and a computer program for calculating shape factors and areas of channels that turn more than 90° and conduct fluids into the backs of wells. The program represents an improvement over a previous Bureau of Mines investigation by using a 4-point Lagrange interpolation equation instead of a 3-point and by summing areas of trapezoids with either x altitudes or y altitudes. Some of the techniques reported in this paper can also be used to compute the areas between contours and the lengths of lines that turn more than 90°.

Jan 1, 1968

By B. D. Nash

The object of this research was to investigate the technical feasibility of preparing chromium metal by the thermal decomposition of bisbenzene chromium. Bisbenzene chromium, a pi-bonded sandwich type organometallic compound, was thermally decomposed under reduced pressure to form a metal plate on a heated substrate. Metal recovery was close to 100 percent of theoretical, with deposition rates up to 20.8 mg/hr/cm2. Metal purity was dependent not only upon the purity of the starting material, but also upon the sublimation rate of bisbenzene chromium. Total detectable metallic impurities ranged from a low of 18 ppm to several hundred ppm. In general, metallic impurities were less than 100 ppm. Carbon, the major nonmetallic impurity, ranged from less than 0.3 percent to more than 10 percent. The carbon contamination is most likely a result of the decomposition of the organic portion of bisbenzene chromium. An unusual property of some of the deposits was their outstanding corrosion resistance. Unlike pure electrolytic chromium, which dissolves readily, these deposits were insoluble in hot mineral acids.

Jan 1, 1968

By H. G. Iverson

The effects of adding boron and boron plus carbon to electrorefined vanadium were evaluated with respect to mechanical properties at low temperatures and response to heat treatment. Grain size was significantly decreased with the addition of 0.05 percent boron, the decreases ranging from 30 percent at 800° C to 75 percent at 1,100° C. Increasing the boron content resulted in only a small increase in strength at room temperature, but at 77° K, boron contents of 0.005 to 0.076 percent increased the yield strength of vanadium over 50 percent, from 70,000 psi to 110,000 psi. When boron and carbon were present together, the individual grain-refining effects obtained with either element were retained. Approximately a twofold increase in strength was obtained by age-hardening the alloys containing both boron and carbon. Alloys with only boron additions did not age-harden.

Jan 1, 1968

By K. R. Dorman

To develop the potential of precast concrete sets as a support medium in underground mines, a three-piece precast concrete drift set was designed for a small opening and tested to destruction in an underground straining frame. Thirty-six tests were made with three sizes of members using three different loading conditions. In addition, 14 members were tested individually in the laboratory. Test results are compared with theoretical calculations. A cost comparison shows the use of concrete sets would be advantageous where conventional wooden timber requires excessive replacement.

Jan 1, 1968

By John S. Berber

Olefin and paraffin mixtures (C10-C16 and C10-C22) were separated from low-temperature lignite tar by urea adduction and sulfated to yield secondary alkyl sulfate detergents. The C10 ?C16 secondary alkyl sulfate showed a 99.3 percent biodegradability, and the C10-C22 fraction showed a 96.8 percent biodegradability, exceeding the required standard of 80 percent for the biodegradability of anionic detergents in washing and cleaning compounds. Chlorination of paraffins yielded a detergent of 93.2 to 93.4 percent biodegradability.

Jan 1, 1968

By Herbert R. Babitzke

The purpose of this investigation was to optimize the high-temperature properties of columbium and tantalum. Columbium and tantalum were combined with selected alloying elements to achieve solid solution and dispersion strengthening. Fifty-six alloys were evaluated to determine their formability, hardness, strength at elevated temperatures, and oxidation resistance. The following six alloys showed high-temperature strength: [Cb-15Hf-5W-2Zr-4Al-4Ti-2N Cb-15Hf -5W-5Zr Cb-15.3Ti-4.1Zr-13.7Hf Ta-20Hf-4Al Ta-30Hf-4Al Ta-20Hf-5W-4Al] At 1,200° C, the columbium alloys had strength values of 40,000 psi or greater, and the tantalum alloys had strength values from 50,000 to 58,000 psi. For a 2-hour test period at 1,000° C, weight gains of only 9 and 8 mg/cm2, respectively, were observed on oxidation testing of two alloys, Cb-15Hf-5W-2Zr-4Al-4Ti-2N and Ta-20Hf-5W-4Al.

Jan 1, 1968

By R. O. Dannenberg

A metallic displacement process, utilizing easily available steel wool or steel window screen, was devised and successfully used for the recovery of silver from waste photographic fixing solutions. Laboratory and prolonged commercial-scale testing established that the iron filament type unit will efficiently precipitate silver, as a high-grade sludge, from acidic waste photographic fixing solutions ranging in grade from less than 1 to over 10 grams of silver per liter. Data and design information are presented to facilitate the construction and operation of a practical unit of any desired size. A smelting process for recovering pure silver from precipitated sludge containing 27 to 80 percent silver was devised.

Jan 1, 1968

By A. G. Starliper

Laboratory studies were made to produce whiskers of tungsten over a wide range of operating temperatures. Hydrogen reduction of tungsten hexachloride in a vacuum furnace at temperatures from 2,7000 to 3,3000 C yielded a small quantity of tungsten whiskers, provided a low degree of supersaturation was maintained. Direct measurements of 3,000,000 to 4,000,000 psi were obtained for the ultimate tensile strengths of individual whiskers averaging 3 to 4 microns in diameter with average aspect ratios of 1,000. This compares with strengths of 300,000 to 400,000 psi for 13-micron-diameter commercial filaments.

Jan 1, 1968

By J. L. Reuss

The Bureau of Mines investigated the technical feasibility of smelting copper concentrates containing chalcocite (Cu2S) and native copper using nonpyritic sulfur-bearing materials to aid matte formation. The procedure consisted of combining various proportions of commercial chalcocite concentrate, smelter slag, fluxes, and matte-forming constituents to produce charges of comparable compositions. The mixtures were charged in fire-clay crucibles and smelted in an induction furnace at 1,300° C. The research proved that either sulfur or gypsum can replace pyrite as a matte-forming material, and that gypsum produces an exceptionally high-grade copper matte. The addition of small quantities of metallic iron to the nonpyritic smelting charge furthers the removal of sulfur, improves the recovery of copper, and makes it possible to utilize gypsum as the exclusive flux and matte-forming ingredient, thereby eliminating the necessity of adding limestone.

Jan 1, 1968