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By William J. Campbell

Three types of X-ray analytical instrumentation were compared for applications in the secondary brass and bronze industry. The instruments were a conventional X-ray spectrograph, a portable X-ray spectrograph, and a radioiso-topic X-ray analyzer using balanced filters. The following two general applications were considered: Rapid identification for sorting scrap metals and quantitative analyses to provide guidance in the melting and casting of alloys. Twenty-three analyzed copper-base alloys were used as standards. Although the alloys varied widely in composition, matrix correction procedures were not necessary except for copper. The conventional X-ray spectrograph provides positive identification of the alloys and quantitative values for the six elements investigated--aluminum, copper, iron, lead, tin, and zinc. Equivalent results were obtained with the portable X-ray spectrograph for those elements whose characteristic X-rays are in the wavelength range of the instrument. The radioisotopic X-ray analyzer distinguishes certain groups of alloys and provides quantitative determinations for copper, lead, tin, and zinc. The sensitivity of the analyzer was marginal for the determination of small concentrations of elements of atomic number 26 or lower.

Jan 1, 1972

By J. A. Lamonica

The Bureau of Mines studied two types of approved coal mine dust personal samplers to determine the effect of decreasing the amplitude of airflow velocity fluctuations on cyclone performance. Results indicate that more dust is collected when pulsation free flow is used. Velocity fluctuations were reduced by means of a pulsation damper; damper efficiency of about 85 percent was needed to reduce the fluctuations to an acceptable level. The data were obtained employing both pulsating and non-pulsating flow. A comparison was made of (1) the masses of respirable coal dust as determined by weighing and of (2) the particle size distributions as determined by an electronic counter. An empirical relationship is given between the ratio of masses collected using pulsating and nonpulsating flow (M') and the ratio of the maximum air velocity to the minimum air velocity (V') as measured in the cyclone entrance channel.

Jan 1, 1972

By H. E. Powell

The smelting of brass and bronze generates a dust composed primarily of zinc oxide, with lesser amounts of other metal oxides, such as copper, lead, and tin. The small quantity of this waste generated by individual smelters and the relatively low unit value of the contained metals, suggests the desirability of reclaiming the metals onsite or at some nearby point. The Bureau of Mines has developed a process that fits these requirements. The technique consists of (1) dissolving zinc and copper from the dust with sulfuric acid, (2) recovery of copper by cementation, (3) recovery of zinc as zinc sulfate crystals, and (4) recovery of lead and tin as a salable residue. Alternatively, zinc may be recovered by electrodeposition. Free acid is recycled and no major pollution problems are generated by the process.

Jan 1, 1972

By I. D. Shah

Thermal decomposition of copper (II) sulfate (CUS04) and copper (II) oxy-sulfate (CuO?CUS04) are important steps in the overall oxidative roasting of covellite (CuS) and chalcocite (Cu2S). Nonisothermal thermogravimetric techniques were used to investigate the decomposition reactions in flowing Na and air. Thermal decomposition of CUS04 and CuO?CUS04 followed "linear" kinetics with an apparent activation energy of 55±2 and 66±3 kcal per mole decomposed, respectively. These apparent activation energies comply with those previously reported when isothermal kinetic techniques were used. The addition of oxygen decreased the rate of decomposition, while small amounts of iron which were admixed with CuO?CUS04 did not have a significant effect. Neither oxygen nor iron had any appreciable effect on the apparent activation energy of the decomposition reaction.

Jan 1, 1972

By Ted C. Briggs

A special high-pressure Burnett-type compressibility apparatus was constructed and used to determine compressibility factors for pure helium, pure nitrogen, and nine helium-nitrogen mixtures containing 89.47, 79.04, 69.69, 60.09, 49.24, 41.02, 30.99, 20.53, and 10.67 mole-percent helium. A total of 161 runs were made consisting of 2,355 observed pressures. Data were obtained at 0°, 25°, and 50° C and at pressures to 1,000 atmospheres. A power series in the reciprocal volume, commonly called a Leiden series, is used to represent the compressibility factors. Three parameters in the series are required to represent helium, five parameters to represent nitrogen, and from three to five parameters to represent the mixtures. Compressibility factors are believed to be accurate to better than 0.1 percent over the entire pressure, temperature, and composition range.

Jan 1, 1972

By R. P. Vinson, Abdurrahman Cetinbas, Joseph Cervik, M. G. Zabetakis

The effect of water infusion on the flow of methane and on the production of dust was investigated at an active face in the Pittsburgh coalbed. The average total flow of methane at the face decreased by approximately 79 percent, whereas the flow from the ribs increased about 24 percent after infusion. On the day after infusion, dust concentrations appear to have been reduced; however, the presence of large quantities of rock dust obscured the results on the following days.

Jan 1, 1972

By Abdurrahman Cetinbas

The effect of water infusion on the flow of methane and on the production of dust was investigated at an active face in the Pittsburgh coalbed. The average total flow of methane at the face decreased by approximately 79 percent, whereas the flow from the ribs increased about 24 percent after infusion. On the day after infusion, dust concentrations appear to have been reduced; however, the presence of large quantities of rock dust obscured the results on the following days.

Jan 1, 1972

By Martin H. Stanczyk

Ultrafine grinding of the industrial minerals mica, pyrophyllite, talc, marble, barite, and fluorite was accomplished using the Bureau-developed and patented attrition-grinding process. The materials, representing minerals of diverse physical characteristics, were batch ground in a 10-inch-diameter machine using statistically designed experimental test programs. The tests were made to determine large effects of variables such as feed pulp density, grinding medium size, and quantity of the electrical energy consumed during grinding on product particle size and bulk density. In designing the test programs, it was assumed that there was no interaction between the variables. Relatively coarse commercial flotation concentrates of mica, barite, and fluorspar and mine-run products of pyrophyllite, talc, and marble were readily ground into subsieve size ranges. Considering the great amount of particle size reduction obtained, the electrical energy requirements for grinding were very low. In general, the test results indicated that the best conditions for particle size reduction were approached when grinding with the coarser fraction of sand grinding media, the higher-sand-to-mineral weight ratio, and the higher feed pulp density.

Jan 1, 1972

By J. M. Singer

The objective of this investigation was to determine minimum air velocities and entrainment rates for coal and rock dust dispersion in wind tunnel experiments under conditions that simulate dispersion from surfaces in coal mines where airflows are induced by weak gas explosions. Dust deposits were bed-or ridge-shaped; particle sizes were 6 to 80 microns (cohesive deposits) or 100 to 150 microns (free-flowing deposits); and wind tunnels were 7.62 cm wide by 5.08 cm high by 300 cm long, and 2.4 m wide by 1.5 m high by 215 m long. The investigation showed that minimum air velocities (directed at mid-height) of separate, layered, or mixed piles of coal dust and rock dust were within the range 5 to 30 m/sec, independent of size of wind tunnel. This finding considerably facilitates scaling of data to mine-size passageways. Free-flowing deposits dispersed relatively slowly by single-particle detachment; cohesive dusts dispersed faster by the breaking and lifting of large clumps along weak failure flames; particle dispersion occurred in flight. Layered or mixed deposits of coal and rock dust did not disperse selectively. Semiempirical expressions were derived relating minimum air velocities and dispersion rates to dust-pile geometry, cohesion, porosity, and bulk density.

Jan 1, 1972

By L. A. Neumeier

The Bureau of Mines evaluated creep properties of Zn-Cu-Ti alloys that were annealed after finish-rolling either cold) or at 480° F (249° C). Compositions ranged up to 1.25 pct Cu and 0.36 pct Ti. Most data are for sheet annealed after finish-rolling to 92-pct total reduction. Annealing times were varied at temperatures between 320° and 560° F (160° and 293° C). For a number of the alloys, annealing after hot-rolling at 480° F affects creep properties very differently in longitudinal and transverse sheet directions. The detrimental result is that the anisotropy in creep properties between the two directions can be vastly increased. Conversely, specific annealing treatments of certain heavily cold-rolled alloys result in surprisingly low anisotropy in creep properties and the low anisotropy coincides with excellent creep resistance for both directions. Supplemental data are presented on tensile, hardness, and thermal expansion properties, and microstructures.

Jan 1, 1972

By P. S. Lewis

Shortage of natural gas is reviving interest in low-Btu fuel gas made by gasifying coal in fixed-bed producers. The Bureau of Mines gasified strongly caking Pittsburgh bed coal over test periods lasting four days in an experimental gas producer located at Morgantown, W. Va, Mechanical stirring throughout the fuel bed was effective for keeping the fuel moving and this stirring made the operation successful; hence, the gas producer was named the stirred-bed producer. Nuclear density gages were applied as control instruments to indicate coal flow and fuel level, and to record the frequency and location of void spaces in the bed, The gas, of nominal 140 to 165 Btu/scf calorific value, could be burned in a boiler for generating steam.

Jan 1, 1972

By Martin S. Oudenhoven

This report describes the results of a Bureau of Mines investigation in which the stress concentrations and distributions caused by inclusions in a strained elastic plate were determined, Finite element analyses were made for 168 models containing single inclusions of elliptical, ovaloidal, and rectangular shape. The variables studied included: horizontal-to-vertical loading ratios, (Sh/Sv) of 0,0.33,0.5, and 1.0; width-to-height ratios (w/h), of 0.25, 0.5, 2, and 4; and Young's modulus of inclusion to Young?s modulus of plate ratios (K ratios) of 0.33, 0.5, 2.0, and 5.0. The results show that the theory for elliptical inclusions can accurately predict the average stress along the x and y axes of symmetry for circular, ovaloidal, and rectangular inclusions from the width-to-height and K ratios. The actual inclusion shape was insignificant, suggesting that the average stresses in other inclusions of irregular shape (orebodies) can be estimated with the theory for an elliptical inclusion. An application of this technique to mining problems is presented. The stresses in the elliptical inclusions were uniform throughout the inclusion for all the models studied.

Jan 1, 1972

By James L. Konchesky

Crushed coal, consisting of a wide range of sizes, was effectively blended by recycling it through a bin equipped with a particle distributor. Vertical blending was accomplished by simply recycling the coal; it was not significantly influenced by the horizontal blending that was achieved by the distributor. The method was effective, even though the coal was wet and possessed poor flowing characteristics. Recirculation appears capable of providing uniform blends of solids that can be more efficiently processed. Recirculation also appears useful, preceding packaging operations, to insure for blending of solids into specification products. Continuous measurement of the bulk density of the coal by a gamma ray meter proved to be an effective monitor of vertical blending effectiveness.

Jan 1, 1972

By L. A. Haas

S02 reduction with CO was studied in an integral flow reactor at a nominal flow of 0.5 liter per minute. Reactant gas contained 3 percent SO2, 6 percent CO, and the balance He. SO2 conversion was determined for three different types of catalysts. The first consisted of 16 commercial catalysts used for various chemical syntheses. Only the commercial catalysts which contained transition metals in alumina removed more than 30 percent 80a at temperatures below 510° C. Two other types of catalysts were prepared in the laboratory either by pelletizing equal amounts of powdered alumina and transition metal oxides or by impregnating commercial alumina tablets with transition metal ions. Regardless of preparation techniques, Cr and Fe in alumina were the two best catalysts. The observed results suggest that an intermediate (SCO) is formed by the interaction of surface metal sulfides and carbonyls. Alumina then catalyzes the interaction of SCO with S02 to form the end products (sulfur and carbon dioxide). Over 80 percent S02 was removed at 460° C with 2 grams alumina impregnated with 2.5 percent iron.

Jan 1, 1972

By O. Q. Leone

Composite diaphragms were used in the investigation of electrowinning Ti from TiC14 in a fused LiCl-KCI-TiC'2 electrolyte. Composite diaphragms tested were of two general classes--those consisting of two or more solid materials, and those which contained, in addition, a loose material. An electrowinning cell using a flat diaphragm is described. The maximum current density for these diaphragms was 300 amp per ft2. Lower currents permitted longer operation times. The composite diaphragms gave electrode efficiencies that averaged approximately 60 percent, and the electrowon titanium was of good quality--some Brinell hardnesses were as low as 68.

Jan 1, 1972

By Fred N. Kissell

Methane-flow and pressure data taken from a mine in the Pocahontas No. 3 coalbed are compared with flow rates from lump coal obtained in laboratory experiments. From this, it is concluded that the main source of gas is the intact coalbed rather than a "crushed zone" near the working face. The permeability and sorption capacity of the intact coalbed are calculated and gas emission rates are theoretically accounted for.

Jan 1, 1972

By Fred N. Kissell

Methane-flow and pressure data taken from a mine in the Pocahontas No. 3 coalbed are compared with flow rates from lump coal obtained in laboratory experiments. From this, it is concluded that the main source of gas is the intact coalbed rather than a "crushed zone" near the working face. The permeability and sorption capacity of the intact coalbed are calculated and gas emission rates are theoretically accounted for.

Jan 1, 1972

By H. Carroll

An ozone detector was built and evaluated for its applicability in smog-chamber studies. The detection method is based on the reaction of ozone with ethylene and the measurement of resultant chemiluminescence. In the first phase of evaluation, the detector's response to ozone was studied as a function of several instrument parameters, and optimum conditions were defined for the maximum and most stable responses to ozone. In subsequent evaluations, the method was checked for sensitivity, precision, and interferences and was compared with two alternative methods. Results showed the chemiluminescence method to be acceptably sensitive and precise for smog-chamber studies and superior to the Mast ozone meter and KI (colorimetric 1 percent neutral-potassium iodide method) methods in that it is specific for ozone.

Jan 1, 1972

By W. H. Eddy

The Bureau of Mines conducted laboratory batch and continuous flotation processing tests on waste granite fines from South Carolina to determine the possibility of recovering high-quality feldspar and glass sand. Three flotation systems were used for removal of the iron-bearing biotite: Two employed an alkaline anionic-cationic circuit and the third employed an acid cationic circuit. Commercial-grade products were obtained when the remaining biotite was magnetically removed from the feldspar and quartz concentrates. Continuous flotation processing yielded a feldspar concentrate containing, in percent, 3.60 Na20, 5.60 K20, and 2.25 Ca0, with recoveries of 75.3, 66.6, and 72.6 percent, respectively. The feldspar tailing was high quality glass sand containing 98.0 percent Si02 and 0.025 percent Fe203; about 60 percent of the quartz was recovered.

Jan 1, 1972

By J. J. Henn

A process is evaluated for recovering metallurgical-grade manganese are from the low-grade manganiferous iron ores of the Cuyuna Range, Minnesota. The process, developed by the Bureau of Mines, employs high-temperature sulfatization of the are to form manganese sulfate and reduction of the are to convert the iron to a magnetic oxide. The roasted ore is water-leached to dissolve the manganese sulfate, which is then separated from the leach residue, is crystallized, and is calcined to produce the manganese product. Iron is recovered from the leach residue by magnetic separation, and is pelletized and calcined to produce byproduct iron ore pellets. The fixed capital cost for a plant yielding a product containing 100 tons of manganese per day is $19.6 million on a mid-1970 basis when the raw are contains 4.84 percent manganese. The estimated operating cost of the plant is $211 per ton of contained manganese. Graphs are included to show the effects of ore cost and varying manganese content of the raw ore on the estimated operating cost.

Jan 1, 1972