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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 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 C. Melvin Lepper

A solid-state amplifier for the bridge circuit of an atomic-absorption mercury detector is presented and described. Operational advantages over previously used circuitry include improved time and temperature stability, increased measurement accuracy, and simplified setup, calibration, and operation.

Jan 1, 1972

By Mark I. Copeland

A study was conducted to determine if commonly used alloying additions or coating materials can prevent the formation of a liquid-copper phase during the reheating of copper-containing steels. If so, the tendency of such steels to surface-crack during hot-working might be eliminated. Steel specimens were scaled by heating them either isothermally or in a programed manner that simulated industrial furnace practice. Metallographic examination of the heated specimens showed that molten fayalite (Fe2Si04) completely prevented the formation of liquid copper at the surface. Fayalite, which melts at 2,200° F (1,205° C), was formed by internal oxidation of the silicon contained in the steel. By forming complex molten oxides, coatings of borax glass were also effective in preventing the occurrence of liquid copper at the steel surface.

Jan 1, 1972

By R. L. Schmidt

One of a series published by the Bureau of Mines covering research investigations in rock drillability, this report of field drilling results extends earlier laboratory findings and provides a relatively simple procedure for predicting percussive drilling rates with reasonable accuracy. Two percussive drills mounted on a truck were used to drill a total of 25 rock types, and the results were used to develop a prediction equation. The equation was tested on a set of unrelated laboratory percussive drilling data, and the comparison between predicted and actual rates is shown in tabular form.

Jan 1, 1972

By George A. Savanick

The objective of this research is to develop a method for measuring the tensile strength at the interface between minerals in rock. These measurements reflect the strength of the attractive forces operating at crystalline interfaces in rock. Since these forces act in opposition to the forces set up in various rock fragmentation processes, measuring their strength may help in designing more efficient methods of rock fragmentation. The method developed for measuring the strength of intergranular adhesion in rock involves separating a bicrystal from the rock and determining the tensile strength at its solid-solid interface. This technique has been successfully applied to the study of quartz-feldspar interfaces separated from massive pegmatites, graphic granite, and the Rockville granite, yielding average tensile strengths of 5.86, 8.62, and 10.65 meganewtons per meter squared (MN/m2) (850, 1,250, and 1,524 psi, respectively). The data this technique provides indicate that the members of these bicrystals are strongly adherent. Examirtation of bicrystals broken at the crystalline interfaces indicates that the bonds responsible for this adhesion operate over only a portion of the interfacial area. This work conclusively demonstrates that tensile strength tests can be conducted on small selected areas; for example, grain boundaries in rock. The small-scale zones of strength or weakness determined in this way can be related to the overall strength of the rock.

Jan 1, 1972

By O. Q. Leone

A processing unit was developed for the complete cleaning of titanium alloy chips. The process uses solvent degreasing, magnetic separation, and anodic solution of nonmagnetic impurities in 10 weight-percent sulfuric acid. Vacuum arc-melted ingots weighing approximately 10 pounds each were prepared from cleaning chips according to ingot specifications.

Jan 1, 1973

By John Ward Smith

Aragonite, co-occurring with calcite and dolomite as matrix minerals, has been discovered in Mahogany zone oil shales of Colorado's Eocene Green River Formation, posing puzzles on the geochemical patterns of their separate origins, reasons for their simultaneous existence, and their interrelation. The presence of aragonite is demonstrated by X-ray diffraction. Amounts of aragonite and dolomite are significantly and inversely related, but the calcite quantity is essentially independent of either aragonite or dolomite quantity. A geochemical pattern outlining the deposition conditions that created the Green River Formation oil shale is postulated from characteristics of the oil shale. The development of the three separate carbonates--aragonite, calcite, and dolomite--the inverse relationship between aragonite and dolomite, and the independence of amounts of calcite and the other two carbonates are shown to be natural consequences of this oil-shale genesis pattern.

Jan 1, 1973

By J. S. Miller

The Bureau of Mines developed methods for fragmenting oil shale formations with chemical explosives to prepare oil shale for in situ retorting and to evaluate the extent of fragmentation by various methods. A combination of three methods of explosive fracturing was used: (1) The displacement and detonation of a liquid chemical explosive in a natural fracture system; (2) the use of 60-pct dynamite to relieve stress conditions of the rock around the wellbore; and (3) the use of pelletized TNT in a series of wellbore shots to fragment the oil shale. An attempt was made to seal or grout around the fragmented oil shale by drilling 67 holes and displacing approximately 200 bbl of neat cement in the fracture system to aid in evaluating the fragmented zone, Seven methods were used to evaluate the fragmented zone. The primary evaluation method was the recording of seismic waves to delineate the fragmented zone with results based on arrival time, amplitude, and record quality. The data from the seismic measurements indicated the extensively fragmented zone was approximately 95 ft in diameter and 70 ft thick. Results of the remaining methods of evaluating fractures--including air-flow tests, coring of the expected fragmented zone, elevation measurements to indicate overburden crowning, and surveys with high-speed camera, impression packer, and down-hole camera--agreed with and supported the data from seismic measurements. Further field application of explosive fracturing and evaluation methods is needed to determine when a zone of oil shale is effectively fragmented for efficient in situ retorting.

Jan 1, 1973

By G. A. Wancheck

Shear tests were performed on several prepared samples of granular and powdery bulk materials to investigate the following parameters: Particle size and distribution, particle movement, moisture content, consolidation of material, bulk density, void ratio, porosity, volume change, and strain rate. A series of shear tests was performed with weight-percent-ratios of minus 0.185-inch tertiary sand and 1-1/2-by l/2-inch tertiary gravel mixtures, and weight-percent-ratios of minus 200-mesh limestone (rock dust) and minus 200-mesh bituminous float coal dust. A comparison was made for shear test results obtained with rectangular and circular shear cells utilizing the large and small direct shear testers. Specifically, the shear results obtained include the angle of internal friction or shear strength of the tested material under known consolidating pressures, and the kinematic angle of friction or coefficient of friction between the interface of a bulk material and a sample wall material. The experimental procedure, tests, and results are given for each parameter investigated.

Jan 1, 1973

By Ronald A. Munson

Samples of the naturally occurring zeolites phillipsite, clinoptilolite, erionite, and chabazite have been surveyed for their gas adsorption, ion exchange, and other characteristics. Chabazite and erionite, which are generally more stable, also have higher methane adsorption capacities than do the other natural zeolites. Both natural erionite and natural chabazite are classified as small-port zeolites on the basis of their inability to adsorb chlorotrifluoromethane. In the range of 8 to 100 mesh, the adsorptive capac-ity of natural zeolites is improved only slightly by a decrease in particle size. The capacity of natural clinoptilolite to adsorb methane is increased by cation replacement by the hydrogen ion and decreased by exchange with calcium ion. Natural phillipsite, which is easily decomposed by heat, adsorbed methane to a limited extent.

Jan 1, 1973

By D. S. Burgess

This report summarizes the incidents that preceded the December 9, 1970, propane-air explosion in Port Hudson, Mo., and then attempts to establish the nature of the explosion from the ensuing events. Special emphasis is given to possible ignition sources, the distribution of flammable vapors, and the analysis of blast damage. Both near-and far-field damage indicated that this explosion may be attributed to the detonation of propane in air with an energy release equivalent to that from about 50 tons of detonating TNT.

Jan 1, 1973

By A. G. Kim

Methane and other hydrocarbon gases, byproducts of coalification, are emitted from coal at widely varying rates and often present ventilation problems during mining. The air in some coal mines apparently contains no methane. To determine if coals from mines which bid no history of detectable gas emission contained adsorbed methane, samples of coal at the shaft bottom and at an active face were obtained and placed in sealed metal cylinders. The atmosphere around the coal was sampled and analysed by gas chromatography. Methane, ethane, ethylene, propane, propylene, and butane were found to have been desorbed from these coals. Hydrogen and helium were also detected. An estimate of the amount of residual gas per ton A coal indicated that coal samples from the active face generally contained more adsorbed gas than coal samples obtained from the shaft bottom, although in both instances the total amount of gas was relatively small.

Jan 1, 1973

By J. B. Rosenbaum

Prolonged laboratory and limited pilot plant tests have shown that the Bureau of Mines buffered S02 -H2S process is capable of removing 95 to 99 percent of the S02 from industrial waste gases. Most of the S02 is converted to elemental sulfur; only about I percent converted to sulfate The process comprises (1) washing the flue gas to remove particulates and S03, (2) absorption of the S02 in citric acid or other carboxylate solution, (3) reaction of the loaded solution with H2S in a closed vessel to precipitate the absorbed S02 as elemental sulfur, and (4) separation of the sulfur from the regenerated solution by oil flotation and melting. Two-thirds of the molten sulfur is converted to H2S for use in the sulfur precipitation step by reacting sulfur vapor with natural gas and steam in the presence of an alumina catalyst. The chemistry and mechanism of the process are described, initial laboratory and pilot plant data are summarized, and second-generation laboratory operation and pilot plant design are reviewed. Preliminary cost estimates are presented for recovering sulfur from copper smelter gas, powerplant flue gas, and Claus plant tail gas.

Jan 1, 1973

By M. Hertzberg

Results of a comprehensive study of the absolute spectral radiance of the infrared emissions from methane-air explosions are reported. The spectral growth of these expanding flames were recorded with a time resolution of 1 msec in the spectral range of 1.7 to 5.0 µm. Time-resolved spectra were obtained for methane-air mixtures as a function of stoichiometry, nitrogen dilution, and Halon dilution, in a 9-liter vessel under different venting conditions. Data are also presented for coal dust-air explosions. Temperatures, obtained from the absolute radiances and from a band ratio technique for methane-air, are internally consistent and are generally 50° to 200°K below adiabatic flame temperatures. All near limit mixtures gave essentially the same flame temperatures (1,500° to 1,600° K) regardless of whether the limit was obtained by dilution with excess air, excess methane, excess nitrogen, or Halon. The coal dust explosion spectrum is essentially a blackbody continuum at 1,500° K with some selective emission at 4.4 µm from hotter CO2. The data are analyzed in terms of the radiative dynamics of a sperically expanding flame zone. The importance of radiative transport is assessed. An equation is derived which relates the instantaneous fraction of combustion power radiated to adiabatic variables.

Jan 1, 1973

By Stanley C. Rhoads

The Bureau of Mines investigated the complete ternary system K2 HfF6¬K2ZrF6-l.25 weight-percent HF at 40° C. In addition, solubility curves have been established at 25°, 30°, 500, 60°, and 70° C. These solubility data implemented a study of hafnium enrichment in feed solutions for liquid-liquid extraction processes.. Selected K2HfF6-K2 ZrF6-1.25 weight-percent HF mixtures were equilibrated in a constant temperature bath. Compositions of the equilibrated solutions and wet residues were established from combined hafnium and zirconium oxide and total fluorine analyses. All solubility curves were essentially parallel on triangular coordinates. At 40° C, the solid phase of the K2HfF6-K2ZrF6-1.25 percent HF system is a series of solid solution hydrates with K2HfF6-H20 and K2ZrF6.3H2O segments existing at the respective extremes. Since this system contains K2HfF6-H20 and K2ZrF6.3H20 segments, it is not ideal for simple separation of high-purity K2HfF6 from K2HfF6-K2ZrF6 mixtures by recrystallization. However, it would be useful for producing hafnium-enriched feed solutions from zircon concentrates for liquid-liquid extraction of hafnium from zirconium.

Jan 1, 1973

By H. B. Carroll

This Bureau of Mines report evaluates the performance of commercially available portable instrumentation for the detection of carbon monoxide, carbon dioxide, oxygen, and methane at conditions simulating an industrial work atmosphere. Portable instrumentation included in the study was gas-detection tubes (length-of-stain and color intensity), catalytic detector, liquid absorption detectors, paramagnetic oxygen detector, galvanic detector, and pelement or hot-wire methane detectors. Evaluation of the instruments was in atmospheres with 50 and 80 percent relative humidities at 75° F and containing test gas concentrations of 0.1, 0.25, 0.50, 1.0, 1.5, and 2.0 times the thresh-old limit value. Correlation of the results from the portable gao analyzer with measurement from the standard instruments was made by calculating and plotting an estimated line of regression, prediction, and confidence limits and the correlation coefficient for each detector system. Relative humidity in the 50-to 80-percent range did not appear to contribute to instrumental uncertainties in either performance or operation. Considerable deviation in detection precision between the portable gas-detection systems and the standard systems was established, especially at the lower gas concentration levels. The main difference or inconsistency in toxic gas concentrations determined with length-of-stain tubes resulted from the observer's interpretation of the results rather than difference in the tubes themselves.

Jan 1, 1973

By H. W. Leavenworth

Research was conducted by the Bureau of Mines to develop a technique to grow metallic fibers from a sulfide mineral. In this research, chalcopyrite (CuFeS2) was made sulfur deficient, and the remaining sulfur partitioned to the iron in the mineral to liberate metallic copper, or to the copper to liberate metallic iron. The metals formed on the surface as fibers and in the interior as spherical particles. Fiber growth is very fast. Lengths of 3 to 4 cm form in a matter of minutes, and the diameter of individual fibers is less than 1 µm. The mechanism of fiber growth is explained, and the reactions are reversible as predicted. Copper fibers can be made to grow from the surface at 400° C or to dissolve back onto the solid surface and be replaced by iron fibers at 625° C. Growth and dissolution can also be controlled to form copper/iron duplex fibers.

Jan 1, 1974

By Clarence O. Babcock

This report describes the results of a Bureau of Mines investigation in which an elastic inclusion, orebody, or mining system is replaced for purposes of analysis with an imaginary effective inclusion of rectangular shape that encloses the region. This effective inclusion has averaged physical properties that are directly related to the average inclusion stresses. The results were in excellent agreement with those predicted by Donnell's theory (2)2 for an isotropic elliptical inclusion in a state of plane strain for all height-to-width ratios and for all degrees of inclusion hardness from very soft to very hard. The results are exact for an isotropic circular inclusion and provide an easy method of evaluating the stresses obtained by cylindrical inclusions in boreholes when the Poisson's ratio for both host and inclusion equals 0.25 for plane strain or 0.333 for plane stress. The theory was also used to predict the average stresses in 48 finite-element models of single transversely isotropic inclusions of ovaloid and rectangular shape. An interesting and useful observation from this work was that the forces on elliptical inclusions in the x and y directions, produced by applied uniaxial stresses in the y and x directions, respectively, were equal in magnitude but opposite in sign when the applied stresses were equal. This occurred when the plane strain condition was used with a Poisson's ratio of 0.25. The practical usefulness of the method is given by treating a variety of mining problems: (1) The average stresses in an orebody of irregular shape; (2) the average stresses in single-level room-and-pillar mining systems; (3) the average stresses in multiple-level room-and-pillar mining systems; (4) the effect of mining sequence on the average stresses produced during mining; (5) the stresses in cylindrical borehole plug related to host rock stresses as a function of plug hardness; and (6) methods for simplifying finite-element analysis of complex structures.

Jan 1, 1974

By Laxman S. Sundae

A Bureau of Mines investigation was conducted to determine the effect of specimen volume on the apparent tensile strength of disks of St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite. The investigation used a technique developed by the Bureau to determine apparent tensile strength. Because the test specimens were selected without macroscopic defects, that is, cracks, joints, and planes of weakness, the strength variations are solely due to microscopic features. Several replications of each test were performed. Data for each set of specimens were fitted to a power law of the form y = axb, where y = apparent tensile strength, x = specimen volume, and a and b are constants. This power law is essentially a form of Weibull's theory. The average coefficients of correlation for St. Cloud Gray Granodiorite, Lithonia granite, and Rockville granite were 0.85, 0.53, and 0.78, respecitvely. In all cases a decrease in strength with increasing volume was noted; in the extreme case, a decrease of 40 pct was noted with an elevenfold increase in volume. The decrease in strength with increasing specimen volume is explained in terms of Weibull's theory.

Jan 1, 1974