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By J. W. Thompson, M. N. RICH

That there is wide interest in the preparation and properties of metallic zirconium and its salts is indicated by the many articles recently published in scientific and technical journals and the many patents issued. The compounds of zirconium have numerous important uses and more uses will doubtless be found. In the course of the special work on rare metals that were of military importance during the war, the authors of this bulletin were detailed to the Golden mining experiment station of the Bureau of Mines to prepare metallic zirconium and to investigate its properties. A number of investigations in recent years have indicated that sintered or coherent zirconium metal is very resistive to acids; that it can be used for electrodes, and it probably will find metallurgical uses. A steel containing zirconium has been proposed for use in armor plate and automobile parts, and nickel-zirconium alloys have been suggested for high-speed cutting tools and for cutlery. Numerous articles in scientific journals have recommended the use of zirconium oxide as a refractory, an abrasive, a pigment in paints, and as an opaquing agent in enamel ware. The salts have been used in the textile industry' as a mordant and also for weighting silk. When the authors began their investigation, they found it necessary to collect all of the available literature on the general subject of zirconium and its compounds. Pure salts could not be obtained on the market, and in order to get these, as a preliminary step to the preparation of the metal, the literature had to be classified and the methods of preparing the salts investigated. Also, there was much difficulty at first in making satisfactory analyses, and this phase of the work received careful attention. As it was necessary to begin with a historical review of the literature, such a review is given as Part I of this report, and a bibliography is included as Part IV. References to the numbered items in this bibliography are made throughout the text, the usual footnote references being omitted. Analyses of the products and conclusions as to their purity are given under the descriptions of methods of preparation. A table showing the properties of the amorphous metal, and another showing the properties of the coherent metal, will be found under appropriate headings in Part II. No attempt has been made in the historical review to discuss fully all the published information about zirconium and its compounds, but only such material has been assembled as has a direct bearing upon the present work. Considerable difficulty was experienced in collecting this material because of the confusion of terms by various authors who perhaps did not thoroughly understand the chemistry of zirconium.

Jan 1, 1921

By Arne Landsberg

Experiments were made with a batch reactor to determine the effect of gas pressures, temperature, and gamma radiation intensity on the reaction CO + Ch ? COC12. The equation, [dp = 0.0110 (1 - 0.01t) (PCOI)1/2 PC12] where [dP] is the change of pressure of phosgene with time (atm/hr), t is the temperature (°C), PCO and PC12 are the reactant pressures (atm), and I is the radiation intensity (r/hr), was found to best fit the data. Oxygen and a large ratio of reactor surface to volume retarded the reaction, but inert gases had no effect. A low-temperature reactor system is proposed to take advantage of the conditions which give a high reaction rate with gamma radiation and a simple scheme of product purification.

Jan 1, 1970

By T. R. Achenbach

1. This, the final report to the U. S. Bureau of Mines on the program with the subject title, presents the data obtained from June 29, 1973, to April 20, 1974. 2. Operating in the Illinois #6 coal seam, the effectiveness of foam opposed to water was compared in reducing respirable coal dust. A combination of 39 foam generators and 14 water sprays were used during the foam tests. Sixty one water sprays were operated during the water tests. Data from 24 shifts using foam and 21 shifts using water are presented. 3. Additional work on foam generator design should be undertaken to provide coverage to a wider area with foam. 4. The general attitude of those working on the foam program and with the miner at the face was positive. It is urged that the work be continued. 5. The minor respiratory irritations evidently caused by an aerosol effect of the surfactant should be investigated. 6. The statistical analysis of the tests will be made and reported by the U. S. Bureau of Mines.

Jan 1, 1974

By M. E. Poad

Structural properties of steel-fiber-reinforced shotcrete and polymer-impregnated shotcrete, both plain and fiber-reinforced, were investigated by the Federal Bureau of Mines, Spokane Mining Research Center. The research center has found that flexural strengths can be increased by as much as 106 percent, and splitting-tensile strength by 50 percent, by introducing randomly oriented steel fibers. A slight decrease of compressive strength was found in the fiber-reinforced shotcrete. Polymer-impregnated shotcrete exhibited a threefold to fourfold increase in compressive and splitting-tensile strength. The techniques of preparing shotcrete with the dry process, using both fast-set agents and regulated-set cement, are described, along with the results of physical-property testing. Physical properties include compressive and splitting-tensile strengths, tangent and secant moduli, and stress-strain curves for plain shotcrete, fiber-reinforced shotcrete, and polymer-impregnated plain and fiber-reinforced shotcrete. Flexural strengths for plain and fiber-reinforced shotcrete are also reported. Steel-fiber shotcrete is the more promising of the new structural materials for ground support, and additional research is recommended.

Jan 1, 1975

By E. M. Murphy

Comparative data from ASTM method of test E-162 and large-scale trials in the Experimental Mine show that the flame-spread quality of brattice cloth and other ventilation control materials can effectively be evaluated by either method. Materials having a flame spread index of 25 or less, as determined by the simpler and more economical laboratory test ASTM E-162, do not present a serious fire hazard when used in coal mines.

Jan 1, 1972

[Determine how subsidence resulting from underground coal mining affects surface structures, and evaluate the usefulness s of the tiltmeter for monitoring foundation movement. Approach The Bureau of Mines is studying foundation response to mine subsidence in order to determine how subsidence-induced ground movements affect foundations in place directly above the mint. These investigations are essential if economic mitigation and repair techniques are to be made. In addition, commercially available tiltmeter are being evaluated (or use as a cost-effective monitoring technique. To study foundation response and to evaluate the tiltmeter system, full-scale model foundations were constructed, instrumented, and monitored for three years. Vertical and horizontal displacements, tilt magnitudes and directions, and observed damages were recorded. Displacements were compared with measured lilt to determine if the tiltmeter was tracking foundation response to subsidence, The Bureau developed a computer software package to aid in the reduction and analysis of the tiltmeter data.]

Jan 1, 1988

By Michael J. Sapko, Gregory M. Green, Kenneth L. Cashdollar

The National Institute for Occupational Safety and Health (NIOSH) and the Mine Safety and Health Administration (MSHA) conducted a joint survey to determine the range of coal particle sizes found in dust samples collected from intake airways of US coal mines. The last comprehensive survey of this type was performed in the 1920s. The size of the coal dust is relevant to the amount of rock dust required to inert the coal dust, with more rock dust needed to inert finer sizes of coal dust. Dust samples were collected by MSHA inspectors from several mines in each of MSHA's 10 bituminous Coal Mine Safety and Health Districts. Samples were normally collected in several intakes at each mine. The laboratory analysis procedures included acid leaching of the sample to remove the limestone rock dust, sonic sieving to determine the dust size, and low-temperature ashing of the sieved fractions to correct for any remaining incombustible matter. The results indicate that particle sizes of mine coal dust in intake airways are finer than those measured in the 1920s. This finer size coal dust in intake airways would require more incombustible matter to be effectively inerted than the 65% incombustible specified in current regulations.

By N. E. Hanna

An investigation was made of pressure pulses produced by unconfined explosive blasts in underground openings. Four tests were made with TNT or modified amatol charges ranging in weight from 60 to 2,000 pounds; each test involved either single or multiple charges. Pressure-time profiles were obtained using mechanical self-recording pressure gages. The cube-root scaling law for peak pressure was found to be valid within about 1 tunnel diameter; at greater distances, the pressures obtained along direct paths were generally higher than this scaling law would indicate.

Jan 1, 1968

By Harold E. Marr

A simple algorithm is presented for processing digitized X-ray spectra obtained with a Si(Li) or Ge(Li) semiconductor detector coupled to a multi- channel analyzer. The simplified least-squares procedure is used to smooth out the statistical fluctuations in the spectrum by repeatedly fitting a quad- ratic equation to a predetermined number of channels and performing a traveling smooth across the spectrum. A logarithmic transform is applied to the raw data to minimize the distortion of the gaussian-shaped peak profiles. The efficacy of the technique is evaluated by observing the distortion of several gaussian-shaped peaks that have been subjected to the smoothing operation. The locations of maximums and minimums in the spectrum are predicted in the process as well as the values of the peak heights. The convolution integers from a least-squares fit of a quadratic equation are calculated as part of a FORTRAN subroutine. The building-block approach to computer programing in a small laboratory is discussed.

Jan 1, 1972

By Sterling J. Anderson

To define the technical competence and capabilities of a nonexplosive excavation concept, the Bureau of Mines conducted reduced-scale laboratory tests of a mechanical excavation tool called a rock splitter. Hydraulically actuated splitters, capable of generating both radial and axial loads on a predrilled hole, were designed and fabricated. Through paired variable testing and drifting simulation, reduced-scale splitter performance was evaluated in concrete. Testing proved that the rock splitter is capable of excavating within the highly confined drift set-ting and that it offers a distinct advantage over splitters that can generate radial loads only.

Jan 1, 1982

By D. A. Keefe, O&apos

The electrowinning of beryllium from beryllium oxide (BeO) using a molten-salt electrolyte composed of 56 LiF-37 BeF2-7 BeO (mole-percent) was investigated. Anodes made of porous carbon were found to be superior in current-carrying capacity and gave a lower cell voltage than other types of anode material tested. When porous carbon anodes were used) the resultant increase in anode area prevented anode passivation. The cell voltage was 3.3 volts) and electrode current efficiencies of 50 to 70 percent were obtained. The electrodeposited beryllium was recovered as beryllium powder or was coalesced to metal beads by heating to 1,300° C.

Jan 1, 1970

By R. Karl Zipf

Multiple seam mining interactions caused by full extraction mining, whether due to undermining or overmining, frequently involve tensile failure of the affected mine roof. The adverse ground control conditions may prevent mining for both safety and economic reasons. Prior researchers have identified the geometric, geologic and mining factors controlling multiple seam mining interactions. This numerical study examines the mechanics of these interactions using a modeling procedure that 1) incorporates the essential constitutive behavior of the rock such as strain-softening of the intact rock and shear and tensile failure along bedding planes and 2) captures the geologic variability of the rock especially the layering of weak and strong rocks and weak bedding planes. Specifically, the numerical study considered the effect of vertical stress, interburden thickness, and the immediate roof quality of the affected seam in both undermining and overmining situations. The models show that for overburden-to-interburden thickness (OB/IB) ratios of less than 5, interactions do not occur, and that for OB/IB more than 50, extreme interaction is a certainty. In between, the possibility of an interaction was found to depend on gob width-to-interburden thickness ratio, site specific geology and horizontal stress to rock strength ratio in addition to the OB/IB ratio. The models also showed that horizontal stress was profoundly altered well above or below a full extraction area and that these changes are likely to influence the success or failure of multiple seam mining. The role of horizontal stress in multiple seam mining interactions has received little attention in prior investigations. Four factors control the mechanics of multiple seam mining interactions: 1. vertical stress concentration 2. horizontal stress concentration 3. stress re-direction 4. bedding plane slip bands A combination of vertical and horizontal stress increase and high stress gradients in the vicinity of full extraction areas re-orients principal stresses into a very unfavorable direction. This seemingly small stress re-orientation has a profound adverse effect on bedded rock.

By Wilbert J. Huff

This is the sixth of a series of annual reports describing the work of the Explosives Division, Bureau of Mines, United States Department of the Interior.3/ It deals particularly with the activities of the division from July 1, 1940 to June 30, 1941. The studies outlined in this and preceding reports of the series have been conducted under the direction of the author and the respective unit leaders, to whom specific credit is given.

Jan 1, 1942

By Wilbert J. Huff

This is the sixth of a series of annual reports describing the work of the? Explosives Division, Bureau of Mines, United States Department of the Interior.3/ It deals particularly with the activities of the division from July 1, 1940, to June 30, 1941. The studies outlined in this and preceding reports of the series have been conducted under the direction of the author and the respective unit leaders, to whom specific credit is given.

Jan 1, 1942

By Annie G. Smelley

As part of its program to develop technology that will encourage maximum utilization of the Nation's mineral resources, the Bureau of Mines conducted research on debrining potash-clay waste slurries by means of flocculation with a high-molecular-weight polymer and subsequent solid-liquid separation on a rotating trommel screen. In laboratory batch tests, potash-clay waste slurries were consolidated from initial clay contents of 8 pct to final contents of 30 pct with a polymer dosage of 1.2 Ib/ton of dry clay waste. Small-scale continuous tests yielded debrined products containing 20 pct solids using a polymer dosage of 1 Ib/ton of dry clay solids.

Jan 1, 1983

By Andrew M. Leszcykowski

In 1984, personnel from the U.S. Bureau of Mines examined 41,550 acres of the North Fork Owyhee River Wilderness Study Area for mineral resources. This study area, in southwestern Idaho, is underlain by tuffs and basalt of Tertiary age. There are no known mines, claims, or prospects in or near the area. The northeast and southwest corners of the area are covered by oil and gas leases or lease applications, but no known exploration has been conducted. On Nickel Creek and Pleasant Valley Tables, in the southern part of the area, thin flows of vesicular, moss-covered basalt occur that are suitable for use as decorative building stone. The stone available for exploitation crops out over several square miles. However, more suitable material, outside the study area, is closer to potential markets.

Jan 1, 1986

By M. Kanefsky

Two channel polarity coincidence and polarity difference statistics are analyzed. The signal, common to both channels, consists of sinusoidal bursts where the exact frequency of the signal is nearly known, but other parameters such as amplitude, phase, and pulse starting time are unknown. The noise inputs are dependent, narrow band, Markov processes. It is shown that the performance depends not only on the signal uncertainties, but on the precise shape of the cross-correlation functions between the noise in-puts. By using two polairty difference statistics in addition to the polarity coincidence statistic, it is shown that the decrease in performance, as well as the cost of hard limiting due to correlated inputs, can be made small.

Jan 1, 1981

As mine haulage vehicles become larger, the danger to a driver during a fire emergency is increased by the greater height of the cab above ground. Also, property damage due to fires on bigger trucks can be substantial. To solve this problem, the Department of Interior's Bureau of Mines, through two research and development contracts with FMC Corporation, San Jose, California, has developed two reasonably priced, reliable automatic fire sensing and suppression prototype systems for large haulage vehicles. At the onset of the large mobile equipment fire protection contract effort, it was learned that fires were frequently experienced in open-pit mine haulage equipment, especially large trucks. As the size of equipment has grown, so has the hazard presented to an operator forced to leave his truck in a hurry when fire breaks out and his normal path to the ground is blocked by flames. His only recourse is to jump from the cab platform to the ground, and the one-story drop of 10 feet or more can severely injure him. It is with these factors in mind that a program was undertaken to provide a fire detection and extinguishing capability tor the large mobile equipment, especially trucks, used in open pit mines.

Jan 1, 2012

By Thomas J. Peters

Tungsten, silver, lead, zinc, and placer gold occur in the Cucamonga B RARE II area (no. B5174). A strata-bound, scheelite-bearing zone at the Blue Diamond prospect (fig. 1, no. 1) contains an estimated 16,000 tons (15,000 t) of identified, subeconomic resources averaging 0.16 percent tungsten trioxide (W03). There is a high potential for discovering additional tungsten resources at this property. The California-Hercules prospect (fig. 1, no. 5) ha; a mineral occurrence which contains an estimated 1,000 tons (900 t) of tactite averaging 1.3 oz silver per ton (45 g/t), 0.75 percent lead, and 0.72 percent zinc. Another occurrence, at the Blew Jordam Prospect (fig. 1, no. 4) has an estimated 100 tons (90 t) of tactite averaging 10 oz silver per ton (340 ,/t), 3.75 percent zinc, and 2.3 percent lead. There is a moderate potential for discovering silver, lead, and zinc resources at these prospects, which are in metamorphic pendants. There are a few lode gold prospects in the area (fig. 1, nos. 3, 11, 14) are on geologic structures which parallel the San Andreas Fault, northeast of the area. These deposits are not well exposed and have been historically unproductive. Placer gold in area B occurs locally in the beds of intermittent tributaries to Lytle Creek (fig. 1, nos. 10, 12, 13) in concentrations as high as $1.17 per cu yd ($1.53/cu m, at a gold price of $450 per troy oz). The deposits have no significant volume, but could be utilized for recreational panning and suction dredging. In the Cucamonga C RARE II area (No. C5174) placer gold occurrences locally contain as much as $1.23 per cu yd ($1.61/cu m). However, gravel containing the gold appears to be limited to stream beds, and does not occur in sufficient quantity to constitute resources. Recreational panning and dredging also may occur in this area.

Jan 1, 1983

By R. E. Mussier

This investigation was made to study new methods to prepare high-purity yttrium metal, Various methods were used to prepare pure intermediate compounds, primarily chlorides, bromides, and iodides, which were subsequently reduced to metal. The process found most suitable for the preparation of pure anhydrous yttrium chloride involved thermal dehydration of a mixture of hydrated yttrium chloride and ammonium chloride while under vacuum. Yttrium bromide and iodide were prepared most effectively by the direct halogenation of yttrim carbide. Yttrim carbide was obtained by reacting and melting yttrium oxide-carbon mixtures in a carbon-arc furnace. Yttrium halides were purified by vacuum distillation and reduced by alkali or alkaline-earth metals. Lithium and sodium proved to be the best reductants from the standpoint of yield (>95 pct) and purity (>99.8 pct) of the yttrium. The product of the reduction step was sponge metal, which was consolidated readily by conventional cold-mold, arc-melting procedure. The purest yttrium obtained in laboratory scale work was prepared by sodium reduction of yttrium chloride and contained only 125 pp oxygen; other impurities did not exceed 1,000 ppm. In larger scale tests yttrium containing only 800 to 1,000 ppm total impurities was obtained by lithium reduction of yttrium chloride. The tensile properties of high-purity yttrium were determined. Mechanical tests showed that yttrium can be forged, extruded, rolled, spot welded, and deep drawn.

Jan 1, 1963