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By P. M. Johnson

A design for a laser-powered optical interferometer, using a specimen whose thermal expansion is to be measured as part of the optical system, was conceived and applied in a prototype dilatometer. The object of thin work was the development of an absolute dilatometer capable of use at elevated temperature, particularly above 1,000° C. The prototype has been operated at temperatures exceeding 1,510° C. Results obtained with this device agree within 2.5 percent with the published data for the coefficient of expansion of columbium.

Jan 1, 1968

By M. J. Ferrante

The preparation and subsequent reduction of vanadium trichloride was investigated as a process for the production of high-purity vanadium metal. Chlorine was reacted with vanadium oxide in the presence of carbon to vanadium tetrachloride. The contaminant vanadium oxytrichloride was also formed and later converted to tetrachloride by reaction with chlorine in the presence of activated charcoal. Vanadium tetrachloride was stirred continuously during thermal dissociation to vanadium trichloride powder from which volatile contaminants were removed by distillation. The vanadium trichloride powder was reduced to vanadium sponge by controlled feeding of the trichloride into molten magnesium. Excess reductant and byproduct salt were removed from the vanadium sponge by high-vacuum distillation. Batches as large as 6.5 kilograms of sponge metal were prepared at an average reaction efficiency of 98 percent. Vanadium sponge after consolidation by arc-melting contained 820 to 11330 ppm of interstitial impurities and had a hardness between Rockwell B 40 and 70, This metal exhibited excellent workability at room temperature. The purification of impure vanadium metal by electron-beam melting resulted in lowering interstitial impurities from 1,890 to 504 ppm and hardness from Rockwell B 87 to 28.

Jan 1, 1968

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 Eldon C. Pattee

Reconnaisance samples of reported beryllium occurrences in Idaho, Washington, Montana, and Oregon were chemically and spectroscopically tested in a mobile laboratory. The two predominant types of occurrences were green beryl associated with Cretaceous intrusions and disseminated aquamarine associated with Tertiary intrusions. Although the beryllium content of known deposits in the Northwest is too low for economic development at present, total submarginal-grade beryllium resources in pegmatites are estimated to be 570,000 to 1,870,000 tons containing 0.024 to 0.167 BeO. A potential source of 500,000 to 700,000 tons of beryllium-bearing tactite in Idaho and Montana averages 0.033 to 0.080 percent BeO.

Jan 1, 1968

By F. W. Wood

The use of consumable.-electrode arc melting as a production technology is growing. One advantageous feature of this process is that it avoids ingot contamination by soluble crucible materials by employing a chilled metal crucible. Because the thermal balance under these conditions is rather delicate and does not necessarily provide a favorable environment for solidification, catastrophic imbalances can occur. The effectiveness and mechanistic roles of various factors are mostly unknown, and more intelligent insight regarding the distribution of temperature and heat is needed. Experience has provided several pertinent observations, some of which are quite superficial. The most meaningful data have resulted from studies of molten pool shapes and sizes and from measurements of heat flow through crucible walls. Overall experience, intuitively interpreted and supplemented, is sufficient nevertheless as a basis for a boundary-value treatment of the problem. A mathematical analysis based on a separation of variables, using conventional differential equation methods, provides a useful solution. For a cylindrical ingot, the temperature varies as a Bessel function of an argument proportional to the radius and as an exponential function of longitudinal position. Trial calculations using the problem solution seem to verify the general correctness of the result as compared with experience. The role and nature of solution parameters are also clarified, though not entirely resolved. It is revealed that the barrier to heat flow at the ingot-crucible surface has a prominent influence. Utility of the model embodied in the problem solution is readily demonstrated by considering a variety of contemporary questions about arc melting, and it is hoped that utility can be enhanced by improvement of the model.

Jan 1, 1968

By Robert A. Bradburn

The Bureau of Mines has developed a miniature, portable two-level oxygen-deficiency alarm and produced three prototype models. Each operates from a 4.2-v dc power source, and the highest current drain of any model is 80 ma. An electrochemical cell, which produces an electrical output in proportion to the partial pressure of oxygen to which it is exposed, is used as an oxygen detector. The output of the cell is applied to an electronic circuit that detects two different levels of oxygen percentage below that of normal air, and produces distinct audible signals at these levels. The hazard alarm mode is activated when the oxygen percentage first drops below normal and produces a 500-cps "beep" tone with an intermittency of 1 cps. The danger mode produces a continuous 500-cps audible signal when the oxygen percentage drops still lower.

Jan 1, 1968

By Martin H. Stanczyk

Bench scale, laboratory batch attrition grinding tests were made of a coarse commercial kaolin in a stainless steel, 5-inch-diameter attrition grinding machine to study the effect of a number of basic operating variables on particle size reduction and electric energy consumption. The results of the investigation showed that the more important operating variables influencing the efficiency of kaolin comminution and energy consumption requirements were type, size, and shape of grinding media, grinding media to clay weight ratio, peripheral rotor speed, clay slip pulp density, degree of pulp dispersion, and the angular arrangement of the rotor and stator bars. The tests also indicated that variables having less influence on grinding efficiency and energy consumption were pulp temperature, design of rotor cage, rotor clearance, rotor-stator bar interval, addition agents, pulp level, degree of pulp aeration, and chamber liners. The research showed that grinding media had the greatest influence on abrasion of machine parts and that spherical-shaped grinding media were superior to sharp angular or long bladed media with respect to media degradation, machine abrasion as well as grinding efficiency.

Jan 1, 1968

By W. L. Acherman

The Bureau of Mines found the chemical and galvanic corrosion behavior of the TZM and molybdenum-30 tungsten alloys to be generally equal or superior to that of unalloyed molybdenum in many aqueous solutions of acids, bases, and salts. Notable exceptions occurred in 1 [N] nitric acid, where both alloys corroded appreciably faster than molybdenum. In mercuric chloride solutions, the TZM alloy was susceptible to a type of crevice corrosion which was not due to differential aeration. The alloys were usually not adversely affected by con-tact with dissimilar metals in galvanic couple experiments, but the dissimilar metals sometimes corroded galvanically. Both alloys were resistant to substitute ocean water spray at 60° C.

Jan 1, 1968

By John R. Hoskins

The Bureau of Mines conducted an investigation to more exactly define the influence of some end conditions on the laboratory-determined uniaxial compressive strength of rock samples. Limestone, marble, sandstone, and granite were used to provide a range of specimen modulus of elasticity from 2.7 X 106 psi to 10 x 106 psi. Four variables were studied: Nonparallelism and surface texture of specimen ends were the specimen variables investigated; the end platen size and the adjustable or spherical head friction were the machine variables studied. It was concluded that the loading ends of small laboratory models and samples should be prepared with surface irregularities that do not vary from a plane surface by more than 0.001 inch. It was also concluded that nonparallelism of the specimen ends should not exceed 8 minutes for a rigid head load or 15 minutes for an adjusting head load. The measured compressive strength of specimens prepared with these tolerances will be statistically the same with any diameter or thickness of platen and any degree of head friction if initial alinement of the specimen is assured.

Jan 1, 1968

By Elbridge W. Gresseth

Rock deformational structures in a deep mine were analyzed by petrofabric techniques to learn (1) the relative magnitude and direction of the principal stresses involved in tectonic deformations prior to mining, (2) the preferred orientation of rock planar discontinuities which define rock anistropy prior to mining, and (3) the relationship of mining-induced rock failure to inherent rock stresses and inherent rock anisotropy. Rock fabric elements used for petrofabric analysis consisted of bedding planes, faults, joints, fractures, foliation, sericite plane (001), quartz axis [0001], quartz deformation lamellae, and microfractures. Structures and structural symmetries from different areas within the mine and from different scales of observation were compared to learn the nature of rock anisotropy and the orientation of the principal stresses defined by rock deformations. Analysis of such fabric as regional and macroscopic faults, b-c joints, quartz [0001], sericite (001), and microfractures, indicate that during the epochs of tectonic deformation, the maximum and minimum principal stresses were horizontally oriented and acted along northwest and northeast axes, respectively. This condition of regional stress appears to have continued during folding and the associated period of faulting. The most recent tectonic deformation represents a rotation of the minimum principal stresses into a vertical position, as shown by the development of a tensile joint system, quartz deformation lamellae, and microfractures. Good interscale correlation and statistical homogeneity of tectonic fabric indicate a stress field homogeneity in this area during tectonic deformation. Rock physical anisotropy is genetically associated with tectonic fabric and consists of preferentially oriented planar discontinuities intersecting along a nearly vertical axis. The mining-induced deformations were correlated with the inherent rock anisotropy which either directly controls or greatly affects their development. This phase of rock deformation shows a greater degree of stress field heterogeneity than was the case with tectonic deformations This is explained as a result of nonconfinement afforded by underground openings and the increase in ground stresses due to mining activity"

Jan 1, 1968

By E. A. Mihok

A pilot plant for treating mine drainage by neutralization with limestone was designed, fabricated, and operated by the Bureau of Mines. The process consists of (1) producing a very fine (minus 400-mesh) limestone slurry, (2) mixing the slurry with the mine water, (3) aerating the resulting mixture to remove carbon dioxide and precipitate iron, and (4) separating the solids from the liquid by sedimentation. A mine discharge of pH 2.8, containing 1,700 ppm total acidity, 36 ppm ferrous iron, and 360 ppm total iron, was treated at rates from 300 to 400 gpm. The treated water ultimately reached a pH of 7.4 and contained no detectable iron. The resulting sludge compacted to approximately one-third the volume of sludge from mine water neutralized with lime. The advantages of the limestone process, compared with the conventional lime process are as follows: Widespread distribution and lower cost of run-of-mine, indigenous limestone; simplicity of plant design; reduced hazards and plant operating and maintenance costs accruing from the use of a less reactive chemical agent; higher solids concentration of the precipitated sludge; and no deleterious effect caused by accidental overtreatment. While total process costs could not be determined, it is conservatively estimated that the cost of treating mine water by the limestone process is one-third to one-half the cost of the lime process, depending on the characteristics of the water to be treated and the availability and quality of limestone used.

Jan 1, 1968

By Robert L. de Beauchamp

The Bureau of Mines designed a chlorination apparatus to prepare CrCl2 free of CrCl3 by the direct reaction of chlorine and chromium. Equipment and procedures were developed for routine preparation of 25-pound batch quantities of anhydrous CrCl2. Calcium, iron, nickel, and silicon impurities were in the 0.01 to 0.05 percent range, and all other impurities were below 0.01 percent.

Jan 1, 1968

By David E. Nicholson

The Bureau of Mines has constructed a special compression chamber for developing stress-strain relationships of mine backfill and simulating the high compressive ground pressures encountered in underground mines. A one-dimensional, or Earth-Pressure-at-Rest model is proposed for backfills subjected to these pressures. Results of the compression tests performed in the chamber indicate that reliable stress-strain relationships can be developed from these tests. The primary objective of the test series was to evaluate the effectiveness of compaction of common backfills in retarding ground closure. Analysis of the stress-strain data shows an eightfold reduction in relative strain in optimum well-graded, compacted backfills over poorly graded, loose backfill material. Analysis of the one-dimensional compression test data also indicates a significant retardation of transmitted stress in dense compacted samples of backfill and natural sands. Although not fully understood, a deformation mechanism is thought to occur at the intergranular contacts in cyclic fashion causing frictional heat loss and a reduction in transmitted stresses in the densely packed materials. The experimental values of transmitted stress are compared with theoretical values of effective stress calculated from the one-dimensional compression relationships developed by Hendron (4).3 These experimental values of transmitted stress compare very closely with the theoretical values of effective stress.

Jan 1, 1968

By H. V. Makar

Laboratory tests were performed to obtain a quantitative description of the effectiveness of sodium sulfate (Na2SO4) for removing copper from molten iron and to determine the effectiveness of Na2SO4 on actual auto scrap. The tests were conducted on induction melted heats of iron averaging 0.58 and 1.50 percent initial copper and on cupola-melted auto scrap containing 0.45 percent initial copper. The Na2SO4 was added in powder form in amounts ranging from 2.9 to 43.8 percent of the weight of iron being treated. The data showed that copper removal for the various Na2SO4 treatments followed a similar trend, regardless of the iron composition that was tested. The equation Y = 1 - e-3.23x approximately reflects the relationship between copper removal and amount of Na2SO4 added, where Y is the fraction of copper removed and x is the ratio of the weight of Na2SO4 added to the weight of metal treated. Copper removals ranged from 3.3 to 74.5 percent and reductions down to less than 0.10 percent final copper were achieved in the auto scrap. Copper removals were generally accompanied by sulfur removal, and initial sulfur contents ranging from 0.10 to 0.20 percent were reduced to as low as 0.02 percent. High temperatures and long slag reaction times tended to induce copper and sulfur reversion from the slag, but, generally, the Na2SO4 treat¬ments were effective up to approximately 2,820° F with reaction times not exceeding 7 minutes.

Jan 1, 1968

By R. H. Oitto

To determine whether reflectors could substitute for the trip lights referred to in the Federal Mine Safety Code, the Bureau of Mines studied trip safety devices under simulated haulageway conditions. The noticeability of reflectors compared with trip lights and fluorescent panels was evaluated from distances of up to 850 feet with light source intensities of up to 1-6 foot-candles (ft c). Reflectors tested consisted of a reflective lens in a holder secured to a frame that can be attached to a trip. Reflectors were found to be suitable for use as a trip safety device. In fact, for the conditions in many underground haulageways some reflectors would be more effective than a permissible trip light.

Jan 1, 1968

By C. B. Kenahan

The Bureau of Mines is developing methods for reclaiming the metal and mineral values contained in municipal incinerator residues. This report describes the first phase of the research, in which reliable methods for sampling and analyzing municipal residues were established and the composition and characteristics of the residues were determined. Samples were obtained from a variety of grate-type furnaces and also from a rotary kiln furnace. The samples were processed on a batch basis and separated into their natural categories by a variety of methods including screening, magnetic separation, air separation techniques, and handpicking. The main components of the residues were determined to be metal and metal oxides, glass, and ash.

Jan 1, 1968

By J. W. Town

The Bureau of Mines determined the physical properties of southeastern Idaho phosphate fines as related to mineral composition, particle size and liberation, beneficiation, and potential use in structural clay products. The phosphate mineral in the fines was identified by unit-cell dimensions to be essentially the same as the phosphate mineral fluorapatite identified in the coarser sizes. The mean particle frequency as determined by electron-microscopy and pipet-analyses was between 0.5 and 0.2 micron. Liberation of the phosphate could not be definitely determined because of the weathered condition of the minerals and their extreme fineness. No beneficiation scheme was developed that would concentrate the phosphate into a marketable fertilizer product; therefore, forming and firing tests were made to demonstrate that the fines can be used to manufacture structural clay products.

Jan 1, 1968

By K. R. Dorman

To further investigate the potential of precast concrete sets as a support medium for underground mines, the Bureau of Mines designed a five-piece precast concrete drift set for a small opening and tested it to destruction in a straining frame. Twenty-seven tests were made with three sizes of members using three loading conditions. In addition, six tests were made with sets in a distorted configuration, Test results and typical failure patterns are presented. A comparison of results with those previously reported for the three-piece set shows the five-piece set supports considerably larger total loads than does the three-piece set of equivalent cross section designed for the same size of opening. Recommendations are made for improvements in design.

Jan 1, 1969

By R. K. Koch

The vapor pressures of liquid titanium and liquid platinum were studied under the Bureau of Mines program for the determination of thermochemical data on the transition elements. Beating was done in a 2-kw electron-beam furnace with a water-cooled copper crucible to contain the melt. Temperature was measured with a disappearing-filament brightness pyrometer. The vapor pressure data for liquid titanium in the range 2,008° to 2,379° K are represented by the least-squares derived equation [log p (atm) = 6.268 - 22, T] Two series of determinations were made on liquid platinum. Results of the first series are expressed by the least-squares derived equation [log p (atm) = 8.240 - 30,460T] for the range 2,0860 to 2,4200 K. Results of the second series are expressed by the least-squares derived equation [log p (atm) = 7.795 - 29,580 T] in the range 2,045° to 2,442° K. Third-law evaluations of each series gave mean standard heats of sublimation of 112.4 kcal/mole, 133.3 kcal/mole, and 133.8 kcal/mole for titanium first series on platinum, and second series on platinum, respectively. Second-law heats of sublimation and equations for heats, free energies, and entropies of vaporization were obtained from sigma plots of each data set.

Jan 1, 1969

By K-H. Frohne

This report presents a study of the Cooper sand of the Fork Run pool of Warren and McKean Counties, Pa., and a prediction of the secondary oil recovery by gasflooding the reservoir. A computer program employing a modification of the Craig, Geffen, and Morse secondary recovery calculation was used to make the gas flood performance forecast and is presented in the appendix. The Cooper sand reservoir in the Fork Run pool lies at a depth of about 1,900 feet and covers an area 1/2 mile wide by 2-1/4 miles long. Original oil in place is estimated to have been 8,266,000 STB. The primary recovery mechanism is solution gas drive, and ultimate primary recovery may reach 20 percent over a well life of 90 years. Two computer predictions were made for gas flooding the Cooper reservoir. The first was for a 25-acre pilot five-spot utilizing existing wells, but project economics were poor since only 25 percent of injection gas is utilized for pilot oil recovery. Recovery was 71,000 STB, or 22 percent of oil in place at flood initiation, but required 25,700 scf gas injected per STB of oil recovered. In the second prediction, pilot area performance was projected for the entire Fork Run pool, and economics became good. Recovery was 1,753,000 STB from 25 five-spots after the injection of only 6,400 scf per STB of oil recovered.

Jan 1, 1969