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By R. K. Koch

The vapor pressures of liquid columbium and liquid hafnium were deter-mined by the Langmuir free evaporation method as a part of the Bureau of Mines program on the study of transition metals. An electron-beam furnace with a water-cooled copper crucible was used for melting. Temperature was measured with a two-color ratio pyrometer. Least-squares analyses of the vapor pres-sure data gave the following equations: [Logp (atm) = 5 .429 -31,310 T] for liquid columbium in the range 2,740° - 3,140° K, and [Log p (atm) = 5,690 28 T] for liquid zirconium in the range 2,500° -2,810° K. Third-law evaluations of each data set gave mean heats of sublimation (298.15° K) of 175.1±3.2 kcal/mole and 148.3±1.2 kcal/mole for columbium and hafnium, respectively. Second-law standard heats of sublimation determined from sigma plots and from sigma-prime plots agreed fairly well with the third-law values. The sigma-prime plots gave standard entropies of sublimation of 30.96±0.84 eu and 33.S6±0.44 eu for columbium and hafnium, respectively.

Jan 1, 1968

By C. M. Mason

Mechanical mining produces large quantities of very fine coal dust called float dust. The associated increase in hazard requires a reexamination of the Bureau of Mines method of evaluating the incendivity of explosives in coal dust-gas-air mixtures. A technique recently developed by Bureau of Mines laboratories for evaluating the incendivity of explosives in coal dust-air mixtures was applied, with modifications, to coal dust-air-natural gas mixtures. A series of permissible explosives were evaluated by this modified technique. Results indicate that the modified technique could be the basis of a more discriminatory procedure than that presently in use.

Jan 1, 1968

By Ronald P. Hollenbeck

Shales in the Appalachian Region of Kentucky and Tennessee were sampled and tested to determine their use as raw materials for the manufacture of lightweight aggregate by the rotary-kiln method. Nine samples were obtained from eastern Kentucky and 143 samples were obtained from eastern Tennessee. As a result of preliminary testing of these samples, two sources in eastern Kentucky and 11 sources in eastern Tennessee were resampled for rotary-kiln tests. The rotary-kiln tests showed the two sources in Kentucky and seven sources in Tennessee contained shale that would produce satisfactory aggregate. Lightweight aggregate processed from these nine sources was tested in concrete shapes and was found to be suitable for use in structural concrete.

Jan 1, 1968

By A. G. Starliper

The Bureau of Mines made laboratory investigations to determine the feasibility of utilizing fine tungsten wires to reinforce a number of nonferrous metals and alloys and a superalloy, S-8l6. The composites of tungsten filament and metals were chosen to attain elevated temperature strength and corrosion resistance. Oriented clean or precoated tungsten wires were incorporated with the other metals by extrusion, swaging, and infiltration casting. Although widely varying characteristics were found in the composites, none were considered satisfactory for high-temperature use, chiefly because of reactions between the matrix metal-tungsten surface. Diffusion, solution, and chemical reactions between matrix and tungsten wires were sufficiently slow for some combinations, such as 15 v/o 8-816, to exhibit increased high-temperature strength for a limited time. A few metals failed to wet or bond to the tungsten surfaces, while a few responded after precoating with a third metal.

Jan 1, 1968

By D. E. Wolfson

The Bureau of Mines carbonized 21 coal samples from Fayette, Greene, and Washington Counties, Pa., at 900° C, using the Bureau of Mines-American Gas Association (BM-AGA) method, and determined yields of products and physical properties of the coke. These samples represented high-volatile A Pittsburgh, Sewickley, Waynesburg, and Upper Freeport and medium-volatile Upper Freeport and Lower Kittanning coals. About 20 percent of all coals presently carbonized in commercial coke ovens in the United States are mined in Greene and Washington Counties, principally from the Pittsburgh seam. Sulfur content of the Pittsburgh coals in these counties is moderately high (1.0 to 3.2 percent) but, because of extremely large reserves, accessibility to eastern United States markets and excellent blending characteristics to yield strong coke, these counties will continue to be an important source of metallurgical coals in the future. Most coals from the other seams contained more than 2 percent sulfur, which would limit their use as metallurgical coals.

Jan 1, 1968

By Jerry L. Huiatt

An accurate and reproducible procedure was developed using the gas-liquid chromatograph to quantitatively measure oleic acid on flotation products and in flotation water phases. The method comprised extraction of the oleic acid from the mineral surfaces with alcoholic NaOH, esterification of the extracted oleate, and chromatography of the methyl ester with an internal standard. Quantitative analysis of oleic acid on flotation products from test tube and bench-scale flotation tests with pure minerals and with natural ores proved the applicability of the method on a variety of minerals. The accountability of oleic acid added was 100 percent, ±5 percent.

Jan 1, 1968

By A. F. Colombo

Bench-scale research was undertaken to determine if adding ammonia to cyanide leaching solutions would enhance the extraction of copper from an argillaceous Michigan copper ore. Two leaching techniques, (1) rolling using a tumbling bottle and (2) aerating using a modified Buchner funnel, and variations in pulp temperature; were employed in evaluating the effect of ammonia concentration on copper extraction. Under these experimental conditions, the extraction of copper was shown to be independent of ammonia concentration and entirely dependent on cyanide concentration.

Jan 1, 1968

By E. L. Litchfield

The electrification of ammonium nitrate-fuel oil (AN-FO) blasting agents by pneumatic loaders is described and discussed. The consequences of the electrification are considered in light of the initiation requirements of electric blasting caps. It is recommended (1) that semiconductive loading tubing be utilized and (2) that the resistivity of the AN-FO be controlled; it is further recommended that the operator (3) test to assure continuity of the electric detonator legwire-bridgewire-legwire circuit prior to insertion of the cap into charge or borehole, (4) keep the legwires shunted but not otherwise connected to ground during loading of the blasting agent into the borehole, (5) assure that the borehole is discharged prior to hooking up the detonator leads, (6) assure that he is himself discharged prior to handling the detonator leads, and (7) assure that the blasting cap leads are never carried to the AN-FO loader. The basis and significance of these recommendations are explained.

Jan 1, 1968

By Philip C. Good

Red mud residue from Bayer process treatment of Jamaican bauxite was dewatered in batch and in continuous centrifuges. Solids content of the residue was increased from its original value of 20 to 25 percent to about 40 percent by centrifuging. Clear effluent amounting to approximately 40 percent of the slurry liquid was recovered containing dissolved alumina and soda values for potential recycle to the alumina plant" Addition of a chemical flocculant to the centrifuge increased capacity by about 35 percent. Manufacturer's estimate of large-scale equipment requirements, based on data collected in this investigation, was that a proposed installation for dewatering 16,000 tons per day of Jamaican red mud would require twenty-two 24-by 60-inch solid-bowl-type centrifuges. Cost analysis of a proposed installation, based on a Jamaican red mud tonnage of 16,000 per day, is included also.

Jan 1, 1968

By Manuel Gomez

Bituminous coals having maximum fluidity values in the 40- to 25,400-dial-divisions-per-minute (ddpm) range were carbonized in a continuous, entrained-bed reactor. Carbonization was conducted in an 8-inch diameter, vertical reactor at temperatures from 955° to 1,345° F and at air-to-coal ratios ranging from 4.63 to 16.12 scf/lb of moisture-and ash-free coal charged. Carbonization rates from about 118 to 360 lb/hr, as-carbonized basis, were examined. It was demonstrated that carbonization temperature and air-to-coal ratio must exceed minimum values for continuous operation. Within the operating conditions discussed, highly fluid bituminous coal was carbonized to produce tar and nonagglomerated char. The yield of tar ranged from 21.3 to 38.9 gallons per ton and the char yield ranged from 1,109 to 1,563 pounds per ton, all units expressed on a moisture-and ash-free basis. It was demonstrated that the maximum fluidity and the average size of the coal along with the air-to-coal ratio and the carbonization temperature act together to influence the carbonization product yields and certain properties of the products. Prediction equations were developed from the data for product yields and selected properties of the char, tar, and gas.

Jan 1, 1968

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 C. M. Mason

A method for evaluating the relative incendivity of detonating cord in natural gas-air mixtures was developed. The method consisted of firing short lengths of cord in bundles to determine the number of strands per bundle which would ignite natural gas-air mixtures 50 percent of the time in the 45-cubic-foot gallery of the Bureau of Mines. The relative efficiency of a flame quenching agent, potassium acid tartrate (KHT), when incorporated in both the pentaerythritol tetranitrate (PETN) core and the polyethylene sheath, was explored. The effects of sheath thickness, sheath composition, core weight, and core composition were evaluated. The bundle method established a quantitative scale for evaluating the relative incendivity of cords. The relative incendivity determined by the bundle method was then compared with the incendivity of 100-foot lengths of detonating cord when initiated in 8 percent natural gas in the 640-cubic-foot gallery of the Bureau of Mines.

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 H. A. Tucker

This Bureau of Mines investigation was conducted to determine the appropriate quantities of rare-earth methals (REM) in the form of silicides to add to an alloy steel for the purpose of increasing toughness and ductility. The work was conducted in a vacuum induction furnace with the rare-earth additions required to deoxidize and desulfurize a simulated basic oxygen furnace (BOF) vacuum-degassed steel initially containing 0.013 to 0.016 percent sulfur. The product proved to be as good or better than the best basic electric furnace steel of the same composition made by the steel industry. Twenty-three experimental heats of 5 Ni-Cr-Mo-V steel were made, cast into 50-1b ingots, and hot-worked in a press and a rolling mill to ½ inch plates which were then heat-treated to 130/150 ksi4 yield strength. Impact and tension tests showed that the addition of 0.025 to 0.100 percent, or ½ to 2 lb per ton, respectively, of rare-earth metals when compounded with silicon were appropriate for increasing toughness and ductility. These quantities resulted in retained cerium contents between 0.014 to 0.025 percent, and increased the Charpy V-notch energy absorption and the percent reduction of area significantly as compared with base heats at the same sulfur content levels. All the test heats, including those with additions of REH of as much as 4 lb/ton, had greater Charpy V-notch energy absorption values than the base composition could have developed at the starting sulfur range of 0.013-0.016 wt pct.

Jan 1, 1968

By Frank G. Horino

The Bureau of Mines studied the uniaxial compressive strength of model rock pillars as a function of the angle and spacing of noncohesive planes of weakness. The model pillars were prepared from NX 2-l/8-inch diameter drill core of limestone, sandstone, and granite, and the planes of weakness were diamond saw cuts ground flat and smooth. The angle of the planes of weakness, measured from the horizontal, varied from zero to 57° in approximately 15° increments. When two planes of weakness were used, the thickness-to-diameter ratio of the wafer was 1/4, 1/2, and 1, Approximately 400 model pillars were tested in uniaxial compression. The results indicate that the uniaxial compressive strength of model pillars decreases rapidly as the angle of the plane of weakness increases from 30° to 57°, and that the spacing of these planes of weakness has only a minor effect on the strength. The effect of the number of horizontal planes of weakness, with a spacing of 1/4 and 1/2 of the diameter, upon the compressive strength of model pillars was also investigated. These results indicate that as the number of planes of weakness increases the compressive strength of the pillar decreases. Normalizing the data provides useful estimates of model pillar strengths for any rock type.

Jan 1, 1968

By John J. Henn

An evaluation is presented for an ammonium sulfate leaching process designed to extract manganese from Cuyuna, Minn., and Aroostook, Maine, deposits. In this process the manganese and iron in the ore are reduced to MnO and Fe 3 0 4 in a shaft furnace; the reduced ore is then leached with ammonium sulfate solution forming soluble manganous sulfate while leaving most of the iron undissolved. After filtration, the manganese and some impurities are precipitated from solution as carbonates which are then pelletized and calcined to form a product composed mainly of Mn3O4. The plants are designed to produce 100 tons per day of manganese contained in a product that is suitable for the production of ferromanganese. A byproduct credit, together with the extra processing cost, is included for the Cuyuna ore processing plants because Fe2O3 may be recovered for use in blast furnaces. The estimated operating costs per ton of manganese, excluding income taxes and return on investment, are: [ ] The process with or without byproduct recovery, when treating Cuyuna or Aroostook ores, is not economically competitive with ores available at $71.43 per ton of contained manganese.

Jan 1, 1968

By Everett A. Sondreal

Data are presented on the characteristics of lignites with emphasis on the composition and fusion properties of the ash. Differences in the analyses of commercial-grade lignites are related primarily to variations in moisture and ash contents. Lignite ash is generally characterized by high concentra¬tions of alkaline earth oxides and a greater tendency for retention of sulfur in the ash than higher-rank coals. Composition of ash varies significantly within and between mines. The differences within mines are significant for short distances and may be eliminated under certain circumstances by normal mixing occurring during mining. The sulfur in lignite averages 0.6 percent and is found primarily in the organic or pyritic forms with only a trace of the sulfate. During the stan¬dard laboratory asking procedures, from 60 to 100 percent of the original sul¬fur is retained in the lignite ash. Trace elements, such as uranium and germanium, in the ash from commercial¬-grade lignites are present in low concentrations, but others, primarily copper and silver, are present in specific samples in concentrations approaching those found in some commercial ores.

Jan 1, 1968