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By E. Morrice

Techniques developed by the Bureau of Mines for the preparation of high-purity rare-earth metals and their alloys by electrolysis of the oxides in fluoride media are summarized. Cerium, lanthanum, neodymium, praseodymium, dysprosium, gadolinium, and yttrium metals, the mixture didymium, and specific alloys of these metals and samarium with iron, nickel, chromium, and cobalt were prepared. Individual metals were electrodeposited in the liquid state on tungsten or molybdenum cathodes. Alloys were prepared by electrodepositing the rare-earth metal on a consumable cathode, at a temperature above the melting point of the eutectic formed between the rare-earth element and the cathode material. Cells were designed for electrowinning metal products in gram and pound quantities, and methods for continuous electrowinning of cerium and lanthanum were developed.

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 J. G. Donaldson

The Bureau of Mines investigated the formation of boron and boron-carbide coatings by vapor-phase reactions. Optimum parameters were determined for hydrogen reduction of boron trichloride and for the fonnation of boron-carbide coatings on graphite by reaction with the depositing boron. At 1,300° C, about 85 percent of the boron was deposited. Tungsten substrates did not react with the boron deposit; other substrates reacted to various extents. The hydrogen reduction of boron tribromide was briefly investigated. Boron carbide was deposited at 1,300° C by adding methane to the boron trichloride-hydrogen feed gas. The chemical composition of the vapor-deposited boron carbide approximated B4C. A method of etching B4C was developed to study its microstructure. When boron was deposited on graphite at 1,500° C, very hard, uniform, strongly adherent coatings of B4C were formed that might be useful in rocket nozzle applications.

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 A. W. Henderson

Methods for converting WOCl4 to WCle were investigated in small-scale, laboratory apparatus to devise a method for preparing pure WCls suitable for conversion to tungsten metal. Chlorine, COCI2, and CCI4, alone and in combination with various forms of carbon, were tested as chlorinating agents at various temperatures. More than 95 percent conversion of WOCl4 to WCls was achieved with all reagents at 8000 C in the presence of activated carbon. Only CCl4 maintained its effectiveness in the absence of carbon at 800° C. The effectiveness of carbon was found to be related directly to its surface area.

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 J. Hudy

The performance of six dense-medium washers was evaluated in five preparation plants. Three of the plants were making a two-product separation that produced a clean coal and a refuse; one plant employed dense-medium vessels in series to effect a primary and a secondary separation; and one plant was equipped with a two-compartment washer effecting two separations in one vessel. The separate secondary drum-type washer produced a low-ash metallurgical coal and an intermediate-ash product suitable for plant fuel or steam generation. The two-compartment washer produced a premium anthracite product and a middlings product. The sharpness-of-separation values ranged from good to excellent for the five primary separations and for the secondary separation.

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 J. W. Eckerd

Metal production rates of 42 to 45 tons per day were obtained with hollow-core anthracite briquets in an experimental blast furnace. Tuyere pressures were about the same for both coke and briquet operations, but from 150 to 175 pounds more of briquets were required per ton of metal than were needed with coke. Furnace operations were comparatively smooth, furnace hanging occurring less often than in previous tests with anthracite briquets. Dust production was substantially higher than with coke, however, and metal quality could not be controlled by corrective burdening and moisture control.

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

By Ralph B. Adair

The Bureau of Mines conducted laboratory and small-scale, continuous tests of weathered mica-pegmatite ores from Randolph County, Ala., to determine the feasibility of recovering commercial-grade mica concentrates by flotation. Two flotation methods were used in continuous tests for recovery of mica. One method utilized acid-cationic flotation for the recovery of coarse mica and alkaline-anionic-cationic flotation for recovering fine mica. This method yielded mica concentrates containing 98.6 percent mica with a recovery of 85.9 percent. The other method was based on the Bureau-developed alkaline-anionic-cationic method, and yielded concentrates containing 97.5 percent mica with a recovery of over 90 percent. In both methods, preconcentration of the ground ore on a Humphreys spiral was employed to reject over half of the feed in a product virtually free of mica.

Jan 1, 1968

By J. J. Demeter

Anthracite from the four producing regions in Pennsylvania was both ashed in the laboratory and burned on a chain-grate stoker to determine the sulfur-retention properties of its ash. The retention of sulfur in laboratory-prepared anthracite ash was shown to be related to ashing temperature and to the amounts of sulfur and calcium present in the coal. At the usual laboratory ashing temperature of 750° C sulfur retention ranged from 0.8 to 13.2 percent of the total coal sulfur. Sulfur retention in the ash was negligible, o to 0.3 percent, at 1,200° C, which is the thermal decomposition temperature of calcium sulfate; thus calcium sulfate does not form and cannot serve as a sulfur-retaining agent. In several tests the anthracite was mixed with 6 or 10 percent dolomite prior to firing in the chain-grate stoker. The dolomite did not improve sulfur retention owing to the high temperature in the fuel bed. Sulfur retention was, however, related to the unburned carbon in the ash. The relationship of the percentage of original coal sulfur retained in the ash (Y) to the percentage of the original carbon in the coal remaining in the ash (X) is expressed by Y = -0.579 + 0.914X. The percentage of sulfur retained is almost directly proportionate to the percentage of original coal carbon in the ash.

Jan 1, 1968

By Kenneth H. Johnston

Information and data necessary for research on improving methods of oil recovery from low-permeability reservoirs and for comparison and evaluation of performance of such reservoirs with those producing from more permeable sands were obtained. Core analyses, well logs, production tests, well stimulation techniques, primary and secondary production records, and data on two water-flood projects were examined for wells producing from the Bartlesville sand, West Avant field, Osage County, Okla. Overall recovery from the study area was generally poor with only 9.0 percent of the pore volume recovered to January 1, 1968. Larger fracture treatments (8,000 to 12,000 gal) could have resulted in an increase in primary oil recovery. Secondary recovery by water-flooding accounted for only 1.9 percent of the pore volume because of the inability to control the large volume of injection fluid that escaped from the flood patterns and the excessive volumes of water produced with the oil. Future waterflood development in other low-permeability reservoirs should include the drilling of new input wells, use of injectivity surveys to locate possible natural fracture systems, or zones of high permeability, and control of injection fluids by altering flood patterns and/or plugging of the more permeable zones.

Jan 1, 1968

By H. G. Iverson

An investigation was conducted on the conditions affecting the precipitation of aluminum by autoclaving synthetic solutions containing Na2SO4, Al2(SO4)3, H2SO4, and H2O. Virtually all of the alumina could be precipitated as natroalunite (NaAl3(SO4)2 (OH)6). This product could be readily filtered and dried. Results are reported in terms of alumina precipitated in this compound and not in terms of alumina itself. Solutions of ~ 0.30, ~ 0.60, and ~ 0.80 mole/liter A1203 and various concentrations of H2SO4 and Na2S04 were investigated. The optimum time and temperature for autoclaving were 20 to 30 minutes at 200° C. The highest yields of natroalunite were obtained from solutions containing little H2SO4 and ~ 2 moles Na2SO4 per mole A1202. Acid in quantities of 0.3 to 0.5 mole/mole of alumina in solution depressed the yield to 90 percent or less. In differential thermal analysis, at 1,000° C the natroalunite precipitate decomposed without melting to yield SO, and SO2 gases, a solid composed of Na2SO4, and gamma and alpha Al203. Continued heating to 1,200° C produced No SO, and alpha A1303. Water-leaching of this product removed the Na2S04 and left a final residue of alpha A1203.

Jan 1, 1968

By John B. Shutack

In an effort to improve the performance of the explosive-anchored rock bolt, the Bureau of Mines studied the effect of the detonation velocity of the explosive and type of charge (linear or nonlinear) on the fracturing tendency of the anchor tube. Also, different types of tubing were compared to determine the one most suitable for use as an anchor tube. The Bruceton up-and-down method was applied in tests in which steel shooting blocks having boreholes ranging from 1-3/8 to 2-1/8 inches in diameter were used. Of the four types of tubing evaluated, a welded A-178 tubing that was drawn over a mandrel and renormalized gave the most promising results. The A-179 seamless tubing that is normally used with the explosive bolt was the most inferior. Both types, however, gave significantly better anchorage than the conventional shell when tested in both laboratory and underground experiments. Within the range of velocities studied (5,000 to 7,000 m/sec), the type of explosive showed no significant effect on anchor-tube performance. In general; linear explosive charges provided better anchorage than nonlinear charges.

Jan 1, 1968

By R. E. Thill

The ultrasonic pulse measurement system described measures velocities of longitudinal (compressional) and shear waves in rock to give values that can be used with density values to determine the dynamic elastic constants of rock. A special feature of this pulse measurement system is its unique acoustical bench that minimizes errors in pulse transit times that are commonly associated with coupling, sample alinement, and sample orientation. Some special features of the acoustical bench are its highly versatile transducer cartridges, a pneumatic ram coupling device, an orientation mechanism, and a vacuum chuck sample holder. The lathe-bed-like construction of the acoustical bench assures automatic alinement of samples and versatility in accommodating samples of various shapes and sizes.

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