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By J. L. Hoffman, F. W. Wood, R. A. Beall, W. E. Anable

For melting and purifying reactive and refractory metals , two electronbeam furnaces have been constructed and operated on the principle of highpowered vacuum diodes . It was necessary to design the vacuum and electrical systems , mechanical features , and operating procedures to cope with dynamic conditions . Vacuums of 10-5 torr , tens of kilowatts of power at 5 to 10 kilovolts , and the evolution of impurities at thousands of liters per minute constitute a challenging combination . The furnaces have been used to melt either button specimens weighing several hundred grams or , by feeding material as a consumable electrode , small ingots weighing several kilograms . Hafnium is among the metals that can be purified . For example , hafnium starting material with Rhn 94B was softened to Rhn 70B after 2 hours of melting under a 25 - kw electron beam , and impurity levels were reduced as follows : Oxygen , from 700 to 350 ppm ; nitrogen , from 71 to 20 ppm ; hydrogen , from 6 to 1 ppm ; aluminum from 75 to < 20 ppm ; chromium , from 80 to < 10 ppm ; iron , from 100 to 40 ppm ; and silicon , from 40 to < 20 ppm .

Jan 1, 1963

By Albert W. Deurbrouck

This report describes the preparation characteristics of the significant coalbeds in Russell County , Va . Almost 2 million tons of coal was mined in 1961 ; 75 percent of the coal was cleaned mechanically in preparation plants in the county . The coal of Russell County is ranked as medium- to high- volatile bituminous , contains small amounts of sulfur , and generally requires some cleaning to reduce the ash content to limits acceptable for metallurgical purposes .

Jan 1, 1963

By H. A. Dierks, H. B. Link

The purpose of this investigation was to develop a practical feeder apparatus to introduce comparatively large pieces of coal and similar material into a pipeline under pressure in connection with the vertical hydraulic transportation of solids , termed " hydraulic hoisting . " This method of hoisting the precrushed run - of - mine product of an underground mine has been given unusually wide attention abroad and could be of considerable significance to the U.S. mining industry in its search for operating improvements and cost reduction . A lock-hopper assembly was developed after a series of sinking velocity tests were made by dropping anthracite in a column of water . The system functioned reliably as an automatically operated feeder apparatus .

Jan 1, 1964

By A. F. Colombo, D. W. Frommer

Bench- scale tests were made to determine the applicability of flotation as a means of upgrading finished and semifinished magnetic concentrates prepared from reductively roasted iron ores . Both anionic and cationic flotation methods were used to remove siliceous gangue from the magnetic concentrates and produce upgraded products . Seven magnetic concentrates , containing from 6.7 to 13.7 percent SiO2 , were improved by the flotation treatment , yielding final concentrates containing less than 6.0 percent Si02 . Cationic flotation methods were studied on four of the seven samples ; of this group only one sample yielded better results by cationic flotation than by the anionic method .

Jan 1, 1964

By J. C. Meeks, C. L. Klingman

An instrument that is sensitive , portable , safe , and low in cost was developed by the Bureau of Mines for detecting helium leaks by comparing the thermal conductivity and flow rate of the atmosphere around the suspected leak against a reference of helium- free air . A vacuum pump pulls the sample gas through a restriction and over thermistor elements , the combined electrical output of which is affected by thermal conductivity and flow rate of the sample gas . Tests showed that the battery - operated Helium Leak Detector was effective and rugged instrument that could be operated safely in explosive atmospheres . The instrument could also detect , but not identify , other gases such as methane , hydrogen , argon , carbon dioxide , and Freon 12 .

Jan 1, 1964

By T. A. Henrie, J. D. Marchant, E. S. Shedd

Cerium metal was electrowon in a fluoride bath from cerous oxide and tapped from the cell during prolonged operation . Electrolyte constituents were CeF , BaF₂ , and LiF. Twenty- seven pounds of metal of 99.8 percent purity were produced at a rate of 3 pounds per hour and tapped from the cell . Principal impurities were molybdenum , aluminum , oxygen , and carbon . The operating parameters , such as electrode geometry , bath compositions , and oxide feed rate , were investigated . Anode reactions were found to be important factors in cell operation . Stable cerous oxide reacted more uniformly at the anode surface than ceric oxide . Electrowinning was conducted in crucible hearths consisting of both frozen electrolyte and molybdenum metal . Both materials proved satisfactory and did not react with the molten cerium . Stable cerous oxide was prepared by carbothermic reduction and used as a feed material . Cell design proved to be an important factor in continuous cell operation . Complementary to the investigations of electrowinning of cerium , the metal was purified by electrorefining in a chloride electrolyte .

Jan 1, 1964

By Dean C. Holt

This work was done to appraise the potential of titanium minerals in known titanium- bearing placer deposits and potential titanium- bearing placer areas in western Montana . Reconnaissance studies were made of more than 225 stream areas . Churn drilling and other placer exploration techniques were used in sampling eight deposits . The sampling results indicate that areas containing more than 10 pounds of ilmenite and other titanium- bearing black - sand minerals per cubic yard occur in the Bitterroot , Upper Clark Fork , and Jefferson River drainages . The chief source for the constituents of the black sands appears to be the Idaho batholith , and the highest black - sand concentrations are generally found near the source . Sample testing methods include gravity and magnetic separation and visual microscopic as well as chemical and radiometric analyses on deposits sampled in detail .

Jan 1, 1964

By Theodore L. Turner, Joseph H. Swift

A study on a small laboratory scale was made of the use of ammoniacalammonium carbonate for batch leaching Mn from low- grade manganiferous materials ( 6 to 16 pct Mn) obtained from deposits in the southern district of Aroostook County , Maine . These materials were partially reduced at 500 ° to 700 ° C with H₂ or CO and then leached with solutions of NH and CO₂ dissolved in water . Extraction of 80 to 90 pct of the Mn was obtained from some sample materials , but 10 to 34 pct of the iron was also extracted . Material from the Littleton Ridge deposit contained manganese intimately associated with Fe , a condition which contributed to difficulties in obtaining a commercially acceptable product . Extensive investigations of the leach and reduction processes with various mixtures of H₂ and water vapor , and CO and CO₂ , failed to disclose a set of conditions for selectively leaching the manganese . Finely divided metallic Fe was probably produced during the reduction steps so that Fe was leached with the Mn in the subsequent extractions .

Jan 1, 1964

By Charles J. Stehlik

This report deals with the changing behavior of mine roof bolt and roof rock as a result of repetitious production blasting . Observations were made in the upper shale production headings at the White Pine Copper Co. room and pillar mine , White Pine , Mich . Roof bolt compression pads and a stratascope were used in the investigations , which were carried out in three separate test sites in which nearly identical procedure produced comparative , repetitive , and anomalous observations . Results indicate roof bolt tension change and roof quality deterioration anomalies were coincident with blasting . The hypothesized cause of the anomalies is a seismic shock generated by the blasts .

Jan 1, 1964

By E. R. Andersen, F. E. Block, T. T. Campbell

This work was done to develop methods for increasing the yields and purity of vanadium prepared by bomb reduction of vanadium compounds . Compounds reduced were V₂ 05 , V203 , VC , and VC13 . Sodium , calcium , and magnesium were used as reductants . Variables considered included reductant form , bomb size , pressure during reaction , method of ignition , and the use of slag fluidizing additives . It was concluded that yields of 85 to 90 percent can be effected by the calcium reduction of V205 in reactors measuring as much as 14 inches in diameter and 60 inches in height . Optimum charge composition included V₂05 , 65 percent excess calcium , and 0.4 moles sulfur per mole vanadium . Purity of the vanadium produced in large reactors varied from 99.5 to 99.8 percent . The higher purity metal , depending upon the amounts of interstitial impurities present , was usually cold ductile . Although high yields of up to 99.5 percent can be effected by bomb reduction of VC1 , the high pressures developed in the bombs and attack of the reactor walls by the byproduct chloride slags discourages this method of preparing vanadium . It was found that significant purification of impure regulus metal occurred when it was hydrided , crushed , acid leached , and vacuum dehydrided . Metal so treated can readily be converted to ductile sheet . A cost estimate based on the production of 100 tons of vanadium per year was prepared . It was concluded that pure ductile vanadium could be produced for approximately $ 20.00 per pound .

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Robert Madden

Experiments were made in a semicontinuous unit to provide engineering data for designing experimental continuous systems . These systems would be used to study the hydrogasification of hvab coal and char (from lowtemperature carbonization ) to high - Btu gas . In experiments at 800 ° C and with a coal residence time of several seconds , yields of hydrocarbon gases increased from about 2,000 scf / ton of maf coal at 250 psig to 7,000 scf at 1,000 psig . With 15 minutes residence time , yields increased from 8,000 scf/ton of maf coal at 250 psig to 17,500 cubic feet at 1,000 psig . In all cases , small quantities of heavy oils were produced along with the gaseous hydrocarbons . Production of oils could be minimized with a corresponding increase in gaseous hydrocarbons by increasing the retention time of the volatiles within the hot zone . Yields of gaseous hydrocarbons from char were slightly greater than from coal under similar conditions . Although the hydrogasification reaction is very pressure dependent , substantial quantities of coal (40 to 60 percent ) could be reacted to gaseous hydrocarbons at pressures as low as 50 psig provided reaction temperatures were increased to 1,200 ° C. It was also demonstrated that a hvab coal could be hydrogasified continuously without incurring agglomeration . This was achieved by dispersing coal in a relatively large reactor with concurrent flow of hydrogen . At 1,000 psig and 800 ° C , it was possible to react about 35 percent of the coal and to produce a gas containing up to 52 percent methane .

Jan 1, 1964

By Richard F. Link, George S. Koch

Through the use of statistical methods, estimates of metal content and tonnage of an ore body made by using data from 18 diamond-drill holes are compared with actual values established with data from 1,829 drift samples. The reliability of the estimates made from the drill holes is assessed in several ways. The relationship of metal content (assay-width product) to grade is explained. It is concluded that useful estimates can be made from 18 drill holes provided that reasonable assumptions are made and certain risks accepted. The ore body investigated is the Don Tomas vein of the Frisco mine, San Francisco del Oro, Chihuahua, Mexico.

Jan 1, 1964

By J. W. Eckerd, W. S. Sanner, P. L. Woolf, R. E. McKeever

The Bureau of Mines experimental blast furnace was operated successfully with anthracite metallurgical briquets . Tuyère pressures were higher and more erratic than for operations using coke , and furnace " hangs " occurred more frequently . Higher hot - blast temperatures were required to maintain the quality of the metal . By using higher hot blast temperatures , the fuel and production rates and slag volumes were comparable to those obtained for all - coke operation . The anthracite metallurgical briquets exhibited excellent mechanical strength and descended through the shaft of the furnace with little breakage or reduction in size .

Jan 1, 1964

By Richard W. Lewis, Lloyd Carpenter

The objective of the investigation was to determine spectrochemically 19 elements in the general range of 0.5 to 1,000 ppm in high - purity hafnium and its compounds . Samples were converted thermally to hafnium dioxide , mixed with buffer - carrier - internal standards , and excited by a dc arc . Spectra were recorded on photographic plates . Transmittance values were recorded densitometrically and converted to relative - intensity ratios . Four groups of standards were used to establish analytical curves from which the concentrations of impurities were obtained . Average precision of the method was 14.2 percent relative standard deviation , and relative error was 4.2 percent .

Jan 1, 1964

By C. H. Schack, K. C. Dean

An investigation was made to devise and evaluate a flexible flotation method for beneficiating typical tactite types of calcareous scheelite - bearing ores ; these scheelite - bearing ores are available in large tonnages in deposits containing 0.2 to 0.3 pct tungsten trioxide . The objective was to achieve a high recovery of the tungsten in concentrates , containing a minimum of 10 pct WO3 , that would be suitable for chemical processing into high- quality synthetic scheelite . The principal problems encountered and resolved by bench- scale flotation tests on ore samples from five different deposits were to define the conditions and reagent combinations essential for ( 1 ) achieving selective flotation of a small amount of scheelite from a large amount of calcite and ( 2 ) controlling the effect of small amounts of calcium , magnesium , and iron salts in the ores and water used . The flotation process was evolved from batch tests and continuous runs in a pilot - scale mill with a capacity of 100 lb per hour . The flotation process comprised ( 1 ) removal of sulfide minerals , ( 2 ) conditioning the residual ore pulp with sodium carbonate , quebracho , and trisodium phosphate , and ( 3 ) rougher flotation and single - stage cleaning of a scheelite concentrate . In a pilot plant run , over 91 pct of the tungsten was recovered from ore containing 0.27 pct WO3 , in a concentrate containing 11.2 pct WO3 .

Jan 1, 1964

By William I. Nissen, Richard Havens

Continuous flotation studies were made at a 50 - lb - per - hr feed rate to confirm the effectiveness of a batch - scale procedure for concentrating phenacite and bertrandite minerals from Mount Wheeler ores that contained , in percent , 0.47 , 0.78 , and 4.7 BeO . The procedure for selective froth flotation of the beryllium minerals from a gangue composed chiefly of calcite , fluorite , and mica comprised closely controlled preconditioning with sodium fluoride and sodium hexametaphosphate in a series of small mechanically agitated tanks and use of a mixture of oleic acid with kerosine , fuel oil , or turpentine as a collector . It was difficult to adapt the laboratory flotation procedure to continuous operation . The principal problem of achieving adequate conditioning to depress calcite and fluorite ultimately was resolved by conditioning in series . Thereafter , three ore samples of different grades treated on a continuous basis yielded concentrates containing from 12 to 25 percent Beo from these relatively complex and difficult ores . Recoveries , on a BeO basis , ranged from 75 to 88 percent . Losses , which primarily were due to incomplete liberation , probably could be lowered in a commercial operation .

Jan 1, 1964

By I. L. Nichols, K. C. Dean, P. H. Johnson

Hydrochloric acid , sulfuric acid , and chloridizing roast- water leaching methods for dissolution of cesium and rubidium from Maine , Canada , and Southern Rhodesia pollucite ores and their flotation products were investigated by small- scale tests . Optimum conditions were determined to be ( 1 ) for hydrochloric acid leaching , use 12.7 equivalents of 8.8 normal acid per equivalent of cesium in the sample and leach for 6 hours at 100 ° C ; ( 2 ) for sulfuric acid leaching , use 12.7 equivalents of 14.4 normal acid and leach for 2 hours at 120° C ; and (3 ) for chloridizing roast - water leaching , roast minus 200 - mesh ore, limestone , and calcium chloride in a ratio of 2 : 4 : 1 , respectively , for 1 hour at 900 ° C , and leach the calcine for 1 hour at 80 ° C with enough water to give 35 pct solids . Extractions of cesium from ores and flotation products containing over 20 pct cesium were in excess of 97 , 93 , and 96 pct for the hydrochloric acid , sulfuric acid , and chloridizing roast - water leach processes , respectively .

Jan 1, 1964

By R. J. Leary, W. M. Mahan, F. X. Tartaron

A new type of apparatus for prerefining molten blast furnace iron and to reduce the cost of subsequent steelmaking consists of a funnel - shaped device lined with firebrick into which a horizontal stream of molten pig iron is directed tangentially at the top . The rotary motion thus induced causes the stream to flatten itself upon the wall and flow in a spiral path to the outlet ; thus , the device was termed " vortex cone .' Oxygen and other refining agents are impinged upon the flowing metal in the cone where reaction is facilitated by the large metal surface exposed and the turbulent flow pattern . Experiments with water in 1 - foot - diameter funnels provided an idealization of the flow patterns to be expected with molten iron . A brick - lined reactor 3 feet in diameter was built for desiliconizing molten pig iron in lots of 1 to 2 tons . At flow rates of 0.3 to 0.5 ton min - 1 (430 to 720 tons per day ) this apparatus was 64- to 90 - pct effective in desiliconization with oxygen efficiencies of 19 to 41 pct . Detailed experiments to develop basic engineering data are underway , and adaptation of this principle to other reactions and reactants is planned .

Jan 1, 1964

By H. R. Babitzke, H. Kato, M. D. Carver

A number of columbium and tantalum alloys were investigated to determine their suitability for use at elevated temperatures . Columbium-vanadium , tantalum-vanadium , and tantalum-hafnium alloys , and also columbium- 10 wt pct titanium alloys modified with additions of 0.1 to 2 mole pct ZrO2 , TiO2 , ZrB₂ , TiB , ZrC, or TiC were prepared and examined . Workability , tensile properties , and oxidation resistance were tested . Of the columbium alloys studied , the columbium- 12 at . pct vanadium exhibited the best properties ; it compared closely with the columbium- 10 at . pct vanadium alloy studied in a previous investigation.

Jan 1, 1964

By H. E. Powell, T. E. Hill, W. A. Calhoun

The object of this investigation was to determine the effectiveness of certain cationic flotation collectors , Ethomeens , in recovering fine particles of lead minerals from mill tailings at a grade equal , at least , to that of the mill feed ( 1.7 percent lead ) . The Ethomeens , derived from tertiary amines having one fatty alkyl group and two polyoxyethylene groups attached to the nitrogen , were evaluated by bench- scale flotation tests . The 14 Ethomeens tested consisted of four groups : Coco amine , soybean amine , tallow amine , and stearyl amine . The best results were obtained with coco amine C / 12 , soybean amine S/ 15 , tallow amine T / 12 , and stearyl amine 18/20 . From a feed containing 0.23 percent lead , rougher concentrate grades of 2.12 to 3.89 percent lead were obtained , with recoveries of 17.3 to 27.5 percent of the total lead . Some of the lead mineral particles recovered had diameters of less than 1 micron . In comparative tests , the Ethomeens , or polyethoxylated amine types of cationic surface active agents , were more selective than conventional xanthate collectors for flotation of slimed lead minerals .

Jan 1, 1964