Search Documents

By Robert K. Koch, Henry E. Blake

Laboratory tests were made to determine if aluminum fluoride of commercial grade could be synthesized by reacting alumina hydrate with dilute ( 25 to 75 grams per liter of fluorine ) aqueous fluoride solutions . • Products containing up to 90 percent aluminum fluoride ( A1F ) were synthesized by reaction of alumina trihydrate ( A120 3H2O) with either dilute hydrofluoric acid ( HF ) or ammonium fluoride ( NHF) solutions , the ammonium fluoride solution resulting from ammonia ( NH ) desilication of a hydrofluoricfluosilicic acid ( HF - H₂ SiF ) solution . Fluorine recoveries of over 80 percent were obtained with either type of solution . The hydrated precipitates of AlF, and ( NH4 ) , A1F ( ammonium aluminum fluoride ) obtained by reacting hydrated alumina with these solutions were subsequently converted to anhydrous AlF, by controlled heating .

Jan 1, 1964

By G. W. Birge, D. E. Wolfson, J. H. Lynch

Fourteen coal samples representing the Flag , Fire Clay , Whitesburg , Amburgy , Upper Elkhorn No. 3 , Upper Elkhorn No. 2 , Upper Elkhorn No. 1 , and Lower Elkhorn beds in Letcher County , Ky . , were carbonized by the Bureau of Mines - American Gas Association ( BM- AGA ) method , and yields of products and physical properties of cokes were determined . The samples tested were high- volatile A bituminous in rank , with dry , mineral - matter- free fixed - carbon contents ranging from 55.3 to 62.2 percent . Five of the samples , as received , were chemically unsuitable for metallurgical use because of excessive ash and/ or sulfur content . Generally , strength indexes of the cokes were low and all of the coals would require blending with higher rank coal to obtain satisfactory blast furnace fuel .

Jan 1, 1964

By Henry M. Harris, Hal J. Kelly

Electrical dewatering tests are described in which the laboratory cells were designed for continuous operation using an endless metal belt as the anode . The test slurries were dilute , containing from 2.5 to 14.4 percent solids (specific gravity of 1.02 to 1.10 ) that were all minus 8 microns in size . Recovery of the solids of low water content was the practical objective of the investigation . Process variables evaluated and reported are : The effect of feed rate , amount of electrolyte , samples from different sources , and the use of two cells in series . These variables are evaluated on the basis of yield of clay per kilowatt - hour , recovery , and the amount of solids in the deposited clay . Recovery , yield , and solid content of the belt anode product are interdependent , and changes that will improve one of these characteristics often are accomplished at the expense of the others . Tests in which recoveries range from 50 to 60 percent usually result in yields of 8 to 9 kilograms (kg ) of dry clay per kilowatt- hour (kwhr ) . Under these conditions , the solid content of the deposited clay approximates 50 percent . One test sample , composed of kaolinite , showed very high yield , 13 to 16 kg per kwhr ; high recovery , 53 to 58 percent ; and 52 to 54 percent solids in the cake .

Jan 1, 1964

By F. E. Joyce, Charles Prasky

This report describes the response to high- temperature sulfatization of a variety of manganese minerals and companion compounds which may occur either as a principal component or as a gangue material in low- grade manganese deposits . Fourteen manganese samples representing oxide , carbonate , and silicate minerals as well as seven compounds which might occur as gangue with manganese minerals were tested batchwise in a bench- scale apparatus under conditions which would be favorable for the sulfatization of manganese . The manganese minerals substantiated thermodynamic predictions and responded to sulfatization but to varying degrees . The gangue materials , MgO , MgCO,, CaO , and CaCO3 , were sulfatized readily in contrast to the iron oxides and the aluminacontaining material which were not .

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 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 T. A. Henrie, E. K. Kleespies

Electrolytic studies were conducted to determine the transfer rates of the alloying constituents from molten titanium anodes to solid titanium cathodes in molten salt systems . The metals , nickel , tin , copper , bismuth , and manganese , were selected on the basis of thermodynamic data and the melting point of the alloy system . The transfer of nickel , tin , and bismuth was very low . The content of these elements in the cathode was in the range of less than 0.01 to 0.001 percent . The copper transfer was 0.6 to 0.8 weight - percent in electrolytes containing titanium chlorides and 0.12 weight - percent in titanium fluoride salt systems . The manganese transferred at rates comparable to that of titanium . Highpurity titanium and titanium- manganese alloys of uniform composition were produced by electrorefining molten titanium alloys in chloride electrolytes . Comparisons are made between the calculated and the actual quantities of metal transfer .

Jan 1, 1964

By T. E. Green, E. F. Spano, W. J. Campbell

A combined ion exchange X- ray spectrographic method was evaluated for the determination of 11 metallic elements in high - purity tungsten : Aluminum , calcium , chromium , cobalt , copper , iron , magnesium , manganese , nickel , titanium , and zinc . Copper , nickel , and manganese in the 5- to 100 - microgram range ( 1 to 20 parts per million based on 5 - gram samples of tungsten ) , calcium in the 10- to 100 - microgram range , and cobalt in the 5- to 20 - microgram range can be determined within an accuracy of ± 10 percent of the amount present . Limits of detection of these elements are 0.05 to 0.14 microgram . The overall method was unsatisfactory for the determination of aluminum , chromium , iron , magnesium , titanium and zinc in tungsten .

Jan 1, 1964

By A. G. Starliper, H. Kenworthy

A procedure was developed for the separation of lead and sulfur in industrial concentrates of galena by a combination of chlorination and fused - salt electrolysis . Galena could not be satisfactorily electrolyzed in the various media tried ; however , when it was treated with chlorine the resulting lead chloride could be effectively separated electrically into lead and chlorine . An apparatus was designed and constructed to chlorinate galena and to volatilize simultaneously most of the chloridized impurities . By electrolyzing the chlorinated concentrate , a high percentage of lead was recovered . Anodic chlorine was drawn from the cell and was used to chlorinate new feed . In many runs , the recovered metal analyzed from 99.8 to 99.9 percent lead . Lead was also distributed as a chloride in the bath , and a small portion was in the volatile fraction produced during the chlorination step . During a tinuous operation , only 0.1 percent of the total lead was discarded ; 99.9 percent was accounted for in the metal , electrolytic bath , and washed or leached chlorination condensate which was essentially lead chloride . About 95 percent of the sulfur from the galena was recovered as a byproduct of over 90 - percent grade .

Jan 1, 1964

By T. A. Henrie, D. C. Fleck, D. G. Kesterke

Uranium metal was electrowon from uranium dioxide dissolved in fluoride melts . The UO₂ was fed directly to the cell in a continuous manner . Electrolysis was performed at 1 , 200 ° to 1,300 ° C in electrolytes composed of UF4 , LiF , and BaFa . A single regulus of metal was collected in a confined area of the crucible . Product purity of 99.8 percent was attained . Carbon was the major contaminant . Compartmented cells were studied as a means of confining the oxide feed to the vicinity of the anodes .

Jan 1, 1964

By F. E. Block, T. T. Campbell, D. Z. Hobbs

Several methods were investigated for the preparation of high- purity elemental boron in an attempt to develop a feasible process for producing boron on a large scale . In the work described in this report , the metal was prepared by metering boron trichloride gas into a crucible containing molten metal reductants . It was necessary to remove reaction byproducts by acid and aqueous leaching . Magnesium and sodium were tested as reductants , but best results were achieved using lithium or zinc as reductants . Contaminants originating from the materials of construction were the chief impurities in boron made by this method . Impurities ranged from 0.5 to 5.0 percent . Impure boron ( 85 to 90 percent ) was also prepared by the magnesium reduction of boron trioxide in a thermite - type reaction . This product contained magnesium as the chief contaminant . Impure boron made in this way could be upgraded by fusing with potassium fluoborate or potassium acid fluoride . After acid leaching the fusion cake , a product containing 95 to 97 percent boron was obtained . Analytical techniques for accurate determination of impurities in elemental boron are a major problem , requiring solution before a valid comparison can be made of the quality of boron prepared by these various methods .

Jan 1, 1964

By R. A. Beall, S. L. Ausmus

The development of a completely water - free expendable graphite mold material , useful for reactive metal castings , has been detailed . Mixing and curing variables have been evaluated both by physical testing of the material itself and by castings of titanium , zirconium , and hafnium . The blend of powdered graphite , cornstarch , dextrin , cereal binder , linseed oil , and Carbowax -4000 is a successful mix when mulled in a carbon dioxide atmosphere , and properly cured and fired . The primary advantage of this material is its adaptability to standard foundry techniques ; i . e . , core blowing and hand ramming . Temperatures in the curing and firing cycles do not exceed 960 ° C , and no vacuum firing is required .

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 R. D. Groves

Laboratory research has demonstrated that high - grade copper powders can be produced under controlled conditions from cement copper products . The technique should enable small producers to prepare a directly marketable product by means other than smelting and electrolytic purification . A continuous drum- type precipitator was the preferred unit for producing fine - sized particles of cement copper that were further processed by chemical digestion in a copper sulfate solution , by reduction and sintering in a hydrogen atmosphere , and by grinding to a powder . The effects of variables related to all stages of the process were investigated . Treatment of leach solutions from three different sources resulted in copper powders containing 99.2 to 99.8 pct Cu , apparent densities of 1.97 to 2.25 grams per cu cm , good powder flow rates , and a size distribution of 54.9 to 60.1 pct minus 325 - mesh material .

Jan 1, 1964

By W. D. Ludemann, E. A. Loria, E. A. Rowe

The isothermal recrystallization of electrorefined vanadium has been studied as a function of annealing time , temperature , and prior deformation . Specimens were cold- rolled from 30- to 75 - percent reduction in thickness , then annealed from 700 ° to 1,200 ° C at time periods ranging from 1 minute to 96 hours . The course of recrystallization was followed by means of hardness , metallographic , and X- ray techniques , and a recrystallization diagram was constructed . Interpretation of the data indicated that there was around 50- percent softening due to recovery ( first stage of softening) before recrystallization began . The defining of recrystallization limits with respect to the amount of deformation was precisely established for electrorefined vanadium . More than 30- percent reduction was necessary for recrystallization to occur at 850 ° C. With 60- percent reduction , it was initiated at 750 ° C and completed at 950° C. The activation energy for recrystallization , as derived from the data , was 95,300 cal per mole for 60 - percent reduction and annealing at 750 ° to 900 ° C. Recrystallization by the mechanism of nucleation and growth was the principal process during the second stage of softening . minor part of the second stage of softening took place as strain- induced boundary migration , which was observed in specimens reduced 30 percent , bent in L- shape , and annealed at 950 ° C. Grain size decreased significantly only with the largest reductions and annealing between 750 ° and 950 ° C. Grain growth was expressed by the empirical relation D = KKtt"" ,, the exponent being the same at 60- percent reduction and annealing from 750 ° to 900 ° C. Accordingly , the activation energy for grain growth was 75,000 cal per mole .

Jan 1, 1964

By K. K. Kelley, L. B. Pankratz, W. W. Weller

The heat capacity of columbium (niobium) carbide (CbC ) was measured over the temperature range from 51 ° to 298 ° K, and the entropy at 298.15° K was evaluated . Also , the heat content above 298.15 ° K of columbium carbide was measured to 1,800 ° K. The results were combined with the known heat of formation at 298.15 ° K to obtain values of the heat and free energy of formation over the temperature range from 298.15 ° K to 2,000 ° K.

Jan 1, 1964

By Green A. D M

The establishment of the Imperial Smelting Furnace at Sulphide Coporation Pty. Limited for the smelting of zinc and lead made it necessary to design and install sintering capacity to produce approximately 500 t.p.d. of zinc-lead sinter. The updraught sintering process installed is a recent development and the plant was designed with adequate flexibility and equipment to enable operating staff to investigate the process and achieve maximum production under optimum operating conditions.Sulphur dioxide gases from the sinter machine are passed to a contact acid plant for the manufacture of sulphuric acid.

Jan 1, 1964

By Donald W. Mitchell, John Nagy

Observations made on coking of coal, deposition of soot, dust transport, flame, violence, and related phenomena following experimental coal-dust explosions are summarized. Data are given on gas explosion pressure, flame length, flame velocity, and variation of these parameters with concentration. Conclusions from these observations are useful in preventing similar occurrences in operating mines and serve as a guide in improving safety.

Dec 1, 1963

By W. E. Lamont, R. E. Perry, I. L. Feld

The Bureau of Mines conducted research to determine the conditions required to sinter a pyrrhotite calcine into a product suitable for iron blast furnace feed . The calcine , a fine - grained iron oxide produced by roasting sulfide flotation concentrate , analyzed about 60 percent iron and 1 percent sulfur . Sintering of the calcine without prior pelletization was not successful whereas firing of preformed calcine charges yielded acceptable sinter products . Batch tests were made to study the effect of the following variables on the sinter quality : Size of green pellets in the charge , quantity and type of internal carbonaceous fuel used , depth of sinter bed , moisture content of the charge , flux additions , and binder additions . The batch and continuous sinter tests showed that minus 1 / 4 - inch pellets prepared from a mixture of the calcine , coke , dolomite , and water gave sinter cakes analyzing 57 to 61 percent iron and 0.05 to 0.02 percent sulfur .

Dec 1, 1963

The old De Beers mine, which lies northwest of Dutoitspan mine at Kimberley, was the mine which launched Cecil Rhodes (In his historical career. It was the nucleus of the De Beers Mining Co. Ltd., formed in 1880, which later became De Beers Consolidated Mines Ltd. Inactive for more than a half century, the De Beers Mine is being rejuvenated for a new era of operations. Both mines were on the Vooruitzicht farm owned by the De Beers brothers, who had bought it from the Orange Free State Government ten years previously for £50. Although the brothers sold it soon after the discovery of diamonds at Dutoitspan, they are remembered for having given their name to the foremost diamond mining company in the world. Diamonds worth nearly R180,000,000 have come from this ground, and more will be recovered when the mine is re-opened.

Jan 9, 1963