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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 A. F. Colombo, R. T. Sorensen, D. W. Frommer

The Bureau of Mines developed a flotation method for concentrating spiral tailing produced from pilot plant tests on the Champion mine ore fines . The feed material contained about 49 percent Fe and 15 percent SiO2 and was posed mostly of specular hematite , muscovite , and chlorite . Bench- scale , batch flotation research developed a reagent suite composed of tall oil - fatty acid , fuel oil , sulfuric acid , sodium fluoride , and sodium silicate for recovery of iron minerals in the froth product . Concentrate made with the reagent suite contained 87.3 percent of the iron and analyzed 65.6 percent Fe and 1.9 percent SiO2 . Continuous flotation tests were made with a nominal feed rate of 400 lb /hr , but without middling recirculation . Using nearly the same amount and complement of reagents as in the batch tests , three similar continuous tests gave concentrates averaging 63.9 percent Fe and 3.1 percent Sio while recovering about 86 percent of the iron .

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 Robert H. Merrill, James V. Williamson, David M. Ropchan, George H. Kruse

In- situ rock stresses were determined by flatjack and borehole - deformation methods . Estimates of the stress distribution around a flatjack were obtained by a combination of flatjack and borehole - gage techniques . The investigations were part of a study , conducted jointly by the State of California and the Federal Bureau of Mines , to determine the stress in rock at the site of an underground powerplant for the Oroville Dam near Oroville , California . The stress distribution around each of three flatjacks was nonsymmetric ; however , stresses obtained from 9 flatjack and 157 borehole measurements are considered reasonably accurate for engineering purposes . The stress near the edge of the openings is between 800 and 1,600 psi ; the stress in the undisturbed rock is approximately 500 psi , nearly hydrostatic .

Jan 1, 1964

By F. E. Block, Stephen D. Hill

The necessity for measuring radiation dose is encountered in studying both the beneficial and damaging effects of ionizing radiation on materials . It is also necessary to know the radiation dose absorbed by the reactants in order to evaluate the efficiency of reactions or processes that are promoted by radiation . Thus , a significant effort was made at the Albany cobalt 60 facility to investigate techniques by which the exposure radiation dose can be determined . Methods including ferrous sulfate , ceric sulfate , and methyl methacrylate chemical dosimeters , ion chamber dosimetry , and an absolute radiation calorimeter were investigated . Isodose curves were constructed for several standard source configurations using the dosimetry techniques which were investigated .

Jan 1, 1964

By R. T. DeWoody, W. C. Miller, W. Chester

Studies were made to determine the effect of the shape of a pneumaticrock- drill exhaust muffler on its efficiency, and the origin and reduction of exit noise from the mufflers. Tests of mufflers of three different shapes proved that the shape is not critical and that a muffler could be incorporated into the shell of the drill. Petal diffusers are beneficial in reducing exit noise but add another projection to the machine. Increasing the number of exit openings while maintaining the same area of exit opening has a markedly beneficial effect on the exit noise and appears to be the most satisfactory treatment.

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 E. G. Davis, H. P. LeVan, L. S. Smith

Leaching of a Georgia umber ore when using both ferrous sulfate and pickle liquor was studied in the laboratory . The ferrous sulfate content of the leach solution was the major factor affecting the extraction of manganese from the ore . Time , temperature , and the sulfuric acid content of the leach solutions had relatively little effect on leaching of manganese from the ore ; however , these factors did affect the amount of iron extracted from the umber and/or precipitated from solution . Simulated countercurrent leaching of the ore with pickle liquor containing 130 gpl (grams per liter ) ferrous sulfate ( 48 gpl ferrous iron ) produced a pregnant solution having 16 gpl manganese and 41 gpl iron . Filtration tests of the leach slurries indicated that separating the leach solution and solids by vacuum filtration was impractical , whereas pressure filtration was feasible when the cake thickness was limited to about three- fourths of an inch . Fired pellets of the filter cake yielded a firm , hard product analyzing 56 percent iron and less than 0.1 percent sulfur .

Jan 1, 1964

By D. K. Deardorff, Laurance L. Oden, H. Kato, M. I. Copeland

The equilibrium relationship of hafnium and tantalum was studied to facilitate alloy and property investigations . The data obtained are presented graphically as the equilibrium diagram . Alloys were prepared from high - purity components by nonconsumabletungsten- electrode arc melting . Data for the equilibrium diagram were obtained by optical pyrometry , metallography , X- ray diffraction of heat treated specimens , X- ray diffraction using a high- temperature camera , and differential thermal analysis . During the investigations , a casting apparatus was constructed , and the existing melting - point apparatus was improved . The bcc allotrope of hafnium forms a continuous series of solid solutions , called beta , with tantalum which exhibit a minimum melting point at 20 wt pct tantalum and 2,110 ° C. At 24 wt pct tantalum and 1,050 ° C , hafnium- rich beta decomposes in a monotectoid reaction to yield alpha and tantalum- rich beta . The monotectoid isotherm extends from 5.5 to 60 wt pct tantalum . The twophase region , in which hafnium- rich and tantalum- rich beta solid solutions are immiscible , rises to a maximum temperature of 1,265 ° C at 38 wt pct tantalum . The solubility of hafnium in tantalum decreases from 40 wt pct at the monotectoid temperature to 20 wt pct at 750 ° C.

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 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 K. E. Tame

As part of a Bureau of Mines survey of radioactive waste disposal , a laboratory investigation was made to study such problems in carbonate leaching mills . Because uranium concentrators employing carbonate leaching with caustic precipitation normally recycle barren solutions to the washing circuit , the disposal of liquid radioactive wastes is automatically controlled . However , it was deemed important to determine the actual radium 226 concentrations occurring in this type of milling so that the survey of the entire industry would be complete . The laboratory procedure consisted of leaching the ground ore at 85 ° to 90 ° C and 50 pct solids for 6 hours in a sodium carbonate - sodium bicarbonate solution . The pulp was filtered to obtain a pregnant solution that was reacted with sodium hydroxide to precipitate the uranium as sodium diuranate . Regeneration of the barren solution was accomplished by gassing with carbon dioxide . The solution then was reused by advancing the solution through the washing to the leaching operations . The radioactivity in the pregnant solution was unusually high , averaging 6,500 disintegrations per minute ( dpm ) of radium 226 per liter . However , over 95 pct of the radium was precipitated with the uranium . Consequently , no buildup of radium occurred upon reuse of the barren solutions for washing .

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 M. M. Tilman

The purpose of this investigation was to determine the effects of small amounts of cobalt in nickel on the tensile properties and hardness of representative types of austenitic stainless steels . Cobalt substitutions for nickel up to 2 weight - percent were made in types 302 and 309 stainless steels . Data were obtained at room temperature for tensile strength , yield strength , percentage elongation , percentage reduction in area , and hardness . In type 302 steels , tensile strength and hardness increased with increased percentages of cobalt , percentage elongation and reduction in area decreased , and yield strength showed little change . Property changes were largely due to the reduction of nickel content rather than to the addition of cobalt . In type 309 steels , only minor variations were observed for the properties investigated ; the effects of the relatively snall cobalt substitutions and nickel reductions were somewhat reduced by the higher total alloy content .

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