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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 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 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 Harry R. Nicholls

As part of the pre- and post - shot mine examination at Project GNOME , acceleration data were recorded underground from a series of chemical explosive shots . The cube root of the charge weight was used to scale acceleration and distance because charge weight was not constant . Regression analysis of particle acceleration - distance data gave the following propagation equation : A W1 /3 = 5.10 x 105 ( R / W¹ / 3 ) −2 .43 The quantity A W1 /3 is scaled particle acceleration expressed in g's - lbs¹ / 3 , and R/W1 /3 is scaled distance expressed in ft / lbs¹ /3 Data obtained from the nuclear explosion were scaled and fall within one standard deviation of the calculated propagation law for the smaller shots . Cube root scaling laws were adequate to group acceleration data from explosive charges varying by a factor of more than 1 x 10 in charge weight and over shot - to - gage distances varying from 100 to 46,000 feet . Data obtained from a series of small tests provided sufficient data from which reliable predictions of acceleration could be made for the large nuclear explosion .

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

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 C. D. McMaster, John C. Hartley

Three systems that monitor ventilating fans are described . These electronic monitoring systems automatically perform most of the operations required to conform with the provisions of the Federal Mine Safety Code in the event of fan failure or slowdown .

Jan 1, 1964

By Frank B. Fulkerson

A study was made of the economic factors governing silver production in the Coeur d'Alene mining region, Shoshone County, Idaho. Production and other statistics were analyzed. It was concluded that if the rapid rise in the open market price that began late in 1961 continues, greater production of the metal should result from the mines of the Coeur d'Alene mining region. However, the output gain would be limited, because costs per ton of ore mined would rise as production was increased beyond optimum capacity. Advances in the price of silver would increase the size of ore reserves by making some marginal ore profitable to mine and by providing greater funds for exploration projects that might result in discoveries adding to the reserves. Output of byproduct silver from Lead-zinc mining probably will not exceed 4.3 million ounces, judging from the trend from 1946 to 1961.

Jan 1, 1964

By Frank B. Fulkerson

A study was made of the economic factors governing silver production in the Coeur d'Alene mining region, Shoshone County, Idaho. Production and other stat is tics were analyzed. It was concluded that if the rapid rise in the open market price that began late in 1961 continues, greater production of the metal should result from the mines of the Coeur d?Alene mining region. However, the output gain would be limited, because costs per ton of ore mined would rise as production was increased beyond optimum capacity. Advances in the price of silver would increase the size of ore reserves by making some marginal ore profitable to mine and by providing greater funds for exploration projects that might result in discoveries adding to the reserves. Output of byproduct silver from lead-zinc mining probably will not exceed 4.3 million ounces, judging from the trend from 1946 to 1961.

Jan 1, 1964

By J. A. Ruppert, P. M. Sullivan

A process was developed on a laboratory scale in which iron contained in galvanizers ' zinc dross and aluminum contained in scrap zinc die - cast alloy were removed simultaneously . Melting both types of scrap together in the proper proportions resulted in formation of solid intermetallic Fe₂ Alg , which was readily removed from the melt by filtration and centrifugation . Recovery was 87 to 92 percent of the available zinc . Refined filtrate contained 0.02 percent iron and 0.20 percent aluminum. Aluminum content was further reduced to less than 0.01 percent by fluxing with zinc chloride . Low temperatures employed and inexpensive equipment requirements make the process commercially attractive .

Jan 1, 1964

By John Ward Smith, Neil B. Young

Shale specific - gravity to oil - yield relationships were developed for black shales of the New Albany Formation of Kentucky from data collected on core samples representing the complete section of the formation in three counties . Linear equations for estimating oil yield from measured specific gravity and for estimating specific gravity from measured oil yield were shown to be applicable within small error limits to all the sites tested . Variation in pyrite content is the largest source of error .

Jan 1, 1964

By T. F. Curry, L. B. Berger, H. A. Watson, S. J. Pearce

The conduct of work at elevated air pressures , such as in caissons and in tunnel - driving in subaqueous strata , poses safety problems not encountered in mining and tunneling operations at ordinary atmospheric pressure . This publication discusses some of the problems involved and presents information on the following subjects : ( 1 ) Physiological effects of gases at elevated pressure . ( 2 ) Use of respiratory protective equipment in rescue or recovery operations in event of fire or other emergency in pressurized tunnels . ( 3 ) Effect of elevated pressure on performance of some gasdetecting instruments ; interpretation of the results . Various types of respiratory protective devices are discussed in relation to their possible use at elevated pressures , especially the 2 - hour , selfcontained , recirculating - oxygen - breathing apparatus , which has had wide use in the United States during rescue and recovery work in the mining industry . A modified procedure that eliminates the hazard of oxygen poisoning enabling the safe use of this apparatus at elevated pressures , up to 45 pounds per square inch , gage , and tests to verify its practicability are described . procedure involves control of the partial pressure of oxygen in the breathing

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 Robert T. Beckman

The results of a preliminary investigation of compressive strength versus length-diameter (L/D) ratios of potash specimens and the statistical treatment of the data are summarized in this report. The purpose of the study was to evaluate a laboratory method for obtaining estimates of the strength of potash pillars during robbing operations. The specific objectives of this preliminary investigation were to test the method and the reliability (confidence limits) of the data, and to determine the number of additional specimens necessary for given confidence limits. The specimens were taken from three sites at two mines in New Mexico. The statistical analyses included the determination of the confidence limits for the data and the number of additional specimens necessary to obtain confidence limits of ±500 and 100 psi. The testing method was found acceptable, and estimates of the comprehensive strength, within 1500 psi, could be obtained by testing about 110 additional specimens from the three sites. The compressive strength of the specimens tested fits an empirical equation of the type

Dec 1, 1963