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By H. R. Babitzke, H. Kato, R. E. Siemens

An investigation was made to provide further information for evaluating columbium- hafnium alloys for use as high - temperature structural materials . The columbium- hafnium system was investigated between 700 ° and 2,400 ° C by melting point , thermal analysis , X - ray diffraction , electrical resistivity , and metallographic techniques . The equilibrium diagram is the beta isomorphous type , with columbium tending to stabilize the beta phase . Addition of 60 atomic percent columbium stabilizes the beta phase at 700 ° C. The allotropic transformation temperature of hafnium is 1,750 ° ± 20 ° C. A minimum melting point occurs near 75 atomic percent hafnium .

Jan 1, 1964

By Richard F. Hewlett

This Bureau of Mines report presents the computer programing methods and mathematics required to generate either random numbers or normal random numbers to be used for the construction of statistical probability models for simulating mineral deposits by Monte Carlo techniques . Theoretical frequency functions are evaluated as an illustration of simulation applications . Numerical and analytical methods of simulating and dissecting some complex frequency distributions are described .

Jan 1, 1964

By Charles H. Atkinson, Robert T. Johansen

Tremendous volumes of petroleum ( crude oil and natural gas ) at present cannot be recovered economically . The feasibility of using nuclear explosions for production stimulation therefore has been investigated . Data from underground nuclear tests conducted by the Atomic Energy Commission were reviewed , and the physical effects were evaluated for stimulating petroleum production . Calculations of the effect on ultimate recovery of increasing reservoir temperature with nuclear explosives showed disappointingly small increases . Production increases caused by fracturing of massive low- permeability reservoirs appear technically and economically promising . Petroleum reservoirs that might be converted from submarginal to commercial production are being located and evaluated as to potential reserves and as a location for a field test .

Jan 1, 1964

By L. H. Adami, E. G. King

The heats of formation of four sulfides --MnS ( alabandite ) , FeS ( hexagonal pyrrhotite ) , ZnS ( wurtzite ) , and CdS ( greenockite ) -- were determined by hydrochloric acid solution calorimetry . The heats of formation from the metals and rhombic sulfur at 298.15 ° K are , respectively , -51.01 ± 0.19 , -23.81 ± 0.24 , -45.86 ± 0.20 , and -35.70 ± 0.30 kcal /mole . The corresponding free energies of formation were calculated from the heats of formation and the pertinent entropy values .

Jan 1, 1964

By J. B. Zink, M. J. Peterson

A semiquantitative spectrochemical method was developed and applied to the analysis of ash of U.S. coals . A low- temperature ashing procedure was used to minimize the loss of volatile elements . The analytical procedure provides for the estimation of 68 elements including major , minor , and trace constituents . Standards for the trace elements were prepared in a synthetic base mixture that approximates the average composition of U.S. coal ashes . Excitation was achieved with a d- c arc , spectra were recorded photographically , and interpretation was made by visual comparison of spectra of unknowns with spectra of graded standards series . Thirty- six trace elements were found in the analysis of 900 samples . Details of the procedure are presented , including sample and standards preparation , excitation and exposure conditions , spectral lines used , and approximate limits of detectability .

Jan 1, 1964

By Wesley T. Holmes II, Lloyd H. Banning

Electric - smelting studies were made on titaniferous materials obtained from the Klukwan and Snettisham , Alaska ; Choteau , Mont .; and Iron Mountain , Wyo . , deposits with the objective of determining the feasibility of producing pig iron and an enriched titania slag in one test series and pig iron alone in another test series . In addition , related studies were conducted to determine the amenability of Choteau crude ore to wet -magnetic separation and to determine the quality of steel that could be produced from the titaniferous pig iron . The continuous smelting tests were made in a three - phase , submerged - arc , electric furnace , and the laboratory steelmaking tests were made in a singlephase electric - arc furnace . A continuous , belt - type , wet - magnetic separator was used in conjunction with a ball mill and a spiral classifier in recovering titaniferous magnetite from the crude Choteau ore . Pig irons containing less than 0.05 percent phosphorus or sulfur were readily produced from the titaniferous materials ; iron recoveries ranged from 92 to 98 percent . The Choteau ore was ground to minus 65 - mesh to produce a concentrate containing 60 percent or more iron . The steel produced from the titaniferous pig iron was a high - quality product .

Jan 1, 1964

By R. L. Crosby, L. W. Higley

Magnesium- rich magnesium- aluminum- zirconium alloys in the cast and in the extruded and heat- treated condition were studied to identify the phases present and to determine phase distribution . In cast alloys , two intermetallic compounds were identified : ZrAla by X- ray diffraction ; and Mg₁ Al₁₂ by microscopical observation . Based on microscopical comparisons between the known phases in the cast structures and the phases in the structures of extruded and heat - treated rods , ZrAl₂ and Mg1 , Al12 were identified in the structure of the latter . The presence of these intermetallic compounds in rod specimens could not be confirmed by X- ray diffraction . ZrAl₂ was observed in the structure of extruded and heat - treated rod specimens containing as little as 0.01 weight - percent zirconium . The presence of aluminum restricts the solubility of zirconium in magnesium because of the strong tendency to form ZrAla . This intermetallic compound segregated in clusters of small particles in the matrix of cast alloys , and only slight improvement in distribution was noted when the alloying techniques were varied .

Jan 1, 1964

By W. J. Boone, Will E. DeVaney, Lowell Stroud

This report is the fifth in a series presenting equilibrium vapor - liquid data for helium- bearing natural gases . It covers a 0.41 - mole - percent - helium natural gas that may be processed in the Department of the Interior's longrange helium conservation program . A Bureau of Mines phase equilibrium apparatus was used to obtain 139 samples of equilibrium vapor and liquid phases at 85 experimental conditions at temperatures from 0 ° to -299 ° F and at pressures from 100 to 500 psia . An appendix covers phase data at 100 , 200 , and 300 psia and at temperatures from -125 ° to -275 ° F for the dehydrated gas containing its original concentration ( 0.2 mole - percent ) of carbon dioxide , and the effect of a preliminary hydrocarbon trap upon subsequent vapor - liquid compositions .

Jan 1, 1964

By Bernard Porter, E. A. Brown

Electrical conductivities and densities of the LiF- UF , LiF- ThF4 , NaF - C1F4 , and NaF - ThF systems were measured as functions of composition and temperature . The specific conductance and density varied linearly with temperature . Molar and equivalent volumes , as well as heats of activation for conductance , were calculated from the experimental data . At 1,000 ° C , the molar volumes ranged from 16 to 40 cubic centimeters per mole and the specific conductance ranged from 9.8 to 2.5 per ohm- centimeter as the actinide metal fluoride concentration changed from 0 to 60 mole - percent . Heats of activation for conductance were 3 to 7 kcal per mole . The data are interpreted on the basis of a semilattice model for the melts .

Jan 1, 1964

By Richard F. Hewlett

Numerous populations of assays have been simulated for a range of assay values representative of low-grade mineral deposits to facilitate the study of problems encountered in evaluating these deposits. Analysis of these simulated populations of assays (obtained by using statistical probability models for the simulation) makes possible the quantification of the effects of (1) various composite assay intervals, (2) ore reserve computational methods, (3) uneven assay intervals, and (4) various cutoff grades on both the precision and the accuracy of the estimated average grade and tonnage of ore.

Jan 1, 1964

By D. J. Donaven, Manuel Gomez, W. S. Landers

Bulk density tests were made on a Western U.S. coke oven plant blend to obtain bulk density control data that would be directly transferable to plant practice . Maximum bulk density values were obtained at zero surface moisture . Increase in surface moisture to about 6 percent decreased the bulk density to a minimum value . Increase in the fine grinding of the blend , at constant surface moisture , decreased the bulk density . The effect of oil on bulk density was observed with five oils at concentrations ranging from 1/8 to 1-1 / 2 gallons per ton . Maximum bulk densities were obtained within the 1 / 2- to 1 - gallon - per - ton range . Essentially the same bulk densities were obtained with petrolatum- and nonpetrolatum- containing oils . Storage effects were observed on samples tested at selected intervals from 0 to 56 days . No significant change in bulk density took place if no surface moisture was lost during storage .

Jan 1, 1964

By C. E. Armantrout, H. Kato, M. I. Copeland

The data collected during this investigation indicate that the chromiumgadolinium system has extensive liquid immiscibility and one eutectic point . Liquid immiscibility occurred at temperatures above the monotectic isotherm , 1,830 ° C , which extended from less than 0.25 to about 85 weight - percent gadolinium . The eutectic was at 96 percent gadolinium and 1,170 ° C. Gadolinium and chromium were the only phases in this system . There was a solid solubility of less than 0.25 percent gadolinium in chromium at 1,730 ° C and less than 0.10 percent chromium in gadolinium at 1,160 ° C. The alloys were prepared by nonconsumable - electrode arc - melting , and the alloy system was investigated by heat treatment , metallography , thermal analysis , and X- ray diffraction . All the melting , heat treatments , and thermal analyses were conducted in a vacuum or in helium because of the reactivity of chromium and gadolinium with the components present in the atmosphere at elevated temperatures .

Jan 1, 1964

By R. V. Lundquist, H. Leitch

Sodium aluminate is the principal aluminum compound formed in the sinters prepared by the lime - soda sinter process for recovering aluminum from silicate source materials . The properties and characteristics of this compound were studied to improve the efficiency of the process . Crystalline sodium aluminate was prepared by sintering stoichiometric quantities of soda ash and calcined alumina for 1 hour at 1,250 ° C. The extent of aluminum extraction from sodium aluminate was determined in water and in solutions of NaOH and Na₂ CO3 . Nearly complete extraction of aluminum from sodium aluminate was achieved only in solutions containing free NaOH in excess of that supplied by the salt through hydrolysis . About 42.2 to 68.8 percent of the aluminum was extracted in water or in solutions of Na₂ CO . The precipitation of alumina trihydrate from sodium aluminate solutions was shown to be part of a continuous , reversible reaction according to the equation Al (OH ) A1 (OH )3 + OHThe reverse reaction dissolves alumina trihydrate in NaOH solutions to produce sodium aluminate . Approximate equilibrium concentrations were determined for the reaction at 30° , 50 ° , and 70 ° C. False apparent equilibrium conditions for the dissolution reaction appear when only a small excess of alumina trihydrate is present in the NaOH solutions . A large excess of alumina trihydrate must be present before the true equilibrium point is assured . The engineering significance of the data is summarized , showing controls that should be exercised for a successful and efficient process .

Jan 1, 1964

By Michael G. Zabetakis, Aldo L. Furno, George H. Martindill

Hydrazine vapor is flammable in the absence of air at elevated temperatures and atmospheric pressure . The minimum concentrations of benzene , toluene , m- xylene , cumene , and n- heptane needed to inhibit flame propagation through vapor mixtures of hydrazine and hydrocarbon were determined at 125 ° C and atmospheric pressure . These concentrations can be correlated with either the heat of formation or the heat capacity of the hydrocarbon .

Jan 1, 1964

By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By F. R. Cattoir, T. A. Sullivan

Commercial uranium metal was electrore fined to a high- purity product using molten- salt electrolytes in an inert atmosphere cell . Electrorefined uranium that contained , after consolidation , less than 30 ppm of metallic impurities was prepared . A method of leaching the electrolyte crystals to remove the salts was developed . Cathode current efficiencies from 90 to 100 percent were obtained . Two molten- salt electrolytes were prepared and evaluated : (1 ) lithium chloride - potassium chloride - uranium trichloride and ( 2 ) sodium chloridepotassium chloride - uranium trichloride . Very little difference was found in the purity of the uranium metal produced in either system . The lithium chloride - potassium chloride - uranium tri - chloride electrolyte was preferable from an operational standpoint .

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 J. O. Winget

Phosphonic acid and iminodiacetic acid chelating resins were investigated to assess their potential as selective ion exchangers for separating lanthanide elements and yttrium . The affinity of phosphonic acid resin for lanthanides increases with increasing atomic number , and that of iminodiacetic acid resin for lanthanides increases with atomic number to a maximum for element 62 and then declines with atomic number throughout the remainder of the series . Elution sequences of the elements with mineral acid eluants corresponded favorably with equilibrium data , whereas the elution sequence obtained with chelating eluants was proportional to the relative values of the stability constants of the chelating agents with the lanthanides . Separation of lanthanide mixtures into groups of light and heavy elements with iminodiacetic acid resin appears feasible .

Jan 1, 1964

By K. K. Kelley, W. W. Weller

This report contains experimentally determined heat capacity data for four crystalline sulfides -- AsS , GeS , NiS , and Ni3 S₂ -- over the temperature range from 50 ° to 298.15 ° K. The heat capacity data were used to evaluate the entropies of the sulfides at 298.15 ° K. Entropies of formation from the metals and rhombic sulfur and from the metals and diatomic sulfur gas are also included .

Jan 1, 1964

By J. B. Zadra, J. M. Gomes, Don H. Baker

Electrolytic deposition at 1,000 ° C in an electrolyte essentially consisting of 7 parts sodium pyrophosphate , 2 parts sodium chloride , and 1 part sodium tetraborate yielded tungsten of 99.9 percent purity . Scheelite concentrates containing 25 to 73 percent WO, and varying quantities of iron , lime , and silica were used as feed materials for the electrolysis . The metal contained less than 0.01 weight - percent each of iron , calcium , silicon , aluminum , carbon , and oxygen . Modification of the electrolyte permitted deposition of equal - quality metal from scheelite concentrates containing higher quantities of iron , calcium , and silica . The electrolytic separation of molybdenum and tungsten was accomplished by minor variations in the operating procedures .

Jan 1, 1964