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By J. R. Hauger, P. A. Romans, W. J. Niebuhr

With suitable instrumentation and techniques it is possible to determine the presence of tantalum in columbium to 20 ppm . This paper discusses the selection of X- ray spectrographic instrumentation and describes a technique for accomplishing the low level determination of tantalum . An ion- exchange method of separating tantalum from columbium is also described .

Jan 1, 1964

By A. L. Service, C. C. Popoff

Phosphate deposits in Montana , Idaho , Wyoming , and Utah are important factors in the mineral , agricultural , and industrial economy in the western part of the Nation . This report presents background information , including geology , mining , beneficiation , processing , resources , and economics , assembled to provide a comprehensive introduction to a series of four area reports . About 20 percent of the Nation's phosphate is produced from the Western field where there were 6 surface and 9 underground mines in operation in 1963 . This region also has an estimated 58 percent of the Nation's phosphate reserves , and continuing development is assured by these abundant resources and an increasing demand for phosphate products . Long range forecasts indicate that the United States will continue to use increasing amounts of both agricultural and industrial phosphate products . Beneficiation has become an important part of the phosphate processing industry , and two flotation plants and several washing plants were in operation in 1963. Recent studies by the Bureau of Mines Metallurgy Research Center , Albany , Oreg . , have been directed toward developing flotation processes applicable to treatment of marginal phosphate rock . Other Bureau of Mines research is being directed toward improved methods of ore recovery , ground control , and mining .

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 J. H. Holden, G. R. Strimbeck, L. F. Willmott, W. R. Huff

A pilot - scale fluidized feeder was developed for continuously feeding up to 1 ton of pulverized coal per hour to a pressure gasifier . Fluidization in the 3 - foot - diameter by 34-1 / 2 - foot - high feeder is effected by two streams of inert gas , a technique called zone fluidization . A stream of inert gas through a drilled plate in the base of a central column near the bottom of the feeder fluidizes the coal . Another stream through a drilled plate in the annulus between the central column and feeder wall provides a source of semifluidized coal for the central column . Fluidized coal from the central column discharges through an extraction funnel and discharge line . Zone fluidization provided good fluidization with moderate requirement for fluidizing gas . Instruments were developed for metering and recording the flow rate of fluidized coal . A system was developed for storing , and weighing pulverized coal , and then delivering it in fluidized form at about 1 to 8 tons per hour .

Jan 1, 1964

By M. M. Wong, J. E. Klosterman

Scrap beryllium chips ( nominally 96 to 97 percent Be ) were electrore fined in a prototype cell with 408 lb of electrolyte composed of 52.4 mole - percent LiCl , 36.3 mole - percent KC1 , and 11.3 mole - percent BeCl2 . The cell temperature was 500 ° C. In a typical 10-3 /4 - hour deposition cycle , 0.415 pound of metal was produced ; the metal contained impurities in parts per million as follows : C , 700 ; 0 , 610 ; Al , 34 ; Ca , 32 ; Cu , 20 ; Fe , 25 ; Mg , 9 ; and Mn , 23 . Operation of the prototype cell for 2 years demonstrated that adapting the electrorefining process to an enlarged scale of operation presented few difficulties in mechanical functions , maintenance of optimum operating conditions , and control of product purity . After the spent anode feed was leached in a 5 - percent nitric acid solution and the fine - sized particles were removed , it was recycled in some tests . The metal produced was somewhat higher in impurities than metal from the fresh scrap chips .

Jan 1, 1964

By Leonard Obert

A triaxial procedure is described for measuring the modulus of elasticity and Possion's ratio of stress relief cores , that is , the concentric hole cores obtained by the overcoring technique . The elastic constant determinations can be made at stress levels comparable with those encountered in underground mining . The results from tests on an aluminum alloy calibration specimen and four rock specimens are included .

Jan 1, 1964

By James S. Browning, W. H. Eddy

Laboratory batch and small - scale continuous flotation tests were conducted on a ferruginous barite - fluorspar ore from near Sweetwater , Tenn . , to determine the feasibility of producing commercial - grade fluorspar and barite concentrates . The lignin sulfonate - sodium fluoride - fatty acid method of floating fluorspar produced acid - grade concentrates . Flotation of the barite from the fluorspar tailing using petroleum sulfonate yielded concentrates suitable for use as a weighting agent in oil -well drilling muds . The continuous flotation tests , treating about 150 pounds of ore per hour , yielded fluorspar concentrates that assayed 98.3 percent CaF2 and barite concentrates that assayed 91.2 percent BaSO4 . The recovery of the two minerals was 91.2 and 85.2 percent , respectively .

Jan 1, 1964

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 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 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