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By Scott W. Hazen

This report presents the results of a statistical analysis of a limited amount of sample and assay data from a production panel in an open - pit phosphate mine in the Phosphoria formation in Idaho . A frequency distribution analysis is shown for the assays , sample interval lengths , and products of assay and sample interval length for the millshale , furnace - shale , and main phosphate beds . Correlation techniques were used to show the relationships between assays and sample interval lengths . Within- drill - hole and between - drill - hole correlation were also examined as a means of predicting grade trends in the ore . Simulation methods , utilizing a digital computer , were used to establish assay populations that could be used for estimating grade of ore , cutoff grades , and deposit or bed identification .

Jan 1, 1964

By K. A. Fowler, L. W. Higley

The effect of uranium on the transformation kinetics and the hardenability of a low- alloy steel was evaluated . Isothermal transformation curves were developed from metallographic studies , and hardenability was determined by standard Jominy end- quench tests . For the steels investigated , the addition of 0.15 weight- percent uranium was found to produce a significant shift in the isothermal transformation curve and caused a related increase in hardenability . These effects diminished rapidly when the uranium content was increased above 0.2 weight - percent .

Jan 1, 1964

By Sarkis G. Ampian

Published optical microscopic and X- ray diffraction characteristics of the following compounds are critically evaluated and compared with Bureau of Mines data : Tricalcium aluminate , calcium monoa luminate , dodecacalcium heptaluminate , dicalcium silicate , tricalcium silicate , and sodium aluminate . A recommended set of definitive optical and X- ray diffraction characteristics is presented . These values are used to identify products of the lime soda sinter process for production of alumina . Polymorphism of gamma- , beta- , and alpha prime - dicalcium silicate is reexamined , and new data are presented on polymorphism of tricalcium silicate and sodium aluminate by high- temperature X- ray diffractometry . Polymorphism is not observed for tricalcium aluminate , calcium monoaluminate , and dodecacalcium heptaluminate . Bureau of Mines data indicating a stoichiometry of 12Ca0.7A10 for the phase 5Ca0.3A1 0₂ are discussed . A critical review of the literature concerning calcium dia luminate and sodium undecaluminate ( 8 -A10 ) is also included .

Jan 1, 1964

By M. E. Tyrrell, J. Koster

This work was undertaken to determine the feasibility of making mixed diborides of two metals directly from the metal oxides , boron carbide and carbon . The diborides (Ti , V ) , B₂ , (Ti , Cb) B₂ , and ( Ti , Ta ) B₂ were prepared in a crucible resistance furnace at 2,100 ° C , and X- ray- diffraction analyses showed each was a homogeneous solid solution containing approximately equal molar contents of the given diborides . The diboride powders were cold - pressed ; sintered to 2,300 ° C , and evaluated for mechanical strength , rate of oxidation , and resistance to molten metals . The diboride ( Ti , Ta ) B₂ exhibited the best mechanical properties ; the diboride ( Ti , Cb ) B₂ , the lowest cumulative rate of oxidation . The mixtures were stable in the presence of molten aluminum and copper but were attacked by molten Ti , Zr , and Cr .

Jan 1, 1964

By Scott W. Hazen, Richard F. Link, George S. Koch

The Mi Vida mine , Big Indian district , San Juan County , Utah , is in an ore deposit of uranium and vanadium minerals disseminated in certain sedimentary beds of the Triassic Chinle formation . Statistical analysis of assays of samples taken from the ore body affords an estimate of the grade of the ore body and provides a prediction about the direction of best mineralization beyond the sampled area . The basic data analyzed are assay results for uranium ( Uз Og ) , vanadium (V₂O ) , and lime (CaO ) from 225 channel samples cut at 79 sample points . Through the use of appropriate statistical methods , particularly regression analysis , the grade of ore may be estimated more precisely than by conventional means , and the most favorable direction to extend the mine may be predicted . Frequency distributions of assay residuals for uranium , vanadium , and lime are compared to frequency distributions of assays without regard to trend . Correlations among these variables are obtained and interpreted . The statistical methods employed illustrate certain techniques that may be used to analyze assay data from ore deposits in general .

Jan 1, 1964

By H. D. Hess, C. P. Mabie

This report describes in detail the results of petrographic research conducted on 21 phosphate ores representing important deposits in southwestern Montana , southeastern Idaho , and northeastern Utah . The ores are described and categorized by mineralogical and chemical composition , thermal behavior of organic carbon , and textural constitution . Descriptive and genetic classification schemes applicable to western phosphate ores are discussed ; results from related studies made of the collophane mineralogy are also presented . The latter studies were centered on determining unit - cell dimensions and CO₂ , P2O5 , and fluorine content of collophane concentrates of 11 high - grade phosphate- rock hand specimens selected solely for this purpose . On the basis of this investigation , operational methods have been developed for quantitatively describing textural and compositional features that are likely to be significant in determining the response of phosphate ores to conventional beneficiation treatments ; systems for classifying the ores in relation to these features have been proposed . Studies to date point out distinct textural and compositional variations in the western phosphates and illustrate their importance in determining optimum beneficiation procedure .

Jan 1, 1964

By William I. Nissen, Richard Havens

Continuous flotation studies were made at a 50 - lb - per - hr feed rate to confirm the effectiveness of a batch - scale procedure for concentrating phenacite and bertrandite minerals from Mount Wheeler ores that contained , in percent , 0.47 , 0.78 , and 4.7 BeO . The procedure for selective froth flotation of the beryllium minerals from a gangue composed chiefly of calcite , fluorite , and mica comprised closely controlled preconditioning with sodium fluoride and sodium hexametaphosphate in a series of small mechanically agitated tanks and use of a mixture of oleic acid with kerosine , fuel oil , or turpentine as a collector . It was difficult to adapt the laboratory flotation procedure to continuous operation . The principal problem of achieving adequate conditioning to depress calcite and fluorite ultimately was resolved by conditioning in series . Thereafter , three ore samples of different grades treated on a continuous basis yielded concentrates containing from 12 to 25 percent Beo from these relatively complex and difficult ores . Recoveries , on a BeO basis , ranged from 75 to 88 percent . Losses , which primarily were due to incomplete liberation , probably could be lowered in a commercial operation .

Jan 1, 1964

By D. Bienstock, J. H. Field, M. J. Lempel

A computer program is presented to perform the detailed and numerous calculations required for determining the interface temperatures and steady - state heat flow through a furnace wall composed of several refractories in layers . A method is developed that will allow the designer to determine the various thicknesses for each refractory layer to minimize either the total wall thickness or the cost of the wall per unit of area . A sample problem is presented and analyzed to illustrate the techniques involved .

Jan 1, 1964

By J. B. Zadra, H. J. Heinen

Electrowinning molybdenum from oxide feed materials dissolved in a variety of molten baths was investigated . A NaCl - NaF - Na₂ B₁ O -Mo0, system operating at 1,000 ° C in a cell without a protective atmosphere gave the best current efficiency , metal - to - cathode adherence , and purity of electrowon Technical - grade molybdic oxide , containing associated impurities of aluminum , iron , copper , silicon , and tungsten in combined quantities of 10 percent , was used as feed material to produce dendritic crystals of molybdenum metal containing less than 0.5 percent total base metal , carbon , and oxygen impurities . Arc - melting molybdenum electrowon from either chemically pure or commercial - grade Mo0, produced ingots that contained less than 0.1 percent total impurities and had hardness readings of 168 to 200 Vhn .

Jan 1, 1964

By R. V. Lundquist, A. E. Morris, E. L. Singleton

This experimental research was performed to determine rate - of - reaction constants on the MnO - C and Mn , C₂ - 3MnO systems at 1,100 ° , 1,150 ° , and 1,185 ° C. Reactions were conducted at atmospheric pressure under controlled flow of purified helium through the furnace chamber . The weight - loss method defined reduction percentages , and reaction products were identified by X- ray methods . The system Mn0 - C followed a linear reaction rate , and experimental results produced an apparent activation energy of 55.8 kcal per mole of Mn0 . The system Mn, C - 3Mn0 followed a parabolic rate of reaction law and yielded an apparent activation energy of 114.4 kcal per mole for the reaction .

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Robert Madden

Experiments were made in a semicontinuous unit to provide engineering data for designing experimental continuous systems . These systems would be used to study the hydrogasification of hvab coal and char (from lowtemperature carbonization ) to high - Btu gas . In experiments at 800 ° C and with a coal residence time of several seconds , yields of hydrocarbon gases increased from about 2,000 scf / ton of maf coal at 250 psig to 7,000 scf at 1,000 psig . With 15 minutes residence time , yields increased from 8,000 scf/ton of maf coal at 250 psig to 17,500 cubic feet at 1,000 psig . In all cases , small quantities of heavy oils were produced along with the gaseous hydrocarbons . Production of oils could be minimized with a corresponding increase in gaseous hydrocarbons by increasing the retention time of the volatiles within the hot zone . Yields of gaseous hydrocarbons from char were slightly greater than from coal under similar conditions . Although the hydrogasification reaction is very pressure dependent , substantial quantities of coal (40 to 60 percent ) could be reacted to gaseous hydrocarbons at pressures as low as 50 psig provided reaction temperatures were increased to 1,200 ° C. It was also demonstrated that a hvab coal could be hydrogasified continuously without incurring agglomeration . This was achieved by dispersing coal in a relatively large reactor with concurrent flow of hydrogen . At 1,000 psig and 800 ° C , it was possible to react about 35 percent of the coal and to produce a gas containing up to 52 percent methane .

Jan 1, 1964

By Gilbert M. Farrior

Tests of resistance to molten metals , to oxidation at elevated temperatures , and to various chemical reagents were made for a series of compositions in the TiB₂ - CrB₂ subsystem . In reaction with molten metals , there was no noticeable difference in reaction of the various compositions in the ( Ti , Cr ) B₂ series . The oxidation tests were ( 1 ) a rising - temperature test in which the specimen temperature was increased 4° per minute to 1,200 ° C and ( 2 ) a constanttemperature test in which the specimen temperature was held constant at 1,000 ° C. Compositions near Tio.6 Cro.4 B2 had the best oxidation resistance . Ti。.6 The chromium- rich alloys showed marked superiority to the titanium- rich alloys in resistance to corrosion by the chemical agents investigated . The chemical reagents used were sulfuric , nitric , and hydrochloric acids and sodium hydroxide of different concentrations .

Jan 1, 1964

By J. W. Eckerd, W. S. Sanner, P. L. Woolf, R. E. McKeever

The Bureau of Mines experimental blast furnace was operated successfully with anthracite metallurgical briquets . Tuyère pressures were higher and more erratic than for operations using coke , and furnace " hangs " occurred more frequently . Higher hot - blast temperatures were required to maintain the quality of the metal . By using higher hot blast temperatures , the fuel and production rates and slag volumes were comparable to those obtained for all - coke operation . The anthracite metallurgical briquets exhibited excellent mechanical strength and descended through the shaft of the furnace with little breakage or reduction in size .

Jan 1, 1964

By E. C. Tarpley, R. A. Drogowski, R. F. Abernethy

Three of the test methods frequently used for the determination of moisture in the analysis sample of coal were employed in analyzing a series of coals ranging in rank from anthracite to lignite . For most coals , the variation between the three methods are within the tolerances allowed between duplicate determinations by the same method . The processing variables studied included atmosphere , flow rate of atmosphere , inert atmospheres , oven temperatures , heating time , exposure of the dried coal to laboratory air , and surface area of the test sample . Unless close control is kept on these variables , erratic results will be obtained .

Jan 1, 1964

By K. A. Fowler, L. W. Higley

Steels with an alloying addition of depleted uranium were studied to develop successful melting , casting , and fabricating methods ; to obtain data on mechanical properties ; and to determine the effects of this alloying element . Uranium in amounts up to 1.5 percent was added to steel - base compositions containing approximately 0.5 percent carbon , 2 percent nickel , 0.25 to 2.0 percent silicon , and 0.75 percent manganese in both vacuum- melted and air -melted heats . Radiation levels were monitored for all operations . Bureau of Mines research at the Rolla Metallurgy Research Center showed that uranium additions did not increase tensile strength ; that hot - shortness occurred during forging above 1,090 ° C because of the presence of a low melting point constituent of a eutectic type ; and although a measurable amount of radioactive contamination resulted from processing , the quantity was never large enough to require the work area to be identified as a radiation area .

Jan 1, 1964

By R. V. Lundquist, H. Leitch

The solubility characteristics of three calcium aluminates , 12Ca0 · 7A120½ 3Ca0 A1203 , and 4Ca0 A12 03 Fe2O3 , were determined in water and in solutions of NaOH and Na₂ CO₂ to more clearly define their role in relation to the recovery of aluminum by the lime sinter and the lime - soda sinter processes . The calcium aluminates were prepared by sintering stoichiometric mixtures of CaCO3 , Al2O3 3H20, and Fe 0 at 1,375 ° C. The rates and extent of aluminum extractions were determined . The aluminum extractions from the aluminates were dependent on the presence of carbonate ions in the leach solutions , temperature , time , leach solution composition , and solid - liquid ratio of the slurry . The aluminum extracted from the calcium aluminates in water and in NaOH solutions varied from 4.6 to 22.9 percent . Virtually , complete extraction could generally be obtained for 12Ca0.7A120 and 4Ca0.A12 03 • Fe₂ 03 ; in one instance it was obtained for 3Ca0.A1203 , when an excess of carbonate ions was present over that required for the conversion of all of the calcium in the aluminates into CaCO3 . In some cases of poor aluminum recoveries , extractions could be improved by regrinding and releaching the solid residues .

Jan 1, 1964

By Earl L. Phillips

The Bureau of Mines conducted laboratory tests on samples of pozzolaniccement concrete to develop a low- strength backfill . Results show that support costs can be lowered by replacing a portion of the portland cement in mine backfill with pozzolan ( fly ash ) and lime . Unconfined compression tests on various ratios of fly ash to cement in 84 samples produced compressivestrength curves that can be used to estimate the best backfill mix for any mine .

Jan 1, 1964

By James M. Nishi, Lloyd Carpenter

Sixteen elements were determined spectrochemically in the general range of 3 to 1,000 ppm in high - purity columbium . Samples were converted thermally to Cb2 O , mixed with graphite and Ge02 , and excited for 15 seconds using a 15 - ampere dc arc . For the molybdenum determination , the oxidized samples were mixed with NaCl and Geo₂ and excited for 30 seconds . Spectra were recorded on photographic plates , and spectral line transmittance values were measured photometrically . Relative - intensity ratios of selected analytical and internal standard spectral lines were plotted against concentrations of standards to form curves from which concentrations of impurities were read . Average precision of the method was 11.2 percent relative standard deviation .

Jan 1, 1964

By Alla D. Mah

The energies of combustion of zirconium carbide and hafnium carbide were measured by combustion calorimetry and the heats of combustion and formation. of zirconium carbide and hafnium carbide were derived . The results are-- ZrC AH298.15 ( combustion) = -308.60 ± 0.55 kcal /mole , AH298.15 ( formation) -47.0 ± 0.6 kcal /mole , AH298.15 = HfC (combustion ) = -306.08 ± 0.20 kcal/mole , AH298.15 ( formation) -52.3 ± 0.4 kcal /mole . = INTRODUCTION This report contains the results of calorimetric measurements to obtain the heats of formation of zirconium carbide ( ZrC) and hafnium carbide ( HfC) . The work was conducted as part of a Bureau of Mines program for determining the heats of formation of oxides , carbides , and nitrides by combustion calorimetry . Combustion calorimetry is one of the most precise calorimetric techniques . The chief obstacle to obtaining accurate heat of formation values for carbides , and the chief reason for the variation in the results of different investigators , is the lack of purity of the carbide samples . Corrections for impurities always involve assumptions which lead to uncertainties . In general , a large impurity correction is accompanied by a large uncertainty in the final result .

Jan 1, 1964

By V. E. Edlund

This report presents the results obtained in a study of the technical feasibility of recovering a usable pig iron by pyrometallurgical treatment of typical copper reverberatory slags . The iron in the slag was readily reduced with carbon , but the copper and sulfur content of the metal was best controlled by a three - stage procedure comprising ( 1 ) melting the slag with pyrite to remove copper as a low- grade matte , ( 2 ) smelting the partly decopperized slag with fluxes and carbon to reduce the iron , and ( 3 ) refining the impure iron alloy from step 2 with a flush slag to remove sulfur and residual copper . Laboratory - scale tests demonstrated that washing with 8 wt pct of pyrite lowered the copper content of a typical reverberatory slag from 0.58 to 0.12 Subsequent smelting of a mixture composed of 70 pct decopperized slag , 25 pct lime , and 5 pct coke reduced 84 pct of the iron to metal containing 2.27 pct sulfur . This metal then was successfully desulfurized by treatment with a basic flush slag to produce a finished metal that contained , in percent , 93.5 Fe , 0.02 S , 0.26 Cu , and 4.9 C. Overall recovery of iron under the conditions of trial was about 80 pct . This could be increased if higher tolerances for copper could be accepted . Commercial processing would be accomplished in three furnaces with molten materials passing from one to another . Currently produced smelter slag could be treated fairly inexpensively , because the molten product would require only a little additional heat to produce an iron byproduct that undoubtedly would be attractive to local foundries .

Jan 1, 1964