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By T. A. Henrie, E. K. Kleespies

Carbon reduction of rutile and ilmenite in nitrogen and ammonia atmospheres was studied as a method of preparing titanium nitride . Ammonia was a better nitriding agent than nitrogen . The contact between the solid reactants , carbon and rutile , was a prime factor in nitrogen atmospheres and was of lesser import in dissociated ammonia . The reduction process for conversion of rutile to the nitride required carbon . The nitriding of ilmenite- carbon mixtures produced titanium nitride and elemental iron .

Jan 1, 1964

By D. W. Bridges, S. R. Borrowman

Thorium and yttrium oxides were recovered from siliceous ores of the Powderhorn , Colo . , area . Processing comprised ( 1 ) acid curing and subsequent ( 2 ) acid baking , ( 3 ) leaching , and ( 4) solvent extraction of thorium , using a primary alkylamine , and yttrium , using di - 2 - ethylhexyl phosphoric acid . About 95 pct of the contained thorium and yttrium was recovered from ore containing 1.2 pct Th02 and 0.5 pct Y₂ 03. The thoria product was 99 pct Tho ; the yttria product was 77 pct Y₂ 03. A 150 - to - 1 concentration ratio was effected on the latter , but some contaminating lanthanon - group oxides remained .

Jan 1, 1964

By Donald W. Mitchell, John Nagy, Edwin M. Murphy

To increase safety and productivity in mining , the potential uses and hazards of rigid foam were investigated by the Bureau of Mines Experimental Coal Mine . This research resulted in the development of chemical formulations , spraying equipment , and application procedures that permit safe and effective use of urethane foams for improving mine ventilation , for reducing weathering of mine rock and steel , for constructing seals in fire areas , and for thermal insulation .

Jan 1, 1964

By Robert J. Brennan, Edward R. Navrocky, John W. Buch

In an effort to establish a highly productive mechanized mining system for anthracite beds pitching between 10 ° and 20 ° , for which conventional mobile equipment is not adaptable , the Bureau carried out an experiment in longwall mining using an Anderton- type drum cutter loader and friction - type yielding steel roof supports . The roof- support system proved to be inadequate for breaking the overhanging roof at the break line supports , with the result that the roof broke over the solid coal . The accompanying subsidence destroyed the continuity of the roof in the work area , and the project was discontinued .

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 M. H. Kersten, G. A. Brady, Jerry W. Ramsey

Anthracite samples were oxidized with nitric acid to prepare products representing intermediate stages of oxidation . Similar oxidizing conditions affected different anthracites to varying degrees as characterized by peptization behavior with 0.1 N NaOH . Techniques used in attempts to separate and characterize the products included esterification , absorption spectrophotometry , sublimation , chromatography , electrophoresis , metal salt formation , and solvent extraction . Mellitic acid , either free or in the form of metallic salts , was identified in the acid- soluble products from 10 tests in which the anthracite was treated with nitric acid for periods varying from 24 to 1,000 hours . pentacarboxylic acid was also found in some products . Other benzene carboxylic acids were not present in amounts detectable by the methods used in this study . The acid- insoluble residue from nitric acid treatment varied significantly in solubility behavior toward different classes of solvents . The most effective ones tried included polar oxygenated solvents and pyridine . Infrared spectra of the extracted material indicated that similar compounds were extracted by the different solvents . Aliphatic amines and aniline peptized the residue and o- toluidine reacted with it . Organic material separated from the residue by peptization with dimethylformamide contained 1 percent ash , consisting of more than 50 percent zirconium .

Jan 1, 1964

By Foster Fraas

The response of minerals in magnetic separators is in accordance to dynamic rather than static magnetic susceptibility values . The dynamic value varies with respect to both passage speed through the separating field and time of exposure in a preliminary treatment field . Tests on 16 minerals and solids have demonstrated that both of these factors affect different minerals in different ways .

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 K. K. Kelley, L. B. Pankratz

The heat contents of four silicate minerals -- akermanite , cordierite , gehlenite , and merwinite --were measured from 298 ° to around 1,700 ° K by the dropping method . The results were compiled into tabular and equation forms suitable for thermodynamic calculations . The heat contents of these compounds are nearly additive with respect to their constituent oxides .

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 W. A. Stickney, J. W. Town

Studies on continuous - circuit leach - aluminum precipitation and leachelectrodeposition of mercury were made by the Bureau of Mines to determine optimum conditions and cost estimates for recovering mercury from mercury sulfide flotation concentrates . With 150 grams of sodium sulfide and 50 grams of sodium hydroxide per liter , from 98 to 99.8 percent of the mercury was extracted from flotation concentrates , with about 0.5 pound of sodium hydroxide used per pound of mercury produced . Precipitation of mercury from the caustic - sulfide solution with minus 8 - mesh aluminum shot required about 0.2 pound of aluminum per pound of mercury produced at a cost of $ 0.05 per pound of mercury . Electrodeposition cost with 7 mill power , based on 50 percent current efficiency , was below 2 mills per pound of metal deposited . Feed solutions ranged from 10 to 130 grams of mercury per liter , and current densities , from 2 to 70 amperes per square foot . The cost of open- pit mining 250 tons per day was estimated at $ 1.75 per ton , and flotation - leachingelectrodeposition of the ore , at $ 3.54 , resulting in a cutoff grade of about 0.1 percent mercury . The cost of underground mining 50 tons per day was estimated at $ 20.00 per ton , and the cost of milling the ore was estimated at $ 13.33 , which resulted in a cutoff grade of 0.6 percent mercury .

Jan 1, 1964

By L. B. Pankratz, R. Barany, W. W. Weller

Experimental determinations were made of the heats of formation at 298.15 ° K of cuprous ferrite and cupric ferrite ; the heat capacity of cuprous ferrite was measured over the temperature range from 50 ° to 298 ° K and the entropy at 298.15 ° K was evaluated ; the heat contents of cuprous ferrite and cupric ferrite above 298.15 ° K were measured to 1,500 ° K and 1,100 ° K , respectively . These thermodynamic values were combined with other pertinent data to obtain heat and free energy of formation values at high temperatures . The stability of the two ferrites with respect to their constituent oxides is discussed . Thermodynamic values are included for the decomposition of cupric ferrite to form cuprous ferrite , magnetite , and oxygen .

Jan 1, 1964

By F. E. Walker, S. J. Aresco, J. B. Janus

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal , expressed in British thermal units , and the composition as shown by proximate analyses . To these , when required , are added the ash- softening temperature , the free- swelling index , and the Hardgrove grindability index . Under most of these specification contracts the bidders guarantee the quality of the coal , and that guaranteed by the successful bidder becomes the standard of his contract . The deliveries are sampled in accordance with instructions 4/ issued by the Bureau of Mines ; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and , if it is not , a price adjustment is made . Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks ) provide valuable data for use in evaluating future bids . In addition , the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal . The Government purchased approximately 5 million tons of coal in fiscal year 1963 . In connection with these purchases , the Bureau analyzed 6,999 samples . These are published ( table 1 ) for the use of Government officials and the public . A series of publications has been completed on coal analyses by States or , where production is small in any one State , by groups of adjacent States . In addition to analytical data showing composition and quality of coals of the States , the publications contain brief descriptions

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 Michael G. Zabetakis, Israel Liebman, Henry E. Perlee

Flammability studies conducted to date on stratified methane - air and pentane - air mixtures in air indicate that location and extent of a flammable layer are affected by molecular diffusion , gas motion , and propagation of flame . In initially quiescent mixtures , the lower limit - of - flammability zone may be determined by assuming molecular diffusion alone governs mixing rate . The upper limit - of - flammability zone can be predicted in this manner only for stratified layers with small concentration gradients ( less than 0.2 volumepercent per inch ) ; where large concentration gradients are encountered ( for example , as much as 30 volume - percent per inch ) , the initial - mixture methane concentrations that yield flammable mixtures are larger than anticipated . Flames propagating through heterogeneous quiescent methane - air atmospheres in the direction of the concentration gradient exhibit flame speeds at any point that corresponds to the flame speed of the homogeneous gas mixture having the same gas composition as that of the point in the heterogeneous system . In flowing mixtures with large concentration gradients , the degree of mixing prior to ignition does not appear to affect the flame velocity and emitted radiation appreciably in a 6.5 - ft - diameter gallery .

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 K. K. Kelley, W. W. Weller

The heat capacities of four crystalline silicates of barium ( BaSiO3 , BaSiO4 , Ba Si¸0 , and BaSi₂0 ) and two crystalline silicates of strontium (SrSio and Sr₂Sio ) were measured over the temperature range from 51 ° to 298° K. The results were used to evaluate the entropies at 298.15 ° K. The entropy values were joined with known heats of formation to obtain the free energies of formation of the silicates with respect to their constituent oxides at 298.15 ° K.

Jan 1, 1964

By D. C. Crowell, A. G. Loomis

Both Dimensional and Inspectional Analysis are developed from fundamental concepts , and dimensionless groups are derived which represent the viscous , capillary , and gravitational forces existing in two - phase , incompressible flow in petroleum reservoirs . It is shown how properly scaled models may be devised by means of the foregoing groups . Laboratory measurements with such models faithfully duplicate the behavior of the reservoir on a miniature dimensional and compressed time scale , and when all the pertinent variables are evaluated , the model is a most effective tool for the study of complex fluid displacements in the reservoir . Applying the Principle of Similitude , it is shown how dimensionally scaled models are applied to various types of reservoir displacements : ( 1 ) Oil displaced by water , ( 2 ) gas displaced by water , and ( 3 ) miscible displacement . The special case of water displacing gas by imbibition is analyzed , and it is shown that the dimensionally scaled model must be fabricated of sandstone rather than unconsolidated sand , which is generally used in such models . This report is intended to be a review and summary of the application of Dimensional Analysis to reservoir displacement problems for those who are beginning the study of this useful and interesting method .

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