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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 Thomas C. Miller, Rudolph Sporcic

A relatively simple and inexpensive encapsulated hydraulic device has been developed by the Bureau of Mines to facilitate study of coal bumps , and to measure pressure changes in a coalbed as it is subjected to roof loading during mining . Construction of the device and application techniques are described . Preliminary feasibility tests in the laboratory and field indicate that the device responds satisfactorily to pressure changes in coal created by roof loading .

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

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 Gus Pantages, Bernard D. Blaustein, Charles Zahn, Irving Wender

Oils from coal hydrogenation have been examined at the Bureau of Mines to learn whether any centers of the optical activity reported in coal would survive catalytic hydrogenation at 450-525 ° C and about 8,000 psig pressure , and , if so , to obtain information about the nature of the active products . Oils from carbonization tars also were examined . Optical activity was found in the majority of the distillate fractions of the hydrogenation oils and in almost all distillates from the carbonization tars . No activity was observed in the tar - acid and tar - base fractions examined . Methods for isolating optically active concentrates included distillation through a packed column , liquid chromatography on silica gel , and adduction with urea . For the materials so processed , the optical activity segregated mainly in the paraffin - naphthenic and the hydroaromatic fractions . Although the specific compounds responsible for the optical activity were not isolated , experimental and spectrometric findings indicate that alkylsubstituted cycloalkane , cycloalkene , and hydroaromatic structures are most likely responsible for the optical activity of the concentrates . The optically active centers probably derived mainly from the steroids and terpenes in the biological materials that participated in the formation of coal .

Jan 1, 1964

By M. J. Kovalik, D. E. Wolfson, F. Fischler

Plastometric tests were made to determine the maximum thickness of the plastic layer for different U.S. coals . The effect of test variables on the maximum thickness of the plastic layer was studied . The values for the maximum thickness of the plastic layer were found to be related to the Gieseler maximum fluidity , plastic temperature range , free swelling index , and other plastic properties of coals . Only a general relationship was observed between the plastometric parameters obtained in these tests and the coking properties of coal .

Jan 1, 1964

By C. J. Walker, Ray V. Huff

The feasibility of inert - gas cushions in underground gas storages was studied by the Bureau of Mines in accordance with a continuing program of cooperative research between the natural gas industry -- through the American Gas Association . As mixing of the inert - gas cushion with the stored natural gas is undesirable , the various mechanisms tending to bring about such mixing were the subjects of both theoretical and experimental studies . These studies indicated the practicability of such cushions is dependent upon both reservoir and operating conditions . Equations and tables of illustrative data relating the various reservoir and operating conditions to the expected time required for undesired mixing to occur in ideal reservoirs are presented . This information permits estimating the relationship of such factors in actual storage operations .

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

Information is presented on remote sealing of a mine passageway through a borehole by five methods : PPnneeuummaattiicc injection of mineral wool and sand, ureaformaldehyde foam , balloons , urethane foam, and caving by blasting . An adaptation of the method using pneumatically conveyed mineral wool was tried in an operating mine . Further research is needed to simplify and to improve the techniques involved , as well as to explore the possibilities of other methods and combinations .

Jan 1, 1964

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 R. L. Hopkins, H. T. Rall

A continuous method has been developed for preparing thiolacetic acid . Acetic anhydride and hydrogen sulfide are passed concurrently over an amine ion- exchange resin , under 20 - psi pressure . The thiolacetic acid , a product of the reaction , is flashed continuously from the crude reaction mixture and is purified by fractional distillation . The yield of thiolacetic acid is in excess of 80 percent based on the acetic anhydride charged . INTRODUCTION In the synthesis of reference compounds needed in the identification of sulfur compounds in petroleum , thiolacetic acid has become an important reagent because of its use in the synthesis of thiols by addition to appropriate olefins : R - CH = CH₂ + CH3 - COSH R- CH2 - CH2 - S - COCH R - CH2 - CH₂ - SH + CH3COONa NaOH (1 ) The commonly used procedures for its preparation , as described by Clark and Hartman (1 )4 and by Ellingboe (2 ) , are based on the batchwise reaction of acetic anhydride with hydrogen sulfide :

Jan 1, 1964