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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 B. H. Eccleston, R. F. Kendall, D. E. Hirsch, Norman G. Foster

The mass spectra of 23 alkylthiophenes are presented , including 21 that have not been previously reported . Correlations between mass spectra and the structure of the thiophene homologs are discussed . Comparisons with , and corroboration of , earlier workers ' correlations and predictions are made . Several additional correlations are reported to enable the spectroscopist to identify the substituents on alkyl - substituted thiophenes , and the relationship of the mono - substituted and 2,5 - disubstituted alkylthiophenes is discussed in detail .

Jan 1, 1964

By M. H. Stanczyk, I. L. Feld

Dewatering of typical Florida phosphate rock slime by electro - osmotic techniques was investigated to determine if a compacted , plastic solid product could be obtained with simultaneous recovery of the water for re - use . Tests with porous cathodes and rod - type anodes imbedded in dilute slime charges of up to 4 tons in weight showed that the slime could be dewatered to about 35 percent solids . The dewatered products had the consistency of modeling clay . In the large - scale tests using 2.5 - foot electrode spacings , about 21 kilowatthours of power were consumed per ton of water removed in thickening the slime from 17 to 25 percent solids , but the rate of water removal was so slow that the process was not considered commercially feasible . Other tests made with electrode spacings of from 2.5 to 8 feet showed that more rapid dewatering could be obtained but that the power required was excessive . However , for special uses such as stabilizing slime pond dikes where the cost of dewatering might not be a prime requisite , high voltages could be used to rapidly remove the water . Tests of 400 - pound slime charges using a combination of electroosmosis and vacuum filtration showed that the rate of dewatering could be expedited . The average power required to thicken a ton of slime from 15 to 35 percent solids was 5 and 50 kilowatt - hours when operating the electroosmotic filtration cell at potentials of 20 and 100 volts , respectively . calculated filtration area of about 10 square feet per ton of slime treated per day was required to thicken the slime from 15 to 35 percent solids .

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 Louis A. Panek, John A. Stock

A flat slot is created in rock to cause stress relief effects in a pair of hydraulic borehole pressure cells (previously installed in drill holes above and below the slot ) , which act as sensing devices . This relief is annulled by repressuring the slot by means of a flat hydraulic cell . The slot pressure at annulment is taken to be the existing ground stress at right angles to the plane of the slot . A number of trial installations in the rib of a mine drift showed that for a valid determination of ground stress the sensing devices that respond to relief and repressuring must be within a specified zone close to the pressure transmitter ; otherwise the indicated ground stress may be excessive . By using an additional pair of borehole pressure cells , installed a few feet away , the existing rock stress can be redetermined at intervals , irrespective of a change of stress intensity subsequent to the initial installation . Based on these findings , equipment and procedures have been developed that make possible the installation and operation of a permanent rock stress monitoring station for observing mining - induced stress changes . The station consists of a 12 - in - wide hydraulic pressure cell cemented in a flat slot and four 2- by 8 - in flat hydraulic pressure cells in nearby drill holes . All drilling for the installation can be done with an air leg drill and conventional bits . Once the installation is completed , all required information is obtained by Bourdon pressure gage readings . The apparatus is simple , relatively inexpensive , and reliable under operating conditions in a wet mine . Unlike most methods of rock stress determination , this scheme permits periodic remeasurement of absolute rock pressure over several years , without additional drilling or instrumentation . Similar to other flat slot procedures , stress measurements are obtained without making auxiliary tests to determine elastic

Jan 1, 1964

By H. Kato, G. Asai, R. Blickensderfer, R. Siemens

Some relationships were established among crystallographic orientation , rollability , deformation texture , annealing behavior , slip planes , and ductile- brittle bend transition temperature of molybdenum single crystals . Six large molybdenum single crystals obtained from an ingot melted by electron beam were oriented by X - ray diffraction and rolled on crystallographic planes of low indices in a known direction . During room temperature rolling , cleavage occurred on 100 type planes . At 300 ° C the crystals were rolled to 95- percent reduction in thickness . The crystals ( 001 ) [ 110 ] and ( 011 ) [ 100 ] were most easily rolled . Pole figures were used to correlate the deformation textures of the rolled crystals with the initial crystallographic orientation . Several of the textures which developed could be explained as a rotation about a < 110 > axis of symmetry . The cube crystal ( 001 ) [ 100 ] retained much of its " cubic " orientation . The (001 ) [ 110 ] crystal developed the simplest texture , whereas the ( 211 ) [ 113 ] and ( 211 ) [ 120 ] crystals developed the most complex textures . The 1 - hour recrystallization temperature of the crystal ( 211 ) [ 113 ] was 700 ° C , which is about 300 ° C lower than that of commercial polycrystalline molybdenum . The poles of the slip planes ( as determined from gross slip lines at relatively low magnification ) tended to lie within 20 to 60 degrees of the pole of the rolling plane . The Knoop hardness was slightly dependent upon crystallographic orientation but more dependent upon rolling direction . The ductile- brittle bend transition temperature was dependent upon the rolling orientation and the dislocation density .

Jan 1, 1964

By David W. Wisecarver

This report describes a tool to engage and/or place a Bureau of Mines type gage to measure borehole deformation in a horizontal , 1½ - inch - diameter , stress relief borehole . The tool was successfully used at a borehole depth of 105 feet . Practical usage up to borehole depths of 200 feet might be realized . The tool was designed to work inside EX- size ( 1½ - inch ID ) diamond - drill drive casing used as drill rod and through which the deformation gage is guided into an EX- size stress relief borehole . Through laboratory experiments it was found that by exercising a reasonable amount of care the deformation gage could be placed at a point within a ± .01 foot distance of a predetermined depth in a horizontal EX- size hole and that the deformation measuring piston or plunger of the gage could be oriented in the borehole within 0.5 ° of a preselected angle of orientation in a vertical plane .

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 Raymond W. Hiteshue, Sam Friedman, Martin D. Schlesinger

The Bureau of Mines in cooperation with the El Paso Natural Gas Co. investigated the effect of high temperature and pressure at short residence times on the hydrogenation of a New Mexico coal to gaseous and liquid hydrocarbons . The study was made in a bench - scale semicontinuous unit at pressures of 500 to 6,000 psig , 480 ° to 1,000 ° C , and residence times of less than 1 minute to 15 minutes . Ammonium heptamolybdate was impregnated on the coal to furnish 1 percent molybdenum based on maf coal . Coal could be rapidly hydrogenated at elevated temperatures and pressures to yield large quantities of gaseous hydrocarbons and small quantities of lowboiling oils , high in single - ring aromatics . At 800 ° C and 6,000 psig and a residence time of 1 minute , the yield of hydrocarbon gas was 43 percent and of liquid hydrocarbons 9 percent , based on maf coal . With a 15 - minute residence time , the yield of gaseous hydrocarbons increased to 68 percent with a decrease in yield of oil to 6 percent . At higher hydrogen velocities , the yields of oil were much greater but contained large quantities of asphaltene . Low concentrations of molybdenum (0.01 and 0.1 percent ) or a high concentration of iron ( 1 percent ) were ineffective at 800 ° C , 6,000 psig , and short residence time .

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 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 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 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 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 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 Oliver C. Fursman, Lloyd H. Banning

This research was undertaken to determine the feasibility of producing steel from hydrogen - reduced , pyrophoric iron powder . Before steelmaking tests were begun , investigations were made to develop procedures for handling the pyrophoric powder safely , and melting tests were made in a single - phase , electric - arc furnace to determine inert gas requirements for preventing powder oxidation . Steelmaking tests were conducted in a conventional electric - arc furnace , usually by a two - slag basic procedure . Results of the research indicated that ( 1 ) pyrophoric powder can be handled safely and can be prevented from oxidizing excessively during charging and melting in electric - arc steelmaking furnaces ; ( 2 ) little , if any , more electrical energy is required for melting Cerro Bolivar iron powder per unit of contained iron than is required for melting heavy melting scrap ; ( 3 ) high - quality steel can be produced readily from high- grade iron powder , having recoveries up to 95 percent of the total iron ; ( 4 ) steel can be produced from simulated titaniferous , chromiferous , and manganiferous iron powders ; and ( 5 ) the electrical energy required for melting increases with increase in the proportion of slag - forming constituents in the furnace charge .

Jan 1, 1964

By H. R. Babitzke, H. Kato, M. D. Carver

A number of columbium and tantalum alloys were investigated to determine their suitability for use at elevated temperatures . Columbium-vanadium , tantalum-vanadium , and tantalum-hafnium alloys , and also columbium- 10 wt pct titanium alloys modified with additions of 0.1 to 2 mole pct ZrO2 , TiO2 , ZrB₂ , TiB , ZrC, or TiC were prepared and examined . Workability , tensile properties , and oxidation resistance were tested . Of the columbium alloys studied , the columbium- 12 at . pct vanadium exhibited the best properties ; it compared closely with the columbium- 10 at . pct vanadium alloy studied in a previous investigation.

Jan 1, 1964

By Robert M. Becker

This report (the second in a series of five) presents the mathematical development in extending the theory of sample reliability from a sample consisting of a fixed number of items to a sample consisting of a fixed amount of items. Examples of a fixed amount of items per sample are samples consisting of a fixed weight or a fixed volume of unequal size particles. The probability distribution functions (those here called the compound binomial and compound multinomial functions) are developed from fundamentals. Their distributions are generalized to include some measured characteristic of the items. Infinite population moments are derived from moment-generating functions, while finite population moments are developed from corresponding infinite population moments using the finite probability operator defined in part 1 of this series.

Jan 1, 1964