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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, C. W. Houck

Mixtures of zirconium diboride and refractory metals of group VI were resistance sintered to high - density compacts using modified electric welding equipment . To evaluate the use of chromium , molybdenum , or tungsten as binders for zirconium diboride the sintered compacts were examined in polished sections and tested for crushing strength , hardness , microhardness , oxidation rate , and resistance to mechanical shock . Chromium yielded the highest compressive strength , the greatest resistance to mechanical shock and oxidation , and a satisfactory Rockwell hardness . Molybdenum did not yield a satisfactory cermet . Tungsten yielded compacts having high microhardness but very low mechanical strength .

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 V. E. Homme, M. M. Wong

Tests were made in reactors ranging from 12 to 30 inches in diameter to develop methods for the preparation of sodium chloride - titanium lower chlorides ( dichloride and trichloride ) melts that contain titanium predominantly in the divalent state . Such melts are desirable as a starting material for the production of titanium metal or as an electrolyte for electrorefining of titanium . Sodium reduction of TiCl with an 18 - hour period of holding the reaction products in the molten state produced melts that contained titanium lower chlorides in TiCl₂ - to - TiCl , molar ratio of approximately 8 to 1. Sodium reduction of TiCl in a reactor with a shielded pipe weir , that required no melt -holding period , produced melts with a TiCl₂ - toTiCl , molar ratio as low as 4 to 1 . Reduction of TiCl4 with scrap titanium metal in molten sodium chloride produced relatively pure melts containing about 27 percent titanium in a Ticl₂ - to - Ticl , molar ratio of approximately 4 to 1 .

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 Charles C. Myers, Robert M. Doerr

The apparatus described was developed for determining the kinetics of gas - solid reactions at high temperatures by measuring the volume of gas consumed with respect to time . This apparatus consists essentially of a horizontal precision- bore glass tube connecting a small reaction chamber in a furnace to a large constant - temperature reservoir . A drop of mercury in the tube separates the two sides of the system and serves as an indicator that moves at a speed proportional to the rate of gas consumption . The sensitivity of the apparatus depends inversely on both the density of the gas in the system and the cross - sectional area of the tube ; with a tube having an area of 0.079 cm² , the sensitivity for oxygen at 308 ° K and 0.5 atm is 20 cm/mg . The reproducibility of data with the volumetric apparatus is good .

Jan 1, 1964

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 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 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 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 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 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