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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 T. Estelle Gardner, A. R. Taylor

Heat capacity measurements were made on sodium bromide ( NaBr ) and sodium iodide ( NaI) in the temperature ranges of 7 ° to 300 ° K and 56 ° to 300 ° K using an adiabatic calorimeter . Smooth values of heat capacity, entropy , enthalpy function , and free- energy function were calculated from the heat capacity data at 10° K intervals and at 273.15° and 298.15° K. Entropy and free energy of formation values at 298.15° K also were calculated for the two compounds using entropy values determined in this study and other data reported in the literature . The entropy values calculated at 298.15 ° K were 20.75 ± 0.06 entropy units (eu ) for sodium bromide and 23.55 ± 0.07 eu for sodium iodide .

Jan 1, 1964

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

Electrolytic studies were conducted to determine the transfer rates of the alloying constituents from molten titanium anodes to solid titanium cathodes in molten salt systems . The metals , nickel , tin , copper , bismuth , and manganese , were selected on the basis of thermodynamic data and the melting point of the alloy system . The transfer of nickel , tin , and bismuth was very low . The content of these elements in the cathode was in the range of less than 0.01 to 0.001 percent . The copper transfer was 0.6 to 0.8 weight - percent in electrolytes containing titanium chlorides and 0.12 weight - percent in titanium fluoride salt systems . The manganese transferred at rates comparable to that of titanium . Highpurity titanium and titanium- manganese alloys of uniform composition were produced by electrorefining molten titanium alloys in chloride electrolytes . Comparisons are made between the calculated and the actual quantities of metal transfer .

Jan 1, 1964

By D. A. Elkins

Design plans and detailed cost estimates of mining and treating ore from Maggie Canyon deposit by two alternative methods which can be used in the event of a sudden need to exploit this resource are given . Lower costs are estimated for the operation employing oil - emulsion flotation . The total capital investment required for this operation is estimated at $ 11,750,000 . Assuming an 85 percent recovery in mining , 55.6 pct of the manganese in the ore reserve would report in 153,333 tons of ferromanganese containing 75 pct manganese . The production cost for the 5 - year operation would be about $ 245 per ton of ferromanganese . The total annual operating cost would be approximately $ 7.5 million , distributed , in pct , as follows : Mining 11.9 , milling 24.4 , sintering 9.9 , smelting 47.2 , hauling ore and sinter 2.8 , and general offices 3.8 . Recovery and costs are both higher for the operation employing dithionate leaching . In this operation the required investment is about $ 17,220,000 . Manganese recovery would be 67.6 pct in 186,160 tons of ferromanganese . Production cost would be about $ 284 per ton of ferromanganese . The total annual operating cost would be about $ 10,575,000 , distributed , in pct , as follows : Mining 8.4 , milling 44.4 , sintering 7.4 , smelting 34.7 , hauling ore and sinter 1.3 , and general offices 3.8 . Potential process modifications might reduce the operating cost of the first operation by as much as 7 pct and that of the second operation by as much as 9.5 pct , but exploitation of the deposit by the techniques studied is not economical today .

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 D. E. Redmon

Linear programing provides a mathematical technique by which activities can be planned in such a way that an optimal result is obtained. Routine applications of linear programing require only a knowledge of algebra. However, a complete understanding of the fundamentals of linear programing requires a knowledge of advanced mathematics. The purpose of this publication is clarification of terminology and illustration of applications in comparatively simple mining problems. Two mining situations are considered: Mine stopes from which ore is to be produced at a minimum production cost; also, uranium mines from which ore is transported to one mill, a maximum monetary value is desired. The details of data arrangement for solution by linear programing are described and the solutions are presented. Results of these solutions indicate successful applications of linear programing to mine production scheduling.

Jan 1, 1964

By H. R. Shell, John L. Miller, M. V. Denny

In the mica research program conducted by the Bureau of Mines at Norris , Tenn . , many micas other than silicon fluorphlogopite have been synthesized . It has been well established since the initiation of the program that synthetic micas are important materials useful for their superior or unique properties as well as substitutes for natural micas . The possibility of controlling the physical properties of synthetic mica by isomorphic substitution of other ions in the fluorphlogopite lattice further emphasizes the importance of these materials . Accurate measurement and reporting of their properties constitute an essential part of the research program . The study of germanium fluorphlogopite is in keeping with the requirements of a comprehensive study on isomorphic substitution , specifically to identify precisely the material -- chemically , structurally , and optically . The X- ray measurements , including indexed powder and single crystal data , with a description of the methods used to obtain these data , are provided . 5 Earlier work on germanium mica by R. A. Hatch et al . (5) gave an estimate of the cell parameters from X - ray powder data , but no attempt was made to index the diffraction pattern or to determine the space group symmetry . Later work by E. A. Schatz and J. C. Withers (9) listed X- ray and optical measurements , but no attempt was made to index the mica or determine its symmetry . Roth (7) found that germanium dioxide having the a - quartz structure , when heated with equimolar percentages of MgO , CaO , Sr0 , or Ba0 at 1,235 ° C , formed ABO3 -type compounds , e.g. MgGe03 isostructural with enstatite (MgSiO3 ) . Geo₂ also has a rutile - type polymorph with Ge ++ ions in octahedral coordination . Germanium was substituted for silicon in the serpentine structure by Roy and Roy (8 ) using hydrothermal techniques . These authors wrote as follows : "The substitution of Ge + for Si + yielded a magnesia - germania serpentine , formed easily in euhedral hexagonal plates which in some instances were visible in the light microscope . Electron micrographs and the sharp X - ray diffraction patterns confirm a plate - like rather than tubular habit . " It has been shown in this investigation that substitution of germanium for silicon in the mica structure is readily accomplished without radically changing the characteristics of the mica . Substitutions in the mica structure take place in three locations : Tetrahedral , octahedral , and interlayer positions . The tetrahedral positions are normally occupied by Sit or by a combination of Sit with Al +3 the most common combination being 2A1 +3 and 6Si +4 · , The octahedral position , which has six - fold coordination in phlogopite , contains a larger cation such as magnesium . In muscovite it contains only 2A1 ions ; therefore , this mica is considered a dioctahedral mica , whereas phlogopite is considered trioctahedral . +3 The interlayer position has twelve - fold coordination with six oxygen ions from each of two adjacent tetrahedral silica layers . This is the cleavage plane of the mica and commonly contains the largest cation in the mica structure (e.g. potassium) .

Jan 1, 1964

By D. W. Bridges, Donald R. Peterson, Masami Hayashi

Techniques are described for recovering about 80 pct of the cobalt and nickel contained in superalloy scrap by anodic dissolution of the scrap and simultaneous electrodeposition of a pure cobalt - nickel alloy at the cathodes in an electrolytic cell partitioned by permeable diaphragms into separate anode and cathode compartments . Superalloy scrap was alternatively prepared for subsequent anodic dissolution either by melting and casting massive scrap into suitably sized anodes , by packing moderate - sized discard scrap in inert metal baskets that subsequently served as anodes , or after concentrating the superalloy portion of grinding debris , by magnetic separation to reject corundum or other abrasives , slagging any remaining abrasives from molten grindings , and finally casting the superalloy metal into anodes . In the processing , purified electrolyte -- 1 N in NiSO4 and in NiCl₂ , and 0.1 N in CoSO4 and in CoCl2 --was charged to the cathode compartments and discharged from the anode compartments at a rate sufficient to overcome the backward migration of ionic impurities from the anodes to the cathodes . Discharged electrolyte was purified by reacting it first with SO2 and next with limestone , and then recirculated to the cathode compartments , in which a 50 pct cobalt - 50 pct nickel alloy was deposited on either blanks of stainless steel or starting sheets of cobalt - nickel alloy . The process was made self - sustaining by either adding H2SO4 to the catholyte feed to throttle the rate of cobalt - nickel deposition , thereby compensating for the slower rate of cobalt - nickel dissolution from the anode and losses occurring in electrolyte purification , or alternatively , adding H₂SO4 to

Jan 1, 1964

By K. K. Kelley, L. B. Pankratz, W. W. Weller

The heat capacity of columbium (niobium) carbide (CbC ) was measured over the temperature range from 51 ° to 298 ° K, and the entropy at 298.15° K was evaluated . Also , the heat content above 298.15 ° K of columbium carbide was measured to 1,800 ° K. The results were combined with the known heat of formation at 298.15 ° K to obtain values of the heat and free energy of formation over the temperature range from 298.15 ° K to 2,000 ° K.

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 G. V. Sullivan, G. F. Workentine

Beneficiation studies were conducted by the Bureau of Mines on three samples of low- grade chromite - bearing material from the Stillwater complex of Montana . The objective of the study was to develop methods for recovering chromite from low- grade materials to improve the domestic reserve situation . Samples were obtained from the three largest deposits in the district , Mouat , Benbow , and Gish . The chromic oxide ( Cr₂ 0 ) content of the ore and of the chromite was about the same in each of the samples . The major gangue constituents ranged from clean olivine in the Mouat sample to such altered minerals as serpentine and talc in the Benbow and Gish samples . Tabling , flotation , high- tension electrostatic separation , and combinations of processes were applied to each ore . Treatment of the Mouat sample ( 9.95 percent Cr₂ 0 ) by high- tension electrostatic separation , a combination of tabling and high- tension electrostatic separation , and tabling with middling retreatment resulted in concentrates that graded 42.8 , 42.0 , and 40.7 percent Cr₂03 at chromium recoveries of 85 , 86 , and 84 percent , respectively . Other techniques were less selective . 2 The Benbow sample ( 7.75 percent Cr₂0 ) responded most selectively to tabling with middling retreatment and a combination of tabling and hightension electrostatic separation to produce concentrates of 40.1 and 39.5 percent Cr₂g with each process having a chromium 2 recovery of 69 percent . Response of the Gish sample ( 8.04 percent Cr₂03 ) to the various concentration techniques was about the same as that of the Benbow sample , but in general , somewhat less selective . A combination of tabling and high- tension electrostatic separation resulted in a concentrate that contained 71 percent The Mouat mine was reopened in 1953 when the American Chrome Co. contracted with the Federal Government to produce 900,000 tons of chromite concentrate . The ore , averaging 20.2 percent Cr₂03 , was treated by tabling to produce a 38.5 - percent Cr₂ O concentrate.

Jan 1, 1964

By J. J. Pfeiffer, J. W. Myers, A. A. Orning

A study was made of the feasibility of using washery refuse in the manufacture of lightweight aggregate for building materials . Preliminary caking and burning tests showed that the refuse could be converted into lightweight aggregate but that refuse passing a No. 14 U.S. Standard screen could not be used without additional processing . The aggregate was prepared by pelletizing the refuse and burning out the carbonaceous material on a chain- grate in a refractory - lined furnace . A small stationary - grate furnace was used to study the process variables involved and establish optimum ignition and combustion conditions . Maximum ignition rates were obtained at air rates of approximately 200 lb per sq ft hr , but air rates of 450 or higher were required in the burnout period to obtain temperatures high enough to sinter the ash . The data obtained from this unit were used as a guide in the operation of the chain- grate furnace . In the chain - grate furnace , satisfactory results were obtained by using primary air rates of 200 lb per sq ft hr in the ignition zone and 500 lb per sq ft hr in the burnout zone . The ignition- zone air was preheated to 500 ° F , but the air for burnout was not preheated . A total of 2-1/2 tons of aggregate was prepared in this unit and made into experimental block . A commercial development based upon the results of this study yielded a product which met the ASTM specifications C 130-42 for lightweight aggregate , and blocks made from the aggregate were of good color , durable , and light - inweight .

Jan 1, 1964

By R. T. DeWoody, W. C. Miller, W. Chester

Studies were made to determine the effect of the shape of a pneumaticrock- drill exhaust muffler on its efficiency, and the origin and reduction of exit noise from the mufflers. Tests of mufflers of three different shapes proved that the shape is not critical and that a muffler could be incorporated into the shell of the drill. Petal diffusers are beneficial in reducing exit noise but add another projection to the machine. Increasing the number of exit openings while maintaining the same area of exit opening has a markedly beneficial effect on the exit noise and appears to be the most satisfactory treatment.

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 E. G. Davis, H. P. LeVan, L. S. Smith

Leaching of a Georgia umber ore when using both ferrous sulfate and pickle liquor was studied in the laboratory . The ferrous sulfate content of the leach solution was the major factor affecting the extraction of manganese from the ore . Time , temperature , and the sulfuric acid content of the leach solutions had relatively little effect on leaching of manganese from the ore ; however , these factors did affect the amount of iron extracted from the umber and/or precipitated from solution . Simulated countercurrent leaching of the ore with pickle liquor containing 130 gpl (grams per liter ) ferrous sulfate ( 48 gpl ferrous iron ) produced a pregnant solution having 16 gpl manganese and 41 gpl iron . Filtration tests of the leach slurries indicated that separating the leach solution and solids by vacuum filtration was impractical , whereas pressure filtration was feasible when the cake thickness was limited to about three- fourths of an inch . Fired pellets of the filter cake yielded a firm , hard product analyzing 56 percent iron and less than 0.1 percent sulfur .

Jan 1, 1964

By David Schlain, C. B. Kenahan, F. X. McCawley

The electrodeposition of protective coatings of tungsten from a sodium and lithium borate - tungstate - tungstic oxide fused salt electrolyte was investigated . Soluble tungsten anodes were employed . Deposits were made on molybdenum , Carpenter 20 stainless steel , Inconel , and nickel . An atmosphere of argon was maintained around the electrolytic cell , and the electrolyte was stirred by rotating the cathode . Thick deposits of tungsten (up to 26 mils ) were made at a temperature of 900 ° C and cathode current densities of 0.3 to 0.4 ampere per square inch with high current efficiencies . The effects of variations in temperature , current density , electrolyte agitation , and tungstic oxide content of the electrolyte and of the presence of impurities such as moisture , air , iron , and nickel were investigated .

Jan 1, 1964

By Sabri Ergun, Robert W. Smith, Victor H. Tiensuu

Factual geometries are considered for X- ray scattering studies of weakly absorbing materials by both reflection and transmission methods . These studies are usually made on slab specimens to obtain adequate scattered intensities ; however , the intensities are appreciably influenced by absorption of the X-rays in passing through the specimens . Conventional equations derived to account for this absorption are based on idealized geometries , but for polycrystalline carbons the use of idealized geometries leads to several percent error in the corrections to be made . Use of factual geometries substantially reduces this error .

Jan 1, 1964

By F. E. Block, T. T. Campbell, D. Z. Hobbs

Several methods were investigated for the preparation of high- purity elemental boron in an attempt to develop a feasible process for producing boron on a large scale . In the work described in this report , the metal was prepared by metering boron trichloride gas into a crucible containing molten metal reductants . It was necessary to remove reaction byproducts by acid and aqueous leaching . Magnesium and sodium were tested as reductants , but best results were achieved using lithium or zinc as reductants . Contaminants originating from the materials of construction were the chief impurities in boron made by this method . Impurities ranged from 0.5 to 5.0 percent . Impure boron ( 85 to 90 percent ) was also prepared by the magnesium reduction of boron trioxide in a thermite - type reaction . This product contained magnesium as the chief contaminant . Impure boron made in this way could be upgraded by fusing with potassium fluoborate or potassium acid fluoride . After acid leaching the fusion cake , a product containing 95 to 97 percent boron was obtained . Analytical techniques for accurate determination of impurities in elemental boron are a major problem , requiring solution before a valid comparison can be made of the quality of boron prepared by these various methods .

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 R. L. Hopkins, H. T. Rall, H. J. Coleman, C. J. Thompson

Two methods were tested for separating sulfur compounds in certain petroleum fractions into types . Such separation is preliminary to identifying the compounds . Each method involved extraction of sulfides from petroleum sulfur concentrates . In the first method , the sulfur concentrate was reacted with methyl - ptoluenesulfonate to form sulfonium compounds from which unreacted portions of the sample were removed by washing with solvent . The sulfides then were recovered by heating the sulfonium compounds with anhydrous triethanolamine . The second method consisted of passing anhydrous hydrogen iodide into a n-butane solution of the sample cooled in dry ice , whereupon the hydrogen iodide adducted with the sulfides to form sulfonium compounds . These adducts separated as crystalline solids or , more frequently , as glassy viscous liquids . The sulfide was regenerated by adding water to the filtered sulfonium compound and was recovered by steam distillation or by extraction with pentane . These methods have been evaluated , using individual pure sulfur compounds and blends of sulfur compounds . They also have been applied successfully to separating sulfides from sulfur concentrates derived from petroleum fractions .

Jan 1, 1964