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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 Vernom F. Swanson, George E. Fish

A study was made during 1959-60 of reported nelsonite occurrences in Nelson and Amherst Counties, Va. The investigation was limited to core drill- ing on one deposit and beneficiation studies on three deposits. Three diamond-drill holes totaling 562 feet were drilled on the E. M. Hughes property to determine subsurface continuity. Although outcrops as much as 30 feet wide were present on this property, the only nelsonite intersected in the holes ranged from 4 to 18 inches thick. The ilmenite content of the core ranged from 50 to 75 percent. These nelsonite deposits are of secondary importance as a source of titanium, being small, rarely exceeding 1,500 feet in length and 30 feet in width, but they are high grade. Due to the proximity of some of the bodies it might be possible to mine several of them as one operation feeding one mill. Electromagnetic separation on composited samples recovered 83.0 percent of the Tio as an ilmenite concentrate in 68.5 percent of the weight. Two flotation procedures were developed. The first method, using oleic acid as a collector and fluo silicic acid as an apatite depressant on deslimed feed, produced an overall recovery of 59.3 percent in batch tests. The second procedure eliminated desliming. Laurylamine hydrochloride removed silicates in an acid pulp followed by an alkaline apatite flotation with oleic acid as the collector and dextrine as the ilmenite depressant. The ilmenite-rich tailing represented a 66.2-percent recovery of Tio in the batch tests.

Jan 1, 1964

By Edward Cogan

Equilibrium phase diagram studies of zirconium- rare earth metal alloys by the Bureau of Mines at its Albany Metallurgy Research Center prompted the development of a rapid gravimetric method for determining rare earths in zirconium in which the rare earths are absorbed from sulfuric acid solution of the alloy on a cation exchange resin . The sample in 10 percent H2SO4 is introduced into the column , the zirconium is eluted with 10 percent H2SO4 , and the rare earths are eluted with (NH4 )2SO4 solution and precipitated with NH4OH . A tracer technique was employed to determine the efficiency of the procedure . Y203 and europium 154 - 152 (Oak Ridge ) were added to 10 g of zirconium and taken through the entire procedure . Recovery averaged 97.6 percent on 0.002 μg europium in the rare earth fraction . Rare earths were determined in the range 0.10 to 90 percent .

Jan 1, 1964

By Paul W. Johnson, Ralph C. Kirby, Frank A. Peters

Alumina can be recovered from clay , using 30 percent nitric acid for digestion . Calcined clay is crushed and then digested at 325 ° F and 85 psig pressure with less than stoichiometric nitric acid required to form normal aluminum nitrate . In this way , a solution containing both normal aluminum nitrate , Al ( NO3 ) 3 , and basic aluminum nitrate , assumed to be Al ( OH ) ( NO3 ) 2 , is formed , and in which iron is virtually insoluble . The solution is filtered and then concentrated in vacuum evaporators to crystallize normal aluminum nonahydrate . The crystals are washed with 50 percent nitric acid and then decomposed to alumina and nitrogen oxides . The design that has been developed for this process is based on published work . For a plant producing 1,000 tons of alumina a day , the estimated operating cost is $60.69 per ton of alumina , and the estimated fixed capital cost is $ 76 million using a Marshall and Stevens chemical equipment index basis of 240.0 . This process is not competitive under current economic conditions with the production of alumina from bauxite via the Bayer process . For lowering costs , future research should include study of leaching at lower temperatures under atmospheric pressure and alternate aluminum nitrate decomposition methods .

Jan 1, 1964

By Oliver Q. Leone

Three electrorefining cells were designed to investigate various factors associated with the electrorefining of reject - grade titanium sponge . Operation of the cells provided information on cell design as well as on how design and operating variables affected the quality of the titanium product . A sodium chloride - titanium chloride electrolyte was used , and the electrolyte chambers had capacities ranging from 400 to 3,500 pounds of molten salt . Major factors investigated were electrolyte composition , temperature and useful life , effect of various cathode shapes and materials of construction , methods for removing cathode deposits , effect of current density and cell potential , and the mechanics of deposit growth and crystal morphology . One of the cells was in intermittent operation over a 4 - year period and produced 2 tons of refined titanium . A product with a hardness of 80 or less Bhn (Brinell hardness number ) was consistently and easily obtained . Some metal with a hardness of less than 60 Bhn was produced . In one of the cells in which the electrolyte was held at operating temperature with an internal heater an ac input of 25 kw maintained 3,500 pounds of electrolyte at 850 ° C , but with an external heater 35 kw was required to maintain 400 pounds at 850° C.

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 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, D. C. Fleck, D. G. Kesterke

Uranium metal was electrowon from uranium dioxide dissolved in fluoride melts . The UO₂ was fed directly to the cell in a continuous manner . Electrolysis was performed at 1 , 200 ° to 1,300 ° C in electrolytes composed of UF4 , LiF , and BaFa . A single regulus of metal was collected in a confined area of the crucible . Product purity of 99.8 percent was attained . Carbon was the major contaminant . Compartmented cells were studied as a means of confining the oxide feed to the vicinity of the anodes .

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 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 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