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By C. A. Pearson, W. D. Dietzman, M. E. Hawkins

Results of chemical analyses and electrical resistivity measurements of 422 samples of oilfield brines from 120 east Texas fields in Railroad Commission of Texas Districts 5 and 6 are presented in tabular form . These samples represent water from all of the major petroleum- productive formations in the area . Water analyses and electrical resistivity data , when fully utilized by proper study techniques , are useful tools in the solution of many engineering problems such as detection of well leaks , identification of water sources , and interpretation of electrical well logs . In the area included in this study , these representative data should facilitate the solution of problems in which water analysis and water resistivity are factors .

Jan 1, 1964

By Joseph A. Sutton, John D. Corrick

The chemistry involved in the microbial dissolution of iron and copper from such sulfide minerals as pyrite, chalcopyrite, chalcocite, cove11ite, and bornite is described. The chemical criteria used to evaluate the activity of microorganisms on these minerals were changes in pH, ferric iron produced, and oxygen consumption. In a series of experiments in which a ferrous sulfate nutrient solution was percolated over small portions of the above-mentioned copper sulfide minerals for 56 days, the iron-oxidizing bacteria Ferrobaci11us ferrooxidans and Thiobaci11us ferrooxidans were capable of bringing about the dissolution of 23.7 percent of the copper from chalcocite, 56.3 percent of the copper from cove11ite, and 29.8 percent of the copper from bornite by the microbial production of ferric sulfate which reacted with these minerals. Laboratory tests have demonstrated that pure strains of the iron-oxidizing bacteria act as catalysts to the ferrous iron being oxidized by the Oxygen of a system containing pyrite and chalcopyrite. In a series of experiments during which nutrient solution was percolated over pyrite for 70 days, the ferric iron produced by the iron-oxidizing bacteria was 112 to 120 times greater than that produced atmospherically.

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Paul Dobransky, Robert Madden

A hvab coal was carbonized in a closed system at 600 ° C and 40 to 1 , 200 psig to produce a high- Btu gas and char . By retaining the volatiles within the system, it was possible to virtually eliminate production of tars and oils . Depending on pressure and residence time , yields of combustible gases (72 to 92 percent methane ) amounted to 4,000 to 6,000 cubic feet per ton of maf coal and gross heating values of these gases varied from 830 to 960 Btu per cubic foot . Yields of char (maf ) were about 1,600 pounds per ton of maf coal . Increased residence time favored production of gases but reduced their heating values , whereas increase in pressure resulted in somewhat higher heating values and lower production . Similar effects were observed from the carbonization of a low- temperature tar . If these results could be translated to an economical carbonization process for producing high- Btu gas from coal , the demand for coal could be expanded by 40 to 50 million tons per year . Because of large yields of char , a process of this type would obviously have to be integrated with coal - fired power plants . Fortunately , operations could be conducted at essentially atmospheric pressure as product gas under this condition can be obtained in satisfactory yields and with good quality .

Jan 1, 1964

By W. P. Haynes, A. J. Youngblood, J. J. Demeter

Synthesis of high - Btu gas , using the Fischer - Tropsch reaction was investigated in a tube - wall reactor of 2 - inch steel . The catalyst was carbonexpanded iron ( CEI ) , formed on the walls of a steel reactor by exposing the reactor to 1H₂ + 100 synthesis gas under certain conditions . Advantages to be gained from successful development of the CEI - coated tube- wall reactor are elimination of catalyst plant and catalyst handling and charging operations , high- temperature operation , and a relatively low- cost , reactor -heat recovery system . In one test ( TW- 8 ) in which the reactor was filled with CEI , the reactor was operated for 1,910 hours before the test was stopped because of excessive pressure drop caused by carbon deposition . The pressure drop was satisfactory for 1,000 hours of operation at an hourly space velocity of 300 , but it increased rapidly at space velocities of 600 and 1,000 . When operated at a space velocity of 300 , with a ratio of 1 to 1 recycle at 534 ° C , a conversion of 72 percent of the 3H + 100 synthesis gas was achieved . The product gas had a heating value of about 610 Btu per cubic foot and could be suitably upgraded to 900 - Btu gas by subsequent use of a nickel catalyst . CEI did not operate effectively as a film catalyst under conditions of generation tried in this study . Generally , operation of the 2 - inch reactor with CEI catalyst was unsatisfactory because of poor reproducibility of the activation step and poor temperature control resulting in high- operating temperatures and eventual plugging of the reactor . Tests using CEI in fixed , packed beds suggest that the most likely application for CEI in producing high - Btu gas would be a moving - bed reactor , where sufficient bed movement and heat removal are provided to prevent plugging .

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 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 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 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 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 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 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