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By J. C. Meeks, C. L. Klingman

An instrument that is sensitive , portable , safe , and low in cost was developed by the Bureau of Mines for detecting helium leaks by comparing the thermal conductivity and flow rate of the atmosphere around the suspected leak against a reference of helium- free air . A vacuum pump pulls the sample gas through a restriction and over thermistor elements , the combined electrical output of which is affected by thermal conductivity and flow rate of the sample gas . Tests showed that the battery - operated Helium Leak Detector was effective and rugged instrument that could be operated safely in explosive atmospheres . The instrument could also detect , but not identify , other gases such as methane , hydrogen , argon , carbon dioxide , and Freon 12 .

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 John Nagy, Austin R. Cooper

Information is presented on the pressure and rate of pressure development during a dust explosion . The data were obtained in laboratory studies in a 75- cubic inch vessel with mineral , agricultural and chemical dusts . The factors investigated include dust concentration , oxygen concentration of the atmosphere , admixed inert powder , and admixed moisture . Information is given also on the effects of these factors on the composition of the atmosphere after the explosion .

Jan 1, 1964

By R. W. Hiteshue, C. O. Hawk, H. H. Ginsberg, M. D. Schlesinger

The Bureau of Mines studied single - step catalytic vapor - phase hydrogenation of oils derived from coal and oil shale . Treatment of middle oil , from hydrogenation of bituminous coal , gave good yields of gasoline with a German - made molybdenum- zinc - chromium catalyst . The Bureau also achieved good results with duplicates of this catalyst made from domestic raw materials . In one set of experiments with the German catalyst , 38 to 52 wt pct of feed was converted to gasoline . The total liquid product was 91 to 98 wt pct of the feed . Not all this gasoline can be claimed as production , however , because about 20 pct of the feed was in the gasoline range , and part of it undoubtedly survived the hydrocracking treatment . Hydrogenation of crude shale oil in the presence of cobalt molybdate catalyst produced a total liquid product of 89 wt pct of feed . The hydrogenation converted 27 wt pct of feed to gasoline and 44 wt pct of feed to diesel fuel . The remaining liquid product , 18 wt pct of feed , was residue boiling above diesel fuel . The gasoline was of poor quality , with an octane number of 39.1 . The overall product seemed a suitable feed stock for a conventional refining operation . Coker distillate hydrogenation , using a cobalt molybdate catalyst , gave a total liquid product of 97 vol pct of feed ; of this product 60 vol pct was jet fuel and 40 vol pct was diesel fuel . High nitrogen and sulfur in all three of these raw materials severely poison the usual refining catalysts . Thus , the common objective in these

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 G. W. Birge, D. E. Wolfson, J. G. Walters

Seventeen samples were carbonized by the BM -AGA pilot - plant test method and in industrial ovens . Chemical and physical properties of the samples were determined , and the physical properties of the cokes prepared by the two methods were compared . Since the capacity of the plants from which these samples were obtained is about 30 percent of the 1959 total for the United States , the data given in this report are indicative of the chemical and physical properties of blends used to produce industrial cokes and the acceptable chemical and physical properties of the resultant coke .

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 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 W. L. Falke

Research was conducted to develop methods on a laboratory scale for recovering manganese from manganiferous slimes and limestones . The procedure is a low- temperature modification of the carbamate process , in which manganese is dissolved and the valence reduced by treating slimes and limestones with controlled amounts of sulfurous acid . Manganese ( II) hydroxide is precipitated and leached with ammonium carbamate solution , and manganese carbonate is separated by warming the leach solution . A major portion of the reagents is regenerated and recirculated . About 75 percent of the total manganese in manganiferous slimes , and from 50 to 75 percent of the total manganese in manganiferous limestones , are recovered as manganese carbonate containing 45 percent manganese .

Jan 1, 1964

By F. R. Cattoir, R. E. Cumings

Columbium metal was electrorefined in a fused - salt electrolyte . Excellent results were obtained in lowering the impurity content in a 94 - percent columbium anode feed material to produce a 99.8- percent - pure metal . The reductions of the major impurities follow : Oxygen from 19,800 to 500 ppm , carbon from 9,700 to 25 ppm , iron from 9,200 to 630 ppm , nitrogen from 2,100 to 90 ppm , and silicon from 750 ppm to not detected . Columbium with a purity of 99.9 percent was produced from 99.5- and 99.8 - percent grades of columbium. The investigation was devoted to the evaluation of a fused - fluoride - salt electrolyte ( KF - NaF- K₂ CbF, ) for electrorefining columbium. The effects of the columbium concentration and the voltage upon the product's purity were investigated . The effect on the cathode current efficiency of ampere - hours of deposition and the formation of a dual valence state of the columbium was also investigated .

Jan 1, 1964

By D. J. Donaven, Manuel Gomez, W. S. Landers

Bulk density tests were made on a Western U.S. coke oven plant blend to obtain bulk density control data that would be directly transferable to plant practice . Maximum bulk density values were obtained at zero surface moisture . Increase in surface moisture to about 6 percent decreased the bulk density to a minimum value . Increase in the fine grinding of the blend , at constant surface moisture , decreased the bulk density . The effect of oil on bulk density was observed with five oils at concentrations ranging from 1/8 to 1-1 / 2 gallons per ton . Maximum bulk densities were obtained within the 1 / 2- to 1 - gallon - per - ton range . Essentially the same bulk densities were obtained with petrolatum- and nonpetrolatum- containing oils . Storage effects were observed on samples tested at selected intervals from 0 to 56 days . No significant change in bulk density took place if no surface moisture was lost during storage .

Jan 1, 1964

By C. E. Wicks, J. E. Tress, F. E. Block

The Bureau of Mines investigated the effects of gamma radiation on materials and chemical reactions to obtain information that could be of value in modern metallurgical practices . Various combinations of metals and their ores and compounds were irradiated in attempts to effect reactions that might be applicable in the extraction and separation of metal values from minerals and The types of reactions studied included complexing of salts , decomposition of hydrated salts , metal chlorination reactions , leaching of ores and minerals , halogen exchange , and various reducing reactions . All irradiations were performed at the Materials Testing Reactor Gamma Facility of the U.S. Atomic Energy Commission at Idaho Falls , Idaho . Spent fuel elements were utilized as the source of the gamma radiation . Some irradiation - induced changes , ranging from mere color change to participation in chemical reactions , were noted . The greatest value of these investigations , however , was the experience acquired , which should be valuable in future explorations of similar nature .

Jan 1, 1964

By Oren C. Baptist, Carlon S. Land, Eliot J. White

The water sensitivity of the oil - gas - producing sandstones in three fields in the Patrick Draw area of southwestern Wyoming was estimated by laboratory testing . The tests used to estimate sensitivity , which is a measure of the loss of well productivity if the producing formation is invaded by fresh water , are : Porosity ; permeability to gas , water , and brines ; saturation characteristics with air displacing water from the samples and by mercury injection ; and identification of clay minerals by X - ray diffraction . Laboratory results indicate that the degree of water sensitivity of the sands in the Patrick Draw, Table Rock , and Desert Springs fields vary , in that order , from moderately sensitive to highly sensitive . The main cause of the sensitivity appears to be the movement of fine particles in the pores , but the swelling of a small amount of an expandible clay mineral may also contribute to the permeability reduction observed in the samples . Laboratory results further indicate that the permeability of the sands to fresh water is seriously reduced if they are first flushed with sodium chloride brine ; calcium chloride brine is less harmful to the sands than sodium chloride brine . The low original permeability of the oil sand in the Patrick Draw field , together with its moderate sensitivity , indicate that the rate of water injection for the secondary recovery of oil will be low . Limited field experience in two pilot - injection wells confirms this prediction .

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 R. V. Lundquist, H. Leitch

Sodium aluminate is the principal aluminum compound formed in the sinters prepared by the lime - soda sinter process for recovering aluminum from silicate source materials . The properties and characteristics of this compound were studied to improve the efficiency of the process . Crystalline sodium aluminate was prepared by sintering stoichiometric quantities of soda ash and calcined alumina for 1 hour at 1,250 ° C. The extent of aluminum extraction from sodium aluminate was determined in water and in solutions of NaOH and Na₂ CO3 . Nearly complete extraction of aluminum from sodium aluminate was achieved only in solutions containing free NaOH in excess of that supplied by the salt through hydrolysis . About 42.2 to 68.8 percent of the aluminum was extracted in water or in solutions of Na₂ CO . The precipitation of alumina trihydrate from sodium aluminate solutions was shown to be part of a continuous , reversible reaction according to the equation Al (OH ) A1 (OH )3 + OHThe reverse reaction dissolves alumina trihydrate in NaOH solutions to produce sodium aluminate . Approximate equilibrium concentrations were determined for the reaction at 30° , 50 ° , and 70 ° C. False apparent equilibrium conditions for the dissolution reaction appear when only a small excess of alumina trihydrate is present in the NaOH solutions . A large excess of alumina trihydrate must be present before the true equilibrium point is assured . The engineering significance of the data is summarized , showing controls that should be exercised for a successful and efficient process .

Jan 1, 1964

By Scott W. Hazen

This report presents the results of a statistical analysis of a limited amount of sample and assay data from a production panel in an open - pit phosphate mine in the Phosphoria formation in Idaho . A frequency distribution analysis is shown for the assays , sample interval lengths , and products of assay and sample interval length for the millshale , furnace - shale , and main phosphate beds . Correlation techniques were used to show the relationships between assays and sample interval lengths . Within- drill - hole and between - drill - hole correlation were also examined as a means of predicting grade trends in the ore . Simulation methods , utilizing a digital computer , were used to establish assay populations that could be used for estimating grade of ore , cutoff grades , and deposit or bed identification .

Jan 1, 1964

By K. A. Fowler, L. W. Higley

The effect of uranium on the transformation kinetics and the hardenability of a low- alloy steel was evaluated . Isothermal transformation curves were developed from metallographic studies , and hardenability was determined by standard Jominy end- quench tests . For the steels investigated , the addition of 0.15 weight- percent uranium was found to produce a significant shift in the isothermal transformation curve and caused a related increase in hardenability . These effects diminished rapidly when the uranium content was increased above 0.2 weight - percent .

Jan 1, 1964

By George H. Holmes

Beryllium deposits in the northern Virgin Mountains , Clark County , Nev . , and Mohave County , Ariz . , about 70 miles northeast of Las Vegas , were investigated by the Bureau of Mines . The investigation indicated a widespread occurrence of beryllium- bearing pegmatites within an extensive belt of mica - schist . Several deposits with significant beryllium mineral concentrations were encountered . Only a few of the samples analyzed contained more than 1 percent beryllium oxide ( BeO ) ; in many of the samples , no beryllium was reported . The average tenor of samples from the more important occurrences was 0.25 percent BeO . Chrysoberyl is the predominant beryllium mineral in the pegmatite sills ; beryl predominates in the more massive bodies . Minute quantities of cesium and lithium minerals also occur , but no columbium , tantalum , or other rare minerals were found . Ore dressing tests on a composite sample containing 0.28 percent BeO which was representative of the pegmatite sills , indicated an 85 percent recovery of the chrysoberyl ( 70 percent recovery of total BeO ) by gravity concentration in a concentrate containing 17.6 percent BeO .

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 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