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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

By W. A. Stickney, J. W. Town

Studies on continuous - circuit leach - aluminum precipitation and leachelectrodeposition of mercury were made by the Bureau of Mines to determine optimum conditions and cost estimates for recovering mercury from mercury sulfide flotation concentrates . With 150 grams of sodium sulfide and 50 grams of sodium hydroxide per liter , from 98 to 99.8 percent of the mercury was extracted from flotation concentrates , with about 0.5 pound of sodium hydroxide used per pound of mercury produced . Precipitation of mercury from the caustic - sulfide solution with minus 8 - mesh aluminum shot required about 0.2 pound of aluminum per pound of mercury produced at a cost of $ 0.05 per pound of mercury . Electrodeposition cost with 7 mill power , based on 50 percent current efficiency , was below 2 mills per pound of metal deposited . Feed solutions ranged from 10 to 130 grams of mercury per liter , and current densities , from 2 to 70 amperes per square foot . The cost of open- pit mining 250 tons per day was estimated at $ 1.75 per ton , and flotation - leachingelectrodeposition of the ore , at $ 3.54 , resulting in a cutoff grade of about 0.1 percent mercury . The cost of underground mining 50 tons per day was estimated at $ 20.00 per ton , and the cost of milling the ore was estimated at $ 13.33 , which resulted in a cutoff grade of 0.6 percent mercury .

Jan 1, 1964

By James A. Wasson, Harry R. Johnson, Dean W. Boley

The Cow Run sand was cored and electrical and radioactivity surveys were made in C. E. Vandevender well 35 in the Burning Springs pool of the Burning Springs oilfield , Wirt County , W. Va . Laboratory tests , reservoir - fluid analysis , well - log interpretation , and available field data indicate that a substantial quantity of oil may be recovered from this pressure - depleted reservoir by waterflooding . Two formations erroneously believed to be the First and Second Cow Run sands were similarly evaluated in A. E. Mackintosh well 8 , Anns Run Pool , Wirt County , W. Va . , but were found unsuitable for secondary - recovery operations .

Jan 1, 1964

By F. E. Walker, S. J. Aresco, J. B. Janus

The Bureau of Mines has been active in promoting the purchase of coal for Government use under specifications that define the requirements in terms of heating value of the coal , expressed in British thermal units , and the composition as shown by proximate analyses . To these , when required , are added the ash- softening temperature , the free- swelling index , and the Hardgrove grindability index . Under most of these specification contracts the bidders guarantee the quality of the coal , and that guaranteed by the successful bidder becomes the standard of his contract . The deliveries are sampled in accordance with instructions 4/ issued by the Bureau of Mines ; the samples are analyzed in the Bureau laboratory to determine whether the coal is of the quality guaranteed by the contractor and , if it is not , a price adjustment is made . Analyses of the delivered coal and tipple samples (samples collected at mine tipples as coal is being loaded into railroad cars or trucks ) provide valuable data for use in evaluating future bids . In addition , the continuous sampling of coal as delivered is a check on the practical results obtained in burning the coal . The Government purchased approximately 5 million tons of coal in fiscal year 1963 . In connection with these purchases , the Bureau analyzed 6,999 samples . These are published ( table 1 ) for the use of Government officials and the public . A series of publications has been completed on coal analyses by States or , where production is small in any one State , by groups of adjacent States . In addition to analytical data showing composition and quality of coals of the States , the publications contain brief descriptions

Jan 1, 1964

By Albert J. Rambosek

The objective was to obtain qualitative information on (1 ) the stress field in a core stub at the bottom, or face , of a cored borehole and (2 ) whether , and at what distance , in terms of core diameters from the face of the borehole , relief of stresses in the core is complete . The photoelastic and brittle lacquer techniques of stress analysis were used to determine the pattern of stresses in two- dimensional models , simulating the bottom of a borehole with a projecting stub of core . The core was stress- free at 1-1 /2 core diameters or more from the face of the simulated borehole . The analyses of the isoclinic and isochromatic patterns in the core near the face of the borehole reveal why core occasionally breaks into thin plates , when core or stress - relief drilling is attempted in highly stressed rock masses , such as heavily loaded mine pillars . stub broke away from the bottom in a hydrostatically loaded artificial rock specimen in a manner indicating that core " wafering" can result from tensile stresses developed in the core when a coring bit penetrates the highly stressed rock mass .

Jan 1, 1964

By Albert W. Deurbrouck

This report describes the preparation characteristics of the Pittsburgh and Upper Freeport coalbeds in Hancock , Brooke , Ohio , and Marshall Counties , W. Va . Over 4.5 million tons of coal was produced in these four counties in 1962. Most of this production came from the Pittsburgh coalbed . Twelve coal samples were collected for this study , 11 from the Pittsburgh bed and 1 from the Lower Freeport bed . Two of these samples could be upgraded to produce metallurgical - grade coal . The sulfur content of the Pittsburgh- bed coals was generally excessive --as high as 4.9 percent in the raw coal and 3.19 percent in the float 1.30 specific gravity fraction . The rank of the coals in this area ranges from high-volatile A to high-volatile B bituminous .

Jan 1, 1964

By F. W. Hoertel

Tungsten from the hydrogen reduction of WF was vapor - deposited to coat MERM (Material Evaluation Rocket Motor ) graphite and rhenium- lined graphite nozzles . These nozzles have surface configurations that preclude the conventional fabrication of high- density- tungsten liners . Operation at 550 ° C produced selectively placed uniform coatings of specified thicknesses at near theoretical density . An acceptable coating could not be deposited on a beryllia nozzle because of an undesirable side reaction between the substrate and one or more of the products of the reduction reaction .

Jan 1, 1964

By F. E. Block, Stephen D. Hill

The necessity for measuring radiation dose is encountered in studying both the beneficial and damaging effects of ionizing radiation on materials . It is also necessary to know the radiation dose absorbed by the reactants in order to evaluate the efficiency of reactions or processes that are promoted by radiation . Thus , a significant effort was made at the Albany cobalt 60 facility to investigate techniques by which the exposure radiation dose can be determined . Methods including ferrous sulfate , ceric sulfate , and methyl methacrylate chemical dosimeters , ion chamber dosimetry , and an absolute radiation calorimeter were investigated . Isodose curves were constructed for several standard source configurations using the dosimetry techniques which were investigated .

Jan 1, 1964

By Paul E. Bennett, James S. Browning, Thomas L. McVay

Continuous 1.0- to 1.5 - ton - per - hour pilot plant flotation tests were made to determine the technical and economic feasibility of recovering beryl from flotation tailing being produced at the spodumene concentrator of the Foote Mineral Company , Kings Mountain , N.C. Best results were obtained when using an acid circuit and amine - type cationic reagents to float a bulk beryl - feldspar concentrate and then selectively floating the beryl away from the feldspar , using a petroleum sulfonate collector . About 77 percent of the beryllium in the pilot plant feed was recovered in a concentrate containing 6.42 percent BeO . The capital cost of an integrated flotation plant capable of treating 500 dry tons of spodumene mill tailing per day for recovery of beryl and feldspar is estimated at $ 210,000 . Indicated direct operating costs for the plant were $ 1.52 per ton of dry spodumene flotation tailing treated . This approximated the value of beryl recovered , but potential profits of about the same magnitude lie in concurrent recovery of marketable spodumene and feldspar byproducts .

Jan 1, 1964

By H. R. Shell, Robert C. Johnson, Wilbur H. Warwick

Alpha silicon nitride fibers , Si3N4 , were successfully grown in graphite crucibles by a new method utilizing silicates and silicon ( S in equations below) as sources of silicon and using carbon , aluminum , and silicon as reducing agents (R in equations below ) . The basic reaction mechanism is believed to be generally as follows : 1,300 - 1,500 ° C S + R + N₂ SiO + RO + N₂ › 3Si0 + R + 2N₂ _1,300 - 1,500° C 3RO + Si¸N • ( 1 ) ( 2 ) A build - up of coatings on the solid raw- material particles hindered the evolution of silicon or silicon monoxide vapor and thereby slowed down further formation of silicon nitride fibers . Free oxygen in the crucible caused the formation of amorphous silicon dioxide ( SiO2 ) fibers . This problem was solved by passing , entering , and exiting gases through layers of lump graphite inside the reaction vessel . The silicon nitride fibers grew best around 1,400 ° C. Nitrogen flow rates from 4 to 6 liters per minute were adequate . The fiber widths were generally only a few microns whereas their lengths sometimes reached one - quarter inch or more . Chemical and X- ray analyses indicated that bulk fiber samples were usually 80 to 90 percent Si3N4 . The fibers had good oxidation resistance to about 1,260 ° C. Thermal shock resistance was excellent . Electrical resistance was determined .

Jan 1, 1964

By H. D. Hess, C. P. Mabie

This report describes in detail the results of petrographic research conducted on 21 phosphate ores representing important deposits in southwestern Montana , southeastern Idaho , and northeastern Utah . The ores are described and categorized by mineralogical and chemical composition , thermal behavior of organic carbon , and textural constitution . Descriptive and genetic classification schemes applicable to western phosphate ores are discussed ; results from related studies made of the collophane mineralogy are also presented . The latter studies were centered on determining unit - cell dimensions and CO₂ , P2O5 , and fluorine content of collophane concentrates of 11 high - grade phosphate- rock hand specimens selected solely for this purpose . On the basis of this investigation , operational methods have been developed for quantitatively describing textural and compositional features that are likely to be significant in determining the response of phosphate ores to conventional beneficiation treatments ; systems for classifying the ores in relation to these features have been proposed . Studies to date point out distinct textural and compositional variations in the western phosphates and illustrate their importance in determining optimum beneficiation procedure .

Jan 1, 1964

By D. W. Bridges, R. O. Dannenberg, Laird Crocker

Preliminary solvent extraction studies , reported by the Bureau of Mines (5) , have been continued and expanded to improve on the previous estimate of process requirements . The solvent extraction portion of the process was examined at a scale large enough to enable meaningful extrapolation of the results to geometrically similar equipment of plant size . About 82 pct of the beryllium was recovered from approximately 0.5 pct beryllium oxide (Be0) Spor Mountain , Utah , ore by a process involving ( 1 ) sulfuric acid leaching , ( 2 ) counter current decantation (CCD ) washing , (3 ) iron ( III) reduction by sodium hydrosulfide ( NaHS ) , ( 4 ) beryllium solvent extraction by di - 2- ethylhexyl phosphoric acid ( EHPA) , ( 5 ) caustic stripping of beryllium- bearing EHPA, (6 ) hydrolysis of sodium beryllate - caustic strip liquor , and (7 ) calcination of beryllium hydroxide (Be ( OH ) 2 ) formed in step (6 ) . The resulting beryllia assayed 98 to 99 pct Be0 and was suitable for most nonnuclear uses . Best overall results were obtained by using pH 2 , 1.6 grams of BeO per liter of leach liquor as feed and 0.25 N EHPA in kerosine containing 2 wt vol pct (grams per 100 ml of solution ) isodecanol ( IDA ) as solvent . Analysis of the data indicated that a commercial plant would achieve 95- pct overall extraction operating at 45 ° C with 20 hp per 1,000 gal of dispersion in each of seven mixer- settlers , having 290 gal per ton of ore hourly mixer capacity and 90 gal per ton of ore hourly settler capacity . At least 79 lb H2SO4 , 13 lb sodium hydroxide (NaOH ) , 3 lb NaHS , 0.25 lb kerosine , 0.07 lb polyacrylic flocculant , 0.03 lb EHPA , and 0.007 lb IDA would be required in H2SO4 leaching and subsequent processing to recover 1 lb BeO .

Jan 1, 1964

By Raymond W. Hiteshue, Sam Friedman, Martin D. Schlesinger

The Bureau of Mines in cooperation with the El Paso Natural Gas Co. investigated the effect of high temperature and pressure at short residence times on the hydrogenation of a New Mexico coal to gaseous and liquid hydrocarbons . The study was made in a bench - scale semicontinuous unit at pressures of 500 to 6,000 psig , 480 ° to 1,000 ° C , and residence times of less than 1 minute to 15 minutes . Ammonium heptamolybdate was impregnated on the coal to furnish 1 percent molybdenum based on maf coal . Coal could be rapidly hydrogenated at elevated temperatures and pressures to yield large quantities of gaseous hydrocarbons and small quantities of lowboiling oils , high in single - ring aromatics . At 800 ° C and 6,000 psig and a residence time of 1 minute , the yield of hydrocarbon gas was 43 percent and of liquid hydrocarbons 9 percent , based on maf coal . With a 15 - minute residence time , the yield of gaseous hydrocarbons increased to 68 percent with a decrease in yield of oil to 6 percent . At higher hydrogen velocities , the yields of oil were much greater but contained large quantities of asphaltene . Low concentrations of molybdenum (0.01 and 0.1 percent ) or a high concentration of iron ( 1 percent ) were ineffective at 800 ° C , 6,000 psig , and short residence time .

Jan 1, 1964

By Robert L. Rough, William E. Eckard

Laboratory data obtained from a Bureau of Mines rotary air core of a well near Sugar Grove , Warren County , Pa . , were instrumental in initiating hydraulic fracturing in the area to stimulate oil recovery from Glade sand oil reservoirs . This report outlines the general geology , lease development , reservoir- rock characteristics , and oil - production history of Glade and Clarendon sand reservoirs in Warren County . The methods of well completion for single- stage and multiple- stage hydraulic fracturing of old and new wells are discussed , and a range of hydraulic fracture treatment data from 29 Glade sand and 10 Clarendon sand wells is presented . A composite decline curve representing oil - production data from six wells shows probable results of hydraulic fracturing . Average cumulative oil production during the first 100 days after hydraulic fracturing with a sand - carrying liquid is compared with production after conventional shooting with liquid nitroglycerin .

Jan 1, 1964

By Harry R. Nicholls

As part of the pre- and post - shot mine examination at Project GNOME , acceleration data were recorded underground from a series of chemical explosive shots . The cube root of the charge weight was used to scale acceleration and distance because charge weight was not constant . Regression analysis of particle acceleration - distance data gave the following propagation equation : A W1 /3 = 5.10 x 105 ( R / W¹ / 3 ) −2 .43 The quantity A W1 /3 is scaled particle acceleration expressed in g's - lbs¹ / 3 , and R/W1 /3 is scaled distance expressed in ft / lbs¹ /3 Data obtained from the nuclear explosion were scaled and fall within one standard deviation of the calculated propagation law for the smaller shots . Cube root scaling laws were adequate to group acceleration data from explosive charges varying by a factor of more than 1 x 10 in charge weight and over shot - to - gage distances varying from 100 to 46,000 feet . Data obtained from a series of small tests provided sufficient data from which reliable predictions of acceleration could be made for the large nuclear explosion .

Jan 1, 1964

By M. E. Kundick, W. E. Dieter, L. Cohen

The major details of design and maintenance of a seamless stainless steel fume hood system , developed by the Bureau of Mines , are described and illustrated . Operating and housekeeping routines are outlined .

Jan 1, 1964

By A. Gene Collins, Cynthia A. Pearson, Cathy J. Waters

The chemistry of selenium and tellurium is discussed , along with a method of preparing a synthetic oilfield brine , an oilfield brine sampling method , and methods for determining selenium and tellurium in complex oilfield brines . Selenium either can be reduced to the elemental form with sulfur dioxide and determined semiquantitatively by color comparison of the red amorphous form or can be converted to selenite and determined quantitatively by reacting it with 3,3 ' - diaminobenzidine and obtaining its spectral absorbance at 420 mu . Tellurium can be reduced to the elemental form with hypophosphorous acid , and the spectral absorbance of its red hydrosol can be measured at 400 mu . Less than 0.05 mg / 1 of selenium and 0.1 mg / 1 of tellurium can be determined by the described methods .

Jan 1, 1964

By R. H. Harrison, D. R. Douslin

The thermodynamic properties H - H° , (H - H° ) /T , S - Sideal , S - S° Fide al F - F° , (F F° ) /T , and activity coefficient Y for perfluorocyclobutane were calculated as functions of temperatures ( 115.22 ° to 350 ° C) and molal density (0.75 to 6.5 moles / liter ) . Improved analytical and graphical correlating techniques are described .

Jan 1, 1964

By G. H. Cobb, J. L. Johnson, H. H. Heady

An infrared absorbance technique is described for analyzing anodic gases produced during the electrowinning of uranium , thorium , and rare - earth metals in molten fluorides . Typical components determined qualitatively in a gas sample are CO , CO₂ , CF4 , C₂ Fe , C3F8 , COS , CS₂ , and SiF4 . About 20 minutes are required to record and interpret the spectrogram , and report quantitative results for CO, CO₂ , CF4 , and SiF . The procedure is used for control during electrolysis .

Jan 1, 1964